Filters comprising oxygen-depleted SiC membranes

Patent metadata

Field	Value
Publication number	US-11033863-B2
Application number	US-201515536780-A
Country	US
Kind code	B2
Filing date	Dec 18, 2015
Priority date	Dec 18, 2014
Publication date	Jun 15, 2021
Grant date	Jun 15, 2021

Abstract

A filter for the filtration of a fluid, such as a liquid, includes or composed of a support element made of a porous ceramic material, the element having a tubular or parallelepipedal shape delimited by an external surface and including, in its internal portion, a set of adjacent channels with axes parallel to one another and separated from one another by walls of the porous inorganic material, wherein at least a portion of the channels and/or at least a portion of the external surface are covered with a porous separating membrane layer, wherein the layer is made of a material essentially composed of sintered grains of silicon carbide (SiC), and the weight content of elemental oxygen of the layer is less than 0.5%.

First claim

The invention claimed is:

1. A filter for the filtration of a fluid, comprising or composed of a support element made of a porous ceramic material, said support element having a tubular or parallelepipedal shape delimited by an external surface and comprising, in its internal portion, a set of adjacent channels with axes parallel to one another and separated from one another by walls of said porous ceramic material, wherein:
at least a portion of said channels are covered on their internal surface with a first porous separating membrane layer and/or at least a portion of said external surface is covered with a second porous separating membrane layer;

wherein:
said first and second porous separating membrane layers are made of a material essentially composed of recrystallized sintered grains of silicon carbide (SiC),
a weight content of elemental oxygen of the first and second porous separating membrane layers is less than 0.4%,
a porosity of the first and second porous separating membrane layers is between 30% and 70% and a median pore diameter of the first and second porous separating membrane layers is between 10 nanometers and 5 micrometers,
the recrystallized SiC represents more than 99% of the weight of the material constituting the first and second porous separating membrane layers,
an atomic concentration of oxygen measured by XPS at a surface of the SiC grains is less than 10%, on the basis of the total amount of the elements Si, C and O,
a carbon/oxygen ratio measured by XPS at a surface of the SiC grains is greater than 4.

2. The filter as claimed in claim 1 , wherein a median size of the SiC grains in said material is between 20 nanometers and 10 micrometers.

3. The filter as claimed in claim 1 , wherein the weight content of elemental oxygen of the material constituting each of the first and second porous separating membrane layers is less than or equal to 0.3%.

4. The filter as claimed in claim 3 , wherein the weight content of elemental oxygen of the material constituting each of the first and second porous separating membrane layers is less than or equal to 0.3%.

5. The filter as claimed in claim 1 , wherein the porous support element comprises or is composed of a material chosen from silicon carbide SiC, recrystallized SiC, silicon nitride, silicon oxynitride, silicon aluminum oxynitride or a combination of these.

6. The filter as claimed in claim 5 , wherein silicon carbide is liquid-phase or solid-phase sintered SiC, the silicon nitride is Si 3 N 4 , and silicon oxynitride is Si 2 ON 2 .

7. The filter as claimed in claim 1 , wherein an open porosity of the material constituting the porous support element is between 20% and 60%, a median pore diameter of the material constituting the porous support element being between 5 and 50 micrometers.

8. The filter as claimed in claim 1 , additionally comprising one or more primer layers arranged between the porous ceramic material constituting the porous support element and the material constituting each of the first and second porous separating membrane layers.

9. A process for manufacturing a separating membrane layer, in a tangential or frontal filter for the filtration of a fluid, the filter comprising or composed of a support element made of a porous ceramic material, said support element having a tubular or parallelepipedal shape delimited by an external surface and including a set of adjacent channels with axes parallel to one another and separated from one another by walls of said porous ceramic material, wherein at least a portion of said channels are covered on their internal surface with a first porous separating membrane layer and/or at least a portion of said external surface is covered with a second porous separating membrane layer,
wherein:
said first and second porous separating membrane layers are made of a material essentially composed of recrystallized sintered grains of silicon carbide (SiC), a weight content of elemental oxygen of the first and second porous separating membrane layers is less than 0.4%,
a porosity of the first and second porous separating membrane layers is between 30% and 70% and a median pore diameter of the first and second porous separating membrane layers is between 10 nanometers and 5 micrometers,
the recrystallized SiC represents more than 99% of the weight of the material constituting the first and second porous separating membrane layers,
an atomic concentration of oxygen measured by XPS at a surface of the SiC grains is less than 10%, on the basis of the total amount of the elements Si, C and O,
a carbon/oxygen ratio measured by XPS at a surface of the SiC grains is greater than 4,

the process comprising:
preparing a slip from a powder of silicon carbide particles having a mean size of between 20 nanometers and 10 micrometers,
applying said slip to the support element, under conditions that enable the formation of a thin layer of the slip on an internal part of the channels of said filter,
drying and then firing under an inert gas atmosphere at a temperature between 1400° C. and 2000° C. and for a time sufficient to obtain a porous separating membrane layer on their internal surface of said channels essentially composed of recrystallized sintered silicon carbide (SiC) grains,
performing a treatment for eliminating some of the residual elemental oxygen present at a surface of said grains such that a weight content of residual elemental oxygen of the porous separating membrane layers is less than 0.4%.

10. The process as claimed in claim 9 , wherein the treatment for eliminating some of the residual elemental oxygen present at the surface of said grains is performed by the action of hydrofluoric acid or by a heat treatment under a hydrogen-containing reducing atmosphere.

11. A method comprising utilizing a filter for the filtration of a fluid, the filter comprising or composed of a support element made of a porous ceramic material, said support element having a tubular or parallelepipedal shape delimited by an external surface and comprising, in its internal portion, a set of adjacent channels with axes parallel to one another and separated from one another by walls of said porous ceramic material, wherein at least a portion of said channels are covered on their internal surface with a first porous separating membrane layer and/or at least a portion of said external surface is covered with a second porous separating membrane layer; wherein:
said first and second porous separating membrane layers are made of a material essentially composed of recrystallized sintered grains of silicon carbide (SiC), a weight content of elemental oxygen of the first and second porous separating membrane layers is less than 0.4%.

12. The method as claimed in claim 11 , wherein the filter is utilized for filtering an aqueous liquid.

Assignees

• Saint Gobain Centre De Rechersches Et Detudes Europeen
• Centre Nat Rech Scient
• Univ Montpellier
• Enscm
• Saint Gobain Centre De Rech Et Detudes European

Inventors

• Urffer Daniel
• Guizard Christian

Classifications

• B01D67/00413

  by agglomeration of nanoparticles · CPC title

• B01D67/0093

  Chemical modification · CPC title

• B01D2323/081

  Heating · CPC title

• B01D67/00411

  by sintering · CPC title

• B01D71/0215 Primary

  Silicon carbide; Silicon nitride; Silicon oxycarbide · CPC title