JP4409071B2 - Backing plate for sputtering target made of copper or copper alloy and processing method thereof - Google Patents
Backing plate for sputtering target made of copper or copper alloy and processing method thereof Download PDFInfo
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- JP4409071B2 JP4409071B2 JP2000268021A JP2000268021A JP4409071B2 JP 4409071 B2 JP4409071 B2 JP 4409071B2 JP 2000268021 A JP2000268021 A JP 2000268021A JP 2000268021 A JP2000268021 A JP 2000268021A JP 4409071 B2 JP4409071 B2 JP 4409071B2
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- copper
- backing plate
- copper alloy
- sputtering target
- benzotriazole
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims description 38
- 229910052802 copper Inorganic materials 0.000 title claims description 38
- 239000010949 copper Substances 0.000 title claims description 38
- 229910000881 Cu alloy Inorganic materials 0.000 title claims description 31
- 238000005477 sputtering target Methods 0.000 title claims description 19
- 238000003672 processing method Methods 0.000 title description 2
- 238000002845 discoloration Methods 0.000 claims description 39
- 230000003647 oxidation Effects 0.000 claims description 29
- 238000007254 oxidation reaction Methods 0.000 claims description 29
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 19
- 239000003112 inhibitor Substances 0.000 claims description 18
- 239000012964 benzotriazole Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 230000001590 oxidative effect Effects 0.000 claims description 14
- -1 azole compound Chemical class 0.000 claims description 13
- ZDDUSDYMEXVQNJ-UHFFFAOYSA-N 1H-imidazole silane Chemical compound [SiH4].N1C=NC=C1 ZDDUSDYMEXVQNJ-UHFFFAOYSA-N 0.000 claims description 11
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 11
- 238000004649 discoloration prevention Methods 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 238000004544 sputter deposition Methods 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000003860 storage Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 150000003851 azoles Chemical class 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- IIHZFDWNRJRKDC-UHFFFAOYSA-N 2-(1h-imidazol-2-ylamino)ethanol Chemical compound OCCNC1=NC=CN1 IIHZFDWNRJRKDC-UHFFFAOYSA-N 0.000 description 1
- JWYUFVNJZUSCSM-UHFFFAOYSA-N 2-aminobenzimidazole Chemical compound C1=CC=C2NC(N)=NC2=C1 JWYUFVNJZUSCSM-UHFFFAOYSA-N 0.000 description 1
- QRZMXADUXZADTF-UHFFFAOYSA-N 4-aminoimidazole Chemical compound NC1=CNC=N1 QRZMXADUXZADTF-UHFFFAOYSA-N 0.000 description 1
- LRUDIIUSNGCQKF-UHFFFAOYSA-N 5-methyl-1H-benzotriazole Chemical compound C1=C(C)C=CC2=NNN=C21 LRUDIIUSNGCQKF-UHFFFAOYSA-N 0.000 description 1
- 229910000906 Bronze Inorganic materials 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910017813 Cu—Cr Inorganic materials 0.000 description 1
- LHTCIUDQXWZXBU-UHFFFAOYSA-N N-(2H-benzotriazol-4-ylmethyl)-2-ethylhexan-1-amine Chemical compound C(C)C(CNCC1=CC=CC=2NN=NC=21)CCCC LHTCIUDQXWZXBU-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- DMFGNRRURHSENX-UHFFFAOYSA-N beryllium copper Chemical compound [Be].[Cu] DMFGNRRURHSENX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Landscapes
- Anti-Oxidant Or Stabilizer Compositions (AREA)
- Physical Vapour Deposition (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は、銅又は銅合金製バッキングプレートに酸化変色防止処理を施し、スパッタリングプロセスの高度な清浄雰囲気において使用可能な銅又は銅合金製スパッタリングターゲット用バッキングプレート及びその処理方法に関する。
【０００２】
【従来の技術】
スパッタリングターゲットのバッキングプレートには、銅（無酸素銅など）及び銅合金（Ｃｕ−Ｃｒ合金、りん青銅、ベリリウム銅など）が広く使用されている。このようなバッキングプレートは、通常インジウムなどのボンディング剤にてターゲットと接合されており、ターゲット使用後は再度新しいターゲットをボンディングすることにより数回使用される。
このバッキングプレートはターゲットと接合され、最終的に真空梱包又はアルゴンガス封入梱包されて出荷されているが、運搬、保管などを行っている場合等に、バッキングプレートが変色する。
このため、梱包作業は湿度及び温度をコントロールしたクリーンルーム内で行っている。しかし、銅は変色しやすい金属であり、運搬や保管中にターゲットが変色してしまう場合がある。特に、保管期間が長い場合は変色が著しい。
この変色原因については、現在のところ明確な結論は出ていないが、変色部に酸化銅が生成していることが確認されているので、酸化による変色が主要な原因と考えられる。したがって、ここではこのような変色を「酸化変色」と呼ぶこととする。
【０００３】
さて、このようなバッキングプレートの酸化変色は、例えば真空シール部に発生した場合にスパッタ装置内の真空度が上がらない原因となり、また酸化部が剥離した場合にはパーティクルの原因となってしまい製品価値を大きく損なってしまうことがあった。
また、冷却水と接するところでは、冷却効率の低下を引き起してしまうという問題があった。そして、このような酸化変色はバッキングプレートを再度使用する際に除去しなければならないので、再生コストを上げてしまう原因となった。
このようなことから、銅又は銅合金製スパッタリングターゲット用バッキングプレートの酸化変色を防止し、運搬や保管の期間を延ばすことができるようにすると共に、スパッタリングプロセスの高度な清浄雰囲気において使用できるバッキングプレートが必要となった。
【０００４】
【発明が解決しようとする課題】
以上から、本発明は銅又は銅合金製バッキングプレートの運搬や保管の期間を延ばすと共に、再生コストを低減させ、スパッタリングプロセスの高度な清浄雰囲気において使用できる銅および銅合金製バッキングプレートを提供することを課題とするものである。
【０００５】
【課題を解決するための手段】
本発明者らは、バッキングプレートの酸化変色を防止することを目的に鋭意研究した結果、銅又は銅合金製スパッタリングターゲット用バッキングプレートに特定の酸化変色防止剤を施すことにより、上記の問題を解決できるとの知見を得た。
本発明はこの知見に基づいて、
１ ベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物からなる酸化変色防止剤を施したことを特徴とする銅又は銅合金製スパッタリングターゲット用バッキングプレート
２ 銅又は銅合金製バッキングプレートをベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物からなる酸化変色防止剤の溶液に浸漬するか又は該溶液を銅又は銅合金製バッキングプレートに噴霧することを特徴とする銅又は銅合金製スパッタリングターゲット用バッキングプレートの酸化変色防止処理方法
３ ベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物からなる酸化変色防止剤による処理後、有機溶剤中で超音波洗浄することを特徴とする上記２記載の銅又は銅合金製スパッタリングターゲット用バッキングプレートの酸化変色防止処理方法
を提供するものである。
【０００６】
【発明の実施の形態】
本発明は、銅又は銅合金製スパッタリングターゲット用バッキングプレートの酸化変色防止剤としてベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物が該ターゲットの運搬、保管期間を延ばし、スパッタプロセスをより安定化させ、信頼性の高い銅および銅合金の薄膜形成に極めて有効であることが分かった。
後述する実施例に示すように、このような酸化変色防止剤はスパッタリングによる薄膜形成に有害物質とはならず、しかも効果的に酸化変色を防止できる。
従来、ベンゾトリアゾール等は銅又は銅合金製材料の酸化変色防止剤として一般的に知られている材料ではあるが、バッキングプレートに利用することは考えられないことであった。それは、ベンゾトリアゾール等の酸化変色防止剤がスパッタリング中に汚染物質となる虞があったからである。
【０００７】
しかし、後述の実施例に示すように、ベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物からなる酸化変色防止剤に起因する汚染は全くないことが分かった。
これによって、ベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物からなる酸化変色防止剤を施したバッキングプレートが、スパッタリングに使用することが可能となり、しかもこの酸化変色防止剤は、運搬や保管の際に銅又は銅合金製スパッタリングターゲット用バッキングプレートの酸化変色を効果的に抑制できるという優れた特徴を有する。
ベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物は、具体的には１，２，３−ベンゾトリアゾール、１［（２エチルヘキシルアミノ）メチル］ベンゾトリアゾール、５−メチル・１Ｈベンゾトリアゾール、２−アミノイミダゾール、２−（ヒドロキシエチルアミノ）イミダゾール、２−アミノベンズイミダゾールなどがある。
以上により、銅又は銅合金製バッキングプレートの運搬や保管の期間を延ばすと共に、スパッタリングプロセスの高度な清浄雰囲気において使用可能な銅および銅合金製スパッタリングターゲット用バッキングプレートを提供することが可能となった。
【０００８】
ベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物からなる酸化変色防止剤の銅又は銅合金製バッキングプレートへの適用は、ベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物からなる溶液に浸漬するか又は該溶液を銅又は銅合金製バッキングプレートに噴霧することによって、処理することができる。
この酸化変色防止剤による銅又は銅合金製スパッタリングターゲット用バッキングプレートへの処理後、エタノールなどの有機溶剤中で超音波洗浄することが望ましい。上記エタノール等の有機溶剤中で超音波洗浄を使用することによって、余分な酸化変色防止剤を除去し、むらのない均一な酸化変色防止膜を形成することができる。有機溶剤としてこの他、メタノール、プロパノール、イソプロパノール、ブタノール、イソプタノール、アセトン等を使用することができる。
【０００９】
さらに、上記エタノール超音波洗浄等による洗浄後、窒素ガス等の不活性ガス吹き付けによる乾燥処理を施すことが望ましい。これによって、銅又は銅合金製スパッタリングターゲット用バッキングプレートのベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物からなる酸化変色防止剤による酸化変色防止機能をさらに向上かつ安定化させることができる。
次に、本件発明を実施例に基づいて説明する。なお、以下に示す実施例等は、本件発明の好適な一例を示すもので、これによって本件発明を制限するものではない。すなわち、本件発明は明細書全体に亘って記載される技術思想の中で実施例以外の変形や態様を全て包含するものである。
【００１０】
【実施例及び比較例】
無酸素銅製のバッキングプレートφ約４００ｍｍ×厚さ約５ｍｍ、高さ約８０ｍｍを、５−メチル・１Ｈベンゾトリアゾールをエタノールに０．１グラム／リットルの割合で溶解した溶液に１５秒間浸漬した。
浸漬後、バッキングプレート表面の溶液が乾燥しない内に、超音波洗浄器にて超音波振動を与えたエタノール中に５秒間浸漬した後、これをさらに窒素ガスを吹き付けて乾燥させた。
比較例として、同無酸素銅製のバッキングプレートを超音波洗浄器にて超音波振動を与えたエタノール中に５秒間浸漬して、窒素ガスを吹き付けて乾燥させたバッキングプレートを作製した。
このような処理を行ったバッキングプレートを湿度９０％、温度６０°Ｃの恒湿恒温槽に４８時間保持（高湿、高温処理による加速試験）し、その結果を目視により観察し、変色の程度を判定した。
この結果を、表１に示す。
【００１１】
【表１】
上記の結果、銅製バッキングプレートの表面に酸化変色防止膜が形成されていることが確認できた。次に、この酸化変色防止膜を形成した銅製バッキングプレートを使用し、該銅製バッキングプレートにチタンターゲットを接合してスパッタリングを実施した。
これによると、スパッタ中のチャンバー内雰囲気の質量分析結果から５−メチル・１Ｈベンゾトリアゾールとエタノールを使用した場合に検出されると考えられる１２Ｃ＋、１５ＣＨ３ ＋のイオンは全く検出されなかった。
【００１３】
また、本発明のこのようなバッキングプレートを多数回使用しても、従来のバッキングプレートの酸化変色に起因すると考えられるような、例えば真空シール部に発生した場合のスパッタ装置内の真空度が上がらないという事故は全くなかった。さらに、バッキングプレートの酸化変色部が減少するに伴い、それが剥離する率も大幅に減少し、パーティクルの原因となることもなかった。
また、バッキングプレートを再生使用する際に除去しなければならない酸化変色部も減少するので、再生処理が極めて容易となり、そのための再生コストを著しく減少できるという効果があった。
以上から、銅又は銅合金製スパッタリングターゲット用バッキングプレートの酸化変色を防止し、運搬や保管の期間を延ばすことができるようにすると共に、スパッタリングプロセスの高度な清浄雰囲気において使用できるバッキングプレートを提供することが可能となった。
【００１４】
【発明の効果】
本発明は、ベンゾトリアゾール若しくはその誘導体又はイミダゾールシラン等のアゾール系化合物からなる酸化変色防止剤をバッキングプレートに施すことにより、運搬や保管の際に銅又は銅合金製スパッタリングターゲット用バッキングプレートの酸化変色を効果的に抑制できるという優れた特徴を有する。
しかもこの酸化変色防止剤は、スパッタリングプロセス中において汚染源となることがなく、高度な清浄雰囲気において使用できるという著しい効果を有する。
これによって、本発明による銅および銅合金製スパッタリングターゲット用バッキングプレートは、スパッタプロセスをより安定化させ、信頼性の高い銅および銅合金の薄膜形成を可能にするものである。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a copper or copper alloy sputtering target backing plate that can be used in a highly clean atmosphere of a sputtering process by subjecting a copper or copper alloy backing plate to an oxidation discoloration prevention treatment, and a method for treating the same.
[0002]
[Prior art]
Copper (such as oxygen-free copper) and copper alloys (such as Cu—Cr alloy, phosphor bronze, and beryllium copper) are widely used for the backing plate of the sputtering target. Such a backing plate is usually bonded to a target with a bonding agent such as indium, and after the target is used, it is used several times by bonding a new target again.
The backing plate is bonded to the target and finally shipped after being vacuum-packed or packed with argon gas, but the backing plate changes color when it is transported or stored.
For this reason, packing work is performed in a clean room in which humidity and temperature are controlled. However, copper is a metal that easily discolors, and the target may discolor during transportation and storage. In particular, when the storage period is long, discoloration is remarkable.
Although there is no clear conclusion about the cause of this discoloration, it has been confirmed that copper oxide is generated in the discolored portion, and therefore discoloration due to oxidation is considered to be the main cause. Accordingly, here, such discoloration is referred to as “oxidation discoloration”.
[0003]
Such oxidation discoloration of the backing plate causes, for example, the vacuum degree in the sputtering apparatus not to increase when it occurs in the vacuum seal portion, and causes particles when the oxidation portion peels off. There was a case where the value was greatly lost.
In addition, there is a problem that the cooling efficiency is lowered in contact with the cooling water. Such oxidative discoloration must be removed when the backing plate is used again, which increases the regeneration cost.
Therefore, it is possible to prevent oxidation discoloration of the copper or copper alloy sputtering target backing plate, extend the period of transportation and storage, and can be used in a highly clean atmosphere of the sputtering process. Needed.
[0004]
[Problems to be solved by the invention]
As described above, the present invention provides a copper and copper alloy backing plate that can be used in a highly clean atmosphere of the sputtering process while extending the period of transportation and storage of the copper or copper alloy backing plate, reducing the regeneration cost. Is an issue.
[0005]
[Means for Solving the Problems]
As a result of intensive research aimed at preventing oxidation discoloration of the backing plate, the present inventors solved the above problem by applying a specific oxidation discoloration inhibitor to the copper or copper alloy sputtering target backing plate. I learned that I can do it.
The present invention is based on this finding,
1 Backing plate for sputtering target made of copper or copper alloy, which is provided with an oxidative discoloration inhibitor comprising benzotriazole or a derivative thereof or an azole compound such as imidazole silane. 2 Backing plate made of copper or copper alloy is made of benzotriazole or Backing for a sputtering target made of copper or copper alloy, which is immersed in a solution of an oxidative discoloration inhibitor comprising the derivative or an azole compound such as imidazole silane or sprayed on a copper or copper alloy backing plate 3. Method for preventing oxidation discoloration of plate 3 After the treatment with an oxidation discoloration inhibitor comprising an azole compound such as benzotriazole or a derivative thereof or imidazole silane, ultrasonic cleaning is performed in an organic solvent, There is provided an oxidation discoloration prevention processing method for alloy sputtering target for the backing plate.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
In the present invention, benzotriazole or a derivative thereof or an azole compound such as imidazolesilane as an oxidation discoloration inhibitor for a copper or copper alloy sputtering target backing plate extends the transportation and storage period of the target, thereby further stabilizing the sputtering process. It was found that the method is extremely effective for forming a thin film of copper and copper alloy with high reliability.
As shown in the examples described later, such an oxidative discoloration inhibitor does not become a harmful substance for forming a thin film by sputtering, and can effectively prevent oxidative discoloration.
Conventionally, benzotriazole or the like is a material generally known as an oxidative discoloration inhibitor for copper or a copper alloy material, but it cannot be used for a backing plate. This is because an oxidation discoloration inhibitor such as benzotriazole may become a contaminant during sputtering.
[0007]
However, as shown in the Examples described later, it was found that there was no contamination due to the oxidative discoloration inhibitor comprising benzotriazole or a derivative thereof or an azole compound such as imidazole silane.
This makes it possible to use a backing plate coated with an oxidative discoloration inhibitor made of benzotriazole or a derivative thereof or an azole compound such as imidazole silane for sputtering, and this oxidative discoloration preventive agent can be used for transportation and storage. In particular, it has an excellent feature that it can effectively suppress oxidative discoloration of a copper or copper alloy sputtering target backing plate.
Specific examples of azole compounds such as benzotriazole or derivatives thereof or imidazolesilane include 1,2,3-benzotriazole, 1 [(2ethylhexylamino) methyl] benzotriazole, 5-methyl-1H benzotriazole, 2- Examples include aminoimidazole, 2- (hydroxyethylamino) imidazole, and 2-aminobenzimidazole.
As described above, it has become possible to provide a copper and copper alloy sputtering target backing plate that can be used in a highly clean atmosphere of the sputtering process while extending the period of transportation and storage of the copper or copper alloy backing plate. .
[0008]
Application of oxidation discoloration inhibitor consisting of benzotriazole or its derivatives or azole compounds such as imidazole silane to copper or copper alloy backing plate is immersed in a solution consisting of azole compounds such as benzotriazole or its derivatives or imidazole silane Or by spraying the solution onto a copper or copper alloy backing plate.
It is desirable to perform ultrasonic cleaning in an organic solvent such as ethanol after the treatment of the copper or copper alloy sputtering target backing plate with the oxidation discoloration inhibitor. By using ultrasonic cleaning in an organic solvent such as ethanol, an excess oxidation discoloration inhibitor can be removed, and a uniform oxidation discoloration prevention film without unevenness can be formed. In addition, methanol, propanol, isopropanol, butanol, iseptanol, acetone and the like can be used as the organic solvent.
[0009]
Furthermore, it is desirable to perform a drying process by blowing an inert gas such as nitrogen gas after the above-described ethanol ultrasonic cleaning or the like. Thereby, the oxidation discoloration prevention function by the oxidation discoloration prevention agent comprising an azole compound such as benzotriazole or a derivative thereof or imidazole silane of the copper or copper alloy sputtering target backing plate can be further improved and stabilized.
Next, this invention is demonstrated based on an Example. In addition, the Example shown below shows a suitable example of this invention, and does not restrict | limit this invention by this. That is, the present invention includes all modifications and modes other than the embodiments in the technical idea described throughout the specification.
[0010]
[Examples and Comparative Examples]
An oxygen-free copper backing plate φ of about 400 mm × thickness of about 5 mm and height of about 80 mm was immersed in a solution of 5-methyl · 1H benzotriazole dissolved in ethanol at a rate of 0.1 g / liter for 15 seconds.
After the immersion, the solution on the surface of the backing plate was not dried, but was immersed for 5 seconds in ethanol subjected to ultrasonic vibration with an ultrasonic cleaner, and then this was further dried by blowing nitrogen gas.
As a comparative example, a backing plate made of the oxygen-free copper was immersed in ethanol subjected to ultrasonic vibration for 5 seconds with an ultrasonic cleaner, and dried by blowing nitrogen gas.
The backing plate subjected to such treatment is kept in a thermo-hygrostat at a humidity of 90% and a temperature of 60 ° C. for 48 hours (acceleration test by high-humidity and high-temperature treatment), and the result is visually observed to determine the degree of discoloration. Was judged.
The results are shown in Table 1.
[0011]
[Table 1]
As a result, it was confirmed that an oxidation discoloration prevention film was formed on the surface of the copper backing plate. Next, a copper backing plate on which this oxidation discoloration preventing film was formed was used, and a titanium target was joined to the copper backing plate to carry out sputtering.
According to this, 12 C + and 15 CH 3 + ions, which are considered to be detected when 5-methyl · 1H benzotriazole and ethanol are used, are not detected at all from the mass analysis result of the atmosphere in the chamber during sputtering. It was.
[0013]
Further, even when such a backing plate of the present invention is used many times, the degree of vacuum in the sputtering apparatus when it occurs in, for example, a vacuum seal portion, which is thought to be caused by oxidation discoloration of the conventional backing plate, is increased. There was no accident. Furthermore, as the oxidation discoloration portion of the backing plate decreased, the rate at which the backing plate peeled off was significantly reduced, and no particles were caused.
In addition, since the oxidation discoloration portion that must be removed when the backing plate is recycled and used is reduced, the recycling process becomes extremely easy, and the cost for the reproduction can be significantly reduced.
As described above, it is possible to prevent oxidation discoloration of a copper or copper alloy sputtering target backing plate, extend the period of transportation and storage, and provide a backing plate that can be used in a highly clean atmosphere of a sputtering process. It became possible.
[0014]
【The invention's effect】
The present invention provides an oxidation discoloration inhibitor made of benzotriazole or a derivative thereof or an azole compound such as imidazole silane to the backing plate, thereby oxidizing the discoloration of the copper or copper alloy sputtering target backing plate during transportation or storage. It has the outstanding characteristic that it can suppress effectively.
Moreover, this oxidation discoloration inhibitor does not become a contamination source during the sputtering process, and has a remarkable effect that it can be used in a highly clean atmosphere.
As a result, the copper and copper alloy sputtering target backing plate according to the present invention stabilizes the sputtering process and enables highly reliable copper and copper alloy thin film formation.
Claims (3)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000268021A JP4409071B2 (en) | 2000-09-05 | 2000-09-05 | Backing plate for sputtering target made of copper or copper alloy and processing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| JP2000268021A JP4409071B2 (en) | 2000-09-05 | 2000-09-05 | Backing plate for sputtering target made of copper or copper alloy and processing method thereof |
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| JP2002069630A JP2002069630A (en) | 2002-03-08 |
| JP4409071B2 true JP4409071B2 (en) | 2010-02-03 |
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| EP1556526B1 (en) * | 2002-10-21 | 2009-03-11 | Cabot Corporation | Method of forming a sputtering target assembly and assembly made therefrom |
| CN104513952B (en) * | 2013-09-30 | 2017-07-11 | 宁波江丰电子材料股份有限公司 | The preparation method and target material assembly of target material assembly |
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