Method for making composite carbon nanotube structure
US-2015368107-A1 · Dec 24, 2015 · US
US9434650B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9434650-B2 |
| Application number | US-201314434679-A |
| Country | US |
| Kind code | B2 |
| Filing date | Oct 9, 2013 |
| Priority date | Oct 9, 2012 |
| Publication date | Sep 6, 2016 |
| Grant date | Sep 6, 2016 |
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The present invention relates to method for forming a porous ceramic material, the method comprising the steps of: providing a suspension of polymer-coated ceramic particles in a first solvent; contacting the suspension with a second solvent, whereby a ceramic material precursor is formed from the polymer and ceramic particles, heating the ceramic material precursor to at least partially decompose the polymer within the precursor into solid deposits, and then sintering the ceramic material precursor to form a porous ceramic material.
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The invention claimed is: 1. A method for forming a porous ceramic material, the method comprising the steps of: providing a suspension of polymer-coated ceramic particles in a first solvent; contacting the suspension with a second solvent, whereby a ceramic material precursor is formed from the polymer and ceramic particles, heating the ceramic material precursor in the presence of oxygen to at least partially decompose the polymer within the precursor into solid deposits, then sintering the ceramic material precursor under an inert atmosphere to form a porous ceramic material; and then heating the porous ceramic material under an oxygen-containing atmosphere to remove the solid deposits. 2. The method according to claim 1 , wherein the inert atmosphere comprises nitrogen. 3. The method according to claim 1 , wherein the ceramic particles comprise one or more metal oxides selected from Al 2 O 3 , ZrO, SiO 2 , CeO 2 , TiO 2 and mixtures of two or more thereof. 4. The method according to claim 1 , wherein the ceramic particles have a longest average diameter of from 5 to 0.01 microns. 5. The method according to claim 1 , wherein the polymer comprises one or more invertible polymers. 6. The method according to claim 1 , wherein the solid deposits comprise carbon deposits. 7. The method according to claim 1 , wherein the first solvent comprises one or more of N-methyl-2-pyrrolidone, dimethyl sulphoxide, tetrahydrofuran and Dimethyl acetamide. 8. The method according to claim 1 , wherein the second solvent comprises water. 9. The method according to claim 1 , wherein the ceramic material precursor is sintered at a temperature of from 1200 to 1600° C. 10. The method according to claim 1 , wherein the porous ceramic material is in the form of a hollow fiber. 11. The method according to claim 1 , wherein the step of heating the ceramic material precursor comprises heating the ceramic material precursor in air at a temperature sufficient to cause at least partial decomposition of the polymer. 12. The method according to claim 1 , wherein the porous ceramic material is a porous ceramic membrane. 13. The method of claim 1 , wherein: the ceramic material precursor is sintered under an inert atmosphere at a temperature of from 1000 to 1300° C. to form the porous ceramic material; and the porous ceramic material is heated under an oxygen-containing atmosphere of greater than 600° C. to remove the solid deposits. 14. The method according to claim 1 , wherein heating of the ceramic material precursor in the presence of oxygen to at least partially decompose the polymer within the precursor into solid deposits occurs as a multi-step operation. 15. The method according to claim 1 , wherein the ceramic material precursor is heated in the presence of oxygen at a temperature of from 450 to 550° C. to at least partially decompose the polymer within the precursor into solid deposits. 16. The method according to claim 1 , wherein during heating of the ceramic material precursor in the presence of oxygen to at least partially decompose the polymer within the precursor into solid deposits the temperature is ramped at a rate of from 1 degree/minute to 25 degrees/minute to a desired temperature, followed by ramping the temperature down from the desired temperature at a rate of from 1 degree/minute to 25 degrees/minute. 17. A method for forming a porous ceramic material, the method comprising the steps of: providing a suspension of polymer-coated ceramic particles in a first solvent; contacting the suspension with a second solvent, whereby a ceramic material precursor is formed from the polymer and ceramic particles, heating the ceramic material precursor to at least partially decompose the polymer within the precursor into solid deposits by heating the ceramic material precursor under an inert atmosphere to decompose the polymer into the solid deposits comprising carbon deposits and then heating under an oxygen-containing atmosphere to partially remove the carbon deposits from the ceramic material precursor; and then sintering the ceramic material precursor to form a porous ceramic material. 18. The method of claim 17 , wherein the ceramic material precursor is heated under the inert atmosphere at a temperature of from 1000 to 1300° C., and then heated under the oxygen-containing atmosphere at a temperature greater than 600° C. 19. A method for forming a porous ceramic material, the method comprising the steps of: providing a suspension of polymer-coated ceramic particles in a first solvent; contacting the suspension with a second solvent, whereby a ceramic material precursor is formed from the polymer and ceramic particles, heating the ceramic material precursor to at least partially decompose the polymer within the precursor into solid deposits by heating the ceramic material precursor under an oxygen-containing atmosphere to partially decompose the polymer into the solid deposits and then under an inert atmosphere to fully decompose the solid deposits into carbon deposits, and then heating under an oxygen containing atmosphere to partially remove the carbon deposits from the ceramic material precursor; and then sintering the ceramic material precursor to form a porous ceramic material. 20. A method for forming a porous ceramic material, the method comprising the steps of: providing a suspension of polymer-coated ceramic particles in a first solvent; contacting the suspension with a second solvent, whereby a ceramic material precursor is formed from the polymer and ceramic particles, heating the ceramic material precursor in a sealed oxygen-containing atmosphere to at least partially decompose the polymer within the precursor into solid deposits and to partially remove the solid deposits from the ceramic material precursor; and then sintering the ceramic material precursor to form a porous ceramic material once there is no oxygen remaining in the sealed atmosphere.
comprising aluminium oxide or hydroxide; comprising bauxite · CPC title
Membrane, sheet, cloth, pad, lamellar or mat · CPC title
at an oxygen percentage above that of air · CPC title
at an oxygen percentage below that of air · CPC title
submicron sized, i.e. from 0,1 to 1 micron · CPC title
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