# US 2025/0158085 A1 · Ti MATERIAL FOR FUEL CELL SEPARATOR AND METHOD OF MANUFACTURING THE SAME

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- Number: US 2025/0158085 A1
- Document ID: US20250158085A1
- Status: Published application
- Kind: A1
- Application number: 18/610,721
- Filed: 2024-03-20
- Published: 2025-05-15
- Earliest claimed: 2023-11-13
- Assignees: Hyundai Motor Company; Kia Corporation
- Applicants: Hyundai Motor Company; Kia Corporation
- Inventors: Dong-Jae Choi; Jae-Woong Choi
- Web page: https://patentgrep.com/patent/US20250158085A1

## CPC

- H01M 8/0215: Glass; Ceramic materials
- C01G 23/047: Titanium dioxide
- C22F 1/183: {of titanium or alloys based thereon}
- C23C 14/0605: {Carbon}
- C23C 14/16: on metallic substrates or on substrates of boron or silicon
- C23C 14/165: {by cathodic sputtering}
- C23C 14/345: {using substrate bias}
- C23C 14/48: Ion implantation
- C23C 14/5806: {Thermal treatment}
- C23C 14/5853: {Oxidation}
- H01M 8/0206: Metals or alloys
- H01M 8/0228: in the form of layered or coated products
- C01P 2002/82: by IR- or Raman-data
- C01P 2002/85: by XPS, EDX or EDAX data
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2006/40: Electric properties
- Y02E 60/50: Fuel cells
- Y02P 70/50: Manufacturing or production processes characterised by the final manufactured product
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- C22F: CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS (surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by this subclass, C23F17/00)
- C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A method of manufacturing a Ti material for a fuel cell separator includes rolling a Ti raw material of a pure Ti material or a Ti alloy material, deposition coating Ti ion particles on the Ti raw material by physical vapor deposition (PVD), and oxidation heat treating to form a conductive oxide layer of a TiO2-x(0<x<1) structure around the Ti ion particles deposited by the deposition coating. According to the present disclosure, the Ti material can be used to achieve both corrosion resistance and conductivity.

## Claims

### Claim 1

A method of manufacturing a Ti material for a fuel cell separator, the method comprising:
rolling a Ti raw material of a pure Ti material or a Ti alloy material;
deposition coating Ti ion particles on the Ti raw material by physical vapor deposition (PVD); and
oxidation heat treating to form a conductive oxide layer of a TiO2-x(0<x<1) structure around the Ti ion particles deposited by the deposition coating.

### Claim 2 (depends on 1)

The method of claim 1, wherein Ar+ ions from the deposition coating etch a portion of a surface oxide layer of the Ti raw material and are ion bombarded on a surface of the Ti raw material.

### Claim 3 (depends on 2)

The method of claim 2, wherein, by the deposition coating, a Ti ion deposited layer is formed on the surface oxide layer, on the etched surface of the Ti raw material and inside underneath the surface oxide layer of the Ti raw material, and an atomic intermix region is formed in which the Ti of the raw material and the deposited Ti ion particles are mixed.

### Claim 4 (depends on 3)

The method of claim 3, wherein the oxidation heat treating is carried out in an atmospheric state, and
wherein Ti elements of the surface oxide layer and the Ti ion particles are reacted with oxygen by the oxidation heat treating to form an atmospheric heat treated oxide layer.

### Claim 5 (depends on 3)

The method of claim 3, wherein in the oxidation heat treating, the conductive oxide layer of the structure TiO2-x(0<x<1) is formed through diffusion rearrangement between Ti particles overdeposited within the Ti ion deposited layer, defects, and O particles introduced from the atmosphere or present within the surface oxide layer.

### Claim 6 (depends on 3)

The method of claim 3, further comprising:
coating C particles on the surface oxide layer and the Ti ion deposited layer after the deposition coating,
wherein the C particles are diffused inside the surface oxide layer and the Ti ion deposited layer by the oxidation heat treating.

### Claim 7 (depends on 3)

The method of claim 3, wherein an acceleration voltage of the deposition coating is 80 to 800 eV.

### Claim 8 (depends on 7)

The method of claim 7, wherein an area fraction (covering %) on the surface of the Ti raw material of the Ti ion deposited layer is 50 to 90%.

### Claim 9 (depends on 3)

The method of claim 3, wherein a thickness of the conductive oxide layer is 50 to 500 nm.

### Claim 10 (depends on 3)

The method of claim 3, wherein a heat treatment temperature of the oxidation heat treating is 580 to 750° C., and a holding time is 1 to 10 minutes.

### Claim 11

A Ti material for a fuel cell separator, the Ti material comprising:
a Ti raw material made of a pure Ti material or a Ti alloy material;
a surface oxide layer formed on the Ti raw material;
a Ti ion deposited layer in which Ti ion particles are deposited and coated by physical vapor deposition (PVD) on the Ti raw material and on the surface oxide layer; and
a conductive oxide layer formed in a TiO2-x(0<x<1) structure around the deposited Ti ion particles.

### Claim 12 (depends on 11)

The Ti material of claim 11, wherein the Ti ion deposited layer is formed on the Ti raw material in which a portion of the surface oxide layer is etched and exposed by Ar+ ions by the PVD.

### Claim 13 (depends on 12)

The Ti material of claim 12, wherein the Ti ion deposited layer is formed on the surface oxide layer, on the etched surface of the Ti raw material and inside underneath the surface oxide layer of the Ti raw material, and an atomic intermix region is formed in which the Ti of the raw material and the deposited Ti ion particles are mixed.

### Claim 14 (depends on 13)

The Ti material of claim 13, further comprising:
an atmospheric heat treated oxide layer formed on the surface oxide layer and on a surface of the etched Ti raw material by reacting Ti elements of the surface oxide layer and the Ti ion particles with oxygen by the oxidation heat treating.

### Claim 15 (depends on 13)

The Ti material of claim 13, wherein, by an oxidation heat treatment, the conductive oxide layer of the structure TiO2-x(0<x<1) is formed through diffusion rearrangement between Ti particles overdeposited within the Ti ion deposited layer, defects, and O particles introduced from the atmosphere or present within the surface oxide layer.

### Claim 16 (depends on 13)

The Ti material of claim 13, further comprising:
C particles coated on the surface oxide layer and on the Ti ion deposited layer and then diffused inside the surface oxide layer and the Ti ion deposited layer by an oxidation heat treatment.

### Claim 17 (depends on 13)

The Ti material of claim 13, wherein the Ti raw material is Ar heat treated or vacuum heat treated.

### Claim 18 (depends on 13)

The Ti material of claim 13, wherein an area fraction (covering %) on the surface of the Ti raw material of the Ti ion deposited layer is 50 to 90%.

### Claim 19 (depends on 13)

The Ti material of claim 13, wherein a thickness of the conductive oxide layer is 50 to 500 nm.
