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Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 1. Revision History Rev # Date October 30, 2008 1 2 3 October 30, 2008 October 30, 2008 October 31, 2008 4 5 6 7 8 November 1, 2008 November 2, 2008 November 2, 2008 November 2, 2008 9 November 3, 2008 Description Introduction, Customer Requirements and Project Background (Sections 2, 2.1) Blocks, Interface Definitions (Sections 2.2.2, 4.1.1) Block Diagrams (Sections 4, 4.1) Compile Project Research and Technology Review Analysis from Individual Reports (Sections 2.2, 2.2.1) Implementation Approaches (Section 3.1) Revision of Blocks (Section 2.2.2) Absolute Minimum Requirements, Desired Feature Set (Sections 2.3.1, 2.3.2) Fix Citations throughout document Revision of Block Diagram and Blocks (Sections 2.2.2, 4.1) Revision of Glossary and Citations, Color Coding, Formatting Details, Edit Absolute Minimum Requirements and Desired Feature Set, Testing (Appendices, Sections 2.3.1, 2.3.2, 6) Additional Block Descriptions, Add to Blocks Section (Section 2.2.2) Contributor(s) Ashley Mason, Todd Waggoner Adam Stone Todd Waggoner Ashley Mason Todd Waggoner Adam Stone Ashley Mason Ashley Mason, Adam Stone, Todd Waggoner Ashley Mason 10 November 3, 2008 11 November 18, 2008 Font Change, Grammatical Revisions Todd Waggoner 12 November 26, 2008 Block Interfaces and Operations (Sections 5.4, 5.5) Todd Waggoner 13 November 27, 2008 Block Interfaces and Operations (Sections 5.1, 5.2, 5.3) Ashley Mason 14 November29, 2008 Block Interfaces and Operations (Sections 5.6, 5.7) Adam Stone 15 November 30, 2008 Block Interfaces and Operations (Sections 5.1 – 5.7) 16 December 5, 2008 Fix font, Label figures and tables, Block Interfaces and Operations (Sections 5.1 – 5.3), Development Plan (Section 8), Testing (Section 6) Additional Seed Layer Comparison Table Todd Waggoner Ashley Mason, Adam Stone, Todd Waggoner Ashley Mason Page 1 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 December 6, 2008 Revision of Block Interface and Operations (Sections 5.4, 5.5), Updated Block Diagram (Section 5) Todd Waggoner December 6, 2008 Revision of Block Interface and Operations (Sections 5.6, 5.7) Additional Actuator Comparison Table Bill of Materials for Actuator Adam Stone 19 December 6, 2008 General Interface Definition (Section 4.1.1) Overall Review of Paper Fix Remaining Suggestions from TA Add Terms to Glossary Ashley Mason, Adam Stone, Todd Waggoner 20 December 7, 2008 Added Mechanical Test Platform Block Descriptions (Section 5.8) Ashley Mason, Todd Waggoner 17 18 Page 2 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 2. Introduction This project stems out of research from Georgia Tech [1]. Previous experiments showed that small amounts of energy could be harvested by coating Kevlar strands with ZnO (zinc oxide) nanowires. When the ZnO nanowires are stressed by linear tension and compression or axial bending they create an electric potential. This piezoelectric property of the ZnO wires is utilized by wrapping together two separate strands of Kevlar coated with these wires. The experimental set-up from Georgia Tech is shown in Fig. 1. A motor is used to pull on a string and actuate the Kevlar strands. On the other end is a spring that returns the strands to equilibrium between pulls. The details of the electrical connections are not shown. The project entails the design of three major sub-systems: synthesis of the nanowires the Fig. 1: Basic Experimental Set-up from Georgia Tech Review Article [1]. The electrical measurement circuit and important things to notice in this image are the wrapping of the fibers and the the mechanical actuation system. coatings on each of the Kevlar strands. For the growth of the wires, hydrothermal, solution-based methods will be pursued in order to allow the use of non-traditional substrates that would be destroyed by traditional furnace growths. Instead of temperatures approaching 1000° C, these nanowires are produced at less than 100° C. Following some initial research in this area by Zhong Wang at GeorgiaTech, the initial substrates of interest are Kevlar strands of fiber [1]. Since these decompose around 400° C, this low-temperature growth method essential. There are multiple steps to the growth process. To successfully grow the nanowires, a seed layer must be deposited. Given the capabilities at Oregon State University, the deposition can be done via Atomic Layer Deposition (ALD), RF magnetron sputtering, or a sol-gel approach. ALD will be the standard method due to having excellent reproducibility and uniform coverage across the entire substrate. Other methods may be used for comparisons to determine which processes yield the best nanowire for piezoelectric energy harvesting purposes. Once the wires are grown, they must be assembled into an actual energy harvesting system. Functionalized Kevlar strands need to be intertwined in order to provide contact between nanowires that will cause a mechanical stress essential to piezoelectric generation. To ensure a net flow of electricity, current should only flow in one direction. This is accomplished by coating one of the Kevlar fibers with a metal such as Al or Au. The difference in Fermi level of the metal and the conduction band of the semiconductor will produce a Schottky barrier that will act like a diode. Next, an electrical test system must be designed to measure the electrical output and ensure electricity is being generated. Due to the expected amounts that will be produced, a picoammeter must be used. This ensures that any small amount of current produced will be successfully detected. To apply an external force to the functionalized Kevlar circuit, a mechanical actuator will be designed. This will reproducibly pull at the Kevlar, causing the nanowires on its surface to interact and bend relative to each other. This bending causes a stress on the lattice and creates a voltage via the direct piezoelectric effect. Although this test bench is being designed around a certain experiment, the objective is to make the system alterable so that alternative materials can be used (such as polyethylene fibers instead of Kevlar, or a different piezoelectric in place of ZnO). Depending on initial measurements, the need to study alternative materials could become prevalent, and the actuation and measurement systems could be used to characterize multiple alternatives. This project is important because piezoelectric energy harvesting could be utilized to power small sensors or medical devices which should not be powered off of batteries. In theory, with enough of the ZnO enhanced Kevlar fibers, portable devices could be powered as well. For example, an exercise shirt could power an iPod. Power sources have been a weak point of electronic devices since the time of their origin. Smaller and lighter voltage sources such Lithium ion batteries and ultracapacitors can greatly increase the mobility of electronic Page 3 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 devices. Their major limitation is the need to be recharged often. Piezoelectric nanowires are different from other alternatives because they are an energy source, not an energy storage device. Another reason that this project is important to the research professor and sponsor is that it is a very controversial topic. Since the original results from Georgia Tech were published, other groups have tried to reproduce the original experiments and have been suspicious about where the power output is coming from. Researchers at the Max Plank Institute believe that the output is actually coming from the measurement circuit, rather than the ZnO wires themselves. Currently, no other data refuting the Georgia Tech claims has been published, so contributing to this research cause is critical. 2.1 Customer Requirements and Project Background The proposed platform will be used in order to study the accuracy of previous studies and to try and soothe some of the controversy around the originally published results from Georgia Tech. Since this project’s funding coming from a research grant, the various systems encompassing the project must be made to scientifically prove (or disprove) that piezoelectric energy harvesting is possible from nanowires. Because of research requirements, it is essential that everything made is well documented and can stand up to academic scrutiny for publication. The most important part of this design is that all steps must be repeatable and reliable between runs. There are also strict noise constraints because the measurements of interest are expected to be in the pA range. Ideally, the system should be small enough to be mobile, although this may not be critical because the bench should only be used in a low-noise environment. If needed, the entire apparatus should be able to fit into a dark box or Faraday cage to eliminate outside interference and generation of photocarriers within the semiconductor. For instance, moving the measurement equipment to Kelley Engineering Center for the Engineering Expo is probably not critical because of the noise that would be introduced by the surrounding projects. Instead of mobility, emphasis should be placed on the ease of building the system. Since other researchers should be able to utilize this test bench design, the building and analytical processes should be as simple as possible, low cost and well documented. This system should be able to function on its own rather than be part of a larger system. Results should be analyzed in-depth and be documented well enough to be published in peerreviewed journals. A reliable test system made within a short amount of time which is easy to build and highly accurate can resolve some confusion in the research world. As with a more conventional market, the research market is very competitive as far as publishing and the timelines that are associated with projects and results. The trade-offs to be cautious about here are the creation and evaluation of an accurate system and being prepared to publish in a reasonable time period. Lastly, the final materials used in the fibers and materials should be as easy to synthesize as possible. Working with chemicals can be a dangerous process, especially depending on the availability of required safety equipment. Since repeatability is critical for this system, the chemical processes will be under review. 2.2 Project Research While studying this specific research interest, it is important to review other similar technologies. One technology that can be used for the same purpose is that of thermopiles. Thermopiles are a collection of many thermocouples. Thermopiles generate an electric potential by drawing energy from heat. They only work where there is a thermal gradient. Thermoelectric generators have been developed for the human body. These can theoretically power devices indefinitely. By using the heat from the human body (most commonly the forehead) the thermoelectric generators can generate enough power to individually sustain some devices like a brainwave monitor [2]. The thermocouples are made of a silicon and germanium compound, poly-SiGe. This material was chosen to take advantage of the Thomson effect. Thermoelectrics use a temperature gradient created by heating one side and cooling the other to induce an electric potential. SiGe is a commonly used thermoelectric that is manufactured with an air gap in the center. The size of the gap is selected so that heat flow through the gap and through the SiGe is the same, ensuring maximum power output [3]. The SiGe is attached on either side by a silicon plate, one for the cooler side and one for the hot side as shown in Fig. 2. Page 4 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Fig. 2: SiGe thermocouple system [3] An efficient way to link many of these is in a rim shape. This topology creates an efficient thermal circuit where air can flow from the center outwards much like a desktop chassis. With current designs thermopiles can generate power in the milliwatt range indefinitely with a human heat source. Another interesting nanowire energy harvesting project are the photosensitive nanowires created by Harvard chemists. These wires are made of layers of three different types of silicon. With the different electrical properties of these different types of silicon the wires are photovoltaic. These can convert 3.4% of the energy from sunlight into electricity with up to a 5% efficiency [4]. Sunlight is one of the least power dense sources available, especially considering the low efficiencies of current photovoltaic devices. Harvard chemists believe they will be able to increase the efficiency of the nanowires by researching alternate internal structures for the nanowires. Another method of energy harvesting would be to use a micro-electro-mechanical system (MEMS) in the form of a linear inertial energy scavenger, Fig. 3. Fig. 3: MEMS Energy Harvester [6] If the MEMS uses an electromagnetic energy conversion system there would be a coil on the proof mass. Dampening changes the vibrational energy of the device into an electrical potential. The power output of such a device is highly dependent on the frequency of vibration, a drawback that piezoelectric nanowires do not have. These take a fairly complex system of micromachining to fabricate and cannot be made much smaller than the mm range with current technology [6]. The most important project to refer to would be the ZnO nanowire research that the Georgia Institute of Technology conducted recently. This research is somewhat different than other nanowire energy sources in that the nanowires are not meant to be stretched or compressed, but bent. The core of the fiber is Kevlar, for its strength and flexibility. There are 5 layers to each fiber: the inner-most being the Kevlar core, next is a layer of tetraethoxysilane (TEOS), a ZnO seed layer, another TEOS layer, and finally the ZnO nanowires. The outer surface is covered in radially grown ZnO nanowires. The TEOS layers help form better quality bonds with the other layers and improve the bending performance of the surface ZnO nanowires. Fig. 4 gives a diagram of the cross section of a fiber and shows SEM images of the ZnO nanowires. Page 5 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 The method of energy harvesting is to coat one fiber with a surface of gold (Au) and intertwine it with another fiber without Au. The gold creates a Schottky junction so that current is allowed to flow from the gold surface to the ZnO nanowire. As linearly axial vibrations are induced on the pair of fibers the ZnO fibers will be bent with respect to the gold coated fiber and generate an electric potential due to its piezoelectric properties. The efficiency of ZnO wires was found to be 17 – 30% [7]. These were tested and found to give a current output of ~5pA. The Georgia Tech researchers believe that the output current is smaller than expected, due to cracks in the seed layer. This damage significantly increases the fiber's inner resistance. The open circuit voltage was also measured to be ~1 – 3mV. This would mean the power output of a single fiber would be ~1 – 15fW (femptoWatts). In an attempt to increase power output, the researchers deposited a conducting layer onto the fiber before the ZnO layer, which decreased the inner resistance from 1GΩ to 1kΩ. The output current Fig. 4: ZnO nanowire cross section and SEM images [1] was found to increase from ~4pA to ~4nA, a factor of 1000. This shows that the inner resistance of the fiber is about linearly proportional to the power output. This means any method of reducing the inner resistance could significantly improve power output. The size, durability, and flexibility of these nanowires provide the ability to use them on clothing [8]. One issue with human-powered energy devices is where to place them for maximum efficiency. During different types of activities, the efficiency can change dramatically. It would be advisable to map out accelerations of different body parts for each of these activities by using accelerometers. This data could be used to find where to place piezoelectric nanogenerators to produce the most energy [9]. ZnO-coated Kevlar will be used as nanogenerators in this project because growth processes are wellresearched. As time allows, other materials outside of the original scope of the design project will also be studied. There are multiple methods to grow nanowires, and these methods become more complicated depending on the target type of wires as well as the substrate which the wires are being grown on. Although ZnO nanowires are most commonly made by gas-phase approaches, these methods require temperatures of 450 – 900 oC. Because of the needed non-traditional substrate, a different method must be explored [10]. Table 1 is a summary of different types of nanowires and their associated most common growth methods [11]. Because of the types of materials being looked at (piezoelectric growth species and Kevlar substrate), material options and processing temperatures are limited. There seem to be three main options if other materials are to be explored. The easiest would be continuing to use ZnO because this material is commonly worked with due to its many useful properties as a wide band-gap semiconductor. Not only is ZnO piezoelectric, but it is also used for its conductivity, high voltage-current non-linearity, sensitivity to various gases and chemicals, optical properties and catalytic activity [12]. ZnO has three key advantages over other related materials: it exhibits both piezoelectric and semiconducting properties (useful for sensors and transducers), this material is biosafe (can be used in medical applications with little toxicity) and ZnO exhibits the most diverse nanostructure configurations including nanowires, nanobelts, nanosprings, nanorings, nanobows and nanohelices [13]. One reason this project will initially use ZnO is due to the amount of synthesis research that has been done with ZnO over other materials. In a research sense, it could be more beneficial to explore these other options, but this experimentation may be outside the scope of this project. The benefits of BaTiO3 or PZT would be their increased charge constant (piezoelectric constant) in comparison to ZnO. BaTiO3 wires can traditionally be prepared in a “salt-assisted high-temperature solid-state chemical reaction”, which causes problems if Kevlar Page 6 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 strands are chosen as a growth substrate [14]. Either alternative growth methods of the BaTiO3 need to be examined or a replacement for the Kevlar that can withstand higher temperatures needs to be found for this synthesis [5]. Table 1: Materials and Methods Summary Table [10] Another aspect of this project is to examine multiple methods of measuring possible piezoelectric output. Many different picoammeters already exist on the market. The price ranges starts from as little as a few hundred dollars to over a thousand. This is a viable option, since the product is guaranteed to measure in the desired current range and has the least amount of uncertainty. Page 7 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Alternatively, Oregon State University has a number of older semiconductor parameter analyzers and picoammeters in Owen. These tools can likely be made to work, but are obviously a shared resource. Any connections to the equipment must be very temporary (based on BNC connections) so that other students may continue to utilize the devices as needed. In the electrical characterization lab on the third floor of Owen, the equipment includes: HP 4140B picoammeter and DC Voltage source, HP 4192A LF impedance analyzer, HP 4145B semiconductor parameter analyzer, and an Agilent 4156C precision semiconductor parameter analyzer. The HP 4140B is primarily used for dielectric breakdown testing and a control interface would most likely be necessary in order to take and store desired measurements. The 4145B and 4156C are currently attached to probe stations inside of dark boxes. Design considerations must be taken to bypass the probe stations without interfering with anyone else’s future measurements. Additionally, the 4145B and 4156C use a Source Monitor Unit (SMU) to apply a voltage through a semiconducting device and measuring current response. It’s currently unclear if these will read desired currents without an applied voltage bias. The last option is to design and build something in-house. A few sample picoammeter circuits are available online, but SPICE analysis would be necessary to determine possible viability. Building something has the least guarantee to work, but gives the most customizability. There are current Opamps in the marketplace designed for use within picoammeters, such as the CA3420 from Intersil [15]. In general, picoammeter circuits are very similar to a standard Digital Multi-Meter (DMM). The main difference is in a burden voltage. This is the voltage drop across the measurement device, and should be as low as possible. Input current is another important consideration for amplifiers in a picoammeter circuit. The CA3420 has a fairly constant input current of 1 pA, an important consideration in this case. Fig. 5: Low Noise Opamp Circuit [15] Page 8 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 2.2.1 Technology Review Analysis – Systems Overall Comparision The following table is a comparison between ZnO energy harvesting technology and other alternative energy sources, a brief summary can be found after the tables. The relative terms in this table (large, medium, small, easy, difficult, etc.) are used to compare different technologies. Although these terms are not quantifiable the comparison chosen is sufficient for this overview. Table 2: Similar Technology Comparison Table Technology Efficiency Ease of manufacturing Size (relative) 17-30% Power Output Relative nW range (small) ZnO nanowires Medium Very small Photoelectric nanowires Thermo couples 3.40% pW range (very small) Medium Very small 3-7% Medium Medium MEMS electromagnetic MEMS electrostatic ~20% mW range (relatively high) nW range (small) Medium-difficult Medium ~20% nW range (small) Medium-difficult Medium MEMS piezoelectric ~20% nW range (small) Medium-difficult Medium Wind ~50% W range for vehicle adapted wind Easy Very large Solar cells 30-60% mW range per cell Easy-medium Large EM converters ~60% pW range (very small) Medium Large Technology Effect on movement Durability Reliability of application Lifetime Environmental Impact ZnO nanowires Negligible Durable Dependent on frequency of stress Undetermined Unknown Photoelectric nanowires Negligible Less than ZnO Dependent on light Undetermined Unknown Thermo couples Slight Very durable Very reliable with a human source Long Recyclable MEMS electromagnetic Slight Somewhat durable Dependent on frequency of stress Medium Recyclable MEMS electrostatic Slight Somewhat durable Dependent on frequency of stress Medium Recyclable MEMS piezoelectric Slight Somewhat durable Dependent on frequency of stress Medium Recyclable Wind Noticeable Reliable Short Recyclable Solar cells Noticeable Dependent on light Medium Recyclable EM converters Slight Somewhat durable Somewhat durable Durable Reliable depending on location Long Recyclable Page 9 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 ZnO nanowires: Some strengths are that they are very small and light and can be attached to the surface of clothing. Also, they are not noticeable in weight to the wearer. The power conversion efficiency is also very good. The Kevlar core of the fibers ensures excellent durability and flexibility. The best point about this technology is that it is exactly what is trying to reproduced. Some of the difficulties are growing wires with consistent structures. There are also questions on the validity of this technology. Photoelectric nanowires: Some of the positive things about this are that they can be interwoven with clothing, and are negligible to the wearer. Some of the drawbacks are that they are less durable than the ZnO nanowires because of the 3 layers of silicon that make up the wire. It also has a low efficiency. This coupled with the fact that its power source is relatively low in power density (sunlight) results in its low power output. All three MEMS devices can be described here. The positive aspects are that they have a higher power output ratio per device than any of the nanowires. Another is that they are a proven technology and already in the marketplace. Some drawbacks are that they have a shorter lifetime than other technologies because of their moving parts. Also it takes a significant amount of micromachining to create each device. Wind: Mobile versions of wind power have mostly been developed for vehicles. It has not been very popular due to competition with other technologies, its size, and also can have a noticeable drag effect depending on the way it is designed. The positives are that it can have a higher power output than other energy harvesting techniques. Solar cells: Positives are that they have good efficiency compared to other methods, and easy to manufacture. They have a significant size which severely limits their mobility. EM converters: Small size and micromachining requirements are limited. Power source density is low, which results in a low power output. Page 10 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Method Comparison The following tables are a comparison between different growth mechanisms for nanowire synthesis. Table 3: Method Comparison Table Wire Length Wire alignment Aspect Ratio Density Process Time Hydrothermal using Hot Plate [1,10,11] 1.5 – 2 µm Can obtain good alignment, (± 10o from perpendicular) Wires are usually grown pretty dense, hopefully should still allow enough space for bending Typically 10 – 12 hours, can see growth in as little as 2 hours Vapor-Solid [25] VLS [24] 3 – 10 µm ~ 20 µm Aligned Aligned Using Zinc Nitrate and HMTA can only get ratios of up to ~50, can introduce extra items into solution to help with this problem ~ 100 25 – 75 ~ 1 hour 1 – 1.5 hours Hydrothermal using Microwave [26] ~ 300 nm Can obtain good alignment, (± 10o from perpendicular) Sparse Depends on patterning of catalyst nanobeads Same as with Hydrothermal ~3 3 – 15 minutes Temperature Uniformity Method Difficulty Level Required Equipment Hydrothermal using Hot Plate [1,10] ~ 80 oC Fairly simple Vapor-Solid [25] 600 – 1000 oC Hotplate, solution, Zinc Nitrate, HMTA, thermometer, stirrer Furnace, Gases, Precursors, deposition tool for seed layer VLS [24] 600 – 1000 oC Good uniformity, problems stem from cracks in seed layer Good uniformity within only a few cm range in furnace Uniformity depends on catalyst Hydrothermal using Microwave [26] ~ 80 – 100 oC Good Fairly simple Moderately simple, requires patterning of gold catalyst Easy Furnace, Gases, Precursors, deposition tool for gold catalyst Solution and microwave For this project, available choices are mainly between the Hydrothermal Hot Plate and Hydrothermal Microwave methods because of the breakdown temperature of the Kevlar. The Hot Plate method has been known to give a better aspect ratio, but the Microwave method takes significantly less time. Page 11 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Material Comparison The following tables are a comparison between piezoelectric materials which could potentially be used for this project. Table 4: Material Comparison Table Crystalline Structure Toxicity Ease of Processing Cost of Production Other applications ZnO [10, 16] Wurzite Easy, massproduced Cheap, easily made precursors Laser diodes, LEDs BaTiO3 [5, 17, 18] Perovskite Easy in smaller quantities Moderate Capacitor dielectric, Thermal switches PZT [19] Perovskite Biosafe, safe except for ZnO fumes Usual warnings with handle (do not inhale, wear gloves, etc.) Lead poisoning, not fully investigated Moderate, hard to control Zr/Ti ratio Cheap in small quantities FRAM, ceramic resonators GaN [20] Wurzite LEDs, solar cells Wurzite Difficult, requires sapphire, ZnO or SiC substrates for highly crystalline material, hard to scale up Mass-produced, easy to form Expensive substrates, normal crystals can be cheaply produced CdS [21, 22, 23] Not fully investigated, dust is irritating to skin, lungs and eyes Toxic to kidneys, lungs, liver, suspected carcinogen Cheap Solar cells, photoresistors Piezoelectric Constant Lattice Constant (at 300 K, in Å) Seed Layer Growth Amount of Research ZnO [5, 16, 21] BaTiO3 [6, 18, 18] Low High 4.580 4.020 Sputtering, CVD, ALD Sintering BaCO3 and TiO2, Hydrothermal PZT [5, 19] High a=3.992; c = 4.108 CVD, Sol-Gel GaN [5, 20] Low a=3.189; c=5.185 MBE, MOCVD CdS [21, 22, 23] Moderate a=4.160; c=6.756 MOCVD, Sputtering, Sol-Gel Most common for nanowires Research into variance of refractive index, research switched to PZT when it was discovered Some for MEMS, AFM cantilevers Well researched for blue LEDs, lasing Well researched in alternative applications, nanowire research less common Page 12 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Seed Layer Coating Comparison The following table describes three different methods which can be used for thin-film deposition. In this project these techniques are being compared to determine the best option for the seed layer coating. Only relative terms (short, medium, high, low, etc.) are needed in this comparison. Table 5: Seed Layer Coating Comparison Table Sputtering ALD Sol-Gel Precursors or Sources Solid target of deposition material is used Non-reactive argon plasma Chemicals in gas phase Substrate Limitations Works for flat substrates Vacuum Condition High vacuum required Processing Time Medium Works for all substrates Long Chemicals in liquid solution Works for all substrates Low vacuum required Vacuum not required Short Measurement Comparison The following tables are comparisons of possible measurement technologies which could be utilized. Table 6: Measurement Technology Comparison Table Resolution HP 4140B [3] HP 4145B [4] Agilent 4156C [5] CA3420 [27] Keithley 6485[7] Keithley 6487 [8,9] 1 fA 50 fA 1 fA Unknown 10 fA 10 fA Minimum Range (+/-) 1 pA 1000 pA 10 pA 1.5 pA 2 nA 2 nA AD795 [10,11] Teltron 2808 [12] Transimpedance Amplifier [13] 1 pA Unknown 0.1 pA 4 nA 200 pA 204.6 pA Integration Time HP 4140B [3] HP 4145B [4] Agilent 4156C [5] CA3420 [27] Keithley 6485 [7] Keithley 6487 [8,9] 133 ms 3.6 ms Unknown 2 µs 1 ms 1 ms AD795 [10,11] Teltron 2808 [12] Transimpedance Amplifier [13] 100 µs Unknown 120 µs Accuracy @ Min. Range 5% 1% 4% Unknown 0.4% 0.3% Unknown Unknown Unknown Voltage Burden Estimated Cost Free Free Free Obsolete Need Quote $2995 ~$10 with sampling IC $355 ~$25 Display (digits) <10µV Unknown Unknown Unknown <200µV <200µV 3½ N/A N/A * 5½ 5½ Unknown Unknown Unknown * * 4½ Portability Minimal Minimal Minimal Good Medium Medium Good Good Good Utility Beyond Original Project Good Good Good Little Medium Medium Little Poor Medium *Need DMM or some other measurement device to obtain output. Page 13 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 The transimpedance amplifier shown in Fig. 6 uses an integrator, switching a large feedback resistor for a capacitor and using hold or reset switches. In the specific example cited, it also uses a LM555, EPROM, and LCD display. The LM555 handles timing for integration and the EPROM holds look-up tables to match the voltage output to a corresponding four-digit picoamp equivalent. This look-up is done based upon an A/D converter's output. The EPROM data is then output to an LCD driver and displayed for the user. Fig. 6: Fast-Settling Picoammeter [33] For this project, one of the most important parts will be to test the nanowires. Therefore, a test bed needs to be created to accurately measure the induced voltage of a stressed wire. The stressing of the wire also needs to be very accurate. Although project goals include looking for a way to test the functionalized Kevlar strands, a starting place could be testing a single wire. One possible setup could be one that researchers at the University of Illinois used to apply tension to BaTiO3 nanowires [5]. The setup is illustrated in Fig. 7. Fig. 7: Testing setup from University of Illinois for testing a single BaTiO3 nanowire [5] The piezostack is used to apply tension to the mobile base at low frequencies (~30Hz). In this experiment the energy harvested was in the attojoule range so the charge amplifier (in this case the A250F, Amptek, Inc.) is needed to amplify the current to a level of magnitude high enough to accurately measure it. The nanowire was Page 14 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 fixed at both ends using a localized electron beam to deposit platinum (Pt) inside a scanning electron microscope (SEM). Fig. 8 shows the amplification circuit in schematic form. Fig. 8: Schematic representation of testing system [5] The current source represents the nanowire under stress generating an electric current. Rnw is the total resistance of the nanowire and Cnw is the total capacitance, including parasitic capacitance, of the wire. The current can be modeled by: i is the current, d is the charge constant, and E is the Young’s modulus of the piezoelectric element, F (1) is the applied load, A is the load area, and epsilon is the resulted strain [5]. The project will require development of a mechanical actuation system. Although the procedure described above is helpful in intermediate testing the final product will have to be different. Fundamentally, this actuation device will be used to stretch the Kevlar strands relative to one another. In order to have the best design for this project, each piece needs to be examined separately and the best choice for that part should be made. Actuation Technology Comparison A comparison table for actuating technologies is shown below in Table 7. Table 7: Actuation Technology Comparison Table Positional Accuracy Range Speed (max) Cost Power VCS-10H [38] ±200nm 10mm 20,000mm/s $1500 ±12V to ±24V DC T-LA13 [43] ±0.1μm 13mm 4mm/s $782 15V DC FA-MS-8-12-4" [44] Unknown 4inches 44.45mm/sec $75 12V DC Mini 0 [45] Unknown 100mm 40mm/s Unknown 24V DC Pro165 Linear Stage [46] ±6μm 600mm 300mm/s “low”; otherwise unspecified Unknown Page 15 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 2.2.2 Technology Review Analysis – Blocks [B1] Seed Layer Coating: This block is required to produce a ZnO seed layer. The seed layer is a thin film, coating the entire Kevlar strand and provides nucleation sites for nanowire growth to begin. Without the seed layer, nanowires would not grow on the surface because there is no compatible crystalline structure on the bare Kevlar. The seed layer can be deposited in a number of ways at Oregon State University and is tabulated below in sub-blocks B1B, B1C, and B1D: [B1A] TEOS: TEOS Attributes Enhances bonding strength between Kevlar substrate and seed layer Improves mechanical performance of fiber Cross linked chains bind the bases of the nanowires together with more strength Without the TEOS layer there were problems with the bonding between Kevlar and the ZnO seed layer. TEOS not only enhances the bond strength, but also binds the bases of the nanowires together so that the fiber can be flexed and bent at greater angles. [B1B], [B1C], [B1D] Seed Layer Deposition: Methods Strengths Sputtering Evenly distributed across sputtering surface Accurate thickness of deposition layer Atomic Layer Deposition (ALD) Very uniform deposition surface Do not have to rotate Kevlar Sol-Gel Solution based Weaknesses Requires high vacuum Requires rotation of Kevlar strand for uniform coverage Slow Expensive, flammable precursors Non-uniform deposition layer for a cylindrical substrate Low temperature Sputtering and ALD both produce very even deposition layers. ALD will be used because the Kevlar strand does not have to be rotated and the tool is owned by the research professor. Page 16 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 [B2] Hydrothermal Nanowire Growth: This block is the single most important piece of the entire system. This project is research based, trying to find an optimal method and procedure for ZnO nanowire growth. The nanowires must be of sufficient size to ensure proper contact between Kevlar strands. Methods Microwave Hot plate Strengths Temperatures do not exceed Kevlar breakdown temp. Equipment needed is readily available and generally inexpensive Growth time is 3 to 15 minutes Lengths and widths of nanowires close to desired values Inexpensive equipment Weaknesses Shorter and wider nanowires than other methods Unwanted crystal deposition during growth process Much more growth time than other methods Uses more power than microwave Kevlar makes a good substrate due to its very high tensile strength and flexibility. Unfortunately, it breaks down at temperatures needed for other growth methods. The only remaining growth options for a Kevlar core are hydrothermal growth methods. Growth time is significantly longer for the Hot Plate method than the other method, but lengths and aspect ratios are closer to the desired results. The Microwave method cuts down the growth time significantly, but the process seems to be very length limited. There are other agents that can be added to the chemical solution to limit growth in one direction and increase aspect ratio. In both of these methods unwanted crystal deposition can be remedied with sonication. Although the bonding between the Kevlar core and the seed layer is not ideal, it has been improved using a TEOS layer. [B3] Wound Kevlar: Au coated Kevlar Strand Coated with layer of Au ~300nm thick Au acts as Schottky barrier allowing current to only flow one way Movement of Au coated nanowires is considered negligible Kevlar Strand Nanowires on the Kevlar strand act as cathode for the Schottky junction with the Au coated nanowires Nanowires are bent from pressure from the Au coated nanowires The piezoelectric properties of the ZnO nanowires generates an electric current The functionalized Kevlar strand pairs act together to form a voltage potential across the surface. When the gold coated wires press against the uncoated wires, both will bend. This causes a voltage potential across a nanowire’s diameter to be produced from the strain on the crystal lattice. The gold has a sufficiently different work function to create a Schottky barrier. This prevents current from flowing as the Kevlar strands move back to equilibrium when the nanowires would be bent the other way. In essence, the gold is essential to creating a rectifier that ensures a net current. Page 17 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 [B4] Picoammeter: The picoammeter block allows for testing of any piezoelectric power generation from the actuated Kevlar strands. The data provided by this block is what will actually be analyzed to determine the usefulness of this novel approach of energy harvesting. Without it, there is no quantifiable information to propose and support a theory with. Device Existing devices on OSU campus Implement custom design Purchase an existing one Advantages No cost, local, no design or build time Able to design to custom specs No design or build time, accurate and reliable measurements Disadvantages May not fit project needs, may not be able to get access to it Time to design, acquire materials, and build Cost, finding one with enough accuracy The most ideal situation would have been to use the equipment that is on campus. This equipment would have the advantage of no cost, no design and build times, and accurate results. A limiting factor is that the integration time for sampling may be too long, and something that samples faster might have to be pursued. The equipment already on campus would have been able to meet the requirements of the original project. Recent redesigns have made the design of a picoammeter circuit in parallel ideal. One of the desired requirements for this project is having a working display at the engineering expo. Since the picoammeter on campus is a public piece of equipment, it cannot be removed from Owen. The design of a picoammeter circuit will allow the creation of a portable display. [B4A] Probes: Probes Features Sense voltage across stressed fiber Fixed positioning Concerns Capacitance added to the circuit due to the probes EM noise coupling Probes are needed to detect any induced voltage across the fibers. Capacitance added to the circuit by the probes could be significant because of the very low power levels expected. The length of the probes could be a problem — if too much EM noise couples onto them. This could greatly distort the outcome of the measurements. [B4B] Amplifier: Amplifier Features Amplifies induced voltage to attain clear measurements Low noise opamp Concerns Enough gain to detect picoamp signals EM noise The purpose of the amplifier is to boost the signal to a measurable quantity. Opamps are usually a significant source of noise at such low currents. To get around this, more expensive BiCMOS or JFET technologies can be used to produce a very low-noise opamp. No matter what is done to make a more ideal amplifier, input impedance and noise will be the primary factors that could limit useful measurement ranges. Page 18 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 [B5] Computer Processing: This block allows for logging data measurements and performing calculations on the measured data. It is essential to fit measured data to the input frequency and amplitude of actuation to see if there is any actual energy harvesting. Logged data can either be input directly or with a USB thumb drive. If it were to be input directly through a port, this would require an additional ADC circuit to convert the analog voltage output of the picoammeter into a digital value. To use a thumb drive, all that would be required is a digital oscilloscope with the capability to save logged data to such a thumb drive. Useful Programs Excel HyperTerminal Windows XP Advantages Allows for data logging Familiar and very customizable interface Easily interchangeable and upgradeable [B5A] I/O: I/O Devices Keyboard Mouse Monitor Flash drives Standard USB interface Standard USB interface Standard LCD Removable This is the general I/O interface with the PC. Standard I/O capabilities for user input, data storage, and viewing are required. [B5B] PC: Features Able to interface with various equipment such as picoammeter or motor controller Programming of the controller Stores Results Software to record measurements Inexpensive This will be a basic computer setup with measurement software, and an interface to the controller. Must be able to run and compile C programs. This is what will be used to program the controller. [B6] Actuator: The actuator is essential to providing the needed strain on piezoelectric nanowires for voltage generation. Without it there would be no test to see if the nanowires are suitable for piezoelectric energy harvesting. The block must also be flexible enough to allow for a variety of input frequencies and amplitudes in order to find the most ideal test conditions. Strengths Voice coil provides unrivaled speed and position resolution Allows for simple attachment of Kevlar Controlled with microprocessor for control Weaknesses Motor coil will need to be shielded to lower inductive noise with measurement circuit Maximum stroke of 10 mm Page 19 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 This actuator uses a simple voice coil motor that simply pushes or pulls a coil of wire. The actuator may be problematic due to using an electric motor since it will inherently generate noise. This must be overcome with adequate shielding and distance from the actual Kevlar. The actuator must also allow for the easy attachment of the Kevlar strands to be tested. Since the Kevlar has a diameter of 14 µm, it must be able to apply strain without damaging the Kevlar or interfering with the electrical measurements of the Kevlar. [B6A] Spring: Strengths Simple Replaceable or Upgradeable Weaknesses Possible to overstretch Force constant must be compatible with motor (< 1.5 lbs/ 10 mm) Potential for oscillations The spring allows for one side to remain firmly attached and helps prevent applying too much force on the Kevlar. The spring also helps return the Kevlar to equilibrium, although it is possible oscillations will cause the Kevlar to slacken and unwind in some way to affect uniform measurements. Note that this might not appear in the final design if it is determined to be unnecessary. [B6B] Mounting Brackets: Strengths Simple and reusable Interchangeable Weaknesses Might damage seed layer and affect conductivity of Kevlar Potential to interfere with electrical measurements by adding unknown capacitive effects Constant location for ensuring equal test lengths between different samples Mounting brackets will be used to attach the Kevlar to the voice coil and spring. This allows for it to remain in tension during testing. The specific design is not finalized due to concerns about lowering the overall conductivity of the Kevlar and interfering with the electrical connection to the picoammeter. [B6C] Voice Coil: Strengths Simple design Built-in positional feedback circuit Maximum bandwidth of 1 kHz Weaknesses Limited to 10 mm stroke Low constant force (1.5 lbs.) 200 nm repeatability which is higher than the associated controller for it Sub-micron positioning resolution (150 nm) No commutator Voice coil motors are one of the most simplistic types of motors. By applying a current to a coil, a magnetic field will be created that attracts it toward or repels it away from a permanent magnet that surrounds the coil. Altering the magnitude and direction of the current, this coil can be easily made to move backwards and forwards at a given frequency. A coil is also simple enough that it is easy to control its position relative to the magnetic stator. By attaching the strand of Kevlar to this motor, the desired actuation can occur that will affect the piezoelectric nanowires. Page 20 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 [B7] Controller: This block handles all commands to the linear actuator. It ensures that actuation of the Kevlar fiber remains consistent in both amplitude and frequency during testing. The block is programmed by a PC which allows for a simple interface with no learning curve. This block is essential to ensuring a repeatable test that can be performed on any number of Kevlar strands. Strengths 16-bit A/D Converter allowing for 150 nm resolution with specified voice coil Programmable through standard RS-232 connection Can be programmed to produce accurate sine waves Weaknesses Extra piece of equipment with associated cost Limited programmability Needs external power supply The controller will be used to hand I/O for the voice coil motor [B6]. This allows for very accurate and precise control over the position of the motorized stage. Additionally, it will protect the motor in case it draws too much current or overheats. Since it can be programmed via HyperTerminal, accurately varying the frequency and amplitude of motion will be easy to accomplish up to 10 kHz, far beyond the desired range for this project. [B7A] Motor Power Supply: Strengths ±12V to ±35V DC 10 A peak Current limiting Internal current amplifier Weaknesses Built-in, so no adjustments can be made Poorly defined in datasheet Single-phase output (No AC Motors) Requires interface with PC The SCA 814 Servo Controller includes a ±12V to ±35V DC current amplifier with a 10 A max supply. This allows for complete control over the motor to come from the controller, without worrying about connecting another power supply for the motor. This will also act as a current limiter to prevent damage to the motor while still ensuring it can supply necessary peak current during actuation. [B7B] A/D Converter: Strengths 16-bit 150 nm resolution with 10 mm stroke motor Weaknesses Resolution dependant on full stroke of motor Poorly defined in datasheet A 16-bit converter allows for superior measurement capabilities. The control this offers is greater than desired, but this allows for finely tuning the amplitude of actuation on the Kevlar strands. It also ensures that every cycle has uniform amplitude and consistent timing. [B7C] Microprocessor: Strengths RISC Upgradeable Weaknesses Limited access to programmability Uncertain of specific capabilities RISC architecture allows for an inexpensive processor to easily interface with the I/O of the controller. It is also programmable so that any sort of desired waveform may be produced and output to the motor. The processor ensures that the voice coil goes to a desired location without going too far. Page 21 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 2.3 Feature Set 2.3.1 Absolute Minimum Requirements The following list of minimum requirements is necessary to ensure that the project is working properly. In order to pursue this project, the system must be well-characterized and proven so that no doubts are cast upon the measurements taken. Each piece of the project must be strong both on its own and on a system level. There are specific requirements for the grown nanowires to give the best chances for piezoelectric generation. Constraints should be put on both the mechanical actuation system and the electrical measurement circuit so that the designs are carefully contemplated. By meeting all of the requirements, 100 points will be received. Each requirement is weighted by relative importance. Well-defined method of nanowire production that repeatedly produces aligned ZnO nanowires. * (7 points) Nanowire at least 1 µm in length and have an aspect ratio of at least 10:1. (7 points) Nanowire density must be low enough to allow movement in the wires but high enough to ensure enough output that it is detectable (10 – 50 µm-2). (7 points) Adhesion of seed layer to Kevlar can withstand actuation for 100 cycles without showing signs of separation. This ensures durability of the seed layer and uniform wire coverage on the Kevlar. (15 points) Picoammeter circuit must accurately be able to measure in 50 pA quantities to adequately test nanowires output. (15 points) Sample rate of electrical measurements must be a minimum of 1 kHz. This ensures sampling at a rate much greater than the input frequency from the actuator. (7 points) Kevlar attachment to mechanical actuator must allow for replacement of different samples. (15 points) Mechanical actuator must have positional precision of at least 0.1 mm so as to make a repeatable set of input forces. (5 points) Mechanical system should not interfere with electrical measurements, ie. any noise from a motor should be filtered out. * (7 points) Pull on Kevlar should be adjustable (from 0.1 to 5 mm if necessary) to find an optimal stroke that stresses system without permanently damaging the Kevlar and nanowires. * (5 points) Mechanical actuation system must have a variable frequency of 1 – 20 Hz. (5 points) Analysis and theory of results. * (5 points) * Certain requirements cannot be firmly quantified. Whether these requirements have been met will be evaluated by the research professor. Page 22 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 2.3.2 Desired Feature Set The following goals are those that have been deemed less critical to success. Given time and resources, an effort to achieve these goals shall be made over the course of the project. Failure to achieve some or all of these points not affect the basic ability to characterize as-grown ZnO nanowires. The desired requirements can be worth a total of 50 extra credit points. Examine possible alternative materials such as polyethylene fibers instead of Kevlar, other piezo materials rather than ZnO, aluminum rather than gold for a Schottky barrier, etc. * (10 points) Compare results from piezoelectric and non-piezoelectric growth materials. * (5 points) Nanowires should be 3µm long with an aspect ratio over 100:1. These would most likely improved results. (10 points) Electrical measurements sampled at 0.5 MHz or higher. This will better show any spikes in current as the system tries to reach equilibrium. (5 points) Entire system portable and stable enough to exhibit a working test procedure at Engineering Expo. (15 points) Change mechanical actuation frequency to 100 – 200 Hz and determine the effects of higher frequencies on material breakdown. (5 points) * Certain requirements cannot be firmly quantified. Whether these requirements have been met will be evaluated by the research professor. 3. Architectural Overview The piezoelectric energy harvesting project entails the growth and characterization of piezoelectric nanowires. ZnO nanowires will primarily be used, though other materials are of interest if time allows. ZnO was chosen primarily for having a well-characterized growth method compatible with the chosen substrate material. Most methods of growing nanowires involve a furnace at temperatures approaching 1000° C. Since Kevlar is used as a substrate, it decomposes above 400° C and a low-temperature method is needed. Hydrothermally grown ZnO allows for nanowires to be deposited in a solution of water, below its boiling point of 100° C. The Kevlar substrates must be functionalized with nanowires, and the nanowires must be suited for piezoelectric purposes. The growth method must be tailored to produce single-crystalline [0001] ZnO nanowires of at least 1 μm in length. Additionally, the wires must be aligned normal to the Kevlar's surface. To test the nanowire structure, an actuator must be used to apply an external modulus. The Kevlar attached to this actuator must be consistently wound between samples to ensure consistency. In addition, the linear actuator must be controlled with a precision down to 0.1mm. The actuation system must also allow for easy connections of an electrical measurement circuit to the Kevlar strands. The electrical test circuit will consist of a picoammeter designed to measure currents down to 1 pA. This system must be able to measure data over time at a sampling rate of at least 1 kHz. Any noise on the circuit should be tested and accounted for. Any output from the functionalized Kevlar must be significantly larger than the background levels of noise. The measured data should be stored for analysis and comparisons between different experimental trials as well as for control runs. Page 23 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 3.1 Implementation Approaches Option 1: Microwave Growth of ZnO Nanowires HP 4140B Picoammeter and DC Voltage Source CA3420 Opamp picoammeter circuit Equipment Solutions VCS10H [38] Equipment Solutions SCA814 Linear Servo Controller [39] Producing ZnO nanowires with a microwave was chosen because of its growth time. The nanowires can be made in as little as five minutes, making it possible to produce as many test samples as required. Microwaves are inexpensive and easy to attain, which makes the process cost-effective. The HP 4140B was chosen because of its availability in the EECS Electrical Characterization Lab in Owen Hall. Its datasheet suggests being able to measure down to 1 fA. This is mostly likely due to a voltage burden of less than 10 µV, which is the best of all researched possibilities. A picoammeter circuit using the CA3420 opamp is being designed so a portable display can be at the expo. The HP 4140B will still be necessary to characterize the designed circuit. A voice coil motor was chosen because of its simplicity in design, fast response time for attaining higher frequencies, and positional resolution. A controller is attached to the voice coil to ensure consistent timing and position of the voice coil. Option 2: Hot Plate Growth of ZnO Nanowires Agilent 4156C Precision Semiconductor Parameter Analyzer Firgelli PQ12S Linear Actuator Hot plate growth uses the same reactants as the preferred microwave method. The only difference is that heat is applied to the solution via a hot plate instead of microwaves. Initial microwave results showed shorter and broader NWs than obtained from a hot plate. If this cannot be improved, hot plate growth will most likely provide the best wires for testing. Since growths take a minimum of 12 hours, development of this method should be done in parallel to microwave growths. The Agilent 4156C was chosen because it has a better integration time than the picoammeter, meaning it can sample more quickly. The resolution will suffer slightly as a result, but should still be acceptable depending upon input noise. Noise might be a factor because semiconductor parameter analyzers use a Source Measure Unit (SMU) that generally sources voltage to a semiconductor and measures current response. Actuation can be accomplished with a Firgelli PQ12S Linear Actuator. The unit has small size, but is not as responsive or accurate as a voice coil. Motor noise will be less of a problem, and the control could be as simple as applying a sinusoidal waveform through an amplifier to power the actuator. Option 3: AD795 Precision FET Opamp Microwave Growth of ZnO Nanowires Futaba S148 Analog Rotary Servo [40] Linear Servo Conversion Kit [41] The AD795 IC provides very low input current and sampling of up to 0.5 MHz. The associated circuit has a maximum bias current of 1 pA and the faster sampling rate should help to reduce noise in the circuit. A potentially inexpensive alternative for actuation uses a Futaba S148 rotary servo converted to a linear servo. This provides accurate control but servos tend to be much slower and this may limit the actuation frequency range. There are only two options for growth methods, so the more efficient method is chosen. Page 24 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Option 1 is chosen because of its quick approach to characterization. Microwave-based growth provides the quickest method of nanowire synthesis. This allows for many growth runs in a shorter amount of time, making it much faster to begin characterization and process optimization. The picoammeter is ready to be used in Owen, although different probes will be used for this sensing application. The HP 4140B can also be used to characterize an additional designed circuit. A picoammeter circuit using the CA3420 opamp is being created so a portable display can be at the expo. Using a voice coil motor provides simplistic operation, especially when coupled with the servo controller. Since the microcontroller is from the same company, compatibility is assured. The voice coil will provide the most positional precision of any other alternative as well as the largest frequency range. Given possible shortcomings of this option (nanowire lengths will possibly remain too short, picoammeter cannot sample fast enough, etc.), hot plate growth and an alternative picoammeter circuit will continue to be researched in parallel. 4. Top Level Description The goal of this project is to develop a testbed for piezoelectric nanowires. Fig. 9 shows a very high level block diagram which will be explained deeper in Section 4.1. The important thing to notice is that only one input, power to the system, is planned for. From there, the goal of the project is to get reasonable data of a welldesigned evaluation platform. Fig. 9: Top Level Block Diagram Page 25 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 4.1 Top Level Block Diagram Fig. 10: Top Level Block Diagram Page 26 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 4.1.1 Top Level Interface Definition Signals Kevlar Seed layer adhesion Chemicals Description Core of fibers TEOS used to strengthen bond between Kevlar and seed-layer Used in DI Water solution to form ZnO nanowires Temperature Necessary temperature for growth Growth Time Amount of time to form correctly dimensioned nanowires, varies depending on method Seed layer is applied to Kevlar to promote self-assembly of nanowires ZnO nanowires with desired dimensions for piezoelectric energy harvesting Used to form a Schottky junction with the uncoated wires Cleans fibers after hydrothermal growth Kevlar w/ seed layer Nanowires Gold Evaporation Sonication Functionalized Kevlar strands Strands to be used for actuation to measure possible output current Current Output from the nanowires Voltage Unamplified voltage from the functionalized Kevlar strand .csv file used for programming position of actuator Computer communication bus Mechanically applied using voice coil Code Data Actuation Position Vbb Vcc Vdd Power Used in actuation length settings Power for computer processing block Power for controller block Power for picoammeter block Power for actuator from controller block Feedback Control signal for microprocessor Command Correction instruction from feedback signal RS-232 Probes Interface for controller Low noise probes used to connect picoammeter circuit to the system Measure Amplified current output from functionalized Kevlar strands converted into a voltage Details High tensile and shearstrength Tetraethyl orthosilicate Attributes Flexible Zinc nitrate Zn(NO3)2 Hexamethylene tetramine (HMTA) Polyethylene imine Room temp. (Stage1) (80-95)˚C (Stage2) 150˚C (Stage3) 10 to 12 hours for hotplate 3 to 15 minutes for microwave Kevlar thoroughly cleaned Surface coating of TEOS Length of at least 1 μm Aspect ratio of at least 10:1 ~300nm thick gold layer on the nanowires Ultrasonic frequencies (20 kHz – 40 kHz sweep) Duration of sonication can be altered Uniform wire density on surface One strand coated with ZnO nanowires and evenly distributed Au layer One strand only covered with ZnO nanowires Expected values in picoampere range (> 50pA) Frequency control algorithms Between PC and I/O Variable force and distance Variable frequency (1 – 20 Hz) Set with software 120 V AC rms 15 A ± 12 – 35 V DC ± 6V DC ±12 – 24V AC Voltage varies depending on frequency and length 15 A peak current 2.86 A max current 12 A peak current 16 – bit signal (0 – 5V DC) Varies depending on load Control signal for the motor power supply (changes actuator position) (0 – 5V DC) Varies depending on load 9 pin, serial, 5V DC BNC Connectors 0 – 50µA current Current depends on voltage which varies with load 0 – 50µA current Current depends on voltage which varies with load Less than 20 pF capacitance Page 27 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5. Block Descriptions 5.1. Seed Layer Coating Diagram Fig. 11: Seed Layer Coating Diagram 5.1.1 Seed Layer Coating Interface Definition Signals Kevlar Seed Layer Adhesion Input/Output Input Intermediate Surface Texture similar to plastic Kevlar coated with TEOS Kevlar with Seed Layer Output from Seed Layer Creating Mechanism Plastic is now covered with more growth favoring ZnO seed layer Diameter 14 µm 14 µm Thin layer of TEOS 14 µm from Kevlar (20 nm thick seed layer) Conductivity None None Semiconducting seed layer 5.1.2 Seed Layer Coating Operation A seed layer is needed to begin the process of growth utilizing self-assembly principles. The seed layer will create an energetically favorable growth environment for the ZnO nanowires. Possible output currents from the piezoelectric nanowires will use the seed layer for conduction. This seed layer needs to be firmly attached to the seed layer, and TEOS will be used to ensure a strong bond between the Kevlar and seed layer. 5.1.2A TEOS Tetraethyl orthosilicate (TEOS) is a chemical that is used to create a surface more favorable for growth of the zinc oxide seed layer. To make a comparison, when depositing films on silicon wafers, the wafer will already have a natural oxide (silicon dioxide) which will make the surface more favorable for growth because of free hydroxyl groups to bond to. Since Kevlar is a plastic-like material, using TEOS will create this oxide layer and promote growth of zinc oxide. 5.1.2B Sputtering Deposition using sputtering is facilitated by heating a target and bombarding it with a non-reactive material (usually argon plasma). Because this takes place in high vacuum, particles freed from the target can deposit directly onto the desired substrate surface. This is a line-of-sight deposition, so to coat a strand of Kevlar it would need to be mounted in such a way to rotate evenly. For zinc oxide deposition, a zinc target is used and a small amount of oxygen flows over the substrate. Page 28 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5.1.2C ALD Atomic Layer Deposition is used for deposition of thinner films. Multiple precursors are introduced to the chamber individually. Although ALD is similar to more traditional Chemical Vapor Deposition (CVD), the chemical reactions are split into half-reactions by separating the administration of each precursor. By keeping these precursors separate, thinner films can be achieved. Additionally, each reaction is self-limiting which means that thickness can be controlled down to a single layer of atoms. Unlike sputtering, this has the added advantage of coating the entire substrate surface without rotation. 5.1.2D Sol-Gel A chemical solution method can be used to create materials as well. Usually used for metal oxides, a gel is formed and then deposited onto the substrate by either dip-coating or spin-coating. This is a low-cost and low-temperature method, and doping or adding extra components is simple. The chemical slurry that is formed allows for uniform coverage and dispersion over smoothly polished substrates. For a non-traditional substrate such as Kevlar, Sol-Gel deposition methods are limited by the cylindrical shape. To illustrate, when spin-coating, the gel would only be able to cover a certain amount of the substrate. In the case of dip-coating, a thickness gradient would occur in the seed layer from pulling the substrate out of the solution. Although pulling at a slow and steady rate would allow for a uniform film, Atomic Layer Deposition still produces a more conformal seed layer. 5.2 Hydrothermal Nanowire Growth Diagram Fig. 12: Hydrothermal Nanowire Growth Diagram 5.2.1 Hydrothermal Nanowire Growth Interface Definition Signals Kevlar with Seed Layer Input/Output Input Materials Plastic covered ZnO seed layer Process Details N/A Conductivity Semiconducting seed layer Chemicals Input N/A N/A Temperature Input Hexamethylene tetramine Polyethylene imine Zinc Nitrate Hydrate DI Water N/A Range of 80 – 90 C N/A Growth Time Input N/A N/A Nanowires Output Zinc Oxide Varies with Hydrothermal method choice N/A To be determined Page 29 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5.2.2 Hydrothermal Nanowire Growth Operation Two options for hydrothermal growths exist. Attributes of each method are discussed in the following sections. Both of these methods utilize a mixture of hexamethylene tetramine, zinc nitrate hydrate, polyethylene imine and DI water. The heating mechanisms of each method lead to variances in nanowire properties. Currently, the two most significant variables are growth time and aspect ratio. When studying material properties later in the project, one method may yield nanowires with better electrical conductivity. 5.2.2A Microwave Kevlar breaks down at approximately 400 °C, limiting growth methods to hydrothermal options because of the higher processing temperatures (~ 900 °C) required for other methods. Hydrothermal growth utilizing a microwave would be preferable because growth times are on the order of 5 – 10 minutes. An additional advantage from shorter growth time is that any crystals that happen to form in solution do not have enough time to grow to sufficient sizes and deposit on the Kevlar surface. If crystals are still present, their smaller size would make sonication faster. One issue that has been noticed with this method is the length limitation. Nanowire lengths currently attained from this method are on the order of 300 nm rather than the desired lengths of ~ 3um. 5.2.2B Hot Plate Average growth times for this method are about 10 – 12 hours. The longer growth times are undesirable. Average lengths for the hot plate hydrothermal method up to this point are approximately 1 µm, which is a three-fold increase over the microwave method. 5.3 Wound Kevlar Diagram Fig. 13: Wound Kevlar Diagram 5.3.1 Wound Kevlar Interface Definition Signals Nanowires Input/Output Input Purpose Piezoelectric energy harvesting Material Zinc Oxide Sonication Input Used to remove large crystal growths (dendrites) Acetone or Isopropyl alcohol Gold Evaporation Input Gold Current Output Gold will be evaporated onto ZnO coated Kevlar strand Main output under study Functionalized Kevlar Strands Output Complete electrical circuit generated by bending of nanowires Kevlar coated with Zinc Oxide nanowires, one strand with Au coating, one without N/A Desired Features Aspect ratio of 10:1 Length of ~3 µm Variable frequency and variable duration Uniform coverage of nanowires Study possible output to beyond a reasonable doubt Consistent winding between samples Page 30 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5.3.2 Wound Kevlar Operation The expected output current will come from the interaction of the two functionalized strands of Kevlar. The relative motion between the two strands will bend the ZnO nanowires while the Au coated nanowire will act as a negative electrode. 5.3.2A Au Coated Kevlar Strand One of the Kevlar strands with zinc oxide nanowires will be coated with gold. Gold is used because of a large work function at 5.1 eV when compared to the bandgap of ZnO at 3.3 eV [42]. Two strands are wound together to form a Schottky barrier, forcing current to flow through a loop from the bent zinc oxide wires to the Au coated wires. The flow of the current is shown in Fig. 14. Fig. 14: Nanowire Current Generation Circuit 5.3.2B Kevlar Strand This Kevlar strand is only coated with zinc oxide wires. In order to complete the circuit described above, both are necessary to wind around the other. This ensures that nanowires strain other nanowires, taking advantage of their piezoelectric properties. Consistent winding techniques need to be developed to reduce major sources of human error. 5.4 Picoammeter Diagram Fig. 15: Picoammeter Block Diagram Page 31 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Fig. 16: Amplifier and Power Diagram 5.4.1 Picoammeter Interface Definition Signals Vdd Input/Output Input Description Common Supply Voltage Picoammeter Equipment Voltage: 120 VAC Current: 10 A Max Current Input Output from the nanowires Voltage: Not yet determined (Depends on magnitude of nanowire strain) Current: 0-100 pA Type: Analog Voltage Intermediate Voltage to be amplified Measure Output Amplified signal used for measurement Voltage: Attenuated from input current due to probe length Current: 0-100 pA Type: Analog Voltage: 0 – 5V Current: 50 µA Type: Digital Picoammeter Circuit Voltage: ±6 V from batteries Current: 2.86 A Max Voltage: Not yet determined (Depends on magnitude of nanowire strain) Current: 0-100 pA Type: Analog Voltage: Attenuated from input current due to probe length Current: 0-100 pA Type: Analog Voltage: -1.5 – 1.5V Current: 15 µA Type: Digital 5.4.2 Picoammeter Operation The picoammeter is essential for actually measuring data. Due to the amounts of current expected (around 50 pA), this circuit has the tightest design constraints compared to every other block. This picoammeter functions around the CA3420 opamp from Intersil. It has low-noise and high gain properties that make it work well for this application, although high gain also limits its unity-gain bandwidth to 500 kHz. By having a high input impedance of the circuit, combined with a low bias current of the opamp, very little of the current from the nanowires is wasted and a voltage associated with this current will appear across the inputs of the amplifier. This is amplified 100,000x so the current can be more readily measured. The selected circuit also has a potentiometer to compensate for any voltage offset caused by process variations. This allows for the amplifier to be tuned so that 0 pA actually outputs 0 mV. There is also another variable resistor in the resistor network to compensate for any variations in the 1% tolerance resistors. 5.4.2A Probes When connecting probes to functionalized Kevlar, a method needs to be developed to minimize damage to the ZnO seed layer. Since the seed layer conducts the desired current, it is essential to have a good Ohmic contact with the probes. The actual probe model has yet to be determined. Probes will either be connected directly to the Kevlar or to clamps which will attach the Kevlar to the voice coil actuator. BNC connectors will be utilized because coaxial shielding in the wires will reduce noise. Also, available current sensing equipment utilizes the same connections. Probes for this application are typically around 20 pF, although it is possible to get active probes that reduce the capacitance further. Page 32 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Because of the low frequencies that are expected, this should not have a major influence and can most likely be ignored. 5.4.2B Amplifier Two amplifier options will be explored in parallel. This approach will help clarify if amplifier noise is responsible for previous results from Georgia Tech. The HP 4140B picoammeter is available in Owen Hall and can be used as a control for studying the picoammeter circuit. The HP 4140B will also be used for initial characterization of the ZnO nanowires until completion of the alternative circuit. The picoammeter circuit will utilize a low-noise opamp to provide amplification. The initial schematic is shown in Fig. 17. Alterations may be made to the schematic based upon SPICE results of the proposed design. The specified CA3420 opamp from Intersil will be modeled in SPICE based upon its datasheet and then the entire circuit will be simulated. Modifications will be made as necessary to ensure design specifications are met. Initial SPICE analysis was done by assuming the opamp is ideal with a single pole. The measured output is always at M, and the circuit is tunable by adjusting where the feedback of the opamp is connected in a resistor network. In Fig. 18, the output is graphed against a sweeping input current and the feedback is attached to the ±5 pA tap. Fig. 19 shows the same thing but attached to the ±50 pA tap. These simulations suggest good linearity between input current and output voltage. These output voltages will be read by an ADC and then sent to the computer. Alternatively, a digital oscilloscope could be used to log data and transfer it to PC with a USB thumb drive. This is attractive because it would eliminate any switching noise from the device as well as simplify the circuit. To power the measurement circuit, two 6V lantern batteries will be used when taking measurements. For testing purposes, the circuit can be connected directly to a benchtop power supply. The batteries are used because of both portability and isolation. Rectifying power from a wall outlet will always have some amount of ripple voltage that can skew results. A pair of low dropout (LDO) linear regulators will be used to power the +1.5V and -1.5V supply rails to the opamp. Ideally, these LDOs will be combined onto a single IC with a connection for ground as well. This would make sure that any ripples seen on the positive or negative voltage rails would be minimized. Fig. 17: Low Noise Opamp Circuit [27] Page 33 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Fig. 18: 5 pA Tap on Circuit Fig. 19: 50 pA Tap on Circuit Page 34 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5.5 Computer Processing Diagram Fig. 20: Computer Processing Block Diagram 5.5.1 Computer Processing Interface Definition Signals Vbb Input/Output Input Description Common Supply Voltage Interface Wall outlet Measure Output from picoammeter circuit Amplified signal used for measurement Display Output VGA Monitor Output Depends on picoammeter choice: Existing equipment uses RS-232 Picoammeter circuit interface still needs to be studied RGB or DVI output User Input Input Keyboard and Mouse USB peripherals Data Intermediate Data for processing and then output Internal system bus Signal Details Voltage: 120 VAC Current: 15 A Max Voltage: -1.5 – 1.5V Current: 15 µA Type: Digital Voltage: 0 – 5V Current: 50 µA Type: Digital Voltage: 0 – 5V Current: 50 µA Type: Digital Voltage: 0 – 5V Current: 50 µA Type: Digital 5.5.2 Computer Processing Operation Computer Processing is implemented with a standard PC running Windows XP. This allows for any computer equipped with a RS-232 serial port to interface with the rest of the system. The PC will handle programming of the voice coil controller’s microprocessor and collecting measurements from the picoammeter. The microprocessor will be controlled by outputting a .csv file containing positional data. The positional data is in the form of a sine wave, so the voice coil can be actuated as desired. The computer also handles the logging and analysis of experimental data. By characterizing noise, the average noise level should be able to be mathematically removed from actual measurements from actuated Kevlar. Each set of data taken can be used to find the most optimal conditions for piezoelectric generation. Page 35 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5.5.2.A I/O The I/O block handles any general inputs and outputs for the PC. This includes any logged data through the USB or RS-232 ports. It also includes VGA output to a monitor for displaying information. USB and RS-232 are standardized port configurations, so there is no chance of incompatibility between devices that use these. USB is used for user input devices such as the keyboard and mouse. It can also handle data transfer from a portable flash memory stick. The I/O block handles communicates with the picoammeter and controller blocks. The picoammeter collects data that is then transferred to the computer through this block. The controller interfaces with the computer processor via the RS-232. This allows a user to program the actuator block for any sort of positional input. 5.5.2.B PC PC processes all incoming and outgoing data. It also provides a platform for the user to interface with for calculations, analysis, and voice coil programming. The PC runs a Windows-based operating system of either XP or Vista. The main programs the user will use in this project are Excel and HyperTerminal. Excel allows for easy manipulation of data arrays. This is useful to easily make a positional waveform and save to a .csv file. It also is a useful tool for storing, calculating, and graphing data. HyperTerminal is used to communicate with the controller block for programming. 5.6 Actuator Diagram Fig. 21: Actuator Block Diagram 5.6.1 Actuator Interface Definition Signals Functionalized Kevlar Strands Input/Output Input Description Wound Kevlar strands (one covered with zinc oxide wires, one covered with zinc oxide wires coated with gold) Power Input Power supplied from voice coil motor controller Position Input/Output Position of voice coil will be read and programmed by the motor controller Accuracy: ±200nm Interface Need to determine final design Need to clamp or bond Kevlar to actuator while still allowing easy interchangeability High Density DB-15 style connection. High Density DB-15 style connection. Signal Details N/A Power range: ±12 – 24 V Current: 12A Type: AC Voltage: 0 – 5V Current: 50 µA Type: Analog Page 36 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5.6.2 Actuator Operation The voice coil acts as the actuation mechanism in the mechanical system. Power is an input which gives the inner coil enough energy to accelerate relative to the rest of the stage. The chosen voice coil has a built in position sensor which allows positional data to be read by another device (therefore the “Position” signal is an output of the Actuator block). Actuation acts an input and output to the voice coil. This is because the coil is fed frequency and magnitude actuation data to which it responds to. There is also a feedback loop on the actuator output intended for the actuation motion to self correct errors; in this way it is also an input. 5.6.2A Spring To return the actuated Kevlar back to its original position while retaining tension, a spring will be used. This spring will be attached to a static surface and the side of the Kevlar fiber, which is not being actuated. The actual spring to be utilized has not yet been determined. 5.6.2B Mounting Brackets Mounting brackets are required to attach the voice coil to a solid surface to prevent the entire device moving from applying stress on the fibers. The final design of these brackets, or some other mounting mechanism, is still to be determined. The critical design considerations are that the Kevlar samples need to be easy to exchange, the Kevlar needs to be firmly connected and the brackets cannot damage the strands. 5.6.2C Voice Coil The voice coil is a single piece of equipment that will be purchased from Equipsolutions. The Kevlar strands will be attached to the head of the voice coil, and the coil (while powered) will induce the mechanical stress on the fibers. The VCS-10H voice coil takes an input voltage of ±12V to ±24V. As the current used will go to the conduction coil, the actual power is a function of the current (which will be sinusoidal). The voice coil will be programmed so that the position of the head can be known at any point in its period to ±200nm of accuracy. 5.7 Controller Diagram Fig. 22: Controller Block Diagram Fig. 23: Microprocessor Sub-Block Diagram Page 37 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5.7.1 Controller Interface Definition Signals Vcc Input/Output Input Description Powers controller Interface Four circuit Mini-Fit Jr. RS-232 Input Communication from computer RS-232 Position Input/Output Motor controller will position voice coil Accuracy: High Density DB-15 style connection, pin 2. Power Output Powers voice coil High Density DB-15 style connection. Programming Intermediate Allows the processor to execute instructions specified by a user System bus ±200nm Signal Details Power range: ±12 – 35 V Peak Current: 15 A Type: DC Power range: ±5V Current: 50 µA Type: DC Power range: ±5V Current: 50 µA Type: DC Power range: ±12 – 24 V Peak Current: 12A Type: AC Power: 5V Current: 50μA Type: DC 5.7.2 Controller Operation A control system is required to operate and give parameters to the voice coil. Vcc ranges from ±12V to ±35V DC and powers the controller. RS-232, a standard serial connection, will be used in conjunction with a PC to program the controller. The outputs of this block are position and power. The power is used as the power input for the voice coil. The controller has an onboard current amplifier so the controller is capable of supplying the required current. The position output consists of programmed values on the controller. 5.7.2A Motor Power Supply The motor power supply is used to power the voice coil. The main component of this is a built-in current amplifier. This component is part of the controller and will supply an output voltage of ±12 – 24 V, and a maximum output current of 12A. 5.7.2B A to D Converter The function of this block is to transform analog positional information from the voice coil and convert it into a digital format for the microprocessor. This 16-bit analog to digital converter is built into the controller. This is ideal because it enables users to get a 200nm resolution. The voltage range of this feedback signal is 0-5V AC. 5.7.2C Microprocessor The microprocessor aids in the control of the voice coil during actuation by transforming userspecified positional data into a control signal. The voice coil’s current position is fed back to the processor through the A to D converter. With this information, the control signal to the power supply allows for output waveform modification. In Fig. 23, the microprocessor is broken down into two more sub-blocks. 5.7.2C.i RISC The RISC chip processes user-supplied code and positional data from the voice coil. From this information, it outputs data to the power supply. The power supply utilizes this data by altering its output as needed so that the voice coil moves to a new position. New positional data is read, further adjusting output so that the coil can quickly and accurately arrive at the correct position. Page 38 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5.7.2C.ii Code The user-supplied code is entered as a .csv file containing positional data. This will be in the form of a sine wave for voice coil actuation. Pseudo-code for these operations follows: Loop Goto position x = sin(f*t) //f is frequency Delay(0.001 seconds) // because of 1kHz bandwidth Until (0>1) //infinite loop until turned off 5.8 Mechanical Test Platform Diagram Fig. 24: Mechanical Test Platform Diagram Page 39 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5.8.1 Mechanical Test Platform Diagram Signals Vcc Input/Output Input Description Powers controller Interface Four circuit Mini-Fit Jr. Vdd Input Common Supply Voltage Power cord RS-232 Input Communication from computer RS-232 Position Intermediate Motor controller will position voice coil Accuracy: High Density DB-15 style connection, pin 2. Power Intermediate Powers voice coil High Density DB-15 style connection. Current Intermediate System bus Measure Intermediate Allows the processor to execute instructions specified by a user Amplified signal used for measurement Functionalized Kevlar Strands Intermediate N/A Nanowires Input Kevlar coated with Zinc Oxide nanowires, one strand with Au coating, one without Zinc oxide nanowires Signal Details Power range: ±12 – 35 V Peak Current: 15 A Type: DC Voltage: ±6 V from batteries Current: 2.86 A Max -ORVoltage: 120 VAC Current: 10 A Max Power range: ±5V Current: 50 µA Type: DC Power range: ±5V Current: 50 µA Type: DC Power range: ±12 – 24 V Peak Current: 12A Type: AC Power: 5V Current: 50μA Type: DC Voltage: -1.5 – 1.5V Current: 15 µA Type: Digital -ORVoltage: 0 – 5V Current: 50 µA Type: Digital N/A N/A N/A ±200nm RS-232 -ORUSB 5.8.2 Mechanical Test Platform Operation The mechanical test platform is the base for all of the measurement blocks to be placed on. This block symbolizes how individual blocks will come together once each functions properly. The four pieces that make up this block are the wound Kevlar, picoammeter, actuator and controller. Each block has been individually described in previous sections. Page 40 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 6. Testing 6.1 Minimum Requirements Testing Successful Nanowire Synthesis Well-defined method of nanowire production that repeatedly produces aligned ZnO nanowires. * 1. Prepare 5 samples from different growth batches using chosen growth parameters. 2. Properly mount samples for high quality SEM images. Previous mounting steps were as follows: i. Firmly attach copper grounding straps to SEM stage. ii. Apply carbon tape to stage on top of copper grounding straps. iii. Attach sample to carbon tape and press firmly on Kapton tape which is still connected to ends of samples. iv. Firmly attach additional copper grounding straps covering Kapton tape to keep samples from drifting during imaging. v. Coat entire stage with carbon to hopefully decrease charging of the sample. vi. Follow proper steps for traditional SEM equipment use and imaging. 3. Take images of samples. The images should not be corrupted due to charging effects, that comparisons will have to be performed at consistent magnification and that images must be representative of the sample. 4. Evaluate images. Pass: Research professor signs off below that there is sufficient evidence provided through SEM images that the chosen process parameters yield consistent samples. Fail: Not enough evidence is provided to convince the research professor that consistency between samples was achieved. Nanowire at least 1 µm in length and have an aspect ratio of at least 10:1 1. Prepare sample using chosen growth parameters. 2. Properly mount samples for high quality SEM images. Previous mounting steps were as follows: i. Firmly attach copper grounding straps to SEM stage. ii. Apply carbon tape to stage on top of copper grounding straps. iii. Attach sample to carbon tape and press firmly on Kapton tape which is still connected to ends of samples. iv. Firmly attach additional copper grounding straps covering Kapton tape to keep samples from drifting during imaging. v. Coat entire stage with carbon to hopefully decrease charging of the sample. vi. Follow proper steps for traditional SEM equipment use and imaging. 3. Take images of samples. The images should not be corrupted due to charging effects, that comparisons will have to be performed at consistent magnification and that images must be representative of the sample. 4. Study images. Use measurement tools to show length and widths of nanowires on SEM images. Pass: SEM images show that nanowires are longer than 1 µm AND that the aspect ratio is greater 10:1. than Fail: Nanowires are less than 1 µm long OR the aspect ratio is less than 10:1. Page 41 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Nanowire density must be low enough to allow movement in the wires but high enough to ensure enough output that it is detectable. (~10 – 50 µm-2) 1. Prepare sample using chosen growth parameters. 2. Properly mount samples for high quality SEM images. Previous mounting steps were as follows: i. Firmly attach copper grounding straps to SEM stage. ii. Apply carbon tape to stage on top of copper grounding straps. iii. Attach sample to carbon tape and press firmly on Kapton tape which is still connected to ends of samples. iv. Firmly attach additional copper grounding straps covering Kapton tape to keep samples from drifting during imaging. v. Coat entire stage with carbon to hopefully decrease charging of the sample. vi. Follow proper steps for traditional SEM equipment use and imaging. 3. Take five representative images of sample. The images should not be corrupted due to charging effects, that comparisons will have to be performed at consistent magnification and that images must be representative of the sample. 4. Study images. Use Paint to analyze the density of the nanowires over the surface of the samples: i. Use scale bar on image to determine the conversion factor between pixels and µm. ii. Draw a unit square (size will vary with image magnification) and count the number of nanowires within the square. iii. Average density values from the five images. Pass: SEM images and analysis show that average nanowire density is between 10 – 50 µm-2. Fail: SEM images and analysis are not conclusive OR average nanowire density is less than 10 µm-2 OR greater than 50 µm-2. Adhesion of seed layer to Kevlar can withstand actuation for 100 cycles without showing signs of separation. This ensures durability of the seed layer and uniform wire coverage on the Kevlar. * 1. Take images of seed layer of one Kevlar sample from growth batch. 2. Use another Kevlar strand to be actuated for 100 cycles. 3. Prepare actuated sample for SEM imaging. 4. Properly mount samples for high quality SEM images. Previous mounting steps were as follows: i. Firmly attach copper grounding straps to SEM stage. ii. Apply carbon tape to stage on top of copper grounding straps. iii. Attach sample to carbon tape and press firmly on Kapton tape which is still connected to ends of samples. iv. Firmly attach additional copper grounding straps covering Kapton tape to keep samples from drifting during imaging. v. Coat entire stage with carbon to hopefully decrease charging of the sample. vi. Follow proper steps for traditional SEM equipment use and imaging. 5. Take images of samples. The images should not be corrupted due to charging effects, that comparisons will have to be performed at consistent magnification and that images must be representative of the sample. 6. Study images. Seed layer should be firmly attached to Kevlar. Pass: SEM images and analysis show no damage to the seed layer (peeling, cracking, etc.) Fail: SEM images and analysis show damage to the seed layer (peeling, cracking, etc.) Page 42 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Accurate Electrical Measurements Picoammeter circuit must accurately be able to measure in 50 pA quantities to adequately test nanowires output. 1. Create current source circuit which can produce a reliable output. 2. Connect circuit to picoammeter in series. 3. Measure output. 4. Compare experimental results with expected output current from circuit and HP 4140B. Pass: The picoammeter can successfully measure currents in 50 pA quantities. Fail: The picoammeter cannot successfully measure currents in 50 pA quantities. Sample rate of electrical measurements must be a minimum of 1 kHz. This ensures sampling at a rate much greater than the input frequency from the actuator. 1. Connect measurement circuit to the current generator described in the previous test. 2. Take measurements for one minute.* 3. From waveform, count number of acquired data points and confirm that data was sampled at a rate of at least 1kHz. * Measurements will be tracked by using an oscilloscope. Pass: Sampling frequency is calculated to be at least 1 kHz. Fail: Sampling frequency is calculated to be less than 1 kHz. Robust Mechanical System Design Kevlar attachment to mechanical actuator must allow for replacement of different samples. 1. Detach electrical measurement probes from the testing apparatus.* 2. Unclamp the Kevlar sample and remove from testing apparatus. 3. Securely clamp new Kevlar fiber onto the actuation head. 4. Attach electrical measurement probes to the Kevlar samples.* * This will not be necessary if electrical measurement probes do not connect directly to Kevlar. Pass: Complete replacement of Kevlar in one hour or less. Fail: Fail to replace Kevlar sample in the one hour time frame. Mechanical actuator must have positional precision of at least 0.1 mm so as to make a repeatable set of input forces. Voice Coil: 1. Use software to program voice coil positions. 2. Analyze logged data and check bits to ensure 0.1mm or better accuracy. -OR- Page 43 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 General Positional Accuracy: 1. Set actuation device to predetermined position. 2. Set a block using calipers at 0.1mm greater than a position for the actuator to move to. 3. Move the actuator to the new position. 4. Use calipers to determine distance from the block. Pass: Actuator performs functions as programmed. Fail: Actuator does not perform a programmed function as expected. Mechanical system should not interfere with electrical measurements, ie. any noise from a motor should be filtered out. * 1. Prepare two Kevlar fiber samples with a zinc oxide seed layer, but without nanowire growth. 2. Clamp this pair of fibers to the actuation mechanism. 3. Attach electrical measurement probes to the Kevlar. 4. Program an actuation sequence. 5. Analyze any observed current waveform. 6. Characterize noise produced by zinc oxide coated sample using three test runs. 7. As a second test, prepare copper wire for actuation. 8. Repeat steps 2 through 6 for the copper wire. Pass: Research professor signs off that the observed waveform is negligible OR can be mathematically removed during analysis. Fail: Research professor does not sign off observed waveform is not negligible OR cannot be mathematically removed during analysis. Pull on Kevlar should be adjustable (from 0.1 to 5 mm if necessary) to find an optimal stroke that stresses system without permanently damaging the Kevlar and nanowires. * 1. Set a block using calipers a distance of 0.2 mm from the actuation head. 2. Move the actuation head to the 0.2 mm point. 3. Verify the actuator position using calipers. 4. Set a block using calipers a distance of 5 mm from the actuation head. 5. Move the actuation head to the 5 mm point. 6. Verify actuator position using calipers. 7. Properly mount samples for high quality SEM images. Previous mounting steps were as follows: i. Firmly attach copper grounding straps to SEM stage. ii. Apply carbon tape to stage on top of copper grounding straps. iii. Attach sample to carbon tape and press firmly on Kapton tape which is still connected to ends of samples. iv. Firmly attach additional copper grounding straps covering Kapton tape to keep samples from drifting during imaging. v. Coat entire stage with carbon to hopefully decrease charging of the sample. vi. Follow proper steps for traditional SEM equipment use and imaging. 8. Take images of samples. The images should not be corrupted due to charging effects, that comparisons will have to be performed at consistent magnification and that images must be representative of the sample. 9. Evaluate images. Page 44 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Pass: Actuation device is able to vary the pulling distance from 0.2 mm to 5 mm. The Kevlar and zinc oxide seed layer are not damaged at optimized stroke. Fail: Actuation device is unable to vary the pulling distance of 0.2mm to 5 mm OR an optimal stroke cannot be found. Mechanical actuation system must have a variable frequency of 1 – 20 Hz. 1. Design a sensor circuit which will measure each wave cycle of an actuation sequence. 2. Build the fore mentioned circuit. 3. Orient the sensor so as to detect the actuation waveform. 4. Program the actuator for frequencies of 1 and 20 Hz. 5. Activate the actuation device and run for 1 minute at each frequency. 6. Analyze the output waveforms from the sensor circuit. Pass: Mechanical actuation system is able to perform actuation at frequencies of 1and 20 Hz. Fail: Mechanical actuation system does not have a variable frequency OR is unable to actuate with frequencies of 1and 20 Hz. Adequate Analysis of Results Analysis and theory of results. * 1. If a current output is measured, provide a convincing argument that this current is coming from the wires. 2. If there is no output current measured, explain why this is occurring. 3. Data should be sufficient enough to back-up theory and analysis. Pass: Research professor finds analysis of results accurate and adequate. Fail: Research professor does not find analysis complete or satisfactory. * Certain requirements cannot be firmly quantified. Whether these requirements have been met will be evaluated by the research professor. 6.2 Desired Requirements Testing Examine possible alternative materials such as polyethylene fibers instead of Kevlar, other piezo materials rather than ZnO, aluminum rather than gold for a Schottky barrier, etc. * 1. Growth methods for different substrate or nanowires materials are detailed. 2. Test results exist for any additional materials that were explored. 3. Comparisons have been made between ZnO Kevlar with Au Schottky and the alternative. Pass: Alternative materials have been explored and tested to the satisfaction of research professor. Fail: No alternatives were explored OR they were not explored sufficiently and to the satisfaction of research professor. Compare results from piezoelectric and non-piezoelectric growth materials. * 1. Non-piezoelectric material chosen with a known method of nanowires growth compatible with Kevlar substrate. 2. Growth method characterized, samples from method are made. 3. Test using identical procedures that were developed for ZnO-coated Kevlar. 4. Analysis has been completed with identical figures of merit to ZnO-coated Kevlar. Page 45 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 5. Conclusions from analysis can be used to either support or disprove ZnO nanowires can generate energy from piezoelectric strain. Pass: Non-piezoelectric material was tested. Research professor believes results are conclusive. Fail: No tests on non-piezoeletric material performed OR results inconclusive to research professor. Nanowires should be 3µm long with an aspect ratio over 100:1. These would most likely improved results. 1. Prepare sample using chosen growth parameters. 2. Properly mount samples for high quality SEM images. Previous mounting steps were as follows: i. Firmly attach copper grounding straps to SEM stage. ii. Apply carbon tape to stage on top of copper grounding straps. iii. Attach sample to carbon tape and press firmly on Kapton tape which is still connected to ends of samples. iv. Firmly attach additional copper grounding straps covering Kapton tape to keep samples from drifting during imaging. v. Coat entire stage with carbon to hopefully decrease charging of the sample. vi. Follow proper steps for traditional SEM equipment use and imaging. 3. Take images of samples. The images should not be corrupted due to charging effects, that comparisons will have to be performed at consistent magnification and that images must be representative of the sample. 4. Study images. Use measurement tools to show length and widths of nanowires on SEM images. Pass: SEM images show that nanowires are longer than 1 µm AND that the aspect ratio is greater 100:1. than Fail: Nanowires are less than 3 µm long OR the aspect ratio is less than 100:1. Electrical measurements sampled at 0.5 MHz or higher. This will better show any spikes in current as the system tries to reach equilibrium. 1. Connect measurement circuit to the current generator described in the previous test. 2. Take measurements for one minute.* 3. From waveform, count number of acquired data points and confirm that data was sampled at a rate of at least 1kHz. * Measurements will be tracked by using an oscilloscope. Pass: Sampling frequency is calculated to be at least 0.5 MHz. Fail: Sampling frequency is calculated to be less than 0.5 MHz. Change mechanical actuation frequency to 100 – 200 Hz and determine the effects of higher frequencies on material breakdown. 1. Orient the sensor from minimum requirements so as to detect the actuation waveform. 2. Program the actuator for frequencies 100 and 200 Hz. 3. Activate the actuation device and run for 1 minute at each frequency. 4. Analyze the output waveforms from the sensor circuit. Page 46 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Pass: Mechanical actuation system is able to perform actuation at frequencies of 100 and 200 Hz. Fail: Mechanical actuation system does not have a variable frequency OR is unable to actuate with frequencies of 100 and 200 Hz. Entire system portable and stable enough to exhibit a working test procedure at Engineering Expo. 1. Each system component shall weigh no more than 35 lbs. 2. Perform standard test procedure in any room specified by course instructor. Pass: System components weight less than 35 lbs. AND test results do not disagree with previous results in controlled environment. Fail: One or more system components weigh 35 lbs. OR test results disagree with previous results. * Certain requirements cannot be firmly quantified. Whether these requirements have been met will be evaluated by the research professor. Page 47 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 7. Bill of Materials Block Description Manufacturer Voice Coil Actuation mechanism Control of voice coil Linear Power Supply TEOS Equipment Solutions Equipment Solutions Equipment Solutions Alfa Aesar Hydrothermal Nanowire Growth Hydrothermal Nanowire Growth Hydrothermal Nanowire Growth Hydrothermal Nanowire Growth Hydrothermal Nanowire Growth Seed Layer Coating Picoammeter Hexamethylene tetramine Picoammeter Manufacturer Part # VCS-10H Supplier Supplier Part # VCS10H SCA814 Availability Quantity Available Unit Cost $1,500 1 Total Cost $1,500 Available $950 1 $950 LPS24 Available $275 1 $275 40251 Available 500g $43.50 1kg $22.60 100g $62.40 500g $33.40 1 $468.53 40251 Equipment Solutions Equipment Solutions Equipment Solutions Alfa Aesar Alfa Aesar A17213 Alfa Aesar A17213 Available Polyethylene imine Alfa Aesar 40527 Alfa Aesar 40527 Available Zinc Nitrate Hydrate Alfa Aesar 12313 Alfa Aesar 12313 Available Hot Plate VWR 12365-480 VWR 12365480 Available $43.50 for 500g $22.60 for 1kg $62.40 for 100g $33.40 for 500g $468.53 Low Static Kapton Tape 3M 5419 GOLD 1/2IN X 36YD Digi-Key 3M5919 12-ND Available $29.35 1 $29.35 Kevlar DuPont ----- Available ----- 1.5kΩ ± 1% Resistor Vishay/Dale CMF551K500 0FHEB Digi-Key Available 5 $0 Sample $0.85 430Ω ± 1% Resistor 150Ω ± 1% Resistor Vishay/BC Components Vishay/Dale SFR250000430 0FR500 CMF55150R00 FHEB Digi-Key Available $0.19 5 $0.95 Available $0.17 5 $0.85 Picoammeter 11kΩ ± 1% Resistor Vishay/Dale CMF5511K00 0FHEB Digi-Key Available $0.17 5 $0.85 Picoammeter 68Ω ± 1% Resistor 1kΩ potentiometer Panasonic ECG CTS Corporation Electro components CTS Corporation Electro components EPCOS Inc EROS2PHF68R0 296UD102B1 N Digi-Key CMF1.5 0KHFCT -ND PPC430 YCT-ND CMF150 HFCTND CMF11. 0KHFCT -ND P68.0CA CT-ND CT2262ND $0 Sample $0.17 Available $0.171 10 $1.71 2,738 Available $1.51 2 $3.02 296UD103B1 N Digi-Key CT2265ND 5,112 Available $1.51 2 $3.02 B37979N1100J 000 CMF551M000 0FHEB Digi-Key P4837ND CMF1.0 0MHFC T-ND PPCHF1 0MCTND 588HVF120 6T1008J E 27,150 Available Available $0.23 2 $0.46 $0.17 5 $0.85 Available $0.798 5 $3.99 Available $3.95 2 $7.90 Controller Controller Seed Layer Coating Picoammeter Picoammeter SCA814 LPS24 ----- DuPont Digi-Key Digi-Key Picoammeter 10kΩ potentiometer Picoammeter 10 pF capacitor Picoammeter 1MΩ Resistor Vishay/Dale Picoammeter 10MΩ Resistor Vishay/BC Components HVR37000010 05FR500 Digi-Key Picoammeter 10 GΩ Resistor Ohmite HVF1206T100 8JE Mouser Digi-Key Page 48 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Picoammeter AA Batteries Panasonic-BSG LR-6PA/2SB Digi-Key Picoammeter CA3420 Intersil CA3420EZ Intersil Picoammeter 1.5V fixed regulator Rohm BA15BC0T Digi-Key P107ND CA3420 EZ BA15BC 0T-ND In Stock $0.54 4 $2.16 In Stock $0 Sample $1.02 2 $0 Sample $2.04 In Stock 2 Page 49 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 8. Development Plan The next few paragraphs describe the timeline of this project and the associated tasks as well as their dependency on one another. Although set-backs cannot always be planned for, a better understanding of how the tasks are related to one another can help ease the stress of the critical path. Over the break each team member will be taking days off, but the goal is to still keep making progress on the project. For example, parts can be ordered so that the lead times associated with each piece will not be an issue Winter term. Different parts of the project each have associated goals and deadlines so the plans for each piece are described in sections below, with a final project plan as a summary. 8.1 Materials Although the functionalized Kevlar strands are needed for the project, improvements of growth consistency and experiments around altering growth parameters will not disrupt the development of the other sub-blocks. The main issue for the materials part of the project is getting proper access to a high quality scanning electron microscope and reserving sufficient tool time. Hewlett-Packard Corvallis has generously donated visitor access to their Analytical and Development Labs and the time of an experienced technician. After working through the logistics between the legal departments of OSU and HP, the paperwork has been signed and site visits will begin after January 1, 2009. There are two different growth mechanisms that can be used; each method needs to be studied in parallel. The hot plate method produces longer wires, but growth times are significantly longer. On the contrary, the microwave method has the benefit of a significantly shorter growth time but the wires are much shorter. The microwave method is the more favorable method because of the shorter growth time, but both methods need to be improved so that required nanowire dimensions can be achieved. 8.2 Electrical Measurements There are two options for taking electrical measurements. The HP 4140B is available for use in Owen, but one of the desired requirements is to have a working display at the expo. The equipment in Owen is for use in Owen and is not located in a low-noise area. One of the very large issues with the electrical measurements is noise. Not only is a very low-noise environment needed, but the noise that is present has to be well characterized so that it can be subtracted from the performed measurements. One of the more challenging pieces of this part of the project is the design of the picoammeter. There are different options which need to be considered and the members of this team do not have the required specialty in circuit design. For this piece of the project, parts should be ordered over break. There have been some problems with the progress of the actual design so the schedule is already getting tighter. 8.3 Mechanical Actuator The current plan for the mechanical actuator is using a voice coil. The idea behind this is that not only is the voice coil bi-directional but there is also a controller which can be used to track the position of the actuator to an accuracy of 200nm. Since this research project is in the center of a large controversy using the most accurate equipment as possible is vital. Over break, ways that the Kevlar should attach to the voice coil need to be examined. Another good time investment would be ordering the voice coil and controller. Time off of school should be utilized to get more familiar with the voice coil software. 8.4 Project Approach Summary The general approach to this project is to develop each of the subsystems individually. After each piece is completed and verified the project as a whole can be further developed. The design of each system will be performed in accordance with the overall project objectives. Testing is broken up by the subsystem so that if a particular block is not functioning properly, the rest of the project will not be categorized as nonfunctioning. A pass condition exists for each subsystem and failure of one test will not create a domino effect. If proper design considerations are taken, only a few weeks will be needed for complete system integration. Page 50 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Appendix A. Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 References [1] Y. Qin, X. Wang, and Z. L. Wang, “Microfibre–nanowire Hybrid Structure for Energy Scavenging”, Nature, vol. 451, pp. 809 – 814, February 2008. [2] Interuniversity Microelectronics Centre, "Thermopiles in Headband Power Wireless EEG Sensor and 2.4 GHz Transmitter," Wearable Smart Sensors, October 2007. [Online]. Available: http://www.wearablesmartsensors.com/energy_sources.html. [Accessed: November 2, 2008]. [3] Z. Wang, V. Leonov, P. Fiorini, and C. Van Hoof IMEC vzw, Kapeldreef 75, B-3001, Leuven, Belgium, “Micromachined Polycrystalline SiGe-Based Thermopiles for Micropower Generation on Human Body,” Symposium on Design, Test, Integration and Packaging of MEMS/MOEMS, DTIP 2007, Stresa, lago Maggiore, Italy, 284-289. [4] A. Powell, "Nanowire Generates Its Own Electricity," ScienceDaily, October 2007. [Online]. Available: http://www.sciencedaily.com/releases/2007/10/071022161425.htm. [Accessed: November 2, 2008]. [5] Z. Wang, “Voltage Generation from Individual BaTiO3 Nanowires under Periodic Tensile Mechanical Load,” Nano Letters, vol. 7, pp. 2966 – 2969, October 2007. [6] E. Yeatman, P. Mitcheson, A. Holmes, “Micro-Engineered Devices for Energy Harvesting,” IEEE Explore, 2008. [Online]. Available: http://ieeexplore.ieee.org/stamp/stamp.jsp?arnumber=04418950. [Accessed: October 20, 2008] [7] Z. L. Wang and J. Song, “Piezoelectric Nanogenerators Based on Zinc Oxide Nanowire Arrays,” Science, vol 312, pp. 242 – 246, April 2006. [8] Y, Qin, X. Wang, Z.L. Wang, "Microfibre-Nanowire Hybrid Structure For Energy Scavenging," Nature, Vol 451, pp. 809-813, February 2008. [9] M. Sáez, “Energy Harvesting From Passive Human Power,” High Performance Integrated Circuits and Systems Design Group, January 2004. [Online]. Available: http://pmos.upc.es/blues/projects/thesis_project_mateu.pdf. [Accessed: October 20, 2008] [10] L. Greene, B. Yuhas, M. Law, D. Zitoun, and P. Yang, “Solution-Grown Zinc Oxide Nanowires,” Inorganic Chemistry, vol. 45, pp. 7535 – 7543, September 2006. [11] K. S. Shankar and A.K. Raychaudhuri, “Fabrication of Nanowires of Multicomponent Oxides: Review of Recent Advances,” Materials Science and Engineering, vol 25, pp. 738-751, December 2005. [12] Z. R. Tian, J.A. Voigt, J. Liu, B. McKenzie, M. J. McDermott, M. A. Rodriguez, H. Konishi, and H. Xu, “Complex and Oriented ZnO Nanostructures”, Nature, vol 2, pp 821 – 826, November 2003. [13] Z. L. Wang and J. Song, “Piezoelectric Nanogenerators Based on Zinc Oxide Nanowire Arrays,” Science, vol 312, pp. 242 – 246, April 2006. [14] C.K. Tan, G.K.L. Goh, and G.K. Lau, "Growth and Dielectric Properties of BaTiO3 Thin Films Prepared by the Microwave-Hydrothermal Method," Thin Solid Films, vol. 516, pp. 5545-5550, June 2008. [15] Electronics Lab, “Picoammeter Circuit With 4 Ranges – CA3420,” Electronics Lab, 2002-2008. [Online]. Available: http://www.electronics-lab.com/projects/test/011/ [Accessed: October 20, 2008]. Page 51 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 [16] Wikipedia, “Zinc Oxide,” Wikipedia.org, Oct. 18, 2008. [Online]. Available: http://en.wikipedia.org/wiki/Zinc_oxide [Accessed: Oct. 20, 2008]. [17] Azo Materials, “Barium Titanate ( BaTiO3 ) – Properties and Applications,” AzoM.com [Online]. Available: http://www.azom.com/details.asp?ArticleID=2280 [Accessed: Oct. 20, 2008]. [18] Wikipedia, “Barium Titanate,” Wikipedia.org, Aug. 17, 2008. [Online]. Available: http://en.wikipedia.org/wiki/Barium_titanate [Accessed: Oct. 20, 2008]. [19] Wikipedia, “Lead zirconate titanate,” Wikipedia.org, Sep. 1, 2008. [Online]. Available: http://en.wikipedia.org/wiki/Lead_zirconate_titanate [Accessed: Oct. 20, 2008]. [20] Wikipedia, “Gallium(III) Nitride,” Wikipedia.org, Oct. 13, 2008. [Online]. Available: http://en.wikipedia.org/wiki/Gallium_nitride [Accessed: Oct. 20, 2008]. [21] Silicon Far East “Crystal Structures and Lattice Constants,” Siliconfareast.com, 2004. [Online]. Available: http://www.siliconfareast.com/lattice_constants.htm [Accessed: Oct. 20, 2008]. [22] Wikipedia, “Cadmium Sulfide,” Wikipedia.org, Aug. 20, 2008. [Online]. Available: http://en.wikipedia.org/wiki/Cadmium_sulfide [Accessed: Oct. 20, 2008]. [23] ScienceLab.com, “Cadmium Sulfide MSDS,” ScienceLab.com, Oct. 9, 2005. [Online]. Available: http://www.sciencelab.com/msds.php?msdsId=9923232 [Accessed: Oct. 20, 2008]. [24] H. J. Fan, A. S. Barnard, and M. Zacharias, “ZnO Nanowires and Nanobelts: Shape Selection and Thermodynamic Modeling,” Applied Physics Letters, vol. 90, pp. 143116-1 – 143116-3, April 2007. [25] W. Q. Yang, L. Dai, L. P. You, B. R. Zhang, B. Shen, and G. G. Qin, “Catalyst-Free Synthesis of Well-Aligned ZnO Nanowires on In0.2Ga0.8N, GaN, and Al0.25Ga0.75N substrates” Journal of Nanoscience and Nanotechnology, vol. 6, pp. 3780 – 3783, June 2006. [26] H. E. Unalan, P. Hiralal, N. Rupesinghe, S. Dalal, W. I. Milne, and G. A. J. Amaratunga, "Rapid Synthesis of Aligned Zinc Oxide Nanowires," Nanotechnology, vol. 19, pp. 55608-55612, June 2008. [27] Intersil, “CA3420 Data Sheet,” Intersil.com, October 4, 2005. [Online]. Available: http://www.intersil.com/data/fn/fn1320.pdf [Accessed: October 20, 2008]. [28] Agilent Technologies, “4140B pA Meter/DC Voltage Source,” Agilent.com, 1980. [Online]. Available: http://www.home.agilent.com/upload/cmc_upload/All/40B90021.pdf [Accessed: October 20, 2008]. [29] Agilent Technologies, “HP 4145 B Semiconductor Parameter Analyzer,” Agilent.com, February 1986. [Online]. http://www.home.agilent.com/upload/cmc_upload/All/59527838.pdf [Accessed: October 20, 2008]. [30] Agilent Technologies, “Agilent 4156C Precision Semiconductor Parameter Analyzer,” Agilent.com, October 14, 2008. [Online]. Available: http://cp.literature.agilent.com/litweb/pdf/5988-9238EN.pdf [Accessed: October 20, 2008]. [31] Keithley Instruments Inc., “6485 Picoammeter Data Sheet,” Keithley.com, 2008. [Online]. Available: http://www.keithley.com/data?asset=6199 [Accessed: October 20, 2008]. [32] Keithley Instruments Inc., “6485 Picoammeter Data Sheet,” Keithley.com, 2008. [Online]. Available: http://www.keithley.com/data?asset=10756 [Accessed: October 20, 2008]. Page 52 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 [33] Metric Test, “Keithley 6487 Picoammeter/Voltage Source Used Electronic Test Equipment,” Keithley.com, 2008. [Online]. Available: http://www.metrictest.com/product_info.jsp?mfgmdl=KEI%206487&utm_source=google&utm_medium=ppc&ut m_term=keithley%206487&utm_campaign=MetricTest%20USA&gclid=CJyRmZ2FtpYCFRg6awodPllMLA [Accessed: October 20, 2008]. [34] R. Whitehouse, “Fast-Settling Circuit Handles Wide Voltage Range,” EDN.com, September 2008. [Online]. Available: http://www.edn.com/contents/images/6368443.pdf [Accessed: October 20, 2008]. [35] Analog Devices, Inc., “AD795 Data Sheet,” Analog.com, October 2002. [Online]. Available: http://www.analog.com/static/imported-files/data_sheets/AD795.pdf [Accessed: October 20, 2008]. [36] 3B Scientific, “Pico Ammeter Amplifier,” American 3B Scientific, 2008. [Online]. Available: http://www.a3bs.com/shop/u.s.a./teltrontrade/pico-ammeter-amplifier-u18630,p_83_675_0_0_1325.html [Accessed: October 20, 2008]. [37] C.B. Grantham, “Integrator Forms Picoammeter,” EDN.com, July 1997. [Online]. Available: http://www.edn.com/archives/1997/071797/15di_04.htm#Figure%201 [Accessed: October 20, 2008]. [38] Equipment Solutions, "VCS10 Voice Coil Stage," Equipsolutions.com, 2007. [Online]. Available: http://www.equipsolutions.com/vcs10.htm. [Accessed: Nov. 2, 2008.] [39] Equipment Solutions, "SCA814," Equipsolutions.com, 2007. [Online]. Available: http://www.equipsolutions.com/sca814.htm. [Accessed: Nov. 2, 2008]. [40] Futaba, “Futuba S148 Servo Standard Precision,” Futaba, 2007. [Online]. Available: http://www.gpdealera.com/cgi-bin/wgainf100p.pgm?I=FUTM0710 [Accessed: Nov. 2 2008] [41] E-Clec-Tech, “Servos: Linear Servo Conversion Kit,” Electronic Eclectic Technology, 2008. [Online]. Available: http://www.e-clec-tech.com/lisekits.html. [Accessed: Nov. 2, 2008] [42] HyperPhysics, “Work Functions for Photoelectric Effect,” HyperPhysics Quantum Physics. [Online]. Available: http://hyperphysics.phy-astr.gsu.edu/hbase/tables/photoelec.html. [Accessed: Dec. 5, 2008] [43] Zaber, “Miniature Linear Actuators,” zaber.com, 2008. [Online]. Available: http://www.zaber.com/products/product_group.php?group=T-LA&name=Miniature_Linear_Actuator. [Accessed: December 5, 2008] [44] Firgelli Automation, “Mini Style 4” Stroke 8lbs Force Linear Actuator,” firgelliauto.com, 2008. [Online]. Available: http://www.firgelliauto.com/product_info.php?cPath=69&products_id=131 [Accessed: December 5, 2008] [45] Concise Motion, “Miniline O Linear Actuator,” concisemotion.com, 2008. [Online]. Available: http://www.concisemotion.com/Miniline/Mini0.htm [Accessed: December 5, 2008] [46] Aerotech, “PRO165 Linear Stage,” aerotech.com, 2008. [Online]. Available: http://www.aerotech.com/products/stages/pro165.html [Accessed: December 5, 2008] Page 53 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Appendix B. Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Naming Conventions and Glossary Analog Digital Converter (ADC) A device used to convert an analog signal to digital bit values. This allows an arbitrary signal to be read by a computer or microprocessor for processing. Aspect ratio Term used to define nanowire dimensions. Formally defined as length over width. Atomic Layer Deposition (ALD) A method of depositing thin films one monolayer of atoms at a time. This is done in an inert gas environment where one material is introduced to the substrate, purged, and then followed by a second. By repeating this process multiple times, a thin film is grown. AttoSI prefix meaning 1*10-18 Au Gold (periodic table abbreviation) Autoclave Closes heating system to contain water so that solution can be heated above boiling point. Block A block is the basic element of a system. It is a standalone object that performs some function in the system. A block should be ‘small’ enough that everything contained inside of it can be fully understood as a whole, or the contents can be purchased as a whole. Customer Requirement A requirement that may or may not be able to be tested as is. A requirement supplied by the customer, sponsor, or mentor. CVD Chemical Vapor Deposition DI water Deionized water is purified water that has had its mineral cations (eg. sodium, calcium, iron or copper) and anions (eg. chloride or bromide) removed. Dip-coating The substrate is submerged in the coating solution and is slowly pulled out of the solution allowing the solution to cover the substrate. The substrate is then dried to finish creating the thin-film. Discipline Decomposition The process of dividing a system into blocks based on the primary knowledge used in defining each block. (e.g. computer science, electrical, mechanical) Engineering Requirements A requirement that can be tested and evaluated through a step by step process. Usually a numerical specification is included. Page 54 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Environment The set of influences that the system will be operating within. These could include temperature, humidity, immersion, vacuum, etc… EPROM Erasable Programmable Read-Only Memory. A non-volatile memory that will store data even without being powered. Functional Decomposition The process of dividing a system into blocks that represent the required functions. See discipline decomposition, locality decomposition Half-reaction Can be either the oxidation or reduction reaction component of a redox reaction. In order to obtain a half reaction the change in oxidation state of the individual substances is considered. Hydroxyl Group A grouping of chemicals describing molecules which consist of an oxygen atom and a hydrogen atom connected by a covalent bond. Integrated Circuit (IC) A silicon chip encased in a hard plastic with a various number of input and output pins to make connections. The silicon has a circuit made on it with numerous transistors and other components, made together to perform some function. Interface Characteristics Every connection between blocks is defined by a unique name and a list of interface characteristics. These characteristics define an interface to the degree that a block can be built without knowledge of other blocks in the system Photosensitive Nanowires Nanowires acting as antennae that can absorb wavelengths of visible light. Photovoltaic A material characteristic that causes a voltage potential to be produced when light is shown onto the material’s surface. Piezoelectricity A material property where a voltage potential is created from mechanical stress. Platform Used to describe the project as a whole, in its physical aspects and the necessary application functions. Locality Decomposition The process of dividing a system into blocks based on the similarity (locality) of blocks. (e.g. all inputs together, all outputs together) Low Dropout Regulator Linear DC voltage regulator used to create a different input voltage than what is provided by a power supply or batteries. Page 55 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Molecular Beam Epitaxy (MBE) Slow deposition method which allows crystals to grow epitaxially in a vaccuum MOCVD Metal Organic Chemical Vapor Deposition Ohmic Contact A near-ideal metal-semiconductor interface that allows electrons to flow between the two materials with no voltage drop. RISC Reduced Instruction Set Computing. Simpler instructions are used to increase the speed of specified actions. Scanning Electron Microscope (SEM) A type of electron microscope used to image samples by accelerating electrons toward the sample. Because electrons have a much smaller wavelength than visible light, much smaller features can be seen on the sample. Schottky Junction A Schottky Junction uses a metal-semiconductor interface instead of semiconductor-semiconductor interfaces seen in p-n junctions. Due to a difference between the metal’s work function and the semiconductor’s band gap, a diode is formed that only allows current to flow in a single direction. Spin-coating Used to apply uniform thin films to flat substrates. First, an excess amount of a solution is placed on the substrate. The substrate is then rotated at high speed in order to spread the fluid by centrifugal force. Strain Magnitude of deformation in a material under stress. Sub-System This is a grouping of one or more blocks that function together to perform some task. (e.g. a motor and a motor controller perform the task of motion.) System The complete system being designed to study and test piezoelectric nanowires. This includes all blocks in your design. Test bench This phrase is used to describe the combination of the mechanical actuator and electrical measurement systems. Thermopile A stack of alternating types of metal wires. A voltage difference is produced across the wires when heat is applied. By stacking them in series, a higher potential can be produced to power a device. Thomson Effect Describes the heating or cooling of a current-carrying conductor with a temperature gradient. Page 56 of 57 Project Specification – Piezoelectric Nanowires Adapted from ECE 322 Project Spec Ashley Mason, Adam Stone, Todd Waggoner – Group 11 Copyright 2008 – Oregon State University December 7, 2008 Top-Level This refers to the system block diagram containing all blocks in the system. VLS Vapor Liquid Solid growth mechanism Young's Modulus The measure of the stiffness of an isotropic elastic material. Defined as uniaxial stress over uniaxial strain. Page 57 of 57