EP0550071A1
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EP
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Method for manufacturing inorganic membranes by organometallic chemical vapor deposition
Assignee: Air Products and Chemicals Inc
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Filing: 1992-12-30
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Granted: —
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Expires: 2012-12-30
Abstract
Abstract The present invention is a method for manufacturing inorganic membranes which are capable of separating oxygen from air. The membranes comprise a thin layer of a multicomponent metallic oxide which has been deposited onto a porous substrate by organometallic chemical vapor deposition. The inorganic membranes are formed by reacting organometallic complexes corresponding to each of the respective metals making up the multicomponent metallic oxide and an oxidizing agent under conditions sufficient to deposit a thin layer of the multicomponent metallic oxide onto the porous substrate.
Inventors
- 👤 Robin Edward Richards
- 👤 Robert Louis Iampietro
- 👤 Paul Nigel Dyer
Bibliographic Details
Application Number
—
Jurisdiction
EP
Data Source
google_patents
Last Synchronized
2026-10-31 12:02
CPC Classifications
B; B01; B01D; B01D67/00; B01D67/0039; B01D67/0072; B01D67/0044; B01D71/00; B01D71/02; B01D71/022; B01D71/0223; B01D71/02232; B01D71/024; C; C04; C04B; C04B41/00; C04B41/45; C04B41/52; C23; C23C; C23C16/00; C23C16/04; C23C16/045; C23C16/44; C23C16/46; B01D2323/00; B01D2323/08; B01D2323/081; B01D2323/12; B01D2325/00; B01D2325/02; B01D2325/0283; Y; Y10; Y10T; Y10T428/00; Y10T428/12; Y10T428/12014; Y10T428/12028; Y10T428/12042; Y10T428/12479; Y10T428/249921; Y10T428/249953; Y10T428/249955; Y10T428/249956; Y10T428/249957; Y10T428/249967; Y10T428/24997; Y10T428/249981; Y10T428/249994; Y10T428/249999
Claims Analysis
Total Claims: 29
Claim 1
Independent Claim
118 words
A method for manufacturing an inorganic membrane comprising a layer of a multicomponent metallic oxide which has been deposited onto a porous substrate, the method comprising: (a) individually heating organometallic complexes capable of forming a multicomponent metallic oxide comprising at least two different metals to a temperature sufficient to vaporize the organometallic complexes; (b) introducing the vaporous organometallic complexes and an oxidizing agent into a reactor containing a porous substrate to form a mixture of the vaporous organometallic complexes and the oxidizing agent; and (c) depositing a layer of the multicomponent metallic oxide onto the porous substrate by reacting the mixture of organometallic complexes and oxidizing agent at a temperature and pressure sufficient to form the inorganic membrane.
Claim 2
Independent Claim
118 words
A method for manufacturing an inorganic membrane comprising a layer of a multicomponent metallic oxide which has been deposited onto a porous substrate, the method comprising: (a) individually heating organometallic complexes capable of forming a multicomponent metallic oxide comprising at least two different metals to a temperature sufficient to vaporize the organometallic complexes; (b) introducing the vaporous organometallic complexes and an oxidizing agent into a reactor containing a porous substrate to form a mixture of the vaporous organometallic complexes and the oxidizing agent; and (c) depositing a layer of the multicomponent metallic oxide onto the porous substrate by reacting the mixture of organometallic complexes and oxidizing agent at a temperature and pressure sufficient to form the inorganic membrane.
Claim 3
Dependent Claim
36 words
The method according to Claim 1 wherein the reaction according to step (c) occurs at a temperature ranging from 400 ° C to 800 ° C and a pressure ranging from 1 to about 760 torr.
Claim 4
Dependent Claim
39 words
The method according to Claim 2 which further comprises: (d) heat treating the layer of multicomponent metallic oxide at a temperature ranging from 650 °C to 1100 ° C for a period ranging from 10 minutes to five hours.
Claim 5
Dependent Claim
38 words
The method according to Claim 2 wherein the porous substrate is selected from the group consisting of alumina, silica, magnesia, titania, a high temperature oxygen compatible metal alloy, a metal oxide stabilized zirconia, and compounds and mixtures thereof.
Claim 6
Dependent Claim
15 words
The method according to Claim 2 wherein the porous substrate comprises a multicomponent metallic oxide.
Claim 7
Dependent Claim
30 words
The method according to Claim 5 wherein the oxidizing agent is selected from the group consisting of oxygen, air, ozone, N 2 0 and a mixture of water and oxygen.
Claim 8
Independent Claim
137 words
A method for manufacturing an inorganic membrane comprising a layer of a multicomponent metallic oxide containing a Group 2 metal which is deposited onto a porous substrate, the method comprising: (a) individually heating organometallic complexes capable of depositing a multicomponent metallic oxide comprising at least two different metals wherein one of the metals comprises a Group 2 metal, to a temperature sufficient to vaporize the organometallic complexes; (b) introducing the vaporous organometallic complexes and an oxidizing agent into a reactor containing a porous substrate to form a mixture of the vaporous organometallic complexes and the oxidizing agent; and (c) depositing a layer of the multicomponent metallic oxide containing the Group 2 metal onto the porous substrate by reacting the mixture of organometallic complexes and oxidizing agent at a temperature and pressure sufficient to form the inorganic membrane.
Claim 9
Independent Claim
137 words
A method for manufacturing an inorganic membrane comprising a layer of a multicomponent metallic oxide containing a Group 2 metal which is deposited onto a porous substrate, the method comprising: (a) individually heating organometallic complexes capable of depositing a multicomponent metallic oxide comprising at least two different metals wherein one of the metals comprises a Group 2 metal, to a temperature sufficient to vaporize the organometallic complexes; (b) introducing the vaporous organometallic complexes and an oxidizing agent into a reactor containing a porous substrate to form a mixture of the vaporous organometallic complexes and the oxidizing agent; and (c) depositing a layer of the multicomponent metallic oxide containing the Group 2 metal onto the porous substrate by reacting the mixture of organometallic complexes and oxidizing agent at a temperature and pressure sufficient to form the inorganic membrane.
Claim 10
Dependent Claim
36 words
The method according to Claim 7 wherein the reacting according to step (c) occurs at a temperature ranging from 400 ° C to 800 ° C and a pressure ranging from 1 to about 760 torr.
Claim 11
Dependent Claim
43 words
The method according to Claim 8 which further comprises: (d) heat treating the layer of multicomponent metallic oxide containing the Group 2 metal at a temperature ranging from 650 ° C to 1100°C for a period ranging from 10 minutes to five hours.
Claim 12
Dependent Claim
38 words
The method according to Claim 8 wherein the porous substrate is selected from the group consisting of alumina, silica, magnesia, titania, a high temperature oxygen compatible metal alloy, a metal oxide stabilized zirconia and compounds and mixtures thereof.
Claim 13
Dependent Claim
15 words
The method according to Claim 8 wherein the porous substrate comprises a multicomponent metallic oxide.
Claim 14
Dependent Claim
30 words
The method according to Claim 11 wherein the oxidizing agent is selected from the group consisting of oxygen, air, ozone, N 2 0 and a mixture of water and oxygen.
Claim 15
Dependent Claim
28 words
The method according to Claim 12 wherein the multicomponent metallic oxide layer contains a Group 2 metal selected from the group consisting of calcium, strontium, barium and magnesium.
Claim 16
Independent Claim
163 words
A method for manufacturing an inorganic membrane comprising a layer of a mixed conducting oxide represented by the formula La x A 1-x Co y Fe 1-y O 3-z wherein x is between 0 and 1, y is between 0 and 1, z is a number which renders the oxide charge neutral and A is selected from barium or strontium which has been deposited onto a porous substrate, the method comprising: (a) individually heating organometallic complexes comprising lanthanum, cobalt, iron and A to a temperature sufficient to vaporize the organometallic complexes; (b) introducing the vaporous organometallic complexes into a reactor containing a porous substrate and mixing the vaporous organometallic complexes with an oxidizing agent; and (c) depositing a layer of the multicomponent metallic oxide represented by the formula La x A 1-x Co y Fe 1-y O 3-z onto the porous substrate by reacting the mixture of organometallic complexes and oxidizing agent at a temperature and pressure sufficient to form the inorganic membrane.
Claim 17
Independent Claim
163 words
A method for manufacturing an inorganic membrane comprising a layer of a mixed conducting oxide represented by the formula La x A 1-x Co y Fe 1-y O 3-z wherein x is between 0 and 1, y is between 0 and 1, z is a number which renders the oxide charge neutral and A is selected from barium or strontium which has been deposited onto a porous substrate, the method comprising: (a) individually heating organometallic complexes comprising lanthanum, cobalt, iron and A to a temperature sufficient to vaporize the organometallic complexes; (b) introducing the vaporous organometallic complexes into a reactor containing a porous substrate and mixing the vaporous organometallic complexes with an oxidizing agent; and (c) depositing a layer of the multicomponent metallic oxide represented by the formula La x A 1-x Co y Fe 1-y O 3-z onto the porous substrate by reacting the mixture of organometallic complexes and oxidizing agent at a temperature and pressure sufficient to form the inorganic membrane.
Claim 18
Dependent Claim
36 words
The method according to Claim 14 wherein the reacting according to step (c) occurs at a temperature ranging from 450 ° C to 600 ° C and a pressure ranging from 2 to about 10 torr.
Claim 19
Dependent Claim
39 words
The method according to Claim 15 which further comprises: (d) heat treating the layer of multicomponent metallic oxide at a temperature ranging from 650 °C to 1100 ° C for a period ranging from 10 minutes to five hours.
Claim 20
Dependent Claim
22 words
The method according to Claim 15 wherein the organometallic complexes are introduced into the reactor by means of an inert carrier gas.
Claim 21
Dependent Claim
38 words
The method according to Claim 17 wherein the porous substrate is selected from the group consisting of alumina, silica, magnesia, titania, a high temperature oxygen compatible metal alloy, a metal oxide stabilized zirconia and compounds and mixtures thereof.
Claim 22
Dependent Claim
15 words
The method according to Claim 17 wherein the porous substrate is a multicomponent metallic oxide.
Claim 23
Dependent Claim
26 words
The method according to Claim 19 wherein the organometallic complexes comprise Fe(thd) 3 , La(thd) 3 , Co(thd) 2 , (Ba)4 (thd)8 and Sr(thd) 2 .
Claim 24
Dependent Claim
30 words
The method according to Claim 20 wherein the oxidizing agent is selected from the group consisting of oxygen, air, ozone, N 2 0 and a mixture of water and oxygen.
Claim 25
Dependent Claim
38 words
An inorganic membrane formed by the method according to Claim 1 wherein the membrane comprises a multicomponent oxide layer having a thickness ranging from 0.1 µm to about 50 µm which has been deposited onto a porous substrate.
Claim 26
Dependent Claim
43 words
The inorganic membrane formed by the method according to Claim 7 wherein the membrane comprises a multicomponent oxide layer containing a Group 2 metal which has been deposited onto a porous substrate in a thickness ranging from 0.1 µm to about 50 µm.
Claim 27
Dependent Claim
84 words
The inorganic membrane formed by the method according to Claim 14 wherein the membrane comprises a mixed conducting oxide layer represented by the formula La x A 1-x Co y Fe 1-y O 3-z wherein x is between 0 and 1, y is between 0 and 1, z is a number which renders the oxide charge neutral and A is selected from barium or strontium which has been deposited onto a porous substrate in a thickness ranging from 0.1 µm to about 50 µm.
Claim 28
Dependent Claim
11 words
The inorganic membrane according to Claim 24 wherein A is strontium.
Claim 29
Dependent Claim
11 words
The inorganic membrane according to Claim 25 wherein A is barium.
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