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VTT Powder Piloting Service: Facilities

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For more information please visit our website: www.vtt.fi/powder. We are material experts specialized on powder based materials. With Powder Piloting Service we can boost up your development needs and adoption of resource efficient manufacturing and alternative materials for substitution.

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VTT Powder Piloting Service: Facilities

  1. 1. Powder Piloting Service Material solutions, from powder to product. VTT Technical Research Centre of Finland Ltd Facilities www.vtt.fi/powder
  2. 2. Post treatments & characterization Powder Consolidation www.vtt.fi/powder  Gas Atomisation  Spray drying  Plasma spheroidization  Mechanical Alloying & Mixing  Powder Classification  Additive Manufacturing (AM)  Hot Isostatic Pressing (HIP)  Powder Injection Molding (PIM)  Self-Propagating High Temperature Synthesis (SHS)  Thermal Spraying  Laser Cladding  Heat treatments  Surface Treatments  Performance Testing & Validation  Powder Characterization Powder manufacturing
  3. 3. Phenomena and affecting parameters  Multiscale material modelling ProperTuneTM  Materials  Processes  Characterisation  Performance Powder development and production  Metals, ceramics polymers and composites  Milling systems  Gas atomisation  Plasma spheroidization  Spray drying  Post treatments Consolidation  Thermal spraying (TS)  Hot Isostatic Pressing (HIP)  Powder Injection Molding (PIM)  Reactive synthesis  Additive manufacturing Performance  Materials in service environments  Degradation mechanisms  Lifetime evaluation Core competences in powder technology in VTT Material efficiency via tailored material and production routes www.vtt.fi/powder
  4. 4. POST TREATMENTS - THERMAL - CHEMICAL - CLASSIFICATION CERAMIC - COMPOSITE - INTERMETALLIC - AMORPHOUS - METAL ALLOYS CATALYST - THERMAL SPRAY - CLADDINGS - MIM - HIP - LASER SINTERING - CASTINGS - POLYMER COMPOSITES WET & DRY MILLINGSPRAY DRYING FLUIDIZED BED MIXING CHEMICAL SYNTHESIS MECHANO-CHEMICAL SYNTHESIS GAS ATOMIZATION Pilot scale routes for powder processing www.vtt.fi/powder
  5. 5. Powder manufacturing www.vtt.fi/powder
  6. 6.  Gas atomization  Metal powders  Spray drying  Ceramic and composite powders  Optimization of slurry properties  Homogeneous dispersions  Induction plasma reactor  Spheroidization  Synthesis  Purification  Different milling systems:  Mechanical alloying  Raw material modification e.g. grinding fuse and crush powders  SHS-combustion  Composites, intermetallics  Chemical synthesisDifferent milling systems:  Mechanical alloying  Raw material mod. e.g. grinding  Granulation and coating of powders www.vtt.fi/powder Powder processing equipment
  7. 7.  5 kg steel (2 kg Al)  Max. temperature 1750°C  Inert gas atomisation vacuumed/over pressure  Particle median size 10-100 µm adjustable: atomisation pressure, metal throughput rate, viscosity, surface energy  Cyclone separates fines 85 % 1 µm  Cooling rate max. 105-106 Ks -1 Atomisation equipment www.vtt.fi/powder
  8. 8. Atomisation  Gas atomised powders  Both powder metallurgical and thermal spraying  HIP, SPS, Laser, Conventional sintering, Microwave  HVOF, Plasma  Tailored material compositions  Gas atomised powders are spherical  Inert gas atomisation, Ar or N2  High purity  Particle size 2-100 µm  Fines can be removed by air classification, coarse by sieving  Flowability and filling characteristics are good www.vtt.fi/powder
  9. 9. 922/12/2017  TEKSPHERO-15  15 kW induction plasma system for powder spheroidization and purification  Semi continuous approx. 5 liters batch size www.vtt.fi/powder  Improved powder flowing properties  Spheroidized particles provide a more homogeneous and stable flow while feeding.  Decreased powder porosity  Porosity is removed when the material is melted.  The tap density of the powder is increased  Decreased powder friability  The treatment removes internal fractures or weak internal bonds and its end effect is a longer life for the parts.  Enhanced powder purity  Enhance powder purity through the selective/reactive vaporization of impurities. The purity of the initial material by a factor of 10 to 100. Plasma spheroidization
  10. 10. Spray drying  In spray drying, water or alcohol based slurry is introduced into a spray drying chamber through a special atomization nozzle. In the hot gas flow and spherical granulates are formed.  Ceramic and cermet powders for thermal spraying and compaction with different particle size fractions Niro Spray Dryer P-6.3, pilot scale  Rotation atomizer  Particle size range: ~5-70 µm  Drying gas: air  Drying capacity: ~10 l/h Buchi Spray Dryer B-290, laboratory scale  Two-fluid atomizer  Particle size range: ~1-40 µm  Drying gas: air, N2  Drying capasity: ~0,5 l/h​ www.vtt.fi/powder
  11. 11. Fluidized bed Aeromatic MP-1 Fluidized bed can be used for drying, granulation, coating and encapsulating of powders and powder mixtures.  Bach sizes 0,35-6 kg differencing from material  Max. temperature 80°C (plexus cyclone)  Gas velocity 0,4-1,8 m/s  Sieves can be changed according to particle size  Liquid can be feeded both upwards and downwards  Larger granule size than with spray dryer  Closed loop processing by modification of the equipment  Can be scaled up and simulate continuous processes www.vtt.fi/powder
  12. 12. 22/12/2017 12 Indutherm VTC800V  Temperature: 2000°C, temperature read by a optical pyrometer (plus thermocouple up to 1300°C)  Ceramic crucible capacity: total 800 cm³  Flask’s size and Ingot moulds up to maximum ø125 x 220 mm  Automatic running for repeatable results  Melting modes: under higher vacuum, standard atmosphere (inert gas protection) or inert gas overpressure  Induction generator with 20 kW heating power, direct controlling of power  Low frequency induction = excellent mixing of liquid metal  After casting: automatic overpressure routine  Vibration technology ensures casting with excellent form filling, best metal density and top metal microstructure www.vtt.fi/powder Vacuum casting machine
  13. 13. Synthesis of Inorganic Particles Initial phase  synthesis  product Chemical synthesis is intentional chemical reaction to produce new material compositions or coated particles. Examples of result  Silanization of particles  Oxide particles with SOL-GEL  Nano carbides  Catalys synthesis Description of facility  Mixing equipment  Controlled atmosphere furnaces www.vtt.fi/powder
  14. 14. Mechanical milling and alloying  Circulating agitated ball mill  Different type and size of ball mills  Attritor, planetary, vibrating and conventional ball mils  Wet and dry milling  Mixing, alloying, coating, shape modification, grinding, dispersing etc.  50 ml to 20 l vial sizes  Vials and milling media; steel, hard metal, ceramic, rubber  Atmosphere; air, protective gas or reactive gas such as H2 www.vtt.fi/powder Agitated Lab Ball Mill 90 AHM
  15. 15. 22/12/2017 15 Powder Sieving and Classification Hoskawa Alpine  Air classification with integrated jet mill and hammer mill  Capacity 1 – 100kg  Separation of fines  Grinding of brittle materials Laboratory sieves  Sieving, laboratory Analysette  25, 32, 45, 63, 90, 125, 250, 500, 1000 µm  High productivity Douple Shaker sieve system  Continuous high productivity sieving system, capacity with metal powders ~10kg/h www.vtt.fi/powder
  16. 16. Powder consolidation www.vtt.fi/powder
  17. 17. 22/12/2017 17 Additive Manufacturing Selective Laser Melting SLM Solutions SLM 125 HL  Chamber size: 125x125x125 mm  Could be decreased 60x60x60 mm  Laser source: 400W IR fibre laser  Inert gas Ar or N2  Fully controllable process parameters  Suitable for the most of metal alloys www.vtt.fi/powder
  18. 18. Powder consolidation facilitiesHot Isostatic Pressing (HIP) HIP opportunities:  Special PM-Alloys, ceramics and MMCs  Bulk components and thick coatings with high wear and corrosion resistance  Near net shape components with internal structures and channels Example of result:  Steels and super alloys reinforced with oxide, nitride and carbide particles  Copper-steel compoud structure for ITER reactor wall  Optimized cooled plastic mold  High nitrogen steel from gas nitrided AISI 316 powder 5,7 % N (micrograph left) Description of HIP:  Chamber dimensions ø 130x300 mm  Tmax 1450°C or 2000°C  Pressure 207 Mpa (2070 bar), argon  Dilatometry for densification study www.vtt.fi/powder
  19. 19. Powder Injection Molding (PIM) PIM opportunities:  Prototypes and process design  Small complicated 3D-parts from conventional and high strenght wear resistant materials  Materials: stainless steel, carbon steel, copper, titanium and ceramics Example of result  Complicated components at costs of 50 % lower PIM facilities  Injection Molding machine Arburg 60 tn  Thermal, solvent and water de-binding  Sintering in high vacuum molybdenum furnace up to 1360°C or in low vacuum graphite furnace up to 2000°C  Post-treatments of steel components www.vtt.fi/powder
  20. 20. Thermal spray and coating facilities  Coating manufacturing processes  Plasma spraying  HVOF  HVAF  Cold spraying  Arc spraying  Powder and wire flame spraying  Polymer flame spraying  Laser cladding  CMD cladding www.vtt.fi/powderwww.tscf.fi
  21. 21. Post treatments & characterization www.vtt.fi/powder
  22. 22. 22/12/2017 22 TORVAC Compact 30 Model 1218, vacuum furnace (Cambridge Vacuum Engineering Ltd.)  Max. Temperature 1350°C  Possibility to gas quenching  Effective chamber size 200(L) x 400(W) x 200(H) mm  Batch size max. 60 kg  Molybdenum resistors, no carbon contamination  Atmospheres  Vacuum ~10-5 mbar  Argon 50 mbar www.vtt.fi/powder High temperature furnaces
  23. 23. 22/12/2017 23 VERTIVAC 150/2200 high temperature furnace  Effective size; dimeter 150 mm , height 160 mm  Max temperature 2200 °C, with thermocouples 650 °C, pyrometer T>1650 °C  Graphite resistors  Atmospheres  Vacuum 5*10-2 mbar  Argon , Nitrogen or another inert gas with pressure range 50 mbar - 1500 mbar  Argon-Hydrogen mixture gases  Cold box before vacuum pump enabling de- binding  Possibility for example reactive sintering with controllable atmosphere 2,5 - 1500 mbar with gas flow 0 - 30 l/h www.vtt.fi/powder High temperature furnaces
  24. 24. 22/12/2017 24 SARLIN LP25 fluidized bed furnace 200/400  Effective size: diameter 200 mm, height 400 mm  Max. temperature 1080 °C  Fluidized alumina bed provides homogeneous temperature, high thermal transfer and effective gas reactions  Atmospheres  Air  Inners gases: Argon, Nitrogen  Ammonia for nitriding  Hydrogen mixture gases  Propane-air mixture for carburization www.vtt.fi/powder High temperature furnaces
  25. 25. 22/12/2017 25 Rotary tube furnace  Variable tilting angle  Changeable tube  Maximum temperature 1550°C (1450°C in continuous use)  Variable gas atmosphere (air, N2, Ar, H2)  Gas tight 5l feeding  Collecting system Rotary furnace with reactive atmosphere www.vtt.fi/powder
  26. 26. Characterization  Particle size  Malvern mastersizer  Malvern nanosizer/zetasizer  Flowability, apparent density  Hall flow meter  Avalance angle  SEM/EDX  EDX mapping  Optical microscopy  XRD  High resolution detector  Small angle  Thermal analysis  Integrated TG/DSC/MS  Thermal conductivity www.vtt.fi/powder
  27. 27. Equipment for measuring particle size distributions for both wet and dry dispersions. General  Principle: laser light scattering  Measurement media: Liquid (water, ethanol), Air  Size range: wet 0,01-3500 µm; dry 0,1-3500 µm  Dispersion: wet ultrasonic; dry air pressure Optics  Red light source: Max. 4mW He-Ne, 632,8nm Blue light source: Max. 10mW LED, 470nm Detector  Angular range: 0,015-144 degrees www.vtt.fi/powder Particle size distribution Laser diffractometer: Master sizer 3000 (Malvern) Measurement unit AERO S for dry measurements HYDRO LV for wet measurements
  28. 28. 2822/12/2017 Thermal analysis Simultaneous Thermogravimetry (TGA), Differential Scanning Calorimetry (DSC) and Mass Spectrometry (MS) STA 449 F1 Jupiter r  Temperature range: RT to 1500°C (Platinum furnace)  Weighing range: 5000 mg (depends on size of crusible, in this model ~20 µl)  TGA resolution: 0,025 µg  DSC resolution < 1 µW (dependent on sensor)  Atmospheres: inert, oxidizing, reducing, static, dynamic, vacuum  Auto sampler QMS 403 D Aëolos mass spectrometry  Temperature range RT-1600°C  Mass Range 1 to 300 u*  Resolution 0.5 u* www.vtt.fi/powder
  29. 29. Zetasizer Nano ZS Equipment for measuring particle size, molecular size, zeta potential and molecular weight as function of pH Measurement type: Particle size and molecular size  Measurement range: 0,3 nm-10,0 µm  Measurement principle: Dynamic Laser Light Scattering Measurement type: Zeta potential  Measurement range: 3,8 nm-100 µm particle size  Measurement principle: Electrophoretic Laser Light Scattering, Brownian motion Measurement type: Molecular weight Measurement  Range 980 Da-20 Mda (g/mol)  Measurement principle: Static Laser Light Scattering using Debye plot Reference: Malvern website www.vtt.fi/powder Measurement unit Autotitrator
  30. 30. XRD  XRD, X-ray diffraction  High resolution detector  Small angle measurements  Determination of the crystal structure  Phase determination  Crystallinity  Easy conversion to transmission geometry  Measurement of thickness and quality of thin film structures  Measurement of nano-sized structures www.vtt.fi/powder
  31. 31. For more information please visit our website. www.vtt.fi/powder Interested? VTT Technical Research Centre of Finland Ltd

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