JP2646058B2 - Sputter target material and method for producing the same - Google Patents
Sputter target material and method for producing the sameInfo
- Publication number
- JP2646058B2 JP2646058B2 JP5013072A JP1307293A JP2646058B2 JP 2646058 B2 JP2646058 B2 JP 2646058B2 JP 5013072 A JP5013072 A JP 5013072A JP 1307293 A JP1307293 A JP 1307293A JP 2646058 B2 JP2646058 B2 JP 2646058B2
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- JP
- Japan
- Prior art keywords
- tungsten
- target material
- sintering
- sputter target
- rolling
- Prior art date
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- Physical Vapour Deposition (AREA)
Description
【0001】[0001]
【産業上の利用分野】本発明は,スパッターターゲット
材に関し,詳しくは,高純度のタングステン円板からな
るスパッターターゲット材及びその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sputter target material, and more particularly, to a sputter target material made of a high-purity tungsten disk and a method of manufacturing the same.
【0002】[0002]
【従来の技術】従来,スパッターターゲット材として使
用されているタングステンは,タングステン粉末をプレ
スし,又はホットプレスして焼結したものか,CVDに
よって製造されたものが使用されている。2. Description of the Related Art Conventionally, tungsten used as a sputtering target material is obtained by sintering a tungsten powder by pressing or hot pressing, or manufactured by CVD.
【0003】[0003]
【発明が解決しようとする課題】ここで良好なスパッタ
ー材料であるとは,どのようなものかを述べてみる。The following describes what a good sputter material is.
【0004】(1)硬度をHv 400以内にし,スパッ
ター材に必要な材料表面粗さを保持できる。具体的には
Rmax を1μm以下にし得ること。[0004] (1) The hardness was within H v 400, can hold the material surface roughness required for sputtering material. Specifically, R max can be set to 1 μm or less.
【0005】これは,スパッター時にパーティクルが抑
えられるから(パーティクルの絶対条件ではないが)で
ある。[0005] This is because particles are suppressed during sputtering (although this is not an absolute condition for particles).
【0006】(2)Wは元々高比重,しかし密度を上げ
ておく事が最も大切である。(2) W originally has a high specific gravity, but it is most important to increase its density.
【0007】一般的にスパッター材は理論密度の85な
いし90%以上が必須で,最近では93〜95%が望ま
しいとされている。というのはスパッターした時の原子
の飛びがムラない事が望まれる訳でターゲット材を上空
から見た場合なるべく均一にしかも密に配列してるのが
良い。In general, the sputtered material is required to have a density of 85 to 90% or more of the theoretical density, and recently, 93 to 95% is desirable. This is because it is desired that the atoms do not fly evenly when sputtered. Therefore, when the target materials are viewed from above, it is preferable that the target materials be arranged as uniformly and densely as possible.
【0008】又,Wは体心立方型の結晶構造を有してお
りむしろ面方位偏らない事が良く,事実本発明品も別紙
に示す通りランダム方位(無配向)であった。Further, W has a body-centered cubic type crystal structure, and it is rather good that the plane orientation is not deviated. In fact, the present invention also has a random orientation (non-oriented) as shown in the separate sheet.
【0009】(3)結晶粒としては,図3(a)及び図
3(b)の様に考えた場合,図3(b)で示す横並びの
方がスパッター時パーティクルは発生しにくいと考えら
れる。[0009] (3) As the crystal grains, FIG. 3 (a) and FIG.
When considered as shown in FIG. 3 (b), it is considered that particles are less likely to be generated at the time of sputtering in the horizontal arrangement shown in FIG. 3 (b).
【0010】更に,粒径が30μm以下では材質自体の
硬度も上昇する上,粒子が結果として縦並びになったと
同様な配列になり不都合である。また,粒径が300μ
m以上にするには加熱処理費がかかり不適当である。Further, when the particle size is 30 μm or less, the hardness of the material itself increases, and the particles are arranged in the same manner as the vertical arrangement, which is disadvantageous. The particle size is 300μ.
If it is more than m, a heat treatment cost is required, which is not appropriate.
【0011】上記したように,スパッターターゲット材
として使用されているタングステンは,タングステン粉
末をプレスし,焼結したものと,CVDによって製造さ
れたものとが使用されているが,前記したタングステン
粉末をプレスし,焼結したものは,密度が理論密度に対
し97%以上にすることが困難であり,低密度品になる
という欠点を有している。このような,低密度のスパッ
ターターゲット材は,スパッタリングした際,被スパッ
タリング材の状態がムラや気泡等が発生し,高品質の製
品には,向かず適正な材質ではない。As described above, tungsten used as a sputtering target material is obtained by pressing and sintering a tungsten powder, and also manufactured by CVD. Pressed and sintered products have the drawback that it is difficult to achieve a density of 97% or more of the theoretical density, resulting in low density products. Such a low-density sputter target material is not suitable for a high-quality product because the state of the material to be sputtered becomes uneven or bubbles when sputtered.
【0012】一方,後者のCVDによって製造されたも
のは,品質的には問題がないが製造コストが高く,高価
なものになるという欠点を有している。又ホットプレス
によるものは高密度の製品が得難く充分な評価が得られ
ていない。[0012] On the other hand, the latter manufactured by CVD has no drawbacks in terms of quality, but has the drawback that the manufacturing cost is high and expensive. In addition, a hot press cannot obtain a high-density product, and has not been sufficiently evaluated.
【0013】そこで,本発明の技術的課題は,スパッタ
ーターゲット用の材料品質特性を満足し,圧延加工とそ
の後二次加工に於けるトラブルを皆無にし,実用性のあ
る低コストのスパッターターゲット材及びその製造方法
を提供することにある。[0013] Therefore, the technical problem of the present invention is to provide a low-cost sputter target material that can satisfy the quality characteristics of the material for the sputter target, eliminates any troubles in the rolling process and the subsequent secondary process, and is practical. It is to provide a manufacturing method thereof.
【0014】[0014]
【課題を解決するための手段】本発明によれば,タング
ステン焼結体の圧延材であって,前記圧延材は,結晶粒
径が30〜300μmのタングステン粒子を有するとと
もに360〜400の範囲内の硬度と,99.0%以上
の相対密度とを有し,前記タングステン粒子は,細長い
結晶粒子からなり,且つ並び方が長さ方向が板面に沿っ
ている横並びであることを特徴とするタングステンター
ゲット材が得られる。According to the present invention, there is provided a rolled material of a tungsten sintered body, wherein the rolled material has tungsten particles having a crystal grain size of 30 to 300 μm and is in a range of 360 to 400. possess a and hardness, 99.0% or more and the relative density, the tungsten particles are elongated
Consisting of crystal grains and aligned in the length direction along the plate surface
Thus , a tungsten target material characterized by being aligned horizontally can be obtained.
【0015】また,本発明によれば,粉末冶金法によっ
て,タングステン粉末をプレス成型し,焼結し,熱間圧
延するタングステン焼結体の圧延材の製造方法におい
て,焼結の際,真空雰囲気中で1400〜1700℃の
範囲で熱処理を行った後,1800℃以上で焼結を行う
工程と,さらに圧延後,1200〜1500℃の範囲で
結晶粒調整のための熱処理工程とを備えたことを特徴と
するスパッターターゲット材の製造方法が得られる。Further, according to the present invention, in a method for producing a rolled material of a tungsten sintered body in which a tungsten powder is press- molded by powder metallurgy, sintered, and hot-rolled, the method comprises the steps of: After performing heat treatment in the range of 1400 to 1700 ° C in the inside, sintering at 1800 ° C or more, and further rolling, and then in the range of 1200 to 1500 ° C
A method for producing a sputter target material, comprising a heat treatment step for adjusting crystal grains .
【0016】即ち,本発明においては,タングステン粉
末をプレス,焼結した後,一次加工の熱間圧延または鍛
造加工を行うことにより,相対密度(対理論密度比)を
99%以上確保し,高密度品になり,更に,焼結工程に
置ける汚染をなくし,高純度を確保した。That is, in the present invention, after the tungsten powder is pressed and sintered, hot rolling or forging of the primary working is performed to secure a relative density (ratio to the theoretical density) of 99% or more, thereby achieving a high density. It is a high-density product, and furthermore eliminates contamination in the sintering process and ensures high purity.
【0017】また,タングステンは,難加工材のため
に,圧延または,鍛造加工後の二次加工,例えば,切削
加工,穴開け加工に於て,クラックや割れが発生し易
く,二次加工が容易にできる硬度範囲と再結晶粒径の範
囲を究明し,二次加工に於けるトラブルを皆無にした。Tungsten is difficult to process, and therefore, it is easy for cracks and cracks to occur in secondary processing after rolling or forging, such as cutting and drilling. The range of hardness and the range of recrystallized grain size that can be easily obtained were clarified, and troubles in secondary processing were eliminated.
【0018】ここで,本発明においては,タングステン
精練の純化工程によって得られた高純度のタングステン
粉末をプレスし,焼結する際に,最初に真空雰囲気で1
400℃から1700℃の範囲で熱処理を行ってから,
1800℃から2100℃の焼結を行い,焼結体を製作
する。この真空雰囲気の熱処理は,焼結する際のタング
ステンの汚染防止のために行い,炉用耐熱レンガや保温
用耐火物を使用しない真空炉で,ヒータは,タングステ
ンヒータか,モリブデンヒータを使い,真空度は,1.
30×10-3Pa以上の真空度を確保する。焼結する前
に,この真空雰囲気の熱処理を行うことによって,プレ
ス体の密度を向上し,プレス体の気孔率が減少するため
に,焼結時の雰囲気からの汚染が少なくなる。Here, in the present invention, when pressing and sintering the high-purity tungsten powder obtained by the purification process of tungsten refining, first, the tungsten powder is placed in a vacuum atmosphere.
After performing heat treatment in the range of 400 ° C to 1700 ° C,
Sintering is performed at 1800 ° C. to 2100 ° C. to produce a sintered body. This heat treatment in a vacuum atmosphere is performed to prevent contamination of tungsten during sintering, and is a vacuum furnace that does not use heat-resistant bricks for furnaces or refractories for keeping heat. The heater is a tungsten heater or a molybdenum heater. The degree is 1.
A degree of vacuum of 30 × 10 −3 Pa or more is secured. By performing the heat treatment in the vacuum atmosphere before sintering, the density of the pressed body is improved and the porosity of the pressed body is reduced, so that contamination from the atmosphere during sintering is reduced.
【0019】次に,この焼結体を熱間圧延し,このとき
の圧延率を約73.0%以上行うことによって,相対密
度を99.0%以上を確保する。更に,熱処理によって
タングステン円板及び板の硬度をHv360から400
の範囲に軟化し,再結晶粒径を30μmから300μm
の範囲にしてから二次加工を行うことによって,二次加
工が容易にできることを可能にした。Next, the sintered body is hot-rolled, and the rolling ratio at this time is about 73.0% or more, thereby ensuring a relative density of 99.0% or more. Further, the hardness of the tungsten disk and the plate is increased from Hv 360 to 400 by heat treatment.
And the recrystallized grain size is from 30 μm to 300 μm.
By performing the secondary processing after setting the range, the secondary processing can be easily performed.
【0020】[0020]
【実施例】以下,本発明の実施例について,図面を参照
して説明する。Embodiments of the present invention will be described below with reference to the drawings.
【0021】タングステン精練の純化工程によって得ら
れた高純度のタングステン粉末を用いて,プレスし,焼
結する際に,最初に真空雰囲気で1400℃,1700
℃の2種類の温度で熱処理を行ってから,1800℃及
び2100℃の焼結を行い焼結体を製作した。また,真
空雰囲気の熱処理を行わない従来の焼結方法で,製作し
た焼結体を本発明品との比較品として用意した。When pressing and sintering using high-purity tungsten powder obtained by the purification process of tungsten refining, first, at 1400 ° C. and 1700 ° C. in a vacuum atmosphere.
After performing heat treatment at two different temperatures of 1 ° C., sintering was performed at 1800 ° C. and 2100 ° C. to produce a sintered body. Further, a sintered body manufactured by a conventional sintering method without performing heat treatment in a vacuum atmosphere was prepared as a comparative product with the product of the present invention.
【0022】本発明品及び比較品の粉末,焼結体のとき
の化学成分を分析し,その結果を下記の表1に示した。The chemical components of the powder of the present invention and the comparative product and the sintered body were analyzed, and the results are shown in Table 1 below.
【0023】[0023]
【表1】 [Table 1]
【0024】上記表1に示したように,本発明品は,焼
結時に於ける汚染がなく,従来の焼結方法で行った比較
品は,焼結のときに,Al,Si,Feが汚染されてい
る事がわかる。As shown in Table 1 above, the product of the present invention has no contamination at the time of sintering, and the comparative product obtained by the conventional sintering method has Al, Si and Fe at the time of sintering. You can see that it is contaminated.
【0025】これらの汚染物質は電気炉の断熱材,例え
ば,炉用耐熱レンガや保温用耐火物からの混入したもの
であると考えられる。そのため,真空雰囲気の熱処理
は,レンガ等の断熱材を使用しない電気炉で,ヒータ
は,タングステンヒータか,モリブデンヒータを使用
し,真空度は,1.30×10-3Pa以上の真空度を確
保し,雰囲気からの汚染を減少させた。本発明品は,こ
の熱処理を行うことによって,焼結前のプレス体の密度
が従来品よりも上がり,プレス体の気孔率が従来品より
も減少した。そのために,焼結時に於ける雰囲気からの
汚染が従来品よりも少ない焼結体が得られた。It is considered that these contaminants are mixed in from a heat insulating material of an electric furnace, for example, a heat-resistant brick for a furnace or a refractory for keeping heat. Therefore, the heat treatment in the vacuum atmosphere is performed by an electric furnace that does not use a heat insulating material such as a brick. The heater is a tungsten heater or a molybdenum heater, and the degree of vacuum is 1.30 × 10 −3 Pa or more. And reduced pollution from the atmosphere. By performing this heat treatment, the density of the pressed body before sintering of the product of the present invention was increased as compared with the conventional product, and the porosity of the pressed body was reduced as compared with the conventional product. Therefore, a sintered body with less contamination from the atmosphere during sintering than the conventional product was obtained.
【0026】次に,焼結体熱間圧延を行った。そのとき
の加工方法は,水素雰囲気の加熱炉にて1200℃及び
1500℃にて加熱し,1回の加熱で圧延機に1回通
し,その繰り返しを行って所定の圧延率を得た。各パス
毎の圧延率は,圧延前の板厚に対し圧延後約2mm減少
するように圧延した。このときの圧延率と比重との関係
を表2に示す。Next, hot rolling was performed on the sintered body. The working method at that time was heating at 1200 ° C. and 1500 ° C. in a heating furnace in a hydrogen atmosphere, passing through a rolling mill once by one heating, and repeating the process to obtain a predetermined rolling ratio. The rolling ratio for each pass was reduced so that the thickness before rolling was reduced by about 2 mm after rolling. Table 2 shows the relationship between the rolling ratio and the specific gravity at this time.
【0027】[0027]
【表2】 [Table 2]
【0028】表2で示す点をグラフにプロットして圧延
率が73.0%以上行えば,比重は,19.10以上を
確保できた。したがって,相対密度は,99.0%以上
確保できた。If the points shown in Table 2 were plotted on a graph and the rolling reduction was performed at 73.0% or more, the specific gravity could be secured at 19.10 or more. Therefore, the relative density was 99.0% or more.
【0029】更に,圧延後の板及び円板を熱処理によっ
て,Hv360から400の範囲内に軟化させた。この
ときの再結晶粒径は,30μmから300μmの均粒内
であった。2次焼結及び圧延後の熱処理による粒径及び
硬度を表3に示す。Further, the rolled plate and the circular plate were softened by heat treatment in the range of Hv 360 to 400. The recrystallized grain size at this time was within a uniform range of 30 μm to 300 μm. Table 3 shows the particle size and hardness by the heat treatment after the secondary sintering and the rolling.
【0030】[0030]
【表3】 [Table 3]
【0031】熱処理の条件は,圧延後の硬度によって熱
処理の温度を変えて上記の硬度範囲にした。この硬度範
囲にしたものとを比較して,二次加工を行ったところ,
前記したものは,二次加工が容易にできた。一方,後記
のものは,二次加工でクラックや欠けが発生した。な
お,ここで二次加工とは,旋盤加工,ワイヤーカット,
ウォータジェット加工,穴開け加工,平面研磨の事を呼
ぶ。The conditions of the heat treatment were set within the above hardness range by changing the temperature of the heat treatment depending on the hardness after rolling. When the secondary processing was performed in comparison with the hardness within this range,
In the above, secondary processing was easily performed. On the other hand, cracks and chippings occurred in the secondary processing of the later-mentioned ones. The secondary processing here means lathe processing, wire cutting,
It refers to water jet processing, drilling, and plane polishing.
【0032】また,1200℃における焼結体及び15
00℃における焼結体の面方位について測定した。その
結果を図1及び図2に示す。Further, the sintered body at 1200 ° C. and 15
00 was boss measurement attached to the plane orientation of the sintered body in ℃. The results are shown in FIGS.
【0033】図1は,1200℃による焼結体のX線回
折プロフィールで,各ピークのデータを表4に示す。FIG. 1 is an X-ray diffraction profile of the sintered body at 1200 ° C. Table 4 shows data of each peak.
【0034】[0034]
【表4】 [Table 4]
【0035】また,図2は1500℃による焼結体のX
線回折プロフィールで,各ピークのデータを表5に示
す。[0035] Further, X of the sintered body according to FIG. 2 1 5 00 ° C.
Table 5 shows the data of each peak in the line diffraction profile.
【0036】[0036]
【表5】 [Table 5]
【0037】下表6で示すJCPPSカードによる主要
回折面の強度比I/Io に対して,図1及び図2又は上
記表4及び表5で示す本発明品は同一でありランダム方
位(無配向)であることが判明した。The relative intensity ratio I / I o of the main diffraction surface by JCPPS card shown in Table 6 below, the present invention product shown in Figures 1 and 2 or Table 4 and Table 5 are the same random orientation (no Orientation).
【0038】[0038]
【表6】 [Table 6]
【0039】[0039]
【発明の効果】以上の説明から,本発明によれば,精練
技術によって得られた高純度のタングステン粉末を使用
して,製造したタングステン円板及び板は,高純度で,
高密度なものであり,スパッターターゲット用の材料品
質特性を満足し,圧延加工とその後二次加工に於けるト
ラブルを皆無にし,実用性のある低コストの材料を提供
することを可能にした。According to the present invention, according to the present invention, a tungsten disk and a plate manufactured by using a high-purity tungsten powder obtained by a scouring technique have a high purity.
It has a high density, satisfies the material quality characteristics for sputter targets, eliminates any troubles in rolling and subsequent secondary processing, and makes it possible to provide practical and low-cost materials.
【図1】1200℃において再加熱処理を行った本発明
の実施例に係るターゲット材のX線回折プロフィルを示
す図である。FIG. 1 is a view showing an X-ray diffraction profile of a target material according to an example of the present invention which has been subjected to a reheating treatment at 1200 ° C.
【図2】1500℃において再加熱処理を行った本発明
の実施例に係るターゲット材のX線回折プロフィルを示
す図である。2 is a diagram showing an X-ray diffraction profile of the target material according to an embodiment of the present invention conducted a reheating treatment in 1 5 00 ° C..
【図3】(a)は板厚方向へ結晶粒子の中心軸が配向し
た縦並びの状態を示す図である。(b)は板面方向へ結
晶粒子の中心軸が配向した縦並びの状態を示す図であ
る。FIG. 3A is a view showing a vertically aligned state in which central axes of crystal grains are oriented in a plate thickness direction. (B) is a diagram showing a vertically aligned state in which the central axes of the crystal grains are oriented in the plate surface direction.
Claims (3)
テン粒子を有するとともに,Hv 360〜400の範囲
内の硬度と,99.0%以上の相対密度とを有し,前記
タングステン粒子は,細長い結晶粒子からなり,且つ並
び方が長さ方向が板面に沿っている横並びであることを
特徴とするタングステンターゲット材。1. A rolled material of tungsten sintered compact, wherein the rolled material together with grain size having a tungsten particles 30 to 300 [mu] m, and hardness in the range of H v 360~400, 99.0 possess% or more and the relative density, the
Tungsten particles consist of elongated crystal grains and
A tungsten target material, wherein the length direction is side-by-side along the plate surface .
をプレスし焼結し,熱間圧延するタングステン焼結体の
圧延材の製造方法において, 焼結の際,真空雰囲気中で1400〜1700℃の範囲
で熱処理を行った後,1800℃以上で焼結を行う工程
と,さらに,圧延後, 1200〜1500℃の範囲で結晶粒
調整のための熱処理工程とを備えたことを特徴とするス
パッターターゲット材の製造方法。2. A method for producing a rolled material of a tungsten sintered body in which a tungsten powder is pressed, sintered and hot-rolled by powder metallurgy, wherein the sintering is performed in a vacuum atmosphere at a temperature of 1400 to 1700 ° C. After sintering at 1800 ° C or higher, and after rolling , crystal grains in the range of 1200 to 1500 ° C
A method for producing a sputter target material, comprising a heat treatment step for adjustment .
の製造方法において,前記熱間圧延は,加工度が73%
以上で行われ,該熱間圧延によって相対密度を99.0
%以上に上昇させることを特徴とするタングステンスパ
ッターターゲット材の製造方法。3. The method for manufacturing a sputter target material according to claim 2, wherein the hot rolling has a workability of 73%.
The hot rolling was performed to increase the relative density to 99.0.
% Of the tungsten sputter target material.
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JP5013072A JP2646058B2 (en) | 1993-01-29 | 1993-01-29 | Sputter target material and method for producing the same |
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JP5013072A JP2646058B2 (en) | 1993-01-29 | 1993-01-29 | Sputter target material and method for producing the same |
Publications (2)
Publication Number | Publication Date |
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JPH06220625A JPH06220625A (en) | 1994-08-09 |
JP2646058B2 true JP2646058B2 (en) | 1997-08-25 |
Family
ID=11822954
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JP5013072A Expired - Lifetime JP2646058B2 (en) | 1993-01-29 | 1993-01-29 | Sputter target material and method for producing the same |
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JP3721014B2 (en) * | 1999-09-28 | 2005-11-30 | 株式会社日鉱マテリアルズ | Method for manufacturing tungsten target for sputtering |
KR100764325B1 (en) * | 2000-09-07 | 2007-10-05 | 가부시끼가이샤 도시바 | Tungsten spattering target and method of manufacturing the target |
KR100734460B1 (en) | 2003-09-26 | 2007-07-03 | 가부시끼가이샤 도시바 | Sputtering target and process for producing si oxide film therewith |
JP7308013B2 (en) * | 2017-11-10 | 2023-07-13 | Jx金属株式会社 | Tungsten sputtering target and manufacturing method thereof |
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JP3280054B2 (en) * | 1992-02-10 | 2002-04-30 | 日立金属株式会社 | Method for manufacturing tungsten target for semiconductor |
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