JP2015127293A - 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
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Abstract
Description
れている。
30原子%≦[In]≦50原子%・・・(1)
20原子%≦[Ga]≦30原子%・・・(2)
25原子%≦[Sn]≦45原子%・・・(3)
[InGaO3]≧0.05・・・(4)
但し、[InGaO3]=(I(InGaO3)/(I(InGaO3)+I(In2O3)+I(SnO2))
式中、I(InGaO3)、I(In2O3)、およびI(SnO2)はそれぞれ、X線回折で特定されたInGaO3相、In2O3相、SnO2相の回折強度の測定値である。
30原子%≦[In]≦50原子%・・・(1)
20原子%≦[Ga]≦30原子%・・・(2)
25原子%≦[Sn]≦45原子%・・・(3)
[InGaO3]≧0.05・・・(4)
但し、[InGaO3]=(I(InGaO3)/(I(InGaO3)+I(In2O3)+I(SnO2))
式中、I(InGaO3)、I(In2O3)、およびI(SnO2)はそれぞれ、X線回折で特定されたInGaO3相、In2O3相、SnO2相の回折強度の測定値を意味する。
(スパッタリングターゲットの作製)
純度99.99%の酸化インジウム粉末(In2O3)、純度99.99%の酸化ガリウム粉末(Ga2O3)、純度99.99%の酸化錫粉末(SnO2)を表1に示す質量比率および原子比率で配合し、水と分散剤(ポリカルボン酸アンモニウム)を加えて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して造粒を行った。
(予備成形の条件)
成形圧力:1.0ton/cm2
厚みをtとしたとき、成形体サイズ:φ110mm×t13mm
相対密度は、以下のようにして測定した気孔率を引き算することにより求めた。まず、酸化物焼結体の破断面(酸化物焼結体を任意の位置で厚み方向に切断し、その切断面表面の任意の位置)を鏡面研削した試料を用意した。次に、走査型電子顕微鏡(SEM)を用いて1000倍で写真撮影し、50μm角の領域に占める気孔の面積率(%)を測定して気孔率とした。上記試料について、同様の操作を合計20箇所について行い、その平均を当該試料の平均気孔率(%)とした。平均相対密度は、[100−平均気孔率]により算出し、その結果を表4に「相対密度(%)」として記載した。本実施例では、このようにして得られた平均相対密度が90%以上のものを合格と評価した。
表4に記載の「平均結晶粒径(μm)」は以下のようにして測定した。まず、酸化物焼結体の破断面(酸化物焼結体を任意の位置で厚み方向に切断し、その切断面表面の任意の位置)を鏡面研削した試料を用意した。次に、その組織を走査型電子顕微鏡(SEM)を用いて倍率400倍で写真撮影し、任意の方向で100μmの長さの直線を引き、この直線内に含まれる結晶粒の数(N)を求め、[100/N]から算出される値を当該「直線上での結晶粒径」とした。同様に粗大結晶粒が重複しない間隔(少なくとも20μm以上の間隔)で直線を20本作成して各直線上での結晶粒径を算出した。そして、[各直線上での結晶粒径の合計/20]から算出される値を「酸化物焼結体の平均結晶粒径」とした。本実施例では、このようにして得られた酸化物焼結体の平均結晶粒径が10μm以下のものを合格と評価した。
表4に記載の「粗大結晶粒の割合(%)」は以下のようにして測定した。まず、上記平均結晶粒径と同様、酸化物焼結体の破断面をSEM観察して、任意の方向に100μmの長さの直線を引き、この直線上で切り取られる長さが15μm以上の結晶粒を粗大な結晶粒とした。この粗大な結晶粒が直線上に占める長さL(複数ある場合はその総和:μm)を求め、[L/100]から算出される値を当該「直線上での粗大結晶粒の割合」(%)とした。同様に粗大結晶粒が重複しない間隔(少なくとも20μm以上の間隔)で直線を20本作成して各直線上での粗大結晶粒の割合を算出した。そして、[各直線上での粗大結晶粒の割合の合計/20]から算出される値を「酸化物焼結体の粗大結晶粒の割合」(%)とした。本実施例では、このようにして得られた酸化物焼結体の粗大結晶粒の割合が10%以下のものを合格と評価した。
表4に記載の「InGaO3相(%)」は以下のようにして測定した。まず、スパッタリングして得られたスパッタリング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、以下のX線回折により、結晶相の回折線の強度(回折ピーク)を測定して求めた。
分析装置:理学電機社製「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
(連続焼測定)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°
[InGaO3]=I(InGaO3)/(I(InGaO3)+I(In2O3)+I(SnO2))
表4に記載の「ボンディング時の割れ」の有無は以下のようにして測定した。上記機械加工した酸化物焼結体を加熱し、バッキングプレートにボンディングした後、酸化物焼結体表面に割れが生じていないか目視で確認した。酸化物焼結体表面に1mmを超えるクラックが確認された場合を「割れ」があると判断した。ボンディング作業を10回行い、1回でも割れがある場合を不合格と評価して、表4中に「有」と記載した。一方、10回中、1回も割れがない場合を合格と評価して、表4中に「無」と記載した。
本実施例では、従来のIn−Ga−Zn酸化物焼結体(IGZO)に比べて、本発明で規定するIn−Ga−Sn酸化物焼結体(IGTO)の有用性を実証するため、以下の実験を行った。
スパッタリング装置:株式会社アルバック製「CS−200」
DC(直流)マグネトロンスパッタリング法
基板温度:室温
(1)プリスパッタ
ガス圧:1mTorr
酸素分圧:100×O2/(Ar+O2)=0体積%
成膜パワー密度:2.5W/cm2
プリスパッタ時間:10分
(2)本成膜
ガス圧:1mTorr
酸素分圧:100×O2/(Ar+O2)=4体積%
成膜パワー密度:2.5W/cm2
膜厚:40nm
純度99.99%の酸化インジウム粉末(In2O3)、純度99.99%の酸化ガリウム粉末(Ga2O3)、純度99.99%の酸化亜鉛粉末(ZnO2)を表1に示す質量比率および原子比率で配合し、水と分散剤(ポリカルボン酸アンモニウム)とバインダーを加えてボールミルで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して造粒を行った。
(予備成形の条件)
成形圧力:1.0ton/cm2
厚みをtとしたとき、成形体サイズ:φ110mm×t13mm
Claims (7)
- 酸化インジウムと;酸化ガリウムと;酸化錫とを焼結して得られる酸化物焼結体であって、
前記酸化物焼結体の相対密度が90%以上、
前記酸化物焼結体の平均結晶粒径が10μm以下であり、
前記酸化物焼結体に含まれる酸素を除く全金属元素に対する、インジウム、ガリウム、錫の含有量の割合(原子%)を夫々、[In]、[Ga]、[Sn]としたとき、下記式(1)〜(3)を満足すると共に、
前記酸化物焼結体をX線回折したとき、InGaO3相は下記式(4)を満足するものであることを特徴とする酸化物焼結体。
30原子%≦[In]≦50原子%・・・(1)
20原子%≦[Ga]≦30原子%・・・(2)
25原子%≦[Sn]≦45原子%・・・(3)
[InGaO3]≧0.05・・・(4)
但し、[InGaO3]=(I(InGaO3)/(I(InGaO3)+I(In2O3)+I(SnO2))
式中、I(InGaO3)、I(In2O3)、およびI(SnO2)はそれぞれ、X線回折で特定されたInGaO3相、In2O3相、SnO2相の回折強度の測定値である。 - 前記酸化物焼結体の結晶粒径が15μmを超える粗大結晶粒の割合は10%以下である請求項1に記載の酸化物焼結体。
- 前記酸化物焼結体をX線回折したとき、Ga3-xn5+xSn2O16相は含まれないものである請求項1または2に記載の酸化物焼結体。
- 前記酸化物焼結体をX線回折したとき、(Ga、In)2O3相は含まれないものである請求項1〜3のいずれかに記載の酸化物焼結体。
- 請求項1〜4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、比抵抗が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。
- 請求項1〜4のいずれかに記載の酸化物焼結体の製造方法であって、酸化インジウムと;酸化ガリウムと;酸化錫とを混合し、成形型にセットした後、焼結温度850〜1250℃まで昇温した後、該温度域での保持時間0.1〜5時間、加圧圧力59MPa以下で焼結することを特徴とする酸化物焼結体の製造方法。
- 前記焼結温度までの平均昇温速度が600℃/hr以下である請求項6に記載の酸化物焼結体の製造方法。
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