Substrate for solidifying a silicon ingot

Patent metadata

Field	Value
Publication number	US-10023972-B2
Application number	US-201415022440-A
Country	US
Kind code	B2
Filing date	Sep 12, 2014
Priority date	Sep 16, 2013
Publication date	Jul 17, 2018
Grant date	Jul 17, 2018

Abstract

A substrate, in particular intended for contact with liquid silicon, wherein it is at least partially surface-coated with a multilayer coating formed by: at least one layer, known as the adhesion layer, contiguous with the substrate, having an open porosity of at least 30%, and formed of a material comprising silica and silicon nitride, said material having a silica content of between 10 wt.-% and 55 wt.-% in relation to the total weight thereof; and a layer different from the adhesion layer, known as the release layer, located on the surface of the adhesion layer and formed of a material including silica and silicon nitride, said material having a silica content of between 2 wt.-% and 10 wt.-% in relation to the total weight thereof.

First claim

The invention claimed is:

1. A substrate being at least partially surface-coated with a multilayer coating formed from at least:
one layer, termed tie layer, contiguous with said substrate, having an open porosity of at least 30%, and formed from a material based on silica and on silicon nitride, said material having a silica content of between 10% and 55% by weight relative to the total weight thereof, and
one layer distinct from the tie layer, termed release layer, located at the surface of the tie layer, and formed from a material based on silica and on silicon nitride, said material having a silica content of between 2% and 10% by weight relative to the total weight thereof.

2. The substrate as claimed in claim 1 , wherein the material forming the tie layer has a silica content of between 25% and 50% by weight, relative to the total weight thereof.

3. The substrate as claimed in claim 1 , wherein the material forming the release layer has a silica content of between 4% and 10% by weight, relative to the total weight thereof.

4. The substrate as claimed in claim 1 , wherein the tie layer represents at least 80% of the total thickness of said coating.

5. The substrate as claimed in claim 1 , wherein the tie layer has a thickness of between 100 and 500 micrometers, and the release layer has a thickness of between 10 and 100 micrometers.

6. The substrate as claimed in claim 1 , wherein said tie and release layers each have an open porosity.

7. The substrate as claimed in claim 1 , wherein said tie and release layers each have a specific surface area of between 5 m 2 /g and 15 m 2 /g.

8. The substrate as claimed in claim 1 , wherein the tie layer consists of one or more tie sublayer(s), having identical or different compositions.

9. The substrate as claimed in claim 1 , wherein said substrate is formed from a material chosen from silicon carbide, silicon nitride, silica, graphite and composites comprising graphite and silicon carbide or comprising graphite and silicon nitride.

10. The substrate as claimed in claim 1 , being a crucible for solidifying a silicon ingot from molten silicon.

11. A substrate according to claim 1 , being intended for contact with liquid silicon.

12. A process for forming a multilayer coating which has a tie layer and a release layer, on a surface of a substrate, comprising at least:
(a) the formation of a layer, termed tie layer, via:
i) bringing said surface of the substrate into contact with a liquid suspension of powder of silicon nitride and optionally of silica, so as to form thereon a deposit of said suspension,
ii) exposing the deposit formed in (a)i) to a heat treatment under an oxidizing atmosphere and under conditions sufficient to obtain a layer contiguous with said substrate having an open porosity of at least 30%, and formed from a material having a silica content of between 10% and 55% by weight relative to the total weight thereof, and

(b) the formation of a release layer, distinct from the tie layer, via:
i) bringing the surface of the substrate as obtained at the end of a step (a) into contact with a liquid suspension of powder of silicon nitride and optionally of silica, so as to form thereon a deposit of said suspension,
ii) exposing the deposit formed in (b)i) to a heat treatment under an oxidizing atmosphere and under conditions sufficient to obtain a layer located at the surface of the tie layer, and formed from a material having a silica content of between 2% and 10% by weight relative to the total weight thereof.

13. The process as claimed in claim 12 , wherein step (a) is repeated at least once before step (b) is carried out.

14. The process as claimed in claim 12 , wherein step (a)ii) is carried out at a temperature greater than 900° C.

15. The process as claimed in claim 12 , wherein step (b)ii) is carried out at a temperature of less than 900° C.

16. The process as claimed in claim 12 , wherein step (a)ii) is carried out for a period of between 1 and 4 hours and step (b)ii) is carried out for a period of between 1 and 4 hours.

17. The process as claimed in claim 12 , wherein the substrate is a crucible for solidifying a silicon ingot from molten silicon.

18. A process for renewing a layer, termed release layer, on the internal surface of a crucible, already coated with at least one permanent layer, termed tie layer, contiguous with said substrate having an open porosity of at least 30%, and formed from a material having a silica content of between 10% and 55% by weight relative to the total weight of said tie layer, comprising (i) bringing the external surface of the tie layer into contact with a liquid suspension of powder of silicon nitride and optionally of silica, so as to form thereon a deposit of said suspension, and (ii) exposing the deposit formed in i) to a heat treatment under an oxidizing atmosphere and under conditions sufficient to obtain a layer located at the surface of the tie layer formed from a material having a silica content of between 2% and 10% by weight relative to the total weight thereof.

19. A process for solidifying a silicon ingot from molten silicon comprising at least the step of using a substrate as claimed in claim 1 as a crucible.

Assignees

• Commissariat Energie Atomique
• Commissariat Energie Atomique

Inventors

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

Classifications

• C04B41/457

  Non-superficial impregnation or infiltration of the substrate · CPC title

• C04B41/4539

  as a emulsion, dispersion or suspension · CPC title

• C04B35/584

  based on silicon nitride · CPC title

• C01B33/021

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

• C04B41/4582

  Porous coatings, e.g. coating containing porous fillers · CPC title