Nanopowder Production A Comparison of Several Methods

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1 Nanopowder Production A Comparison of Several Methods Gimena Gordillo Xavier Hailey Advisors: Prof. G. A. Mansoori Grad. Student Listowel Agyarko

2 Outline Introduction to Nanotechnology 1. What is Nanotechnology 2. Nanostructures 3. The Importance of Nanotechnology 4. Applications of Nanotechnology Research 1. Objectives 2. Crystallization 3. Nanopowder Production Techniques

3 What is Nanotechnology? Research and Development in the length scale of nanometer range. Build micro and macro materials and products with atomic precision.

4 Nanostructures

5 Importance of Nanotechnology Nanoscale variations effects on atomic structure. Conduction properties Higher density than microstructures. High surface to volume ratio.

6 Applications of Nanotechnology Robots in Living Systems Electronics Catalysts Information Storage Capacity Pharmaceuticals

7 Applications of Nanotechnology Comparison between micro and nano Molybdenum

8 Nanopowders Applications Pharmaceuticals Pigments Polymers Particle Formation Chemical Routes Physical Methods

9 Nanopowder Production Disadvantages of Conventional Methods of Powder Production Particle Size Characteristics Energy Costs Material Liabilities Supercritical Fluids as an Alternative Better Particle Size Characteristics Lower Energy Costs Milder Process

10 Crystallization β= concentration /supersaturation concentration Nucleation vs. Crystal Growth Effects on the size distribution of particles Fig.1. Time vs. Supersaturation Ratio [7]

11 RESEARCH

12 Objectives Study and compare nanopowder production techniques Rapid Expansion of Supercritical Solutions (RESS) Supercritical Anti-solvent (SAS) Particle from Gas Saturated Solutions (PGSS) Depressurization of an Expanded Liquid Organic Solution (DELOS)

13 Rapid Expansion of Supercritical Solutions (RESS) Applications Pharmaceuticals Encapsulation Driving Force Pressure gradient in the nozzle Description of Process 1. Dissolution of Solute 2. Rapid Depressurization 2

14 RESS Process 2

15 Rapid Expansion of Supercritical Solutions (RESS) Working Condition Change Effects Temperature and Pressure Advantages Organic Solvent not required No Environment Hazard Disadvantages Several families are not soluble in CO 2

16 Supercritical Anti Solvent (SAS) Applications Pharmaceuticals Polymers & Biopolymers Catalysts Driving Force Supersaturation Ratio, β>1 Description of Process 1. Dissolution 2. Mixing & Crystallization 3. Stripping

17 SAS Process Liquid CO 2 cylinder Solution vessel Mixing device Heat Exchanger Collecting basket Pump

18 Supercritical Antisolvent (SAS) Working Condition Change Effects Small Effects from Pressure and Temperature Mixing and Droplet Formation in Nozzle Advantages Formation of Particles Solubility Large range of materials Easy Removal of Antisolvent Disadvantages Removal of Solvent

19 Particles from Gas Saturated Solutions (PGSS) Applications Pharmaceuticals, Including Lipids Driving Force Large Drop from Working Pressure to Atmospheric Pressure Description of Process 1. Melting of Solvent Under Pressure 2. Expansion of Solution Through Nozzle

20 PGSS Process Mixing Vessel Pump Nozzle Expansion Vessel CO 2 2 Solvent Recycle Reservoir Recycle

21 Particles from Gas Saturated Solutions (PGSS) Working Condition Change Effects Pressure Effects on Morphology and Aggregation Advantages Broad Range of Materials Solvent-free Process Allows for Encapsulation & Micro Composites Disadvantages SCF Dissolution

22 PGSS SEM images of Theophylline/HPO composite particles formed by PGSS process at 359 K and a. 18 MPa b. 14 MPa to atmospheric conditions [6].

23 Depressurization of an Expanded Liquid Organic Solution (DELOS) Applications Dyes and Chemical Intermediates Specialty Polymers & Explosives Driving Force Large Temperature Gradient Description of Process 1. Dissolution 2. Pressurization 3. Expansion

24 DELOS Process Pump Mixing Vessel CO 2 Expansion Vessel NO 2 Separation Vessel Solvent Reservoir Recycle

25 Depressurization of an Expanded Liquid Organic Solution (DELOS) Working Condition Change Effects Working Pressure & Flow Rate Particle Characteristics & solubility ratio. Advantages Mild Process Allows for Encapsulation Disadvantages Solubility Limit to Process

26 DELOS SEM images of particles produced by DELOS process [

27 Conclusions RESS SAS PGSS DELOS Applications Small Mol. Small Mol. High Purity Larger Mol. Role of SCF Solvent Anti-Solvent Solute Co-Solvent Driving Force Pressure Solubility Temperature Temperature Working Pressure Dependence SCF SCF Morphology SCF Working Temperature Dependence SCF SCF Highest SCF Length of Procedure 2 Steps 3 Steps 2 Steps 3 Steps Particle Size micro & nano micro & nano micro & nano micro & nano Encapsulation Yes Yes Yes Yes

28 Conclusions Selection of Process Supercritical Fluid Interaction With Desired Product Desired Product Characteristics Capital and Operational Costs

29 Future Work Development of Computational Models Building of Experimental Setups Production of Products Analysis of Products

30 Acknowledgements Prof. G. A. Mansoori Graduate Student Listowel Agyarko Prof. R. Turian NSF for Financial Support

31 References 1. Mansoori, G. A. Advances in Atomic & Molecular Nanotechnology NanoMo.htm 5. Fages, J. et al. Particle Generation for Pharmaceutical Applications Using Supercritical Fluid Technology. 6. Rodrigues, M. et al. Microcomposites theophylline/hydrogenated palm oil from a PGSS process for controlled drug delivery systems. 7. Ventosa, N. et al. DELOS Process: a crystallization technique using compressed fluids1. comparison to the GAS crystallization method. 8. Ventosa, N. et al. Depressurization of an Expanded Liquid Organic Solution (DELOS): A New Produce for Obtaining Submicron or Micron Sized Crystalline Particles.

32 Questions?

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