Preparation of nanophase solid state materials

• US 5,417,956 A
• Filed: 08/18/1992
• Issued: 05/23/1995
• Est. Priority Date: 08/18/1992
• Status: Expired due to Fees

• Current Assignee: Worcester Polytechnic Institute
• Original Assignee: Worcester Polytechnic Institute
• Inventors: Moser, William R.
• Primary Examiner(s): LANGEL, WAYNE A
• Application Number:
  US07/931,765
• Time in Patent Office: 1,008 Days
• Field of Search: 423/592, 423/593, 423/598, 423/608, 423/636, 423/625, 423/263, 423/632
• US Class Current: 423/592.1
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 13/36 by precipitation reactions in aqueous solutions C01B13/328 takes precedence
• CPC Class Codes: C01F 7/34 Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
• CPC Class Codes: C01G 23/006 Alkaline earth titanates
• CPC Class Codes: C01G 25/02 Oxides
• CPC Class Codes: C01P 2004/04 obtained by TEM, STEM, STM or AFM
• CPC Class Codes: C01P 2004/50 Agglomerated particles
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer

Abstract

A process for the preparation of nanophase solid state materials having crystallite morphology and particle sizes in the range of from about 1 nm to 30 nm is disclosed. Novel nanophase solid state materials are also disclosed.

Claims

1. A process for producing nanophase solid state materials comprising (1) mixing together a metal containing solution and a second solution containing a precipitating agent to form a mixed solution, (2) pressurizing the mixed solution to a pressure of about 1,000 to 50,000 psig, (3) passing the pressurized mixed solution into a fluidizing apparatus wherein high shear forces act on the mixed solution, creating nanophase solid state materials having nanosize particles having average sizes of from about 1 to 30 nm, (4) depressurizing the mixed solution so as to cause cavitation and (5) separating the nanophase solid material from the cavitated mixed solution.

2. The process of claim 1, wherein the pressure is of from about 25,000 to 50,000 psig.

3. The process of claim 1, wherein the metal containing solution and the precipitating agent containing solution are mixed prior to passage into the fluidizing apparatus.

4. The process of claim 1, wherein the mixed solution is recycled through the fluidizer apparatus.

5. The process of claim 4, wherein the precipitating agent solution is added to the mixed solution as it is recycled.

6. The process of claim 4, wherein the metal containing solution is added to the mixed solution as it is recycled.

7. The process of claim 1, wherein the metal containing solution and the precipitating agent solution are mixed together as they enter the pressurizing pump.

8. The process of claim 1, wherein the metal containing solution is a metal salt solution.

9. The process of claim 1, wherein the salt is selected from the group consisting of nitrate, acetate, chloride, sulfate and bromide.

10. The process of claim 1, wherein the average particle size is less than about 10 nm.

11. The process of claim 1, wherein the average particle size is about 1 to 3 nm.

12. The process of claim 1, wherein the solid state material is crystalized.

13. The process of claim 1, wherein the metal containing solution and the precipitating agent solution are mixed together in a separate vessel.

14. A process for producing a calcined nanophase solid state material comprising (1) mixing together a metal containing solution and a second solution containing a precipitating agent to form a mixed solution, (2) pressurizing the mixed solution to a pressure of about 20,000 to 50,000 psig, (3) passing the pressurized mixed solution into a fluidizing apparatus wherein high shear forces act on the mixed solution, creating nanophase solid state materials having nanosize particles having average sizes of from about 1 to 30 nm, (4) depressurizing the mixed solution so as to cause cavitation and calcination, and (5) separating the calcined nanophase solid material from the cavitated mixed solution.

15. The process of claim 14, wherein the metal containing solution and the precipitating agent containing solution are mixed prior to passage into the fluidizing apparatus.

16. The process of claim 14, wherein the mixed solution is recycled through the fluidizer apparatus.

17. The process of claim 16, wherein the precipitating agent solution is added to the mixed solution as it is recycled.

18. The process of claim 16, wherein the metal containing solution is added to the mixed solution as it is recycled.

19. The process of claim 14, wherein the metal containing solution and the precipitating agent solution are mixed together as they enter the pressurizing pump.