microwave assisted technologies for ceramics and chemical ... assisted technologi… · microwave...
TRANSCRIPT
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Microwave Assisted Technologies for Ceramics and Chemical Processing
Shawn M. Allan*Morgana Fall, Inessa Baranova, Dr. Holly Shulman
Ceralink Inc.October 8, 2008, 2:00 PM
Environmentally Benign Processing II
Pittsburgh, Pennsylvania
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Outline
� Background
� Focus on energy efficient manufacturing
� Technical difficulties
� Engineered solutions
� Case Studies
1. Microwave Assist Technology for Nano-BaTiO3 powder synthesis
2. MAT kiln scale-up for carbon foam & ceramics
3. Microwave Autoclave scale-up for Pt recycling from PEM fuel cells
� Summary
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Materials & Energy
� Heat is ubiquitous to materials processing
� Heating processes are often bottlenecks
� Energy consumption costs, especially for ceramics, is enormous
� Energy is strategic, economic, and environmental issue
� Efficiency is critical to sustainability
� Energy consumption is directly related to pollution
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Microwave Advantages
� Heat materials directly
� Energy applied in volume of product� Yields significant energy savings - 50% or greater
� Less dependence on thermal conductivity
� Leads to fast heating, short cycle time� Fine powders and grain structures
� Fewer pollutants released from clays (e.g., HF)
� Heating can be uniform (e.g. sintering, binder burnout)or non-uniform (e.g. self limiting reaction, joining, LTCC)
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Microwaves - Dielectric Heating
Transparent to microwavesTan δ < 0.01
Reflects microwavesTan δ > 10
Absorb microwave (heats)Tan δ ~ 0.01 - 2
Conductivity increasing* ����
0.0000010.004 - 0.051.012.8Penetration Depth (m)
∞∞∞∞0.08-1.050.0150.0010Tan δδδδ
Aluminum
(bulk**)
Silicon CarbideZirconiaAlumina20°C
2.45 GHz
* Magnetic field may also induce currents leading to heating** Powder metals have measureable dielectric properties
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Dielectric Property Testing
Zirconia and Alumina Insulation
Measured at 2.45 GHz
� Relates to conductivity changes
� Predicts microwave heating behavior
� Higher Tan δ � Better absorption
� Want product to preferentially absorb
� Need radiant heat at low temp
� Avoid thermal runaway at high temp
M ���� TLoss of adsorbedwater
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Technical Difficulties
� Material doesn’t suscept at any temperature
� Material suscepts through part of heat cycle
� Can use susceptors for radiant heat
� Can use MAT (microwaves + electric or gas radiant heat)
� Thermal runaway, non-uniform heating
� Control microwave power input
� Controlled by susceptors and/or MAT for some materials
� Equipment design, availability, and cost
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Engineered Solutions
� Focus on product� Demonstrate feasibility� Scale-up plan, system mock up� Cost benefit / manufacturability analysis� Need for Teams
� Product manufacturer� Equipment companies (e.g. microwaves, kiln builders)� Expertise in microwave + materials interactions
� Find Government support� Strategic products� Dual use equipment� State and Federal energy initiatives
� DoE, NYSERDA, PEDA
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1. MAT Calcination:Self Limiting Synthesis
of Nano-BaTiO3
Dr. Holly S. ShulmanMorgana Fall, Shawn Allan
Ceralink Inc.
Dr. Matt Creedon
Ferro Corp.
NYSERDA
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Calcination and theMixed Oxide Method
� Perovskites: dielectrics, ferroelectrics, piezoelectrics, sensors, transducers, capacitors, data storage elements barium titanate, strontium titanate, PZT
� Relaxors: Niobates
� Phosphors: MgWO4, SrAl2O4
� Superconductors: YBCO
� Conducting ceramics: ITO
� Varistors: ZnO
� Catalysts
� Spinels, ferrites, garnets
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Nanograin Ceramic PowdersDemand for smaller electronic components
���� need for powders with smaller grain size
Chemical Processing� Build up from atomic scale� High purity� Expensive
Mixed Oxide Calcination� Grain growth and hard agglomerates� Addition of Impurities (due to grinding/milling)� Energy intensive
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Mixed Oxide Processfor Perovskites
BaTiO3 Layer
TiO2
particle
BaCO3
particles
Heat
BaCO3 + TiO2 ���� BaTiO3 + CO2
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Dielectric PropertiesTan Delta
1
2
Tmm 1,,,,
Tmm 2,,,,
,,,,
0 200 400 600 800 1000 1200
1 103
0.01
0.1
1
BaTiO3 - Product
Tmm 1,,,,
Tmm 2,,,,
,,,,
0 200 400 600 800 1000 1200
1 104
1 103
0.01
0.1
1
TiO2 - Reactant
1
2
Tmm 1,,,,
Tmm 2,,,,
,,,,
0 200 400 600 800 1000 1200
1 103
0.01
0.1
1
BaCO3 - Reactant
Tan δ δ δ δ of TiO2
higher than BaTiO3 from 700–1100 °C
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Microwave HeatingMicrowave makes it possible to fabricate nano-barium titanate from mixed oxide calcination method
� Selective heating - heat reactants, not final product� Fast Heating - less time for grain growth� Lower process temperature - lower kinetics for grain growth� Enhanced reactions - More complete reactions in less time
Dielectric Properties show pre-cursor powders heat better compared to final product � self limiting reaction
BaTiO3
Layer
TiO2
particle
BaCO3
particles
Microwave energy
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Microwave Assist TechnologySolution: Use Microwave Assist Technology (MAT) to improve traditional calcination method
� Combination of radiant heat (gas or electric) with microwave energy� Balance microwave heat with radiant heat� Patented Technology� Simultaneously apply both microwave and radiant
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MAT ResultsMicrowave Drives Reaction Faster 850 °C Calcining Temperature
BaTiO3
BaCO3
BaCO3Microwave power off
23 35 45 60
Dwell Time
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MAT ResultsMicrowave Drives Reaction Faster 850 °C Calcining Temperature
Microwave power on
BaTiO3
BaCO3
60
Dwell Time
4535
23
BaTiO3
BaCO3
BaCO3Microwave power off
23 35 45 60
Dwell Time
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MAT Results
MAT calcining
850 °C, 35 min dwell
Fully reacted BaTiO3
SSA = 5.85 m2/g
Ds = 170 nm
Conventional calcining
850 °C, 35 min dwell
Incomplete calcine12% BaCO3 present
SSA = 7.44 m2/g
Ds = 134 nm
Conventional calcining
1000 °C, 3 hour dwell
Fully reacted BaTiO3
SSA = 2.30 m2/g
Ds = 550 nm
500 nm 500 nm500 nm
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MAT ResultsEnergy Consumption
0
5
10
15
20
25
30
35
1 2
Energy consumption (kWhrs)
MicrowaveEnergy
ConventionalEnergy
MAT Conventional
0
200
400
600
800
1000
1200
0 1 2 3 4 5
Time (hrs)
Temperature (C)
MAT
Conventional
Parameters
MAT: 850 °C, 35 minute dwell
Conventional: 1000 °C, 3 hr dwell
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MAT ResultsReproducibility 19 runs, 800 °C, 60 min dwellAvg. surface area = 7.6 m2/g ���� particle size 130 nm
range ±25 nm
� Cp = 1.33
� Want Cp to be 1.33 or higher
� Cpk = 1.23
� A process with Cpk over 1 is a capable process.
� The closer Cpk is to Cp, the better
6.0
6.5
7.0
7.5
8.0
8.5
9.0
0 5 10 15 20
Run No.
BaTiO
3 Surface Area (m2/g)
UCL
X
LCL
LSL
USL
5
6
7
8
9
10
120 130 140 150
Ave Particle size (nm)
Suface area (m2/g)
• Specification 170 nm• MLCC thickness 1.0 micron
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SummaryMicrowave Assist TechnologyMicrowave Assist Technology provides:
� Rapid calcining
� Energy savings
� Lower kiln temperature
� Enhanced reactions
� Selective and self limiting heating
� Finer grains
� Applicability to wide range of materials
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2. MAT Firing:Carbon Foam & Bulk Ceramics
Dr. Holly S. ShulmanMorgana Fall, Shawn Allan
Ceralink Inc.
Dr. Drew Spradling
Touchstone Research Laboratory
United States Department of Defense
NYSERDA
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Carbon Foam Firing Challenges� Strategic Material
� Mold for C-C composites� Lightning Protection
� Problem� Large cross-sections� Highly insulating, unusual expansion properties� Inert atmosphere� Maximum process temperature of 1050 °C
Slow, Energy Intensive Firing Cycles ���� 7 days!!
� Solution� Carbon is effective susceptor in microwave field� Increase heating uniformity � faster heating� Use MAT (microwave + electric kiln design)
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Proof of Concept
� Carbon self heats in microwave� Problem � inverse temp profile with pure microwave
� Carbolite burnout furnace
� Modified by Ceralink to accept microwaves
� Allowed firing in 1/10 time
Gas inlet
Microwaveinlet
Carbon MaterialElectric heating elements
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Scale-up Predictions
� MAT 1/10th of firing time for small brick� Anticipate a small sample contribution to fast firing� Predict large scale time/energy reduction of 50%
0
200
400
600
800
1000
0 50 100 150Time (hrs)
Temperature C
Conventional (lg brick)
MAT extrapolation (lg brick)
MAT (sm brick)
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MAT Pilot Scale-up
TEAM Approach� C-FOAM Manufacturer – Touchstone Research Laboratory
� Kiln construction – Harrop Industries
� Microwave equipment supplier – Thermex Thermatron
� MAT design, systems integration, license – Ceralink Inc.
� Support – United States Department of Defense
Specifications:� Elevator Design
� 3ft x 3ft x 3ft workspace
� Inert atmosphere
� 1620 °C Capability
� 915 MHz, Two port
Commissioned: November 2007
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Bulk Ceramic FiringAlumina/SiC Composites
Ceralink has exclusive license in North America to use and sublicense MAT
Material suscepts well
Achieved higher density
Improved product uniformity overConventional and MAT lab kiln
80% process time reduction
Blasch Precision CeramicsAlbany, New York
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Cycle Time and Energy SavingsAlumina/SiC
• 80% energy savings• Similar or better properties• Faster turn-around time• Less product in process
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Porcelain InsulatorsAlumina Replaced Porcelain
� Feasibility testing showed:
� Time and energy savings
� 45 hrs conventional firing � 10 hrs MAT firing
� Full size insulator � 10” core, 72” tall
� Used dielectrics & porcelain science to work out MAT process
MAT kiln
CerMAT- 1700
12 kg, 10” x 12”
Feasibility
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3. Microwave Autoclave for Polymer Fuel Cell
Reclamation
Shawn Allan, Morgana Fall, Dr. Holly S. Shulman
Ceralink Inc.
Dr. Lawrence Shore
BASF Catalysts LLC
United States Department of Energy
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Polymer Fuel Cells
Gas Diffusion Layer
Gas Diffusion Layer
Anode Catalyst Layer
Nafion® Membrane
Cathode Catalyst Layer
5 layer Membrane Electrode Assembly
Recycling Project Goals:
� Digest platinum catalyst into solution
� Avoid burning Nafion membrane
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Precious Metal RecoveryMicrowave Digestion
� Ceralink assisted BASF � $5 mil from DOE to develop a method for precious metal recovery from used fuel cell membranes.
� Current method is ashing: � Fluoropolymer + flame � HF� costly environmental problem
� And…
� Microwave digestion � up to 99% Pt recovery� Improved yield
� Avoid HF generation
� Easier to manage by-products
� Simultaneous recovery of metal and polymer
� Uses for recycled Nafion®
Platinum ���� $511 /m2
Nafion®���� $2,400 /m2
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Microwave Autoclaves
� Short cycle times � Quick process development
� Accelerated reactions (microwave superheating)
� Safety: no physical contact with heat source
� Allows high T-P research without exhaustive materials search
� Significantly lower cost vs. specialty alloy autoclaves
� Cold walls – less system corrosion
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Lab Scale Research� Highly corrosive reagents
� Concentrated HCl, Cl2, Aqua Regia� Easier to neutralize waste acids & emissions� Lab scale containment – PTFE vessels
� Adjust reagent combinations for desired effects� Digest platinum and carbon (1)� Only digest platinum (2)
� 100-200 °C, 10-50 atm, 10-30 minutes
� Versus bench top 70 °C stir plate reaction � Improved yield (up to 50%)� Up to 99% Pt recovery in Microwave Vessels
Treated Nafion membrane Carbon on the Nafionmembrane
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Microwave vs. Benchtop
Stir plate ~70 °C1 atmstirred
Microwave ~200 °C20-40 atm30 minute soakno agitation
Effects �Temperature,Pressure,Stirring,Containment
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Scale-up Challenges
� Identifying critical process component� Microwave, Stirring, Containment, or … ?
� Materials selection for larger vessels� up to 600L
� Reactor design for special environment
� Microwave integration
� Volumetric scaling of high pressure process
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Microwave Autoclave Prototype Team
� Autoclave Engineers is a division of Snap-Tite Corp
� specializes in ASTM standard high pressure vessels
� Microwave Materials Technology (MMT)
� microwave equipment expert
� Ceralink
� design, team coordination, testing
� BASF (Engelhard)
� end user
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Prototype Microwave Autoclave
� 1 kW, 2.45 GHz microwave power
� 200 ºC at 50 atm
� Working volume of 2-5 L
� Integrated computer control
� PTFE inner vessel, 316 SS outer vessel
� Titanium plumbing
� Two reagent metering ports
� Temperature and pressure monitoring
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Ongoing OutcomesBASF Microwave Autoclave
� Successful lab demonstration of platinum and Nafion® recovery
� A patent applied for PEM recovery process
� New microwave autoclave designed and built for process scale up
� Titanium autoclave built to study high P-T without microwave� Aqua regia and wet Cl2 resistant without use of Teflon liner
� Microwave autoclave used for extensive corrosion testing
� BASF designing pilot plant facility
� HF emissions from PEM fuel cell recycling will be avoided
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CommercializationMicrowave Heating Technology
Microwave Assist ShuttleC-Tech UK
Barriers
• Need for demonstration
• Need for specific commercial design
• Need for manufacturability and cost benefit analyses
• Need for funding, government & industry support
Atmosphere MAT Lab KilnCeralink USA
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Summary
� Microwave heating comprises highly efficient process technologies
� Feasibility, cost benefit, and environmental analyses are essential
� Broad feasibility has been demonstrated
� Landscape changing as energy costs rise, need for solutions
� Multidisciplinary teams are needed to bridge the gap for the commercialization of new microwave processes
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Acknowledgments
New York State Energy Research and Development Authority
United States Department of Defense - Dr. Doug Deason at SMDC under a Phase II & Phase III SBIR contract
United States Department of Energy
Come learn more about Ceralink andEnergy Efficient Microwave Heating Technologies
from our partners at the Expo:
Thermex Thermatron Harrop Industries
Carbolite