IP Library Granted Patent US 10,472,287
Granted Patent B2
US 10,472,287 · App. 15/320,727 · Granted Nov 12, 2019

Method of manufacturing a sulfide-based ceramic element, particularly for IR-optics applications

Inventors: Noha Hakmeh (Cesson-Sevigne, FR); Odile Merdrignac-Conanec (Acigne, FR); Xiang-Hua Zhang (Cesson-Sevigne, FR)
Assignees: CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE; UNIVERSITE DE RENNES 1
C04B35/547C01G9/08C04B35/64C04B35/645C04B2235/666C04B2235/667C04B2235/9653
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Quick Facts
Patent No.
US 10,472,287
App. No.
15/320,727
Granted
Nov 12, 2019
Kind
B2
Abstract

A method of manufacturing a sulfide-based ceramic element, such as a transparent infrared optical element, comprises the steps of: synthesizing a sulfide powder; and sintering the powder to form the ceramic element; wherein the step of synthesizing the sulfide powder is performed by combustion in an aqueous solution, the solution comprising water as its only solvent, or containing water as its main solvent and at most 10%, and preferably at most 1% of the overall solvent mass, of one or more combustible solvents. The sulfide powder may be chosen, in particular, among ZnS, BaLa 2 S 4 , CaLa 2 S 4 .

Claims (13)

1. A method of manufacturing a sulfide-based transparent infrared optical ceramic element comprising the steps of:

synthesizing a sulfide powder; and

sintering said powder to form said ceramic element;

wherein said step of synthesizing said sulfide powder is performed by combustion in the presence of water by heating the aqueous solution at a temperature comprised between 400° C. and 800° C., said solution comprising 90-100% water and 0-10% of one or more non-water solvents based on the overall solvent mass.

2. The method according to claim 1 wherein said sulfide powder is chosen among ZnS, BaLa 2 S 4 and CaLa 2 S 4 .

3. The method according to claim 1 wherein said step of synthesizing said sulfide powder comprises preparing an aqueous solution of a metal-containing oxidizing agent and a sulfur-containing organic fuel.

4. The method according to claim 3 wherein said metal-containing oxidizing agent is a metal nitrate.

5. The method according to claim 3 wherein said sulfur-containing organic fuel is a thioamide.

6. The method according to claim 3 wherein said sulfur-containing organic fuel is thioacetamide.

7. The method according to claim 1 wherein said solution is heated at a temperature comprised between 500° C. and 600° C. in a furnace.

8. The method according to claim 1 further comprising a step of performing a thermal post-treatment of said powder under a H 2 S/N 2 flow prior to said sintering step.

9. The method according to claim 1 wherein said step of sintering said powder is performed by a method chosen from: hot pressing, spark plasma sintering, hot isostatic pressing, microwave sintering, natural sintering.

10. The method according to claim 1 wherein said step of sintering said powder is performed in a graphite die, using buffer layers of boron nitride powder interposed between the die and the powder to be sintered.

Assignments (2)
MERGER Recorded Oct 19, 2023
From: UNIVERSITE DE RENNES I
To: UNIVERSITE DE RENNES
Reel/Frame 065490/0667 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 10, 2017
From: HAKMEH, NOHA; MERDRIGNAC-CONANEC, ODILE; ZHANG, XIANG-HUA
To: CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE; UNIVERSITE DE RENNES 1
Reel/Frame 041230/0178 →