# US 2014/0193289 A1 · One-dimensional titanium nanostructure and method for fabricating the same

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- Number: US 2014/0193289 A1
- Document ID: US20140193289A1
- Status: Published application
- Kind: A1
- Application number: 13/846,047
- Filed: 2013-03-18
- Published: 2014-07-10
- Earliest claimed: 2013-01-04
- Assignees: National Chiao Tung University
- Applicants: National Chiao Tung University
- Inventors: Tze-Lung CHEN; Hsin-Tien CHIU; Chi-Young LEE
- Web page: https://patentgrep.com/patent/US20140193289A1

## CPC

- C30B 29/02: Elements
- B22F 1/0547: {Nanofibres or nanotubes}
- B22F 9/30: with decomposition of metal compounds, e.g. by pyrolysis
- C23C 16/08: from metal halides
- C23C 16/46: characterised by the method used for heating the substrate (C23C16/48, C23C16/50 take precedence)
- C30B 25/005: {Growth of whiskers or needles}
- C30B 25/16: Controlling or regulating (controlling or regulating in general G05)
- C30B 29/60: characterised by shape
- C30B 29/602: {Nanotubes}
- B22F 2201/40: Metal compounds
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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)

## Abstract

A one-dimensional titanium nanostructure and a method for fabricating the same are provided. A titanium metal reacts with titanium tetrachloride to form the one-dimensional titanium nanostructure on a heat-resistant substrate in a CVD method and under a reaction condition of a reaction temperature of 300-900° C., a deposition temperature of 200-850° C., a flow rate of the carrier gas of 0.1-50 sccm and a reaction time of 5-60 hours. The titanium nanostructure includes titanium nanowires, titanium nanobelts, flower-shaped titanium nanowires, titanium nanorods, titanium nanotubes, and titanium-titanium dioxide core-shell structures. The titanium nanostructure can be densely and uniformly grown on the heat-resistant substrate. The present invention neither uses a template nor uses the complicated photolithographic process, solution preparation process, and mixing-coating process. Therefore, the process scale-up, cost down, and the simplified production process are achieved.

## Claims

### Claim 1

A method for fabricating a one-dimensional titanium nanostructure, comprising steps:
placing a heat-resistant substrate and a titanium metal in a CVD (Chemical Vapor Deposition) reaction chamber; and
using a carrier gas to transport titanium tetrachloride into said CVD reaction chamber, undertaking a reaction of said titanium metal and said titanium tetrachloride to generate titanium subchloride, and letting said titanium subchloride thermolyze to form a one-dimensional titanium nanostructure on said heat-resistant substrate, under a reaction condition of a reaction temperature of 300-900° C., a deposition temperature of 200-850° C., a flow rate of a carrier gas of 0.1-50 sccm and a reaction time of 5-60 hours.

### Claim 2 (depends on 1)

The method for fabricating a one-dimensional titanium nanostructure according to claim 1, wherein said heat-resistant substrate is made of graphite, and said carrier gas is nitrogen, and wherein said titanium metal reacts with said titanium tetrachloride at a reaction temperature of 500-900° C., and said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 500-850° C., and wherein said flow rate of said carrier gas is 0.1-10 sccm, and said reaction time is 8-30 hours, and wherein said one-dimensional titanium nanostructure is a titanium nanowire having a diameter of 20-50 nm and a length of 2-50 μm, and wherein said titanium nanowire is a monocrystalline titanium nanowire or a polycrystalline titanium nanowire.

### Claim 3 (depends on 2)

The method for fabricating a one-dimensional titanium nanostructure according to claim 2, wherein said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 800-850° C.

### Claim 4 (depends on 2)

The method for fabricating a one-dimensional titanium nanostructure according to claim 2, wherein said monocrystalline titanium nanowire has an FCC lattice structure.

### Claim 5 (depends on 1)

The method for fabricating a one-dimensional titanium nanostructure according to claim 1, wherein said heat-resistant substrate is made of graphite, and said carrier gas is nitrogen, and wherein said titanium metal reacts with said titanium tetrachloride at a reaction temperature of 500-900° C., and said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 475-825° C., and wherein said flow rate of said carrier gas is 0.1-10 sccm, and said reaction time is 5-30 hours, and wherein said one-dimensional titanium nanostructure is a titanium nanobelt having a diameter of 20-150 nm and a length of 1-50 μm, and wherein said titanium nanobelt is a monocrystalline titanium nanobelt or a polycrystalline titanium nanobelt.

### Claim 6 (depends on 5)

The method for fabricating a one-dimensional titanium nanostructure according to claim 5, wherein said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 775-825° C.

### Claim 7 (depends on 5)

The method for fabricating a one-dimensional titanium nanostructure according to claim 5, wherein said monocrystalline titanium nanobelt has an FCC lattice structure.

### Claim 8 (depends on 1)

The method for fabricating a one-dimensional titanium nanostructure according to claim 1, wherein said heat-resistant substrate is made of graphite, a surface of said heat-resistant substrate is roughened to at least have a roughness of 20 nm, and wherein said carrier gas is nitrogen, and wherein said titanium metal reacts with said titanium tetrachloride at a reaction temperature of 700-900° C., and said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 475-825° C., and wherein said flow rate of said carrier gas is 10-20 sccm, and said reaction time is 15-60 hours, whereafter supply of said titanium tetrachloride to said CVD reaction chamber is switched off, and heating is maintained for 3-10 hours, whereafter said CVD reaction chamber is cooled down to an ambient temperature, and said titanium tetrachloride remaining in said CVD reaction chamber is removed, whereafter said one-dimensional titanium nanostructure is taken out of said CVD reaction chamber, whereby said one-dimensional titanium nanostructure is a flower-shaped titanium nanowire having a diameter of 30-100 nm and a length of 2-9 μm, and said flower-shaped titanium nanowire is a monocrystalline flower-shaped titanium nanowire or a polycrystalline flower-shaped titanium nanowire.

### Claim 9 (depends on 8)

The method for fabricating a one-dimensional titanium nanostructure according to claim 8, wherein said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 600-800° C.

### Claim 10 (depends on 8)

The method for fabricating a one-dimensional titanium nanostructure according to claim 8, wherein monocrystalline flower-shaped titanium nanowire has an FCC lattice structure.

### Claim 11 (depends on 1)

The method for fabricating a one-dimensional titanium nanostructure according to claim 1, wherein said heat-resistant substrate is made of graphite, and said carrier gas is nitrogen, and wherein said titanium metal reacts with said titanium tetrachloride at a reaction temperature of 700-900° C., and said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 475-825° C., and wherein said flow rate of said carrier gas is 10-20 sccm, and said reaction time is 15-60 hours, whereafter supply of said titanium tetrachloride to said CVD reaction chamber is switched off, and heating is maintained for 3-10 hours, whereafter said CVD reaction chamber is cooled down to an ambient temperature, and said titanium tetrachloride remaining in said CVD reaction chamber is removed, whereafter said one-dimensional titanium nanostructure is taken out of said CVD reaction chamber, whereby said one-dimensional titanium nanostructure is a titanium nanorod having a diameter of 30-100 nm and a length of 2-9 μm, and said titanium nanorod is a monocrystalline titanium nanorod or a polycrystalline titanium nanorod.

### Claim 12 (depends on 11)

The method for fabricating a one-dimensional titanium nanostructure according to claim 11, wherein said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 600-800° C.

### Claim 13 (depends on 11)

The method for fabricating a one-dimensional titanium nanostructure according to claim 11, wherein monocrystalline titanium nanorod has an FCC lattice structure.

### Claim 14 (depends on 1)

The method for fabricating a one-dimensional titanium nanostructure according to claim 1, wherein said heat-resistant substrate is made of graphite, and said carrier gas is nitrogen, and wherein said titanium metal reacts with said titanium tetrachloride at a reaction temperature of 700-900° C., and said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 475-825° C., and wherein said flow rate of said carrier gas is 10-20 sccm, and said reaction time is 15-60 hours, whereafter supply of said titanium tetrachloride to said CVD reaction chamber is switched off, and said CVD reaction chamber is cooled down to an ambient temperature, whereafter said one-dimensional titanium nanostructure is taken out of said CVD reaction chamber, whereby said one-dimensional titanium nanostructure is a titanium-titanium dioxide core-shell structure having a titanium core and a titanium dioxide shell, and said titanium core has a diameter of 20-100 nm and a length of 2-10 μm, and said titanium dioxide shell has a thickness of 5-50 nm; said titanium core is a monocrystalline titanium core or a polycrystalline titanium core; said titanium dioxide shell is a monocrystalline titanium dioxide shell or a polycrystalline titanium dioxide shell.

### Claim 15 (depends on 14)

The method for fabricating a one-dimensional titanium nanostructure according to claim 14, wherein said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 600-800° C.

### Claim 16 (depends on 14)

The method for fabricating a one-dimensional titanium nanostructure according to claim 14, wherein said monocrystalline titanium core has an FCC lattice structure, and said titanium dioxide shell is Anatase titanium dioxide, Rutile titanium dioxide or Brookite titanium dioxide.

### Claim 17 (depends on 1)

The method for fabricating a one-dimensional titanium nanostructure according to claim 1, wherein said heat-resistant substrate is made of graphite, and said carrier gas is nitrogen, and wherein said titanium metal reacts with said titanium tetrachloride at a reaction temperature of 700-900° C., and said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 475-800° C., and wherein said flow rate of said carrier gas is 10-50 sccm, and said reaction time is 15-60 hours, whereafter supply of said titanium tetrachloride to said CVD reaction chamber is switched off, and heating is maintained for 3-10 hours, whereafter said CVD reaction chamber is cooled down to an ambient temperature, and said titanium tetrachloride remaining in said CVD reaction chamber is removed, whereafter said one-dimensional titanium nanostructure is taken out of said CVD reaction chamber, whereby said one-dimensional titanium nanostructure is a titanium nanotube having a diameter of 10-100 nm and a length of 0.1-9 μm, and said titanium nanotube is a monocrystalline titanium nanotube or a polycrystalline titanium nanotube.

### Claim 18 (depends on 17)

The method for fabricating a one-dimensional titanium nanostructure according to claim 17, wherein said one-dimensional titanium nanostructure deposits on said heat-resistant substrate at a deposition temperature of 600-800° C.

### Claim 19 (depends on 17)

The method for fabricating a one-dimensional titanium nanostructure according to claim 17, wherein monocrystalline titanium nanotube has an FCC lattice structure.

### Claim 20 (depends on 1)

A one-dimensional titanium nanostructure fabricated by the method according to claim 1.
