KR20160149720A - Preparation method of sputtering target and the sputtering target prepared thereby - Google Patents
Preparation method of sputtering target and the sputtering target prepared thereby Download PDFInfo
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- KR20160149720A KR20160149720A KR1020150087254A KR20150087254A KR20160149720A KR 20160149720 A KR20160149720 A KR 20160149720A KR 1020150087254 A KR1020150087254 A KR 1020150087254A KR 20150087254 A KR20150087254 A KR 20150087254A KR 20160149720 A KR20160149720 A KR 20160149720A
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- pressing
- sintered body
- sputtering target
- powder
- pressure
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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
- 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
-
- 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
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
The present invention relates to a method of manufacturing a sputtering target used in a film forming process in manufacturing a semiconductor device and a sputtering target manufactured by the method.
In general, a sputtering target is used in a film forming process for forming a thin film in the production of a semiconductor device. In order to improve the characteristics of the thin film, characteristics such as low resistance, grain refinement, thermal and chemical stability and high purity are required.
Conventionally, such a sputtering target is manufactured by hot rolling the ingot produced by the electron beam melting method, pressurizing and sintering the raw material powder, proceeding hot isostatic pressing, hot pressing (HP) sintering the raw material powder, and then hot rolling .
However, the sputtering target manufactured by the above methods has a problem that it is difficult to form a uniform film on the deposition surface due to particle defects, deformation of the structure after rolling, and the like.
Therefore, there is a demand for development of a method for producing a sputtering target having fine grains and high density and high purity.
SUMMARY OF THE INVENTION It is an object of the present invention to provide a method of manufacturing a sputtering target having fine grains and high density and high purity in order to solve the above problems.
It is another object of the present invention to provide a sputtering target produced by the above-described production method.
In order to accomplish the above object, the present invention provides a method for manufacturing a molded article, comprising the steps of: (a) molding a formed article with a raw material powder; (b) pressing the formed body by cold isostatic pressing; (c) hot pressing the cold isostatic pressed compact to produce a sintered compact; (d) heat treating the sintered body in a reducing or vacuum atmosphere; (e) pressing the heat-treated sintered body under hot isostatic pressing; And (f) recrystallizing the sintered compact by pressurizing the hot isostatic pressing.
The raw material powder may be at least one selected from the group consisting of gold (Au) powder, tantalum (Ta) powder, tungsten (W) powder and tungsten silicide powder.
In addition, the pressure for molding the molded article with the raw material powder may be 25 to 65 MPa.
Further, the pressure for cold isostatic pressing of the formed body may be 1,500 to 2,700 bar.
The pressure for hot-pressing the molded article may be 15 to 20 MPa, the temperature may be 1,550 to 1,950 DEG C, and the time may be 3 to 5 hr.
The temperature for the heat treatment of the sintered body may be 1,600 to 1,900 ° C, and the time may be 3 to 8 hours.
The sintered body may be pressurized by hot isostatic pressing at a temperature of 1,500 to 1,700 ° C, a pressure of 90 to 110 MPa, a time of 2 to 4 hr, and a working vacuum degree of 10 -4 to 10 -5 Torr.
The temperature for recrystallizing the sintered body may be 1,500 to 1,650 DEG C, and the time may be 2 to 6 hours.
Meanwhile, the present invention provides a sputtering target manufactured by the above-described method.
The present invention relates to a method of manufacturing a sputtering target by molding a compact with a raw powder and subjecting the compact to a cold isostatic pressing (CIP), a hot press (HP), a heat treatment in a reducing or vacuum atmosphere, a hot isostatic pressing (HIP) It is possible to provide a sputtering target having fine grain size, high purity and high density.
1 is a flowchart showing a manufacturing process of the sputtering target of the present invention.
2 is an image showing the crystal grains of the sputtering target prepared in Example 1 of the present invention.
Hereinafter, the present invention will be described.
The present invention relates to a method of manufacturing a sputtering target having a fine grain size, high purity and high density by molding a formed body with a raw powder and then stepping the shaped body, and will be described with reference to the drawings.
1. Manufacturing method of sputtering target
(a) Molded body molding
First, a molded body is formed of a raw material powder. The raw material powder preferably has a purity of 99.995 wt% or more, an oxygen content of 500 ppm or less, a carbon content of 100 ppm or less, and a content of nitrogen, hydrogen, and sulfur of 50 ppm or less, respectively, considering the purity of the sputtering target. Such a raw material powder is not particularly limited, but is preferably at least one selected from the group consisting of gold (Au) powder, tantalum (Ta) powder, tungsten (W) powder and tungsten silicide powder.
The method of molding the molded article with the raw material powder is not particularly limited, but a method of charging the raw material powder into the molding die, performing a horizontal operation, and then pressing. At this time, the pressure for forming the molded body is not particularly limited, but is preferably 25 to 65 MPa. If the pressure is less than 25 MPa, the molding density is low and cracks may occur in the molded article. If the pressure exceeds 65 MPa, the molding mold may be damaged or the molded article may be broken.
On the other hand, it is preferable to apply the release material to the outer periphery of the molding die before charging the raw material powder so that the molding can be well separated from the molding die. At this time, if the amount of the releasing material applied is large, the charged raw material powder reacts with the releasing material to act as a contaminant. On the contrary, if the releasing material is small, cracks may occur in the releasing process.
The shaped body of the present invention thus molded has a molding density of 35% or more and is easy to handle, and the sputtering target to be finally produced has a high density.
(b) Cold Isostatic Pressing (CIP)
Thereby pressurizing the formed body by cold isostatic pressing. Specifically, a molded article is put into a plastic container (for example, a rubber container) having a plasticity, or the molded article is vacuum-packed and sealed with a wrapping paper, and then a uniform pressure is applied to the entire surface of the sealed molded article. The pressure at which the molded article is sealed is not particularly limited, but it is preferably 1,500 to 2,700 bar in consideration of the density of the molded article.
As a result of the cold isostatic pressing as described above, the present invention can obtain a molded article having a relative density of 60% or more and a homogeneous isotropy. Also, the sintering temperature can be lowered, so that the carbon content of the formed body can be reduced.
On the other hand, it is preferable that the relative density of the molded body after completion of the cold isostatic pressing treatment is determined by removing moisture outside the wrapping paper surrounding the molded body, removing the wrapping paper, and measuring the dimensions of the molded body. When the relative density is confirmed by using a hydrometer, the moisture penetrates the molded body, and the degree of vacuum may be lowered in the heat treatment process described later.
(c) Hot Press (HP)
The cold isostatically pressed compact is hot-pressed to produce a sintered compact. Specifically, the cold isostatically pressed molded article is placed in a carbon mold, charged into a hot press chamber, and sintered in a state where the exhaust is reduced to 5.0 x 10 -5 torr or less by using a vacuum pump. In this case, the sintering conditions are not particularly limited, but the sintering pressure is 15 to 20 MPa, the sintering temperature is 1,550 to 1,950 ° C, and the sintering time is 3 to 5 hr.
According to the hot press as described above, the present invention can obtain a sintered body having a relative density of 98% or more.
(d) Heat treatment
The sintered body is subjected to heat treatment (non-pressure heat treatment) in a reducing atmosphere or a vacuum atmosphere. At this time, in order to prevent the incorporation of carbon, it is preferable to place the sintered body on a pedestal (plate or setter) made of the same material as the sintered body and perform heat treatment.
The conditions for the heat treatment of the sintered body are not particularly limited, but the temperature for the heat treatment is preferably 1,600 to 1,900 ° C and the time for the heat treatment is preferably 3 to 8 hr. If the heat treatment temperature is less than 1,600 캜, it is difficult to obtain a sintered body having a required relative density or the gas reducing effect may deteriorate, and if it exceeds 1,900 캜, the carbon content may be increased.
According to the present invention, a sintered body having a relative density of 98.5% or more can be obtained by performing a heat treatment in a reducing atmosphere or a vacuum atmosphere.
(e) Hot Isostatic Pressing (HIP)
The heat-treated sintered body is pressurized by hot hydrostatic pressure. Specifically, the sintered body is sintered at a high temperature and a high pressure in the presence of an inert gas (for example, nitrogen, argon, etc.). When the sintered body is pressurized by hot hydrostatic pressure, the inert gas, which is a pressure medium, maintains the equal pressure so that the shape of the sintered body does not change during the sintering and the pores existing in the sintered body due to high temperature and high pressure are minimized to obtain a sintered body having high density have.
The conditions for pressing the sintered compact under hot isostatic pressing are not particularly limited, but the temperature is preferably 1,500 to 1,700 ° C. When the temperature is less than 1,500 ° C, it is difficult to obtain a sintered body having a reduced relative density or a desired relative density, and when the temperature exceeds 1,700 ° C, the crystal grains of the sintered body become coarsened or the gas content increases, This is because the purity can be lowered.
The pressure and time for hot hydrostatic pressure are not particularly limited, but the pressure is preferably 90 to 110 MPa and the sintering time is preferably 2 to 4 hours. The working vacuum degree is preferably 10 -4 to 10 -5 Torr.
According to the present invention, a sintered body having a relative density of 99.3% or more, a crystal grain size of 20 m or less, and oxygen and carbon of 50 ppm or less, respectively, can be obtained.
(f) Recrystallization treatment
The hot-pressing and sintered compact is recrystallized. At this time, the conditions for the recrystallization treatment are not particularly limited, but it is preferable that the heat treatment temperature for the recrystallization treatment is 1,500 to 1,650 DEG C and the time is 2 to 6 hr. If the temperature is less than 1,500 ° C, recrystallization of the sintered body may not occur. If the temperature exceeds 1,650 ° C, the crystal grains of the sintered body may become coarse or the gas content may increase, and the purity of the sintered body may decrease.
According to the recrystallization treatment as described above, the present invention can obtain a sintered body having a relative density of 99.7% or more and a purity of 99.998 wt% or more.
The sintered body obtained through the above process may further be subjected to bonding and processing processes known in the art. Specifically, the sintered body is bonded to a backing plate, processed to a required size, and the bead and arc treatment are performed on the backing plate surface. Then, the sputtering target is manufactured through a cleaning and packaging process.
2. Sputtering target
The present invention provides a sputtering target produced by the above production method. The sputtering target of the present invention has a high density of 99.7% or more, oxygen and carbon of less than 50 ppm each, a high purity of 99.998 wt% or more, and a fine grain size of 20 μm or less.
The field of use of the sputtering target of the present invention is not particularly limited, but is preferably used for wiring formation or electrode formation in the production of a semiconductor device (specifically, IC or LSI of a semiconductor device).
Hereinafter, the present invention will be described in detail with reference to examples. However, the following examples are illustrative of the present invention, and the present invention is not limited by the following examples.
[Example 1]
A tungsten powder containing 450 ppm of oxygen and 100 ppm of carbon and having a particle size of 10 占 퐉 and a purity of 99.995 wt% was charged in a molding die and then mounted on a molding press and subjected to a pressure of 37 MPa to form a molded article having a molding density of 40% And vacuum packed.
Next, a vacuum-packed molded article was subjected to a pressure of 2,000 bar for 1 hour to pressurize it by cold isostatic pressing to produce a molded article having a relative density of 62%.
Then, the molded body was placed in a carbon mold, charged into a hot press chamber, and a pressure of 20 MPa was applied at 1,850 캜 for 3 hours to prepare a sintered body having a relative density of 98.3%.
Next, the sintered body was heat-treated at 1,750 ° C for 5 hours in a vacuum atmosphere to prepare a sintered body having a relative density of 98.6%.
Then, the sintered body was subjected to a pressure of 98 MPa at 1,650 DEG C for 2 hours under a working vacuum degree of 10.sup.- 5 Torr to prepare a sintered body having a relative density of 99.4%.
Finally, the sintered body was recrystallized at 1,600 ° C for 2 hours to obtain a final sintered body.
[Comparative Example 1]
A sintered body was produced in the same manner as in Example 1, except for hot pressing and recrystallization.
[Comparative Example 2]
The sintered body was produced in the same manner as in Example 1, except that the cold isostatic pressing step, the heat treatment step and the recrystallization step were carried out.
[Comparative Example 3]
A tungsten powder containing 450 ppm of oxygen and 100 ppm of carbon and having a particle size of 10 μm and a purity of 99.995 wt% was placed in a carbon mold and charged into a hot press chamber. A pressure of 20 MPa was applied at 1,900 ° C. for 3 hours To prepare a sintered body. The sintered body thus produced was cold-rolled and annealed at a reduction ratio of 20%.
[Experimental Example 1]
The crystal grains of the tungsten sintered body manufactured in Example 1 were confirmed by an optical microscope, and the results are shown in FIG.
Referring to FIG. 2, the tungsten sintered body manufactured by the manufacturing method of the present invention has fine grains.
[Experimental Example 2]
The physical properties of the tungsten sintered bodies prepared in Example 1 and Comparative Examples 1 to 3 were evaluated by the following methods, and the results are shown in Table 1 below.
1. Relative density: Measured using Archimedes' principle (when the theoretical density is 19.3, relative density is 99.5% or higher, it is evaluated as high density)
2. Gas content analysis: Using OHN analyzer and CS analyzer (O content less than 50 ppm and C content less than 50 ppm)
Referring to Table 1, it can be seen that the tungsten sintered body (Example 1) produced by the manufacturing method of the present invention has a high relative density and a low gas content.
[Experimental Example 3]
The purity and grain size of the tungsten sintered bodies prepared in Example 1 and Comparative Examples 1 to 3 were analyzed. The results are shown in Table 2 below.
Referring to Table 2, it can be seen that the tungsten sintered body (Example 1) produced by the manufacturing method of the present invention has high purity and fine grain.
[Production Example 1]
A tungsten sputtering target was prepared by indium-bonding the tungsten sintered body prepared in Example 1 to an aluminum backing plate.
[Comparative Production Examples 1 to 3]
A tungsten sputtering target was prepared in the same manner as in Preparation Example 1, except that the tungsten sintered bodies prepared in Comparative Examples 1 to 3 were used instead of the tungsten sintered body prepared in Example 1, respectively.
[Experimental Example 4]
The tungsten sputtering target prepared in each of Production Example 1 and Comparative Production Examples 1 to 3 was applied to a DC magnetron sputtering apparatus (CENTURA PVD, AMAT Co.) to form a tungsten thin film having a thickness of about 500 Å. At this time, the substrate used for forming the tungsten thin film was a bare wafer (8 inches), and the substrate temperature was room temperature (about 21 to 25 ° C). The deposition power was 2.2 kW and the argon gas was fixed at 75 sccm.
Then, sheet resistance and uniformity of the formed thin film were evaluated by the following methods, and the results are shown in Table 3 below.
1, sheet resistance: Measured using MCP-T610 (MITSUBISHI CHEMICAL COPORATION)
2. Uniformity: Measured by applying the following equation
Referring to Table 3, it can be seen that the tungsten sputtering target manufactured by the manufacturing method of the present invention has low sheet resistance and high uniformity.
Claims (11)
(b) pressing the formed body by cold isostatic pressing;
(c) hot pressing the cold isostatic pressed compact to produce a pressure sintered compact;
(d) heat treating the sintered body in a reducing or vacuum atmosphere;
(e) pressing the heat-treated sintered body under hot isostatic pressing; And
(f) recrystallizing the sintered compact subjected to the hot isostatic pressing.
Wherein the raw material powder is at least one selected from the group consisting of gold (Au) powder, tantalum (Ta) powder, tungsten (W) powder and tungsten silicide powder.
Wherein the pressure for forming the formed body with the raw powder is 25 to 65 MPa.
And a pressure for pressing the formed body by cold isostatic pressing is 1,500 to 2,700 bar.
Wherein the pressure for hot-pressing the molded body is 15 to 20 MPa, the temperature is 1,550 to 1,950 占 폚, and the time is 3 to 5 hr.
Wherein the temperature for heat-treating the sintered body is 1,600 to 1,900 占 폚 and the time is 3 to 8 hours.
Wherein the temperature at which the sintered compact is pressurized by hot isostatic pressing is 1,500 to 1,700 ° C, the pressure is 90 to 110 MPa, the time is 2 to 4 hr, and the working vacuum degree is 10 -4 to 10 -5 Torr.
Wherein the sintered body is subjected to a recrystallization treatment at a temperature of 1,500 to 1,650 DEG C and a time of 2 to 6 hours.
A relative density of 99.7% or more, a grain size of 20 占 퐉 or less, a content of oxygen and carbon of 50 ppm or less, and a purity of 99.998 wt% or more.
A sputtering target used for wiring or electrode formation of semiconductor devices.
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020150087254A KR20160149720A (en) | 2015-06-19 | 2015-06-19 | Preparation method of sputtering target and the sputtering target prepared thereby |
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| KR1020150087254A KR20160149720A (en) | 2015-06-19 | 2015-06-19 | Preparation method of sputtering target and the sputtering target prepared thereby |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019031647A1 (en) * | 2016-10-07 | 2019-02-14 | 소문숙 | Oled organic thin-film layer forming method using rf sputtering device, rf sputtering device, and device for forming target used in rf sputtering device |
| WO2019117384A1 (en) * | 2017-12-14 | 2019-06-20 | 엘티메탈 주식회사 | Sputtering target for electromagnetic shielding, and method for producing same |
| KR20190073913A (en) * | 2017-12-19 | 2019-06-27 | 엘티메탈 주식회사 | A sputtering target whose deposition rate is controlled and a method for manufacturing the same |
| KR20210008689A (en) * | 2019-07-15 | 2021-01-25 | 주식회사 더방신소재 | Manufacturing method of high purity ITO target |
| CN116813343A (en) * | 2023-07-04 | 2023-09-29 | 有研资源环境技术研究院(北京)有限公司 | Inorganic electrochromic film-forming material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110042216A (en) | 2009-08-12 | 2011-04-25 | 가부시키가이샤 아루박 | Sputtering target and method for manufacturing a sputtering target |
-
2015
- 2015-06-19 KR KR1020150087254A patent/KR20160149720A/en unknown
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110042216A (en) | 2009-08-12 | 2011-04-25 | 가부시키가이샤 아루박 | Sputtering target and method for manufacturing a sputtering target |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019031647A1 (en) * | 2016-10-07 | 2019-02-14 | 소문숙 | Oled organic thin-film layer forming method using rf sputtering device, rf sputtering device, and device for forming target used in rf sputtering device |
| WO2019117384A1 (en) * | 2017-12-14 | 2019-06-20 | 엘티메탈 주식회사 | Sputtering target for electromagnetic shielding, and method for producing same |
| KR20190073913A (en) * | 2017-12-19 | 2019-06-27 | 엘티메탈 주식회사 | A sputtering target whose deposition rate is controlled and a method for manufacturing the same |
| KR20210008689A (en) * | 2019-07-15 | 2021-01-25 | 주식회사 더방신소재 | Manufacturing method of high purity ITO target |
| CN116813343A (en) * | 2023-07-04 | 2023-09-29 | 有研资源环境技术研究院(北京)有限公司 | Inorganic electrochromic film-forming material and preparation method thereof |
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