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Freeze Granulation for
Processing of Nano Materials
     Kent Rundgren, President of PowderPro AB

                      Sweden




                 NanoMaterials 2010       www.powderpro.se
Freeze Granulation Process
        Spray freezing                          Freeze drying
Suspension               Air                                         Vacuum


 Atomisation                                                      Sublimation

                                Frozen
  Instant                      granules
 freezing

                                               Ice                   Condensation
                                                     - 30oC



       Liquid nitrogen (- 196oC)


                               NanoMaterials 2010             www.powderpro.se
Freeze Granulation vs Spray Drying

 Freeze granulation                                   Spray drying

No 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
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
Freeze Granulation of nanopowders

                 Nanopowder




 Re-dispersed          No            Granulated
to 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
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
PowderPro AB

Founded in 2000, as a spin-off company from the Swedish
Ceramic 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 freeze
granulation can improve processes and output quality




                        NanoMaterials 2010        www.powderpro.se
Freeze Granulator



                                                         Models: LS-2
                                                         and LS-6




Small scale with capacity to process up to 6 litre suspension per hour
Medium scale with capacity of processing 25 litre per hour is under
development



                           NanoMaterials 2010           www.powderpro.se
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
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
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
Granule properties




Free-flowing granules with a wide granule size distribution (20–500 μm)
Density depends on solids in suspension
Size depends on suspension viscosity and granulation parameters


                           NanoMaterials 2010         www.powderpro.se
Re-dispersibility of submicron powders - 1
Freeze granulated/freeze-dried powders can be re-dispersed with impeller
stirring 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
Re-dispersibility of submicron powders - 2
Powders, 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
Granules of ”nano”powders




Granule based on 10-30 nm                      Granule based on 500 nm particles
particles at low concentration                       at high concentration

                                 NanoMaterials 2010            www.powderpro.se
Freeze Granulation of nanopowders

                 Nanopowder




 Re-dispersed          No            Granulated
to 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
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
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
  customers

PowderPro has close collaboration with Swerea IVF
AB in research related to freeze granulation in a wide
range of material/applications


                   NanoMaterials 2010     www.powderpro.se
Mission



PowderPro's mission is to provide first-class Freeze
Granulation and drying techniques for processing of
ceramic and metal powders, nanomaterials, diamonds,
proteins, enzymes, fine chemicals and pharmaceuticals.




                    NanoMaterials 2010      www.powderpro.se
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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Freeze granulation of nanomaterials from PowderPro Sweden

  • 1. Freeze Granulation for Processing of Nano Materials Kent Rundgren, President of PowderPro AB Sweden NanoMaterials 2010 www.powderpro.se
  • 2. Freeze Granulation Process Spray freezing Freeze drying Suspension Air Vacuum Atomisation Sublimation Frozen Instant granules freezing Ice Condensation - 30oC Liquid nitrogen (- 196oC) NanoMaterials 2010 www.powderpro.se
  • 3. Freeze Granulation vs Spray Drying Freeze granulation Spray drying No 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. 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. Freeze Granulation of nanopowders Nanopowder Re-dispersed No Granulated to 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. 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. PowderPro AB Founded in 2000, as a spin-off company from the Swedish Ceramic 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 freeze granulation can improve processes and output quality NanoMaterials 2010 www.powderpro.se
  • 8. Freeze Granulator Models: LS-2 and LS-6 Small scale with capacity to process up to 6 litre suspension per hour Medium scale with capacity of processing 25 litre per hour is under development NanoMaterials 2010 www.powderpro.se
  • 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. 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. 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. Granule properties Free-flowing granules with a wide granule size distribution (20–500 μm) Density depends on solids in suspension Size depends on suspension viscosity and granulation parameters NanoMaterials 2010 www.powderpro.se
  • 13. Re-dispersibility of submicron powders - 1 Freeze granulated/freeze-dried powders can be re-dispersed with impeller stirring 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. Re-dispersibility of submicron powders - 2 Powders, 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. Granules of ”nano”powders Granule based on 10-30 nm Granule based on 500 nm particles particles at low concentration at high concentration NanoMaterials 2010 www.powderpro.se
  • 16. Freeze Granulation of nanopowders Nanopowder Re-dispersed No Granulated to 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. 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. 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 customers PowderPro has close collaboration with Swerea IVF AB in research related to freeze granulation in a wide range of material/applications NanoMaterials 2010 www.powderpro.se
  • 19. Mission PowderPro's mission is to provide first-class Freeze Granulation and drying techniques for processing of ceramic and metal powders, nanomaterials, diamonds, proteins, enzymes, fine chemicals and pharmaceuticals. NanoMaterials 2010 www.powderpro.se
  • 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