JP5967983B2 - シリコン含有膜及びシリコン含有膜形成方法 - Google Patents
シリコン含有膜及びシリコン含有膜形成方法 Download PDFInfo
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- JP5967983B2 JP5967983B2 JP2012050961A JP2012050961A JP5967983B2 JP 5967983 B2 JP5967983 B2 JP 5967983B2 JP 2012050961 A JP2012050961 A JP 2012050961A JP 2012050961 A JP2012050961 A JP 2012050961A JP 5967983 B2 JP5967983 B2 JP 5967983B2
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims description 57
- 229910052710 silicon Inorganic materials 0.000 title claims description 53
- 239000010703 silicon Substances 0.000 title claims description 51
- 238000000034 method Methods 0.000 title description 13
- 239000010408 film Substances 0.000 claims description 163
- 238000005229 chemical vapour deposition Methods 0.000 claims description 46
- 239000000758 substrate Substances 0.000 claims description 36
- 239000010409 thin film Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 239000010410 layer Substances 0.000 description 199
- 230000004888 barrier function Effects 0.000 description 66
- 239000007789 gas Substances 0.000 description 51
- 239000002585 base Substances 0.000 description 30
- 238000007789 sealing Methods 0.000 description 20
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 16
- 125000004430 oxygen atom Chemical group O* 0.000 description 16
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 14
- 230000015572 biosynthetic process Effects 0.000 description 13
- 238000011156 evaluation Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 9
- 238000010248 power generation Methods 0.000 description 7
- 239000002356 single layer Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000011241 protective layer Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000001133 acceleration Effects 0.000 description 5
- 229910010272 inorganic material Inorganic materials 0.000 description 5
- 239000011147 inorganic material Substances 0.000 description 5
- 239000011368 organic material Substances 0.000 description 5
- 229910052814 silicon oxide Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000007740 vapor deposition Methods 0.000 description 5
- 238000001678 elastic recoil detection analysis Methods 0.000 description 4
- 239000005038 ethylene vinyl acetate Substances 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
- 238000010030 laminating Methods 0.000 description 4
- 150000003961 organosilicon compounds Chemical class 0.000 description 4
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005001 rutherford backscattering spectroscopy Methods 0.000 description 4
- 238000006557 surface reaction Methods 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005401 electroluminescence Methods 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 2
- 229910003472 fullerene Inorganic materials 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 150000003377 silicon compounds Chemical class 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
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- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 230000002040 relaxant effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Description
上記第1化学蒸着層の厚み(L1)は5〜400nmであり、上記第2化学蒸着層の厚み(L2)は5〜500nmであることが好ましい。
さらに、上記第1化学蒸着層と第2化学蒸着層とが交互に複数層形成されていることが好ましい。
上記複数の第1化学蒸着層のトータルの厚みは、5n〜500(nm)[nは第1化学蒸着層の層数]であることが好ましい。
本発明の積層体は、上記シリコン含有膜と、基材とを備えている。
上記基材は、Ag、Al、Mo、ZnO、ITO、BZO、AZOならびにGZOからなる群から選択された何れかの電極膜を含んでいてもよい。
本発明のシリコン含有膜は、プラズマCVD法により形成され、第1化学蒸着層と、プラズマCVD法により形成された第2化学蒸着層とを備えている。第1化学蒸着層と第2化学蒸着層は、交互に複数層(n層)設けられていてもよい。nは、1以上の整数であり、好ましくは1〜10の整数、より好ましくは1〜7の整数とすることができる。また、第1化学蒸着層と第2化学蒸着層との間には、他の層が形成されていてもよい。具体的には、nが7の場合には、シリコン含有膜は、交互に設けられた各7層の第1化学蒸着層と第2化学蒸着層とを有する(7層/7層)。また、応力緩和層n層とバリア層n+1層が交互に積層されていてもよく、バリア層が2層に対して応力緩和層が1層積層されたような形態でもよい。また、応力緩和層n+1層とバリア層n層が交互に積層されていてもよく、応力緩和層が2層に対してバリア層が1層積層されたような形態でもよい。
第1化学蒸着層(以下、応力緩和層と称する場合がある)は、シリコン元素を含み、酸素濃度が0元素%以上10元素%未満である。応力緩和層は、ケイ素原子と酸素原子とに加えて、炭素原子を含んでいても良い。本発明において、応力緩和層の組成は、酸素原子が10元素%未満であり、ケイ素原子が例えば10〜20元素%、炭素原子が例えば20〜35元素%であってもよい。さらに、水素原子を例えば30〜55元素%含んでいても良い。窒素原子は、例えば、10元素%以下(0〜10元素%程度)含んでいてもよい。
第2化学蒸着層(以下、バリア層と称する場合がある)は、シリコン元素を含み、酸素濃度が35元素%超70元素%以下である。バリア層は、酸素原子が60〜70元素%であり、ケイ素原子が例えば30〜35元素%であってもよい。さらに炭素原子を含んでいても良い。さらに、水素原子を例えば5元素%以下(0〜5元素%程度)含んでいても良い。窒素原子は含まれていなくてもよい。
本発明のシリコン含有膜では、第1化学蒸着層の厚み(L1)と第2化学蒸着層の厚み(L2)の比L2/L1が1.5〜9である。L2/L1がこのような範囲にあることにより、低応力でかつ水分を吸収を少なくできる。L2/L1は、1.8〜8であることが好ましく、2.5〜8であることがより好ましい。L1、L2は、単層の厚みであっても良く、または、トータル厚みであっても良い。
本発明において、上記の各層及び膜中の酸素原子の濃度は、ラザフォード後方散乱分光法(RBS)、及び、水素前方散乱分析法を用いた組成分析(HFS)により決定できる。ケイ素原子、炭素原子の濃度も同様に測定できる。水素原子についてはRBSでは分析できないため、HFSにより測定する。
図1〜3に本発明の一実施形態に係るシリコン含有膜100、200、300をそれぞれ含む積層体1A、1B、1Cを概略的に示す。図1の積層体1Aでは、シリコン含有膜100は、各1層の応力緩和層4、バリア層2から構成される。8は基材であり、この基材上に、下地膜6、応力緩和層4、バリア層2がこの順に積層されている。図2、3の積層体1B、1Cでは、シリコン含有膜200、300は、各2層の交互に積層された応力緩和層4、バリア層2から構成される。そして、基材8上に、下地膜6、応力緩和層4、バリア層2、応力緩和層4、バリア層2がこの順に積層されている。積層体1Cは、積層体1Bと比較して、バリア層の厚みが広い例を示している。積層体において、下地膜は設けなくてもよい。また、応力緩和層とバリア層の積層順は任意であり、基材上にバリア層が積層され、その上に応力緩和層が積層されていてもよく、その逆でもよい。
(i) 基材/(下地膜:設けなくても良い。以下同じ)/応力緩和層/バリア層/・・・/応力緩和層/バリア層
(ii) 基材/(下地膜)/バリア層/応力緩和層/・・・/応力緩和層/バリア層
(iii) 基材/(下地膜)/応力緩和層/バリア層/・・・/バリア層/応力緩和層
(iv) 基材/(下地膜)/バリア層/応力緩和層/・・・/バリア層/応力緩和層
上記基材としては、有機物からなる膜、無機物からなる膜、有機物と無機物の双方を含む膜が挙げられる。基材における有機物としては、PETフィルム等のポリマーフィルムが挙げられる。また、無機物としては、Ag、Al、Mo、ZnO、ITO、BZO、AZO、ならびにGZO等の電極膜などが挙げられる。
上記下地膜としては、プラズマCVD法により形成され、ケイ素原子と酸素原子とを少なくとも含んでおり、酸素原子の濃度が10〜35元素%である膜等が挙げられる。下地膜は、主として、シリコン含有膜と基材との密着性を向上させるために設けることが出来る。
上記積層体の製造方法は、基材上に、酸素原子を含有する有機ケイ素化合物からなる原料ガスを用いてプラズマCVD法により下地膜を形成する第1工程と;第1工程で形成した下地膜上に、有機ケイ素化合物と水素原子を含有する化合物とからなる原料ガスを用いてプラズマCVD法により、第1化学蒸着層を形成する第2工程と;有機ケイ素化合物と酸素原子を含有する化合物とからなる原料ガスを用いてプラズマCVD法により、第2化学蒸着層を形成する第3工程とを含んでいてもよい。第2、3工程を交互に複数回行うことにより、複数層の第1化学蒸着層と第2化学蒸着層が交互に積層された積層体を得ることができる。第1工程は行わなくても良く、基材上に先ず第3工程により第2化学蒸着層を形成し、その後第2工程を行っても良い。
図6に、本発明の一実施形態に係る薄膜太陽電池セル20の断面を概略的に示すと、21はプラスチック基板、22はITO電極である。23はフタロシアニン蒸着膜、24はフラーレン蒸着膜である。25はLiF層、26はAg電極である。これらの、有機物と無機物を含む基板上に、シリコン含有膜1が積層されている。
ガラス基板の表面の一部に、厚さ200nmのAg層を形成した。この基板を、Ag層を有する面がループアンテナ側に向くように、成膜室内の基板固定台上に配置した。次に排気系により成膜室の内圧を9.9×10-5Pa以下になるまで減圧した。成膜室内の減圧が完了後、HMDSOガスを成膜室に導入した。HMDSOガスの導入速度は、3sccm〜45sccmとした。
実施例1において、応力緩和層ならびにバリア層の膜厚、積層数を表2に示すように変更した以外は実施例1と同様にして、各積層体を得た。比較例2と5では、バリア層は設けなかった。
実施例1〜5ならびに比較例1〜8で得られた積層体の、製膜直後の剥がれ状態を目視観察した。結果を下記の基準により評価した。結果を表2に示す。
○:シリコン含有膜の浮きや剥がれが観察されなかった
×:シリコン含有膜の浮きや剥がれが観察された
実施例1〜5ならびに比較例2、3、5〜8で得られた積層体を、85℃、85%RHの環境に放置し、加速試験を行った。製膜直後と、加速試験後500時間後、1000時間後のシリコン含有膜の基材からの剥離状態を目視観察した。結果を下記の基準により評価した。結果を表2に示す。
○:シリコン含有膜の浮きや剥がれが観察されなかった
△:ボツボツと剥離が観察された
×:全面剥離した
1A、1B、1C 積層体
2 バリア層
4 応力緩和層
6 下地膜
8 基材
20 薄膜太陽電池セル
21 プラスチック基板
22 ITO電極
23 フタロシアニン蒸着膜
24 フラーレン蒸着膜
25 LiF層
26 Ag電極
Claims (7)
- シリコン濃度が10元素%以上20元素%未満であり、水素濃度が30元素%以上55元素%未満であり、炭素濃度が20元素%以上35元素%未満であり、酸素濃度が10元素%以下である、第1化学蒸着層と;シリコン濃度が30元素%以上35元素%未満であり、水素濃度が5元素%以下であり、酸素濃度が35元素%超70元素%以下である、第2化学蒸着層と;を備えたシリコン含有膜であって、
該第1化学蒸着層の厚み(L1)と該第2化学蒸着層の厚み(L2)の比L2/L1が1.5〜9である、シリコン含有膜。 - 該第1化学蒸着層の厚み(L1)が5〜400nmであり、該第2化学蒸着層の厚み(L2)が5〜500nmである、請求項1記載のシリコン含有膜。
- 前記第1化学蒸着層と第2化学蒸着層とが交互に複数層形成された、請求項1又は2記載のシリコン含有膜。
- 前記複数の第1化学蒸着層のトータルの厚みが5n〜500(nm)[nは第1化学蒸着層の層数]である、請求項3記載のシリコン含有膜。
- 請求項1〜4の何れか1項に記載のシリコン含有膜と、基材とを備えた、積層体。
- 前記基材が、Ag、Al、Mo、ZnO、ITO、BZO、AZOならびにGZOからなる群から選択された何れかの電極膜を含む、請求項5記載の積層体。
- 請求項1〜6記載のシリコン含有膜を含む、有機エレクトロルミネセンス素子または薄膜太陽電池セル。
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