Die and piston of an SPS apparatus, SPS apparatus comprising same, and method of sintering, densification or assembly in an oxidising atmosphere using said apparatus

Patent metadata

Field	Value
Publication number	US-11642724-B2
Application number	US-201615772219-A
Country	US
Kind code	B2
Filing date	Nov 3, 2016
Priority date	Nov 4, 2015
Publication date	May 9, 2023
Grant date	May 9, 2023

Abstract

A die or piston of a spark plasma sintering apparatus, wherein the die or piston is made from graphite and the outer surfaces of the die or piston are coated with a silicon carbide layer with a thickness of 1 to 10 micrometres, the silicon carbide layer being further optionally coated with one or more other layer(s) made from a carbide other than silicon carbide chosen from hafnium carbide, tantalum carbide and titanium carbide, the other layer(s) each having a thickness of 1 to 10 micrometres. A spark plasma sintering (SPS) apparatus comprising the die and two of the pistons, defining a sintering, densification or assembly chamber capable of receiving a powder to be sintered, a part to be densified, or parts to be assembled. A method of sintering a powder, densifying a part, or assembling two parts by means of a method of spark plasma sintering (SPS) in an oxidising atmosphere, using the spark plasma sintering (SPS) apparatus.

First claim

The invention claimed is:

1. A conventional spark plasma sintering apparatus comprising a conventional die and two conventional pistons, defining a sintering, densification or assembly chamber capable of receiving a powder to be sintered, a part to be densified, or parts to be assembled, wherein said conventional die has been replaced with a coated die, wherein said coated die is made of graphite and the outer surface of said coated die is coated with a homogenous layer made of silicon carbide having a thickness of 1 to 10 μm, said layer made of silicon carbide being further optionally coated with one or more other layer(s) made of a carbide other than silicon carbide, chosen from hafnium carbide, tantalum carbide and titanium carbide, said other layer(s) each having a thickness of 1 to 10 μm, and wherein said die is configured to conduct a pulsed current from 200 to 6000 A and/or a voltage of 1 to 8 volts and wherein said die is further configured to resist degradation at temperatures of between 700° C. and 1450° C.

2. A conventional spark plasma sintering apparatus comprising a conventional die and two conventional pistons, defining a sintering, densification or assembly chamber capable of receiving a powder to be sintered, a part to be densified, or parts to be assembled, wherein both of said conventional pistons have been replaced with coated pistons, wherein each of said coated pistons is made of graphite and the outer surfaces of each of said coated pistons are coated with a homogenous layer made of silicon carbide having a thickness of 1 to 10 μm, said layer made of silicon carbide being further optionally coated with one or more other layer(s) made of a carbide other than silicon carbide, chosen from hafnium carbide, tantalum carbide and titanium carbide, said other layer(s) each having a thickness of 1 to 10 μm, and wherein each of said coated pistons are configured to conduct a pulsed current from 200 to 6000 A and/or a voltage of 1 to 8 volts and wherein said coated pistons are further configured to resist degradation at temperatures of between 700° C. and 1450° C.

3. The spark plasma sintering apparatus according to claim 1 , wherein the outer surfaces of said coated die are coated with a layer made of silicon carbide by a “CVD” chemical vapour deposition method, and said layer made of silicon carbide is further optionally coated with one or more other layer(s) made of a carbide other than silicon carbide, chosen from hafnium carbide, tantalum carbide and titanium carbide, by a “CVD” chemical vapour deposition method.

4. The spark plasma sintering apparatus according to claim 2 , in which the outer surfaces of each of said coated pistons are coated with a layer made of silicon carbide by a “CVD” chemical vapour deposition method, and said layer made of silicon carbide is further optionally coated with one or more other layer(s) made of a carbide other than silicon carbide, chosen from hafnium carbide, tantalum carbide and titanium carbide, by a “CVD” chemical vapour deposition method.

5. The spark plasma sintering apparatus according to claim 1 further comprising replacement of said conventional pistons with coated pistons, wherein each of said coated pistons is made of graphite and the outer surfaces of each of said coated pistons are coated with a layer made of silicon carbide having a thickness of 1 to 10 μm, said layer made of silicon carbide being further optionally coated with one or more other layer(s) made of a carbide other than silicon carbide, chosen from hafnium carbide, tantalum carbide and titanium carbide, said other layer(s) each having a thickness of 1 to 10 μm.

6. The spark plasma sintering apparatus according to claim 1 , further comprising a flexible graphite sheet placed within said sintering, densification or assembly chamber such that, when said powder is received therein, the flexible graphite sheet is between said powder and inner walls of said sintering, densification or assembly chamber, wherein said flexible graphite sheet is coated with a layer of boron nitride on a face thereof.

7. The spark plasma sintering apparatus according to claim 5 , wherein the two coated pistons comprise an upper piston and a lower piston, further comprising an upper electrode, a lower electrode, and a vacuum chamber, said vacuum chamber enclosing said die, said upper piston, and said lower piston, said upper electrode electrically conducted to said upper piston via upper spacers, plates or discs, said lower electrode electrically conducted to said lower piston via lower spacers, plates or discs.

8. The spark plasma sintering apparatus according to claim 7 , further comprising a flexible graphite sheet placed within said sintering, densification or assembly chamber such that, when said powder is received therein, the flexible graphite sheet is between said powder and inner walls of said sintering, densification or assembly chamber, wherein said flexible graphite sheet is coated with a layer of boron nitride on a face thereof.

Assignees

• Commissariat Energie Atomique
• Centre Nat Rech Scient

Inventors

• Allemand Alexandre
• Largeteau Alain
• U-Chan Chung Seu
• Le Petitcorps Yann
• Roger Jérôme

Classifications

• C23C16/325

  Silicon carbide · CPC title

• C04B2235/6583

  Oxygen containing atmosphere, e.g. with changing oxygen pressures · CPC title

• C04B35/457

  based on tin oxides or stannates · CPC title

• C04B2235/666

  Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS] · CPC title

• C04B35/016

  based on manganites · CPC title