JP5318932B2 - 酸化物焼結体およびスパッタリングターゲット、並びにその製造方法 - Google Patents
酸化物焼結体およびスパッタリングターゲット、並びにその製造方法 Download PDFInfo
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- JP5318932B2 JP5318932B2 JP2011242892A JP2011242892A JP5318932B2 JP 5318932 B2 JP5318932 B2 JP 5318932B2 JP 2011242892 A JP2011242892 A JP 2011242892A JP 2011242892 A JP2011242892 A JP 2011242892A JP 5318932 B2 JP5318932 B2 JP 5318932B2
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- 238000005477 sputtering target Methods 0.000 title claims description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 100
- 239000011701 zinc Substances 0.000 claims description 87
- 238000005245 sintering Methods 0.000 claims description 70
- 239000011787 zinc oxide Substances 0.000 claims description 49
- 239000013078 crystal Substances 0.000 claims description 32
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 229910003437 indium oxide Inorganic materials 0.000 claims description 12
- 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 12
- 238000002441 X-ray diffraction Methods 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 230000002159 abnormal effect Effects 0.000 description 31
- 238000004544 sputter deposition Methods 0.000 description 28
- 238000000034 method Methods 0.000 description 23
- 239000010936 titanium Substances 0.000 description 20
- 239000004065 semiconductor Substances 0.000 description 19
- 239000011777 magnesium Substances 0.000 description 18
- 239000010955 niobium Substances 0.000 description 16
- 239000010408 film Substances 0.000 description 15
- 230000008569 process Effects 0.000 description 15
- 238000005336 cracking Methods 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- 239000010409 thin film Substances 0.000 description 11
- 239000012298 atmosphere Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 238000005259 measurement Methods 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 229910007541 Zn O Inorganic materials 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005238 degreasing Methods 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 239000004677 Nylon Substances 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
- 238000002447 crystallographic data Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910020923 Sn-O Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 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
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Description
0.27≦[In]/[Zn]≦0.45
([Ti]+[Mg]+[Al]+[Nb])/([Zn]+[In]+[Ti]+[Mg]+[Al]+[Nb])≦0.05
0.1≦ZnmIn2O3+m/(ZnmIn2O3+m+In2O3+ZnO)<0.75
0.05≦In2O3/(ZnmIn2O3+m+In2O3+ZnO)≦0.7
0.05≦ZnO/(ZnmIn2O3+m+In2O3+ZnO)≦0.7
(但し、ZnmIn2O3+mはZn5In2O8、Zn6In2O9、Zn7In2O10の合計である。)
分析装置:理学電機製「X線回折装置RINT−1500」
分析条件:
ターゲット:Cu
単色化:モノクロメートを使用(Kα)
ターゲット出力:40kV−200mA
(連続測定)θ/2θ走査
スリット:発散1/2°、散乱1/2°、受光0.15mm
モノクロメータ受光スリット:0.6mm
走査速度:2°/min
サンプリング幅:0.02°
測定角度(2θ):5〜90°
参考文献(1)M.Nakamura, N.Kimizuka and T.Mohri: J. Solid State Chem. 86(1990) 16-40
参考文献(2)M.Nakamura, N.Kimizuka, T.Mohri and M.Isobe: J. Solid State Chem. 105(1993) 535-549
ZnmIn2O3+m化合物(相)は、本発明の酸化物焼結体を構成する酸化亜鉛と酸化インジウムが結合して形成されるものである。この化合物の結晶構造は六方晶であり、酸化物焼結体のキャリア移動度向上に大きく寄与すると共に、後記するIn2O3、及びZnOと共に含有させることによって、異常放電を大幅に抑制する効果を発現する。
本発明の酸化物焼結体は、相対密度が非常に高く、95%以上であり、好ましくは97%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、0.1Ω・cm以下であり、好ましくは0.01Ω・cm以下である。これにより、異常放電を抑制でき、一層スパッタリング中での異常放電を抑制した成膜が可能となり、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。
相対密度は、スパッタリング後、ターゲットをバッキングプレートから取り外して鏡面研磨し、反射電子顕微鏡(SEM)で観察して気孔率を測定して求めた。具体的にはSEM観察(1000倍)して写真撮影し、50μm角の領域における気孔占有面積率を測定して気孔率とした。異なる任意の20視野を観察し、その平均値を当該試料の平均気孔率とした。100%から気孔率を引いた値を焼結体の相対密度(%)とした。相対密度は95%以上を合格と評価した。
焼結体の比抵抗は、上記製作したスパッタリングターゲットについて四端子法により測定した。比抵抗は0.1Ω・cm以下を合格と評価した。
各結晶相の比率は、スパッタリング後、ターゲットをバッキングプレートから取り外して10mm角の試験片を切出し、X線回折で回折線の強度を測定して求めた。
分析条件:
ターゲット:Cu
単色化:モノクロメートを使用(Kα)
ターゲット出力:40kV−200mA
(連続測定)θ/2θ走査
スリット:発散1/2°、散乱1/2°、受光0.15mm
モノクロメータ受光スリット:0.6mm
走査速度:2°/min
サンプリング幅:0.02°
測定角度(2θ):5〜90°
[ZnmIn2O3+m]=I(ZnmIn2O3+m)/(I(ZnmIn2O3+m)+I(In2O3)+I(ZnO))
[In2O3]=I(In2O3)/(I(ZnmIn2O3+m)+I(In2O3)+I(ZnO))
[ZnO]=I(ZnO)/(I(ZnmIn2O3+m)+I(In2O3)+I(ZnO))
異常放電は、スパッタリング中の異常放電の回数を測定して評価した。具体的には、1分間のスパッタリングを300回繰り返し、スパッタリング後に取り出したターゲットを目視で観察し、異常放電の痕跡、および割れの個数を数えることで求めた。異常放電は、異常放電回数が6回以下を合格と評価した。また割れはターゲットに割れが発生していない場合を合格とした。
キャリア移動度は、上記のスパッタリング条件で成膜した薄膜を用いて作成したチャネル長10μm、チャネル幅100μmの薄膜トランジスタの移動度を測定した。キャリア移動度は15cm2/Vs以上を合格と評価した。
Claims (3)
- 酸化亜鉛と;酸化インジウムと;Ti、Mg、Al、およびNbよりなる群から選択される少なくとも1種の金属の酸化物と、を混合および焼結して得られる酸化物焼結体であって、
前記酸化物焼結体をX線回折したとき、ZnmIn2O3+m(mは5〜7の整数)、In2O3、及びZnOの各結晶相を含むと共に、相対密度95%以上、比抵抗0.1Ω・cm以下であり、
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]、[In]、[Ti]、[Mg]、[Al]、および[Nb]としたとき、[Zn]に対する[In]の比、[Zn]+[In]+[Ti]+[Mg]+[Al]+[Nb]に対する[Ti]+[Mg]+[Al]+[Nb]の比は、それぞれ下式を満足し、
前記酸化物焼結体に含まれる前記Zn m In 2 O 3+m 、前記In 2 O 3 、及び前記ZnOの合計に対する各結晶相の体積比は、下式を満足することを特徴とする酸化物焼結体。
0.27≦[In]/[Zn]≦0.45
([Ti]+[Mg]+[Al]+[Nb])/([Zn]+[In]+[Ti]+[Mg]+[Al]+[Nb])≦0.05
0.1≦Zn m In 2 O 3+m /(Zn m In 2 O 3+m +In 2 O 3 +ZnO)<0.75
0.05≦In 2 O 3 /(Zn m In 2 O 3+m +In 2 O 3 +ZnO)≦0.7
0.05≦ZnO/(Zn m In 2 O 3+m +In 2 O 3 +ZnO)≦0.7
(但し、Zn m In 2 O 3+m はZn 5 In 2 O 8 、Zn 6 In 2 O 9 、Zn 7 In 2 O 10 の合計である。) - 請求項1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。
- 請求項1に記載の酸化物焼結体の製造方法であって、
酸化亜鉛と;酸化インジウムと;Ti、Mg、Al、およびNbよりなる群から選択される少なくとも1種の金属の酸化物とを混合し、黒鉛型にセットした後、焼結温度850〜1050℃、該温度域での保持時間1〜10時間で焼結する第一の焼結工程と、
前記第一の焼結工程後、焼結温度1000〜1050℃(但し、第一の工程の焼結温度よりも高い温度)、該温度域での保持時間0.5〜10時間で焼結する第二の焼結工程とを包含すると共に、
前記第一の焼結工程と前記第二の焼結工程を、加圧圧力100〜500kgf/cm2で行うことを特徴とする酸化物焼結体の製造方法。
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