Process for producing thin transparent ceramic parts and thin transparent ceramic parts

Patent metadata

Field	Value
Publication number	US-12024468-B2
Application number	US-201917413116-A
Country	US
Kind code	B2
Filing date	Dec 10, 2019
Priority date	Dec 14, 2018
Publication date	Jul 2, 2024
Grant date	Jul 2, 2024

Abstract

The invention relates to the field of ceramics and concerns a method for use in displays of electronic devices with high mechanical stress, for example. The object of the present invention is to provide a method by means of which thin ceramic parts having thicknesses of substantially <1 mm with high transparency are produced. The object is achieved by a method for producing thin transparent ceramic parts, in which ceramic powders are mixed together with a solvent and a monomer and a photoinitiator, and at least 0.0005% by mass of a photoinitiator is added, the mixture is subsequently introduced into a mould, then the mixture is irradiated for at least 1 min with light which has a wavelength for activating the photoinitiator, the moulded body is subsequently removed from the mould and dried, and then the debinding and sintering of the moulded body is carried out.

First claim

The invention claimed is:

1. A process for producing thin, <1 mm thick, transparent ceramic parts, having a transparency of RIT >70% of the theoretically possible transmission for ceramic materials of non-cubic crystal structure and having a transparency of RIT >90% of the theoretically possible transmission for ceramic materials of cubic crystal structure and a low frequency <50/cm 3 of visible defects >20 μm,
wherein ceramic powders for producing a transparent ceramic are mixed in conjunction with at least one solvent and at least one monomer and at least one photoinitiator,
wherein the solvents employed are solvent water or aqueous solvents or mixtures,
wherein the powders have a BET specific surface area of at least 6-20 m 2/ g, and during the mixing or subsequently at least 2% by mass of monomers capable of free-radical polymerization and 0.0005% to 0.05% by mass of a photoinitiator are added to the mixture, and the mixture is subsequently degassed and introduced into a mold which may comprise a carrier,
wherein monomers are added to the mixture in a mass ratio of monomer having one double bond: monomer having at least two double bonds of 2:1 to 5:1,
wherein molds having molded bodies having thicknesses of 10 to 1300 μm are employed,
wherein the mold is transparent at least for light having a wavelength necessary for activation of the photoinitiator, the mixture in the mold being subsequently irradiated at least one minute with light comprising at least one wavelength for activating the photoinitiator,
wherein after the first mixture further mixtures having an identical or different composition may be introduced into the mold atop a respectively irradiated mixture,
wherein after each introduction of a mixture an irradiation is performed, the molded body being subsequently demolded from the mold and dried and subsequently a debindering and sintering of the molded body is performed and subsequently a mechanical machining for producing the thin transparent ceramic parts may be carried out; and
wherein light in the wavelength range of 200-450 nm is used for irradiation.

2. The process as claimed in claim 1 , wherein the ceramic powders employed are selected from aluminum oxide, spinel MgAl 2 O 4 , cubic zirconium oxide, aluminum oxynitride AlON, yttrium oxide, yttrium aluminum garnet (YAG) Y 3 Al 5 O 12 , magnesium oxide.

3. The process as claimed in claim 1 , wherein the mixing is performed by milling in an attritor or a ball mill.

4. The process as claimed in claim 1 , wherein the monomers employed are methacrylamide or polyethylene glycol 1000 dimethacrylate, 2-hydroxyethyl methacrylate, tetrahydrofuryl methacrylate, 2-carboxyethyl acrylate, N,N-dimethylacrylamide, 1-vinyl-2-pyrrolidone and polyethylene glycol 1000 monomethyl ether monomethacrylate, N,N-methylenebisacrylamide and PEO(5800)-b-PPO(3000)-b-PEO(5800) dimethacrylate and/or mixtures of these monomers.

5. The process as claimed in claim 1 , wherein the photoinitiator employed is 1-hydroxycyclohexylphenylketone or 2-hydroxy-2-methylpropiophenone.

6. The process as claimed in claim 1 , wherein the degassing is performed under vacuum.

7. The process as claimed in claim 1 , wherein a carrier made of a porous material is employed.

8. The process as claimed in claim 1 , wherein the mixture in the mold is irradiated with light over 5 min to 20 min.

9. The process as claimed in claim 1 , wherein the mixture is introduced into the mold and subsequently irradiated and subsequently the mixture of a mixture having a different composition is introduced into the mold atop the previously irradiated mixture two or more times and after each introduction of a mixture said mixture is irradiated.

10. The process as claimed in claim 1 , wherein in the case of repeated introduction of mixtures into the mold identical or different amounts of mixture are introduced, wherein the individual mixtures are introduced atop one another to effect complete or partial coverage.

11. The process as claimed in claim 1 , wherein in the case of introduction of mixtures of different compositions the mixtures are irradiated with light of different or identical wavelength and/or for different or identical durations.

12. The process as claimed in claim 1 , wherein during production of the molded body as a gel body, dried gel body, green body and sintered body in the sequence of the process procedure the process conditions are realized under atmospheric conditions and/or pressurelessly.

13. The process as claimed in claim 1 , wherein known auxiliary and additive substances are employed for the suspending, mixing and producing of the molded bodies up to the gel body.

14. The process as claimed in claim 1 , wherein the drying of the molded body is performed in a polymer solution and atop and/or between carriers.

15. The process as claimed in claim 14 , wherein the polymer solution employed is selected from water soluble or alcohol-soluble polymers, such as polyvinyl alcohol, polyvinyl acetate, polyacrylamide, polyamide, polyethylene oxide, polyacrylate, polyvinylpyrrolidone, polyethylene glycol and/or derivatives or mixtures thereof.

16. The process as claimed in claim 1 , wherein the sintering is performed under the sintering conditions known for the sintering of transparent ceramics and/or to produce warpage-free transparent ceramics the parts are subjected to mechanical load at least during the sintering.

17. The process as claimed in claim 1 , wherein after the sintering of the molded body a mechanical machining of the sintered body by sawing, grinding and/or polishing is performed.

18. The process as claimed in claim 1 , wherein molds which realize molded bodies having thicknesses of 50 to 1000 μm are employed.

19. The process as claimed in claim 1 , wherein molds which realize molded bodies having thicknesses of 100 to 500 μm are employed.

20. The process as claimed in claim 1 , wherein a carrier made of paper sheets, membranes or ceramic films is employed.

Assignees

• Fraunhofer Ges Forschung
• Fraunhofer Ges Zue Foerderung Der Angewandten Forschung E V

Inventors

• Hildebrandt Stefanie
• Hutzler Thomas
• Berger Lutz-Michael

Classifications

• C04B2237/343

  Alumina or aluminates · CPC title

• C04B35/6455

  Hot isostatic pressing · CPC title

• C04B35/63424

  Polyacrylates; Polymethacrylates · CPC title

• C04B35/6261

  Milling · CPC title

• C04B35/44

  based on aluminates · CPC title