CN117082951A - 小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法 - Google Patents
小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法 Download PDFInfo
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- CN117082951A CN117082951A CN202311122199.0A CN202311122199A CN117082951A CN 117082951 A CN117082951 A CN 117082951A CN 202311122199 A CN202311122199 A CN 202311122199A CN 117082951 A CN117082951 A CN 117082951A
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- Prior art keywords
- quantum dot
- light emitting
- emitting diode
- nickel oxide
- nickel
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 83
- 239000002096 quantum dot Substances 0.000 title claims abstract description 62
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 44
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 230000005540 biological transmission Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 150000002815 nickel Chemical class 0.000 claims abstract description 5
- 239000013110 organic ligand Substances 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 239000010410 layer Substances 0.000 claims description 74
- 239000000243 solution Substances 0.000 claims description 30
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000003446 ligand Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
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- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000004528 spin coating Methods 0.000 claims description 9
- -1 thiobetaine Chemical compound 0.000 claims description 9
- JJMDCOVWQOJGCB-UHFFFAOYSA-N 5-aminopentanoic acid Chemical compound [NH3+]CCCCC([O-])=O JJMDCOVWQOJGCB-UHFFFAOYSA-N 0.000 claims description 8
- 229920002873 Polyethylenimine Polymers 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
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- 238000000137 annealing Methods 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 229920003227 poly(N-vinyl carbazole) Polymers 0.000 claims description 6
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
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- 238000010276 construction Methods 0.000 claims description 5
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- GQEZCXVZFLOKMC-UHFFFAOYSA-N 1-hexadecene Chemical compound CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 239000012296 anti-solvent Substances 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 4
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- 230000035484 reaction time Effects 0.000 claims description 4
- 150000003376 silicon Chemical class 0.000 claims description 4
- 239000011550 stock solution Substances 0.000 claims description 4
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 claims description 4
- KORKIRUGUNPQML-UHFFFAOYSA-N 2-(2-aminobenzoyl)benzoic acid Chemical compound NC1=CC=CC=C1C(=O)C1=CC=CC=C1C(O)=O KORKIRUGUNPQML-UHFFFAOYSA-N 0.000 claims description 3
- JXSRRBVHLUJJFC-UHFFFAOYSA-N 7-amino-2-methylsulfanyl-[1,2,4]triazolo[1,5-a]pyrimidine-6-carbonitrile Chemical compound N1=CC(C#N)=C(N)N2N=C(SC)N=C21 JXSRRBVHLUJJFC-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000002346 layers by function Substances 0.000 claims description 3
- JMWUYEFBFUCSAK-UHFFFAOYSA-L nickel(2+);octadecanoate Chemical compound [Ni+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O JMWUYEFBFUCSAK-UHFFFAOYSA-L 0.000 claims description 3
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 3
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- PSBDWGZCVUAZQS-UHFFFAOYSA-N (dimethylsulfonio)acetate Chemical compound C[S+](C)CC([O-])=O PSBDWGZCVUAZQS-UHFFFAOYSA-N 0.000 claims description 2
- XFXSJOHJDZJFCP-UHFFFAOYSA-N 2-(4-methylsulfonylphenyl)ethanamine Chemical compound CS(=O)(=O)C1=CC=C(CCN)C=C1 XFXSJOHJDZJFCP-UHFFFAOYSA-N 0.000 claims description 2
- GEQBRULPNIVQPP-UHFFFAOYSA-N 2-[3,5-bis(1-phenylbenzimidazol-2-yl)phenyl]-1-phenylbenzimidazole Chemical group C1=CC=CC=C1N1C2=CC=CC=C2N=C1C1=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=C1 GEQBRULPNIVQPP-UHFFFAOYSA-N 0.000 claims description 2
- LGDCSNDMFFFSHY-UHFFFAOYSA-N 4-butyl-n,n-diphenylaniline Chemical compound C1=CC(CCCC)=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 LGDCSNDMFFFSHY-UHFFFAOYSA-N 0.000 claims 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 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 241000208818 Helianthus Species 0.000 claims description 2
- 235000003222 Helianthus annuus Nutrition 0.000 claims description 2
- ZDXPYRJPNDTMRX-VKHMYHEASA-N L-glutamine Chemical compound OC(=O)[C@@H](N)CCC(N)=O ZDXPYRJPNDTMRX-VKHMYHEASA-N 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- 239000005662 Paraffin oil Substances 0.000 claims description 2
- 229920001167 Poly(triaryl amine) Polymers 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 2
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- 230000015572 biosynthetic process Effects 0.000 claims description 2
- ODWXUNBKCRECNW-UHFFFAOYSA-M bromocopper(1+) Chemical compound Br[Cu+] ODWXUNBKCRECNW-UHFFFAOYSA-M 0.000 claims description 2
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 2
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
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- WGEFECGEFUFIQW-UHFFFAOYSA-L calcium dibromide Chemical compound [Ca+2].[Br-].[Br-] WGEFECGEFUFIQW-UHFFFAOYSA-L 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
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- 229940116318 copper carbonate Drugs 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 claims description 2
- GBRBMTNGQBKBQE-UHFFFAOYSA-L copper;diiodide Chemical compound I[Cu]I GBRBMTNGQBKBQE-UHFFFAOYSA-L 0.000 claims description 2
- RJYMRRJVDRJMJW-UHFFFAOYSA-L dibromomanganese Chemical compound Br[Mn]Br RJYMRRJVDRJMJW-UHFFFAOYSA-L 0.000 claims description 2
- XRWMGCFJVKDVMD-UHFFFAOYSA-M didodecyl(dimethyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCC XRWMGCFJVKDVMD-UHFFFAOYSA-M 0.000 claims description 2
- GPAYUJZHTULNBE-UHFFFAOYSA-N diphenylphosphine Chemical compound C=1C=CC=CC=1PC1=CC=CC=C1 GPAYUJZHTULNBE-UHFFFAOYSA-N 0.000 claims description 2
- 238000001548 drop coating Methods 0.000 claims description 2
- RAQDACVRFCEPDA-UHFFFAOYSA-L ferrous carbonate Chemical compound [Fe+2].[O-]C([O-])=O RAQDACVRFCEPDA-UHFFFAOYSA-L 0.000 claims description 2
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- GYCHYNMREWYSKH-UHFFFAOYSA-L iron(ii) bromide Chemical compound [Fe+2].[Br-].[Br-] GYCHYNMREWYSKH-UHFFFAOYSA-L 0.000 claims description 2
- BQZGVMWPHXIKEQ-UHFFFAOYSA-L iron(ii) iodide Chemical compound [Fe+2].[I-].[I-] BQZGVMWPHXIKEQ-UHFFFAOYSA-L 0.000 claims description 2
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- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 2
- OTCKOJUMXQWKQG-UHFFFAOYSA-L magnesium bromide Chemical compound [Mg+2].[Br-].[Br-] OTCKOJUMXQWKQG-UHFFFAOYSA-L 0.000 claims description 2
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- JOCJYBPHESYFOK-UHFFFAOYSA-K nickel(3+);phosphate Chemical compound [Ni+3].[O-]P([O-])([O-])=O JOCJYBPHESYFOK-UHFFFAOYSA-K 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 claims description 2
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Abstract
本发明涉及量子点显示照明技术领域,且公开了小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,S1将镍盐、掺杂盐、有机配体和溶剂相混合,在一定温度和真空度下,以一定的速度搅拌一定的时间,待溶液变成黄绿色时,通入惰性气体,升高到一定的温度,反应一定的时间,获得灰黑色的氧化镍纳米颗粒的原液。该溶液法制备出的NiO纳米晶颗粒尺寸在3‑12nm,具有超小的尺寸,且制备方法简便易行、成本低廉、重复性高、结晶性好、无杂质峰,不需要高温反应,反应体系稳定,且产物可以很好分散在非极性溶剂中,同时具有很好的胶体稳定性,所形成的薄膜致密平坦、起伏度较小,具有高的空穴迁移率,可以应用于多种高性能的QLEDs的传输层。
Description
技术领域
本发明涉及量子点显示照明技术领域,具体为小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法。
背景技术
在学术和工业领域中,量子点发光二极管(QLEDs)被认为是最有发展潜力的显示器件,由于QLEDs可以通过调节荧光量子点的尺寸而改变电致发光峰的位置,同时拥有较低的制作成本,更宽的色域和更纯的色度,因此在显示和照明领域具有很大应用前景,在传统的QLEDs器件中,聚磺酸掺杂的聚噻吩(PEDOT:PSS)作为QLEDs的空穴传输层,但PEDOT:PSS是由高分子聚合物配成的水溶液,有较强的酸性,可以解离ITO中In3+离子,导致In3+离子渗透到PEDOT:PSS中,从而降低PEDOT:PSS空穴注入性能,同时当QLED器件处于空气中时,PEDOT:PSS就会吸收空气中的水分子和氧分子,增大薄层电阻,导致器件性能的降低,而无机金属氧化物材料作为空穴注入层,不受水氧的影响,同时空穴迁移率大、透光滤高、而且还可以通过掺杂的方法进行带隙和性能的调节。
一方面,现有的技术合成的NiO纳米颗粒的尺寸较大,工艺复杂、大多数为百纳米级甚至为微米级的颗粒,无固定形貌,均匀性较差,这种NiO颗粒导致制备的QLEDs传输层材料的起伏度,覆盖率,损害了QLEDs器件的发光性能;另一方面,传统的NiO材料制备采用高温煅烧法,能耗大,成本高,获得的纳米颗粒只能分散在乙醇、水等极性溶剂中,无法在极性溶剂敏感的基底材料上进行旋涂,且纳米颗粒分散性差,成膜覆盖率差,成膜性低,而我们报到的方法成本低,重复性高,且制备的NiO材料能分散在甲苯、正己烷等非极性溶剂中,可以在极性溶剂敏感的基底材料上进行旋涂,因此具有一定的应用潜力。
综上所述,传统的QLEDs器件采用有机物PEDOT:PSS作为空穴注入层,当器件处于空气中时,极易吸收空气中的水氧,从而导致QLEDs器件的性能降低,影响其应用,为了克服钙钛矿量子点荧光稳定性弱的问题,本发明提出了一种简单的、溶液加工的于氧化镍纳米颗粒空穴传输层的量子点发光二极管器件及其制备方法,显著提高了QLEDs器件的工作稳定性。
发明内容
为实现上述目的,本发明提供如下技术方案:小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其制备方法包括以下步骤:
S1:将镍盐、掺杂盐、有机配体和溶剂相混合,在一定温度和真空度下,以一定的速度搅拌一定的时间,待溶液变成黄绿色时,通入惰性气体,升高到一定的温度,反应一定的时间,获得灰黑色的氧化镍纳米颗粒的原液;
S2:将氧化镍纳米颗粒进行配体交换反应,将一定浓度的镍纳米颗粒加入一定量的交换配体,在一定的温度下,经过一定时间的搅拌,获得功能性的氧化镍纳米颗粒;
S3:随后将反溶剂加至功能化氧化镍纳米晶的原溶液中,以一定的速度离心一定的时间,随后将获得的沉淀内加入溶剂再分散,重复离心步骤多次,去除氧化镍纳米晶在合成过程中产生的反应废料,获得干净氧化镍纳米颗粒;
S4:构筑QLED发光器件,QLED器件包括:透明导电基底、氧化镍纳米颗粒传输层、界面修饰层、量子点发光层、顶部电荷传输层、界面修饰层和电极;其中,在透明导电基底上形成氧化镍纳米颗粒空穴传输层,量子点发光层通过成膜工艺在氧化镍纳米颗粒传输层上形成量子点发光层,在量子点发光薄膜上形成顶部电荷传输层,在顶部电荷传输层上制备电极,在量子点发光层的上界面或下界面添加界面修饰层,提升器件的性能,随后对构筑器件进行封装,封装材料为紫外固化胶以及超薄的载玻片。
优选的,所述步骤S1中镍盐为硝酸镍、磷酸镍、硫酸镍、碳酸镍、硬脂酸镍、溴化镍、氯化镍、碘化镍中的一种或多种,二价金属盐为硝酸铁、硝酸镁、硝酸铜、硝酸锶、碳酸铁、碳酸铜、碳酸锶、硬脂酸铜、溴化铁、溴化锰、溴化镁、溴化铜、溴化锌、溴化锶、溴化钙、碘化铁、碘化铜、碘化锶中中的一种或多种,有机配体可以是但不局限于辛酸、油酸、硬脂酸,溶剂可以是但不局限于石蜡油、十六烯、十八醇和十八烯。
优选的,所述步骤S1中真空下的反应的温度为40~100℃,反应时间为10~60min,真空度为0.01~0.5Torr,通入惰性气体后的反应的时间2~5小时,反应的温度为100~500℃。
优选的,所述步骤S2中交换配体为多齿型的氨基配体、羧基配体、硫基配体、磺基配体、磷基配体中的一种或多种,例如三辛基膦、三丁基膦、二苯基膦、双十二烷基二甲基溴化铵、磺基甜菜碱、磷胆碱、氨基酸、5-氨基水杨酸、5氨基戊酸、2-氨基二苯甲酮-2'-羧酸、硫代甜菜碱、谷氨酰胺、2-(4-(甲基磺酰基)苯基)乙胺、2,2'-亚氨基二苯甲酸等。
优选的,所述步骤S2中对于10mL的NiO纳米颗粒,功能交换配体的量为0.01~0.5mL。
优选的,所述步骤S3中离心剂和与溶剂的体积比为0.2~3:1,离心速度为3000~5000rpm,离心时间为3~30min,NiO纳米颗粒的浓度为5~50mg/mL,氧化镍纳米颗粒的粒径尺寸为3~12nm。
优选的,所述步骤S3中溶剂为甲苯、正己烷、环己烷、苯、氯仿、葵烷、氯苯、辛胺、辛烷中的一种,反溶剂为乙醇、甲醇、丁醇、乙酸乙酯、丙酮中的一种。
优选的,所述步骤S4中NiO纳米颗粒墨水的浓度为3-50mg/mL,薄膜的厚度为6~50nm,NiO纳米颗粒薄膜的退火温度为60~500℃,退火时间为10~60分钟;量子点发光层为钙钛矿量子点ABX3(A=FA、MA、Cs、Rb、K;B=Pb、Sn、Bi、Mn;X=Cl、Br、I)、II-IV和III-V族量子点(ZnS、CdSe、InP、CdSe@ZnS)、碳点、石墨烯量子点、硅量子点;电子传输层分为有机电子传输层和无机电子传输层两种,有机电子传输层为1,3,5-三(1-苯基-1H-苯并咪唑-2-基)苯(TPBi)、富勒烯及其衍生物(C60、C70、PC61BM、PC71BM),无机电子传输层为氧化锡(SnO2)、氧化锌(ZnO)或氧化钛(TiO2)。
优选的,所述步骤S4中除金属电极外,各个功能层的成膜工艺为旋涂、刮涂、卷对卷、滴涂或丝网印刷中一种或多种,所述电极为镍、钛、钙、铝、铜、银、金、碳和石墨烯电极中的一种。
优选的,所述步骤S4中发光层下面的界面修饰层为有机空穴传输层为聚(3-己基噻吩-2,5-二基)(P3HT)、[双(4-苯基)(2,4,6-三甲基苯基)胺](PTAA)、聚(9,9-二辛基芴-CO-N-(4-丁基苯基)二苯胺)聚(TFB)、(4-丁基苯基二苯胺)(Poly-TPD)、聚(N-乙烯基咔唑)(PVK)或2,2',7,7'-四[N,N-二(4-甲氧基苯基)氨基]-9,9'-螺二芴(Spiro-OMeTAD);发光层上面的界面修饰层为(BCP)、聚乙烯亚胺(PEI)、聚乙氧基乙烯亚胺(PEIE)、氟化锂(LiF)、碳酸铯(Cs2CO3)、氧化钼(MoO3)、聚甲基丙烯酸甲酯(PMMA)或8-羟基喹啉铝(Alq3)。
与现有技术相比,本发明提供了小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,具备以下有益效果:
一方面,现有的技术合成的NiO纳米颗粒的尺寸较大,工艺复杂、大多数为百纳米级甚至为微米级的颗粒,无固定形貌,均匀性较差,这种NiO颗粒导致制备的QLEDs传输层材料的起伏度,覆盖率,损害了QLEDs器件的发光性能;另一方面,传统的NiO材料制备采用高温煅烧法,能耗大,成本高,获得的纳米颗粒只能分散在乙醇、水等极性溶剂中,无法在极性溶剂敏感的基底材料上进行旋涂,且纳米颗粒分散性差,成膜覆盖率差,成膜性低,而我们报到的方法成本低,重复性高,且制备的NiO材料能分散在甲苯、正己烷等非极性溶剂中,可以在极性溶剂敏感的基底材料上进行旋涂,因此具有一定的应用潜力,同时我们的方法制备出的NiO纳米晶颗粒尺寸在3-5nm,具有极小尺寸的特征,且制备方法简便易行、成本低廉、重复性高、结晶性好、无杂质峰,而且不需要高温反应,反应体系稳定,且产物可以长时间保存且待用,所形成的薄膜致密平坦、起伏度较小,同时具有高的空穴迁移率。
附图说明
图1为本发明实施例一制备得到的初始Fe:NiO纳米颗粒的透射电镜形貌图;
图2为本发明实施例一制备得到的初始Fe:NiO纳米颗粒的XRD粉末衍射图;
图3为本发明实施例一制备得到的初始Fe:NiO纳米颗粒的原子力显微镜图;
图4为本发明实施例一制备得到的初始Fe:NiO纳米颗粒的透过率图;
图5为本发明实施例一制备得到的CdSe@ZnS量子点的透射电镜形貌图;
图6为本发明实施例一制备得到的QLEDs器件的能级图;
图7为本发明实施例一制备得到的QLEDs器件的电压亮度图;
图8为本发明实施例一制备得到的QLEDs器件的亮度外量子效率图;
图9为本发明实施例二制备得到的超小氧化镍纳米颗粒的粒径分布图;
图10为本发明实施例二制备得到的氧化镍的能谱图;
图11为本发明实施例二制备得到的CsPbBr3量子点的透射电镜形貌图;
图12为本发明实施例二制备得到的CsPbBr3量子点的荧光图;
图13为本发明实施例二制备得到的QLEDs器件的电压亮度图;
图14为本发明实施例三制备得到Ni 2P的XPS图;
图15为本发明实施例三制备得到NiO纳米颗粒O1s的XPS图;
图16为本发明实施例三制备得到的硅量子点的透射电镜形貌图;
图17为本发明实施例三制备得到的Si QLEDs器件示意图。
具体实施方式
实施例一
小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法的实施例
请参阅图1-8,小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其制备方法包括以下步骤:
S1:将0.5mmol的碳酸镍、3mmol十八醇、0.1mmol碳酸铁、2mL油酸加到10ml十八烯中,并加入高温磁子,确保溶液在反应过程中充分搅拌;然后抽真空至0.03Torr,打开磁力搅拌器,将温度设成80℃,充分反应30min,然后待溶液变成澄清的黄绿色时,然后通入氮气后,将反应溶液升温至270°C,反应3h,然后获得灰黑色Fe:NiO纳米颗粒的原溶液;
S2:取10mL的Fe:NiO的原溶液,将0.5mmol的5-氨基戊酸加入,在120°C的温度下,搅拌12h,获得功能化Fe:NiO纳米颗粒,然后加入适当乙醇使功能化Fe:NiO完全析出,然后8000rpm离心5min,然后分散在甲苯中,且反复离心分散三次,最后将Fe:NiO纳米颗粒分散于甲苯,随后用0.22um的滤膜过滤,过滤液待用,如图1所示,Fe:NiO纳米颗粒的形貌为球形,并且尺寸均一,具有高的单分散,粒径的尺寸分布大概为5~10nm,同时Fe:NiO纳米颗粒的粉末具有清晰的衍射峰,说明Fe:NiO纳米颗粒具有高的结晶性,如附图2所示,同时根据Debye-Scherrer公式,D=Kλ/(βcosθ),可以从XRD的最强衍射峰推断出Fe:NiO的平均粒径为5.6纳米;
S3:将商用的ITO用氮气枪吹掉表面的大颗粒尘埃,然后分别放入洗涤剂、超纯水、丙酮、异丙醇常温超声15min,最后用氮气快速吹干表面,然后将上述洗涤好的ITO正面朝上,放入紫外臭氧清洗仪中,处理15min,来增加ITO表面清洁性和亲水性,接着取出ITO,将所合成的Fe:NiO分散在甲苯中,浓度为(5mg/ml),取Fe:NiO氯苯溶液,在匀胶机里以3000rpm条件下保持1min,立即放在加热台上退火,条件为150℃,保持15min取下,立即转入氮气保护下的手套箱中进行旋涂,所制备的Fe:NiO纳米颗粒薄膜的覆盖率高,粗糙度低,对随后功能层的沉积没有影响,如附图3所示。在可见光范围内,其透光率大于85%,说明Fe:NiO纳米颗粒传输层不会造成出光的损失,非常适合可见光QLED传输层的构筑,如附图4所示。然后取60μLTFB氯苯溶液,在3000rpm条件下保持旋转45s,接着放在热台上150℃退火30min取下,然后旋涂CdSe@ZnS绿光量子点甲苯溶液,溶度为18mg/ml,在3000rpm条件下保持旋转45s,所采用的CdSe@ZnS绿光量子点呈球形,粒径尺寸大约为10nm,如附图5所示。将所合成好的ZnO量子点乙醇溶液,滴加到旋转的ITO/Fe:NiO/TFB/QDs器件上,然后3000rpm条件下保持旋转45s,放于加热台上,条件60℃,保持30min取下,最后将上述构筑的ITO/Fe:NiO/TFB/QDs/ZnO器件放于热蒸发镀膜机中,蒸镀铝电极,然后将上述完成的ITO/Fe:NiO/TFB/QDs/ZnO/Al的完整器件在手套箱中进行封装,所用材料为紫外固化胶,用紫外灯照射1min,使紫外胶固化,整个器件构筑过程完成,器件的能级示意图如图6所示,由于Fe:NiO纳米颗粒薄膜高的空穴迁移率,所制备的绿光QLEDs器件在6.4V实现了66420cd/m2的亮度,如图7所述,以及获得20.47cd/m2的外量子效率,如图8所示;
实施例二
小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法的实施例
请参阅图9-13,小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其制备方法包括以下步骤:
S1:将0.5mmol的硝酸镍、3mmol十八醇、0.01mmol硝酸锶、2mL油酸加到10ml十八烯中,并加入高温磁子,确保溶液在反应过程中充分搅拌,然后抽真空至0.05Torr,打开磁力搅拌器,将温度设成100℃,充分反应30min,然后待溶液变成澄清的黄绿色时,然后通入氮气,将反应溶液升温至270℃,反应3h,然后获得灰黑色Sr:NiO纳米颗粒原溶液;
S2:取10mL的Sr:NiO的原溶液,将0.5mmol的2-氨基二苯甲酮-2'-羧酸加入,在120℃的温度下,搅拌12h,获得功能化Sr:NiO纳米颗粒,然后加入适当甲醇使功能化Sr:NiO完全析出,然后5000rpm离心5min,然后分散在正己烷中,且反复离心分散三次,最后将Sr:NiO纳米颗粒分散于正己烷中,随后用0.22um的滤膜过滤,过滤液待用,对所制备的Sr:NiO过滤液进行粒径分布测试,粒径分布结果表现为尺寸分布范围在4-10nm,大多数Sr:NiO纳米颗粒集中在10nm,如图9所示。随后对Sr:NiO纳米颗粒进行能谱表征,表征谱出现了明显的镍和氧的峰,且镍和氧的原子比为41.46:58.54,如图10所示,这可能由于Sr:NiO纳米颗粒表面存在配体的缘故,同时也没发现明显的锶元素的特征峰,这可能由于锶元素掺杂量少的缘故;
S3:将商用的ITO用氮气枪吹掉表面的大颗粒尘埃,然后分别放入洗涤剂、超纯水、丙酮、异丙醇常温超声15min,最后用氮气快速吹干表面,然后将上述洗涤好的ITO正面朝上,放入紫外臭氧清洗仪中,处理15min,来增加ITO表面清洁性和亲水性,接着取出ITO,将所合成的Sr:NiO分散在正己烷中,浓度为8mg/ml,取Fe:NiO氯苯溶液,在匀胶机里以3000rpm条件下保持1min,立即放在加热台上退火,条件为150℃,保持15min取下,立即转入氮气保护下的手套箱中进行旋涂,然后取60μLPVK氯苯溶液,在3000rpm条件下保持旋转45s,接着放在热台上150℃退火30min取下,然后旋涂CsPbBr3绿光钙钛矿量子点甲苯溶液,溶度为18mg/ml,在3000rpm条件下保持旋转45s,所使用的CsPbBr3绿光钙钛矿量子点为纳米立方体,分散性良好,尺寸大约在12nm左右,如图11所示,且CsPbBr3量子点的荧光峰在524nm,半峰宽高仅为18nm,如图12所示,随后将所合成好的ZnO量子点氯苯溶液,滴加到旋转的ITO/Sr:NiO/TFB/CsPbBr3QDs器件上,然后3000rpm条件下保持旋转45s,放于加热台上,条件60℃,保持30min取下,最后将上述构筑的ITO/Sr:NiO/PVK/CsPbBr3QDs/ZnO器件放于热蒸发镀膜机中,蒸镀铝电极,然后将上述完成的ITO/Sr:NiO/PVK/CsPbBr3QDs/ZnO/Al的完整器件在手套箱中进行封装,所用材料为紫外固化胶,用紫外灯照射1min,使紫外胶固化,整个器件构筑过程完成,由于Sr:NiO纳米颗粒薄膜高的空穴迁移率,所制备的绿光CsPbBr3QLEDs器件在5.8V实现了18130cd/m2的亮度,如图13所示;
实施例三
小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法的实施例
请参阅图14-17,小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其制备方法包括以下步骤:
S1:将0.5mmol的硬脂酸镍、3mmol十八醇、0.1mmol硬脂酸铜、2mL油酸加到10ml十八烯中,并加入高温磁子,确保溶液在反应过程中充分搅拌;然后然后抽真空至0.04Torr,,打开磁力搅拌器,将温度设成60℃,充分反应30min,然后待溶液变成澄清的黄绿色时,通入氮气,将反应溶液升温至250℃,反应3h,然后获得灰黑色Cu:NiO纳米颗粒原液;
S2:取10mL的Cu:NiO的原溶液,将0.5mmol的5氨基戊酸加入,在120°C的温度下,搅拌12h,获得功能化Cu:NiO纳米颗粒,然后加入适当乙醇使功能化Cu:NiO完全析出,然后8000rpm离心5min,然后分散在氯苯中,且反复离心分散三次,最后将Cu:NiO纳米颗粒分散于氯苯,随后用0.22um的滤膜过滤,过滤液待用,如图14所示,Cu:NiO纳米颗粒的X射线光电谱表明样品具有明显的O1s和Ni2p的特征峰,说明我们确实合成了Cu:NiO纳米颗粒,如图14和15所示;
S3:将商用的ITO用氮气枪吹掉表面的大颗粒尘埃,然后分别放入洗涤剂、超纯水、丙酮、异丙醇常温超声15min,最后用氮气快速吹干表面,然后将上述洗涤好的ITO正面朝上,放入紫外-臭氧清洗仪中,处理15min,来增加ITO表面清洁性和亲水性,接着取出ITO。将所合成的Cu:NiO分散在氯苯中,浓度为10mg/ml,取Fe:NiO氯苯溶液,在匀胶机里以4000rpm条件下保持1min,立即放在加热台上退火,条件为100℃,保持30min取下,立即转入氮气保护下的手套箱中进行旋涂,然后旋涂硅量子点(SiQDs)的乙醇溶液,溶度为18mg/ml,在3000rpm条件下保持旋转45s,硅量子点的分散性良好,尺寸均一,具有均匀的粒径,如图16所示,将所合成好的Mg:ZnO量子点氯苯溶液,滴加到旋转的ITO/Cu:NiO/TFB/SiQDs器件上,然后4000rpm条件下保持旋转45s,放于加热台上,条件60℃,保持30min取下,最后将上述构筑的ITO/Cu:NiO/SiQDs/Mg:ZnO器件放于热蒸发镀膜机中,蒸镀铝电极,然后将上述完成的ITO/Cu:NiO/SiQDs/MgZnO/Al的完整器件在手套箱中进行封装,所用材料为紫外固化胶,用紫外灯照射1min,使紫外胶固化,整个器件构筑过程完成,器件的整个示意图如图17所示;
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (10)
1.小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:其制备方法包括以下步骤:
S1:将镍盐、掺杂盐、有机配体和溶剂相混合,在一定温度和真空度下,以一定的速度搅拌一定的时间,待溶液变成黄绿色时,通入惰性气体,升高到一定的温度,反应一定的时间,获得灰黑色的氧化镍纳米颗粒的原液;
S2:将氧化镍纳米颗粒进行配体交换反应,将一定浓度的镍纳米颗粒加入一定量的交换配体,在一定的温度下,经过一定时间的搅拌,获得功能性的氧化镍纳米颗粒;
S3:随后将反溶剂加至功能化氧化镍纳米晶的原溶液中,以一定的速度离心一定的时间,随后将获得的沉淀内加入溶剂再分散,重复离心步骤多次,去除氧化镍纳米晶在合成过程中产生的反应废料,获得干净氧化镍纳米颗粒;
S4:构筑QLED发光器件,QLED器件包括:透明导电基底、氧化镍纳米颗粒传输层、界面修饰层、量子点发光层、顶部电荷传输层、界面修饰层和电极;其中,在透明导电基底上形成氧化镍纳米颗粒空穴传输层,量子点发光层通过成膜工艺在氧化镍纳米颗粒传输层上形成量子点发光层,在量子点发光薄膜上形成顶部电荷传输层,在顶部电荷传输层上制备电极,在量子点发光层的上界面或下界面添加界面修饰层,提升器件的性能,随后对构筑器件进行封装,封装材料为紫外固化胶以及超薄的载玻片。
2.根据权利要求1所述的小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:所述步骤S1中镍盐为硝酸镍、磷酸镍、硫酸镍、碳酸镍、硬脂酸镍、溴化镍、氯化镍、碘化镍中的一种或多种,二价金属盐为硝酸铁、硝酸镁、硝酸铜、硝酸锶、碳酸铁、碳酸铜、碳酸锶、硬脂酸铜、溴化铁、溴化锰、溴化镁、溴化铜、溴化锌、溴化锶、溴化钙、碘化铁、碘化铜、碘化锶中的一种或多种,有机配体可以是但不局限于辛酸、油酸、硬脂酸,溶剂可以是但不局限于石蜡油、十六烯、十八醇和十八烯。
3.根据权利要求1所述的小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:所述步骤S1中真空下的反应的温度为40~100℃,反应时间为10~60min,真空度为0.01~0.5Torr,通入惰性气体后的反应的时间2~5小时,反应的温度为100~500℃。
4.根据权利要求1所述的小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:所述步骤S2中交换配体为多齿型的氨基配体、羧基配体、硫基配体、磺基配体、磷基配体中的一种或多种,例如三辛基膦、三丁基膦、二苯基膦、双十二烷基二甲基溴化铵、磺基甜菜碱、磷胆碱、氨基酸、5-氨基水杨酸、5氨基戊酸、2-氨基二苯甲酮-2'-羧酸、硫代甜菜碱、谷氨酰胺、2-(4-(甲基磺酰基)苯基)乙胺、2,2'-亚氨基二苯甲酸等。
5.根据权利要求1所述的小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:所述步骤S2中对于10mL的NiO纳米颗粒,功能交换配体的量为0.01~0.5mL。
6.根据权利要求1所述的小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:所述步骤S3中离心剂和与溶剂的体积比为0.2~3:1,离心速度为3000~5000rpm,离心时间为3~30min,NiO纳米颗粒的浓度为5~50mg/mL,氧化镍纳米颗粒的粒径尺寸为3~12nm。
7.根据权利要求1所述的小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:所述步骤S3中溶剂为甲苯、正己烷、环己烷、苯、氯仿、葵烷、氯苯、辛胺、辛烷中的一种,反溶剂为乙醇、甲醇、丁醇、乙酸乙酯、丙酮中的一种。
8.根据权利要求1所述的小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:所述步骤S4中NiO纳米颗粒墨水的浓度为3-50mg/mL,薄膜的厚度为6~50nm,NiO纳米颗粒薄膜的退火温度为60~500℃,退火时间为10~60分钟;量子点发光层为钙钛矿量子点ABX3(A=FA、MA、Cs、Rb、K;B=Pb、Sn、Bi、Mn;X=Cl、Br、I)、II-IV和III-V族量子点(ZnS、CdSe、InP、CdSe@ZnS)、碳点、石墨烯量子点、硅量子点;电子传输层分为有机电子传输层和无机电子传输层两种,有机电子传输层为1,3,5-三(1-苯基-1H-苯并咪唑-2-基)苯(TPBi)、富勒烯及其衍生物(C60、C70、PC61BM、PC71BM),无机电子传输层为氧化锡(SnO2)、氧化锌(ZnO)或氧化钛(TiO2)。
9.根据权利要求1所述的小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:所述步骤S4中除金属电极外,各个功能层的成膜工艺为旋涂、刮涂、卷对卷、滴涂或丝网印刷中一种或多种,所述电极为镍、钛、钙、铝、铜、银、金、碳和石墨烯电极中的一种。
10.根据权利要求1所述的小尺寸氧化镍纳米颗粒传输层的量子点发光二极管及制备方法,其特征在于:所述步骤S4中发光层下面的界面修饰层为有机空穴传输层为聚(3-己基噻吩-2,5-二基)(P3HT)、[双(4-苯基)(2,4,6-三甲基苯基)胺](PTAA)、聚(9,9-二辛基芴-CO-N-(4-丁基苯基)二苯胺)聚(TFB)、(4-丁基苯基二苯胺)(Poly-TPD)、聚(N-乙烯基咔唑)(PVK)或2,2',7,7'-四[N,N-二(4-甲氧基苯基)氨基]-9,9'-螺二芴(Spiro-OMeTAD);发光层上面的界面修饰层为(BCP)、聚乙烯亚胺(PEI)、聚乙氧基乙烯亚胺(PEIE)、氟化锂(LiF)、碳酸铯(Cs2CO3)、氧化钼(MoO3)、聚甲基丙烯酸甲酯(PMMA)或8-羟基喹啉铝(Alq3)。
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2023
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