PROCESS FOR PREPARING ADVANCED CERAMIC POWDERS USING ONIUM DICARBOXYLATES

• US 20090250850A1
• Filed: 04/03/2009
• Published: 10/08/2009
• Est. Priority Date: 04/03/2008
• Status: Active Grant

• Current Assignee: Sachem, Inc.
• Original Assignee: Sachem, Inc.
• Inventors: Wilson, Wilfred Wayne
• Granted Patent: US 7,867,471 B2
• Time in Patent Office: Days
• US Class Current: 264/624
• CPC Class Codes: C01B 13/18 by thermal decomposition of compounds, e.g. of salts or hydroxides
• CPC Class Codes: C01G 23/006 Alkaline earth titanates
• CPC Class Codes: C01P 2002/72 by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2004/60 Particles characterised by their size
• CPC Class Codes: C01P 2004/61 Micrometer sized, i.e. from 1-100 micrometer
• CPC Class Codes: C04B 2235/3203 Lithium oxide or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3206 Magnesium oxides or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3208 Calcium oxide or oxide-forming salts thereof, e.g. lime
• CPC Class Codes: C04B 2235/3213 Strontium oxides or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3224 Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
• CPC Class Codes: C04B 2235/3225 Yttrium oxide or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3227 Lanthanum oxide or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3229 Cerium oxides or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3251 Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3256 Molybdenum oxides, molybdates or oxide forming salts thereof, e.g. cadmium molybdate
• CPC Class Codes: C04B 2235/3258 Tungsten oxides, tungstates, or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3272 Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
• CPC Class Codes: C04B 2235/3275 Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
• CPC Class Codes: C04B 2235/3284 Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
• CPC Class Codes: C04B 2235/3286 Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
• CPC Class Codes: C04B 2235/3298 : Bismuth oxides, bismuthates or oxide forming salts thereof, e.g. zinc bismuthate
• CPC Class Codes: C04B 2235/449 : Organic acids, e.g. EDTA, citrate, acetate, oxalate
• CPC Class Codes: C04B 2235/5436 : micrometer sized, i.e. from 1 to 100 micron
• CPC Class Codes: C04B 2235/5481 : Monomodal
• CPC Class Codes: C04B 35/01 : based on oxide ceramics
• CPC Class Codes: C04B 35/016 : based on manganites
• CPC Class Codes: C04B 35/16 : based on silicates other than clay zircon C04B35/48
• CPC Class Codes: C04B 35/44 : based on aluminates
• CPC Class Codes: C04B 35/447 : based on phosphates , e.g. hydroxyapatite
• CPC Class Codes: C04B 35/457 : based on tin oxides or stannates
• CPC Class Codes: C04B 35/46 : based on titanium oxides or titanates containing also zirconium or hafnium oxides, zirconates or hafnates C04B35/49
• CPC Class Codes: C04B 35/4682 : based on BaTiO3 perovskite phase
• CPC Class Codes: C04B 35/47 : based on strontium titanates
• CPC Class Codes: C04B 35/472 : based on lead titanates
• CPC Class Codes: C04B 35/481 : containing silicon, e.g. zircon
• CPC Class Codes: C04B 35/486 : Fine ceramics
• CPC Class Codes: C04B 35/49 : containing also titanium oxides or titanates
• CPC Class Codes: C04B 35/491 : based on lead zirconates and lead titanates , e.g. PZT
• CPC Class Codes: C04B 35/495 : based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
• CPC Class Codes: C04B 35/497 : based on solid solutions with lead oxides
• CPC Class Codes: C04B 35/50 : based on rare-earth compounds non-oxide rare earth compounds C04B35/5156
• CPC Class Codes: C04B 35/505 : based on yttrium oxide

Abstract

A process of producing a ceramic powder including providing a plurality of precursor materials in solution, wherein each of the plurality of precursor materials in solution further comprises at least one constituent ionic species of a ceramic powder, combining the plurality of precursor materials in solution with an onium dicarboxylate precipitant solution to cause co-precipitation of the ceramic powder precursor in a combined solution; and separating the ceramic powder precursor from the combined solution. The process may further include calcining the ceramic powder precursor.

Claims

1. A process of producing a ceramic powder comprising:

providing a plurality of precursor materials in solution, wherein each of the plurality of precursor materials in solution further comprises at least one constituent ionic species of a ceramic powder;

combining the plurality of precursor materials in solution with an onium dicarboxylate precipitant solution to cause co-precipitation of the ceramic powder precursor in a combined solution; and

separating the ceramic powder precursor from the combined solution.

2. The process of claim 1 wherein the precipitant solution is substantially free of ammonium ion.

3. The process of claim 1 wherein the onium dicarboxylate comprises a quaternary onium having general formula (II):

4. The process of claim 1 wherein the onium dicarboxylate comprises a tertiary sulfonium having general formula (III):

5. The process of claim 1 wherein the onium dicarboxylate comprises a tertiary sulfoxonium having general formula (IV):

6. The process of claim 1 wherein the onium dicarboxylate comprises an imidazolium having general formula (V):

7. The process of claim 1 wherein the onium dicarboxylate comprises one or more of oxalate, malonate, succinate, glutarate, adipate, carbonate, maleate, fumarate, phthalate, isophthalate and terephthalate.

8. The process of claim 7 wherein the onium dicarboxylate comprises tetramethyl ammonium oxalate.

9. The process of claim 1 wherein the onium dicarboxylate comprises tetramethyl ammonium oxalate and a second onium oxalate wherein the second onium has a general formula (II):

10. The process of claim 1 wherein the precursor materials comprise ions of one or a combination of two or more of:

Mg, Ca, Sr, Ba, Al, Si, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Y, Zr, Nb, Mo, Tc, Ru, Rh, Th, Pd, Ag, Cd, In, Sn, Sb, Si, La, Hf, Ta, W, Re, Os, Ir, Pt, Tl, Pb, Bi, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Dy, Er, Ho, Er, Tm, Tb, Th, Pa, U, Np and Pu.

11. The process of claim 1 further comprising calcining the ceramic powder precursor to form a ceramic powder.

12. The process of claim 11 wherein the calcining is carried out at a temperature in the range from about 200°

C. to about 1500°

C. for a time in the range from about 1 minute to about 24 hours.

13. The process of claim 11 further comprising sintering the ceramic powder subsequent to the calcining.

14. The process of claim 13 wherein the sintering is carried out at a temperature in the range from about 1000°

C. to about 3000°

C. for a time in the range from about 1 minute to about 24 hours.

15. The process of claim 1 wherein the ceramic powder exhibits at least one improved property comprising one or more of improved particle size distribution, reduced particle size, reduced metal impurities and improved particle morphology, improved compositional homogeneity, improved control of stoichiometry, improved re-dispersability and enhanced chemical stability, as compared to a ceramic powder made by a process not including the onium dicarboxylate as precipitant.

16. A process of producing a ceramic powder comprising:

providing a plurality of precursor materials in solution, wherein each of the plurality of precursor materials in solution further comprises at least one constituent ionic species of a ceramic powder,

combining the plurality of precursor materials in solution with an onium oxalate precipitant solution substantially free of ammonium ion to cause co-precipitation of the ceramic powder precursor in a combined solution;

separating the ceramic powder precursor from the combined solution;

calcining the separated ceramic powder precursor to form a ceramic powder;

forming the ceramic powder into a green body; and

sintering the green body.

17. The process of claim 16 wherein the onium dicarboxylate comprises a quaternary onium having general formula (II):

18. The process of claim 16 wherein the onium dicarboxylate comprises a tertiary sulfonium having general formula (III):

19. The process of claim 16 wherein the onium dicarboxylate comprises a tertiary sulfoxonium having general formula (IV):

20. The process of claim 16 wherein the onium dicarboxylate comprises an imidazolium having general formula (V):

21. The process of claim 16 wherein the onium dicarboxylate comprises tetramethyl ammonium oxalate.

22. The process of claim 16 wherein the onium dicarboxylate comprises tetramethyl ammonium oxalate and a second onium oxalate wherein the second onium has a general formula (II):

23. The process of claim 16 wherein the precursor materials comprise ions of one or a combination of two or more of:

Mg, Ca, Sr, Ba, Al, Si, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Y, Zr, Nb, Mo, Tc, Ru, Rh, Th, Pd, Ag, Cd, In, Sn, Sb, Si, La, Hf, Ta, W, Re, Os, Ir, Pt, Tl, Pb, Bi, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Dy, Er, Ho, Er, Tm, Tb, Th, Pa, U, Np and Pu.

24. The process of claim 16 wherein the calcining is carried out at a temperature in the range from about 200°

C. to about 1500°

C. for a time in the range from about 1 minute to about 24 hours.

25. The process of claim 16 wherein the sintering is carried out at a temperature in the range from about 1000°

C. to about 3000°

C. for a time in the range from about 1 minute to about 24 hours.

26. The process of claim 16 wherein the ceramic powder exhibits at least one improved property comprising one or more of improved particle size distribution, reduced particle size, reduced metal impurities and improved particle morphology, improved compositional homogeneity, improved control of stoichiometry, improved re-dispersability and enhanced chemical stability, as compared to a ceramic powder made by a process not including the onium dicarboxylate as precipitant.