JP2009105044A - 分散型無機電界発光素子およびその製造方法 - Google Patents
分散型無機電界発光素子およびその製造方法 Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 39
- 239000006185 dispersion Substances 0.000 title claims abstract description 12
- 238000005401 electroluminescence Methods 0.000 title claims abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000012702 metal oxide precursor Substances 0.000 claims abstract description 31
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 30
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- -1 BaTiO 3 Inorganic materials 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- 230000005684 electric field Effects 0.000 claims description 4
- 238000000034 method Methods 0.000 description 14
- 239000002245 particle Substances 0.000 description 10
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- 229910052801 chlorine Inorganic materials 0.000 description 7
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- 239000000243 solution Substances 0.000 description 6
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- 238000004544 sputter deposition Methods 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000004373 Pullulan Substances 0.000 description 3
- 229920001218 Pullulan Polymers 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 229920001940 conductive polymer Polymers 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 235000019423 pullulan Nutrition 0.000 description 3
- VUTWBSJIBAPTLY-UHFFFAOYSA-N 1-tert-butyl-2-(2-phenylethynyl)benzene Chemical group C(C)(C)(C)C1=C(C=CC=C1)C#CC1=CC=CC=C1 VUTWBSJIBAPTLY-UHFFFAOYSA-N 0.000 description 2
- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
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- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 2
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 2
- 229920001197 polyacetylene Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 229960002796 polystyrene sulfonate Drugs 0.000 description 2
- 239000011970 polystyrene sulfonate Substances 0.000 description 2
- 239000005361 soda-lime glass Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910052950 sphalerite Inorganic materials 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- RGSINQHSYQBZBN-UHFFFAOYSA-N 1-(2-phenylethynyl)-2-(trifluoromethyl)benzene Chemical group FC(F)(F)C1=CC=CC=C1C#CC1=CC=CC=C1 RGSINQHSYQBZBN-UHFFFAOYSA-N 0.000 description 1
- KXJGSNRAQWDDJT-UHFFFAOYSA-N 1-acetyl-5-bromo-2h-indol-3-one Chemical compound BrC1=CC=C2N(C(=O)C)CC(=O)C2=C1 KXJGSNRAQWDDJT-UHFFFAOYSA-N 0.000 description 1
- IOPDYTCCKSYLJG-UHFFFAOYSA-N 3,3,3-trifluoroprop-1-ynylbenzene Chemical group FC(F)(F)C#CC1=CC=CC=C1 IOPDYTCCKSYLJG-UHFFFAOYSA-N 0.000 description 1
- FASNPPWZLHQZAJ-UHFFFAOYSA-N 3,3-dimethylbut-1-ynylbenzene Chemical group CC(C)(C)C#CC1=CC=CC=C1 FASNPPWZLHQZAJ-UHFFFAOYSA-N 0.000 description 1
- CKJRIVCXNKBSQQ-UHFFFAOYSA-N 9h-carbazole;2-phenylethynylbenzene Chemical group C1=CC=C2C3=CC=CC=C3NC2=C1.C1=CC=CC=C1C#CC1=CC=CC=C1 CKJRIVCXNKBSQQ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 101100476480 Mus musculus S100a8 gene Proteins 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910004116 SrO 2 Inorganic materials 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- INNSZZHSFSFSGS-UHFFFAOYSA-N acetic acid;titanium Chemical compound [Ti].CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O INNSZZHSFSFSGS-UHFFFAOYSA-N 0.000 description 1
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229940009827 aluminum acetate Drugs 0.000 description 1
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- WBCLXFIDEDJGCC-UHFFFAOYSA-N hexafluoro-2-butyne Chemical group FC(F)(F)C#CC(F)(F)F WBCLXFIDEDJGCC-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000553 poly(phenylenevinylene) Polymers 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000323 polyazulene Polymers 0.000 description 1
- 229920000015 polydiacetylene Polymers 0.000 description 1
- 229920000414 polyfuran Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- UZIXCCMXZQWTPB-UHFFFAOYSA-N trimethyl(2-phenylethynyl)silane Chemical group C[Si](C)(C)C#CC1=CC=CC=C1 UZIXCCMXZQWTPB-UHFFFAOYSA-N 0.000 description 1
- CCGULKCUSSEENW-UHFFFAOYSA-N trimethyl-[2-(2-phenylethynyl)phenyl]silane Chemical group C[Si](C)(C)C1=CC=CC=C1C#CC1=CC=CC=C1 CCGULKCUSSEENW-UHFFFAOYSA-N 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
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- C09K11/615—Halogenides
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- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
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- H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
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- H05B33/00—Electroluminescent light sources
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
【解決手段】本発明の分散型無機電界発光素子は、基板と、基板上に形成されてなる透明電極と、上部電極とを有する分散型無機電界発光素子において、蛍光体表面の少なくとも一部に金属酸化物がコーティングされてなる発光体を含む電界発光層が、透明電極と上部電極との間に積層されてなる。また、本発明の分散型無機電界発光素子の製造方法は、(a)金属酸化物前駆体溶液と蛍光体とを混合することによって、蛍光体表面の少なくとも一部に金属酸化物前駆体をコーティングする段階;(b)金属酸化物前駆体がコーティングされた蛍光体を乾燥することによって、発光体を形成する段階;および(c)発光体を含む電界発光層を、透明電極と上部電極との間に形成する段階を含む。
【選択図】図2
Description
Yoshimasa A、Ono、Electroluminescent Display、1995
[実施例1]
(発光体の調製)
SOG(spin on glass、512B、ハネウェル社製)4.1gを超音波洗浄器(SH−2100、セハン・ウルトラソニック株式会社製)に準備した後、ZnS:Cu,Cl蛍光体2gを添加しながら5時間超音波をかけてSOGを蛍光体表面にコーティングした。この後、混合溶液を、濾紙を用いて濾過して溶媒を除去し、さらに、常温で乾燥することによって発光体を得た。得られた発光体の透過型電子顕微鏡(TEM)写真を図3に示す。図3を参照すると、蛍光体表面に金属酸化物としてのSiO2が100nmの厚さで均一にコーティングされたことが確認できる。
1.8mmの厚さのガラス基板(ソーダ石灰ガラス)上にインジウムスズ酸化物(ITO)をスパッタリング法で塗布して1500Åの厚さの透明電極を形成した。その後、上記で製造した発光体30gとシアノエチルプルラン樹脂12gとを攪拌機を用いて混合した後、この混合物をスピンコーティング法(1000rpm)で透明電極上に25μmの厚さで塗布して130℃の電気オーブンで30分間乾燥し、電界発光層を形成した。次に、アルミニウム(Al)をスパッタリング法で1500Åの厚さで塗布した後、130℃の電気オーブンで30分間乾燥して上部電極を形成することによって分散型無機EL素子を製造した。
実施例1の(発光体の調製)の操作を3回繰り返すことによって、ZnS:Cu,Cl蛍光体2gに対してSOG4.1gを3回(計12.3g)コーティングした。これ以外は実施例1と同様の方法で分散型無機EL素子を製造した。
実施例1の(発光体の調製)の操作を5回繰り返すことによって、ZnS:Cu,Cl蛍光体2gに対してSOG4.1gを5回(計20.5g)コーティングした。これ以外は実施例1と同様の方法で分散型無機EL素子を製造した。
SOGに代えて、TEOS(tetraethyl orthosilicate、シグマ・アルドリッチ株式会社製)を用いたことを除いては、実施例1と同様の方法で分散型無機EL素子を製造した。
1.8mmの厚さのガラス基板(ソーダ石灰ガラス)上にITOをスパッタリング法で塗布して1500Åの厚さの透明電極を形成した。ZnS:Cu,Cl蛍光体30gをプリンティング法で250μmの厚さの発光層を形成し、SiO2をプラズマ化学気相蒸着法(PECVD)で3000Åの厚さで誘電層を形成した。さらに、アルミニウム(Al)をスパッタリング法で1500Åの厚さで塗布した後、130℃で30分間乾燥して上部電極を形成することによって分散型無機EL素子を製造した。
実施例1〜4および比較例1で作製した分散型無機EL素子の輝度を測定した。分散型無機EL素子の上下部電極を連結して印加される電圧および電流は、オシロスコープ(infiniium oscilloscope、アジレント・テクノロジー株式会社製)で測定し、輝度は色彩輝度計(BM−7、株式会社トプコン製)で測定した。なお、測定時の周波数は400Hzであった。駆動電圧に対する輝度を図4に示す。
2 透明電極、
3a 第1誘電層、
3b 第2誘電層、
4 発光層、
5 金属酸化物、
6 上部電極、
7 蛍光体、
8 発光体、
9 電界発光層。
Claims (12)
- 基板と、前記基板上に形成されてなる透明電極と、上部電極とを有する分散型無機電界発光素子において、
蛍光体表面の少なくとも一部に金属酸化物がコーティングされてなる発光体を含む電界発光層が、前記透明電極と前記上部電極との間に積層されてなることを特徴とする分散型無機電界発光素子。 - 前記金属酸化物の抵抗率が、105Ω・cm以上であることを特徴とする、請求項1に記載の分散型無機電界発光素子。
- 前記蛍光体にコーティングされた前記金属酸化物の厚さが、10〜500nmであることを特徴とする、請求項1または2に記載の分散型無機電界発光素子。
- 前記金属酸化物が、SiO2、Al2O3、BaTiO3、およびTiO2からなる群から選択される少なくとも1種を含むことを特徴とする、請求項2または3に記載の分散型無機電界発光素子。
- 前記上部電極と前記電界発光層との間に誘電層をさらに含む、請求項1〜4のいずれか1項に記載の分散型無機電界発光素子。
- 前記透明電極と前記電界発光層との間に誘電層をさらに含む、請求項1〜5のいずれか1項に記載の分散型無機電界発光素子。
- (a)金属酸化物前駆体溶液と蛍光体とを混合することによって、蛍光体表面の少なくとも一部に金属酸化物前駆体をコーティングする段階;
(b)前記金属酸化物前駆体がコーティングされた蛍光体を乾燥することによって、発光体を形成する段階;および
(c)前記発光体を含む電界発光層を、透明電極と上部電極との間に形成する段階を含む分散型無機電界発光素子の製造方法。 - 前記コーティングは、超音波装置、機械式攪拌機、磁気攪拌機、およびホモジナイザーからなる群から選択される少なくとも1種を用いて行われることを特徴とする、請求項7に記載の分散型無機電界発光素子の製造方法。
- 透明電極と、上部電極とを有する分散型無機電界発光素子の製造方法において、
金属酸化物前駆体溶液と蛍光体とを混合した後、前記蛍光体に金属酸化物前駆体を有機バインダーと混合されたペースト組成物の形態で前記透明電極にコーティングする段階と、
前記金属酸化物前駆体がコーティングされた蛍光体を乾燥して有機バインダーを除去し、前記透明電極および前記上部電極間に発光層と誘電層とを一体化して形成する段階とを含み、
前記金属酸化物前駆体が105〜106Ω・cmの金属酸化物の固有抵抗を表すことを特徴とする、分散型無機電界発光素子の製造方法。 - 前記コーティングは、超音波装置、機械式攪拌機、磁気攪拌機、およびホモジナイザーからなる群から選択される少なくとも1種を用いて行われることを特徴とする、請求項9に記載の分散型無機電界発光素子の製造方法。
- 前記蛍光体にコーティングされた前記金属酸化物の厚さが、10〜500nmであることを特徴とする、請求項9または10に記載の分散型無機電界発光素子の製造方法。
- 前記金属酸化物が、SiO2、Al2O3、BaTiO3、およびTiO2からなる群から選択される少なくとも1種を含むことを特徴とする、請求項9〜11のいずれか1項に記載の分散型無機電界発光素子の製造方法。
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