JP5337224B2 - 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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Description
0.27≦[In]/[Zn]≦0.45
([Ti]+[Mg]+[Al]+[Nb])/([Zn]+[In]+[Ti]+[Mg]+[Al]+[Nb])≦0.1
ZnmIn2O3+m/(ZnmIn2O3+m+In2O3+ZnO)≧0.75
0.005≦In2O3/(ZnmIn2O3+m+In2O3+ZnO)≦0.15
0.005≦ZnO/(ZnmIn2O3+m+In2O3+ZnO)≦0.20
(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。
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85%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、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85%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100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2回以下を合格と評価した。
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)相を主相とし、In2O3、及びZnOの各結晶相を含むと共に、相対密度85%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])≦0.1
Zn m In 2 O 3+m /(Zn m In 2 O 3+m +In 2 O 3 +ZnO)≧0.75
0.005≦In 2 O 3 /(Zn m In 2 O 3+m +In 2 O 3 +ZnO)≦0.15
0.005≦ZnO/(Zn m In 2 O 3+m +In 2 O 3 +ZnO)≦0.20
(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950〜1050℃、該温度域での保持時間0.1〜5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1100〜1200℃、該温度域での保持時間0.1〜5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。
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2011242891A JP5337224B2 (ja) | 2011-11-04 | 2011-11-04 | 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 |
PCT/JP2012/078327 WO2013065786A1 (ja) | 2011-11-04 | 2012-11-01 | 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 |
TW101140799A TW201333230A (zh) | 2011-11-04 | 2012-11-02 | 氧化物燒結體及濺鍍靶,以及其製造方法 |
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