JP2009114531A - SnO2系スパッタリングターゲット - Google Patents
SnO2系スパッタリングターゲット Download PDFInfo
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- 238000005477 sputtering target Methods 0.000 title claims abstract description 34
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 33
- 238000004544 sputter deposition Methods 0.000 abstract description 20
- 230000002093 peripheral effect Effects 0.000 abstract description 7
- 238000004299 exfoliation Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 44
- 239000000843 powder Substances 0.000 description 16
- 239000000758 substrate Substances 0.000 description 12
- 238000011156 evaluation Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 238000005245 sintering Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910000410 antimony oxide Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000181 anti-adherent effect Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- XXLJGBGJDROPKW-UHFFFAOYSA-N antimony;oxotin Chemical compound [Sb].[Sn]=O XXLJGBGJDROPKW-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
【解決手段】本発明のSnO2系スパッタリングターゲットは、10ppmを越え1質量%未満のSb2O3と、合計質量が20質量%以下であるTa2O5および/またはNb2O5と、残部としてのSnO2および不可避不純物とからなる焼結体からなる。
【選択図】図1
Description
本発明によるSnO2系スパッタリングターゲットは、10ppmを越え1質量%未満のSb2O3と、合計質量が20質量%以下、好ましくは1〜20質量%であるTa2O5および/またはNb2O5と、残部としてのSnO2および不可避不純物とからなる焼結体からなる。このようなSnO2系焼結体をスパッタリングターゲットとして使用すると、膜応力が絶対値で小さいスパッタ膜が得られ、スパッタリングの際にスパッタカソードの周辺構造物からの膜剥離を少なくすることができる。
本発明によるSnO2系スパッタリングターゲットの製造方法は特に限定されないが、以下に示される好ましい態様に従い行うことができる。すなわち、本発明の好ましい態様によれば、まず、SnO2を主成分とし、Sb2O3を10ppmを越え1質量%未満含み、Ta2O5および/またはNb2O5を合計質量で20質量%以下含む、未焼結の成形体を用意する。本発明において未焼結の成形体は、上記組成を含む原料粉を成形したものであればいかなる方法により成形されたものであってもよく、例えば、SnO2粉末、Sb2O3粉末、Ta2O5粉末、およびNb2O5粉末を上記組成を満たすような配合量比で混合して原料粉を調製し、この原料粉を成形することにより作製することができる。
(1)スパッタリングターゲットの作製
まず、以下の4種類の原料粉末を用意した。
SnO2粉末:純度99.99%(4N)、平均粒径0.7〜1.1μm、比表面積2.0〜2.7m2/g
Ta2O5粉末:純度99.9%(3N)、平均粒径0.6〜0.8μm、比表面積2.0〜3.1m2/g
Nb2O5粉末:純度99.9%(3N)、平均粒径0.6〜1.0μm、比表面積2.1〜2.7m2/g
Sb2O3粉末:純度99.9%(3N)、平均粒径0.6〜1.0μm、
各例について、上記4種類の原料粉末を、それぞれ秤量し、ドライボールミルで21時間混合した。この混合粉にポリビニルアルコール水溶液を添加し、充分混合した後、400×800mm寸法の金型に充填し、800kgf/cm2の圧力にてプレス成形した。この成形体を80℃で12時間乾燥させた。この乾燥体を、酸素雰囲気下で、表1に示される焼成温度で8時間焼成し、焼結体を得た。この際、昇温速度は400℃/時間、降温速度は100℃/時間に制御した。得られた焼結体を直径152.4mm、厚さ5mmの大きさに機械加工して、SnO2系スパッタリングターゲットを得た。また、焼結体の加工端材について、乳鉢を用いて粉砕し、テフロン(登録商標)製容器に、その粉砕粉、硝酸と塩酸の混酸、および超純水を加え加水分解した後、定溶液とした。得られた定溶液中のTa、Nb、およびSbの各元素の測定を、ICP質量分析装置(Agilent社製4500)を用いて、ICP質量分析法で行った。酸化物換算した値を表1に示す。
得られたスパッタリングターゲットについて、以下に示される各種評価試験を行った。
各スパッタリングターゲットの相対密度をアルキメデス法により測定した。このとき、各原料の密度をSnO2:6.95g/cm3、Ta2O5:8.74g/cm3、Nb2O5:4.47g/cm3として加重平均密度(理論密度)を算出し、この加重平均密度を100%として相対密度を算出した。その結果は、表1に示される通りであった。
例1〜37で得られたスパッタリングターゲットを無酸素銅製のバッキングプレートにメタルボンディングした。そして、メタルボンディングした各スパッタリングターゲットについて、以下に示されるスパッタ条件で、直流電源を用いたスパッタリングを行い、シリコンウェーハにスパッタ成膜した。
カソード:強磁場磁気回路
ターゲット/基板間距離:50mm
スパッタ室到達圧力:<1×10−4Pa
基板温度:室温(加熱無し)
導入ガス:アルゴン+酸素(酸素濃度1体積%)
導入ガス分圧:0.67Pa
直流印加電力:360W
膜厚:500nm
基板:φ4inch×525μm シリコンウェーハ
σ=Eb2/{6(1‐ν)*rd}
σ:応力
E:基板のヤング率
b:基板の厚さ
ν:基板のポアソン比
d:膜厚
r:成膜後の基板の曲率半径(ニュートン法により測定)
例1〜37で得られたスパッタリングターゲットを、図1に示されるスパッタリング装置を用いて以下の通りにして膜剥離の評価を行った。図1に示されるスパッタリング装置は、チャンバー1内に、ターゲット2が載置されるためのバッキングプレート3と、バッキングプレート3と対向して設けられる基板ホルダー4とを備えてなる。そして、チャンバー1内には、ターゲット2およびバッキングプレート3の側面を保護するアースシールド5と、チャンバー1への被膜形成を防止する防着板6とがさらに設けられる。
カソード:強磁場磁気回路
スパッタ室到達圧力:<1×10−4Pa
導入ガス:アルゴン+酸素(酸素濃度1体積%)
導入ガス分圧:0.67Pa
直流印加電力:360W
膜厚:500nm
スパッタ時間:連続30hr放電
アースシールド:アランダム#60ブラスト処理品
基板ホルダー:アランダム#60ブラスト処理品
防着板:アランダム#60ブラスト処理品
2 ターゲット
3 バッキングプレート
4 基板ホルダー
5 アースシールド
6 防着版
Claims (5)
- 10ppmを越え1質量%未満のSb2O3と、合計質量が20質量%以下であるTa2O5および/またはNb2O5と、残部としてのSnO2および不可避不純物とからなる焼結体からなる、SnO2系スパッタリングターゲット。
- Sb2O3の含有量が11〜9000ppmである、請求項1に記載のスパッタリングターゲット。
- Sb2O3の含有量が100〜6000ppmである、請求項1に記載のスパッタリングターゲット。
- Sb2O3の含有量が300〜2000ppmである、請求項1に記載のスパッタリングターゲット。
- Ta2O5の含有量が0〜15質量%であり、かつNb2O5の含有量が0〜15質量%である、請求項1〜4に記載のスパッタリングターゲット。
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JP2007291592A JP5249560B2 (ja) | 2007-11-09 | 2007-11-09 | SnO2系スパッタリングターゲット |
CNA2008800012016A CN101568665A (zh) | 2007-11-09 | 2008-11-06 | SnO2系溅射靶 |
PCT/JP2008/070215 WO2009060901A1 (ja) | 2007-11-09 | 2008-11-06 | SnO2系スパッタリングターゲット |
KR1020097010025A KR101138700B1 (ko) | 2007-11-09 | 2008-11-06 | SnO2계 스퍼터링 타겟 |
TW097143165A TWI406963B (zh) | 2007-11-09 | 2008-11-07 | Tin oxide sputtering target |
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JP2013507526A (ja) * | 2009-10-15 | 2013-03-04 | ユミコア エセ.アー. | 酸化スズセラミックスパッタリングターゲットおよびその製造方法 |
WO2017022499A1 (ja) * | 2015-08-04 | 2017-02-09 | 三井金属鉱業株式会社 | 酸化スズ、燃料電池用電極触媒、膜電極接合体及び固体高分子形燃料電池 |
WO2018220953A1 (ja) * | 2017-05-30 | 2018-12-06 | 株式会社アルバック | 透明導電膜 |
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JPH0853761A (ja) * | 1993-07-28 | 1996-02-27 | Asahi Glass Co Ltd | 透明電導膜の製造方法 |
JP3957917B2 (ja) * | 1999-03-26 | 2007-08-15 | 三井金属鉱業株式会社 | 薄膜形成用材料 |
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JPH0853761A (ja) * | 1993-07-28 | 1996-02-27 | Asahi Glass Co Ltd | 透明電導膜の製造方法 |
JP3957917B2 (ja) * | 1999-03-26 | 2007-08-15 | 三井金属鉱業株式会社 | 薄膜形成用材料 |
Cited By (6)
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JP2013507526A (ja) * | 2009-10-15 | 2013-03-04 | ユミコア エセ.アー. | 酸化スズセラミックスパッタリングターゲットおよびその製造方法 |
WO2017022499A1 (ja) * | 2015-08-04 | 2017-02-09 | 三井金属鉱業株式会社 | 酸化スズ、燃料電池用電極触媒、膜電極接合体及び固体高分子形燃料電池 |
US20180175398A1 (en) * | 2015-08-04 | 2018-06-21 | Mitsui Mining & Smelting Co., Ltd. | Tin oxide, electrode catalyst for fuel cells, membrane electrode assembly, and solid polymer fuel cell |
US10615425B2 (en) | 2015-08-04 | 2020-04-07 | Mitsui Mining & Smelting Co., Ltd. | Tin oxide, electrode catalyst for fuel cells, membrane electrode assembly, and solid polymer fuel cell |
WO2018220953A1 (ja) * | 2017-05-30 | 2018-12-06 | 株式会社アルバック | 透明導電膜 |
JP2018206467A (ja) * | 2017-05-30 | 2018-12-27 | 株式会社アルバック | 透明導電膜 |
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JP5249560B2 (ja) | 2013-07-31 |
WO2009060901A1 (ja) | 2009-05-14 |
KR101138700B1 (ko) | 2012-04-19 |
CN101568665A (zh) | 2009-10-28 |
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