CN112126903A - Manufacturing method of tungsten sintered target material - Google Patents

Manufacturing method of tungsten sintered target material Download PDF

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Publication number
CN112126903A
CN112126903A CN202010959121.4A CN202010959121A CN112126903A CN 112126903 A CN112126903 A CN 112126903A CN 202010959121 A CN202010959121 A CN 202010959121A CN 112126903 A CN112126903 A CN 112126903A
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CN
China
Prior art keywords
target material
tungsten
sintering
sintered
sintered target
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.)
Pending
Application number
CN202010959121.4A
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Chinese (zh)
Inventor
大岩一彦
姚科科
廣田二郎
中村晃
林智行
山田浩
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Zhejiang Best Semiconductor Technology Co ltd
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Zhejiang Best Semiconductor Technology Co ltd
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Priority to CN202010959121.4A priority Critical patent/CN112126903A/en
Publication of CN112126903A publication Critical patent/CN112126903A/en
Pending legal-status Critical Current

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    • 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
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • 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
    • 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
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Abstract

The invention discloses a method for manufacturing a tungsten sintering target, which is characterized by comprising the steps of taking a high-purity tungsten powder sintering target used for sputtering, and filling tungsten raw material powder with the purity of 99.999% and the particle size of 3-5 mu m into a part consumed by the sintering target; placing the sintered target material filled with the tungsten raw material powder in a vacuum heat treatment furnace, and performing vacuum treatment at 5X 10‑2At a pressure below Pa, at 700-Maintaining at 1400 deg.C for 2 hr for degassing, introducing hydrogen, and heating under vacuum pressure of 10-1000Pa for 1-5 hr for degassing; performing vacuum hot pressing on the degassed sintering target material to finish the step of primary sintering; finishing secondary sintering of the sintered target material after primary sintering by a hot isostatic pressing technology; finally, grinding the whole surface of the secondarily sintered tungsten plate through mechanical processing to obtain a tungsten sintered target material; the method has the advantages of effectively improving the utilization rate of the target material and reducing environmental pollution.

Description

Manufacturing method of tungsten sintered target material
Technical Field
The invention relates to a method for manufacturing a tungsten sintering target.
Background
For thin film formation, such as conventional semiconductor and electronic equipment, the sputtering target is used at an efficiency of 30 to 40%, and up to 70% of the target is discarded without sputtering, relative to the weight of the target when new. In the conventional manufacturing method, the manufacturing yield of the input raw material of the sintered target material is about 55%, and the use efficiency after sputtering is only 40%, so the amount used for sputter deposition is only 20% of the input raw material. The target material also contains limited resources such as rare metals, and the like, and needs to be effectively utilized from the viewpoint of environmental protection, including recovery, so that the manufacturing cost is effectively reduced and the environmental resources are protected.
Disclosure of Invention
The invention aims to provide a method for manufacturing a tungsten sintering target material, which can effectively improve the utilization rate of the target material.
The technical scheme adopted by the invention for solving the technical problems is as follows: a manufacturing method of a tungsten sintering target material comprises the following steps: and (3) taking the high-purity tungsten powder sintering target material used for sputtering, filling tungsten raw material powder with the purity of 99.999% and the grain size of 3-5 mu m into the part consumed by the sintering target material, and sintering again by degassing, vacuum hot pressing and hot isostatic pressing technologies to form the tungsten sintering target material.
The method comprises the following specific steps:
(1) removing the back plate from the high-purity tungsten powder sintered target material and the back plate which are jointed after sputtering film formation, taking the sintered target material to remove surface dirt, carrying out acid washing, placing the sintered target material at the bottom of a sintering clamp, and filling tungsten raw material powder with the purity of 99.999 percent and the grain diameter of 3-5 mu m in the consumed part of the sintered target material;
(2) placing the sintered target material filled with the tungsten raw material powder in a vacuum heat treatment furnace, and performing vacuum treatment at 5X 10-2Keeping the temperature of 700-1400 ℃ for 2 hours under the pressure below Pa for degassing, then introducing hydrogen, and continuing heating for 1-5 hours under the vacuum pressure of 10-1000Pa for degassing;
(3) the degassed sintered target material is hot-pressed in vacuum at 5X 10-2Pa, temperature of 1600-1900 ℃ and pressure of 400-600kg/cm2Processing for 120-480min under the condition of (1) to finish primary sintering;
(4) the sintered target material after the primary sintering is kept for 480min at 1800-2000 ℃ and 140-200MPa by a hot isostatic pressing technology, and the secondary sintering is finished;
(5) and (3) grinding the whole surface of the secondarily sintered tungsten plate by 1-1.5mm through mechanical processing to obtain the tungsten sintered target material with the purity of 99.999 percent or more and the density of 99 percent or more.
Compared with the prior art, the invention has the advantages that: the present invention provides a method for manufacturing a tungsten sintered target, which can reuse a target used after sputter deposition without being wasted, redissolved, or powdered. According to the present manufacturing method, the manufacturing yield from the input raw material can be greatly improved from 55% to 80% in comparison with the conventional method.
Drawings
FIG. 1 is a schematic view of the manufacturing process of the tungsten sintered target of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1:
a method for manufacturing a tungsten sintered target material, as shown in fig. 1, comprises the following steps: taking a high-purity tungsten powder sintering target material used for sputtering, filling tungsten raw material powder with the purity of 99.999 percent and the grain diameter of 3-5 mu m into the part consumed by the sintering target material, and sintering again by degassing, vacuum hot pressing and hot isostatic pressing technology to form the tungsten sintering target material, which comprises the following specific steps:
(1) removing the back plate from the high-purity tungsten powder sintered target material and the back plate which are jointed after sputtering film formation, taking the sintered target material to remove surface dirt, carrying out acid washing, placing the sintered target material at the bottom of a sintering clamp, and filling tungsten raw material powder with the purity of 99.999 percent and the grain diameter of 3-5 mu m in the consumed part of the sintered target material;
(2) placing the sintered target material filled with the tungsten raw material powder in a vacuum heat treatment furnace, and performing vacuum treatment at 5X 10-2Keeping the temperature below Pa for 2 hours at 1000 ℃ for degassing, introducing hydrogen, and continuously heating for 1-5 hours under the vacuum pressure of 10-1000Pa for degassing;
(3) the degassed sintered target material is hot-pressed in vacuum at 5X 10-2Pa, temperature 1800 ℃ and pressure 500kg/cm2Treating for 240min under the condition of (1) to finish primary sintering;
(4) the sintered target material after the primary sintering is kept for 240min at 1900 ℃ and 180MPa through a hot isostatic pressing technology, and secondary sintering is completed;
(5) and (3) grinding the whole surface of the secondarily sintered tungsten plate by 1-1.5mm through mechanical processing to obtain the tungsten sintered target material with the purity of 99.999 percent or more and the density of 99 percent or more.
Example 2:
the difference from example 1 is that:
(2) placing the sintered target material filled with the tungsten raw material powder in a vacuum heat treatment furnace, and performing vacuum treatment at 5X 10-2Keeping at 700 deg.C for 2 hr under Pa, degassing, introducing hydrogen gas, and heating under vacuum pressure of 10Pa for 5 hr to degas;
(3) the degassed sintered target material is hot-pressed in vacuum at 5X 10-2Pa, temperature 1600 ℃ and pressure 400kg/cm2Processing for 480min under the condition of (1) to finish primary sintering;
(4) and (3) the sintered target material after the primary sintering is kept for 480min at 1800 ℃ and 140MPa through a hot isostatic pressing technology, so that the secondary sintering is completed.
Example 3:
the difference from example 1 is that:
(2) placing the sintered target material filled with the tungsten raw material powder in a vacuum heat treatment furnace, and performing vacuum treatment at 5X 10-2Keeping at 1400 deg.C for 2 hr under Pa, degassing, introducing hydrogen gas, and heating under vacuum of 1000Pa for 1 hr to degas;
(3) the degassed sintered target material is hot-pressed in vacuum at 5X 10-2Pa, temperature 1900 deg.C and applied pressure 600kg/cm2Treating for 120min under the condition of (1) to finish primary sintering;
(4) and (3) keeping the sintered target material subjected to the primary sintering for 120min at 2000 ℃ and under 200MPa through a hot isostatic pressing technology, and finishing the secondary sintering.
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art should also realize that changes, modifications, additions and substitutions can be made without departing from the true spirit and scope of the invention.

Claims (2)

1. A method for manufacturing a tungsten sintered target is characterized by comprising the following steps: and (3) taking the high-purity tungsten powder sintering target material used for sputtering, filling tungsten raw material powder with the purity of 99.999% and the grain size of 3-5 mu m into the part consumed by the sintering target material, and sintering again by degassing, vacuum hot pressing and hot isostatic pressing technologies to form the tungsten sintering target material.
2. The method for manufacturing the tungsten sintered target according to claim 1, comprising the following steps:
(1) removing the back plate from the high-purity tungsten powder sintered target material and the back plate which are jointed after sputtering film formation, taking the sintered target material to remove surface dirt, carrying out acid washing, placing the sintered target material at the bottom of a sintering clamp, and filling tungsten raw material powder with the purity of 99.999 percent and the grain diameter of 3-5 mu m in the consumed part of the sintered target material;
(2) placing the sintered target material filled with the tungsten raw material powder in a vacuum heat treatment furnace, and performing vacuum treatment at 5X 10-2Keeping the temperature of 700-1400 ℃ for 2 hours under the pressure below Pa for degassing, then introducing hydrogen, and continuing heating for 1-5 hours under the vacuum pressure of 10-1000Pa for degassing;
(3) the degassed sintered target material is hot-pressed in vacuum at 5X 10-2Pa, temperature of 1600-1900 ℃ and pressure of 400-600kg/cm2Processing for 120-480min under the condition of (1) to finish primary sintering;
(4) the sintered target material after the primary sintering is kept for 480min at 1800-2000 ℃ and 140-200MPa by a hot isostatic pressing technology, and the secondary sintering is finished;
(5) and (3) grinding the whole surface of the secondarily sintered tungsten plate by 1-1.5mm through mechanical processing to obtain the tungsten sintered target material with the purity of 99.999 percent or more and the density of 99 percent or more.
CN202010959121.4A 2020-09-14 2020-09-14 Manufacturing method of tungsten sintered target material Pending CN112126903A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112643188A (en) * 2020-12-30 2021-04-13 浙江最成半导体科技有限公司 Vacuum diffusion bonding method for target and back plate

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001342562A (en) * 2000-06-01 2001-12-14 Hitachi Metals Ltd Target material and manufacturing method
JP2003193111A (en) * 2001-12-27 2003-07-09 Nippon Steel Corp Method for manufacturing tungsten sputtering target
JP2007314883A (en) * 2007-06-11 2007-12-06 Nikko Kinzoku Kk Method for producing tungsten sintered compact target for sputtering
CN101748361A (en) * 2008-12-11 2010-06-23 上海广电电子股份有限公司 Method for manufacturing sputtering target
JP2010159482A (en) * 2009-01-07 2010-07-22 Solar Applied Materials Technology Corp Refurbished sputtering target and method for making the same
CN102343437A (en) * 2011-11-11 2012-02-08 宁波江丰电子材料有限公司 Method for manufacturing tungsten target material
CN104694895A (en) * 2013-12-05 2015-06-10 有研亿金新材料股份有限公司 W-Ti alloy target material and manufacturing method thereof
KR20160067490A (en) * 2014-12-04 2016-06-14 희성금속 주식회사 Refurbishing method of tungsten spent target and reuse tungsten target for forming wiring and electrode prepared thereby
CN105986160A (en) * 2016-06-24 2016-10-05 贵研铂业股份有限公司 Method for preparing large-size high-purity tungsten titanium alloy target materials

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001342562A (en) * 2000-06-01 2001-12-14 Hitachi Metals Ltd Target material and manufacturing method
JP2003193111A (en) * 2001-12-27 2003-07-09 Nippon Steel Corp Method for manufacturing tungsten sputtering target
JP2007314883A (en) * 2007-06-11 2007-12-06 Nikko Kinzoku Kk Method for producing tungsten sintered compact target for sputtering
CN101748361A (en) * 2008-12-11 2010-06-23 上海广电电子股份有限公司 Method for manufacturing sputtering target
JP2010159482A (en) * 2009-01-07 2010-07-22 Solar Applied Materials Technology Corp Refurbished sputtering target and method for making the same
CN102343437A (en) * 2011-11-11 2012-02-08 宁波江丰电子材料有限公司 Method for manufacturing tungsten target material
CN104694895A (en) * 2013-12-05 2015-06-10 有研亿金新材料股份有限公司 W-Ti alloy target material and manufacturing method thereof
KR20160067490A (en) * 2014-12-04 2016-06-14 희성금속 주식회사 Refurbishing method of tungsten spent target and reuse tungsten target for forming wiring and electrode prepared thereby
CN105986160A (en) * 2016-06-24 2016-10-05 贵研铂业股份有限公司 Method for preparing large-size high-purity tungsten titanium alloy target materials

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112643188A (en) * 2020-12-30 2021-04-13 浙江最成半导体科技有限公司 Vacuum diffusion bonding method for target and back plate

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Application publication date: 20201225

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