GB2085032A - Isostatic Pressing of Chromium Sputtering Targets - Google Patents

Isostatic Pressing of Chromium Sputtering Targets Download PDF

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Publication number
GB2085032A
GB2085032A GB8129663A GB8129663A GB2085032A GB 2085032 A GB2085032 A GB 2085032A GB 8129663 A GB8129663 A GB 8129663A GB 8129663 A GB8129663 A GB 8129663A GB 2085032 A GB2085032 A GB 2085032A
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United Kingdom
Prior art keywords
chromium
sleeve
pressure
alloy
gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
GB8129663A
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WC Heraus GmbH and Co KG
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WC Heraus GmbH and Co KG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by WC Heraus GmbH and Co KG filed Critical WC Heraus GmbH and Co KG
Publication of GB2085032A publication Critical patent/GB2085032A/en
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F3/15—Hot isostatic pressing
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Powder Metallurgy (AREA)
  • Heat Treatment Of Nonferrous Metals Or Alloys (AREA)

Abstract

Crack-free and pore-free targets for cathodic sputtering are produced from chromium or chromium base alloys in the form of powders, pressed articles or cast members by introducing the chromium material into a metal sleeve, evacuating and sealing the latter, and subjecting the encapsulated material to pressurised gas at 600-1500 DEG C and 700- 3100 bar. The metal sleeve is subsequently removed by mechanical or chemical action.

Description

SPECIFICATION Method for the Production of Targets of Chromium or Chromium Alloy This invention relates to a method for the production of moulded bodies of chromium or a chromium base alloy which are suitable for use as targets for cathodic sputtering.
It is known ta use targets of chromium which have been electrolytically deposited onto a support for the application of thin chromium layers by cathodic sputtering. This "electrolytic chromium" has, however, a relatively high content of gases, notably of oxygen.
Moulded bodies of chromium and chromium alloys, for example Cr80Fe20 and Cr90Al 10, which are suitable for use as targets are produced by smelting or by mono-axial hot pressing of the metal powder. Such moulded bodies are, however, porous and, when produced by smelting are also full of cracks so that disturbance in the layer formation may occur during the cathodic sputtering.
It is therefore the object of the invention to provide a method for the production of crack-free and pore-free targets of chromium or a chromium-base alloy.
This object is achieved according to the invention by introducing chromium or a chromium-base alloy into a metal sleeve, which is then evacuated, rendered gas tight and thereafter exposed to the action of a gas or gaseous mixture at a pressure of the order of 700 to 3,100 bars and a temperature of the order of 600 to 1 ,500 C which is maintained until the density of the resulting moulded body substantially corresponds with the theoretical density and then, after returning to room temperature and normal pressure, is separated from the moulded body.
The chromium or the chromium alloy, for example Cr80Fe20 Cr90Al 10 or Cr70Ni30, is introduced in powder form, preferably as a powder having a particle size between 20 and 200 ,um, as a compact which has been obtained by hot or cold pressing of the powder or as a porous casting produced from the melt, into the metal sleeve. In the case of the chromium alloy a powder mixture consisting of the individual components of the alloy or a compact obtained therefrom by hot or cold pressing can be inserted.
For the purpose of the present invention these unalloyed starting materials, which form the corresponding chromium alloy during the carrying out of the process can also be used as starting materials.
In the case of chromium a pressure of 1,200 bars and a temperature of 1 ,3400C are preferably used.
The pressure and temperature processing takes place in the presence of an inert gas, more especially argon or nitrogen, or a mixture of these gases.
To secure an improvement in the desorption of the gases adsorbed on the surface of the starting material introduced into the metal sleeve, it has proved advantageous during the evacuation of the latter to heat, preferbaly to approximately 2000C.
The sleeve is preferably a steel sleeve which is separated from the retained moulded body of mechanical treatment or by pickling.
The moulded target bodies produced according to the process of the invention are homogeneous, crack-free and pore-free.
The method of the invention is illustrated by the following example: Example A disc (diameter 225mm, thickness 15mm) having an approximately 70% theoretical density obtained by cold isostatic pressing of chromium powder having a particle size of 60 to 150 jum at a pressure of 2500 bars, is placed within a steel sleeve the internal measurements of which sleeve correspond with the measurements of the disc, said sleeve having a wall thickness of 2mm. The steel sleeve is provided with a steel cover having substantially the same wall thickness, into which cover a steel tube is welded for evacuation of the steel sleeve, and a gas-tight weld is made between sleeve and cover.The steel sleeve is then evacuated through the steel tube while heating the steel sleeve and the disc placed within it at approximately 2000C (approximately 10-3 to 10-4 millibar), provided with a gas-tight seal and placed within a pressure container. In the latter the steel sleeve together with the chromium disc is exposed to an argon pressure of 1200 bars and a temperature of 1 ,3400C for 3 hours. Then by reducing the argon pressure it is cooled to room temperature and the steel sleeve is withdrawn from the pressure container. The steel sleeve is then separated from the chromium target by milling.
The method of the invention can be carried out in variable temperature pressing devices which are known in industry and which are operated by means of gas pressure.
Claims
1. A method for the production of a moulded body of chromium or a chromium base alloy suitable for use as a target for cathodic sputtering, characterised in that chromium or the chromium base alloy is introduced into a metal sleeve, which is then evacuated, rendered gas-tight and thereafter exposed to the action of a gas or gaseous mixture at a pressure of the order of 700 to 3100 bars and a temperature of the order of 600 to 1500 C which is maintained until the density of the resulting moulded bodysubstantially corresponds to the theoretical density and then, after returing to room temperature and normal pressure, is separated from the moulded body.
2. A method according to claim 1, characterised in that the chromium or the chromium base alloy is introduced into the metal sleeve in powder form.
3. A method according to claim 1, characterised in that chromium or the chromium
**WARNING** end of DESC field may overlap start of CLMS **.

Claims (6)

**WARNING** start of CLMS field may overlap end of DESC **. SPECIFICATION Method for the Production of Targets of Chromium or Chromium Alloy This invention relates to a method for the production of moulded bodies of chromium or a chromium base alloy which are suitable for use as targets for cathodic sputtering. It is known ta use targets of chromium which have been electrolytically deposited onto a support for the application of thin chromium layers by cathodic sputtering. This "electrolytic chromium" has, however, a relatively high content of gases, notably of oxygen. Moulded bodies of chromium and chromium alloys, for example Cr80Fe20 and Cr90Al 10, which are suitable for use as targets are produced by smelting or by mono-axial hot pressing of the metal powder. Such moulded bodies are, however, porous and, when produced by smelting are also full of cracks so that disturbance in the layer formation may occur during the cathodic sputtering. It is therefore the object of the invention to provide a method for the production of crack-free and pore-free targets of chromium or a chromium-base alloy. This object is achieved according to the invention by introducing chromium or a chromium-base alloy into a metal sleeve, which is then evacuated, rendered gas tight and thereafter exposed to the action of a gas or gaseous mixture at a pressure of the order of 700 to 3,100 bars and a temperature of the order of 600 to 1 ,500 C which is maintained until the density of the resulting moulded body substantially corresponds with the theoretical density and then, after returning to room temperature and normal pressure, is separated from the moulded body. The chromium or the chromium alloy, for example Cr80Fe20 Cr90Al 10 or Cr70Ni30, is introduced in powder form, preferably as a powder having a particle size between 20 and 200 ,um, as a compact which has been obtained by hot or cold pressing of the powder or as a porous casting produced from the melt, into the metal sleeve. In the case of the chromium alloy a powder mixture consisting of the individual components of the alloy or a compact obtained therefrom by hot or cold pressing can be inserted. For the purpose of the present invention these unalloyed starting materials, which form the corresponding chromium alloy during the carrying out of the process can also be used as starting materials. In the case of chromium a pressure of 1,200 bars and a temperature of 1 ,3400C are preferably used. The pressure and temperature processing takes place in the presence of an inert gas, more especially argon or nitrogen, or a mixture of these gases. To secure an improvement in the desorption of the gases adsorbed on the surface of the starting material introduced into the metal sleeve, it has proved advantageous during the evacuation of the latter to heat, preferbaly to approximately 2000C. The sleeve is preferably a steel sleeve which is separated from the retained moulded body of mechanical treatment or by pickling. The moulded target bodies produced according to the process of the invention are homogeneous, crack-free and pore-free. The method of the invention is illustrated by the following example: Example A disc (diameter 225mm, thickness 15mm) having an approximately 70% theoretical density obtained by cold isostatic pressing of chromium powder having a particle size of 60 to 150 jum at a pressure of 2500 bars, is placed within a steel sleeve the internal measurements of which sleeve correspond with the measurements of the disc, said sleeve having a wall thickness of 2mm. The steel sleeve is provided with a steel cover having substantially the same wall thickness, into which cover a steel tube is welded for evacuation of the steel sleeve, and a gas-tight weld is made between sleeve and cover.The steel sleeve is then evacuated through the steel tube while heating the steel sleeve and the disc placed within it at approximately 2000C (approximately 10-3 to 10-4 millibar), provided with a gas-tight seal and placed within a pressure container. In the latter the steel sleeve together with the chromium disc is exposed to an argon pressure of 1200 bars and a temperature of 1 ,3400C for 3 hours. Then by reducing the argon pressure it is cooled to room temperature and the steel sleeve is withdrawn from the pressure container. The steel sleeve is then separated from the chromium target by milling. The method of the invention can be carried out in variable temperature pressing devices which are known in industry and which are operated by means of gas pressure. Claims
1. A method for the production of a moulded body of chromium or a chromium base alloy suitable for use as a target for cathodic sputtering, characterised in that chromium or the chromium base alloy is introduced into a metal sleeve, which is then evacuated, rendered gas-tight and thereafter exposed to the action of a gas or gaseous mixture at a pressure of the order of 700 to 3100 bars and a temperature of the order of 600 to 1500 C which is maintained until the density of the resulting moulded bodysubstantially corresponds to the theoretical density and then, after returing to room temperature and normal pressure, is separated from the moulded body.
2. A method according to claim 1, characterised in that the chromium or the chromium base alloy is introduced into the metal sleeve in powder form.
3. A method according to claim 1, characterised in that chromium or the chromium base alloy is introduced into the metal sleeve in the form of a pressed article.
4. A method according to claim 1, characterised in that chromium or the chromium alloy is introduced into the metal sleeve in the form of a porous and/or fissured casting.
5. A method according to any one of claims 1 to 4, characterised in that, in the case of chromium, a pressure of 1200 bars and a temperature of 1 3400C is used.
6. A method for the production of a moulded body of chromium or a chromium base alloy according to claim 1 and substantially as hereinbefore described with reference to the Example.
GB8129663A 1980-10-04 1981-10-01 Isostatic Pressing of Chromium Sputtering Targets Withdrawn GB2085032A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19803037617 DE3037617A1 (en) 1980-10-04 1980-10-04 METHOD FOR PRODUCING TARGETS FROM CHROME OR CHROME ALLOYS

Publications (1)

Publication Number Publication Date
GB2085032A true GB2085032A (en) 1982-04-21

Family

ID=6113652

Family Applications (1)

Application Number Title Priority Date Filing Date
GB8129663A Withdrawn GB2085032A (en) 1980-10-04 1981-10-01 Isostatic Pressing of Chromium Sputtering Targets

Country Status (4)

Country Link
JP (1) JPS5792103A (en)
DE (1) DE3037617A1 (en)
FR (1) FR2491502A1 (en)
GB (1) GB2085032A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2151261A (en) * 1983-12-14 1985-07-17 Rolls Royce Recovery of machine swarthy hot isostatic pressing

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62174373A (en) * 1985-10-04 1987-07-31 Hitachi Metals Ltd Chromium target material and its production
JPH0699728B2 (en) * 1985-10-31 1994-12-07 東ソー株式会社 Method for manufacturing rolled metal chrome
JPS62107036A (en) * 1985-11-02 1987-05-18 Toyo Soda Mfg Co Ltd Metallic chromium formed body and its production
JP5053961B2 (en) * 2008-09-08 2012-10-24 株式会社東芝 Sputtering target
JP5268771B2 (en) * 2009-05-07 2013-08-21 株式会社東芝 Method for producing sputtering target, method for forming hard film using the same, and hard film coated member
CN103785838B (en) * 2012-11-01 2016-06-01 宁波江丰电子材料股份有限公司 The making method of chromium target
CN105695832A (en) * 2014-11-26 2016-06-22 宁波江丰电子材料股份有限公司 CrMo alloy molding method
CN111604503B (en) * 2020-06-12 2022-03-29 钢铁研究总院 FeCrAl stainless steel composite pipe blank and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2151261A (en) * 1983-12-14 1985-07-17 Rolls Royce Recovery of machine swarthy hot isostatic pressing

Also Published As

Publication number Publication date
FR2491502A1 (en) 1982-04-09
JPS5792103A (en) 1982-06-08
DE3037617A1 (en) 1982-04-22

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WAP Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1)