Freeze Granulation forProcessing of Nano Materials     Kent Rundgren, President of PowderPro AB                      Swede...
Freeze Granulation Process        Spray freezing                          Freeze dryingSuspension               Air       ...
Freeze Granulation vs Spray Drying Freeze granulation                                   Spray dryingNo shrinkage: density ...
Freeze Granulation                                              A variety of applications                 Atomisation     ...
Freeze Granulation of nanopowders                 Nanopowder Re-dispersed          No            Granulatedto nanopowder  ...
Freeze Granulation• Method to preserve nano properties• Method to produce homogeneous granules and preserve  material homo...
PowderPro ABFounded in 2000, as a spin-off company from the SwedishCeramic Institute, to provide equipment for freeze gran...
Freeze Granulator                                                         Models: LS-2                                    ...
Freeze drier GT-2                 Heated trays for quick drying                    Capacity to dry ca 2 litre of          ...
Aspects in processing of small units of matter• Difficulties to retain homogeneity during processing• Difficulties to keep...
Freeze Granulation Process Benefits•   Homogeneous granules    - No cavity or void formation    - No migration of any subs...
Granule propertiesFree-flowing granules with a wide granule size distribution (20–500 μm)Density depends on solids in susp...
Re-dispersibility of submicron powders - 1Freeze granulated/freeze-dried powders can be re-dispersed with impellerstirring...
Re-dispersibility of submicron powders - 2Powders, difficult to deagglomerate, can be dispersed at low concentrations, fre...
Granules of ”nano”powdersGranule based on 10-30 nm                      Granule based on 500 nm particlesparticles at low ...
Freeze Granulation of nanopowders                 Nanopowder Re-dispersed          No            Granulatedto nanopowder  ...
Various aspects and uses• All kinds of material in dispersed form can be granulated• Ideal for preparation of fine powder ...
PowderPro: Offers and Services– Supplies freeze granulation equipments for Lab,  Pilote-scale and production– Carry out te...
MissionPowderPros mission is to provide first-class FreezeGranulation and drying techniques for processing ofceramic and m...
Freeze Granulation - Summary• provides a competitive technique for the manufacture of  granules for various purposes• pres...
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Freeze granulation of nanomaterials from PowderPro Sweden

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PowderPro AB develops, manufactures, markets and sells equipment for Freeze Granulation, i.e. spray freezing and subsequent freeze drying – Spray Freeze Drying.
Freeze Granulation was developed in late 1980s at Swedish Ceramic Institute and it is also a development of Spray Freeze Drying (SFD) and Spray Freezing into Liquid (SFL).
In mid 70th W.W. Rhodes and S. Prochazka (1975) provided the first publications about Freeze Granulation of ceramic powders without defining the advantage or explaining the positive results.

Freeze granulation, spray freezing and subsequent freeze drying (lyophilization or cryodesiccation), a development of Spray Freeze Drying (SFD) and Spray Freezing into Liquid (SFL), was first developed for granulation of ceramic powders at Swedish Ceramic Institute (SCI) in Göteborg in the late 1980′s. It was early shown to be the most suitable method to provide optimal granule properties for lab and research purposes and, later on, also for pilot and production scale processing of ceramics and other powder-based materials.

During the 1990′s, Freeze Granulation was successfully applied in material and processing developments within many research projects and commercial contract work. Specific powder systems from various companies were tested with very good results, demonstrated by homogeneous granulates and improved final component/material properties. However, no commercial equipment was available and therefore PowderPro AB was founded in January 2000 with the objective to provide equipment for the process.

PowderPro AB develops, manufacture, market and sell granulation equipment and carries out test granulations (standard concept), whereas Swerea IVF conducts developments regarding suspension concepts and granulation methodology.

Several companies and research labs around the world have applied the Freeze Granulation process with the support of PowderPro AB. Typical applications for freeze granulation are homogeneous granulation and drying of ceramic powders; oxides (Al2O3, ZrO2, SiO2), nitrides (Si3N4) and carbides (SiC) and also metal oxides, nanomaterials (nanopowders), diamonds, LED Lighting, explosives (igniters, delay elements) and pharmaceuticals like proteins, enzymes and chemicals.

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Freeze granulation of nanomaterials from PowderPro Sweden

  1. 1. Freeze Granulation forProcessing of Nano Materials Kent Rundgren, President of PowderPro AB Sweden NanoMaterials 2010 www.powderpro.se
  2. 2. Freeze Granulation Process Spray freezing Freeze dryingSuspension Air Vacuum Atomisation Sublimation Frozen Instant granules freezing Ice Condensation - 30oC Liquid nitrogen (- 196oC) NanoMaterials 2010 www.powderpro.se
  3. 3. Freeze Granulation vs Spray Drying Freeze granulation Spray dryingNo shrinkage: density and Suspension Shrinkage during drying homogeneity retained droplet increases granule density Void formation Migration of binder and small particles to surface Formation of dried shell Sublimation Liquid transport NanoMaterials 2010 www.powderpro.se
  4. 4. Freeze Granulation A variety of applications Atomisation Instant freezing Spherical Homogenous granules ©Swerea IVF AB Free flowing©Swerea IVF AB Metal powders Bioceramics Ceramics Explosives Biomaterials Diamond tools LED-Lighting materials Grinding wheels Nanopowders Composites Catalysts Chemical Looping Nanomaterials Combustion Pharmaceuticals Material synthesis Chemicals Freeze Granulation – NanoMaterialsOptimised Powder Processing! The Way to 2010 www.powderpro.se www.powderpro.se
  5. 5. Freeze Granulation of nanopowders Nanopowder Re-dispersed No Granulatedto nanopowder agglomer nanopowder ation Dried to powder  Unique process to retain nanomaterial particle size  Nano-particles keep separated  Re-dispersible end-result NanoMaterials 2010 www.powderpro.se
  6. 6. Freeze Granulation• Method to preserve nano properties• Method to produce homogeneous granules and preserve material homogeneity• Method to avoid strong bonding and oxidation• Method to produce granules of nano materials that can be handled and processed in dry state• Method to produce granules, easy to re-disperse to original particle size distribution NanoMaterials 2010 www.powderpro.se
  7. 7. PowderPro ABFounded in 2000, as a spin-off company from the SwedishCeramic Institute, to provide equipment for freeze granulation- a privately owned, expanding company- science-based- affiliated to Swerea IVF AB and Chalmers Industriteknik- especially experienced in the ceramic and powder metallic fields- looking to expand into fields where high-quality freezegranulation can improve processes and output quality NanoMaterials 2010 www.powderpro.se
  8. 8. Freeze Granulator Models: LS-2 and LS-6Small scale with capacity to process up to 6 litre suspension per hourMedium scale with capacity of processing 25 litre per hour is underdevelopment NanoMaterials 2010 www.powderpro.se
  9. 9. Freeze drier GT-2 Heated trays for quick drying Capacity to dry ca 2 litre of granules that is achieved from ca 1 litre powder suspension Driers with much higher capacity exist on the market NanoMaterials 2010 www.powderpro.se
  10. 10. Aspects in processing of small units of matter• Difficulties to retain homogeneity during processing• Difficulties to keep small units separated• Drying from suspension causes agglomeration, segregation and oxidation• Difficulties to obtain handable/processable nanopowders in dry state• Difficulties to re-disperse from dry state NanoMaterials 2010 www.powderpro.se
  11. 11. Freeze Granulation Process Benefits• Homogeneous granules - No cavity or void formation - No migration of any substances or small particles to surface - No, or limited, shrinkage of granules - No formation of a dried shell● Granule density controlled by suspension composition● Vacuum drying minimizes oxidation● High yield, low waste of material● Process allows latex (water insoluble polymers) as binder● Recycling of solvent possible NanoMaterials 2010 www.powderpro.se
  12. 12. Granule propertiesFree-flowing granules with a wide granule size distribution (20–500 μm)Density depends on solids in suspensionSize depends on suspension viscosity and granulation parameters NanoMaterials 2010 www.powderpro.se
  13. 13. Re-dispersibility of submicron powders - 1Freeze granulated/freeze-dried powders can be re-dispersed with impellerstirring to the same de-agglomerated state as with planetary ball milling 1 Viscosity (Pa s) 0.1 Planetary milled (pH=9.8) Impeller stirred (pH=9.2) 0.01 1 10 100 1000 Shear rate (s-1) NanoMaterials 2010 www.powderpro.se
  14. 14. Re-dispersibility of submicron powders - 2Powders, difficult to deagglomerate, can be dispersed at low concentrations, freeze granulated/freeze-dried and re-dispersed at higher concentrations 100 Si3N4 (UBE E10) water suspensions at pH 10 44 vol% As-received Apparent viscosity (Pa s) 10 1 48.4 vol% Pre-treated 0.1 44 vol% Pre-treated 0.01 1 10 100 1000 Shear rate (s-1) NanoMaterials 2010 www.powderpro.se
  15. 15. Granules of ”nano”powdersGranule based on 10-30 nm Granule based on 500 nm particlesparticles at low concentration at high concentration NanoMaterials 2010 www.powderpro.se
  16. 16. Freeze Granulation of nanopowders Nanopowder Re-dispersed No Granulatedto nanopowder agglomer nanopowder ation Dried to powder  Unique process to retain nanomaterial particle size  Nano-particles keep separated  Re-dispersible end-result NanoMaterials 2010 www.powderpro.se
  17. 17. Various aspects and uses• All kinds of material in dispersed form can be granulated• Ideal for preparation of fine powder mixes with suitable additives for subsequent processing• Suspension quality always determines and will reflect the granule quality in terms of homogeneity• Favorable preparation step for material synthesis owing to the homogeneity of the granulated material• Water as medium is preferred but also organic solvents with suitable freezing point (-25 to +10°C) can be used NanoMaterials 2010 www.powderpro.se
  18. 18. PowderPro: Offers and Services– Supplies freeze granulation equipments for Lab, Pilote-scale and production– Carry out test granulations of customer-supplied materials– Supports process implementation and start-up with customersPowderPro has close collaboration with Swerea IVFAB in research related to freeze granulation in a widerange of material/applications NanoMaterials 2010 www.powderpro.se
  19. 19. MissionPowderPros mission is to provide first-class FreezeGranulation and drying techniques for processing ofceramic and metal powders, nanomaterials, diamonds,proteins, enzymes, fine chemicals and pharmaceuticals. NanoMaterials 2010 www.powderpro.se
  20. 20. Freeze Granulation - Summary• provides a competitive technique for the manufacture of granules for various purposes• preserves the material homogeneity• enhances subsequent processing performance• enables equally appropriate process for smaller and larger quantities with equal results• enables controlled granule density can be• provides mild drying with low degree of oxidation NanoMaterials 2010 www.powderpro.se
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