Dec 15, 2018 - ze ss te ch nik. Recycling. Heating Zone. Ultrasonic spray pyrolysis (USP) - theory. Gas. Heating ... Dimensioned: 4,7* 9,5* 5,4 m. ⢠5 Aerosol ...
AMPT 2015, Dec 15th, Madrid
Upscaling of Ultrasonic Spray Pyrolysis for Nano-sized Particle Synthesis G. Alkan, J. Bogovic, S. Stopic, B. Friedrich
IME Process Metallurgy and Metal Recycling, RWTH Aachen University Prof. Dr.-Ing. Dr. h.c. Bernd Friedrich
Increasing demand for nanomaterials
Cosmetics
Textile
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Metallurgie
Medicine
Recycling
Global market for nanoparticles
Electronics
optimistic conservative
5 mton
2 mton
[Nanomaterials future markets, March 2015]
Ultrasonic spray pyrolysis (USP) - theory Heating Zone Evaporation Liquid droplet
Precipitation Thermal Decomposition Solid Particle Formation
Droplet
solvent vapour
Temperature
Shrinkage
Precipitate
Heating Zone Each droplet undergoes same process steps One particle produced per droplet
Gas Flow Rate
Gas Aerosol
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Metallurgie
Ultrasound frequency
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Properties of precursor
USP process is relatively inexpensive, continuous and flexible technique Synthesis of fine metallic, oxide, composite nanoparticles; controlled morphology and defined chemical compositions
Motivation & Objective Problem: Increasing demand; restricted production rates Solution: Upscaling to provide larger amounts of powder for potential users 10 years experience in USP for the synthesis of different products with well controlled properties Cu
Ag&TiO2
Fe-Ni [Stopic et al., 2006]
[Stopic et al., 2005]
[Stopic et al.,2010]
[Bogovic et al.,2014]
[Gürmen et al., 2009]
Ag
RuO2 &TiO2
Objective
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Metallurgie
Assessment of a well-controlled and reproducible demo USP plant for fine metal, oxide, composite nanoparticles mass production in defined chemical compositions, morphology and size that yield in industrialization Recycling
Nano equipments at IME
Horizontal USP equipment Small production rate, 15-125 mg/h Good for determination of process parameters for synthesis of new materials
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Metallurgie
Technical scale USP equipment Relatively increased production, 125-375 mg/h Assesment of vertical system efficiency and process parameters
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Upscaling of USP process
IME Process Knowledge
Application NanoAg Elino Construction
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Metallurgie
IOB Modelling and Optimizing
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Criteria for upscaling Scale-up
Higher Aerosol Throughput
Particle Size, Morphology
Higher Gas Flow Rate
Temp. Profile
Precursor
US Generator Geometry
Droplet size
Flow rate
Productivity
Quality
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Metallurgie
• Residence time f (volume of reactor, gas flow, temperature profile) • Geometry of the reactor
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Demo scale USP equipment
Dimensioned: 4,7* 9,5* 5,4 m • 5 Aerosol generators (Prizma) • 5 Reactors, ø: 60 mm, L: 3600 mm • Resistance-heated Furnace (Elino) • 2 Electrostatic Filters • Vacuum System
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Metallurgie
DFG Deutsche Forschungsgemeinschaft and Land NRW , program “Forschungsgeräte” (INST 222/874-1 FUGG)
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Set-up 1: Aerosol generator and gas system Gas lines
Ultrasonic Aerosol Generator
Gas outlet
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Metallurgie
Prizma USP Generetors • 5*3 Transducer • Automatic Level Control • Continuous work • Prototyp (Prizma-Serbia) • Aerosol output: 6-8 l/h Recycling
Gas inlet
Set-up 2: furnace and reactors
Resistant-heated Furnace • 4 Heating zones • Temperature max. 1000°C • Power: 80kW
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Metallurgie
• 5 Hot wall reactors, ø: 60 mm, L: 3600 mm • Possibility for on-line sampling from each heating zone
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Set up 3: electrofilter (powder collection system)
• • •
Collection of nanoparticle in dry form in electrical field Flexible working conditions: 15-120kV, 0,1-1mA, 130-250°C Redundant circuit for continuous operation
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Metallurgie
• Each filter: 12 collecting electrodes and a hammer system for cleaning • Produced powder is collected in mobile and tight vessel at the bottom of the filter Recycling
First experimental results Precursor: AgNO3 (aq) Temperature: 500/1000/1000/1000°C Carrier Gas: Air Thermal decomposition: AgNO3 → Ag + NO2 + 1/2 O2
Ag
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Metallurgie
• Ideally spherical silver particles • Particle size in the range of 100 nm up to submicron (starting concentration of silver nitrate solution was high) • EDS Analysis confirmed that produced particles were pure Ag Recycling
Summary Conclusion:
• Efficiency of design was assessed • Good control of significant process parameters e.g:: temperature profile, aerosol generation, pressure control, gas flow. • Successful principal transfer from lab scale equipment to this large scale equipment (5m x 12m x 6m). Future Prospective • Further optimization of the process is going to be done in order to obtain better control of nano-product characteristics and increase production rate. • The collecting and handling of the generated powder material must be optimized in order to fulfill pre-industrial standards • Synthesis of new nanomaterials
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• Open for partners from the industry for new applications and projects Recycling
Thanks for your attention!
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Metallurgie
Q&A Recycling