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Dept. of Materials Science & Engineering , National Taiwan University Chapter 3 Furnaces Lecturer: Professor Wei (韋文誠教授) 3/5/2013 助教: 許哲誠 –舊物二號館220室 0971 097 628, [email protected] Dept. of Materials Science & Engineering , National Taiwan University High temperature Processes of Ceramics 1. Expensive step; 2. Necessary for ceramics: sintering, reactions, phase transformation, glass melting, crystal growth; 3. Tend to get desirable properties; 4. Contamination 5. Safety Types of Furnaces • Based on the heat source: (1) Combustion (燃燒式) (2) Electrically Resistive (電阻式) (3) Focused Infrared (紅外線)或 visible light (可見光) (4) Direct heating, microwave (微波) or radiofrequency (RF) Type of furnace (1) periodic or batch type (批次式) (2) continuous (連續式 ) Terminology • Furnace vs. kiln (interchangeable) Furnace vs. ovens (for drying) * Combustion (oxidative process) vs. burning Combustion Furnaces Combustion Heat Generation • Need to know the heat capacity of each species • Cp is the molar heat capacity • Diabatic flame temperature Electrically Heated Furnaces Powder from electricity P=VI=I2R so, heat Q =RI2t (Joule or kWh) • Several advantages (1) easy to measure power input (2) easy to control heating rate and temperature (3) the furnace can be operated in an atmosphere independent of the heating source Batch (or Continuous) Operation Continuous Operation •Tube burner •Thermal shock •Design time-temperature profile Indirect Heating: 1. Induction • Induction furnace -external Cu coil -applied power + impedance of materials -good susceptor: graphite -60-1000 Hz -up to 3000oC -up to kA • Microwave heating • Arc-image furnaces Indirect Heating: comparison • Induction furnace: good in clean, fast, process reproducible, be automated, local heating is possible • Microwave heating: high frequency 0.915 or 2.45 GHz home: 700-1200 W, industry: up to 5 kW • Arc-image furnaces clean, fast and used for crystal growth. • Laser or electron beam heating temperature control is poor Heating Elements • Cost and lift time are also the concern of using the elements SiC Heating Elements • Most widely used non-oxide • < 1500oC • >1500oC oxidation is apparent Manufacturing of SiC (1) In-situ reaction (or called carbon-reduction) method mixture of SiO2 + C is heated to 1900oC (2) Reaction bonding method green (SiC+C powder) bars is immersed in melted Si. (3) Sintering SiC powder with sintering aids (for instance, B+C powder, Al2O3+Y2O3 sintered up to 2300oC. MoSi2 Heating Elements • • • • Brittle Up to 1800oC short period Normal <1700oC Room temperature resistivity is 2.5x10-7ohm-m, but increases to 4x10-6 ohm-m. • Manufacturer: Kanthal Super, made the element in composite with Al-Silicate glass (20 vol%) ZrO2 and SnO2 Heating Elements • Cubic zirconia (c-ZrO2) ex. Ca or Mg doped • For >2000oC heating; • In air or oxidation cond. • Need preheating to 1000oC, then becomes conductive. • SnO2 as electrode in glass melting furnace; • E-conductivity is high at glass melting temp.; • Resist to corrosion • Not discolor the glass. • 60 cm long 15 cm dia., 1400oC sintered electrode; • Free surface of glass batch is low prevent evaporation of low melted species, ex Pb, B. Graphite, Mo and W Heating Element • Graphite is good conductor and less vapor in reducing atmosphere upto 3000oC; • Reactive with oxide ceramics; • Susceptive to oxidation; • All metal oxides are eventually reduced if contacted with graphite. • Mo oxidizes to MoO3 >700oC; • Mo is good conductor and less vapor up to 1500oC; • W is good in inert atmosph. Up to 3000oC; • Susceptive to oxidation; Contamination by W Heating Element a-SiC sample sintered in W-furnace for 12 hr at 1300oC. • Fine W particles are coming from the evaporation of W-element during the heat treatment. Refractory in an Industrial Glass Melting Furnaces • 70% are preformed bricks (定型磚) • Hearth (爐床) Refractory (耐火材) • Iron and steel making • Cu & Al melting • Cement & ore processing • Petro-industry Dolomite 白雲石 Zircon 鋯英石 ZrSiO4 Refractory for Blast Furnace • Slag: protective layer on melted iron, consisted of limestone, SiO2 (from ore), ash and various oxides; Thermal Conductivity of Porous Insulators • Or a simple form, when kc > kp Furniture, Tubes and Crucibles • Important crucible materials; • Boat (船型坩堝) setter plate (棚板) Furniture on Push Car Firing Process (Schedule) • Heat-up stage, soaking stage, and cooling stage • Quartz transformation a to b at 537oC induce …. • Soaking period (持溫時間) Heat Transfer in Furnace • By Conduction/convection/radiation • Conduction: from heating element to air and • hot air to ceramics • Convection: hot air flowing in furnace; is important at lower temperature; • Radiation: hot wall or furniture to others by visible light, and is the most important at high temperature Temperature measurement by Thermo-couple • What do the alloys mean? Constantan, chromel, alumel? Pyrometers (光譜測溫儀) • Radiation effect of object; • Disappearing filament optical pyrometers compare with standard incandescent source! • Advantages Dis-advantages Temperature measurement: Pyrometric Cones • Sensitive to time and temperature • Useful for ceramic sintering Safety • High temperature hazards protective goggle, gloves, hood, and safety glass • Electric hazards >100 mA is lethal, Good insulation from high voltage, power • Chemical hazards in reducing cond. 1. the formation of CO 2. The formation of CN and HCN, Conclusions • Very important tools; • Safety issues; • A tour to lab. 參考資料 Chapter 7 in Ceramic Materials, Science and Engineering, Springer, 2007