JP2019169728A - 金属酸化物半導体層形成用組成物及びそれを用いた金属酸化物半導体層の製造方法 - Google Patents
金属酸化物半導体層形成用組成物及びそれを用いた金属酸化物半導体層の製造方法 Download PDFInfo
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- JP2019169728A JP2019169728A JP2019099590A JP2019099590A JP2019169728A JP 2019169728 A JP2019169728 A JP 2019169728A JP 2019099590 A JP2019099590 A JP 2019099590A JP 2019099590 A JP2019099590 A JP 2019099590A JP 2019169728 A JP2019169728 A JP 2019169728A
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- Prior art keywords
- semiconductor layer
- metal oxide
- oxide semiconductor
- composition
- film
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- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 128
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- 238000004519 manufacturing process Methods 0.000 title claims description 19
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 60
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- 239000002904 solvent Substances 0.000 claims abstract description 24
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- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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Classifications
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- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
- H01L29/7869—Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
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- H01L29/49—Metal-insulator-semiconductor electrodes, e.g. gates of MOSFET
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- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
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Abstract
【解決手段】
一般式[1]で表される溶媒と無機金属塩とを含み、前記無機金属塩がインジウムとガリウムとを含んでおり、前記溶媒がジプロピレングリコールモノメチルエーテルを含む金属酸化物半導体層形成用組成物による。
[化1]
(式中、R1は炭素原子数2〜3の直鎖又は分岐のアルキレン基、R2は炭素原子数1〜3の直鎖又は分岐のアルキル基を表す。)
【選択図】なし
Description
第3観点として、前記無機金属塩が硝酸インジウムである第2観点に記載の金属酸化物半導体層形成用組成物であり、
第4観点として、前記一般式[1]で表される溶媒がジプロピレングリコールモノメチルエーテル、ジプロピレングリコールモノエチルエーテル及びジプロピレングリコールモノプロピルエーテルからなる群から選択される少なくとも1種である第1観点〜第3観点のいずれか一つに記載の金属酸化物半導体層形成用組成物であり、
第5観点として、前記一般式[1]で表される溶媒の含有率が、1〜39質量%であることを特徴とする第1観点〜第4観点のいずれか一項に記載の金属酸化物半導体層形成用組成物であり、
第6観点として、前記無機金属塩に対して1〜1000質量%の第一アミドを含む第1観点〜第5観点のいずれか一つに記載の金属酸化物半導体層形成用組成物であり、
第7観点として、第1観点〜第6観点の何れか一つに記載の金属酸化物半導体層形成用組成物を塗布して前駆体薄膜を形成する工程(a)と、前記前駆体薄膜を150℃以上350℃以下で焼成する工程(b)と、を有する金属酸化物半導体層の製造方法であり、
第8観点として、前記工程(a)と工程(b)との間に、前記前駆体薄膜を120℃以下の温度で乾燥させる工程を有する第7観点に記載の金属酸化物半導体層の製造方法であり、
第9観点として、第7観点〜第8観点の何れか一つに記載の金属酸化物半導体層の製造方法により製造されたものである金属酸化物半導体層であり、
第10観点として、第9観点に記載の金属酸化物半導体層を有すること半導体デバイスであり、
第11観点として、基板と、半導体層と、ソース電極と、ドレイン電極とを少なくとも有し、前記半導体層が第9観点に記載の金属酸化物半導体層である電界効果トランジスタであり、
第12観点として、第7観点に記載の工程(a)と工程(b)の後に、350℃を超え600℃以下で焼成して金属酸化物半導体層を金属酸化物導電層に転換する工程(c)を行う金属酸化物導電体層の製造方法であり、
第13観点として、前記工程(a)と工程(b)との間に、前記前駆体薄膜を120℃以下の温度で乾燥させる工程を有する第12観点に記載の金属酸化物導電体層の製造方法、である。
本発明の金属酸化物半導体層形成用組成物から得られた膜が半導体層であることの確認及び移動度評価は、前記組成物を用いて作成した半導体層を具備した薄膜トランジスタ1D(図2)を作製することで行った。
[式1]
ID=WCμ(VG−VT)2/2L (1)
(式中、Wはトランジスタのチャネル幅、Lはトランジスタのチャネル長、Cは静電容量密度、VTは閾値電圧である。)
25mm×25mmの大きさの熱酸化膜付きの低抵抗シリコン基板上に、0.2μmのポリテトラフルオロエチレン製フィルターを通した金属酸化物半導体層形成用組成物を硬化後の膜厚が9nmになるようにスピンコート法により塗布し、薄膜を形成した。30秒間静置した後、ホットプレートを用いて、60℃5分間の熱処理により金属酸化物半導体層前駆体膜に変換した。最後に、ホットプレートを用いて300℃、60分間の熱処理を行い、硬化膜を得た。この硬化膜の表面を、光学顕微鏡(100倍)を用いて観察した。膜表面にピンホールが見られたものを×、ピンホールが見られないものを○とした。
4インチウェハを4等分したシリコン基板上に、0.2μmのポリテトラフルオロエチレン製フィルターを通した金属酸化物半導体層形成用組成物をスピンコート法により塗布し、薄膜を形成した。ホットプレートを用いて、60℃5分間の熱処理により金属酸化物半導体層前駆体膜に変換した。最後に、ホットプレートを用いて300℃、60分間の熱処理を行い、硬化膜を得た。この硬化膜の膜厚を分光エリプソメトリ法により測定した。
硬化膜の平坦性の評価は、原子間力顕微鏡(AFM)を用いた。実施例及び比較例で作成した薄膜トランジスタの半導体層表面の2μm×2μmの範囲を走査し形状像を得た後、中心線平均粗さ(Ra)を算出した。中心線平均粗さを平坦性(Ra)とした。位相像は、形状像の測定と同時にモニターした。なお、半導体層が形成されていない熱酸化膜付きの低抵抗シリコン基板のRaは0.26nm以下であった。
測定装置:L−traceプローブ顕微鏡(エスアイアイ・ナノテクノロジー社製)
硝酸インジウム(III)水溶液(29.7質量%)と硝酸ガリウム(III)2.77水和物を脱イオン水(DIW)に完全に溶解させたのち、有機溶媒を加えて十分に撹拌し、金属酸化物半導体層形成用組成物1〜6(以下、組成物1〜6)を得た。各成分の添加量は表1の通りである。なお、金属の原子比はIn:Ga=93:7である。
25mm×25mmの大きさの熱酸化膜付きの低抵抗シリコン基板上に、0.2μmのポリテトラフルオロエチレン製フィルターを通した組成物1を硬化膜の膜厚が9nmになるようにスピンコート法により塗布し、組成物1からなる薄膜を形成した後、ホットプレートを用いて、60℃、5分間の熱処理により金属酸化物半導体層前駆体膜に変換した。次に膜中の不純物を除去するため、金属酸化物半導体層前駆体膜にUVオゾン処理を行った。なお、UVオゾン処理は、セン特殊光源(SEN LIGHTS CORPORATION)製のUVオゾン発生装置を用いた。光源はPL2003N−10、電源はUE2003N−7である。最後に、ホットプレートを用いて300℃、60分間の熱処理を行い、硬化膜を得た。得られた硬化膜はRaが0.28nmと良好な値であった。この硬化膜を用いて、前記薄膜トランジスタの作製の手順に従って薄膜トランジスタを作成した。硬化膜はn型の半導体特性を示し、膜が金属酸化物半導体層であることが確認された。移動度は7.5cm2/Vsと高い値を示した。また、ピンホールを評価するため、組成物1を用い前記の成膜性評価の手順に従ってピンホール評価用の硬化膜を作製した。表2の通り、ピンホールは全く発生しなかった。
組成物2を用いたこと以外は実施例1と同様に行って硬化膜を得た。得られた硬化膜はRaが0.28nmと良好な値であり、同時に移動度は6.7cm2/Vsと高い値を示した。
組成物3を用いたこと以外は実施例1と同様に行って硬化膜を得た。
25mm×25mmの大きさの熱酸化膜付きの低抵抗シリコン基板上に、0.2μmのポリテトラフルオロエチレン製フィルターを通した組成物1を硬化後の膜厚が9nmになるようにスピンコート法により塗布し、組成物1からなる薄膜を形成した後、ホットプレートを用いて、60℃、5分間の熱処理により金属酸化物半導体層前駆体膜に変換した。次にホットプレートを用いて300℃、60分間の熱処理を行い、硬化膜を得た。得られた硬化膜はRaが0.27nmと良好な値であった。この硬化膜を用いて、前記薄膜トランジスタの作製の手順に従って薄膜トランジスタを作成した。硬化膜はn型の半導体特性を示し、膜が金属酸化物半導体層であることが確認された。移動度は6.7cm2/Vsと高い値を示した。また、ピンホールを評価するため、組成物1を用い前記の成膜性評価の手順に従ってピンホール評価用の硬化膜を得た。得られた硬化膜はピンホールがなく、平坦な膜が形成できた。
組成物4を用いたこと以外は実施例1と同様に行って硬化膜を得た。得られた硬化膜は、移動度が6.5cm2/Vsであったが、膜表面にピンホールが存在し、さらに、Raが0.59nmと悪く、平坦な膜は形成できなかった。組成物4は実用上使用に適さない。
組成物5を用いたこと以外は実施例1と同様に行って硬化膜を得た。得られた硬化膜は、ピンホールが存在した。また、Raが1.72nmと極めて悪く、平坦な膜は形成できなかった。さらに、移動度は3.3cm2/Vsと悪い値を示した。組成物5は実用上使用に適さない。
組成物6を用いたこと以外は実施例4と同様に行って硬化膜を得た。得られた硬化膜はピンホールがなく、平坦な膜が形成できたが、移動度が4.1cm2/Vsと悪い値を示した。
実施例4と比較例3の膜表面の形状像と位相像を図3〜6に示した。実施例4の膜は、形状像は極めて平坦であるが、位相像にて、位相の濃淡が現れた。AFM測定法による位相は膜の硬度や吸着力により変化するといわれていることから、実施例4の膜は、部位によって表面物性が異なることを示している。膜がInGaOであること、実施例4の膜の移動度が高いことを考慮すると、この位相像の濃淡は、結晶化度の違いを示すものであると推察できる。一方、比較例3の膜は、濃淡のない位相像が得られた。つまり、比較例3に用いられたエチレングリコールは極性が高いため、実施例4のジプロピレングリコールモノメチルエーテルと比較すると膜の中に残存しやすく、膜の硬化(結晶化)を阻害している可能性がある。
硝酸インジウム(III)水溶液(29.7質量%)と硝酸亜鉛(II)水溶液(37.9質量%)を脱イオン水(DIW)に完全に溶解させたのち、有機溶媒を加えて十分に撹拌し、金属酸化物半導体層形成用組成物7、8(以下、組成物7、8)を得た。各成分の添加量は表4の通りである。
25mm×25mmの大きさの熱酸化膜付きの低抵抗シリコン基板上に、0.2μmのポリテトラフルオロエチレン製フィルターを通した組成物7を硬化膜の膜厚が9nmになるようにスピンコート法により塗布し、組成物7からなる薄膜を形成した後、ホットプレートを用いて、60℃、5分間の熱処理により金属酸化物半導体層前駆体膜に変換した。次に膜中の不純物を除去するため、金属酸化物半導体層前駆体膜にUVオゾン処理を行った。なお、UVオゾン処理は、セン特殊光源(SEN LIGHTS CORPORATION)製のUVオゾン発生装置を用いた。光源はPL2003N−10、電源はUE2003N−7である。最後に、ホットプレートを用いて300℃、60分間の熱処理を行い、硬化膜を得た。この硬化膜を用いて、前記薄膜トランジスタの作製の手順に従って薄膜トランジスタを作成した。硬化膜はn型の半導体特性を示し、膜が金属酸化物半導体層であることが確認された。
実施例5と同様に行って硬化膜を形成した後、ホットプレートを用いて400℃、60分間の熱処理を行った。この硬化膜を用いて、前記薄膜トランジスタの作製の手順に従って薄膜トランジスタを作成した。この硬化膜は半導体としては機能しなかったが、高い導電を示し導電体層であることが確認された。本発明の金属酸化物半導体層は、高温で熱処理することで導電体層に変換できることが確認された。
実施例5と同様に行って硬化膜を形成した後、ホットプレートを用いて500℃、60分間の熱処理を行った。この硬化膜を用いて、前記薄膜トランジスタの作製の手順に従って薄膜トランジスタを作成した。この硬化膜は半導体としては機能しなかったが高い導電を示し導電体層であることが確認された。本発明の金属酸化物半導体層は、高温で熱処理することで導電体層に変換できることが確認された。
組成物8を用いた以外は実施例5と同様に行って硬化膜を得た。この硬化膜を用いて、前記薄膜トランジスタの作製の手順に従って薄膜トランジスタを作成した。硬化膜はn型の半導体特性を示し、膜が金属酸化物半導体層であることが確認された。
組成物8を用いた以外は実施例5と同様に行って硬化膜を形成した後、ホットプレートを用いて400℃、60分間の熱処理を行った。この硬化膜を用いて、前記薄膜トランジスタの作製の手順に従って薄膜トランジスタを作成した。この硬化膜は半導体としては機能しなかったが高い導電を示し導電体層であることが確認された。本発明の金属酸化物半導体層は、高温で熱処理することで導電体層に変換できることが確認された。
組成物8を用いた以外は実施例5と同様に行って硬化膜を形成した後、ホットプレートを用いて500℃、60分間の熱処理を行った。この硬化膜を用いて、前記薄膜トランジスタの作製の手順に従って薄膜トランジスタを作成した。この硬化膜は半導体としては機能しなかったが、高い導電を示し導電体層であることが確認された。本発明の金属酸化物半導体層は、高温で熱処理することで導電体層に変換できることが確認された。
2 基板
3 ゲート電極
4 ゲート絶縁膜
5 ソース電極
6 ドレイン電極
7 半導体層(金属酸化物半導体層)
8,10 配線
9,11 電源
12 陽極
13 正孔輸送層
14 発光層
15 電子輸送層
16 陰極
Claims (11)
- 一般式[1]で表される溶媒と無機金属塩とを含み、前記無機金属塩がインジウムとガリウムとを含んでおり、前記溶媒がジプロピレングリコールモノメチルエーテルを含むことを特徴とする金属酸化物半導体層形成用組成物。
- 前記無機金属塩が硝酸インジウム、及び硝酸ガリウムである請求項1に記載の金属酸化物半導体層形成用組成物。
- 前記一般式[1]で表される溶媒の含有率が、1〜39質量%である請求項1又は2に記載の金属酸化物半導体層形成用組成物。
- 前記無機金属塩に対して1〜1000質量%の第一アミドを含む請求項1〜3のいずれか一項に記載の金属酸化物半導体層形成用組成物。
- 請求項1〜4の何れか一項に記載の金属酸化物半導体層形成用組成物を塗布して前駆体薄膜を形成する工程(a)と、前記前駆体薄膜を150℃以上350℃以下で焼成する工程(b)と、を有する金属酸化物半導体層の製造方法。
- 前記工程(a)と工程(b)との間に、前記前駆体薄膜を120℃以下の温度で乾燥させる工程を有する請求項5に記載の金属酸化物半導体層の製造方法。
- 請求項5又は6に記載の金属酸化物半導体層の製造方法により製造されたものである金属酸化物半導体層。
- 請求項7に記載の金属酸化物半導体層を有することを特徴とする半導体デバイス。
- 基板と、半導体層と、ソース電極と、ドレイン電極とを少なくとも有し、前記半導体層が請求項7に記載の金属酸化物半導体層である電界効果トランジスタ。
- 請求項5に記載の工程(a)と工程(b)の後に、350℃を超え600℃以下で焼成して金属酸化物半導体層を金属酸化物導電層に転換する工程(c)を行う金属酸化物導電体層の製造方法。
- 前記工程(a)と工程(b)との間に、前記前駆体薄膜を120℃以下の温度で乾燥させる工程を有する請求項10に記載の金属酸化物導電体層の製造方法。
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JP2014011190A (ja) | 2012-06-27 | 2014-01-20 | Idemitsu Kosan Co Ltd | 半導体用混合溶液、半導体薄膜、および薄膜トランジスタ |
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TWI694526B (zh) | 2020-05-21 |
JP6819896B2 (ja) | 2021-01-27 |
KR102365438B1 (ko) | 2022-02-18 |
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CN106537569B (zh) | 2020-04-03 |
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