# US 5,700,519 A · Method for producing ultra high purity titanium films

> Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt

- Number: US 5,700,519 A
- Document ID: US5700519A
- Status: Granted
- Kind: A
- Application number: 08/369,389
- Filed: 1995-01-06
- Granted: 1997-12-23
- Earliest claimed: 1995-01-06
- Assignees: Sony Corporation; Materials Research Corporation
- Inventors: Raymond K. F. Lam
- Web page: https://patentgrep.com/patent/US5700519A

## CPC

- C22B 34/1263: {obtaining metallic titanium from titanium compounds, e.g. by reduction (C22B34/129 takes precedence)}
- C01G 23/02: Halides of titanium
- C22B 34/1222: {using a halogen containing agent}
- C22B 34/1277: {using other metals, e.g. Al, Si, Mn}
- Y02P 10/20: Recycling
- C22B: PRODUCTION AND REFINING OF METALS (electrolytic C25); PRETREATMENT OF RAW MATERIALS
- 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)
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A method is provided for depositing ultra high purity of greater than 99.998% titanium films which comprises generating gaseous TiI.sub.4 in situ by reacting titanium metal starting material with gaseous iodide in a reaction chamber, purifying the TiI.sub.4 by a double distillation process at reduced pressure to produce ultra high purity of greater than 99.998% TiI.sub.4, transferring the ultra high purity TiI.sub.4 in liquid form to a deposition chamber to vaporize the liquid TiI.sub.4 and contacting a heated titanium substrate with the TiI.sub.4 vapor, thereby depositing the ultra high purity Ti films on the substrate.

## Claims

### Claim 1

A method of making ultra high purity titanium metal, comprising the steps of:
generating gaseous TiI.sub.4 in situ by reacting titanium metal starting material with gaseous iodine in a reaction chamber under vacuum conditions, said reaction occurring at a steady state temperature in the range of about 500.degree.-750.degree. C.;
transferring the gaseous reaction product TiI.sub.4 to a first distillation column;
distilling said TiI.sub.4 in said first distillation column to remove lower volatility impurities, said first distillation column operated at a temperature in the range of about 150.degree.-370.degree. C. and at a pressure in the range of about 0.05-670 torr to produce partially pure TiI.sub.4 ;
transferring the partially pure TiI.sub.4 to a second distillation column;
distilling said partially pure TiI.sub.4 in said second distillation column to remove higher volatility impurities, said second distillation column operated at a temperature in the range of about 150.degree.-370.degree. C. and at a pressure in the range of about 0.05-670 torr to produce ultra high purity of greater than 99.998% TiI.sub.4 ;
transferring the ultra high purity TiI.sub.4 in liquid form to a deposition chamber heated to a temperature of about 200.degree. C. to vaporize the liquid TiI.sub.4 ; and
contacting a titanium deposition substrate located within the deposition chamber and heated to a temperature in the range of about 1100.degree.-1400.degree. C. with the ultra high purity TiI.sub.4 vapor, whereby said TiI.sub.4 decomposes and ultra high purity of greater than 99.998% titanium metal is deposited on said substrate.

### Claim 2 (depends on 1)

The method according to claim 1 wherein said generating step is performed under vacuum conditions at a pressure in the range of about 0.05-670 torr.

### Claim 3 (depends on 2)

The method according to claim 2 wherein said generating step is performed at a pressure in the range of about 0.05-0.1 torr.

### Claim 4 (depends on 1)

The method according to claim 1 wherein said first distillation column is operated at a pressure in the range of about 2.5-4 torr.

### Claim 5 (depends on 1)

The method according to claim 1 wherein said second distillation column is operated at a pressure in the range of about 2.5-4 torr.

### Claim 6 (depends on 1)

The method according to claim 1 wherein said titanium metal starting material has a purity on the order of about 99.9%.

### Claim 7 (depends on 6)

The method according to claim 6 wherein said titanium metal starting material is in the form of a sponge.

### Claim 8 (depends on 1)

The method according to claim 1 wherein said titanium substrate is a high purity titanium filament.

### Claim 9 (depends on 1)

The method according to claim 1 wherein said titanium substrate is a high purity titanium rod.

### Claim 10 (depends on 1)

The method according to claim 1 wherein said titanium substrate is a high purity titanium tube.

### Claim 11 (depends on 1)

The method according to claim 1, further comprising: subjecting the ultra high purity deposited titanium metal to electron beam melting to further purify the titanium metal.