JP6951715B2 - 半導体膜の製造方法及び半導体膜並びにドーピング用錯化合物及びドーピング方法 - Google Patents
半導体膜の製造方法及び半導体膜並びにドーピング用錯化合物及びドーピング方法 Download PDFInfo
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- JP6951715B2 JP6951715B2 JP2018539792A JP2018539792A JP6951715B2 JP 6951715 B2 JP6951715 B2 JP 6951715B2 JP 2018539792 A JP2018539792 A JP 2018539792A JP 2018539792 A JP2018539792 A JP 2018539792A JP 6951715 B2 JP6951715 B2 JP 6951715B2
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Images
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Description
[2] 錯化合物が、XMR1 lR2 mR3 n(式中、Xはハロゲン原子を表し、Mはドーパントを表し、R1、R2及びR3はそれぞれ同一又は異なって、置換基を有していてもよい炭化水素基又は複素環基を表し、l、m及びnはそれぞれ同一又は異なって、0〜3の整数を表す。)で表される化合物である、前記[1]記載の製造方法。
[3] 炭化水素基又は複素環基が、置換基を有している炭化水素基であり、該置換基が、シアノ基である前記[1]記載の製造方法。
[4] ハロゲンが、塩素である前記[1]記載の製造方法。
[5] ドーパントが、Siである前記[1]記載の製造方法。
[6] ドーパント材料を用いてドーピングされた半導体膜を製造する方法であって、前記ドーパント材料が、少なくともシリコンと置換基を有していてもよい炭化水素基又は複素環基とハロゲンとを含有する錯化合物を含むことを特徴とする半導体膜の製造方法。
[7] 錯化合物が、2以上の置換基を有していてもよい炭化水素基又は複素環基を含有する前記[6]記載の製造方法。
[8] 錯化合物が、XSiR1 lR2 mR3 n(式中、Xはハロゲン原子を表し、R1、R2及びR3はそれぞれ同一又は異なって、置換基を有していてもよい炭化水素基又は複素環基を表し、l、m及びnはそれぞれ同一又は異なって、0〜3の整数を表す。)で表される化合物である、前記[6]記載の製造方法。
[9] 炭化水素基又は複素環基が、置換基を有している炭化水素基であり、該置換基が、シアノ基である前記[6]記載の製造方法。
[10] ハロゲンが、塩素である前記[6]記載の製造方法。
[11] 前記[1]〜[10]のいずれかに記載の製造方法を用いて製造される半導体膜。
[12] 半導体膜と、電極とを少なくとも備える半導体装置であって、前記半導体膜が前記[11]記載の半導体膜である半導体装置。
[13] 半導体装置を備える半導体システムであって、前記半導体装置が前記[12]記載の半導体装置である半導体システム。
[14] Siがドーピングされている半導体膜であって、半導体膜が、酸化物半導体を主成分としており、膜表面から少なくとも0.1μm〜0.5μmの深さの範囲において、キャリア密度が1×1018/cm3以上でドーピングされていることを特徴とする半導体膜。
[15] Siがドーピングされている半導体膜であって、膜表面から少なくとも0.3μm以上の深さまでドーピングされており、移動度1cm2/Vs以上であり、膜厚100μm以下であることを特徴とする半導体膜。
[16] キャリア密度が1×1020/cm3以下である、前記[14]又は[15]に記載の半導体膜。
[17] 半導体膜と、電極とを少なくとも備える半導体装置であって、前記半導体膜が前記[14]又は[15]に記載の半導体膜である半導体装置。
[18] 半導体装置を備える半導体システムであって、前記半導体装置が前記[17]記載の半導体装置である半導体システム。
[19] 半導体のドーピングに用いられる錯化合物であって、少なくともドーパントと置換基を有していてもよい炭化水素基又は複素環基とハロゲンとを含有する錯化合物を含むことを特徴とするドーピング用錯化合物。
[20] 錯化合物が、2以上の置換基を有していてもよい炭化水素基又は複素環基を含有する前記[19]記載のドーピング用錯化合物。
[21] 錯化合物が、XMR1 lR2 mR3 n(式中、Xはハロゲン原子を表し、Mはドーパントを表し、R1、R2及びR3はそれぞれ同一又は異なって、置換基を有していてもよい炭化水素基又は複素環基を表し、l、m及びnはそれぞれ同一又は異なって、0〜3の整数を表す。)で表される化合物である、前記[19]に記載のドーピング用錯化合物。
[22] 炭化水素基又は複素環基が、置換基を有している炭化水素基であり、該置換基が、シアノ基である前記[19]記載のドーピング用錯化合物。
[23] ハロゲンが、塩素である前記[19]記載のドーピング用錯化合物。
[24] コランダム構造を有する半導体に用いられる前記[19]記載のドーピング用錯化合物。
[25] 酸化物半導体に用いられる前記[19]記載のドーピング用錯化合物。
[26] ドーピング用錯化合物を用いて半導体のドーピングを行う方法であって、前記ドーピング用錯化合物が、前記[19]〜[25]のいずれかに記載のドーピング用錯化合物であることを特徴とするドーピング方法。
[27] 前記[26]記載のドーピング方法によりドーピングされた半導体。
[28] 膜状である、前記[26]記載の半導体。
[29] 半導体膜と、電極とを少なくとも備える半導体装置であって、前記半導体膜が前記[27]又は[28]に記載の半導体を主成分として含む半導体装置。
[30] 半導体装置を備える半導体システムであって、前記半導体装置が前記[29]記載の半導体装置である半導体システム。
脂肪族複素環基としては、例えば、炭素数2〜14で、異種原子として少なくとも1個、好ましくは1〜3個の例えば窒素原子、酸素原子及び/又は硫黄原子等のヘテロ原子を含んでいる、3〜8員、好ましくは5又は6員の単環、多環又は縮合環の脂肪族複素環基が挙げられる。脂肪族複素環基の具体例としては、例えば、ピロリジル−2−オン基、ピペリジル基、ピペリジノ基、ピペラジニル基、モルホリノ基、モルホリニル基、テトラヒドロフリル基、テトラヒドロピラニル基、チオラニル基又はスクシンイミジル基等が挙げられる。
霧化工程は、前記原料溶液を霧化する。霧化手段は、原料溶液を霧化できさえすれば特に限定されず、公知の手段であってよいが、本発明においては、超音波を用いる霧化手段が好ましい。超音波を用いて得られたミストは、初速度がゼロであり、空中に浮遊するので好ましく、例えば、スプレーのように吹き付けるのではなく、空間に浮遊してガスとして搬送することが可能なミストであるので衝突エネルギーによる損傷がないため、非常に好適である。ミストの液滴のサイズは、特に限定されず、数mm程度であってもよいが、好ましくは50μm以下であり、より好ましくは100nm〜10μmである。
前記基体は、前記半導体膜を支持できるものであれば特に限定されない。前記基体の材料も、本発明の目的を阻害しない限り特に限定されず、公知の基体であってよく、有機化合物であってもよいし、無機化合物であってもよい。前記基体の形状としては、どのような形状のものであってもよく、あらゆる形状に対して有効であり、例えば、平板や円板等の板状、繊維状、棒状、円柱状、角柱状、筒状、螺旋状、球状、リング状などが挙げられるが、本発明においては、基板が好ましい。基板の厚さは、本発明においては特に限定されない。
搬送工程では、前記キャリアガスによって前記ミストを基体へ搬送する。キャリアガスの種類としては、本発明の目的を阻害しない限り特に限定されず、例えば、酸素、オゾン、窒素やアルゴン等の不活性ガス、または水素ガスやフォーミングガス等の還元ガスなどが挙げられるが、本発明においては、キャリアガスとして窒素を用いるのが好ましい。また、キャリアガスの種類は1種類であってよいが、2種類以上であってもよく、キャリアガス濃度を変化させた希釈ガス(例えば10倍希釈ガス等)などを、第2のキャリアガスとしてさらに用いてもよい。また、キャリアガスの供給箇所も1箇所だけでなく、2箇所以上あってもよい。キャリアガスの流量は、特に限定されないが、0.01〜20L/分であるのが好ましく、1〜10L/分であるのがより好ましい。希釈ガスの場合には、希釈ガスの流量が、0.001〜2L/分であるのが好ましく、0.1〜1L/分であるのがより好ましい。
製膜工程では、前記ミストを前記基体表面近傍で反応させて、前記基体表面の一部または全部に製膜する。前記熱反応は、前記ミストから膜が形成される熱反応であれば特に限定されず、熱でもって前記ミストが反応すればそれでよく、反応条件等も本発明の目的を阻害しない限り特に限定されない。本工程においては、前記熱反応を、通常、溶媒の蒸発温度以上の温度で行うが、あまり高すぎない温度以下が好ましい。本発明においては、前記熱反応を、650℃以下で行うのが好ましく、400℃〜650℃の温度で行うのがより好ましい。また、熱反応は、本発明の目的を阻害しない限り、真空下、非酸素雰囲気下、還元ガス雰囲気および酸素雰囲気下のいずれの雰囲気下で行われてもよく、また、大気圧下、加圧下および減圧下のいずれの条件下で行われてもよいが、本発明においては、大気圧下で行われるのが好ましく、窒素雰囲気下でかつ大気圧下で行われるのがより好ましい。なお、膜厚は、製膜時間を調整することにより、設定することができる。
本発明の半導体装置が発光ダイオード(LED)である場合の一例を図9に示す。図9の半導体発光素子は、第2の電極165b上にn型半導体層161を備えており、n型半導体層161上には、発光層163が積層されている。そして、発光層163上には、p型半導体層162が積層されている。p型半導体層162上には、発光層163が発生する光を透過する透光性電極167を備えており、透光性電極167上には、第1の電極165aが積層されている。なお、図9の半導体発光素子は、電極部分を除いて保護層で覆われていてもよい。
1.製膜装置
図1を用いて、本実施例で用いたミストCVD装置を説明する。ミストCVD装置19は、基板20を載置するサセプタ21と、キャリアガスを供給するキャリアガス供給手段22aと、キャリアガス供給手段22aから送り出されるキャリアガスの流量を調節するための流量調節弁23aと、キャリアガス(希釈)を供給するキャリアガス(希釈)供給手段22bと、キャリアガス(希釈)供給手段22bから送り出されるキャリアガスの流量を調節するための流量調節弁23bと、原料溶液24aが収容されるミスト発生源24と、水25aが入れられる容器25と、容器25の底面に取り付けられた超音波振動子26と、内径40mmの石英管からなる供給管27と、供給管27の周辺部に設置されたヒーター28とを備えている。サセプタ21は、石英からなり、基板20を載置する面が水平面から傾斜している。製膜室となる供給管27とサセプタ21をどちらも石英で作製することにより、基板20上に形成される膜内に装置由来の不純物が混入することを抑制している。
ガリウムアセチルアセトナート(ガリウム濃度0.05mol/L)と3―シアノプロピルジメチルクロロシランとを混合し、ガリウムに対するシリコンの原子比が1:0.005となるように水溶液を調整し、この際、36%塩酸を体積比で1.5%含有させ、これを原料溶液とした。
上記2.で得られた原料溶液24aミスト発生源24内に収容した。次に、基板20として、c面サファイア基板をサセプタ21上に設置し、ヒーター28の温度を500℃にまで昇温させた。次に、流量調節弁23a、23bを開いて、キャリアガス源であるキャリアガス供給手段22a、22bからキャリアガスを供給管27内に供給し、供給管27内の雰囲気をキャリアガスで十分に置換した後、キャリアガスの流量を3.0L/分に、キャリアガス(希釈)の流量を0.5L/分にそれぞれ調節した。なお、キャリアガスとして窒素を用いた。
次に、超音波振動子26を2.4MHzで振動させ、その振動を、水25を通じて原料溶液24aに伝播させることによって、原料溶液24aを霧化させてミストを生成させた。このミストが、キャリアガスによって、供給管27に搬送され、大気圧下、500℃にて、基板20表面近傍でミストが熱反応して基板20上に膜が形成された。なお、製膜時間は30分間であり、膜厚は750nmであった。
原料溶液におけるガリウムに対するシリコンの原子比が1:0.002となるように水溶液を調整したこと以外は、実施例1と同様にして、半導体膜を得た。
原料溶液におけるガリウムに対するシリコンの原子比が1:0.001となるように水溶液を調整したこと以外は、実施例1と同様にして、半導体膜を得た。
実施例1〜3において得られた半導体膜につき、SIMS分析(測定装置:CAMECA IMS―7f、1次イオン種:Cs+、1次加速電圧:15.0kV、検出領域:30μmφ)を行った。結果を図3に示す。図3から明らかなように、実施例1〜3にて得られた半導体膜は、膜表面から約0.6μmの深さまで、ケイ素が均質にドーピングされていることがわかる。
実施例1〜3において得られた半導体膜につき、van der pauw法により、ホール効果測定を実施した。実施例1〜3にて得られた半導体膜のキャリア密度は、それぞれ、実施例1が6.7×1018/cm3であり、実施例2が1.71×1019/cm3であり、実施例3が2.29×1019/cm3であった。また、実施例1〜3にて得られた半導体膜の移動度は、それぞれ、実施例1が3.0cm2/Vsであり、実施例2が5.31cm2/Vsであり、実施例3が16.6cm2/Vsであった。
原料溶液におけるガリウムに対するシリコンの原子比が1:0.0001となるように水溶液を調整したこと、製膜時間を1時間としたこと以外は、実施例1と同様にして、半導体膜を得た。
実施例4で得られた半導体膜につき、試験例1と同様にしてSIMS分析を行った。結果を図14に示す。図14から明らかなように膜表面から少なくとも0.1μm〜1.5μmの深さにおいて、ケイ素が均質にドーピングされていることがわかる。
20 基板
21 サセプタ
22a キャリアガス供給手段
22b キャリアガス(希釈)供給手段
23a 流量調節弁
23b 流量調節弁
24 ミスト発生源
24a 原料溶液
25 容器
25a 水
26 超音波振動子
27 供給管
28 ヒーター
29 排気口
101a n−型半導体層
101b n+型半導体層
102 p型半導体層
103 金属層
104 絶縁体層
105a ショットキー電極
105b オーミック電極
121a バンドギャップの広いn型半導体層
121b バンドギャップの狭いn型半導体層
121c n+型半導体層
123 p型半導体層
125a ゲート電極
125b ソース電極
125c ドレイン電極
128 緩衝層
129 基板
131a n−型半導体層
131b 第1のn+型半導体層
131c 第2のn+型半導体層
132 p型半導体層
134 ゲート絶縁膜
135a ゲート電極
135b ソース電極
135c ドレイン電極
138 緩衝層
139 半絶縁体層
141a n−型半導体層
141b 第1のn+型半導体層
141c 第2のn+型半導体層
142 p型半導体層
145a ゲート電極
145b ソース電極
145c ドレイン電極
151 n型半導体層
151a n−型半導体層
151b n+型半導体層
152 p型半導体層
154 ゲート絶縁膜
155a ゲート電極
155b エミッタ電極
155c コレクタ電極
161 n型半導体層
162 p型半導体層
163 発光層
165a 第1の電極
165b 第2の電極
167 透光性電極
169 基板
Claims (22)
- ドーパント材料を用いてドーピングされたガリウムを含む酸化物半導体を主成分とする半導体膜を製造する方法であって、前記ドーパント材料が、少なくともドーパントと置換基を有していてもよい炭化水素基又は複素環基とハロゲンとを含有する錯化合物を含むことを特徴とする半導体膜の製造方法。
- 錯化合物が、XMR1 lR2 mR3 n(式中、Xはハロゲン原子を表し、Mはドーパントを表し、R1、R2及びR3はそれぞれ同一又は異なって、置換基を有していてもよい炭化水素基又は複素環基を表し、l、m及びnはそれぞれ同一又は異なって、0〜3の整数を表す。)で表される化合物である、請求項1記載の製造方法。
- 炭化水素基又は複素環基が、置換基を有している炭化水素基であり、該置換基が、シアノ基である請求項1記載の製造方法。
- ハロゲンが、塩素である請求項1記載の製造方法。
- ドーパントが、Siである請求項1記載の製造方法。
- ドーパント材料を用いてドーピングされたガリウムを含む酸化物半導体を主成分とする半導体膜を製造する方法であって、前記ドーパント材料が、少なくともシリコンと置換基を有していてもよい炭化水素基又は複素環基とハロゲンとを含有する錯化合物を含むことを特徴とする半導体膜の製造方法。
- 錯化合物が、2以上の置換基を有していてもよい炭化水素基又は複素環基を含有する請求項6記載の製造方法。
- 錯化合物が、XSiR1 lR2 mR3 n(式中、Xはハロゲン原子を表し、R1、R2及びR3はそれぞれ同一又は異なって、置換基を有していてもよい炭化水素基又は複素環基を表し、l、m及びnはそれぞれ同一又は異なって、0〜3の整数を表す。)で表される化合物である、請求項6記載の製造方法。
- 炭化水素基又は複素環基が、置換基を有している炭化水素基であり、該置換基が、シアノ基である請求項6記載の製造方法。
- ハロゲンが、塩素である請求項6記載の製造方法。
- Siがドーピングされている半導体膜であって、半導体膜が、ガリウムを含む酸化物半導体を主成分としており、膜表面から少なくとも0.1μm〜0.5μmの深さの範囲において、キャリア密度が1×1018/cm3以上でドーピングされていることを特徴とする半導体膜。
- Siがドーピングされている半導体膜であって、半導体膜が、ガリウムを含む酸化物半導体を主成分としており、膜表面から少なくとも0.3μm以上の深さまでドーピングされており、移動度1cm2/Vs以上であり、膜厚100μm以下であることを特徴とする半導体膜。
- キャリア密度が1×1020/cm3以下である、請求項11又は12に記載の半導体膜。
- 半導体膜と、電極とを少なくとも備える半導体装置であって、前記半導体膜が請求項11又は12に記載の半導体膜である半導体装置。
- 半導体装置を備える半導体システムであって、前記半導体装置が請求項14記載の半導体装置である半導体システム。
- ガリウムを含む酸化物半導体のドーピングに用いられる錯化合物であって、少なくともドーパントと置換基を有していてもよい炭化水素基又は複素環基とハロゲンとを含有する錯化合物を含むことを特徴とするドーピング用錯化合物。
- 錯化合物が、2以上の置換基を有していてもよい炭化水素基又は複素環基を含有する請求項16記載のドーピング用錯化合物。
- 錯化合物が、XMR1 lR2 mR3 n(式中、Xはハロゲン原子を表し、Mはドーパントを表し、R1、R2及びR3はそれぞれ同一又は異なって、置換基を有していてもよい炭化水素基又は複素環基を表し、l、m及びnはそれぞれ同一又は異なって、0〜3の整数を表す。)で表される化合物である、請求項16に記載のドーピング用錯化合物。
- 炭化水素基又は複素環基が、置換基を有している炭化水素基であり、該置換基が、シアノ基である請求項16記載のドーピング用錯化合物。
- ハロゲンが、塩素である請求項16記載のドーピング用錯化合物。
- 前記酸化物半導体がコランダム構造を有する請求項16記載のドーピング用錯化合物。
- ドーピング用錯化合物を用いて半導体のドーピングを行う方法であって、前記ドーピング用錯化合物が、請求項19〜21のいずれかに記載のドーピング用錯化合物であることを特徴とするドーピング方法。
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