JPH05148638A - Production of ito sputtering target - Google Patents
Production of ito sputtering targetInfo
- Publication number
- JPH05148638A JPH05148638A JP3336301A JP33630191A JPH05148638A JP H05148638 A JPH05148638 A JP H05148638A JP 3336301 A JP3336301 A JP 3336301A JP 33630191 A JP33630191 A JP 33630191A JP H05148638 A JPH05148638 A JP H05148638A
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- Prior art keywords
- sintering
- target
- ito
- density
- raw material
- Prior art date
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- Physical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、スパッタリングによ
ってＩＴＯ膜（Indium-Tin Oxide膜) を形成させる際に
使用する焼結タ−ゲットの製造方法に関するものであ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a sintered target used for forming an ITO film (Indium-Tin Oxide film) by sputtering.
【０００２】近年、「ＩＴＯ膜」と呼ばれているところ
の、“ｎ型導電性の半導体特性”を示す In2Ｏ3 ，SnＯ
2 酸化物膜の非常に高い導電性や可視光透過性（透明
性）に注目が集まり、液晶表示装置，薄膜エレクトロル
ミネッセンス表示装置，放射線検出素子，端末機器の透
明タブレット，窓ガラスの結露防止用発熱膜，帯電防止
膜或いは太陽光集熱器用選択透過膜等の多岐にわたる用
途に供されるようになってきた。In recent years, In 2 O 3 and SnO, which are called “ITO film” and exhibit “n-type conductive semiconductor characteristics”,
2 The attention has been paid to the extremely high conductivity and visible light transmissivity (transparency) of the oxide film, and it is used for liquid crystal display devices, thin film electroluminescence display devices, radiation detection elements, transparent tablets for terminal equipment, and dew condensation prevention on window glass. It has come to be used in a wide variety of applications such as a heat generating film, an antistatic film, and a selective permeation film for a solar collector.
【０００３】[0003]
【従来技術とその課題】このＩＴＯ膜は、化合物の熱分
解を利用したスプレイ法やＣＶＤ法等の化学的成膜法、
或いは真空蒸着法やスパッタリング法等の物理的成膜法
等によって形成することができるが、最近では、「大面
積で成膜することが可能でかつ低抵抗膜を再現性良く形
成できる」という利点が着目されたこともあって“スパ
ッタリング法”の採用が広まってきている。2. Description of the Related Art This ITO film is formed by a chemical film formation method such as a spray method or a CVD method utilizing thermal decomposition of a compound,
Alternatively, it can be formed by a physical film forming method such as a vacuum vapor deposition method or a sputtering method, but recently, an advantage that "a large area can be formed and a low resistance film can be formed with good reproducibility" Partly because of the attention paid to, the adoption of the "sputtering method" is spreading.
【０００４】ところで、スパッタリング法によってＩＴ
Ｏ膜を形成する場合には「酸化インジウムと酸化錫から
成るスパッタリングタ−ゲット（以降“ＩＴＯタ−ゲッ
ト”と略称する）」が使用されるが、このＩＴＯタ−ゲ
ットとしては、酸化インジウムと酸化錫の粉末混合体、
或いはこれにド−パントを添加した粉末混合体を常温で
プレス成形し、この成形体を大気中にて１２５０〜１６
５０℃で焼結してから更に機械加工を施したものが一般
に用いられてきた。By the way, by the sputtering method, IT
When forming an O film, a "sputtering target composed of indium oxide and tin oxide (hereinafter abbreviated as" ITO target ")" is used. As the ITO target, indium oxide and Tin oxide powder mixture,
Alternatively, a powder mixture obtained by adding dopant to the mixture is press-molded at room temperature, and the molded product is heated in the atmosphere at 1250 to 16
It has been generally used that it is sintered at 50 ° C. and then further machined.
【０００５】しかし、酸化インジウム粉末や酸化錫粉末
が非常に焼結性の悪い材料であることが影響してか、前
記方法 (コ−ルドプレス大気焼結法) で製造されたＩＴ
Ｏ焼結タ−ゲットには a) スパッタリングが進行するにつれて成膜速度の低下
が目立つ， b) スパッタ時にア−キングと呼ばれる異常放電が発生
し、成膜操作の安定性を害しがちである， c) タ−ゲット寿命が短い， d) スパッタリングが進行するにつれＩＴＯ特有の黒色
化が目立ち、比抵抗，エッチング特性，透過率等のＩＴ
Ｏ膜特性の劣化が顕著となる， 等の不都合が指摘される場合が多かった。However, probably because of the fact that the indium oxide powder and the tin oxide powder are materials having extremely poor sinterability, the IT manufactured by the above-mentioned method (cold press atmospheric sintering method).
In the O-sintered target, a) the deposition rate is conspicuously reduced as the sputtering progresses, b) abnormal discharge called arcing occurs during the sputtering, and the stability of the deposition operation tends to be impaired. c) Target life is short, d) Blackening peculiar to ITO is conspicuous as sputtering progresses, and IT such as resistivity, etching characteristics, transmittance, etc.
It was often pointed out that inconveniences such as the deterioration of O film characteristics became remarkable.
【０００６】そこで、前述した焼結タ−ゲットを製造す
るための一連の工程のうち、 "粉末原料の成形工程" に
ホットプレスを適用した手法（以降“ホットプレス法”
と称する）も実施されるようになったが、このホットプ
レス法で製造されたＩＴＯ焼結タ−ゲットであっても
“成膜速度が時間と共に低下する傾向”や“ア−キング
の発生傾向”にそれほど顕著な改善効果は見られないば
かりか、設備費，ランニングコスト，量産性に劣る等の
新たな製造上の問題が生じ、これらが結局はタ−ゲット
価格に影響することから、やはり工業的に十分満足でき
る手段とは言い難かった。Therefore, of the series of steps for manufacturing the above-mentioned sintered target, a method of applying hot pressing to the "molding step of powder raw material" (hereinafter referred to as "hot pressing method").
However, even with the ITO sintered target manufactured by this hot pressing method, the "deposition rate tends to decrease with time" and "the tendency of arcing". In addition to the notable improvement effect, there are new manufacturing problems such as equipment cost, running cost, poor mass productivity, etc., which eventually affect the target price. It was hard to say that it was an industrially satisfactory means.
【０００７】その上、前記何れの手法を採用した場合に
もＩＴＯ焼結タ−ゲットの製造時に割れが生じる傾向が
あり、特に成膜作業能率向上の点で有利な大型のＩＴＯ
焼結タ−ゲットを安定生産するには不満足なものであっ
た。In addition, when any of the above methods is adopted, cracks tend to occur at the time of manufacturing an ITO sintered target, and in particular, a large ITO which is advantageous in improving the film forming work efficiency.
It was unsatisfactory for stable production of the sintered target.
【０００８】このようなことから、本発明が目的とした
のは、スパッタリング作業中における成膜速度の低下や
ア−キング発生等による成膜操作の不安定化を懸念する
ことのない、均質で価格的にも有利な高品質ＩＴＯ焼結
タ−ゲットを安定に製造できる手段を確立することであ
った。In view of the above, the object of the present invention is to provide a uniform and uniform film without worrying about the instability of the film forming operation due to the decrease of the film forming rate during the sputtering operation or the occurrence of arcing. It was to establish means for stably producing a high quality ITO sintered target which is also advantageous in terms of price.
【０００９】[0009]
【課題を解決するための手段】そして、本発明者等は上
記目的を達成すべく数多くの実験を繰り返しながら鋭意
研究を行った結果、次のような知見を得ることができた
のである。The inventors of the present invention have obtained the following findings as a result of earnest research while repeating many experiments to achieve the above object.
【００１０】(A) 原料粉末の粒径（平均粒径）がＩＴ
Ｏ焼結タ−ゲット製造時における割れの発生に大きな影
響を及ぼしており、この粒径が特定の値以下とならない
ように原料調整を行えばＩＴＯ焼結タ−ゲット製造時の
割れ発生現象を効果的に抑えることができること，(A) The particle size (average particle size) of the raw material powder is IT
O has a great influence on the occurrence of cracks during the production of a sintered target, and if the raw materials are adjusted so that the grain size does not fall below a specific value, the phenomenon of the occurrence of cracks during the production of an ITO sintered target will occur. Can be effectively suppressed,
【００１１】(B) そして、原料粉末の粒径（平均粒
径）は一方でＩＴＯ焼結タ−ゲットの組成ムラや密度ム
ラにも大きく影響する因子であり、ＩＴＯ焼結タ−ゲッ
トの組成ムラや密度ムラが目立つようになるのは前記原
料粉末の粒径が或る特定の値を超えた範囲になった時で
あること，(B) The particle size (average particle size) of the raw material powder is also a factor that greatly affects the composition unevenness and density unevenness of the ITO sintered target, and the composition of the ITO sintered target is The unevenness and the density unevenness become noticeable when the particle diameter of the raw material powder is in a range exceeding a certain value,
【００１２】(C) また、ＩＴＯ焼結タ−ゲットのスパ
ッタ時における成膜速度や成膜速度・成膜操作安定性は
当該ＩＴＯ焼結タ−ゲットの組成ムラ，密度並びに密度
ムラと密接に関連しており、高い成膜速度や良好な成膜
速度・成膜操作安定性を確保するためには組成ムラ及び
密度ムラを抑えると同時に密度を高めることが必要であ
ること，(C) Further, the film formation rate, the film formation rate and the film formation operation stability during sputtering of the ITO sintered target are closely related to the composition unevenness, density and density unevenness of the ITO sintered target. It is related that it is necessary to suppress composition unevenness and density unevenness while at the same time increasing the density in order to secure high film forming speed, good film forming speed, and stability of film forming operation.
【００１３】(D) しかるに、ＩＴＯ焼結タ−ゲットの
製造に使用する原料粉末の粒径（平均粒径）を前記好ま
しい範囲に調整すると共に、得られる焼結タ−ゲットの
密度が特定値以上となるように図れば、成膜速度，成膜
速度・成膜操作安定性の著しい改善が可能となること，(D) However, the particle size (average particle size) of the raw material powder used for producing the ITO sintered target is adjusted to the above-mentioned preferable range, and the density of the obtained sintered target is set to a specific value. If the above is attempted, it is possible to significantly improve the deposition rate, the deposition rate, and the stability of the deposition operation.
【００１４】(E) 更に、ＩＴＯ焼結タ−ゲットの成膜
速度安定性や成膜操作の安定性等にはその密度が密接に
関連していることは上述した通りであるが、バルク抵抗
値もこれに深く係わっており、密度のほかにバルク抵抗
値も特定の領域に調整されたＩＴＯ焼結タ−ゲットでは
スパッタの進行に伴って成膜速度が顕著に低下する現象
が見られないばかりか、スパッタ時におけるア−キング
の発生が少なくなって成膜操作の安定性が格段に向上
し、高性能のＩＴＯ膜を能率良く安定して形成する上で
一層有利となること，(E) Further, as described above, the density is closely related to the film forming rate stability of the ITO sintered target and the stability of the film forming operation. The value is also closely related to this, and in the ITO sintered target in which the bulk resistance value is adjusted to a specific region in addition to the density, there is no phenomenon that the film formation rate significantly decreases with the progress of sputtering. In addition, the occurrence of arcing during sputtering is reduced, the stability of the film forming operation is significantly improved, and it is even more advantageous in efficiently and stably forming a high-performance ITO film.
【００１５】(F) また、従来の「コ−ルドプレス大気
焼結法」や「ホットプレス法」で前記“密度とバルク抵
抗値が特定の領域にあるＩＴＯ焼結タ−ゲット”を安定
して実現する場合には設備の大容量化等が必要である
が、“圧縮成形した酸化物粉末混合体の焼結”を１気圧
以上の高い酸素分圧雰囲気中で実施すれば、格別に大容
量設備を要することもなく上記ＩＴＯ焼結タ−ゲットの
実現が極めて容易となり、製造コストの著しい低減を図
ることも可能となる。しかも、このようにして得られた
焼結ＩＴＯタ−ゲットは、タ−ゲット寿命，スパッタリ
ングにより得られるＩＴＯ膜の性能等、何れを採っても
一段と優れたものとなり、“成膜速度", "膜特性の劣化
の改善" 並びに“成膜操作安定性”の面でも飛躍的な効
果を発揮すること。(F) In addition, the above-mentioned "ITO sintering target having a density and a bulk resistance value in a specific region" is stably stabilized by a conventional "cold press atmospheric sintering method" or "hot pressing method". In order to realize it, it is necessary to increase the capacity of the equipment, but if "sintering of the compression-molded oxide powder mixture" is carried out in an atmosphere with a high oxygen partial pressure of 1 atmosphere or more, the capacity will be extremely large. It becomes extremely easy to realize the above-mentioned ITO sintered target without requiring equipment, and it is possible to significantly reduce the manufacturing cost. Moreover, the sintered ITO target obtained in this way is much superior to the target life, the performance of the ITO film obtained by sputtering, and the like. It also has a dramatic effect in terms of "improvement of deterioration of film characteristics" and "stability of film forming operation".
【００１６】本発明は、上記知見事項等に基づいて完成
されたものであり、「酸化インジウムと酸化錫を主成分
とした原料から粉末冶金法によりＩＴＯタ−ゲットを製
造するに際して、 原料たる酸化インジウム粉末及び酸化
錫粉末として平均粒径が 0.1μｍを超え５μｍ以下のも
のを使用すると共に、 焼結を酸素含有雰囲気中、 更には
加圧酸素雰囲気中（１気圧を超える酸素分圧雰囲気中）
で実施し、 焼結後の密度Ｄ(g/cm3）を 5.50 ≦ Ｄ ≦ 7.23 なる式、或いは該密度Ｄ(g/cm3）とバルク抵抗値ρ(mΩ
cm）を (a) 5.50 ≦ Ｄ ≦ 7.23 ， (b) −0.0676Ｄ＋0.887 ≧ ρ ≧ −0.0761Ｄ＋0.66
6 なる２つの式で表される範囲に調整することにより、 高
い成膜速度，優れた成膜速度安定性，成膜操作安定性，
膜特性の安定性が確保されたＩＴＯ焼結タ−ゲットを割
れを生じたりすることなく安定に、 かつ安価に製造し得
るようにした点」に大きな特徴を有している。The present invention has been completed on the basis of the above-mentioned findings and the like. "When an ITO target is manufactured by a powder metallurgy method from a raw material containing indium oxide and tin oxide as main components, the oxidation as a raw material is performed. Use indium powder and tin oxide powder having an average particle size of more than 0.1 μm and 5 μm or less, and sinter them in an oxygen-containing atmosphere, and further in a pressurized oxygen atmosphere (in an oxygen partial pressure atmosphere exceeding 1 atm).
The density D (g / cm 3 ) after sintering is expressed as 5.50 ≤ D ≤ 7.23, or the density D (g / cm 3 ) and the bulk resistance value ρ (mΩ
cm) is (a) 5.50 ≤ D ≤ 7.23, (b) -0.0676D + 0.887 ≥ ρ ≥ -0.0761D + 0.66
By adjusting to the range expressed by the two equations of 6, high film formation rate, excellent film formation rate stability, film formation operation stability,
It has a major feature in that it is possible to manufacture an ITO sintered target with stable film characteristics stably and inexpensively without causing cracks. "
【００１７】ここで、本発明の条件が適用されるＩＴＯ
焼結タ−ゲットの基本的製造手法としては、従来の「コ
−ルドプレス焼結法」や「ホットプレス法」等の何れで
あっても良い。また、前記「酸素含有雰囲気」には大気
雰囲気や純酸素雰囲気も含まれることは言うまでもな
い。Here, ITO to which the conditions of the present invention are applied
The basic manufacturing method of the sintered target may be any of the conventional "cold press sintering method" and "hot pressing method". Needless to say, the “oxygen-containing atmosphere” includes an air atmosphere and a pure oxygen atmosphere.
【００１８】なお、本発明において、原料粉末の粒径，
タ−ゲットの“密度Ｄ”及び“バルク抵抗値ρ”を前記
の如き範囲に限定した理由は次の通りである。 [A] 原料粉末の粒径 原料粉末の粒径は、ＩＴＯ焼結タ−ゲットの製造性や組
成ムラ，密度，密度ムラ等を通じてその性能に大きな影
響を及ぼす因子である。そして、平均粒径で 0.1μｍ以
下の原料粉末は均質化という側面からは優れているもの
の、その調整に手間や暇がかかってコストアップとなる
ほか、タ−ゲット製造時に割れが発生しやすいという致
命的な問題を引き起こして実質的に大型のタ−ゲットを
製造することができない。一方、平均粒径が５μｍを超
える原料粉末を使用すると工業的な焼結条件では拡散が
十分に行われず、得られる焼結タ−ゲットは組成ムラや
密度ムラのある品質に劣るものとなってしまう。従っ
て、原料粉末の粒径は、平均粒径で 0.1μｍを超え５μ
ｍ以下と定めた。In the present invention, the particle size of the raw material powder,
The reason why the "density D" and "bulk resistance value ρ" of the target are limited to the above ranges is as follows. [A] Particle Diameter of Raw Material Powder The particle diameter of the raw material powder is a factor that greatly affects the performance of the ITO sintered target through manufacturability, composition unevenness, density, density unevenness, and the like. Although the raw material powder having an average particle size of 0.1 μm or less is excellent from the aspect of homogenization, it takes time and time to adjust the raw material powder, resulting in an increase in cost and cracking during target production. It is not possible to produce a substantially large target by causing a fatal problem. On the other hand, if a raw material powder having an average particle size of more than 5 μm is used, diffusion is not sufficiently performed under industrial sintering conditions, and the obtained sintered target is inferior in quality with composition unevenness and density unevenness. I will end up. Therefore, the average particle size of the raw material powder is more than 0.1 μm and 5 μm.
It was defined as m or less.
【００１９】[B] タ−ゲットの密度Ｄ及びバルク抵抗
値ρ ＩＴＯ焼結タ−ゲットの密度Ｄはスパッタ時の成膜速
度，成膜速度安定性，バルク抵抗値と密接に関連する
が、該密度が5.50g/cm3 を下回ると特に成膜速度安定性
が損なわれてスパッタの進行に伴い成膜速度が低下する
現象が目立つようになる。一方、7.23g/cm3 を上回る領
域にまでＩＴＯ焼結タ−ゲットの密度を上昇させること
は「酸素雰囲気中焼結法」によっても非常に困難で、コ
スト的な不利を招くことになる。従って、ＩＴＯ焼結タ
−ゲットの密度が5.50〜7.23g/cm3 となるように調整す
ることと定めた。なお、ＩＴＯ焼結タ−ゲットの密度調
整は、原料粉末の粒度，原料粉末のプレス成形条件，焼
結条件（焼結雰囲気，焼結温度等）を調整して行えば良
い。[B] Target density D and bulk resistance value ρ The density D of the ITO sintered target is closely related to the film formation rate during sputtering, the film formation rate stability, and the bulk resistance value. When the density is less than 5.50 g / cm 3 , the phenomenon in which the deposition rate stability is particularly impaired and the deposition rate decreases with the progress of sputtering becomes conspicuous. On the other hand, it is very difficult to increase the density of the ITO sintered target to a region exceeding 7.23 g / cm 3 even by the "oxygen atmosphere sintering method", which causes a cost disadvantage. Therefore, it was decided to adjust the density of the ITO sintered target to be 5.50 to 7.23 g / cm 3 . The density of the ITO sintered target may be adjusted by adjusting the particle size of the raw material powder, the press molding conditions of the raw material powder, and the sintering conditions (sintering atmosphere, sintering temperature, etc.).
【００２０】また、ＩＴＯ焼結タ−ゲットのバルク抵抗
値ρ(mΩcm）も成膜速度安定性や成膜操作安定性に影響
を及ぼす因子であるが、その値はＩＴＯ焼結タ−ゲット
の密度Ｄに大きく依存する傾向がある。そして、バルク
抵抗値は低いほどスパッタ時におけるア−キングの発生
が少ないので好ましいが、密度5.50〜7.23g/cm3 の領域
で ρ ＜ −0.0761Ｄ＋0.666 を達成することは「加圧酸素雰囲気中焼結法」によって
も非常に困難であり、一方、ＩＴＯ焼結タ−ゲットのバ
ルク抵抗値ρが ρ ＞ −0.0676Ｄ＋0.887 の領域になるとスパッタ時におけるア−キングの発生が
多くなって成膜操作の安定性が損なわれるばかりか、成
膜速度も不安定となってスパッタの進行に伴い成膜速度
が低下する現象が著しくなる傾向が見られる。従って、
必要によりＩＴＯ焼結タ−ゲットのバルク抵抗値ρ(mΩ
cm）を −0.0676Ｄ＋0.887 ≧ ρ ≧−0.0761Ｄ＋0.666 の範囲となるように調整することと定めた。なお、ＩＴ
Ｏ焼結タ−ゲットのバルク抵抗値ρの調整も、原料粉末
の粒度，原料粉末のプレス成形条件，焼結条件（焼結雰
囲気，焼結温度等）を調整して行えば良い。The bulk resistance value ρ (mΩcm) of the ITO sintered target is also a factor affecting the stability of the film forming rate and the stability of the film forming operation. The density D tends to be highly dependent. The lower the bulk resistance value, the less the occurrence of arcing during sputtering, which is preferable. However, achieving ρ <−0.0761D + 0.666 in the region of density 5.50 to 7.23 g / cm 3 means “pressurized oxygen atmosphere”. It is also very difficult to use the "intermediate sintering method". On the other hand, when the bulk resistance value ρ of the ITO sintered target is in the region of ρ> -0.0676D + 0.887, the occurrence of arcing during sputtering increases. Not only the stability of the film forming operation is impaired, but also the film forming rate becomes unstable and the phenomenon that the film forming rate decreases with the progress of sputtering tends to become remarkable. Therefore,
If necessary, the bulk resistance value ρ (mΩ of ITO sintered target)
cm) is adjusted to be in the range of −0.0676D + 0.887 ≧ ρ ≧ −0.0761D + 0.666. In addition, IT
The bulk resistance value ρ of the O-sintered target may be adjusted by adjusting the grain size of the raw material powder, the press molding conditions of the raw material powder, and the sintering conditions (sintering atmosphere, sintering temperature, etc.).
【００２１】続いて、本発明を実施例により比較例と対
比しながら更に具体的に説明する。Next, the present invention will be described more specifically by comparing the present invention with comparative examples.
【実施例】まず、原料粉末として表１に示した粒径（平
均粒径）の酸化インジウム粉と酸化錫粉とを準備し、重
量比で９０：１０となるように均一に混合してから成形
用のバインダ−を加え、これを金型（１６５W ×５２０
L ）へ均一に充填した。続いて、次の各手法に従ってＩ
ＴＯ焼結タ−ゲットを製造した。EXAMPLE First, as raw material powders, indium oxide powder and tin oxide powder having the particle diameters (average particle diameters) shown in Table 1 were prepared and uniformly mixed in a weight ratio of 90:10. A binder for molding is added, and this is put into a mold (165 W x 520 W).
L ) was evenly filled. Then, according to the following methods, I
A TO sintered target was manufactured.
【００２２】Ｉ. コ−ルドプレス大気焼結法 金型に充填した原料混合粉を油圧プレスにて１０００kg
/cm2の圧力で加圧してからこれを８０℃に加熱してバイ
ンダ−中の水分を蒸発させて乾燥し、次いで大気中にて
１６５０℃で９時間焼結する。次に、得られた焼結体の
表面を平面研削盤で削り、側辺をダイヤモンドカッタ−
で切断してタ−ゲット製品とする。I. Cold Press Air Sintering Method 1000 kg of raw material mixed powder filled in a die is pressed by a hydraulic press.
After pressurizing with a pressure of / cm 2 , this is heated to 80 ° C. to evaporate the water content in the binder and dried, and then sintered in air at 1650 ° C. for 9 hours. Next, the surface of the obtained sintered body was ground with a surface grinder, and the side edges were cut with a diamond cutter.
Cut to obtain a target product.
【００２３】II. コ−ルドプレス加圧酸素焼結法 金型に充填した原料混合粉を油圧プレスにて１０００kg
/cm2の圧力で加圧してからこれを８０℃に加熱してバイ
ンダ−中の水分を蒸発させて乾燥し、次いで加圧焼結炉
により２気圧（絶対圧）の純酸素ガス雰囲気中にて１６
５０℃で９時間焼結する。次に、得られた焼結体の表面
を平面研削盤で削り、更に側辺をダイヤモンドカッタ−
で切断してタ−ゲット製品とする。II. Cold Press Pressure Oxygen Sintering Method 1000 kg of raw material mixed powder filled in a die is pressed by a hydraulic press.
It is pressurized at a pressure of / cm 2 and then heated to 80 ° C. to evaporate the water content in the binder to dry it, and then in a pressure sintering furnace to a pure oxygen gas atmosphere of 2 atm (absolute pressure). 16
Sinter at 50 ° C. for 9 hours. Next, the surface of the obtained sintered body was ground with a surface grinder, and the side edges were diamond-cut.
Cut to obtain a target product.
【００２４】この時の「原料粉末平均粒径」，「タ−ゲ
ット製造中での割れ発生の有無」，「得られたＩＴＯ焼
結タ−ゲットの組成ムラの有無」及び「得られたＩＴＯ
焼結タ−ゲットの密度Ｄ及びバルク抵抗値ρ」を対比し
て表１に示す。At this time, "average particle size of raw material powder", "presence or absence of cracking during target production", "presence or absence of compositional unevenness of the obtained ITO sintered target" and "obtained ITO"
The density D and the bulk resistance value ρ of the sintered target are shown in Table 1 in comparison.
【００２５】[0025]
【表１】 [Table 1]
【００２６】表１に示される結果からも明らかなよう
に、「本発明法」によると割れを生じることもなく均質
組成のＩＴＯ焼結タ−ゲットが得られるのに対して、原
料粉末に特定の粒径調整をしなかった「比較法（従来
法）」では製造中に割れを発生したり、得られるＩＴＯ
焼結タ−ゲットに組成ムラを生じることが確認できる。As is clear from the results shown in Table 1, according to the "method of the present invention", an ITO sintered target having a homogeneous composition can be obtained without cracking, whereas the ITO powder is specified as a raw material powder. In the "comparative method (conventional method)" in which the particle size of
It can be confirmed that composition unevenness occurs in the sintered target.
【００２７】そして、上記各方法で得られたＩＴＯ焼結
タ−ゲットを用いてスパッタリング試験を行ったとこ
ろ、 「本発明法で得られたタ−ゲット」 の場合には何れ
も安定した操業下で性能の良好な（低抵抗の）透明ＩＴ
Ｏ膜が形成されたのに対して、「比較法で得られたタ−
ゲット」 を用いた場合には、何れもスパッタの進行につ
れて成膜速度が著しく低下する現象が見られたばかり
か、スパッタ時にア−キングが頻発して操業が不安定化
する傾向が認められた。Then, a sputtering test was conducted using the ITO sintered target obtained by each of the above-mentioned methods, and in the case of "target obtained by the method of the present invention", stable operation was observed. Transparent IT with good performance (low resistance)
Whereas the O film was formed, the “Temperature obtained by the comparison method was used.
When "Get" was used, not only was the phenomenon that the film formation rate significantly decreased with the progress of sputtering, but there was a tendency that arcing frequently occurred during sputtering and operation became unstable.
【００２８】[0028]
【効果の総括】以上に説明した如く、この発明によれ
ば、スパッタ性能の優れたＩＴＯ焼結タ−ゲットをコス
ト安く安定して製造することが可能となるなど、産業上
極めて有用な効果がもたらされる。[Summary of Effects] As described above, according to the present invention, it is possible to stably manufacture an ITO sintered target having excellent sputtering performance at a low cost. Be brought.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成４年１０月２７日[Submission date] October 27, 1992
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００２５[Name of item to be corrected] 0025
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００２５】[0025]
【表１】 [Table 1]
Claims (3)
原料から粉末冶金法によりＩＴＯスパッタリングタ−ゲ
ットを製造するに際して、原料たる酸化インジウム粉末
及び酸化錫粉末として平均粒径が 0.1μｍを超え５μｍ
以下のものを使用すると共に、焼結を酸素含有雰囲気中
で実施し、焼結後の密度Ｄ(g/cm3）を下記式で表される
範囲に調整することを特徴とする、ＩＴＯスパッタリン
グタ−ゲットの製造方法。 5.50 ≦ Ｄ ≦ 7.23 。1. When an ITO sputtering target is manufactured by a powder metallurgy method from raw materials mainly composed of indium oxide and tin oxide, the raw material of indium oxide powder and tin oxide powder has an average particle size of more than 0.1 μm and 5 μm.
ITO sputtering, characterized in that the following is used and sintering is carried out in an oxygen-containing atmosphere to adjust the density D (g / cm 3 ) after sintering to a range represented by the following formula: Target manufacturing method. 5.50 ≤ D ≤ 7.23.
原料から粉末冶金法によりＩＴＯスパッタリングタ−ゲ
ットを製造するに際して、原料たる酸化インジウム粉末
及び酸化錫粉末として平均粒径が 0.1μｍを超え５μｍ
以下のものを使用すると共に、焼結を酸素含有雰囲気中
で実施し、焼結後の密度Ｄ(g/cm3）とバルク抵抗値ρ(m
Ωcm）を下記２つの式で表される範囲に調整することを
特徴とする、ＩＴＯスパッタリングタ−ゲットの製造方
法。 (a) 5.50 ≦ Ｄ ≦ 7.23 ， (b) −0.0676Ｄ＋0.887 ≧ ρ ≧ −0.0761Ｄ＋0.66
6 。2. When an ITO sputtering target is manufactured by a powder metallurgy method from a raw material containing indium oxide and tin oxide as main components, the average particle diameter of the raw material of indium oxide powder and tin oxide powder is more than 0.1 μm and 5 μm.
In addition to using the following, sintering was carried out in an oxygen-containing atmosphere, and the density D (g / cm 3 ) and bulk resistance value ρ (m
Ωcm) is adjusted to a range represented by the following two equations, a method for producing an ITO sputtering target. (a) 5.50 ≤ D ≤ 7.23, (b) -0.0676D + 0.887 ≥ ρ ≥ -0.0761D + 0.66
6.
求項１又は２に記載のＩＴＯスパッタリングタ−ゲット
の製造方法。3. The method for producing an ITO sputtering target according to claim 1, wherein the sintering is performed in a pressurized oxygen atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3336301A JPH05148638A (en) | 1991-11-26 | 1991-11-26 | Production of ito sputtering target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3336301A JPH05148638A (en) | 1991-11-26 | 1991-11-26 | Production of ito sputtering target |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05148638A true JPH05148638A (en) | 1993-06-15 |
Family
ID=18297695
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3336301A Pending JPH05148638A (en) | 1991-11-26 | 1991-11-26 | Production of ito sputtering target |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05148638A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5401701A (en) * | 1992-08-19 | 1995-03-28 | Tosoh Corporation | Ito sintered body and method of manufacturing the same |
| US6051166A (en) * | 1995-12-06 | 2000-04-18 | Sumitomo Chemical Corporation, Limited | Indium oxide-tin oxide powders and method for producing the same |
| US6099982A (en) * | 1996-11-08 | 2000-08-08 | Dowa Mining Co., Ltd. | Starting powders for ITO production, ITO sinters and processes for producing such starting powders and ITO sinters |
| WO2007058318A1 (en) * | 2005-11-21 | 2007-05-24 | Idemitsu Kosan Co., Ltd. | Fired material and process for producing the same |
| JP2007254282A (en) * | 1995-04-18 | 2007-10-04 | Tosoh Corp | Process of preparing sintered ito compact |
| US9279178B2 (en) | 2007-04-27 | 2016-03-08 | Honeywell International Inc. | Manufacturing design and processing methods and apparatus for sputtering targets |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02297813A (en) * | 1989-02-28 | 1990-12-10 | Tosoh Corp | Sintered body of oxide, manufacture thereof, and target using same |
| JPH02297812A (en) * | 1989-02-28 | 1990-12-10 | Tosoh Corp | Sintered body of oxide, manufacture thereof, and target using same |
| JPH03207858A (en) * | 1990-01-08 | 1991-09-11 | Nippon Mining Co Ltd | Production of ito sputtering target |
-
1991
- 1991-11-26 JP JP3336301A patent/JPH05148638A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02297813A (en) * | 1989-02-28 | 1990-12-10 | Tosoh Corp | Sintered body of oxide, manufacture thereof, and target using same |
| JPH02297812A (en) * | 1989-02-28 | 1990-12-10 | Tosoh Corp | Sintered body of oxide, manufacture thereof, and target using same |
| JPH03207858A (en) * | 1990-01-08 | 1991-09-11 | Nippon Mining Co Ltd | Production of ito sputtering target |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5401701A (en) * | 1992-08-19 | 1995-03-28 | Tosoh Corporation | Ito sintered body and method of manufacturing the same |
| JP2007254282A (en) * | 1995-04-18 | 2007-10-04 | Tosoh Corp | Process of preparing sintered ito compact |
| US6051166A (en) * | 1995-12-06 | 2000-04-18 | Sumitomo Chemical Corporation, Limited | Indium oxide-tin oxide powders and method for producing the same |
| US6099982A (en) * | 1996-11-08 | 2000-08-08 | Dowa Mining Co., Ltd. | Starting powders for ITO production, ITO sinters and processes for producing such starting powders and ITO sinters |
| WO2007058318A1 (en) * | 2005-11-21 | 2007-05-24 | Idemitsu Kosan Co., Ltd. | Fired material and process for producing the same |
| US9279178B2 (en) | 2007-04-27 | 2016-03-08 | Honeywell International Inc. | Manufacturing design and processing methods and apparatus for sputtering targets |
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