JP6357757B2 - 酸化物焼結体、それを用いたスパッタリングターゲット及び酸化物膜 - Google Patents
酸化物焼結体、それを用いたスパッタリングターゲット及び酸化物膜 Download PDFInfo
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- JP6357757B2 JP6357757B2 JP2013238195A JP2013238195A JP6357757B2 JP 6357757 B2 JP6357757 B2 JP 6357757B2 JP 2013238195 A JP2013238195 A JP 2013238195A JP 2013238195 A JP2013238195 A JP 2013238195A JP 6357757 B2 JP6357757 B2 JP 6357757B2
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- semiconductor layer
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- 238000005477 sputtering target Methods 0.000 title claims description 28
- 239000004065 semiconductor Substances 0.000 claims description 71
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- 229910052749 magnesium Inorganic materials 0.000 claims description 10
- 229910052684 Cerium Inorganic materials 0.000 claims description 9
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- 229910052746 lanthanum Inorganic materials 0.000 claims description 9
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- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 229910052706 scandium Inorganic materials 0.000 claims description 7
- 229910052715 tantalum Inorganic materials 0.000 claims description 7
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
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- 239000000843 powder Substances 0.000 description 51
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- YWXYYJSYQOXTPL-SLPGGIOYSA-N isosorbide mononitrate Chemical compound [O-][N+](=O)O[C@@H]1CO[C@@H]2[C@@H](O)CO[C@@H]21 YWXYYJSYQOXTPL-SLPGGIOYSA-N 0.000 description 1
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- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- H01L31/0322—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIBIIICVI chalcopyrite compounds, e.g. Cu In Se2, Cu Ga Se2, Cu In Ga Se2
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Description
(1)亜鉛(Zn)と、イオン化ポテンシャルIpが4.5eV≦Ip≦8.0eVであり、かつ原子半径dが1.20Å≦d≦2.50Å以下である元素Xを少なくとも一種類(ただし、Mgのみを添加する場合を除く)含有する酸化物焼結体であって、0.0001≦X/(Zn+X)≦0.20の組成比を有し、焼結密度が95%以上であることを特徴とする酸化物焼結体。
(2)元素Xが、Li、Mg、Ca、Sc、Ti、Sr、Y、Zr、Nb、La、Ce、Nd、Sm、Eu、Ho、Hf、Ta、WおよびBiからなる群から選ばれる少なくとも一つの元素(ただし、Mgのみを添加する場合を除く)である上記(1)に記載の酸化物焼結体。
(3)亜鉛(Zn)と、マグネシウム(Mg)と、元素X(XはLi、Ca、Sc、Ti、Sr、Y、Zr、Nb、La、Ce、Nd、Sm、Eu、Ho、Hf、Ta、WおよびBiからなる群から選ばれる少なくとも一つの元素)を以下の組成比(原子比)で含有する上記(1)または(2)に記載の酸化物焼結体。
0.0001≦X/(Zn+Mg+X)≦0.01
0.0002≦(Mg+X)/(Zn+Mg+X)≦0.20
(4)亜鉛(Zn)と、マグネシウム(Mg)と、元素X(XはSc、Ti、Y、Zr、Nb、La、Ce、Nd、Sm、Eu、Ho、Hf、Ta、WおよびBiからなる群から選ばれる少なくとも一つの元素)を以下の組成比(原子比)で含有する上記(1)または(2)に記載の酸化物焼結体。
0.0001≦X/(Zn+Mg+X)≦0.01
0.0002≦(Mg+X)/(Zn+Mg+X)≦0.20
(5)亜鉛(Zn)と、マグネシウム(Mg)と、元素X(Xは、La、Ce、Nd、Sm、EuおよびHoからなる群から選ばれる少なくとも一つの元素)を以下の組成比(原子比)で含有する上記(1)または(2)に記載の酸化物焼結体。
0.0001≦X/(Zn+Mg+X)≦0.01
0.0002≦(Mg+X)/(Zn+Mg+X)≦0.20
(6)上記(1)〜(5)のいずれかに記載の焼結体を用いるスパッタリングターゲット。
(7)上記(6)に記載のスパッタリングターゲットを用いて得られる酸化物薄膜。
(8)p型半導体である光吸収層とn型半導体層を有する太陽電池であり、n型半導体層が上記(7)に記載の酸化物薄膜である光電変換素子。
(9)上記(6)に記載の焼結体をスパッタリングターゲットとして用いて、n型半導体層を製膜する(8)に記載の光電変換素子の製造方法。
透過率(%)=透過した光の量/入射した光の量×100
酸化物薄膜の製造方法としては、DCスパッタリング法、RFスパッタリング法、ACスパッタリング法、DCマグネトロンスパッタリング法、RFマグネトロンスパッタリング法、ACマグネトロンスパッタリング法、イオンビームスパッタリング法等が適宜選択できる。特に、大面積に均一に、かつ高速製膜可能な点でDCマグネトロンスパッタリング法、RFマグネトロンスパッタリング法、ACマグネトロンスパッタリング法がより好ましい。
以下にそれぞれの工程について詳細に説明する。
各元素の原料粉末は特に限定されるものではなく、例えば、金属酸化物粉末、金属水酸化物粉末、塩化物、硝酸塩、炭酸塩等の金属塩粉末、金属アルコキシド等を用いることが可能であるが、取扱性を考慮すると金属酸化物粉末が好ましい。なお、本発明においては、金属酸化物粉末以外を用いた場合に、粉末をあらかじめ大気中等の酸化性雰囲気で加熱処理等を施して金属酸化物粉末として用いても同様の効果を奏する。なかでも、加熱処理等の操作が工程に含まれ煩雑となるため、原料粉末として金属酸化物粉末を用いることが好ましい。また、金属酸化物粉末の安定性が劣る場合、特にLi、Mg、Caの元素を含有させる場合には取扱い性を考慮すると炭酸塩を用いる方がより好ましい。
成形方法は、金属酸化物の混合粉末(仮焼した場合には仮焼した混合粉末)を目的とした形状に成形できれば特に限定されるものではない。プレス成形法、鋳込成形法、射出成形法等が例示できる。成形圧力はクラック等の発生がなく、取り扱いが可能な成形体が得られれば特に限定されるものではないが、比較的高い成形圧力で、例えばプレス成形の場合、500kg/cm2〜3.0ton/cm2で成形すると、本発明の酸化物焼結体において、元素Xの酸化物粒子が存在しないものが得られやすく、また焼結密度95%以上のものが得られやすい。また成形密度は可能な限り高めた方が好ましい。そのために冷間静水圧(CIP)成形等の方法を用いることも可能である。なお、成形処理に際しては、ポリビニルアルコール、アクリル系ポリマー、メチルセルロース、ワックス類、オレイン酸等の成形助剤を用いても良い。
次に得られた成形体を1050〜1500℃で焼成する。この温度範囲で焼成することにより、微細な平均粒径を有する粒子から成る酸化物焼結体を得ることが可能である。特に酸化亜鉛特有の揮発消失が抑制され、かつ焼結密度を高められる点から、焼成温度は1050〜1450℃の範囲がより好ましい。また焼成温度を1200〜1450℃とすると、元素Xの酸化物塩粒子が存在しないものが得られやすく、また焼結密度95%以上のものが得られやすい。
(太陽電池の作製と評価方法)
始めに、ソーダライムガラス1にMoをスパッタリングにより400nm積層して下部電極2を作製した。p型半導体層3として、スパッタ法によってCuGa/In/Seプリカーサを形成した後、CuGa/In/Seプリカーサを約450〜550℃に加熱し、固相拡散によってCu(Ga,In)Se2膜を形成した。次に前記CIGS表面にスパッタリングターゲットによりn型半導体層4を製膜した。続いて、マグネトロンスパッタリング法により表面電極層5のITO(Indium Tin Oxide)透明導電膜を形成し、反射防止膜MgF2を製膜した後、取り出し電極7にはNiCrとAuとを共蒸着して用いた。
(原料粉末)
用いた原料粉末の物性は表1に示すとおりである。
(BET比表面積)
MONOSORB(米国QUANTACHROME社製)を用い、BET式1点法により測定した。
(粉末の平均粒径)
COULTER LS130(COULTER ELECTRONICS社製)を用い、蒸留水中、液体モジュールで測定した。測定値は体積基準である。
亜鉛、カルシウムの原子数の比が表2に記載の値となるように、酸化亜鉛粉末、酸化マグネシウム粉末を湿式ビーズミルで混合、粉砕し、乾燥した後、直径150mmの金型に充填し、300kg/cm2で一軸成形し、次いで3.0ton/cm2でCIP成形した。得られた成形体を昇温速度50℃/h、降温速度100℃/h、焼成温度1200℃、保持時間3時間、窒素中の条件で焼成して、酸化物焼結体を得た。
焼結体の組成が表2に記載の値となるように使用する粉末を変更した以外は実施例1と同様にして酸化物焼結体を得た。なお、比較例2のみ焼成温度を1000℃に変更した。
(酸化物焼結体の密度)
作製した焼結体を水中で煮沸した後、アルキメデス法で焼結密度の測定を行った。
(スパッタリングターゲットの製造方法)
作製した焼結体を所定の形状に加工してスパッタリングターゲットとして用いた。ターゲットのスパッタリング面となる面は、平面研削盤とダイヤモンド砥粒の砥石を用いて加工した。
(スパッタリングターゲットによるスパッタリング条件)
・装置 :RFマグネトロンスパッタリング装置(アルバック社製)
・磁界強度 :1000Gauss(ターゲット直上、水平成分)
・基板温度 :室温
・到達真空度 :5×10−5Pa
・スパッタリングガス :アルゴン
・スパッタリングガス圧:1.0Pa
・DCパワー :25W/4インチφ
・膜厚 :80nm
膜の組成、電気抵抗および光学特性は、上記と同様の製膜条件でガラス基板上に製膜した試料を用いて以下の方法で測定した。
(薄膜の組成)
ICP発光分光分析装置(セイコーインスツルメンツ社製)を用いて、ICP発光分光分析法により定量を行った。
(薄膜の電気抵抗)
薄膜の電気抵抗はハイレスタUP MCP−HT450型(三菱化学アナリテック社製)を用いて測定した。
(薄膜の透過率)
基板を含めた光透過率を分光光度計U−4100(日立製作所製)で測定し、波長400nmから800nmの透過率の平均値を可視光領域の透過率、波長800nmから1200nmの透過率の平均値を赤外領域の透過率とした。透過率は以下の式で定義される。
透過率(%)=透過した光の量/入射した光の量×100
以上の結果から、本発明の焼結体は、太陽電池作製時において、n型半導体層の作製に用いるためのスパッタリングターゲットとして好適であり、得られた太陽電池は従来の太陽電池と比較して、高い変換効率が得られることが分かった。
2 下部電極膜
3 p型半導体層
4a n型バッファ層
4b n型半導体層
5 上部電極膜
6 反射防止膜層
7 取り出し電極
Claims (7)
- 亜鉛(Zn)と、マグネシウム(Mg)と、イオン化ポテンシャルIpが4.5eV≦Ip≦8.0eVであり、かつ、原子半径dが1.20Å≦d≦2.50Å以下であり、かつ、Li、Ca、Sc、Ti、Sr、Y、Zr、Nb、La、Ce、Nd、Sm、Eu、Ho、Hf、Ta、WおよびBiからなる群から選ばれる少なくとも一つの元素Xを以下の組成比(原子比)で含有し、焼結密度が95%以上であることを特徴とする酸化物焼結体。
0.0001≦X/(Zn+Mg+X)≦0.01
0.10≦(Mg+X)/(Zn+Mg+X)≦0.20 - 亜鉛(Zn)と、マグネシウム(Mg)と、Sc、Ti、Y、Zr、Nb、La、Ce、Nd、Sm、Eu、Ho、Hf、Ta、WおよびBiからなる群から選ばれる少なくとも一つの元素Xを以下の組成比(原子比)で含有する請求項1に記載の酸化物焼結体。
0.0001≦X/(Zn+Mg+X)≦0.01
0.10≦(Mg+X)/(Zn+Mg+X)≦0.20 - 亜鉛(Zn)と、マグネシウム(Mg)と、La、Ce、Nd、Sm、EuおよびHoからなる群から選ばれる少なくとも一つの元素Xを以下の組成比(原子比)で含有する請求項1または2に記載の酸化物焼結体。
0.0001≦X/(Zn+Mg+X)≦0.01
0.10≦(Mg+X)/(Zn+Mg+X)≦0.20 - 請求項1乃至3いずれか一項に記載の焼結体を用いるスパッタリングターゲット。
- 請求項4に記載のスパッタリングターゲットを用いて得られる酸化物薄膜。
- p型半導体である光吸収層とn型半導体層を有する太陽電池であり、n型半導体層が請求項5に記載の酸化物薄膜である光電変換素子。
- 請求項4に記載の焼結体をスパッタリングターゲットとして用いて、n型半導体層を製膜する請求項6に記載の光電変換素子の製造方法。
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