JP7240580B2 - 成膜方法 - Google Patents
成膜方法 Download PDFInfo
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- JP7240580B2 JP7240580B2 JP2017558233A JP2017558233A JP7240580B2 JP 7240580 B2 JP7240580 B2 JP 7240580B2 JP 2017558233 A JP2017558233 A JP 2017558233A JP 2017558233 A JP2017558233 A JP 2017558233A JP 7240580 B2 JP7240580 B2 JP 7240580B2
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- 125000001792 phenanthrenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C=CC12)* 0.000 description 1
- 125000004934 phenanthridinyl group Chemical group C1(=CC=CC2=NC=C3C=CC=CC3=C12)* 0.000 description 1
- 125000001791 phenazinyl group Chemical group C1(=CC=CC2=NC3=CC=CC=C3N=C12)* 0.000 description 1
- 125000001484 phenothiazinyl group Chemical group C1(=CC=CC=2SC3=CC=CC=C3NC12)* 0.000 description 1
- 125000005954 phenoxathiinyl group Chemical group 0.000 description 1
- 125000001644 phenoxazinyl group Chemical group C1(=CC=CC=2OC3=CC=CC=C3NC12)* 0.000 description 1
- 125000002467 phosphate group Chemical class [H]OP(=O)(O[H])O[*] 0.000 description 1
- 230000001443 photoexcitation Effects 0.000 description 1
- 125000004592 phthalazinyl group Chemical group C1(=NN=CC2=CC=CC=C12)* 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 125000004193 piperazinyl group Chemical group 0.000 description 1
- 125000000587 piperidin-1-yl group Chemical group [H]C1([H])N(*)C([H])([H])C([H])([H])C([H])([H])C1([H])[H] 0.000 description 1
- 125000005936 piperidyl group Chemical group 0.000 description 1
- 229920003227 poly(N-vinyl carbazole) Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
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- 229920000767 polyaniline Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920013716 polyethylene resin Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 125000000561 purinyl group Chemical group N1=C(N=C2N=CNC2=C1)* 0.000 description 1
- 125000003373 pyrazinyl group Chemical group 0.000 description 1
- 125000003226 pyrazolyl group Chemical group 0.000 description 1
- 125000001725 pyrenyl group Chemical group 0.000 description 1
- 125000002098 pyridazinyl group Chemical group 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 125000000714 pyrimidinyl group Chemical group 0.000 description 1
- 125000000168 pyrrolyl group Chemical group 0.000 description 1
- 125000002294 quinazolinyl group Chemical group N1=C(N=CC2=CC=CC=C12)* 0.000 description 1
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical class C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 1
- 125000005493 quinolyl group Chemical group 0.000 description 1
- 125000001567 quinoxalinyl group Chemical group N1=C(C=NC2=CC=CC=C12)* 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 125000000547 substituted alkyl group Chemical group 0.000 description 1
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- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 150000000000 tetracarboxylic acids Chemical class 0.000 description 1
- 125000001935 tetracenyl group Chemical group C1(=CC=CC2=CC3=CC4=CC=CC=C4C=C3C=C12)* 0.000 description 1
- 125000003718 tetrahydrofuranyl group Chemical group 0.000 description 1
- 125000001412 tetrahydropyranyl group Chemical group 0.000 description 1
- 125000003831 tetrazolyl group Chemical group 0.000 description 1
- 125000004627 thianthrenyl group Chemical group C1(=CC=CC=2SC3=CC=CC=C3SC12)* 0.000 description 1
- 125000000335 thiazolyl group Chemical group 0.000 description 1
- 125000001544 thienyl group Chemical group 0.000 description 1
- 125000001166 thiolanyl group Chemical group 0.000 description 1
- IBBLKSWSCDAPIF-UHFFFAOYSA-N thiopyran Chemical compound S1C=CC=C=C1 IBBLKSWSCDAPIF-UHFFFAOYSA-N 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 125000005259 triarylamine group Chemical group 0.000 description 1
- 125000004306 triazinyl group Chemical group 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- YFHICDDUDORKJB-UHFFFAOYSA-N trimethylene carbonate Chemical compound O=C1OCCCO1 YFHICDDUDORKJB-UHFFFAOYSA-N 0.000 description 1
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 1
- 150000001651 triphenylamine derivatives Chemical class 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 125000005023 xylyl group Chemical group 0.000 description 1
- 229940063789 zinc sulfide Drugs 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
- 125000004933 β-carbolinyl group Chemical group C1(=NC=CC=2C3=CC=CC=C3NC12)* 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Images
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- B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
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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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- 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
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
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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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- C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4486—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by producing an aerosol and subsequent evaporation of the droplets or particles
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Description
また、本発明者らは、上記知見を得た後、さらに検討を重ねて、本発明を完成させるに至った。
[1] 非プロトン性溶媒を含む原料溶液を霧化または液滴化し、得られたミストまたは液滴をキャリアガスで基体まで搬送し、ついで前記ミストまたは液滴を反応させて前記基体上に成膜することを特徴とする成膜方法。
[2] 非プロトン性溶媒が、下記式(1)で表される前記[1]記載の成膜方法。
[3] 非プロトン性溶媒が、下記式(2)で表される前記[1]記載の成膜方法。
[4] 原料溶液が有機金属ハロゲン化物を含む前記[1]~[3]のいずれかに記載の成膜方法。
[5] 原料溶液がアンモニウム化合物を含む前記[1]~[4]のいずれかに記載の成膜方法。
[6] 前記反応が熱反応であり、前記熱反応を、250℃以下の温度で行う前記[1]~[5]のいずれかに記載の成膜方法。
[7] 基体が、ガラス基板である前記[1]~[6]のいずれかに記載の成膜方法。
[8] 基体が、スズドープ酸化インジウム膜またはフッ素ドープ酸化インジウム膜を含む前記[1]~[7]のいずれかに記載の成膜方法。
[9] 基体が、チタニア膜を含む前記[1]~[8]のいずれかに記載の成膜方法。
[10] 前記[1]~[9]のいずれかに記載の成膜方法により成膜された膜。
[11] ペロブスカイト構造を有する前記[10]記載の膜。
[12] 前記[11]記載の膜を含む光電変換素子。
[13] 原料溶液がアミン誘導体を含む前記[1]または[2]に記載の成膜方法。
[14] 原料溶液が金属錯体を含む前記[1]または[2]に記載の成膜方法。
[15] 基体上に直接または他の層を介して、少なくとも正孔輸送層及び/又は発光層を積層して有機発光素子を製造する方法において、前記正孔輸送層及び/又は発光層の積層を、非プロトン性溶媒を含む原料溶液を霧化又は液滴化し、得られたミスト又は液滴をキャリアガスで基体上まで搬送し、前記基体上で前記ミスト又は液滴を反応させて、前記基体上に成膜することにより行うことを特徴とする有機発光素子の製造方法。
[16] 原料溶液がアミン誘導体を含む前記[15]記載の有機発光素子の製造方法。
[17] 原料溶液が金属錯体を含む前記[15]記載の有機発光素子の製造方法。
[18] 前記[15]~[17]のいずれかに記載の製造方法により製造された有機発光素子。
霧化・液滴化工程は、原料溶液を霧化または液滴化する。霧化手段または液滴化手段は、原料溶液を霧化または液滴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または液滴化手段が好ましい。超音波を用いて得られたミストまたは液滴は、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。液滴サイズは、特に限定されず、数mm程度の液滴であってもよいが、好ましくは50μm以下であり、より好ましくは100nm~10μmである。
前記原料溶液は、非プロトン性溶媒を含んでおり、霧化または液滴化が可能であれば特に限定されず、無機材料を含んでいてもよいし、有機材料を含んでいてもよい。また、前記原料溶液は、無機材料および有機材料の両方の材料を含んでいてもよい。
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。
CH3NH3M1X3 ・・・(I)
(式中、M1は2価の金属イオンであり、Xは、F、Cl、BrまたはIである。)
(R6NH3)2M1X4 ・・・(II)
(式中、R6は炭素数2以上のアルキル基、アルケニル基、アラルキル基、アリール基、複素環基または芳香族複素環基であり、M1は2価の金属イオンであり、Xは、F、Cl、BrまたはIである。)
搬送工程では、キャリアガスでもって前記ミストまたは前記液滴を成膜部(例えば、成膜室)内に設置されている基体まで搬送する。前記キャリアガスとしては、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好適な例として挙げられる。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、流量を下げた希釈ガス(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。
成膜工程では、基体上で前記ミストまたは液滴を反応させることによって、基体上に、成膜する。前記反応は、乾燥による反応であってもよいが、熱による熱反応が好ましく、熱反応は、熱でもって前記ミストまたは液滴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。本工程では、前記熱反応を、通常、250℃以下で行うが、本発明においては、150℃以下が好ましく、140℃以下がより好ましい。本発明においては、低温でも良好に成膜できるので、様々な種類の基板に適用することができ、特に、基板を損傷することなく、より密着性に優れ、且つ膜本来の性質をより良好に発揮できる。下限については、本発明の目的を阻害しない限り特に限定されないが、100℃以上が好ましく、110℃以上がより好ましい。また、前記反応は、本発明の目的を阻害しない限り、真空下、非酸素雰囲気下、還元ガス雰囲気下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いが、非酸素雰囲気下または酸素雰囲気下で行われるのが好ましい。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い。なお、膜厚は、成膜時間を調整することにより、設定することができる。
前記基体は、成膜する膜を支持できるものであれば特に限定されない。伸縮性のある基体であってもよい。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。多孔質構造体であってもよい。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が、0.5μm~100mmが好ましく、1μm~10mmがより好ましい。
より具体的には、光電変換素子用電子輸送層の空孔率Cとしては、緻密層であるのが好ましく、より具体的には例えば、約20%以下であるのが好ましく、約5%以下であるのがより好ましく、約2%以下であるのが最も好ましい。これにより、短絡防止や整流作用といった効果をより向上することができる。ここで、光電変換素子用電子輸送層の空孔率の下限は、可能な限り小さいことが好ましいため、特に限定されないが、通常、約0.05%以上である。
陽極は、公知のものであってよく、前記陽極としては、例えば、前記導電性膜、前記金属膜等として例示したものなどが挙げられる。
前記有機発光素子用正孔輸送層は、通常、陽極から電荷である正孔を注入する機能、正孔を輸送する機能を有する。前記有機発光素子用正孔輸送層は、前記の有機発光素子用正孔輸送層の前駆体溶液を用いて、本発明の成膜方法により得られた膜を主成分として含んでいれば特に限定されない。前記有機発光素子用正孔輸送層の厚さは、特に限定されないが、駆動電圧低下、外部量子効率向上、耐久性向上の観点から、厚さが1nm~5μmであるのが好ましく、5nm~1μmであるのがより好ましく、10nm~500nmであるのが最も好ましい。
前記発光層は、通常、陽極と陰極の間に電圧を印加することで発光する機能を有する。前記発光層は、前記の発光層の前駆体溶液を用いて、本発明の成膜方法により得られた膜を主成分として含んでいれば特に限定されない。前記発光層の厚さは、特に限定されないが、1nm~100μmであるのが好ましく、5nm~50μmであるのがより好ましく、10nm~10μmであるのが最も好ましい。
前記有機発光素子用電子輸送層は、通常、陰極から電子を注入する機能、電子を輸送する機能、陽極から注入され得た正孔を障壁する機能のいずれかを有している。前記有機発光素子用電子輸送層の構成材料は、特に限定されず、公知の材料であってよい。前記有機発光素子用電子輸送層の構成材料としては、例えば、ピリジン、ピリミジン、トリアジン、イミダゾール、トリアゾ-ル、オキサゾ-ル、オキサジアゾ-ル、フルオレノン、アントラキノジメタン、アントロン、ジフェニルキノン、チオピランジオキシド、カルボジイミド、フルオレニリデンメタン、ジスチリルピラジン、フッ素置換芳香族化合物、ナフタレンペリレン等の複素環テトラカルボン酸無水物、フタロシアニン、およびそれらの誘導体(他の環と縮合環を形成してもよい)、8-キノリノ-ル誘導体の金属との錯体やメタルフタロシアニン、ベンゾオキサゾ-ルやベンゾチアゾ-ルを配位子とする金属との錯体に代表される各種錯体等が挙げられる。
陰極は、導電性を有するものであって、電極として機能するものであれば、特に限定されず、公知の陰極であってよい。例えば、絶縁性材料であっても、有機発光素子用電子輸送層に面している側に導電性物質層が設けてあり、電極として使用可能であれば、これを陰極として用いることができる。本発明においては、陰極は、有機発光素子用電子輸送層との接触性が良いことが好ましい。陰極は、有機発光素子用電子輸送層との仕事関数の差が小さく、化学的に安定であることも好ましい。このような材料としては、特に限定されないが、金、銀、銅、アルミニウム、白金、ロジウム、マグネシウム、インジウム等の金属薄膜、炭素、カーボンブラック、導電性高分子、導電性の金属酸化物(インジウム-スズ複合酸化物、酸化錫にフッ素をドープしたもの等)などの有機導電体などが挙げられる。また、陰極の平均厚みもまた、特に限定されないが、約10~1000nmであるのが好ましい。また、陰極の表面抵抗は、特に限定されないが、低いのが好ましく、具体的には、陰極の表面抵抗の範囲は、好ましくは80Ω/□以下であり、より好ましくは20Ω/□以下である。なお、陰極の表面抵抗の下限は、可能な限り低いことが好ましいため、特に限定されないが、0.1Ω/□以上であればよい。
1.成膜装置
図1を用いて、本実施例で用いたミストCVD装置1を説明する。ミストCVD装置1は、キャリアガスを供給するキャリアガス源2と、キャリアガス源2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3と、原料溶液4aが収容されるミスト発生源4と、水5aが入れられる容器5と、容器5の底面に取り付けられた超音波振動子6と、成膜室7と、ミスト発生源4から成膜室7までをつなぐ供給管9と、成膜室7内に設置されたホットプレート8とを備えている。なお、ホットプレート8上には、基板10が設置されている。
メチルアンモニウム鉛ヨウ化物をγ-ブチロラクトンに混合し、これを原料溶液とした。なお、溶液中のメチルアンモニウム鉛ヨウ化物のモル濃度は0.011mol/Lである。
上記2.で得られた原料溶液4aをミスト発生源4内に収容した。次に、基板10として、15mm角のガラス/ITO基板をホットプレート8上に設置し、ホットプレート8を作動させて成膜室7内の温度を120℃にまで昇温させた。次に、流量調節弁3a、3bを開いて、キャリアガス源であるキャリアガス供給手段2a、2bからキャリアガスを成膜室7内に供給し、成膜室7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4L/分に調節した。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6を2.4MHzで振動させ、その振動を、水5aを通じて原料溶液4aに伝播させることによって、原料溶液4aを霧化させてミスト4bを生成させた。このミスト4bが、キャリアガスによって、供給管9内を通って、成膜室7内に導入され、大気圧下、120℃にて、成膜室7内でミストが熱反応して、基板10上に膜が形成された。なお、膜厚は1μmであり、成膜時間は20分間であった。
XRD回折装置を用いて、ペロブスカイト膜の同定を行った。結果を図2に示す。また、得られた膜につき、SEM観察を行った。SEM像を図3に示す。
成膜温度を130℃にしたこと以外は、実施例1と同様にしてペロブスカイト膜を製造した。実施例1と同様にして、X線回折装置を用いて、結晶膜の同定を行ったところ、得られた膜は、ペロブスカイト膜であった。なお、XRDチャートを図4に示す。
成膜温度を125℃にしたこと以外は、実施例1と同様にしてペロブスカイト膜を製造した。実施例1と同様にして、X線回折装置を用いて、結晶膜の同定を行ったところ、得られた膜は、ペロブスカイト膜であった。なお、XRDチャートを図5に示す。
成膜温度を110℃にしたこと以外は、実施例1と同様にしてペロブスカイト膜を製造した。実施例1と同様にして、X線回折装置を用いて、結晶膜の同定を行ったところ、得られた膜は、ペロブスカイト膜であった。
窒素に代えてアルゴンをキャリアガスとして用いたこと以外は、実施例1と同様にしてペロブスカイト膜を製造した。実施例1と同様にして、X線回折装置を用いて、結晶膜の同定を行ったところ、得られた膜は、ペロブスカイト膜であった。
γ-ブチロラクトンの代わりに、γ-ブチロラクタムを用いたこと以外は、実施例1と同様にして成膜した。実施例1と同様にして、X線回折装置を用いて、結晶膜の同定を行ったところ、得られた膜は、ペロブスカイト膜であった。
γ-ブチロラクトンの代わりに、水を用いたこと以外は、実施例1と同様にして成膜した。しかしながら、基板上に膜がつかなかった。
γ-ブチロラクトンの代わりに、メタノールと水との混合溶媒(メタノール:水=95:5)を用いたこと以外は、実施例1と同様にして成膜した。しかしながら、基板上に膜がつかなかった。
成膜温度を115℃にしたこと以外は、実施例1と同様にしてペロブスカイト膜を製造した。実施例1と同様にして、X線回折装置を用いて、結晶膜の同定を行ったところ、得られた膜は、ペロブスカイト膜であった。なお、XRDチャートを図6に示す。
1.成膜装置
図7を用いて、実施例8で用いた成膜装置19を説明する。図7の成膜装置19は、キャリアガスを供給するキャリアガス源2と、キャリアガス源2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3と、原料溶液4aが収容されるミスト発生源4と、水5aが入れられる容器5と、容器5の底面に取り付けられた超音波振動子6と、ホットプレート8と、ホットプレート8上に設置された基板10と、ミスト発生源4から基板10近傍までをつなぐ供給管9とを備えている。
α―NPDをγ―ブチロラクトンに混合し、これを原料溶液とした。なお、溶液中のα―NPDのモル濃度は0.0020mol/Lである。
上記2.で得られた原料溶液4aをミスト発生源4内に収容した。次に、基板10として、15mm角のガラス/ITO基板をホットプレート8上に設置し、ホットプレート8を作動させて基板10の温度を180℃にまで昇温させた。次に、流量調節弁3を開いて、キャリアガス源であるキャリアガス供給手段2から供給されるキャリアガスの流量を4L/分に調節した。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6を2.4MHzで振動させ、その振動を、水5aを通じて原料溶液4aに伝播させることによって、原料溶液4aを霧化させてミスト4bを生成させた。このミスト4bが、キャリアガスによって、供給管9内を通って、基板10へと搬送され、大気圧下、180℃にて、基板10近傍でミストが熱反応して、基板10上に有機発光素子用正孔輸送層が形成された。なお、得られた有機発光素子用正孔輸送層の膜厚は約50nmであり、成膜時間は、10分間であった。また、得られた基板付きの有機発光素子用正孔輸送層の蛍光スペクトルを、励起波長300nmにおいて測定した。図8にその結果を示す。図8からわかるように、得られた基板付きの有機発光素子用正孔輸送層は、波長430~450nmに発光ピークを有していた。
成膜温度を140℃にしたこと以外は、実施例8と同様にして、基板付きの有機発光素子用正孔輸送層を得た。また、実施例8と同様にして、得られた基板付きの有機発光素子用正孔輸送層の蛍光スペクトルを測定した。図8にその結果を示す。図8からわかるように、得られた基板付きの有機発光素子用正孔輸送層は、波長430~450nmに発光ピークを有していた。また、実施例8で得られた基板付きの有機発光素子用正孔輸送層よりも蛍光強度が高く、より良好な発光特性を有していた。
α―NPDの代わりにAlq3を用いて、溶液中のAlq3の濃度を0.0025mol/Lとして混合溶液を作製し、これを原料溶液としたこと、基板として、実施例8で得られた積層体を用いたこと以外は、実施例8と同様に、実施例8で形成した有機発光素子用正孔輸送層上に発光層を形成した。また、得られた発光層の膜厚は約50nmであり、成膜時間は10分間であった。また、実施例8と同様にして、得られた基板付きの発光層の蛍光スペクトルを、励起波長300nmにおいて測定した。図9にその結果を示す。図9からわかるように、得られた基板付きの発光層は、波長500~520nmに発光ピークを有していた。
成膜温度を140℃にしたこと、基板として、実施例9で得られた積層体を用いたこと以外は、実施例10と同様にして、基板付きの発光層を得た。また、実施例8と同様にして、得られた基板付きの発光層の蛍光スペクトルを測定した。図9にその結果を示す。図9からわかるように、得られた基板付きの発光層は、波長500~520nmに発光ピークを有していた。また、実施例10で得られた基板付きの発光層よりも発光強度が高く、より良好な発光特性を有していた。
実施例10で得られた積層体上に、真空蒸着法を用いて、陰極としてアルミニウムを形成し、有機発光素子を製造した。
2 キャリアガス源
3 流量調節弁
4 ミスト発生源
4a 原料溶液
4b ミスト
5 容器
5a 水
6 超音波振動子
7 成膜室
8 ホットプレート
9 供給管
10 基板
19 成膜装置
Claims (13)
- ペロブスカイト構造体の前駆体である有機化合物原料と、該原料を溶解または分散させる環状エステルを有する溶媒とを含む原料溶液を霧化または液滴化し、得られたミストまたは液滴をキャリアガスで基体まで搬送し、ついで前記ミストまたは液滴を反応させて前記基体上に成膜することを特徴とする成膜方法。
- ペロブスカイト構造体の前駆体である有機化合物原料と、該原料を溶解または分散させる環状アミドを有する溶媒とを含む原料溶液を霧化または液滴化し、得られたミストまたは液滴をキャリアガスで基体まで搬送し、ついで前記ミストまたは液滴を反応させて前記基体上に成膜することを特徴とする成膜方法。
- 前記原料溶液が有機金属ハロゲン化物を含む請求項1または2に記載の成膜方法。
- 前記原料溶液がアンモニウム化合物を含む請求項1~3のいずれかに記載の成膜方法。
- 前記反応が熱反応であり、前記熱反応を、250℃以下の温度で行う請求項1~4のいずれかに記載の成膜方法。
- 前記基体が、ガラス基板である請求項1~5のいずれかに記載の成膜方法。
- 前記基体が、スズドープ酸化インジウム膜またはフッ素ドープ酸化インジウム膜を含む請求項1~6のいずれかに記載の成膜方法。
- 前記基体が、チタニア膜を含む請求項1~7のいずれかに記載の成膜方法。
- 前記原料溶液がアミン誘導体を含む請求項1に記載の成膜方法。
- 前記原料溶液が金属錯体を含む請求項1に記載の成膜方法。
- 基体上に直接または他の層を介して、少なくとも正孔輸送層及び/又は発光層を積層して有機発光素子を製造する方法において、前記正孔輸送層及び/又は発光層の積層を、前記正孔輸送層及び/又は前記発光層の前駆体である有機化合物原料と、該原料を溶解または分散させる環状エステルを有する溶媒とを含む原料溶液を霧化又は液滴化し、得られたミスト又は液滴をキャリアガスで基体上まで搬送し、前記基体上で前記ミスト又は液滴を反応させて、前記基体上に成膜することにより行うことを特徴とする有機発光素子の製造方法。
- 前記原料溶液がアミン誘導体を含む請求項11に記載の有機発光素子の製造方法。
- 前記原料溶液が金属錯体を含む請求項11に記載の有機発光素子の製造方法。
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WO2016200897A1 (en) * | 2015-06-08 | 2016-12-15 | The Florida State University Research Foundation, Inc. | Single-layer light-emitting diodes using organometallic halide perovskite/ionic-conducting polymer composite |
JP7391296B2 (ja) * | 2017-10-07 | 2023-12-05 | 株式会社Flosfia | 成膜方法 |
CN109755394B (zh) * | 2017-11-08 | 2021-07-16 | 中国科学院化学研究所 | 一种应用风刀涂布制备钙钛矿太阳能电池的方法 |
JP7165464B2 (ja) * | 2017-12-29 | 2022-11-04 | 株式会社Flosfia | 有機膜の成膜方法 |
CN108594501B (zh) * | 2018-02-26 | 2021-04-27 | 京东方科技集团股份有限公司 | 一种液晶显示面板及其制作方法 |
JP7060206B2 (ja) * | 2018-02-28 | 2022-04-26 | 株式会社Screenホールディングス | 基板処理装置および基板処理方法 |
JP7148766B2 (ja) * | 2018-04-27 | 2022-10-06 | 株式会社Flosfia | カーボンナノチューブ含有膜の成膜方法 |
JP7113425B2 (ja) * | 2018-04-27 | 2022-08-05 | 株式会社Flosfia | 蛍光波長の調整方法 |
WO2020003603A1 (ja) * | 2018-06-26 | 2020-01-02 | 国立大学法人京都大学 | 放射線検出器、及び放射線検出器の製造方法 |
CN109234680B (zh) * | 2018-11-06 | 2019-10-15 | 南京大学 | 一种超薄层状有机分子铁电薄膜的制备方法以及该铁电薄膜的应用 |
CN111384306B (zh) * | 2018-12-29 | 2021-10-29 | Tcl科技集团股份有限公司 | 量子点发光二极管的制备方法 |
US11519086B2 (en) | 2019-05-02 | 2022-12-06 | King Fahd University Of Petroleum And Minerals | Fabrication of photoactive CaTiO3—TiO2 composite thin film electrodes via single step AACVD |
CN111463350A (zh) * | 2020-04-20 | 2020-07-28 | 浙江大学 | 基于钙钛矿量子点的x射线探测器及其制备方法 |
CN112939483B (zh) * | 2021-01-17 | 2022-07-01 | 桂林理工大学 | Ho掺杂Bi2S3纳米薄膜的制备方法 |
CN116288256B (zh) * | 2023-05-17 | 2023-11-07 | 青禾晶元(天津)半导体材料有限公司 | 一种雾化气相沉积装置和雾化气相沉积方法 |
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