JP2009227513A - Method for manufacturing titanium oxide target having high density and low specific resistance - Google Patents
Method for manufacturing titanium oxide target having high density and low specific resistance Download PDFInfo
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Abstract
Description
この発明は、高密度でかつ比抵抗の小さい酸化チタンターゲットの製造方法に関するものである。 The present invention relates to a method for manufacturing a titanium oxide target having a high density and a small specific resistance.
一般に、酸化チタン膜は、高屈折率膜として知られているが、その他光触媒膜、透明導電膜などとして使用されるほか、多層膜の一部の反射防止コート膜、反射増加コート膜、干渉フィルター、偏光膜などとして使用されることが知られており、この酸化チタン膜は金属チタンターゲットを用い、酸素を含む雰囲気中でDCスパッタすることにより成膜することが知られている。しかし、この方法で二酸化チタン膜を成膜すると、成膜速度が極めて遅いために生産性が悪く、したがってコストが高くつく。 In general, the titanium oxide film is known as a high refractive index film. In addition to being used as a photocatalyst film, a transparent conductive film, etc., a part of the antireflection coating film, the reflection increasing coating film, and the interference filter of the multilayer film are used. The titanium oxide film is known to be formed by DC sputtering in an atmosphere containing oxygen using a metal titanium target. However, when a titanium dioxide film is formed by this method, the film formation rate is extremely slow, resulting in poor productivity and high cost.
これを解決するために、TiOx(1<X<2)の成分組成を有する酸化物焼結体からなり、室温での比抵抗値:10Ωcm以上、酸素含有量:35質量%以上のターゲットを作製し、このターゲットを用いてアルゴンと酸素の混合ガス雰囲気中でDC(直流)スパッタすることにより酸化チタン膜を成膜する方法が提案されている。そして、前記TiOx(1<X<2)の成分組成を有する酸化物焼結体からなるターゲットを製造するには、粒径:0.05〜40μmを有する二酸化チタン粉末をカーボンモールドに充填し、温度:1100〜1400℃を保持しながら非酸化性雰囲気中でホットプレスすることにより作製することができるとされている(特許文献1参照)。
しかし、二酸化チタン粉末を非酸化性雰囲気中でホットプレスすることにより作製したTiOx(1<X<2)の成分組成を有する酸化物焼結体からなる従来のターゲットは十分な密度が得られず、さらにDCスパッタする際にターゲットに割れが頻発するという問題点があった。 However, a conventional target made of an oxide sintered body having a component composition of TiOx (1 <X <2) produced by hot pressing titanium dioxide powder in a non-oxidizing atmosphere cannot obtain a sufficient density. In addition, there is a problem that cracks frequently occur in the target during DC sputtering.
そこで、本発明者らはこれら問題点を解決すべく研究を行った。
その結果、原料粉末としてTi2O3粉末およびTiO2粉末を用意し、これら原料粉末を、Ti2O3粉末:1〜20質量%、残部:TiO2粉末となるように配合し混合して得られた混合粉末をカーボンモールドに充填し、不活性ガス雰囲気中、温度:1100〜1300℃、圧力:10〜50MPaでホットプレスすることにより得られた酸化チタンターゲットは、従来の方法で得られた酸化チタンターゲットに比べて高密度となり、さらにDCスパッタに際して割れが発生することが無いと言う、研究結果が得られたのである。
Therefore, the present inventors have studied to solve these problems.
As a result, Ti 2 O 3 powder and TiO 2 powder were prepared as raw material powders, and these raw material powders were blended and mixed so that Ti 2 O 3 powder: 1 to 20% by mass, and the balance: TiO 2 powder. The obtained mixed powder is filled into a carbon mold, and a titanium oxide target obtained by hot pressing in an inert gas atmosphere at a temperature of 1100 to 1300 ° C. and a pressure of 10 to 50 MPa is obtained by a conventional method. Research results have been obtained that the density is higher than that of the titanium oxide target and that no cracking occurs during DC sputtering.
この発明は、かかる研究結果に基づいて成されたものであって、
(1)原料粉末としてTi2O3粉末およびTiO2粉末を用意し、これら原料粉末を、Ti2O3粉末:1〜20質量%、残部:TiO2粉末となるように配合し混合して得られた混合粉末をカーボンモールドに充填し、不活性ガス雰囲気中でホットプレスする酸化チタンターゲットの製造方法、
(2)前記ホットプレスは、温度:1100〜1300℃、圧力:10〜50MPaで行う前記(1)記載のホットプレスする酸化チタンターゲットの製造方法、に特徴を有するものである。
The present invention has been made based on such research results,
(1) Prepare Ti 2 O 3 powder and TiO 2 powder as raw material powders, mix and mix these raw material powders so as to be Ti 2 O 3 powder: 1 to 20% by mass and the rest: TiO 2 powder. Filling the obtained mixed powder into a carbon mold and hot pressing in an inert gas atmosphere, a method for producing a titanium oxide target,
(2) The hot press is characterized by the method for producing a titanium oxide target to be hot-pressed according to (1) described above, which is performed at a temperature of 1100 to 1300 ° C. and a pressure of 10 to 50 MPa.
この発明の酸化チタンターゲットの製造方法は、原料粉末としてTiO2粉末にTi2O3粉末を配合し混合した混合粉末を使用することに特徴を有するものであり、原料粉末として一部Ti2O3粉末をTiO2粉末に添加し混合して得られた混合粉末を使用してホットプレスを行うことにより酸化チタンターゲットの密度が向上し、さらにDCスパッタに際して割れが発生することが無いとう効果を奏するものである。 Method for producing a titanium oxide target of the present invention are those characterized in the use of mixed powder mixed blended Ti 2 O 3 powder to TiO 2 powder as the raw material powder, some Ti 2 O as the raw material powder The density of the titanium oxide target is improved by performing hot pressing using a mixed powder obtained by adding 3 powders to TiO 2 powder and mixing, and further, there is an effect that no cracks are generated during DC sputtering. It is what you play.
原料粉末として一部Ti2O3粉末をTiO2粉末に添加し混合して得られた混合粉末を使用してホットプレスを行うこの発明の方法により作製した酸化チタンターゲットが、原料粉末としてTiO2粉末のみを使用する従来の酸化チタンターゲットの製造方法により作製した酸化チタンターゲットと比較して高密度となり、さらにDCスパッタに際して割れが発生することが無くなる理由は、ホットプレス中にTi2O3とTiO2が反応して導電性の優れたTi9O17酸化物がターゲット全体にわたって均一に生成し、そのためにターゲットの面内および厚み方向の部分的な抵抗差が少なくなってターゲット全体にわたって均一な比抵抗を有するようになり、DCスパッタ中にターゲットに不均一な歪が発生することがないことによるものと考えられる。 A titanium oxide target produced by the method of the present invention in which hot pressing is performed using a mixed powder obtained by adding and mixing a part of Ti 2 O 3 powder to TiO 2 powder as raw material powder, and TiO 2 as raw material powder. The reason why the density becomes higher than that of a titanium oxide target produced by a conventional method of producing a titanium oxide target using only powder, and cracks are not generated during DC sputtering is that Ti 2 O 3 and TiO 2 reacts and Ti 9 O 17 oxide having excellent conductivity is uniformly generated over the entire target. Therefore, the partial resistance difference in the in-plane and thickness direction of the target is reduced, and the entire target is uniform. It has a specific resistance so that non-uniform distortion is not generated on the target during DC sputtering. It is considered to be due.
この発明の製造方法により得られた酸化チタンターゲットは、酸素を含む不活性ガス雰囲気中で通常の条件でDCスパッタを行うことにより従来と同じ優れたTiO2膜を成膜することができる。 The titanium oxide target obtained by the manufacturing method of the present invention can form the same excellent TiO 2 film as conventional by performing DC sputtering in an inert gas atmosphere containing oxygen under normal conditions.
この発明の酸化チタンターゲットを製造する際に使用する混合粉末におけるTi2O3粉末の配合量を1〜20質量%に限定した理由は、Ti2O3粉末の配合量が1質量%未満では、ターゲットの密度が低くなり、さらにDCスパッタ中に割れが発生するので好ましくなく、一方、20質量%を越えて添加すると、ターゲット中に含まれる酸素の量が少なくなってDCスパッタを成膜することにより得られたスパッタ膜の透明性が損なわれるようになるので好ましくないからである。
また、この発明の酸化チタンターゲットの製造方法を実施するためのホットプレス条件は特に限定されるものではないが、ホットプレス温度は通常の1100〜1300℃で行うことが好ましく、さらに圧力は高圧であるほど好ましいので、10MPa以上であることが好ましいが、装置の関係でその上限を50MPa以下に定めた。
The reason why the amount of Ti 2 O 3 powder in the mixed powder used when producing the titanium oxide target of the present invention is limited to 1 to 20% by mass is that the amount of Ti 2 O 3 powder is less than 1% by mass. The density of the target is low, and cracks are generated during DC sputtering, which is not preferable. On the other hand, when the content exceeds 20% by mass, the amount of oxygen contained in the target is reduced to form a DC sputtering film. This is because the transparency of the resulting sputtered film is impaired.
The hot press conditions for carrying out the method for producing a titanium oxide target of the present invention are not particularly limited, but the hot press temperature is preferably 1100 to 1300 ° C., and the pressure is high. Since it is more preferable, the pressure is preferably 10 MPa or more, but the upper limit is set to 50 MPa or less because of the apparatus.
この発明の製造方法によると、従来よりも一層高密度でDCスパッタに際して割れが発生することのない酸化チタンターゲットを得ることができ、この発明の製造方法により作製した酸化チタンターゲットを用いると、一層効率よくDCスパッタを行うことができる。 According to the manufacturing method of the present invention, it is possible to obtain a titanium oxide target that has a higher density than before and does not generate cracks during DC sputtering. When the titanium oxide target produced by the manufacturing method of the present invention is used, DC sputtering can be performed efficiently.
つぎに、この発明の酸化チタンターゲットの製造方法を実施例により具体的に説明する。
原料粉末として、いずれも平均粒径:2μmを有する市販のTiO2粉末およびTi2O3粉末を用意した。
これら原料粉末を表1に示される配合組成となるように秤量し、ジルコニアボールミルで12時間乾式混合した後、得られた混合粉末をカーボンモールドに充填し、表1に示される雰囲気、温度および圧力で表1に示される時間保持することにより直径:160mm×厚さ:7mmの寸法を有するホットプレス体を作製し、このホットプレス体を切削加工し、いずれも直径:152.4mm×厚さ:5mmの寸法をもったターゲットを作製することにより本発明法1〜8および比較法1〜3を実施した。
Next, the production method of the titanium oxide target of the present invention will be specifically described with reference to examples.
As raw material powders, commercially available TiO 2 powder and Ti 2 O 3 powder each having an average particle diameter of 2 μm were prepared.
These raw material powders are weighed so as to have the composition shown in Table 1, and after dry mixing with a zirconia ball mill for 12 hours, the obtained mixed powder is filled into a carbon mold, and the atmosphere, temperature and pressure shown in Table 1 are obtained. The hot press body having the dimensions of diameter: 160 mm × thickness: 7 mm was prepared by holding for the time shown in Table 1, and this hot press body was cut, and both diameters: 152.4 mm × thickness: Invention methods 1 to 8 and comparative methods 1 to 3 were carried out by producing a target having a dimension of 5 mm.
さらに、TiO2粉末のみをカーボンモールドに充填し、表1に示される雰囲気、温度および圧力で表1に示される時間保持することによりホットプレス体を作製し、このホットプレス体を切削加工し、いずれも直径:154mm×厚さ:5mmの寸法をもったターゲットを作製することにより従来法を実施した。 Furthermore, only a TiO 2 powder is filled in a carbon mold, and a hot press body is produced by holding the atmosphere, temperature and pressure shown in Table 1 for the time shown in Table 1, and the hot press body is cut. In either case, the conventional method was carried out by producing a target having a dimension of diameter: 154 mm × thickness: 5 mm.
本発明法1〜8、比較法1〜3および従来法で得られたターゲットの密度を測定し、さらにこれらターゲットを銅製バッキングプレートに半田を用いて接着し、パルスDCスパッタ装置を用い、投入電力:3kWとし、5分間スパッタしたのち1分間休止する操作を10回繰り返すことにより10サイクルスパッタテストを行い、ターゲット表面に割れが発生しているか否かを目視にて確認し、その結果を表1に示した。 The density of the targets obtained by the present invention methods 1 to 8, comparative methods 1 to 3 and the conventional method was measured, and these targets were further bonded to a copper backing plate using solder, and a pulse DC sputtering apparatus was used to input power. : 3 kW, sputtering for 5 minutes and then stopping for 1 minute was repeated 10 times to perform a 10-cycle sputtering test, and whether or not cracking occurred on the target surface was visually confirmed. The results are shown in Table 1. It was shown to.
表1に示される結果から、本発明法1〜8で作製したターゲットは、従来法で作製したターゲットに比べて高密度を有し、さらに10サイクルスパッタテスト後のターゲットに割れが発生することが無いことから、DCスパッタ用ターゲットとして優れた特性を有することがわかる。また、この発明から外れた条件の比較法1〜3で得られたターゲットは好ましくない特性が現れることが分かる。 From the results shown in Table 1, the target produced by the present invention methods 1 to 8 has a higher density than the target produced by the conventional method, and cracks may occur in the target after the 10-cycle sputtering test. Since it does not exist, it turns out that it has the characteristic outstanding as a target for DC sputtering. In addition, it can be seen that the target obtained by Comparative Methods 1 to 3 under conditions deviating from the present invention exhibits undesirable characteristics.
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