IP Library Granted Patent US 10,730,803
Granted Patent B2
US 10,730,803 · App. 15/277,553 · Granted Aug 4, 2020

Cold sintering ceramics and composites

Inventors: Clive A. Randall (University Park, PA); Jing Guo (University Park, PA); Amanda Baker (University Park, PA); Michael Lanagan (University Park, PA); Hanzheng Guo (University Park, PA)
Assignee: The Penn State Research Foundation
C04B35/645B32B5/16B32B7/04B32B9/005B32B9/045B32B9/048B32B15/08B32B15/16B32B18/00B32B27/08B32B27/14B32B27/281B32B27/285B32B27/286B32B27/288B32B27/302B32B27/304B32B27/308B32B27/32B32B27/322B32B27/34B32B27/365B32B27/40C04B35/447C04B35/453C04B35/4682C04B35/486C04B35/495C04B35/5152C04B35/6263C04B35/6264C04B35/62222C04B35/62685C04B35/634C04B35/638B32B2250/02B32B2262/101B32B2262/106B32B2264/107B32B2307/20B32B2307/202B32B2307/204B32B2307/50B32B2307/546B32B2307/702B32B2307/704B32B2307/728B32B2307/732C04B2235/3201C04B2235/3203C04B2235/3224C04B2235/3236C04B2235/3239C04B2235/3256C04B2235/3258C04B2235/3272C04B2235/3284C04B2235/3291C04B2235/3298C04B2235/5436C04B2235/604C04B2235/6026C04B2235/656C04B2235/6562C04B2235/6567C04B2235/6588C04B2235/77C04B2235/785C04B2237/068
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Quick Facts
Patent No.
US 10,730,803
App. No.
15/277,553
Granted
Aug 4, 2020
Kind
B2
Abstract

Cold sintering of materials includes using a process of combining at least one inorganic compound, e.g., ceramic, in particle form with a solvent that can partially solubilize the inorganic compound to form a mixture; and applying pressure and a low temperature to the mixture to evaporate the solvent and densify the at least one inorganic compound to form sintered materials.

Claims (33)

1. A process for preparing a sintered material, the process comprising:

combining at least one inorganic compound in particle form having a particle size of less than 50 μm with a solvent that can partially solubilize the inorganic compound to form a mixture; and

applying pressure and heat to the mixture via an unsealed device exposed to atmospheric pressure to evaporate the solvent such that evaporated solvent leaves the mixture and exits the unsealed device during the applying of the pressure and heat, the applying of the pressure and heat to the mixture densifying said at least one inorganic compound to a relative density of greater than 80%, wherein the applied heat is at a temperature of no more than 200° C. above the boiling point of the solvent at the atmospheric pressure and wherein the at least one inorganic compound and said densified at least one inorganic compound have the same composition.

2. The process according to claim 1 further comprising:

combining the at least one inorganic compound in particle form and at least one other substance with the solvent to form a composite mixture; and

wherein the applying of the pressure and heat is applied to the composite mixture to evaporate the solvent and densify said at least one inorganic compound to the relative density of greater than 80% to form a composite including said at least one other substance with said at least one inorganic compound having said relative density of greater than 80%.

3. The process of claim 2 , wherein the at least one other substance is a polymer.

4. The process according to claim 1 , wherein the solvent includes one or more source compounds that substantially prevent incongruent dissolution of the at least one inorganic compound when in contact with the solvent.

5. The process of claim 1 , wherein the applying of pressure and heat to the mixture to evaporate the solvent and densify said at least one inorganic compound occurs to densify said at least one inorganic compound to a relative density of at least 85% in a time period of no more than 60 minutes.

6. The process of claim 1 , wherein the applying of pressure and heat to the mixture to evaporate the solvent and densify said at least one inorganic compound occurs to densify said at least one inorganic compound to a relative density of at least 90% in a time period of no more than 180 minutes.

7. The process of claim 1 , wherein the solvent includes one or more of a C 1-12 alcohol, ketone, ester, or water, or an organic acid or mixtures thereof wherein the solvent has a boiling point below 200° C. at the atmospheric pressure, the atmospheric pressure being 1 atmosphere.

8. The process of claim 1 , wherein the solvent includes at least 50% by weight of water.

9. The process of claim 1 , wherein the at least one inorganic compound and the solvent are combined by exposing the at least one inorganic compound to a controlled relative atmosphere of the solvent.

10. The process of claim 1 , wherein the applied heat is at a temperature no more than 250° C.

11. The process of claim 1 , wherein the pressure applied during the applying of the pressure and the heat to the mixture is no more than about 5,000 MPa while the unsealed device is exposed to the atmospheric pressure, the atmospheric pressure being 1 atmosphere.

12. The process of claim 1 , wherein the at least one inorganic compound has a particle size of less than 30 μm.

13. The process of claim 1 , further comprising milling the at least one inorganic compound prior to forming the mixture.

14. The process of claim 1 , further comprising forming the mixture on two or more substrates and laminating the two or more substrates with said densified at least one inorganic compound.

15. The process of claim 1 , wherein the solvent is less than 30 wt % of the mixture.

16. The process of claim 1 , wherein the applying of the pressure and heat to the mixture via the unsealed device evaporates most of the solvent from the mixture in an open process at the atmospheric pressure so the evaporated solvent leaves the mixture and is emitted from the device.

17. The process of claim 16 , further comprising:

after the applying of the pressure and heat to the mixture via the unsealed device, further heating the mixture to completely evaporate any remaining portion of the solvent from the mixture.

18. A process for preparing a sintered material, the process comprising:

combining at least one inorganic compound in particle form having a particle size of less than 50 μm with a solvent that can partially solubilize the inorganic compound to form a mixture; and

applying pressure and heat to the mixture via a device to evaporate the solvent, the applying of the pressure and heat to the mixture densifying said at least one inorganic compound to a relative density of greater than 80%, wherein the applied heat is at a temperature of no more than 200° C. above the boiling point of the solvent at 1 atmosphere and wherein the at least one inorganic compound and said densified at least one inorganic compound have the same composition, wherein the applying of the pressure and heat to the mixture via the device evaporates the solvent such that solution-precipitation occurs via the evaporation of the solvent to enable a supersaturated state for driving densification of the at least one inorganic compound.

19. A process for preparing a sintered material, the process comprising:

combining at least one inorganic compound in particle form having a particle size of less than 50 μm with a solvent that can partially solubilize the inorganic compound to form a mixture; and

applying heat and uniaxial pressure to the mixture via a pressing device exposed to atmospheric pressure to evaporate the solvent and densify the at least one inorganic compound to a relative density of greater than 80%, wherein the applied heat is at a temperature of no more than 200° C. above the boiling point of the solvent at the atmospheric pressure and wherein the solvent is evaporated from the mixture during the applying of the heat and the uniaxial pressure and moves away from the pressing device.

20. The process of claim 19 , wherein the solvent is less than 30 wt % of the mixture.

21. The process of claim 19 , wherein the solvent includes at least 50% by weight of water.

22. The process of claim 19 , wherein the applying of the uniaxial pressure and heat to the mixture via the pressing device evaporates the solvent such that solution-precipitation occurs via the evaporation of the solvent to enable a supersaturated state for driving densification of the at least one inorganic compound.

23. The process of claim 19 , wherein the applying of the heat and the uniaxial pressure to the mixture via the pressing device evaporates most of the solvent from the mixture in an open process exposed to the atmospheric pressure to facilitate the evaporated solvent being emitted from the pressing device during the applying of the heat and the uniaxial pressure, the process also comprising:

after the applying of the heat and the uniaxial pressure to the mixture via the pressing device, further heating the mixture to completely evaporate any remaining portion of the solvent from the mixture.

Assignments (2)
CONFIRMATORY LICENSE Recorded Jan 26, 2017
From: PENNSYLVANIA STATE UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 041501/0302 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 4, 2016
From: RANDALL, CLIVE A.; GUO, JING; BAKER, AMANDA; LANAGAN, MICHAEL; GUO, HANZHENG
To: THE PENN STATE RESEARCH FOUNDATION
Reel/Frame 039930/0695 →
Continuity (4)
Continuation PCTUS2016053772 · Sep 26, 2016
Provisional Application 62234389 · Sep 29, 2015
Provisional Application 62349444 · Jun 13, 2016
Related Publication 20170088471A1 · Mar 30, 2017