JP5750063B2 - 酸化物焼結体およびスパッタリングターゲット - Google Patents
酸化物焼結体およびスパッタリングターゲット Download PDFInfo
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- JP5750063B2 JP5750063B2 JP2012025475A JP2012025475A JP5750063B2 JP 5750063 B2 JP5750063 B2 JP 5750063B2 JP 2012025475 A JP2012025475 A JP 2012025475A JP 2012025475 A JP2012025475 A JP 2012025475A JP 5750063 B2 JP5750063 B2 JP 5750063B2
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- 238000005477 sputtering target Methods 0.000 title claims description 48
- 239000011701 zinc Substances 0.000 claims description 42
- 238000005259 measurement Methods 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 23
- 238000005245 sintering Methods 0.000 claims description 23
- 238000004453 electron probe microanalysis Methods 0.000 claims description 22
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- 238000013507 mapping Methods 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000011787 zinc oxide Substances 0.000 claims description 8
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 7
- 229910001887 tin oxide Inorganic materials 0.000 claims description 7
- 229910003437 indium oxide Inorganic materials 0.000 claims description 6
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 description 34
- 239000010409 thin film Substances 0.000 description 28
- 239000004065 semiconductor Substances 0.000 description 27
- 239000010408 film Substances 0.000 description 25
- 150000001875 compounds Chemical class 0.000 description 19
- 238000000034 method Methods 0.000 description 15
- 238000000465 moulding Methods 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 10
- 239000002994 raw material Substances 0.000 description 10
- 229910007604 Zn—Sn—O Inorganic materials 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 229910006404 SnO 2 Inorganic materials 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 239000004677 Nylon Substances 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 229920001778 nylon Polymers 0.000 description 6
- 230000002159 abnormal effect Effects 0.000 description 5
- 230000002411 adverse Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 229910007541 Zn O Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000009694 cold isostatic pressing Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 229910020923 Sn-O Inorganic materials 0.000 description 2
- 229910018956 Sn—In Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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Description
[In]/([Zn]+[Sn]+[In])=0.01〜0.30
[Sn]/([Zn]+[Sn])=0.20〜0.60
[In]/([Zn]+[Sn]+[In])=0.10〜0.30
[Sn]/([Zn]+[Sn])=0.33〜0.60
(ア)測定面積中に占める、Sn濃度が10〜50質量%の領域の比率が70面積%以上である。
(イ)好ましくは、測定面積中に占める、In濃度が2〜35質量%の領域の比率が70面積%以上である。
5質量%の領域をIn2-35と呼ぶ場合がある。
分析装置:JEOL製「電子線マイクロアナライザー JXA8900RL」
分析条件
加速電圧:15.0kV
照射電流:5.012×10-8A
ビーム径:最小(0μm)
測定時間:100.00ms
測定点数:400×400
測定間隔:1μm
測定面積:400μm×400μm
測定位置:板厚方向中央部
測定視野数:1視野
本発明の酸化物焼結体は、測定面積中、Sn濃度が10〜50質量%の領域Sn10-50の占める比率が70面積%以上に制御されている。これにより、ZnO、SnO2、およびIn2O3がほぼ均一に分布するようになり、酸化物焼結体の相対密度向上および比抵抗の低減に大きく寄与するIn−Zn−Sn−O系化合物が、多く存在するようになる。また、上記構成とすることにより、少ないIn量(後記するように、本発明では[In]比の好ましい範囲は0.01〜0.30であり、より好ましくは0.10〜0.30)であっても、低い比抵抗(1Ω・cm以下)と、高い相対密度(90%以上)を実現することができる。
本発明の酸化物焼結体は、好ましくは、測定面積中、In濃度が2〜35質量%の領域In2-35の占める比率が70面積%以上に制御されている。In濃度が2〜35質量%の領域は、その大部分がSn濃度10〜50質量%の領域と重複していることから、上記(イ)の要件を満足することは、前述したIn−Zn−Sn−O系化合物が、測定面積中に多数(70面積%以上)存在することを実質的に意味していると推定される。
本発明の酸化物焼結体は、相対密度が非常に高く、好ましくは90%以上であり、より好ましくは95%以上である。高い相対密度は、スパッタリング中での割れやノジュールの発生を防止し得るだけでなく、安定した放電をターゲットライフまで連続して維持するなどの利点をもたらす。
本発明の酸化物焼結体は、比抵抗が小さく、1Ω・cm以下であることが好ましく、より好ましくは0.1Ω・cm以下である。これにより、直流電源を用いたプラズマ放電などによる直流スパッタリング法による成膜が可能となり、スパッタリングターゲットを用いた物理蒸着(スパッタリング法)を表示装置の生産ラインで効率よく行うことができる。
純度99.99%の酸化亜鉛粉末、純度99.99%の酸化スズ粉末、および純度99.99%の酸化インジウム粉末を[Zn]:[Sn]:[In]=40.0:40.0:20.0の比率で配合し、ナイロンボールミルで20時間混合した。次に、上記工程で得られた混合粉末を乾燥、造粒し、金型プレスにて成形圧力0.5tonf/cm2で予備成形した後、CIPにて成形圧力3tonf/cm2で本成形を行った。このようにして得られた成形体を、1500℃で保持して焼結を行なった。
前述した実験例1の各原料粉末を、[Zn]:[Sn]:[In]=40.0:40.0:20.0の比率で配合し、ナイロンボールミルで20時間混合した。次に、上記工程で得られた混合粉末を乾燥、造粒し、金型プレスにて成形圧力0.5tonf/cm2で予備成形した後、黒鉛型に成形体を装填し、黒鉛型内で30MPaに加圧かつ1100℃で保持して焼結を行ない実験例2の酸化物焼結体を得た。
前述した実験例1において、[Zn]:[Sn]:[In]=48.0:32.0:20.0の比率で配合し、成形体を1600℃で焼結した後、窒素ガス雰囲気にて900℃で6時間熱処理したこと以外は、上記実験例1と同様にして実験例3の酸化物焼結体を得た。
前述した実験例1の各原料粉末を、[Zn]:[Sn]:[In]=53.3:26.7:20.0の比率で配合し、ナイロンボールミルで20時間混合した。次に、上記工程で得られた混合粉末を乾燥、造粒し、金型プレスにて成形圧力0.5tonf/cm2で予備成形した後、黒鉛型に成形体を装填し、黒鉛型内で30MPaに加圧かつ1050℃で保持して焼結を行ない実験例4の酸化物焼結体を得た。
前述した実験例1の各原料粉末を、[Zn]:[Sn]:[In]=45.0:45.0:10.0の比率で配合し、ナイロンボールミルで20時間混合した。次に、上記工程で得られた混合粉末を乾燥、造粒し、金型プレスにて成形圧力0.5tonf/cm2で予備成形した後、黒鉛型に成形体を装填し、黒鉛型内で30MPaに加圧かつ1150℃で保持して焼結を行ない実験例5の酸化物焼結体を得た。
前述した実験例1の各原料粉末を、[Zn]:[Sn]:[In]=48.5:48.5:3.0の比率で配合し、ナイロンボールミルで20時間混合した。次に、上記工程で得られた混合粉末を乾燥、造粒し、金型プレスにて成形圧力0.5tonf/cm2で予備成形した後、黒鉛型に成形体を装填し、黒鉛型内で30MPaに加圧かつ1075℃で保持して焼結を行ない実験例6の酸化物焼結体を得た。
前述した実験例1において、[Zn]:[Sn]:[In]=35.0:35.0:30.0の比率で配合し、成形体を1450℃で保持して焼結したこと以外は、上記実験例1と同様にして実験例7の酸化物焼結体を得た。
前述した実験例1において、[Zn]:[Sn]:[In]=64.0:16.0:20.0の比率で配合し、成形体を1300℃で保持して焼結したこと以外は、上記実験例1と同様にして実験例8の酸化物焼結体を得た。
前述した実験例1において、炉内に成形体を800℃で5時間保持して焼結した後、窒素ガス雰囲気にて750℃で8時間熱処理したこと以外は、上記実験例1と同様にして比較例1の酸化物焼結体を得た。
Claims (6)
- 酸化亜鉛と、酸化スズと、酸化インジウムの各粉末と、を混合および焼結して得られる酸化物焼結体であって、
前記酸化物焼結体に対してEPMAによる面内組成マッピングを行なったとき、測定面積中に占める、Sn濃度が10〜50質量%の領域の比率が70面積%以上であり、かつ前記酸化物焼結体に含まれる金属元素の含有量(原子%)をそれぞれ、[Zn]、[Sn]、[In]としたとき、[Zn]+[Sn]+[In]に対する[In]の比は、下式を満足し、かつ相対密度90%以上、比抵抗1Ω・cm以下であることを特徴とする酸化物焼結体。
[In]/([Zn]+[Sn]+[In])=0.01〜0.30 - 前記酸化物焼結体に対してEPMAによる面内組成マッピングを行なったとき、測定面積中に占める、In濃度が2〜35質量%の領域の比率が70面積%以上であることを特徴とする請求項1に記載の酸化物焼結体。
- 前記酸化物焼結体に含まれる金属元素の含有量(原子%)をそれぞれ、[Zn]、[Sn]、[In]としたとき、[Zn]+[Sn]に対する[Sn]の比は、下式を満足するものである請求項1または2に記載の酸化物焼結体。
[Sn]/([Zn]+[Sn])=0.20〜0.60 - [Zn]+[Sn]+[In]に対する[In]の比は、下式を満足するものである請求項1〜3のいずれかに記載の酸化物焼結体。
[In]/([Zn]+[Sn]+[In])=0.10〜0.30 - [Zn]+[Sn]に対する[Sn]の比は、下式を満足するものである請求項3または4に記載の酸化物焼結体。
[Sn]/([Zn]+[Sn])=0.33〜0.60 - 請求項1〜5のいずれかに記載の酸化物焼結体を用いて得られるスパッタリングターゲットであって、相対密度90%以上、比抵抗1Ω・cm以下であることを特徴とするスパッタリングターゲット。
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