JP5367659B2 - 酸化物焼結体及び酸化物半導体薄膜 - Google Patents
酸化物焼結体及び酸化物半導体薄膜 Download PDFInfo
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- JP5367659B2 JP5367659B2 JP2010194497A JP2010194497A JP5367659B2 JP 5367659 B2 JP5367659 B2 JP 5367659B2 JP 2010194497 A JP2010194497 A JP 2010194497A JP 2010194497 A JP2010194497 A JP 2010194497A JP 5367659 B2 JP5367659 B2 JP 5367659B2
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- metal ion
- sintered body
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- 239000010409 thin film Substances 0.000 title claims description 26
- 239000004065 semiconductor Substances 0.000 title claims description 25
- 229910021645 metal ion Inorganic materials 0.000 claims description 49
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 229910001449 indium ion Inorganic materials 0.000 claims description 13
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910052732 germanium Inorganic materials 0.000 claims description 6
- 229910052748 manganese Inorganic materials 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052796 boron Inorganic materials 0.000 claims description 5
- -1 oxygen ions Chemical class 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 3
- 239000010408 film Substances 0.000 description 42
- 238000004544 sputter deposition Methods 0.000 description 31
- 239000000203 mixture Substances 0.000 description 23
- 239000007789 gas Substances 0.000 description 14
- 239000000843 powder Substances 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 13
- 239000002994 raw material Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 230000002159 abnormal effect Effects 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000005477 sputtering target Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- 238000005245 sintering Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 229910052733 gallium Inorganic materials 0.000 description 5
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical group [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 239000000470 constituent Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000036961 partial effect Effects 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910007541 Zn O Inorganic materials 0.000 description 2
- 229910007604 Zn—Sn—O Inorganic materials 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 231100000989 no adverse effect Toxicity 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000005219 brazing Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000009694 cold isostatic pressing Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Description
本発明に係る酸化物焼結体は、3価のインジウムイオン(In3+)と、2価の金属イオン(X2+)(但し、XはMg、Ca、Co及びMnから選択される1種以上の元素を表す。)と、3価の金属イオン(Y3+)(但し、YはB、Y、Crから選択される1種以上の元素を表す。)又は4価の金属イオン(Z4+)(但し、ZはSi、Ge、Ti、Zrから選択される1種以上の元素を表す。)と、酸素イオン(O2-)とからなる。但し、通常入手可能な原料の精製工程上、不可避的に含まれてくる元素や、酸化物焼結体製造プロセス上不可避的に混入する不純物元素を、不可避的に含まれる濃度程度、例えば各元素10ppm程度まで含むものは本発明に係る焼結体に包含される。
酸化物焼結体の相対密度は、スパッタ時の表面のジュール発生と相関がある。酸化物焼結体が低密度であると、その酸化物焼結体をターゲットに加工してスパッタ成膜する際に、スパッタの成膜の経過に従って、表面にインジウムの低級酸化物である、突起状のノジュールと呼ばれる高抵抗部分が発生し、その後のスパッタ時に異常放電の起点となり易い。本発明では、組成の適正範囲や製造条件の適正化によって酸化物焼結体の相対密度を98%以上とすることができ、この程度の高密度であれば、スパッタ時のノジュールによる悪影響は殆どない。相対密度は好ましくは99%以上であり、より好ましくは99.5%以上である。
なお、酸化物焼結体の相対密度は、酸化物焼結体を所定の形状に加工した後の重量と外形寸法より算出した密度を、その酸化物焼結体の理論密度で除することで求めることができる。
酸化物焼結体のバルク抵抗は、スパッタ時の異常放電の発生のし易さと相関があり、バルク抵抗が高いとスパッタ時に異常放電が発生し易い。本発明では、組成の適正範囲や製造条件の適正化によってバルク抵抗を3mΩcm以下とすることができ、この程度の低バルク抵抗であれば、スパッタ時の異常放電発生への悪影響は殆どない。バルク抵抗は好ましくは2.7mΩcm以下であり、より好ましくは2.5mΩcm以下である。
なお、バルク抵抗は四探針法により抵抗率計を使用して測定することができる。
本発明に係る各種組成の酸化物焼結体は、例えば、原料である酸化インジウム、酸化マグネシウム等の各原料粉体の配合比や原料粉体の粒径、粉砕時間、焼結温度、焼結時間、焼結雰囲気ガス種類等の条件を調整することにより得ることができる。
上記の様にして得られた酸化物焼結体は、研削や研磨等の加工を施すことによりスパッタリング用ターゲットとすることができ、これを使用して成膜することにより、当該ターゲットと同一組成をもつ酸化物膜を形成することができる。加工の際は、平面研削等の方法で表面を研削することによって、表面粗さ(Ra)を5μm以下とすることが望ましい。表面粗さを小さくすることによって、異常放電の原因となるノジュール発生の起点を減少させることができる。
酸化物膜のキャリア濃度は、その膜をトランジスタのチャネル層に使用した際に、トランジスタの各種特性と相関がある。キャリア濃度が高すぎると、トランジスタのオフ時にも、微少漏れ電流が発生してしまい、オンオフ比が低下してしまう。一方、キャリア濃度が低すぎると、トランジスタを流れる電流が小さくなってしまう。本発明では、組成の適正範囲等によって、酸化物膜のキャリア濃度を1016〜1018cm-3とすることができ、この範囲であれば、特性が良好なトランジスタを作製することができる。
移動度はトランジスタの特性の中でも、最も重要な特性の一つであり、酸化物半導体がトランジスタのチャネル層として使用される競合材料であるアモルファスシリコンの移動度である1cm2/Vs以上であることが望ましい。移動度は基本的には、高ければ高いほど良い。本発明に係る酸化物膜は組成の適正範囲等によって、1cm2/Vs以上の移動度を有することができ、好ましくは3cm2/Vs以上の移動度を有することができ、より好ましくは5cm2/Vs以上の移動度を有することができる。これによって、アモルファスシリコンより優れた特性となって、産業上の応用可能性がより高まる。
(ア)焼結体及び膜の組成
SIIナノテクノロジー社製型式SPS3000を用いてICP(高周波誘導結合プラズマ)分析法によって求めた。
(イ)焼結体の相対密度
重量及び外形寸法の測定結果と、構成元素からの理論密度とにより求めた。
(ウ)焼結体のバルク抵抗
四探針法(JIS K7194)により、NPS(エヌピイエス)社製型式Σ−5+装置を用いて求めた。
(エ)膜厚
段差計(Veeco社製、型式Dektak8 STYLUS PROFILER)を用いて求めた。
(オ)膜のキャリア濃度及び移動度
成膜したガラス基板を約10mm角に切り出し、四隅にインジウム電極をつけて、ホール測定装置(東陽テクニカ社製、型式Resitest8200)にセットして測定した。
(カ)膜の結晶又は非晶質構造
リガク社製RINT−1100X線回折装置を用いて結晶性を判定した。このX線回折によって、バックグランドレベル以上の有意なピークが認められなかったことをもって、非晶質と判断した。
(キ)粉体の平均粒径
粉体の平均粒径は、島津製作所製SALD−3100により測定した。
酸化インジウム粉(平均粒径1.0μm)、酸化ケイ素粉(平均粒径1.0μm)、及び、酸化マグネシウム粉(平均粒径1.0μm)を金属元素の原子数比(In:Si:Mg)が0.4:0.3:0.3となる様に秤量し、湿式混合粉砕した。粉砕後の混合粉の平均粒径は0.8μmであった。この混合粉を、スプレードライヤーで造粒後、金型に充填し、加圧成形した後、大気雰囲気中1450℃の高温で10時間焼結した。得られた焼結体を直径6インチ、厚さ6mmの円盤状に加工してスパッタリングターゲットとした。当該ターゲットについて、重量と外形寸法との測定結果と理論密度から相対密度を算出したところ99.5%であった。また、四探針法により測定した焼結体のバルク抵抗は2.2mΩcmであった。
原料粉の組成比を表1に記載のそれぞれの値となる様にした以外は、実施例1と同様にして、酸化物焼結体及び酸化物半導体薄膜を得た。それぞれの相対密度、バルク抵抗、キャリア濃度、移動度は、表1に記載の通りであった。また、焼結体及び膜の組成はそれぞれ原料粉の組成比と同一であった。これらの酸化物半導体薄膜の成膜時には、異常放電は認められなかった。
原料粉の組成比を表1に記載のそれぞれの値となる様にした以外は、実施例1と同様にして、酸化物焼結体及び酸化物半導体薄膜を得た。それぞれの相対密度、バルク抵抗、キャリア濃度、移動度は、表1に記載の通りであった。また、焼結体及び膜の組成はそれぞれ原料粉の組成比と同一であった。
一方、比較例1,4,6〜10では、キャリア濃度が1016cm-3未満であった。
また、比較例1,4,6,8,10では、移動度が1cm2/Vs未満であった。
また、比較例2,3,5では、キャリア濃度が1018cm-3超であった。
Claims (7)
- 3価のインジウムイオン(In3+)と、2価の金属イオン(X2+)(但し、XはCa、Co及びMnから選択される1種以上の元素を表す。)と、3価の金属イオン(Y3+)(但し、YはB、Y、Crから選択される1種以上の元素を表す。)又は4価の金属イオン(Z4+)(但し、ZはSi、Ge、Zrから選択される1種以上の元素を表す。)と、酸素イオン(O2-)とからなり、
3価のインジウムイオン(In3+)、2価の金属イオン(X2+)、3価の金属イオン(Y3+)、及び、4価の金属イオン(Z4+)の原子数比がそれぞれ、
0.2≦[In3+]/{[In3+]+[X2+]+[Y3+]+[Z4+]}≦0.8、
0.1≦[X2+]/{[In3+]+[X2+]+[Y3+]+[Z4+]}≦0.5、及び、
0.1≦{[Y3+]+[Z4+]}/{[In3+]+[X2+]+[Y3+]+[Z4+]}≦0.5
を満たし、相対密度が98%以上である酸化物焼結体。 - バルク抵抗が3mΩ以下である請求項1に記載の酸化物焼結体。
- 3価のインジウムイオン(In3+)と、2価の金属イオン(X2+)(但し、XはCa、Co及びMnから選択される1種以上の元素を表す。)と、3価の金属イオン(Y3+)(但し、YはB、Y、Crから選択される1種以上の元素を表す。)又は4価の金属イオン(Z4+)(但し、ZはSi、Ge、Zrから選択される1種以上の元素を表す。)と、酸素イオン(O2-)とからなり、
3価のインジウムイオン(In3+)、2価の金属イオン(X2+)、3価の金属イオン(Y3+)、及び、4価の金属イオン(Z4+)の原子数比がそれぞれ、
0.2≦[In3+]/{[In3+]+[X2+]+[Y3+]+[Z4+]}≦0.8、
0.1≦[X2+]/{[In3+]+[X2+]+[Y3+]+[Z4+]}≦0.5、及び、
0.1≦{[Y3+]+[Z4+]}/{[In3+]+[X2+]+[Y3+]+[Z4+]}≦0.5
を満たし、キャリア濃度が1016〜1018cm-3である酸化物半導体薄膜。 - 非晶質である請求項3に記載の酸化物半導体薄膜。
- 移動度が1cm2/Vs以上である請求項3又は4に記載の酸化物半導体薄膜。
- 請求項3〜5の何れかに記載の酸化物半導体薄膜を活性層として備えた薄膜トランジスタ。
- 請求項6に記載の薄膜トランジスタを備えたアクティブマトリックス駆動表示パネル。
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