Substrate with low-permeability coating for the solidification of silicon

Patent metadata

Field	Value
Publication number	US-10287703-B2
Application number	US-201415022461-A
Country	US
Kind code	B2
Filing date	Sep 12, 2014
Priority date	Sep 16, 2013
Publication date	May 14, 2019
Grant date	May 14, 2019

Abstract

A substrate characterised in that it is at least partially surface-coated with a coating containing at least one so-called “barrier” layer having silica and one or more material(s) X selected from among SiC, Si, Si 3 N 4 , in which layer the amount of X varies between 25-wt. % and 50.-wt. % in relation to the total weight of the barrier layer, the barrier layer being formed by grains of one or more materials X covered at least partially in a silica shell, and the barrier layer being in direct contact with the substrate.

First claim

The invention claimed is:

1. A crucible wherein it is at least partially surface-coated with a coating containing at least one layer, termed “barrier” layer, comprising silica and one or more material(s) X chosen from SiC, Si and Si 3 N 4 , in which layer the weight amount of X ranges from 25% to 50% relative to the total weight of the barrier layer, said barrier layer being formed from grains of one or more materials X covered at least partially with a silica shell, the barrier layer being placed in direct contact with the crucible, the barrier layer having a thickness between 10 μm and 100 μm,
said crucible being made of a material selected from the group consisting of silicon carbide SiC, silicon nitride Si 3 N 4 , composites comprising graphite and silicon carbide or comprising graphite and silicon nitride, and siliconized graphite.

2. The crucible as claimed in claim 1 , wherein the barrier layer has an open porosity ranging from 0 to 5%.

3. The crucible as claimed in claim 1 , wherein the barrier layer has a permeability of less than 10 −15 m 2 .

4. The crucible as claimed in claim 1 , wherein the barrier layer is in the form of a silica matrix into which are incorporated grains of one or more material(s) X.

5. The crucible as claimed in claim 1 , wherein the barrier layer comprises between 50% and 75% of silica by weight relative to the total weight thereof.

6. The crucible as claimed in claim 1 , wherein the specific surface area of the barrier layer is between 5 cm 2 /g and 5 m 2 /g.

7. The crucible as claimed in claim 1 , wherein the coating also comprises, at the surface of the barrier layer, a release layer.

8. The crucible as claimed in claim 1 , wherein it is a crucible for solidifying silicon.

9. A process for preparing a crucible as claimed in claim 1 , said crucible being at least partially surface-coated with a coating forming a gas barrier, wherein said process comprises at least the steps:
a) providing a fluid medium comprising at least one or more material(s) X chosen from SiC, Si and Si 3 N 4 ;
b) applying said fluid medium to the surface of the crucible in a sufficient amount to form a deposit thereon,
c) treating said deposit under an oxidizing atmosphere, at a temperature of between 1000° C. and 1300° C. and under conditions sufficient to form a “barrier” layer comprising silica and one or more material(s) X chosen from SiC, Si and Si 3 N 4 , in which layer the weight amount of X ranges from 25% to 50% relative to the total weight of the barrier layer, said barrier layer being formed from grains of one or more materials X covered at least partially with a silica shell, the barrier layer being placed in direct contact with the crucible, the barrier layer having a thickness between 10 μm and 100 μm,
said crucible being made up of a material chosen from silicon carbide SiC; silicon nitride Si3N4; composites comprising graphite and silicon carbide or comprising graphite and silicon nitride; and siliconized graphite.

10. The process as claimed in claim 9 , wherein the fluid medium also comprises silica.

11. The process as claimed in claim 9 , wherein it comprises, between step b) of forming a deposit and step c) of treating under an oxidizing atmosphere, at least one step of drying at a temperature of less than 50° C.

12. The process as claimed in claim 9 wherein the step of treating under an oxidizing atmosphere is carried out at a temperature ranging from 1100° C. to 1300° C.

13. The process as claimed in claim 9 , wherein step c) of treating under an oxidizing atmosphere is carried out for a period ranging from 1 hour to 5 hours.

14. The process as claimed in claim 9 , comprising, after the treatment under an oxidizing atmosphere, a step of treating in the presence of a neutral gas at a temperature of between 1400° C. and 1500° C.

15. The process as claimed in claim 9 , wherein step b) is repeated several times before step c) is carried out.

16. The process as claimed in claim 9 , wherein the fluid medium used in step a) comprises one or more material(s) X in an amount ranging from 15% to 35% by weight relative to the total weight of said fluid.

Assignees

• Commissariat Energie Atomique

Inventors

• Garandet Jean-Paul
• Camel Denis
• Drevet Béatrice
• Eustathopoulos Nicolas
• Huguet Charles
• Testard Johann
• Voytovych Rayisa

Classifications

• C04B41/009

  characterised by the material treated · CPC title

• C01B33/021

  Preparation (chemical coating from the vapour phase C23C16/00) · CPC title

• C04B41/89

  for obtaining at least two superposed coatings having different compositions · CPC title

• C04B41/52

  Multiple coating or impregnating {multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation} · CPC title

• C09D1/00

  Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances · CPC title