JP6654753B2 - 基板構造およびその調製方法 - Google Patents
基板構造およびその調製方法 Download PDFInfo
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- JP6654753B2 JP6654753B2 JP2016538483A JP2016538483A JP6654753B2 JP 6654753 B2 JP6654753 B2 JP 6654753B2 JP 2016538483 A JP2016538483 A JP 2016538483A JP 2016538483 A JP2016538483 A JP 2016538483A JP 6654753 B2 JP6654753 B2 JP 6654753B2
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Images
Classifications
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
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- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
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- C23C16/45529—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making a layer stack of alternating different compositions or gradient compositions
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- H—ELECTRICITY
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Description
(上記の式1において、mは1以上であり、
R1は、C1〜20アルキル、C5〜20シクロアルキル、または5〜60個の核原子のアリールもしくはヘテロアリールであり、
Mは、Zn、Sn、In、Cd、Ga、Al、Ti、Si、V、Mn、Fe、Co、Cu、Zr、Ru、Mo、NbおよびWからなる群から選択され、
XまたはYは、O、S、N、NHおよびCOからなる群から選択され、かつXまたはYのいずれか一方はSである。)
0≦(dn/d0)≦0.1(0≦n≦240)。
0≦(dn/d0)≦0.1(0≦n≦240)。
0≦(Dn/D0)≦0.1(0≦n≦240)。
(1)以下の式2によって表される第1の前駆体化合物を用いて、無機分子層を形成する工程、
[式2]M(R21)(R22)...(R2n)
(上記の式2において、Mは、Zn、Sn、Cd、Ti、Si、V、Mn、Fe、Co、Cu、Zr、Ru、Mo、Nb、W、In、Ga、AlおよびTlからなる群から選択され、
nは、金属Mの酸化数の状態に従って決定され、
R21からR2nはそれぞれ独立して、C1〜20アルキル、C1〜20アルコキシド、塩化物の基、水酸化物の基、オキシ水酸化物の基、ニトレート基、カーボネート基、アセテート基、またはオキサレート基である。)および、
(2)以下の式3によって表される第2の前駆体化合物を無機分子層と反応させて、無機分子層上に有機分子層を形成する工程
[式3]R3−S−R4−R5
(上記の式3において、R3は、水素、COR6、C1〜20アルキル、C5〜20シクロアルキル、または5〜60個の核原子のアリールもしくはヘテロアリールであり、
R4は、C1〜20アルキル、C5〜20シクロアルキル、または5〜60個の核原子のアリールもしくはヘテロアリールであり、
R5は、C1〜20アルコキシ基、エーテル基、カルボキシル基、COR6、チオール基およびアミン基からなる群から選択される1つまたは複数の種であり、
R6は、水素、アルコキシ基、エーテル基、カルボキシル基、チオール基、およびアミン基からなる群から選択される1つまたは複数の種である。)
を含む基板構造を調製する方法を提供する。
実施例1において、ジエチル亜鉛(DEZn)の第1の前駆体化合物の噴射時間に従う薄膜の成長速度、および4−メルカプトフェノールの第2の前駆体化合物の噴射時間に従う薄膜の成長速度を測定し、それぞれ図7および図8に示した。
KBrペレットをSi基板および4−メルカプトフェノールの代わりに用いたこと以外は実施例1と同じ方法で調製した有機−無機ハイブリッド薄膜のIR分光学的測定を行った。結果を図9に示す。
上記の実施例1において調製した有機−無機ハイブリッド薄膜のUV−Vis吸収を測定した。結果を図10に示す。図10から、本発明に従う有機−無機ハイブリッド薄膜は、可視光線範囲に吸収が認められないことを確認することができる。
比較例において、ジエチル亜鉛(DEZn)を第1の前駆体化合物として用いて、分子層堆積法に従ってジエチル亜鉛(DEZn)薄膜をSi基板上に堆積させてから、ヒドロキノン(HQ)を第2の前駆体化合物として用いたこと以外は、上記の実施例1と同じ方法で有機−無機ハイブリッド薄膜を調製した。
上記の実施例1の有機−無機ハイブリッド薄膜および比較例において調製した有機−無機ハイブリッド薄膜を空気中に置きながら、厚さの変化を測定して、空気中の安定性を試験した。結果を図11に示す。
実施例2において調製した厚さが50nmの有機−無機ハイブリッド薄膜を、表面粗さについてAFMにより測定した。結果を図13に示す。測定された平均粗さは、2.2Åであった。
実施例3において、トリメチルアルミニウム(TMA)の第1の前駆体化合物の噴射時間に従う薄膜の成長速度、および4−メルカプトフェノールの第2の前駆体化合物の噴射時間に従う薄膜の成長速度を測定し、それぞれ図14および図15に示した。
KBrペレットをSi基板および4−メルカプトフェノールの代わりに用いたこと以外は実施例3と同じ方法で調製した有機−無機ハイブリッド薄膜のIR分光学的測定を行った。結果を図16に示す。
上記の実施例3において調製した有機−無機ハイブリッド薄膜のUV−Vis吸収を測定した。結果を図17に示す。図17から、本発明に従う有機−無機ハイブリッド薄膜は、可視光線範囲に吸収が認められないことを確認することができる。
上記の実施例3の有機−無機ハイブリッド薄膜および比較例において調製した有機−無機ハイブリッド薄膜を空気中に置きながら、厚さの変化を測定して、空気中の安定性を試験した。結果を図18に示す。
実施例4において調製した厚さが50nmの有機−無機ハイブリッド薄膜を、表面粗さについてAFMにより測定した。結果を図20に示す。測定された平均粗さは、2.8Åであった。
上記の実施例5において調製した有機−無機ハイブリッド薄膜:Al2O3薄膜の比率が1:2のときにTEM写真を測定した。結果を図21に示す。図21において、原子層堆積に従うAl2O3薄膜および本発明に従う有機−無機ハイブリッド薄膜が交互に形成されたことを確認することができる。
上記の実施例5において、有機−無機ハイブリッド薄膜の厚さを変えることによって、ピンホール形成阻害率を測定した。結果を図22および図23に示す。
上記の実施例5において調製した有機−無機ハイブリッドの機能性薄膜において、薄膜の総厚を同じに維持しながら、Al2O3薄膜の、本発明に従う有機−無機ハイブリッド薄膜に対する比率に対して、薄膜応力を測定した。結果を図24に示す。
上記の実施例5において調製した有機−無機ハイブリッドの機能性薄膜、および比較例のAl2O3薄膜を、耐水分透過性および耐酸素透過性について測定した。結果を以下の表1および図25に記載する。
20 有機−無機ハイブリッド薄膜
30 酸化物層
40 第1の耐化学薬品層
50 第2の耐化学薬品層
60 保護層
100 Si
Claims (22)
- 基板、
以下の式1:
[式1]−[M−X−R1−Y−]m−
(前記式1において、mは1以上であり、
R1は、置換または非置換の5〜60個の核原子のアリールもしくはヘテロアリールであり、
Mは、Zn、Sn、In、Cd、Ga、Al、Ti、Si、V、Mn、Fe、Co、Cu、Zr、Ru、Mo、NbおよびWからなる群から選択され、
XまたはYは、O、S、N、NHおよびCOからなる群から選択され、かつXまたはYのいずれか一方はSである)
に表される有機−無機ハイブリッド薄膜、および
該有機−無機ハイブリッド薄膜上に、原子層堆積法により設けられたZn、Sn、In、Cd、Ga、Al、Ti、Si、V、Mn、Fe、Co、Cu、Zr、Ru、Mo、NbおよびWからなる群から選択される金属の酸化物層を備える基板構造体。 - 前記有機−無機ハイブリッド薄膜の厚さは、1Åから500Åに及ぶ、請求項1に記載の基板構造体。
- 有機−無機ハイブリッド薄膜およびZn、Sn、In、Cd、Ga、Al、Ti、Si、V、Mn、Fe、Co、Cu、Zr、Ru、Mo、NbおよびWからなる群から選択される金属の酸化物層が機能性薄膜として設けられている請求項1に記載の基板構造体。
- 前記金属酸化物層の厚さは、10Åから2000Åに及ぶ、請求項3に記載の基板構造体。
- 前記基板は、ITO、FTO、ZnO、AZO、CdOおよびTiO2からなる群から選択される導電性透明基板である、請求項1または請求項3に記載の基板構造体。
- 前記基板は、フルオロポリマー樹脂、ポリエステル、ポリアクリレート、ポリアミド、ポリイミドおよびポリカーボネートからなる群から選択されるポリマー基板である、請求項1または請求項3に記載の基板構造体。
- 前記ポリマー基板は、ポリフッ化ビニリデン(PVDF)、ポリエチレンテレフタレート(PET)、ポリエチレンナフタレート(PEN)およびポリメチルメタクリレート(PMMA)からなる群から選択される、請求項6に記載の基板構造体。
- 前記基板と前記有機−無機ハイブリッド薄膜との間に第1の耐化学薬品層をさらに備える、請求項1に記載の基板構造体。
- 前記基板の下方に第2の耐化学薬品層をさらに備える、請求項1に記載の基板構造体。
- 前記有機−無機ハイブリッド薄膜の上部に保護層をさらに備える、請求項1に記載の基板構造体。
- 請求項1に記載の基板構造体を備える発光体。
- 請求項1に記載の基板構造体を備える表示装置。
- 請求項1に記載の基板構造体を備えるソーラー・バッテリ・セル。
- 請求項1に記載の基板構造体を製造する方法であって、
(1)以下の式2によって表される第1の前駆体化合物を用いて、無機分子層を形成する工程、
[式2]M(R21)(R22)...(R2n)
(前記式2において、Mは、Zn、Sn、Cd、Ti、Si、V、Mn、Fe、Co、Cu、Zr、Ru、Mo、Nb、W、In、GaおよびAlからなる群から選択され、
nは、前記金属Mの酸化数の状態に従って決定され、
R21からR2nはそれぞれ独立して、C1〜20アルキル、C1〜20アルコキシド、塩化物の基、水酸化物の基、オキシ水酸化物の基、ニトレート基、カーボネート基、アセテート基、またはオキサレート基である。)および、
(2)以下の式3によって表される第2の前駆体化合物を前記無機分子層と反応させて、前記無機分子層上に有機分子層を形成する工程
[式3]R3−S−R4−R5
(前記式3において、R3は、水素、COR6、C1〜20アルキル、C5〜20シクロアルキル、または5〜60個の核原子のアリールもしくはヘテロアリールであり、
R4は、5〜60個の核原子のアリールもしくはヘテロアリールであり、
R5は、C1〜20アルコキシ基、エーテル基、カルボキシル基、COR6、チオール基およびアミン基からなる群から選択される1つまたは複数の種であり、
R6は、水素、アルコキシ基、エーテル基、カルボキシル基、チオール基、およびアミン基からなる群から選択される1つまたは複数の種である。)
を含む方法。 - 前記工程(1)および前記工程(2)を繰り返し実行することをさらに含む、請求項14に記載の、基板構造体を製造する方法。
- 前記工程(1)に先立って酸化物層を基板表面上に形成する工程をさらに含む、請求項14に記載の、基板構造体を製造する方法。
- Zn、Sn、In、Cd、Ga、Al、Ti、Si、V、Mn、Fe、Co、Cu、Zr、Ru、Mo、NbおよびWからなる群から選択される金属の酸化物層を原子層堆積によって形成する工程(3)をさらに含む、請求項14に記載の、基板構造体を製造する方法。
- 前記工程(1)および前記工程(2)をそれぞれn1回(n1は、1以上である)繰り返し実行した後に、前記工程(3)をn2回(n2は、1以上である)繰り返し実行する、請求項14に記載の、基板構造体を製造する方法。
- 前記工程(1)から前記工程(3)を繰り返し実行する、請求項21に記載の、基板構造体を製造する方法。
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