JPS63111172A - Production of target material - Google Patents
Production of target materialInfo
- Publication number
- JPS63111172A JPS63111172A JP25727786A JP25727786A JPS63111172A JP S63111172 A JPS63111172 A JP S63111172A JP 25727786 A JP25727786 A JP 25727786A JP 25727786 A JP25727786 A JP 25727786A JP S63111172 A JPS63111172 A JP S63111172A
- Authority
- JP
- Japan
- Prior art keywords
- target material
- metal
- grain size
- hot
- annealing
- 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
Links
- 239000013077 target material Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 238000004544 sputter deposition Methods 0.000 claims abstract description 7
- 239000000956 alloy Substances 0.000 claims abstract description 6
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 10
- 239000010409 thin film Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 5
- 238000005266 casting Methods 0.000 description 4
- 239000011651 chromium Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910020630 Co Ni Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002440 Co–Ni Inorganic materials 0.000 description 1
- 229910017061 Fe Co Inorganic materials 0.000 description 1
- 229910017116 Fe—Mo Inorganic materials 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野〕
本発明は、フォトマスク用、磁気記録金属媒体用、磁気
ヘッド用、ミラー用等に、使用されている金属または合
金薄膜用ターゲット材（以下金属ターゲット材と記す）
の改良に関するものである。Detailed Description of the Invention (Industrial Field of Application) The present invention relates to target materials for metal or alloy thin films (hereinafter referred to as (described as metal target material)
This is related to the improvement of.
従来のスパッタリング用金屈ターゲット材は、主に、真
空溶解鋳造法か、粉末焼結法でえられる成形塊（銅塊）
を、所定寸法に切断、切削または研磨等の殿城加工仕上
したものが用いられていた。Conventional Kinku target materials for sputtering are mainly formed ingots (copper ingots) obtained by vacuum melting and casting or powder sintering.
It was used that was finished by cutting, milling, or polishing to a predetermined size.
しかし、真空溶解鋳造法によるものでは結晶粒径の制御
が、困難であったり、また、鋳造欠陥や焼結よる残余空
孔のために、密度も低いものであった。このため従来の
金属ターゲット材では、スパッタ時に、グコー放電の安
定持続が困難となり、その結果として、ターゲット効率
の低下をもたらし、有効利用される部分が少ないという
問題を生じている。However, with the vacuum melting casting method, it is difficult to control the crystal grain size, and the density is low due to casting defects and residual pores due to sintering. For this reason, with conventional metal target materials, it is difficult to sustain a stable gouco discharge during sputtering, resulting in a decrease in target efficiency and a problem in that only a small amount of effective utilization occurs.
そこで、本発明は、スパッタリングを安定化しかつ無駄
を少なく有効に使用できる金属ターゲット材の製造方法
を提供しようとするものである。Therefore, the present invention aims to provide a method for manufacturing a metal target material that can stabilize sputtering and be used effectively with less waste.
本発明は、金属ターゲット材を製造する工程に、熱間も
しくは冷間塑性加工並びに焼鈍を加えることで、結晶粒
径を制御し、空孔がなく均質な金属ターゲット材を供給
することにより、前記問題点を解決するものである。The present invention adds hot or cold plastic working and annealing to the process of manufacturing a metal target material, thereby controlling the crystal grain size and supplying a homogeneous metal target material without voids. It is a solution to a problem.
すなわち、実施例で述べるように、各種合金系に応じて
、４Ｑｍｍないし７０龍厚みのシートバーを、８ないし
１０朋まで熱間圧延（ただし、Ｎｉ系の場合は、後半の
冷間圧延率５０％）したのち、８００°Ｃないし１１５
０℃に、１０分間ないし３０分間保持し、徐冷（５０℃
／ＨＲ）あるいは、空冷すること等によって、存在する
空孔を除去し、また結晶粒径を小さくするとともに、均
一に制御するものである。That is, as described in the examples, a sheet bar with a thickness of 4Q mm to 70 mm is hot rolled to a thickness of 8 to 10 mm depending on the various alloy systems (however, in the case of Ni-based alloys, the latter half cold rolling rate is 50 mm). %) and then 800°C to 115°C.
Hold at 0°C for 10 to 30 minutes and slowly cool (50°C).
/HR) Alternatively, existing pores are removed by air cooling, and the crystal grain size is reduced and uniformly controlled.
本発明によれば、ターゲット材が、スパッタされて、表
面から少しずつ減ってゆく過程で、結晶粒の差異が、ス
パッタ面に現われて、成膜の安定を欠くことや、空孔が
スパーク放電を起こさせることが無く、グロー放電の安
定持続が可能である。According to the present invention, when the target material is sputtered and gradually decreases from the surface, differences in crystal grains appear on the sputtering surface, resulting in unstable film formation and voids causing spark discharge. The glow discharge can be maintained stably without causing any problems.
その結果として、ターゲット材の有効利用率が、高くな
る。As a result, the effective utilization rate of the target material increases.
〔実施例〕
実施例１．Ｎｉ−Ｆｅターゲット
組成が８２．４％Ｎｉ １７．６％Ｆｅ （ｗｔ％）
、真空誘導炉で溶解・精錬・鋳造した鋼塊を、１１５０
℃に加熱して、１８鶴厚さに熱間圧延し、その後、９鶴
まで冷間圧延した後、種々の条件で焼鈍し、結晶粒度を
調べた。この結果を表に示す。[Example] Example 1. Ni-Fe target composition is 82.4%Ni 17.6%Fe (wt%)
, steel ingots melted, refined and cast in a vacuum induction furnace, 1150
℃, hot rolled to a thickness of 18 mm, then cold rolled to a thickness of 9 mm, annealed under various conditions, and the grain size was examined. The results are shown in the table.
このうち代表的なミクロ組織写真（Ｘ１００倍）を第１
図に示す。ＡおよびＢはそれぞれ表のＴＰＮｎｌおよび
４によるものであり、木表から焼鈍により結晶粒径の制
御が可能であることが判る。The first representative microstructure photograph (x100) is
As shown in the figure. A and B are based on TPNnl and 4 in the table, respectively, and it can be seen from the wood surface that the grain size can be controlled by annealing.
実施例’１． Ｃｏ−Ｎｉ−Ｃｒターゲット組成が、
６２．５％Ｃｏ−３０％Ｎｉ−７，５％Ｃｒ（八Ｔ％）
、真空誘導炉で溶解・精錬・鋳造した鋼塊を、１１００
℃で、３７１１厚さのシートバーに鋳造し、得られたシ
ートバーを１１３０°Ｃに加熱後、１０ｍｍに圧延し、
１１００°Ｃ×１５分間の保持後空冷した。Example '1. Co-Ni-Cr target composition is
62.5%Co-30%Ni-7,5%Cr (8T%)
, steel ingots melted, refined and cast in a vacuum induction furnace,
℃, and the obtained sheet bar was heated to 1130°C and rolled to 10mm.
After holding at 1100°C for 15 minutes, it was air cooled.
本実施例によるＭｉ織写真を第２図Ｂに示す。なおＡは
鋳造ままの参考Ｂは焼鈍後のものである。A photograph of the Mi weave according to this example is shown in FIG. 2B. Note that A is as-cast and Reference B is after annealing.
実施例３．純クロムターゲット
純クロムターゲット材（９９，９％以上）を、クロム粉
末をカプセルに封入し、旧Ｐでシートバーに焼結し、１
１００°Ｃで、３０分以上加熱保持後、１０ｍ厚さに熱
間圧延して、１０００℃ないし１１５０℃に３０分間保
持後、曲取りをして約５０℃／ＨＲで徐冷して制作した
。Example 3. Pure chromium target Pure chromium target material (99.9% or more) is encapsulated with chromium powder and sintered into a sheet bar using old P.
After heating and holding at 100°C for 30 minutes or more, hot rolling to a thickness of 10m, holding at 1000°C to 1150°C for 30 minutes, decurving and slowly cooling at about 50°C/HR. .
比較のために、鋳造法によるもの（写真Ａ）、粉末焼結
法によるもの（写真Ｂ）、および本発明によるもの（写
真Ｃ）のミクロ組織を第３図に示す。For comparison, FIG. 3 shows the microstructures of those produced by the casting method (Photo A), those produced by the powder sintering method (Photo B), and those produced by the present invention (Photo C).
また、これらの方法によって作られたクーゲット材の比
重は、それぞれ、Ａ ： ７．１５５． Ｂ ： ７．
１６８゜Ｃ： ７．１８４であり、本発明によるＣは、
ミクロ組織が均質であり、空孔がないことが判る。Further, the specific gravity of the Cougett material made by these methods is A: 7.155. B: 7.
168°C: 7.184, and C according to the present invention is
It can be seen that the microstructure is homogeneous and there are no pores.
上記実施例の他に、Ｃｏ −Ｃｒ系、Ｃｏ−Ｎｉ系、Ｎ
ｉ−、Ｆｅ−Ｍｏ系およびＦｅ −Ｃｏ系についてテス
トした結果、いずれも本発明の適用が可能であり、かつ
結晶粒径制御が可能で、均質化、空孔発生防止の効果が
顕著であることが確認された。In addition to the above examples, Co-Cr type, Co-Ni type, N
As a result of testing on i-, Fe-Mo system, and Fe-Co system, it was found that the present invention can be applied to all of them, the crystal grain size can be controlled, and the effect of homogenization and prevention of pore generation is remarkable. This was confirmed.
以上述べたように、本発明はターゲット材の結晶粒径制
？ｌ［ｌ、均質化、空孔の発生防止を可能とし、これに
よりグロー放電を安定化するとともに使用率が向上する
等、高品質のターゲット材の製造を可能とするものであ
る。As mentioned above, the present invention is based on the crystal grain size control of the target material. This makes it possible to homogenize and prevent the generation of pores, thereby stabilizing glow discharge and increasing the usage rate, making it possible to manufacture high-quality target materials.
第１図は、本発明による１７．６ｗｔ％Ｆｅ−Ｎｉター
ゲット材のミクロ金属組織写真であり、ＡおよびＢはそ
れぞれ表のＴＰＮＩＩ １および２によるもの、第２図
は、本発明の結晶粒径制御効果を説明するミクロ金属組
織写真で、ＡおよびＢはそれぞれ鋳造のままおよび焼鈍
後のもの、第３図は、従来および本発明の製造法による
ミクロ金属組織の比較写真であり、Ａは鋳造法、Ｂは粉
末焼結法、Ｃは本発明によるものである。
第１図 （ｘｌｏｏイ０
第２図（×／ρ０イ幻Figure 1 is a micrometallic structure photograph of a 17.6wt% Fe-Ni target material according to the present invention, A and B are those of TPNII 1 and 2 in the table, respectively, and Figure 2 is a photograph of the crystal grain size of the present invention. Micrometallic structure photographs to explain the control effect, A and B are as-cast and after annealing, respectively. Figure 3 is a comparative photograph of micrometallic structures produced by conventional and inventive manufacturing methods, and A is cast method, B is a powder sintering method, and C is according to the present invention. Figure 1 (xloooi 0 Figure 2 (x/ρ0i illusion)
Claims (1)
れる金属または合金系ターゲット材において、熱間もし
くは冷間塑性加工または熱間および冷間塑性加工並びに
焼鈍を施すことを特長とする、ターゲット材の製造方法
。A metal or alloy target material used in the sputtering process to produce a metal thin film, which is characterized by subjecting it to hot or cold plastic working, hot and cold plastic working, and annealing. Production method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25727786A JPS63111172A (en) | 1986-10-29 | 1986-10-29 | Production of target material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25727786A JPS63111172A (en) | 1986-10-29 | 1986-10-29 | Production of target material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63111172A true JPS63111172A (en) | 1988-05-16 |
Family
ID=17304140
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25727786A Pending JPS63111172A (en) | 1986-10-29 | 1986-10-29 | Production of target material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63111172A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63216966A (en) * | 1987-03-06 | 1988-09-09 | Toshiba Corp | Target for sputtering |
| JP2012052193A (en) * | 2010-09-01 | 2012-03-15 | Jx Nippon Mining & Metals Corp | Indium target and method for manufacturing the same |
| US9023487B2 (en) | 2011-09-21 | 2015-05-05 | Jx Nippon Mining & Metals Corporation | Laminated structure and method for producing the same |
| US9139900B2 (en) | 2011-03-01 | 2015-09-22 | JX Nippon Mining Metals Corporation | Indium target and manufacturing method thereof |
| US9758860B2 (en) | 2012-01-05 | 2017-09-12 | Jx Nippon Mining & Metals Corporation | Indium sputtering target and method for manufacturing same |
| US9761421B2 (en) | 2012-08-22 | 2017-09-12 | Jx Nippon Mining & Metals Corporation | Indium cylindrical sputtering target and manufacturing method thereof |
| US9922807B2 (en) | 2013-07-08 | 2018-03-20 | Jx Nippon Mining & Metals Corporation | Sputtering target and method for production thereof |
-
1986
- 1986-10-29 JP JP25727786A patent/JPS63111172A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63216966A (en) * | 1987-03-06 | 1988-09-09 | Toshiba Corp | Target for sputtering |
| JPH0371510B2 (en) * | 1987-03-06 | 1991-11-13 | Tokyo Shibaura Electric Co | |
| JP2012052193A (en) * | 2010-09-01 | 2012-03-15 | Jx Nippon Mining & Metals Corp | Indium target and method for manufacturing the same |
| US9490108B2 (en) | 2010-09-01 | 2016-11-08 | Jx Nippon Mining & Metals Corporation | Indium target and method for manufacturing same |
| US9139900B2 (en) | 2011-03-01 | 2015-09-22 | JX Nippon Mining Metals Corporation | Indium target and manufacturing method thereof |
| US9023487B2 (en) | 2011-09-21 | 2015-05-05 | Jx Nippon Mining & Metals Corporation | Laminated structure and method for producing the same |
| US9758860B2 (en) | 2012-01-05 | 2017-09-12 | Jx Nippon Mining & Metals Corporation | Indium sputtering target and method for manufacturing same |
| US9761421B2 (en) | 2012-08-22 | 2017-09-12 | Jx Nippon Mining & Metals Corporation | Indium cylindrical sputtering target and manufacturing method thereof |
| US9922807B2 (en) | 2013-07-08 | 2018-03-20 | Jx Nippon Mining & Metals Corporation | Sputtering target and method for production thereof |
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