VTT Powder Piloting Service: Facilities
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Powder Piloting Service Material solutions, from powder to product. VTT Technical Research Centre of Finland Ltd Facilities www.vtt.fi/powder
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Transcript of VTT Powder Piloting Service: Facilities
Powder Piloting Service
Material solutions, from powder to product.
VTT Technical Research Centre of Finland Ltd
Facilities
www.vtt.fi/powder
Post treatments
& characterizationPowder
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
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 VTTMaterial efficiency via tailored material and production routes
www.vtt.fi/powder
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
Powder
manufacturing
www.vtt.fi/powder
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
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
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
922/12/2017
TEKSPHERO-15
15 kW induction plasma system for powder
spheroidization and purification
Semi continuous approx. 5 liters batch size
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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
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
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
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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
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
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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
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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
Powder
consolidation
www.vtt.fi/powder
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Additive ManufacturingSelective 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
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
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
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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
Post treatments
& characterization
www.vtt.fi/powder
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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
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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
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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
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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
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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
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
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Particle size distributionLaser diffractometer: Master sizer 3000 (Malvern)
Measurement unit
AERO S for dry measurements
HYDRO LV for wet measurements
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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
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
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
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For more information
please visit our website.
www.vtt.fi/powder
Interested?
VTT Technical Research Centre of Finland Ltd
