JP2000281431A - Tin dioxide-based sintered compact, material for thin film formation and electroconductive film - Google Patents
Tin dioxide-based sintered compact, material for thin film formation and electroconductive filmInfo
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- JP2000281431A JP2000281431A JP9016199A JP9016199A JP2000281431A JP 2000281431 A JP2000281431 A JP 2000281431A JP 9016199 A JP9016199 A JP 9016199A JP 9016199 A JP9016199 A JP 9016199A JP 2000281431 A JP2000281431 A JP 2000281431A
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- Japan
- Prior art keywords
- sno
- less
- sintered body
- specific resistance
- transparent conductive
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、スパッタリングタ
ーゲットなどの薄膜形成用材料に関し、特にプラズマデ
ィスプレイパネル（ＰＤＰ）やタッチパネル等の透明導
電膜の形成に使用するスパッタリングターゲットに好適
なＳｎＯ2（酸化錫）系焼結体、薄膜形成用材料および
これによって形成された透明導電膜に関するものであ
る。The present invention relates to a material for forming a thin film such as a sputtering target, and more particularly to SnO 2 (tin oxide) suitable for a sputtering target used for forming a transparent conductive film such as a plasma display panel (PDP) or a touch panel. The present invention relates to a sintered body, a material for forming a thin film, and a transparent conductive film formed thereby.
【０００２】ここで、ＳｎＯ2系焼結体とは、ＳｎＯ2を
８０重量％以上、好ましくは９４重量％以上ならびに不
可避的不純物を含む化合物からなる焼結体をいう。Here, the SnO 2 -based sintered body refers to a sintered body composed of a compound containing 80% by weight or more, preferably 94% by weight or more of SnO 2 and an unavoidable impurity.
【０００３】[0003]
【従来の技術】近年、液晶ディスプレイ（ＬＣＤ）に代
わる表示デバイスとして、プラズマディスプレイパネル
（ＰＤＰ）が注目されている。ＰＤＰはＬＣＤに比べ
て、バックライトを要しないため、表示装置をより薄く
形成することができる等の利点を有しており、壁掛けＴ
Ｖ等への応用が期待されている。2. Description of the Related Art In recent years, a plasma display panel (PDP) has attracted attention as a display device replacing a liquid crystal display (LCD). PDPs do not require a backlight as compared with LCDs, and thus have the advantage that a display device can be formed thinner.
Application to V and the like is expected.
【０００４】ＰＤＰには、ＬＣＤと同様、透明電極が必
要不可欠であり、ＩＴＯ（酸化インジウム−酸化錫）膜
やＳｎＯ2系透明導電膜がこれに用いられている。ＩＴ
Ｏ膜は、低抵抗でエッチング特性にもすぐれているが、
高価であり、またＰＤＰ製造プロセス上、耐熱性や耐薬
品性において問題がある。一方、ＳｎＯ2系薄膜は、抵
抗値の点ではＩＴＯ膜に劣るものの、比較的安価であ
り、耐熱性や耐薬品性にもすぐれているという利点を有
している。A transparent electrode is indispensable for a PDP, like an LCD, and an ITO (indium oxide-tin oxide) film or a SnO 2 -based transparent conductive film is used for this. IT
The O film has low resistance and excellent etching characteristics,
It is expensive and has a problem in heat resistance and chemical resistance in the PDP manufacturing process. On the other hand, the SnO 2 -based thin film is relatively inexpensive and has excellent heat resistance and chemical resistance, although it is inferior to an ITO film in terms of resistance value.
【０００５】従来、ＳｎＯ2系焼結体においては、Ｓｎ
Ｏ2薄膜の抵抗値を下げるために酸化第一アンチモン
（Ｓｂ2Ｏ3）を添加することが行われている。このよう
なＳｂ2Ｏ3が添加されたＳｎＯ2焼結体からなるスパッ
タリングターゲットを製造するためには、ホットプレス
（ＨＰ）法が一般に用いられている。ホットプレス法に
おいては、圧力をかけながら焼結を行うため、焼成密度
や強度をある程度向上させる上では有利であるものの、
装置上の制限から大型の焼結体を得ることは容易ではな
い。したがって、従来、大型のスパッタリングターゲッ
トを作製する場合、複数の焼結体を張り合わせてターゲ
ットを構成することが一般に行われている。しかしなが
ら、複数の継ぎ目を有するターゲットを使用してスパッ
タリングによりＳｎＯ2薄膜を形成する場合において
は、継ぎ目からアーキングやノジュールが発生し、安定
な成膜を行うことができないという問題がある。したが
って、継ぎ目のないターゲットやより継ぎ目の少ないタ
ーゲットが要請されていることから、より大型の焼結体
を製造する技術が求められている。Conventionally, in a SnO 2 -based sintered body, Sn
Addition of antimony oxide (Sb 2 O 3 ) has been performed to reduce the resistance value of the O 2 thin film. In order to manufacture such a sputtering target made of a SnO 2 sintered body to which Sb 2 O 3 is added, a hot press (HP) method is generally used. In the hot press method, since sintering is performed while applying pressure, although it is advantageous in improving the firing density and strength to some extent,
It is not easy to obtain a large sintered body due to limitations on the apparatus. Therefore, conventionally, when manufacturing a large-sized sputtering target, it is generally performed to form a target by laminating a plurality of sintered bodies. However, when a SnO 2 thin film is formed by sputtering using a target having a plurality of joints, arcing and nodules are generated from the joints, and there is a problem that stable film formation cannot be performed. Therefore, since a seamless target and a target having a smaller number of joints are required, a technique for manufacturing a larger sintered body is required.
【０００６】大型の焼結体を製造する方法としては、原
料混合粉末をプレス成形して得た成形体を焼結するコー
ルドプレス（ＣＰ）法や、原料混合粉末を鋳込み成形し
て得た成形体を焼結する鋳込み法がある。[0006] As a method for producing a large-sized sintered body, a cold press (CP) method for sintering a compact obtained by press-molding a raw material mixed powder or a molding method obtained by casting a raw material mixed powder is cast. There is a casting method for sintering the body.
【０００７】ところで、ＳｎＯ2系透明導電膜に要求さ
れる特性は、一般に、ＳｎＯ2系透明導電膜の比抵抗が
０．１Ω・ｃｍ以下、膜厚１０００オングストロームに
おける波長５５０ｎｍの光の透過率が８０％以上であ
る。上述したように、Ｓｂ2Ｏ3が添加されたＳｎＯ2薄
膜は、Ｓｂ2Ｏ3が均一に添加されたＳｎＯ2ターゲット
をスパッタリングすることにより成膜される。このよう
にして成膜されたＳｂ2Ｏ3が添加されたＳｎＯ2薄膜は
比抵抗のオーダーが１０-3Ω・ｃｍ、膜厚１０００オン
グストロームにおける波長５５０ｎｍの光の透過率が９
０％程度であり、ＳｎＯ2系透明導電膜に要求される特
性を満足している。By the way, characteristics required for SnO 2 based transparent conductive film is generally less resistivity 0.1 [Omega · cm of SnO 2 based transparent conductive film, the transmittance of the light having the wavelength 550nm in thickness 1000 Å 80% or more. As described above, the SnO 2 thin film to which Sb 2 O 3 is added is formed by sputtering the SnO 2 target to which Sb 2 O 3 is uniformly added. The Sb 2 O 3 -added SnO 2 thin film thus formed has an order of specific resistance of 10 −3 Ω · cm and a transmittance of light of 550 nm wavelength of 550 nm at a thickness of 1000 Å.
This is about 0%, which satisfies the characteristics required for the SnO 2 -based transparent conductive film.
【０００８】しかしながら、Ｓｂ2Ｏ3が添加されたＳｎ
Ｏ2ターゲットを作製する場合、Ｓｂ2Ｏ3が約１０００
℃前後の温度で、大気中、酸素雰囲気中、不活性ガス中
あるいは真空中など一般的な雰囲気条件において溶融す
るため、少なくとも１０００℃以下の温度で熱処理する
必要がある。したがって、ＣＰ法または鋳込み法によっ
て焼結体を焼成する場合は、このように焼成温度に制限
があるため、焼結が十分に進行せず、焼結が不十分な脆
い焼結体しか得ることができないという問題がある。こ
のような脆さを有する焼結体を用いてスパッタリングタ
ーゲットを作製する場合にあっては、その加工中に加工
応力によって焼結体に割れや亀裂が生じたり、あるいは
バッキングプレートへ焼結体をボンディングする際の熱
応力によって割れが生じるという問題がある。このよう
な割れが生じる傾向は、ターゲットの寸法が大型化する
に従って顕著となる。However, Sn added with Sb 2 O 3
When producing an O 2 target, Sb 2 O 3 is about 1000
It is necessary to heat-treat at a temperature of at least 1000 ° C. at about a temperature of about 100 ° C. because it melts under general atmospheric conditions such as the atmosphere, an oxygen atmosphere, an inert gas or a vacuum. Therefore, when sintering the sintered body by the CP method or the casting method, since the sintering temperature is limited as described above, sintering does not sufficiently proceed, and only a brittle sintered body with insufficient sintering is obtained. There is a problem that can not be. When a sputtering target is manufactured using a sintered body having such brittleness, cracks or cracks are generated in the sintered body due to processing stress during the processing, or the sintered body is placed on a backing plate. There is a problem that cracks occur due to thermal stress during bonding. The tendency for such cracks to occur becomes more pronounced as the size of the target increases.
【０００９】したがって、高温での焼結、たとえば１３
００℃以上、好ましくは１４５０℃以上での高温での焼
結が可能なＳｂ2Ｏ3に代わる添加剤が求められている。Accordingly, sintering at a high temperature, for example, 13
There is a need for an alternative to Sb 2 O 3 that can be sintered at high temperatures above 00 ° C., preferably above 1450 ° C.
【００１０】[0010]
【発明が解決しようとする課題】本発明は、上述した従
来技術の問題点に鑑みてなされたものであり、比較的大
型の焼結体を製造することのできるＣＰ法、鋳込み法に
より作製が可能であり、しかも１３００℃以上の高温条
件で焼結することができる、組成のばらつきのなく、か
つ、比抵抗が１×１０7Ω・ｃｍ以下のＳｎＯ2系焼結体
からなる薄膜形成用材料を提供することを目的としてい
る。SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned problems of the prior art, and is manufactured by a CP method or a casting method capable of manufacturing a relatively large sintered body. For forming a thin film made of a SnO 2 -based sintered body having a specific resistance of 1 × 10 7 Ω · cm or less, which can be sintered under a high temperature condition of 1300 ° C. or more and has no variation in composition. It is intended to provide materials.
【００１１】[0011]
【課題を解決するための手段】本発明によるＳｎＯ2系
焼結体は、Ａｌ、Ｓｉ、Ｎｂ、ＴａおよびＹからなる群
から選ばれた少なくとも１種を含有し、その添加量の合
計が酸化物換算で２０重量％以下であり、かつ、比抵抗
が１×１０7Ω・ｃｍ以下であることを特徴とするもの
である。The SnO 2 -based sintered body according to the present invention contains at least one selected from the group consisting of Al, Si, Nb, Ta and Y, and the total amount of the addition is oxidized. It is characterized by being 20% by weight or less in terms of material and having a specific resistance of 1 × 10 7 Ω · cm or less.
【００１２】さらに本発明によるＳｎＯ2系薄膜形成用
材料は、Ａｌ、Ｓｉ、Ｎｂ、ＴａおよびＹからなる群か
ら選ばれた少なくとも１種を含有し、その添加量の合計
が酸化物換算で２０重量％以下であるＳｎＯ2系混合粉
末を成形し、大気雰囲気または酸素雰囲気中において１
３００℃以上で焼結されたＳｎＯ2系焼結体からなり、
その比抵抗が１×１０7Ω・ｃｍ以下であることを特徴
とするものである。Further, the material for forming a SnO 2 -based thin film according to the present invention contains at least one selected from the group consisting of Al, Si, Nb, Ta and Y, and the total amount of the additives is 20 in terms of oxide. % Of SnO 2 -based mixed powder is molded in an air atmosphere or an oxygen atmosphere.
It is composed of a SnO 2 based sintered body sintered at 300 ° C. or higher,
The specific resistance is 1 × 10 7 Ω · cm or less.
【００１３】本発明の好ましい態様においては、ＳｎＯ
2系焼結体は、Ｘ2Ｏ5（Ｘは任意の元素）の酸化形態を
持つ元素を少なくとも１種含有し、その添加量の合計が
酸化物換算で２０重量％以下であるＳｎＯ2系焼結体か
らなり、その比抵抗が１×１０4Ω・ｃｍ以下である。In a preferred embodiment of the present invention, SnO
The SnO 2 -based sintered body contains at least one element having an oxidized form of X 2 O 5 (X is an arbitrary element), and the total amount of addition thereof is 20% by weight or less in terms of oxide. It is made of a sintered body and has a specific resistance of 1 × 10 4 Ω · cm or less.
【００１４】また、本発明の好ましい態様においては、
ＳｎＯ2系薄膜形成用材料は、Ｘ2Ｏ 5（Ｘは任意の元
素）の酸化形態を持つ元素を少なくとも１種含有し、そ
の添加量の合計が酸化物換算で２０重量％以下であるＳ
ｎＯ2系混合粉末を成形し、大気雰囲気または酸素雰囲
気にて１３００℃以上で焼結された比抵抗が１×１０4
Ω・ｃｍ以下であるＳｎＯ2系焼結体からなる。In a preferred embodiment of the present invention,
SnOTwoThe material for forming a thin film is XTwoO Five(X is any element
At least one element having the oxidation form of
In which the total amount of S added is 20% by weight or less in terms of oxide.
nOTwoMolding the mixed powder, and atmosphere or oxygen atmosphere
The specific resistance sintered at 1300 ° C or higher by air is 1 × 10Four
Ω · cm or less SnOTwoIt consists of a sintered body.
【００１５】さらに、この場合の好ましい態様において
は、上記添加成分は、Ｎｂおよび／またはＴａからな
る。Further, in a preferred embodiment in this case, the additional component comprises Nb and / or Ta.
【００１６】また、本発明によるＳｎＯ2系透明導電膜
は、Ａｌ、Ｓｉ、Ｎｂ、ＴａおよびＹからなる群から選
ばれた少なくとも１種を含有し、その添加量の合計が酸
化物換算で２０重量％以下であり、膜厚１０００オング
ストロームにおける波長５５０ｎｍの光の透過率が８０
％以上であり、かつ、比抵抗が０．１Ω・ｃｍ以下であ
ることを特徴とする。The SnO 2 -based transparent conductive film according to the present invention contains at least one selected from the group consisting of Al, Si, Nb, Ta and Y, and the total amount of the additives is 20 in terms of oxide. Wt% or less, and the transmittance of light having a wavelength of 550 nm at a film thickness of 1000 Å is 80%.
% Or more, and the specific resistance is 0.1 Ω · cm or less.
【００１７】さらに、本発明のＳｎＯ2系透明導電膜の
好ましい態様においては、Ｘ2Ｏ5（Ｘは任意の元素）の
酸化形態を持つ元素を少なくとも１種含有し、その添加
量の合計が酸化物換算で２０重量％以下であり、膜厚１
０００オングストロームにおける波長５５０ｎｍの光の
透過率が８０％以上であり、かつ、比抵抗が０．１Ω・
ｃｍ以下である。Further, in a preferred embodiment of the SnO 2 -based transparent conductive film of the present invention, at least one element having an oxidized form of X 2 O 5 (X is an arbitrary element) is contained, and the total amount of the added elements is 20% by weight or less in terms of oxide, and a film thickness of 1
The transmittance of light having a wavelength of 550 nm at 2,000 angstroms is 80% or more, and the specific resistance is 0.1 Ω ·
cm or less.
【００１８】また、本発明の好ましい態様においては、
ＳｎＯ2系透明導電膜は、比抵抗が０．０１Ω・ｃｍ以
下であり、さらに、Ｎｂおよび／またはＴａを含有する
ものである。In a preferred embodiment of the present invention,
The SnO 2 -based transparent conductive film has a specific resistance of 0.01 Ω · cm or less and further contains Nb and / or Ta.
【００１９】さらに、本発明に係るＳｎＯ2系焼結体、
薄膜形成用材料ならびにこれによって得られたＳｎＯ2
系透明導電膜は、実質的にＳｂ2Ｏ3を含有しないか、含
有していたとしてもその量は、１０ｐｐｍ以下である。Further, a SnO 2 -based sintered body according to the present invention,
Thin film forming material and SnO 2 obtained by this
The system transparent conductive film does not substantially contain Sb 2 O 3 , or even if it does, the amount is 10 ppm or less.
【００２０】さらにまた、本発明は、上記薄膜形成用材
料を用いてＳｎＯ2系透明導電膜を成膜する透明導電膜
の製造方法も含む。Further, the present invention also includes a method of manufacturing a transparent conductive film by forming a SnO 2 -based transparent conductive film using the above-mentioned material for forming a thin film.
【００２１】さらに、本発明に係る上記焼結体は、大気
雰囲気または酸素雰囲気にて焼結してなるものであり、
該焼結体は、実質的にＳｂ2Ｏ3を含有しない。Further, the sintered body according to the present invention is obtained by sintering in an air atmosphere or an oxygen atmosphere.
The sintered body does not substantially contain Sb 2 O 3 .
【００２２】本発明による薄膜形成用材料は、所定のバ
ッキングプレート等を具備することによってスパッタリ
ングターゲットへの好適に適用され得る。したがって、
本発明は、スパッタリングターゲットをも包含する。The material for forming a thin film according to the present invention can be suitably applied to a sputtering target by providing a predetermined backing plate or the like. Therefore,
The present invention also includes a sputtering target.
【００２３】[0023]
【発明の実施の形態】本発明による焼結体は、Ａｌ、Ｓ
ｉ、Ｎｂ、ＴａおよびＹからなる群から選ばれた少なく
とも１種を含有し、その添加量の合計が酸化物換算で２
０重量％以下であり、かつ、比抵抗が１×１０7Ω・ｃ
ｍ以下であることを特徴とする。BEST MODE FOR CARRYING OUT THE INVENTION A sintered body according to the present invention comprises Al, S
At least one selected from the group consisting of i, Nb, Ta and Y is contained, and the total amount of the additives is 2 in terms of oxide.
0% by weight or less and a specific resistance of 1 × 10 7 Ω · c
m or less.
【００２４】さらに、本発明によるＳｎＯ2系薄膜形成
用材料は、Ａｌ、Ｓｉ、Ｎｂ、ＴａおよびＹからなる群
から選ばれた少なくとも１種を含有し、その添加量の合
計が酸化物換算で２０重量％以下であるＳｎＯ2系混合
粉末を成形し、大気雰囲気または酸素雰囲気中において
１３００℃以上で焼結されたＳｎＯ2系焼結体からな
り、その比抵抗が１×１０7Ω・ｃｍ以下であることを
特徴としている。Further, the material for forming a SnO 2 -based thin film according to the present invention contains at least one selected from the group consisting of Al, Si, Nb, Ta and Y, and the total amount of addition thereof is calculated as oxide. A SnO 2 -based mixed powder of 20% by weight or less is formed and made of a SnO 2 -based sintered body sintered at 1300 ° C. or more in an air atmosphere or an oxygen atmosphere, and has a specific resistance of 1 × 10 7 Ω · cm. It is characterized as follows.
【００２５】本発明者は、ＳｎＯ2系粉末に、Ａｌ、Ｓ
ｉ、Ｎｂ、ＴａおよびＹからなる群から選ばれた少なく
とも１種を含有し、その添加量の合計が酸化物換算で２
０重量％以下とし、この原料混合粉末を成形・焼結する
ことによって、比抵抗が１×１０7Ω・ｃｍ以下であ
り、比較的大型の焼結体を製造することのできるＣＰ
法、鋳込み法による作製が可能であり、しかも１３００
℃以上の高温条件での焼結が可能になることを見出し
た。本発明はこのような知見によりなされたものであ
る。[0025] The present invention shall, SnO 2 based powder, Al, S
At least one selected from the group consisting of i, Nb, Ta and Y is contained, and the total amount of the additives is 2 in terms of oxide.
By molding and sintering the raw material mixed powder to 0% by weight or less, a CP having a specific resistance of 1 × 10 7 Ω · cm or less and a relatively large sintered body can be manufactured.
It can be manufactured by the casting method or the casting method.
It has been found that sintering under a high temperature condition of not less than ℃ is possible. The present invention has been made based on such findings.
【００２６】上記の添加成分の添加形態については、メ
タル粉、酸化物粉、窒化物粉、水酸化物粉、炭化物粉な
ど特に形態を選ばないが、焼結中におけるガスの発生が
ないメタル粉、酸化物粉での添加が好ましく、比較的高
温まで溶融しない酸化物粉がさらに好ましい。The form of addition of the above-mentioned additive components is not particularly limited, such as metal powder, oxide powder, nitride powder, hydroxide powder, and carbide powder. , Oxide powder is preferable, and oxide powder that does not melt to a relatively high temperature is more preferable.
【００２７】混合方法は、不純物が混入せず、均一に混
合できればよく、一般的には乾式混合、湿式混合などが
知られている。また、共沈法などにより混合粉を作製す
る方法も有効である。The mixing method is not particularly limited as long as it can be uniformly mixed without mixing impurities. Generally, dry mixing, wet mixing and the like are known. Further, a method of producing a mixed powder by a coprecipitation method or the like is also effective.
【００２８】上記添加成分の添加量は、その合計が酸化
物換算で２０重量％以下であり、さらに好ましくは６重
量％以下である。添加量が２０重量％を超えると、焼結
体の比抵抗がいきおい増大し、さらにスパッタリング効
率が低下するので好ましくない。さらに、上記上限値を
超えると、成膜された膜中にも添加成分が析出し、膜の
比抵抗も増大するので好ましくない。The total amount of the above additional components is 20% by weight or less, more preferably 6% by weight or less, in terms of oxide. If the addition amount exceeds 20% by weight, the specific resistance of the sintered body is greatly increased, and the sputtering efficiency is further decreased, which is not preferable. Further, when the value exceeds the above upper limit, the additional component is precipitated in the formed film, and the specific resistance of the film is undesirably increased.
【００２９】本発明のＳｎＯ2系焼結体の好ましい態様
においては、Ｘ2Ｏ5（Ｘは任意の元素）の酸化形態を持
つ元素を少なくとも１種含有し、その添加量の合計が酸
化物換算で２０重量％以下であるＳｎＯ2系焼結体から
なり、その比抵抗が１×１０4Ω・ｃｍ以下である。In a preferred embodiment of the SnO 2 -based sintered body of the present invention, at least one element having an oxidized form of X 2 O 5 (X is an arbitrary element) is contained, and the total amount of the added elements is oxide. It is made of a SnO 2 -based sintered body having a conversion of 20% by weight or less, and has a specific resistance of 1 × 10 4 Ω · cm or less.
【００３０】また、本発明のＳｎＯ2系薄膜形成用材料
は、Ｘ2Ｏ5（Ｘは任意の元素）の酸化形態を持つ元素を
少なくとも１種含有し、その添加量の合計が酸化物換算
で２０重量％以下であるＳｎＯ2系混合粉末を成形し、
大気雰囲気または酸素雰囲気にて１３００℃以上で焼結
された比抵抗が１×１０4Ω・ｃｍ以下のであるＳｎＯ2
系焼結体からなる。Further, the material for forming a SnO 2 -based thin film of the present invention contains at least one element having an oxidized form of X 2 O 5 (X is an arbitrary element), and the total amount of the added elements is expressed in terms of oxide. To form a SnO 2 -based mixed powder of 20% by weight or less,
SnO 2 sintered at 1300 ° C. or more in an air atmosphere or an oxygen atmosphere and having a specific resistance of 1 × 10 4 Ω · cm or less
It consists of a sintered body.
【００３１】本発明による薄膜形成用材料は、所定のバ
ッキングプレート等を具備することによってスパッタリ
ングターゲットへの好適に適用され得る。したがって、
本発明は、スパッタリングターゲットをも包含する。The material for forming a thin film according to the present invention can be suitably applied to a sputtering target by providing a predetermined backing plate or the like. Therefore,
The present invention also includes a sputtering target.
【００３２】本発明による焼結体の製造に際しては、原
料粉末を常法にしたがって混合し、成形し、焼結する諸
工程を含む。成型方法は特に限定されるものではなく、
プレス成形、鋳込み成形などが考えられるが、所定の寸
法に成形できる限り、どのような成型方法でも本発明に
適用することができる。The production of the sintered body according to the present invention includes various steps of mixing, molding and sintering the raw material powders according to a conventional method. The molding method is not particularly limited,
Press molding, cast molding and the like can be considered, but any molding method can be applied to the present invention as long as it can be molded to a predetermined size.
【００３３】本発明に係るＳｎＯ2系焼結体は実質的に
Ｓｂ2Ｏ3を含有しないか、含有していたとしてもその量
は、１０ｐｐｍ以下の不可避的含有量であることから、
従来のようにＳｂ2Ｏ3を含有する原料混合物の焼結の場
合のように焼結温度を１０００℃程度以上に上げること
ができないという焼結条件上の制限がない。すなわち、
本発明においては、焼結条件として、１３００℃以上、
好ましくは１４５０℃以上の温度条件を採用することが
できる。したがって、本発明においては、高温の条件に
よって、強度の高い焼結体が得られることから、比較的
大型の焼結体の製造に適したＣＰ法や鋳込み法を採用す
ることが可能となる。Since the SnO 2 -based sintered body according to the present invention does not substantially contain Sb 2 O 3 , or even if it does, the amount is an unavoidable content of 10 ppm or less.
Unlike the conventional case of sintering a raw material mixture containing Sb 2 O 3 , there is no limitation on the sintering conditions that the sintering temperature cannot be raised to about 1000 ° C. or more. That is,
In the present invention, the sintering conditions are 1300 ° C. or higher,
Preferably, a temperature condition of 1450 ° C. or higher can be adopted. Therefore, in the present invention, a high-strength sintered body can be obtained under high-temperature conditions, so that a CP method or a casting method suitable for manufacturing a relatively large-sized sintered body can be adopted.
【００３４】なお、焼結時間は得ようとする焼結体の寸
法や組成によって適宜選択され得るが、通常、１時間か
ら３０時間が適当であり、好ましくは２時間から１０時
間である。焼結雰囲気は、大気、酸素、還元雰囲気など
特に限定されるものではないが、製造コストの観点か
ら、、大気中、酸素雰囲気中での焼結がより好ましく、
大気雰囲気が特に好ましい。The sintering time can be appropriately selected depending on the size and composition of the sintered body to be obtained, but is usually from 1 hour to 30 hours, preferably from 2 hours to 10 hours. The sintering atmosphere is not particularly limited, such as air, oxygen, and reducing atmosphere.From the viewpoint of manufacturing cost, sintering in air or oxygen is more preferable.
An air atmosphere is particularly preferred.
【００３５】上述した本発明による焼結体は、ＣＰ法、
鋳込み法による製造方法に特に適しているが、同様に、
ＨＰ法、ＨＩＰ法（Hot Isostatic Press法）にも適用
が可能である。The above-described sintered body according to the present invention is obtained by a CP method,
Although particularly suitable for the casting method,
It is also applicable to the HP method and the HIP method (Hot Isostatic Press method).
【００３６】本発明によれば、大型のＳｎＯ2系焼結体
の製造が可能であり、製造法にもよるが、たとえば、３
００×６００×８ｍｍ程度の比較的大型の焼結体を得る
ことができる。According to the present invention, a large-sized SnO 2 -based sintered body can be manufactured.
A relatively large sintered body of about 00 × 600 × 8 mm can be obtained.
【００３７】一般にスパッタリングターゲットによって
成膜を行う場合、その比抵抗が１×１０7Ω・ｃｍ以下
であれば、成膜効率の比較的良好なＤＣスパッタリング
法による成膜が可能となる。この点から、さらに好まし
くは焼結体の比抵抗は、１×１０4Ω・ｃｍ以下が望ま
しく、さらに比抵抗が低いほど好ましい。In general, when a film is formed by a sputtering target, if the specific resistance is 1 × 10 7 Ω · cm or less, the film can be formed by the DC sputtering method having a relatively good film forming efficiency. From this point, the specific resistance of the sintered body is more preferably 1 × 10 4 Ω · cm or less, and the lower the specific resistance, the more preferable.
【００３８】また、焼結体をスパッタリングターゲット
として用いる場合、そのスパッタ面の表面粗さは、一般
にその組成の如何によらず、表面粗さ０．１〜６．０μ
ｍ程度が適当である。When a sintered body is used as a sputtering target, the surface roughness of the sputtered surface is generally 0.1 to 6.0 μm regardless of the composition.
About m is appropriate.
【００３９】上記焼結体からなるスパッタリングターゲ
ットを用いた透明導電膜の成膜方法は特に限定されるも
のではないが、好ましくは工業的に効率の良いスパッタ
リング法を適宜選択することができ、特に好ましくはＤ
Ｃスパッタリング法である。ＳｎＯ2系透明導電膜に要
求される特性は、ＳｎＯ2系透明導電膜の比抵抗が０．
１Ω・ｃｍ以下、膜厚１０００オングストロームにおけ
る波長５５０ｎｍの光の透過率が８０％以上である。上
記本発明によれば、ＳｎＯ2系薄膜の比抵抗は０．１Ω
・ｃｍ以下が可能であり、好ましくは０．０１Ω・ｃｍ
以下であり、より好ましくは０．００７Ω・ｃｍ以下で
ある。また、本発明によって得られるＳｎＯ2系透明導
電膜の透過率は、８０％以上であり、さらに好ましくは
８５％以上である。The method for forming the transparent conductive film using the sputtering target made of the sintered body is not particularly limited, but preferably a sputtering method that is industrially efficient can be appropriately selected. Preferably D
This is a C sputtering method. Properties required for the SnO 2 based transparent conductive film, the resistivity of SnO 2 based transparent conductive film is 0.
The transmittance of light having a wavelength of 550 nm at a resistivity of 1 Ω · cm or less and a film thickness of 1000 Å is 80% or more. According to the present invention, the specific resistance of the SnO 2 -based thin film is 0.1Ω.
· Cm or less, preferably 0.01 Ω · cm
Or less, more preferably 0.007 Ω · cm or less. The transmittance of the SnO 2 -based transparent conductive film obtained by the present invention is 80% or more, and more preferably 85% or more.
【００４０】[0040]
【実施例】実施例１ 純度９９．９９％、平均粒径０．８〜１．４μｍ（光透
過法にて測定）、比表面積２．０〜３．０ｍ2／ｇのＳ
ｎＯ2粉末に市販のＡｌ2Ｏ3、ＳｉＯ2、Ｙ2Ｏ3、Ｔａ2
Ｏ5、Ｎｂ2Ｏ5粉末を個別に５ｗｔ％添加し、ボールミ
ルを用いて２０時間混合した。混合粉にポリビニルアル
コール水溶液を添加し造粒し、４００×８００ｍｍの寸
法のプレス金型に充填し、５００ｋｇ／ｃｍ2の圧力で
プレス成形した。これを８０℃で１５時間乾燥したの
ち、２００℃〜６００℃にて脱脂した物を、酸素雰囲気
１５００℃にて４時間焼結した。なお昇温速度、降温速
度共に１００℃／ｈｒである。このようにして得られた
焼結体を加工して、３００×６００×８ｍｍの寸法のス
パッタリングターゲットを作製した。得られたスパッタ
リングターゲットの表面粗さＲａは０．６μｍ、内部組
織は、添加元素が均一に分散されており、またボアも均
一に分散されていた。スパッタリングターゲットの組成
を分析するとそれぞれの混合粉と同じ組成であった。ス
パッタリングターゲットは着色されており高純度のＳｎ
Ｏ2を焼結したときの白色ではなかった。 EXAMPLE 1 S having a purity of 99.99%, an average particle diameter of 0.8 to 1.4 μm (measured by a light transmission method) and a specific surface area of 2.0 to 3.0 m 2 / g.
nO 2 powder Commercially available Al 2 O 3, SiO 2, Y 2 O 3, Ta2
5 wt% of O 5 and Nb 2 O 5 powders were individually added and mixed for 20 hours using a ball mill. An aqueous polyvinyl alcohol solution was added to the mixed powder, and the mixture was granulated, filled in a press die having a size of 400 × 800 mm, and press-molded at a pressure of 500 kg / cm 2 . This was dried at 80 ° C for 15 hours, and then degreased at 200 ° C to 600 ° C, and sintered at 1500 ° C in an oxygen atmosphere for 4 hours. The rate of temperature rise and the rate of temperature decrease are both 100 ° C./hr. The sintered body thus obtained was processed to produce a sputtering target having a size of 300 × 600 × 8 mm. The obtained sputtering target had a surface roughness Ra of 0.6 μm, and the internal structure was such that the added elements were uniformly dispersed and the bore was also uniformly dispersed. When the composition of the sputtering target was analyzed, the composition was the same as each of the mixed powders. The sputtering target is colored and has high purity Sn
It was not white when O 2 was sintered.
【００４１】得られたスパッタリングターゲットの比抵
抗を表１に示す。比抵抗はＬｏｒｅｓｔａ ＨＰ ＭＧ
Ｐ−Ｔ４１０（三菱化学株式会社製）により測定した。Table 1 shows the specific resistance of the obtained sputtering target. Specific resistance is Loresta HP MG
It was measured by PT-410 (manufactured by Mitsubishi Chemical Corporation).
【００４２】特に、Ｘ2Ｏ5（Ｘは任意の元素）の酸化形
態を持つ元素の添加が比抵抗には効果的であることがわ
かる。In particular, it is found that the addition of an element having an oxidized form of X 2 O 5 (X is an arbitrary element) is effective for the specific resistance.
【００４３】比較例１ 純度９９．９９％、平均粒径０．８〜１．４μｍ（光透
過法にて測定）、比表面積２．０〜３．０ｍ2／ｇのＳ
ｎＯ2粉末に市販のＧｅＯ2、Ｇａ2Ｏ3、Ｂｉ2Ｏ 3、Ｍｎ
2Ｏ3、ＭｎＯ、Ｆｅ2Ｏ3粉末を個別に５ｗｔ％添加し、
ボールミルを用いて２０時間混合した。混合粉にポリビ
ニルアルコール水溶液を添加し造粒し、プレス金型に充
填し、５００ｋｇ／ｃｍ2の圧力でプレス成形した。こ
れを８０℃で１５時間乾燥したのち、２００℃〜６００
℃にて脱脂した物を、酸素雰囲気１５００℃にて４時間
焼結した。なお昇温速度、降温速度共に１００℃／ｈｒ
である。このようにして得られた焼結体を加工して、ス
パッタリングターゲットを作製した。得られたスパッタ
リングターゲットの表面粗さＲａは０．６μｍ、内部組
織は、添加元素が均一に分散されており、またボアも均
一に分散されていた。スパッタリングターゲットの組成
を分析するとそれぞれの混合粉と同じ組成であった。ス
パッタリングターゲットは着色されており高純度のＳｎ
Ｏ2を焼結したときの白色ではなかった。[0043]Comparative Example 1 Purity 99.99%, average particle size 0.8-1.4 μm (light transmission
Measured by excess method), specific surface area 2.0 to 3.0 mTwo/ G of S
nOTwoCommercially available GeO powderTwo, GaTwoOThree, BiTwoO Three, Mn
TwoOThree, MnO, FeTwoOThreeAdd 5wt% of powder individually,
The mixture was mixed using a ball mill for 20 hours. Polyvinyl to mixed powder
Nyl alcohol aqueous solution is added to granulate and filled into a press die.
500kg / cmTwoPress molding. This
After drying it at 80 ° C. for 15 hours,
Degreased at 1500 ° C for 4 hours at 1500 ° C in an oxygen atmosphere
Sintered. In addition, both the heating rate and the cooling rate are 100 ° C / hr.
It is. The sintered body obtained in this way is processed and
A putting target was prepared. The resulting spatter
The surface roughness Ra of the ring target is 0.6 μm,
In the weave, the added elements are evenly dispersed and the bore is even.
Was dispersed in one. Composition of sputtering target
Was analyzed and found to have the same composition as each of the mixed powders. S
The sputtering target is colored and has high purity Sn
OTwoWas not white when sintered.
【００４４】得られたスパッタリングターゲットの比抵
抗を表２に示す。比抵抗はＬｏｒｅｓｔａ ＨＰ ＭＧ
Ｐ−Ｔ４１０（三菱化学株式会社製）により測定した。Table 2 shows the specific resistance of the obtained sputtering target. Specific resistance is Loresta HP MG
It was measured by PT-410 (manufactured by Mitsubishi Chemical Corporation).
【００４５】実施例２ 純度９９．９９％、平均粒径０．８〜１．４μｍ（光透
過法にて測定）、比表面積２．０〜３．０ｍ2／ｇのＳ
ｎＯ2粉末に市販のＴａ2Ｏ5、Ｎｂ2Ｏ5粉末を添加し、
ボールミルを用いて２０時間混合した。混合粉にポリビ
ニルアルコール水溶液を添加し造粒し、４００×８００
ｍｍの寸法のプレス金型に充填し、５００ｋｇ／ｃｍ2
の圧力でプレス成形した。これを８０℃で１５時間乾燥
したのち、２００℃〜６００℃にて脱脂した物を、酸素
雰囲気１５００℃にて４時間焼結した。なお昇温速度、
降温速度共に１００℃／ｈｒである。このようにして得
られた焼結体を加工して、３００×６００×８ｍｍの寸
法のスパッタリングターゲットを作製した。得られたス
パッタリングターゲットの表面粗さＲａは０．６μｍ、
内部組織は、添加元素が均一に分散されており、またボ
アも均一に分散されていた。スパッタリングターゲット
の組成を分析するとそれぞれの混合粉と同じ組成であっ
た。スパッタリングターゲットは着色されており高純度
のＳｎＯ2を焼結したときの白色ではなかった。 Example 2 S having a purity of 99.99%, an average particle diameter of 0.8 to 1.4 μm (measured by a light transmission method) and a specific surface area of 2.0 to 3.0 m 2 / g.
Commercially available Ta 2 O 5 and Nb 2 O 5 powders were added to the nO 2 powder,
The mixture was mixed using a ball mill for 20 hours. An aqueous polyvinyl alcohol solution is added to the mixed powder and granulated, and 400 × 800
500 mm / cm 2
Press molding. This was dried at 80 ° C for 15 hours, and then degreased at 200 ° C to 600 ° C, and sintered at 1500 ° C in an oxygen atmosphere for 4 hours. The heating rate,
Both of the cooling rates are 100 ° C./hr. The sintered body thus obtained was processed to produce a sputtering target having a size of 300 × 600 × 8 mm. The surface roughness Ra of the obtained sputtering target is 0.6 μm,
In the internal structure, the added elements were uniformly dispersed, and the bore was also uniformly dispersed. When the composition of the sputtering target was analyzed, the composition was the same as each of the mixed powders. The sputtering target was colored and was not white when high purity SnO 2 was sintered.
【００４６】得られたスパッタリングターゲットの比抵
抗を表３に示す。比抵抗はＬｏｒｅｓｔａ ＨＰ ＭＧ
Ｐ−Ｔ４１０（三菱化学株式会社製）により測定した。Table 3 shows the resistivity of the obtained sputtering target. Specific resistance is Loresta HP MG
It was measured by PT-410 (manufactured by Mitsubishi Chemical Corporation).
【００４７】実施例３ 実施例２により得られたスパッタリングターゲットを用
いて、スパッタリングによりガラス基板上に成膜した。
この時のスパッタ条件は下記に示す。このようにして得
られたＳｎＯ2系透明導電膜の比抵抗と透過率を測定し
た。その結果を表４に示す。さらに、得られたＳｎＯ2
系透明導電膜をガラス基盤ごと大気中５００℃で３０分
アニールし、アニールされたＳｎＯ2系透明導電膜の比
抵抗と透過率を測定した。その結果を表５に示す。なお
比抵抗はＬｏｒｅｓｔａ ＨＰＭＧＰ−Ｔ４１０（三菱
化学株式会社製）により測定した。 Example 3 Using the sputtering target obtained in Example 2, a film was formed on a glass substrate by sputtering.
The sputtering conditions at this time are shown below. The specific resistance and transmittance of the thus obtained SnO 2 -based transparent conductive film were measured. Table 4 shows the results. Further, the obtained SnO2
The system-based transparent conductive film was annealed together with the glass substrate in air at 500 ° C. for 30 minutes, and the resistivity and transmittance of the annealed SnO 2 -based transparent conductive film were measured. Table 5 shows the results. The specific resistance was measured by Loresta HPMGP-T410 (manufactured by Mitsubishi Chemical Corporation).
【００４８】スパッタ条件 スパッタ圧 ３×１０-3Ｔｏｒｒ Ｏ2 分圧 ０〜９×１０-4Ｔｏｒｒ 投入パワー（定電流源） ３６０ｍＡ 成膜温度 １００℃ カソードマグネット フェライト磁石Sputtering conditions Sputtering pressure 3 × 10 −3 Torr O 2 partial pressure 0-9 × 10 −4 Torr Input power (constant current source) 360 mA Film forming temperature 100 ° C. Cathode magnet Ferrite magnet
【００４９】[0049]
【表１】 [Table 1]
【００５０】[0050]
【表２】 [Table 2]
【００５１】[0051]
【表３】 [Table 3]
【００５２】[0052]
【表４】 [Table 4]
【００５３】[0053]
【表５】 [Table 5]
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｈ０１Ｂ 5/14 Ｈ０１Ｂ 5/14 Ａ ５Ｃ０９４ Ｈ０１Ｊ 9/02 Ｈ０１Ｊ 9/02 Ｆ ５Ｇ３０１ 11/00 11/00 Ａ ５Ｇ３０７ 17/04 17/04 Ｆターム(参考） 4G030 AA12 AA20 AA21 AA36 AA37 AA39 BA02 GA25 GA29 4K029 BA47 BC09 DC05 DC09 5B087 BC33 CC36 5C027 AA01 5C040 FA01 FA02 GA02 GB01 KA04 KB17 KB29 MA26 5C094 AA42 AA43 BA31 EA05 FB02 FB12 GB01 HA08 JA05 JA11 JA20 5G301 CA02 CA12 CA23 CA26 CA30 CD03 CD10 CE02 5G307 FA01 FB01 FC09 FC10 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification code FI Theme coat ゛ (Reference) H01B 5/14 H01B 5/14 A 5C094 H01J 9/02 H01J 9/02 F 5G301 11/00 11/00 A 5G307 17/04 17/04 F term (reference) 4G030 AA12 AA20 AA21 AA36 AA37 AA39 BA02 GA25 GA29 4K029 BA47 BC09 DC05 DC09 5B087 BC33 CC36 5C027 AA01 5C040 FA01 FA02 GA02 GB01 KA04 KB17 KB29 MA26 5C0914 A JA05 JA11 JA20 5G301 CA02 CA12 CA23 CA26 CA30 CD03 CD10 CE02 5G307 FA01 FB01 FC09 FC10
Claims (14)
群から選ばれた少なくとも１種を含有し、その添加量の
合計が酸化物換算で２０重量％以下であり、かつ、比抵
抗が１×１０7Ω・ｃｍ以下であることを特徴とする、
ＳｎＯ2系焼結体。(1) containing at least one member selected from the group consisting of Al, Si, Nb, Ta and Y, the total amount of the additives being 20% by weight or less in terms of oxide, and the specific resistance being 1 × 10 7 Ω · cm or less,
SnO 2 based sintered body.
群から選ばれた少なくとも１種を含有し、その添加量の
合計が酸化物換算で２０重量％以下であるＳｎＯ2系混
合粉末を成形し、大気雰囲気または酸素雰囲気中におい
て１３００℃以上で焼結されたＳｎＯ2系焼結体からな
り、その比抵抗が１×１０7Ω・ｃｍ以下であることを
特徴とする、ＳｎＯ2系薄膜形成用材料。 2. A SnO 2 -based mixed powder containing at least one member selected from the group consisting of Al, Si, Nb, Ta and Y and having a total amount of 20% by weight or less in terms of oxide. molded, it consists SnO 2 based sintered body sintered at 1300 ° C. or higher in an air atmosphere or oxygen atmosphere, characterized in that resistivity thereof is less than 1 × 10 7 Ω · cm, SnO 2 system Materials for forming thin films.
つ元素を少なくとも１種含有し、その添加量の合計が酸
化物換算で２０重量％以下であるＳｎＯ2系焼結体から
なり、その比抵抗が１×１０4Ω・ｃｍ以下であること
を特徴とする、ＳｎＯ2系焼結体。Wherein X 2 O 5 (X is any element) at least one contains, total SnO 2 based sintered than 20% by weight in terms of oxide of the added amount of the element having the oxidized form of A SnO 2 -based sintered body comprising a body and having a specific resistance of 1 × 10 4 Ω · cm or less.
つ元素を少なくとも１種含有し、その添加量の合計が酸
化物換算で２０重量％以下であるＳｎＯ2系混合粉末を
成形し、大気雰囲気または酸素雰囲気にて１３００℃以
上で焼結された比抵抗が１×１０4Ω・ｃｍ以下である
ＳｎＯ2系焼結体からなることを特徴とする、ＳｎＯ2系
薄膜形成用材料。4. A SnO 2 -based mixed powder containing at least one element having an oxidized form of X 2 O 5 (X is an arbitrary element), and the total amount of addition is 20% by weight or less in terms of oxide. molding a, characterized in that it consists of the atmosphere or sintered resistivity at 1300 ° C. or higher in an oxygen atmosphere is not more than 1 × 10 4 Ω · cm SnO 2 based sintered body, SnO 2 based thin film Forming material.
項１または３に記載のＳｎＯ2系焼結体。5. The SnO 2 -based sintered body according to claim 1, which contains Nb and / or Ta.
項２または４に記載のＳｎＯ2系薄膜形成用材料。6. The material for forming a SnO2 thin film according to claim 2, wherein the material contains Nb and / or Ta.
群から選ばれた少なくとも１種を含有し、その添加量の
合計が酸化物換算で２０重量％以下であり、膜厚１００
０オングストロームにおける波長５５０ｎｍの光の透過
率が８０％以上であり、かつ、比抵抗が０．１Ω・ｃｍ
以下であることを特徴とする、ＳｎＯ2系透明導電膜。7. It contains at least one member selected from the group consisting of Al, Si, Nb, Ta and Y, the total amount of addition is 20% by weight or less in terms of oxide, and the film thickness is 100%.
The transmittance of light having a wavelength of 550 nm at 0 Å is 80% or more, and the specific resistance is 0.1 Ω · cm.
A SnO 2 -based transparent conductive film, characterized in that:
つ元素を少なくとも１種含有し、その添加量の合計が酸
化物換算で２０重量％以下であり、膜厚１０００オング
ストロームにおける波長５５０ｎｍの光の透過率が８０
％以上であり、かつ、比抵抗が０．１Ω・ｃｍ以下であ
ることを特徴とする、ＳｎＯ2系透明導電膜。8. At least one element having an oxidized form of X 2 O 5 (X is an arbitrary element), the total amount of addition of which is 20% by weight or less in terms of oxide, and a film thickness of 1000 Å At a wavelength of 550 nm is 80.
Not less than%, and wherein the specific resistance is less than 0.1Ω · cm, SnO 2 based transparent conductive film.
求項８に記載のＳｎＯ2系透明導電膜。9. The SnO 2 -based transparent conductive film according to claim 8, having a specific resistance of 0.01 Ω · cm or less.
求項７または８に記載のＳｎＯ2系透明導電膜。10. The SnO 2 -based transparent conductive film according to claim 7, which contains Nb and / or Ta.
請求項１０に記載のＳｎＯ2系透明導電膜。(11) a specific resistance of 0.01 Ω · cm or less;
The SnO 2 -based transparent conductive film according to claim 10.
料のスパッタリングターゲットへの使用。12. Use of the material for forming a thin film according to claim 2 for a sputtering target.
以下、好ましくは実質的にＳｂ2Ｏ3を含有しない、請求
項１に記載のＳｎＯ2系焼結体。13. The Sb 2 O 3 content in the sintered body is 10 ppm.
The SnO 2 -based sintered body according to claim 1, wherein the sintered body does not substantially contain Sb 2 O 3 .
用材料を用いて請求項７〜請求項１１のいずれか１項に
記載のＳｎＯ2系透明導電膜を成膜する、透明導電膜の
製造方法。14. A transparent conductive film, comprising forming the SnO 2 -based transparent conductive film according to any one of claims 7 to 11 using the material for forming a thin film according to claim 2, 4 or 6. Manufacturing method of membrane.
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