CN117153452A - Composite material, preparation method thereof, light-emitting diode and display device - Google Patents
Composite material, preparation method thereof, light-emitting diode and display device Download PDFInfo
- Publication number
- CN117153452A CN117153452A CN202210552462.9A CN202210552462A CN117153452A CN 117153452 A CN117153452 A CN 117153452A CN 202210552462 A CN202210552462 A CN 202210552462A CN 117153452 A CN117153452 A CN 117153452A
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- Prior art keywords
- electrode
- composite material
- mesoporous
- salt
- oxide particles
- Prior art date
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- 239000002131 composite material Substances 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 78
- 239000011810 insulating material Substances 0.000 claims abstract description 64
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 63
- 239000000463 material Substances 0.000 claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 68
- 239000011787 zinc oxide Substances 0.000 claims description 34
- 229910052751 metal Inorganic materials 0.000 claims description 33
- 239000002184 metal Substances 0.000 claims description 33
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 30
- 239000002096 quantum dot Substances 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 30
- 239000012266 salt solution Substances 0.000 claims description 23
- 150000003751 zinc Chemical class 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 150000003839 salts Chemical class 0.000 claims description 16
- 229910044991 metal oxide Inorganic materials 0.000 claims description 14
- 150000004706 metal oxides Chemical class 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 229910052738 indium Inorganic materials 0.000 claims description 12
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 12
- 229910052741 iridium Inorganic materials 0.000 claims description 12
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 12
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 12
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 12
- 229910001887 tin oxide Inorganic materials 0.000 claims description 12
- 239000007983 Tris buffer Substances 0.000 claims description 11
- -1 carbazole-9-yl Chemical group 0.000 claims description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000012670 alkaline solution Substances 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 9
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000011258 core-shell material Substances 0.000 claims description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 6
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052733 gallium Inorganic materials 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 150000002815 nickel Chemical class 0.000 claims description 6
- 125000001037 p-tolyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)C([H])([H])[H] 0.000 claims description 6
- 150000003481 tantalum Chemical class 0.000 claims description 6
- 150000003608 titanium Chemical class 0.000 claims description 6
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 claims description 6
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- BHHYHSUAOQUXJK-UHFFFAOYSA-L zinc fluoride Chemical compound F[Zn]F BHHYHSUAOQUXJK-UHFFFAOYSA-L 0.000 claims description 6
- UAYWVJHJZHQCIE-UHFFFAOYSA-L zinc iodide Chemical compound I[Zn]I UAYWVJHJZHQCIE-UHFFFAOYSA-L 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 150000003754 zirconium Chemical class 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- 241000764773 Inna Species 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- PJANXHGTPQOBST-VAWYXSNFSA-N Stilbene Natural products C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052793 cadmium Inorganic materials 0.000 claims description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 3
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 claims description 3
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- ZNRKKSGNBIJSRT-UHFFFAOYSA-L dibromotantalum Chemical compound Br[Ta]Br ZNRKKSGNBIJSRT-UHFFFAOYSA-L 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims description 3
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-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
- KYKLWYKWCAYAJY-UHFFFAOYSA-N oxotin;zinc Chemical compound [Zn].[Sn]=O KYKLWYKWCAYAJY-UHFFFAOYSA-N 0.000 claims description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 150000003220 pyrenes Chemical class 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 235000021286 stilbenes Nutrition 0.000 claims description 3
- VIFFBFSYCHETPB-UHFFFAOYSA-D tantalum(5+) pentacarbonate Chemical compound [Ta+5].[Ta+5].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O VIFFBFSYCHETPB-UHFFFAOYSA-D 0.000 claims description 3
- FYNXQOUDSWHQQD-UHFFFAOYSA-N tantalum(5+) pentanitrate Chemical compound [Ta+5].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYNXQOUDSWHQQD-UHFFFAOYSA-N 0.000 claims description 3
- GCPVYIPZZUPXPB-UHFFFAOYSA-I tantalum(v) bromide Chemical compound Br[Ta](Br)(Br)(Br)Br GCPVYIPZZUPXPB-UHFFFAOYSA-I 0.000 claims description 3
- OEIMLTQPLAGXMX-UHFFFAOYSA-I tantalum(v) chloride Chemical compound Cl[Ta](Cl)(Cl)(Cl)Cl OEIMLTQPLAGXMX-UHFFFAOYSA-I 0.000 claims description 3
- LTSUHJWLSNQKIP-UHFFFAOYSA-J tin(iv) bromide Chemical compound Br[Sn](Br)(Br)Br LTSUHJWLSNQKIP-UHFFFAOYSA-J 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- YUOWTJMRMWQJDA-UHFFFAOYSA-J tin(iv) fluoride Chemical compound [F-].[F-].[F-].[F-].[Sn+4] YUOWTJMRMWQJDA-UHFFFAOYSA-J 0.000 claims description 3
- QPBYLOWPSRZOFX-UHFFFAOYSA-J tin(iv) iodide Chemical compound I[Sn](I)(I)I QPBYLOWPSRZOFX-UHFFFAOYSA-J 0.000 claims description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 229940102001 zinc bromide Drugs 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 3
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 3
- LSWWNKUULMMMIL-UHFFFAOYSA-J zirconium(iv) bromide Chemical compound Br[Zr](Br)(Br)Br LSWWNKUULMMMIL-UHFFFAOYSA-J 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 claims description 2
- 125000003983 fluorenyl group Chemical class C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 claims 1
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- 239000010410 layer Substances 0.000 description 132
- 238000002347 injection Methods 0.000 description 24
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- 238000012360 testing method Methods 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 230000000903 blocking effect Effects 0.000 description 6
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- ZOKIJILZFXPFTO-UHFFFAOYSA-N 4-methyl-n-[4-[1-[4-(4-methyl-n-(4-methylphenyl)anilino)phenyl]cyclohexyl]phenyl]-n-(4-methylphenyl)aniline Chemical compound C1=CC(C)=CC=C1N(C=1C=CC(=CC=1)C1(CCCCC1)C=1C=CC(=CC=1)N(C=1C=CC(C)=CC=1)C=1C=CC(C)=CC=1)C1=CC=C(C)C=C1 ZOKIJILZFXPFTO-UHFFFAOYSA-N 0.000 description 1
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- 229910016036 BaF 2 Inorganic materials 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- YERGTYJYQCLVDM-UHFFFAOYSA-N iridium(3+);2-(4-methylphenyl)pyridine Chemical compound [Ir+3].C1=CC(C)=CC=C1C1=CC=CC=N1.C1=CC(C)=CC=C1C1=CC=CC=N1.C1=CC(C)=CC=C1C1=CC=CC=N1 YERGTYJYQCLVDM-UHFFFAOYSA-N 0.000 description 1
- 125000000040 m-tolyl group Chemical group [H]C1=C([H])C(*)=C([H])C(=C1[H])C([H])([H])[H] 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
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- 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 1
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- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229960002796 polystyrene sulfonate Drugs 0.000 description 1
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- 238000004549 pulsed laser deposition Methods 0.000 description 1
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- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The application discloses a composite material, which comprises mesoporous inorganic oxide particles and insulating materials filled in mesopores of the mesoporous inorganic oxide particles. The composite material can directly adjust the conductivity and the electron transmission property of the mesoporous inorganic oxide particles by adjusting the proportion of the insulating material, so that the conductivity and the electron transmission property of the mesoporous inorganic oxide particles can be quickly and effectively adjusted, and the light-emitting diode prepared by taking the composite material as an electron transmission layer material has higher luminous efficiency and longer service life. In addition, the insulating material is directly filled in the mesopores of the mesoporous inorganic oxide particles, and the insulating layer arranged between the electron transmission layer and the luminescent layer can be avoided through a complex preparation process, so that the manufacturing process is simplified, and the cost is saved. In addition, the application also discloses a preparation method of the composite material, a light-emitting diode comprising the composite material and a display device.
Description
Technical Field
The present application relates to the field of display technologies, and in particular, to a composite material, a method for preparing the composite material, a light emitting diode including the composite material, and a display device including the light emitting diode.
Background
Light emitting diodes that are widely used today are Organic Light Emitting Diodes (OLEDs) and quantum dot light emitting diodes (QLEDs). Conventional OLED and QLED device structures generally include an anode, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer, and a cathode. Under the action of the electric field, holes generated by the anode and electrons generated by the cathode of the light-emitting device move, are respectively injected into the hole transmission layer and the electron transmission layer and finally migrate to the light-emitting layer, when the hole transmission layer and the electron transmission layer meet at the light-emitting layer, excitons are generated, and the excitons finally generate visible light in a form of releasing light energy.
In the existing light-emitting diode, especially the quantum dot light-emitting diode, the common electron transport layer mainly comprises electron transport materials containing inorganic semiconductor particles, and the electron transport materials have excellent electron transport performance, so that the light-emitting diode comprising the electron transport materials has good electron mobility, and the electron injection rate in the light-emitting layer of the light-emitting diode is higher than the hole injection rate, so that the electron-hole injection in the light-emitting layer is unbalanced, the efficiency and the service life of the light-emitting diode are affected, and further improvement and development are needed.
Disclosure of Invention
In view of this, the present application provides a composite material that aims to regulate the electron transport rate of existing materials.
The embodiment of the application is realized in such a way that the composite material comprises mesoporous inorganic oxide particles and insulating materials filled in the mesopores of the mesoporous inorganic oxide particles.
Alternatively, in some embodiments of the present application, the composite material is composed of the mesoporous inorganic oxide particles, and an insulating material filled in mesopores of the mesoporous inorganic oxide particles.
Optionally, in some embodiments of the present application, the mass ratio of the mesoporous inorganic oxide particles to the insulating material in the composite material is (92-97): (3-8).
Alternatively, in some embodiments of the present application, the mesoporous inorganic oxide particles are selected from mesoporous ZnO, mesoporous TiO 2 Mesoporous SnO 2 Mesoporous Ta 2 O 3 Mesoporous ZrO 2 Mesoporous poresOne or more of NiO.
Alternatively, in some embodiments of the application, the mesoporous inorganic oxide particles have an average particle size of from 20 to 400nm.
Optionally, in some embodiments of the present application, the insulating material is selected from inorganic insulating materials, and the inorganic insulating materials are selected from one or more of alumina and aluminum nitride.
Alternatively, in some embodiments of the application, the insulating material has an average particle size of 3 to 30nm.
Correspondingly, the embodiment of the application also provides a preparation method of the composite material, which comprises the following steps:
dissolving metal salt in water to obtain a metal salt solution;
dissolving persulfate in water to obtain persulfate solution;
mixing the metal salt solution with the persulfate solution to obtain a mixed solution;
adding an insulating material and an alkaline solution into the mixed solution, and performing hydrothermal reaction to obtain a composite material, wherein the composite material comprises mesoporous inorganic oxide particles and the insulating material filled in mesopores of the mesoporous inorganic oxide particles.
Alternatively, in some embodiments of the application, the temperature of the hydrothermal reaction is 250-500 ℃; and/or
The hydrothermal reaction time is 10 min-5 h.
Optionally, in some embodiments of the present application, the metal salt is selected from one or more of zinc salt, titanium salt, tin salt, nickel salt, tantalum salt, and zirconium salt; and/or
The persulfate is selected from one or more of potassium persulfate, sodium persulfate, ammonium persulfate and sodium peroxodisulfate; and/or
The alkaline solution is selected from one or more of ammonia water, tetramethyl ammonium hydroxide, sodium hydroxide and potassium hydroxide; and/or
The insulating material is selected from inorganic insulating materials, and the inorganic insulating materials are selected from one or more of aluminum oxide and aluminum nitride.
Optionally, in some embodiments of the present application, the zinc salt is selected from one or more of zinc acetate, zinc nitrate, zinc sulfate, zinc chloride, zinc fluoride, zinc bromide, and zinc iodide; and/or
The titanium salt is selected from one or more of titanium nitrate, titanium sulfate and titanium chloride; and/or
The tin salt is selected from one or more of tin chloride, tin fluoride, tin bromide and tin iodide; and/or
The nickel salt is selected from one or more of nickel nitrate, nickel sulfate, nickel chloride, nickel fluoride, nickel bromide and nickel iodide; and/or
The tantalum salt is selected from one or more of tantalum pentabromide, tantalum pentachloride, tantalum carbonate, tantalum nitrate and tantalum bromide; and/or
The zirconium salt is one or more selected from zirconium chloride, zirconium acid, zirconium sulfate and zirconium bromide.
Alternatively, in some embodiments of the application, the concentration of the metal salt solution is 0.01 to 1M; and/or
The concentration of the persulfate solution is 0.005-0.05M; and/or
The pH of the alkaline solution is 10-13.
Alternatively, in some embodiments of the application, the molar ratio of the metal salt to the persulfate salt is (1-10): 1, a step of; and/or
The mass ratio of the metal salt to the insulating material is (10-200): 1.
optionally, in some embodiments of the present application, the composite material includes mesoporous inorganic oxide particles, and an insulating material filled in mesopores of the mesoporous inorganic oxide particles, wherein a mass ratio of the mesoporous inorganic oxide particles to the insulating material is (92 to 97): (3-8); and/or
The average grain diameter of the insulating material is 3-30 nm; and/or
The average particle diameter of the mesoporous inorganic oxide particles is 20-400 nm.
Correspondingly, the embodiment of the application also provides a light-emitting diode, which comprises a laminated anode, a light-emitting layer, an electron transport layer and a cathode, wherein the electron transport layer comprises the composite material, or the electron transport layer comprises the composite material prepared by the preparation method.
Alternatively, in some embodiments of the application, the anode is selected from the group consisting of Ca electrode, ba electrode, ca/Al electrode, liF/Ca electrode, liF/Al electrode, baF 2 Al electrode, csF/Al electrode, caCO 3 Al electrode, baF 2 a/Ca/Al electrode, an Al electrode, a Mg electrode, an Au-to-Mg electrode or an Ag-to-Mg electrode; or alternatively
The light-emitting layer is an organic light-emitting layer or a quantum dot light-emitting layer, and the material of the organic light-emitting layer is selected from 4,4' -bis (N-carbazole) -1,1' -biphenyl: tris [2- (p-tolyl) pyridine-C2, N) iridium (III), 4' -tris (carbazole-9-yl) triphenylamine, tris [2- (p-tolyl) pyridine-C2, N) iridium, a biaryl anthracene derivative, a stilbene aromatic derivative, a pyrene derivative, a fluorene derivative, a blue-emitting TBPe fluorescent material, a green-emitting TTPX fluorescent material, an orange-emitting TBRb fluorescent material and a red-emitting DBP fluorescent material, wherein the material of the quantum dot luminescent layer is one or more selected from single-structure quantum dots and core-shell-structure quantum dots, the material of the single-structure quantum dots, the material of the cores of the core-shell-structure quantum dots and the material of the shells of the core-shell-structure quantum dots are one or more selected from II-VI compounds, III-V compounds and I-III-VI compounds, and the II-VI compounds are one or more selected from CdS, cdSe, cdTe, znS, znSe, znTe, znO, hgS, hgSe, hgTe, cdSeS, cdSeTe, cdSTe, znSeS, znSeTe, znSTe, hgSeS, hgSeTe, hgSTe, cdZnS, cdZnSe, cdZnTe, cdHgS, cdHgSe, cdHgTe, hgZnS, hgZnSe, hgZnTe, cdZnSeS, cdZnSeTe, cdZnSTe, cdHgSeS, cdHgSeTe, cdHgSTe, hgZnSeS, hgZnSeTe and HgZnSte; the III-V compound is selected from GaN, gaP, gaAs, gaSb, alN, alP, alAs, alSb, inN, inP, inAs, inSb, gaNP, gaNAs, gaNSb, gaPAs, gaPSb, alNP, alNAs, alNSb, alPAs, alPSb, inNP, inNAs, inNSb, inPAs, inPSb, gaAlNP, gaAlNAs, gaAlNSb, gaAlPAs, gaAlPSb, gaInNP, gaInNAs, gaInNS b. GaInPAs, gaInPSb, inAlNP, inAlNAs, inAlNSb, inAlPAs and InAlPSb; the I-III-VI compound is selected from CuInS 2 、CuInSe 2 AgInS 2 One or more of the following; or alternatively
The cathode is selected from a metal oxide electrode, a doped metal oxide electrode, a metal simple substance electrode, a graphene electrode or a carbon nano tube electrode, and the material of the metal oxide electrode is selected from SnO 2 、In 2 O 3 The material of the doped metal oxide electrode is selected from one or more of indium doped tin oxide, indium doped zinc tin oxide, fluorine doped tin oxide, antimony doped tin oxide, gallium doped tin oxide, aluminum doped zinc oxide, gallium doped zinc oxide, indium doped zinc oxide, magnesium doped zinc oxide, aluminum doped magnesium oxide, cadmium doped zinc oxide and indium doped cadmium oxide, and the material of the metal simple substance electrode is selected from one or more of nickel, platinum, gold, silver and iridium.
Correspondingly, the embodiment of the application also provides a display device which comprises the light emitting diode.
The composite material comprises mesoporous inorganic oxide particles and insulating materials filled in mesopores of the mesoporous inorganic oxide particles. Therefore, the conductivity and the electron transmission property of the mesoporous inorganic oxide particles can be directly regulated by regulating the proportion of the insulating material, so that the composite material with proper conductivity and electron transmission property is obtained, the rapid and effective regulation of the conductivity and electron transmission property of the mesoporous inorganic oxide particles is realized, and the light-emitting diode prepared by taking the composite material as an electron transmission layer material has higher luminous efficiency and longer service life. In addition, the insulating material is directly filled in the mesopores of the mesoporous inorganic oxide particles, so that the insulating layer is arranged between the electron transmission layer and the light-emitting layer through a complex preparation process for reducing the electron transmission performance of the light-emitting diode during the preparation of the light-emitting diode, thereby simplifying the manufacturing process and saving the cost.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for preparing a composite material according to an embodiment of the present application;
fig. 2 is a schematic structural diagram of a light emitting diode according to an embodiment of the present application;
FIG. 3 is a schematic diagram of another LED according to an embodiment of the present application;
fig. 4 is a schematic structural diagram of another led according to an embodiment of the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present application. Furthermore, it should be understood that the detailed description is presented herein for purposes of illustration and description only, and is not intended to limit the application.
In the present application, unless otherwise indicated, terms of orientation such as "upper" and "lower" are used to generally refer to the upper and lower positions of the device in actual use or operation, and specifically the orientation of the drawing figures; while "inner" and "outer" are for the outline of the device. In addition, in the description of the present application, the term "comprising" means "including but not limited to".
Various embodiments of the application may exist in a range of forms; it should be understood that the description in a range format is merely for convenience and brevity and should not be construed as a rigid limitation on the scope of the application; it is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
The embodiment of the application provides a composite material, which comprises mesoporous inorganic oxide particles and insulating materials filled in mesopores of the mesoporous inorganic oxide particles.
In the composite material, the mass ratio of the mesoporous inorganic oxide particles to the insulating material is (92-97): (3-8), for example, (93-95): (3-8), or (94-96): (3-8), or (92-97): (4-6), or (92-97): (5-7), or (92-97): (4-7). Within the range, the composite material can be made to have suitable conductivity and electron mobility.
In some embodiments, the mesoporous inorganic oxide particles may be, but are not limited to, mesoporous metal oxide particles. The mesoporous metal oxide particles may be selected from, but not limited to, mesoporous ZnO and mesoporous TiO 2 Mesoporous SnO 2 Mesoporous Ta 2 O 3 Mesoporous ZrO 2 And one or more of mesoporous NiO.
In at least one embodiment, the mesoporous inorganic oxide particles are selected from mesoporous ZnO.
In some embodiments, the mesoporous inorganic oxide particles have an average particle size of 20 to 400nm, e.g., 20 to 300nm,20 to 250nm,20 to 200nm,20 to 150nm,20 to 100nm,25 to 80nm, etc., and a surface roughness after film formation of 5 to 20nm.
The resistivity of the insulating material is 10 10 ～10 22 Omega.m. In some embodiments, the insulating material may be selected from, but is not limited to, inorganic insulating materials. The inorganic insulating material may be selected from, but not limited to, one or more of alumina and aluminum nitride. The inorganic insulating material is more easily absorbed into the insulating materialThe mesoporous inorganic oxide particles are in the mesopores of the composite material.
In some embodiments, the inorganic insulating material is a nanoscale inorganic insulating material, i.e., an inorganic nano insulating material, and correspondingly, the aluminum oxide is nano aluminum oxide and the aluminum nitride is nano aluminum nitride.
In some embodiments, the insulating material has an average particle size of 3 to 30nm, such as 3 to 25nm,5 to 20nm,8 to 15nm,4 to 10nm, and the like. The insulating material can be ensured to be uniformly dispersed and filled in the mesopores of the mesoporous inorganic oxide particles within the particle size range, and the controllable conductivity of a film layer formed by the composite material is ensured.
In some embodiments, the composite material is composed of the mesoporous inorganic oxide particles and an insulating material filled in mesopores of the mesoporous inorganic oxide particles.
In still other embodiments, polymethyl methacrylate (PMMA), polymer 2,2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene (Spiro-OMeTAD), and the like, which are known to be added in electron transport layers, may also be included in the composite.
The composite material comprises the mesoporous inorganic oxide particles and an insulating material filled in the mesopores of the mesoporous inorganic oxide particles. Therefore, the conductivity and the electron transmission property of the mesoporous inorganic oxide particles can be directly regulated by regulating the proportion of the insulating material, so that the composite material with proper conductivity and electron transmission property is obtained, the rapid and effective regulation of the conductivity and electron transmission property of the mesoporous inorganic oxide particles is realized, and the light-emitting diode prepared by taking the composite material as an electron transmission layer material has higher luminous efficiency and longer service life. In addition, the insulating material is directly filled in the mesopores of the mesoporous inorganic oxide particles, so that the insulating layer is arranged between the electron transmission layer and the light-emitting layer through a complex preparation process for reducing the electron transmission performance of the light-emitting diode during the preparation of the light-emitting diode, thereby simplifying the manufacturing process and saving the cost.
Referring to fig. 1, the embodiment of the application further provides a preparation method of the composite material, which includes the following steps:
step S11: dissolving metal salt in water to obtain a metal salt solution;
step S12: dissolving persulfate in water to obtain persulfate solution;
Step S13: mixing the metal salt solution with the persulfate solution to obtain a mixed solution;
step S14: adding an insulating material and an alkaline solution into the mixed solution, and performing hydrothermal reaction to obtain a composite material, wherein the composite material comprises mesoporous inorganic oxide particles and the insulating material filled in mesopores of the mesoporous inorganic oxide particles.
The mesoporous inorganic nano particles formed in the hydrothermal reaction process can adsorb the insulating material due to the fact that the mesoporous inorganic nano particles have large specific surface area, and therefore the insulating material is filled in the mesopores of the mesoporous inorganic nano particles.
In the step S11:
the metal salt may be one or more selected from zinc salt, titanium salt, tin salt, nickel salt, tantalum salt and zirconium salt.
The zinc salt can be selected from one or more of zinc acetate, zinc nitrate, zinc sulfate, zinc chloride, zinc fluoride, zinc bromide and zinc iodide. It will be appreciated that the zinc salt may be an anhydrous zinc salt or a hydrated zinc salt.
The titanium salt may be selected from, but not limited to, one or more of titanium nitrate, titanium sulfate and titanium chloride.
The tin salt may be selected from, but not limited to, one or more of tin chloride, tin fluoride, tin bromide and tin iodide.
The nickel salt may be selected from one or more of nickel nitrate, nickel sulfate, nickel chloride, nickel fluoride, nickel bromide and nickel iodide.
The tantalum salt can be selected from one or more of tantalum pentabromide, tantalum pentachloride, tantalum carbonate, tantalum nitrate and tantalum bromide.
The zirconium salt may be selected from one or more of zirconium chloride, zirconium acid, zirconium sulfate, zirconium bromide, but is not limited thereto.
The concentration of the metal salt solution is 0.01 to 1M, for example 0.1 to 0.9M, or 0.2 to 0.8M, or 0.3 to 0.7M, or 0.4 to 0.6M. In the range, the reaction is facilitated, and if the concentration of the metal salt solution is too low, the yield of the product is easy to be low, so that the purification is not facilitated; if the concentration of the metal salt solution is too high, other side reactions may be initiated, resulting in lower purity of the resulting mesoporous inorganic oxide particles.
In the step S12:
the persulfate may be selected from, but not limited to, one or more of potassium persulfate, sodium persulfate, ammonium persulfate, and sodium peroxodisulfate.
In some embodiments, the persulfate solution has a concentration of 0.005 to 0.05M, such as 0.01 to 0.045M, or 0.02 to 0.04M, or 0.025 to 0.03M. Mesoporous inorganic oxide particles can be rapidly and efficiently generated within the range.
In some embodiments, the water in the steps S11 and S12 may be deionized water.
In the step S13:
the molar ratio of the metal salt to the persulfate is (1-10): 1, for example (2 to 9): 1, or (3-8): 1, or (4 to 7): 1, or (5-6): 1. in the range of the molar ratio, the reaction between the metal salt and the persulfate is facilitated, and mesoporous inorganic oxide particles with higher purity can be quickly and efficiently generated.
In the step S14:
the temperature of the hydrothermal reaction is 250-500 ℃ and the time is 10 min-5 h. In the temperature and time range, mesoporous inorganic oxide particles can be effectively generated, and the insulating material is adsorbed by the mesoporous inorganic oxide particles to be filled in the mesopores of the mesoporous inorganic oxide particles.
In some embodiments, the temperature of the hydrothermal reaction is 230 to 280 ℃, alternatively 300 to 450 ℃, alternatively 320 to 430 ℃, alternatively 350 to 400 ℃.
The insulating material is described above and will not be described in detail herein.
In some embodiments, the insulating material is added in an amount of: the mass ratio of the metal salt to the insulating material is (10-200): 1, for example (20 to 180): 1. (30-160): 1. (50-150): 1. (60-120): 1. (80-100): 1 or (90-110): 1.
The alkaline solution can be selected from one or more of ammonia water, tetramethyl ammonium hydroxide, sodium hydroxide and potassium hydroxide.
The pH of the alkaline solution is 10 to 13, for example 10.5 to 12.5, or 11 to 12. In the pH range, the reaction of the metal salt and persulfate is facilitated to generate mesoporous inorganic oxide particles.
In some embodiments, the concentration of the aqueous ammonia is 25-28%. The reaction is facilitated to be carried out forward in the concentration range, the occurrence of side reaction is reduced, and then the mesoporous inorganic oxide particles with high purity are obtained.
It will be appreciated that in the step S14, a step of washing and drying may be further included after the hydrothermal reaction, so as to obtain a composite material with higher purity.
Referring to fig. 2, the embodiment of the application further provides a light emitting diode 100, which includes an anode 10, a light emitting layer 20, an electron transport layer 30 and a cathode 40 sequentially stacked. The electron transport layer 30 includes the composite material described above.
Referring further to fig. 3, in some embodiments, the light emitting diode 100 further includes a hole transport layer 50 between the anode 10 and the light emitting layer 20. In other words, the light emitting diode 100 includes an anode 10, a hole transport layer 50, a light emitting layer 20, an electron transport layer 30, and a cathode 40, which are sequentially stacked.
Referring further to fig. 4, in some embodiments, the light emitting diode 100 further includes a hole injection layer 60 between the anode 10 and the hole transport layer 50. In other words, the light emitting diode 100 includes an anode 10, a hole injection layer 60, a hole transport layer 50, a light emitting layer 20, an electron transport layer 30, and a cathode 40, which are sequentially stacked.
The material of the anode 10 is a conductive material having a relatively low work function. In some embodiments, the anode 10 may be a Ca electrode, a Ba electrode, a Ca/Al electrode, a LiF/Ca electrode, a LiF/Al electrode, a BaF 2 Al electrode, csF/Al electrode, caCO 3 Al electrode, baF 2 Ca/Al electrode, mg electrode, au: mg electrode or Ag: mg electrode.
The light emitting layer 20 may be an organic light emitting layer or a quantum dot light emitting layer. When the light emitting layer 20 is an organic light emitting layer, the light emitting diode 100 may be an organic light emitting diode; when the light emitting layer 20 is a quantum dot light emitting layer, the light emitting diode 100 may be a quantum dot light emitting diode.
The material of the organic light emitting layer is a material known in the art for an organic light emitting layer of a light emitting diode, for example, may be selected from, but not limited to, CBP: ir (mppy) 3 One or more of (4, 4' -bis (N-carbazole) -1,1' -biphenyl: tris [2- (p-tolyl) pyridine-C2, N) iridium (III)), TCTX: ir (mmpy) (4, 4' -tris (carbazol-9-yl) triphenylamine: tris [2- (p-tolyl) pyridine-C2, N) iridium), a biaryl anthracene derivative, a stilbene aromatic derivative, a pyrene derivative, a fluorene derivative, a blue-emitting TBPe fluorescent material, a green-emitting TTPX fluorescent material, an orange-emitting TBRb fluorescent material and a red-emitting DBP fluorescent material.
The material of the quantum dot light emitting layer is a quantum dot material known in the art for a quantum dot light emitting layer of a light emitting diode, and for example, may be one or more selected from, but not limited to, single-structure quantum dots and core-shell structure quantum dots. The material of the single-structure quantum dot, the material of the core-shell structure quantum dot and the material of the shell of the core-shell structure quantum dot can be selected from one or more of group II-VI compounds, group III-V compounds and group I-III-VI compounds, but not limited to the materials. By way of example, the group II-VI compound may be selected from, but is not limited to CdS, cdSe, cdTe, znS, znSe, znTe, znO, hgS, hgSe, hgTe, cdSeS, cdSeTe, cdSTe, znSeS, znSeTe, znSTe, hgSeS, hgSeTe, hgSTe, cdZnS, cdZnSe, cdZnTe, cdHgS, cdHgSe, cdHgTe, hgZnS, hgZnSe, hgZnTe, cdZnSeS, cdZnSeTe, cdZnSTe, cdHgSeS, cdHgSeTe. CdHgSTe, hgZnSeS, hgZnSeTe and HgZnSTe; the III-V compound can be selected from one or more of GaN, gaP, gaAs, gaSb, alN, alP, alAs, alSb, inN, inP, inAs, inSb, gaNP, gaNAs, gaNSb, gaPAs, gaPSb, alNP, alNAs, alNSb, alPAs, alPSb, inNP, inNAs, inNSb, inPAs, inPSb, gaAlNP, gaAlNAs, gaAlNSb, gaAlPAs, gaAlPSb, gaInNP, gaInNAs, gaInNSb, gaInPAs, gaInPSb, inAlNP, inAlNAs, inAlNSb, inAlPAs and InAlPSb; the I-III-VI compound may be selected from, but is not limited to, cuInS 2 、CuInSe 2 AgInS 2 One or more of them.
As an example, the quantum dots of the core-shell structure may be selected from, but not limited to, one or more of CdZnSe/ZnSe/CdZnS/ZnS, cdZnSe/CdZnS/CdSe/CdSeS/CdS, inP/ZnSeS/ZnS, cdZnSe/ZnSe/ZnS, cdSeS/ZnS, cdSe/ZnSe/ZnS, znSeTe/ZnS, cdSe/CdZnSeS/ZnS, and InP/ZnSe/ZnS.
The material of the cathode 40 is a conductive material having a relatively high work function, and the cathode 40 may be selected from, but not limited to, a metal oxide electrode, a doped metal oxide electrode, a metal elemental electrode, a graphene electrode, or a carbon nanotube electrode. The material of the metal oxide electrode may be selected from but not limited to SnO 2 、In 2 O 3 . The material of the doped metal oxide electrode may be selected from, but not limited to, one or more of indium doped tin oxide (ITO), indium doped zinc tin oxide (ITZO), fluorine doped tin oxide (FTO), antimony doped tin oxide (ATO), gallium doped tin oxide (GTO), aluminum doped zinc oxide (AZO), gallium doped zinc oxide (GZO), indium doped zinc oxide (IZO), magnesium doped zinc oxide (MZO), aluminum doped magnesium oxide (AMO), cadmium doped zinc oxide (GTO), indium doped cadmium oxide (ICO). The material of the metal simple substance electrode can be selected from one or more of nickel (Ni), platinum (Pt), gold (Au), silver (Ag) and iridium (Ir).
The material of the hole transport layer 50 may also be a material known in the art for a hole transport layer, for example, may be selected from, but not limited to, 4' -N, N ' -dicarbazolyl-biphenyl (CBP), N ' -diphenyl-N, N ' -bis (1-naphthyl) -1,1' -biphenyl-4, 4 "-diamine (a-NPD), N ' -diphenyl-N, N ' -bis (3-methylphenyl) - (1, 1' -biphenyl) -4,4' -diamine (TPD), N ' -bis (3-methylphenyl) -N, N ' -bis (phenyl) -spiro (spiro-TPD), N ' -bis (4- (N, N ' -diphenyl-amino) phenyl) -N, N ' -diphenyl benzidine (DNTPD), 4' -tris (N-carbazolyl) -triphenylamine (TCTA), 4' -tris (N-3-methylphenyl-N-phenylamino) triphenylamine (m-MTDATA), poly [ (9, 9' -dioctylfluorene-2, 7-diyl) -co- (4, 4' - (N- (4-sec-butylphenyl) diphenylamine)) ] (TFB), poly (4-butylphenyl-diphenylamine) (poly-TPD), poly (N-butylfluorene-2, 7-diyl) co- (4, 4' - (N- (4-sec-butylphenyl) diphenylamine) (poly-TPD), polyaniline, polypyrrole, poly (p-phenylene vinylene), poly (phenylene vinylene) (PPV), poly [ 2-methoxy-5- (2-ethylhexyl oxy) -1, 4-phenylene vinylene ] (MEH-PPV) and poly [ 2-methoxy-5- (3 ',7' -dimethyloctyl oxy) -1, 4-phenylene vinylene ] (MOMO-PPV), copper phthalocyanine, aromatic tertiary amine, polynuclear aromatic tertiary amine, 4 '-bis (p-carbazolyl) -1,1' -biphenyl compound, N, N, N ', N' -tetraarylbenzidine, PEDOT: PSS and derivatives thereof, poly (N-vinylcarbazole) (PVK) and derivatives thereof, polymethacrylate and derivatives thereof, poly (9, 9-octylfluorene) and derivatives thereof, poly (spirofluorene) and derivatives thereof, N, N '-bis (naphthalene-1-yl) -N, N' -diphenyl benzidine (NPB) and spiroNPB.
The material of the hole injection layer 60 may also be a material known in the art for hole injection layers, such as may be selected from, but not limited to, poly (ethylenedioxythiophene): polystyrene sulfonate (PEDOT: PSS), poly (9, 9-dioctyl-fluorene-co-N- (4-butylphenyl) -diphenylamine) (TFB), polyarylamines, poly (N-vinylcarbazole), polyaniline, polypyrrole, N, N, N ', N ' -tetrakis (4-methoxyphenyl) -benzidine (TPD), 4-bis [ N- (1-naphthyl) -N-phenyl-amino ] biphenyl (. Alpha. -NPD), 4' -tris [ phenyl (m-tolyl) amino ] triphenylamine (m-MTDATA), 4', 4' -tris (N-carbazolyl) -triphenylamine (TCTA), 1-bis [ (di-4-tolylamino) phenylcyclohexane (TAPC), 4' -tris (diphenylamino) triphenylamine (TDATA) doped with tetrafluoro-tetracyano-quinone dimethane (F4-TCNQ), p-doped phthalocyanines (e.g., F4-TCNQ-doped zinc phthalocyanine (ZnPc)), F4-TCNQ doped N, N ' -diphenyl-N, one or more of N ' -di (1-naphthyl) -1,1' -biphenyl-4, 4' -diamine (alpha-NPD), hexaazabenzophenanthrene-capronitrile (HAT-CN), nickel oxide, molybdenum oxide, tungsten oxide, vanadium oxide, molybdenum sulfide, tungsten sulfide and copper oxide.
It will be appreciated that the led 100 may further include functional layers conventionally used in leds to help improve led performance, such as an electron blocking layer, a hole blocking layer, an electron injection layer, an interface modification layer, and the like.
It is understood that the materials of the layers of the led 100 may be adjusted according to the light emitting requirements of the led 100.
It is understood that the light emitting diode 100 may be a front-mounted light emitting diode or an inverted light emitting diode.
The electron transport layer 30 of the light emitting diode 100 contains the composite material of the present application, the composite material includes mesoporous inorganic oxide particles and insulating materials filled in the mesopores of the mesoporous inorganic oxide particles, and the insulating materials can effectively reduce the electron transport performance of the mesoporous inorganic oxide particles, reduce the rate of electron injection into the light emitting layer 20, and improve the carrier balance of the light emitting diode 100, thereby having higher light emitting efficiency and longer service life. In addition, compared with the arrangement of an insulating layer between the electron transmission layer and the luminescent layer, the application directly fills the insulating material in the mesopores of the inorganic semiconductor particles, and the process is simple and easy to control.
The application also relates to a preparation method of the light-emitting diode, which comprises the following steps:
step S21: providing a substrate having an anode 10;
step S22: forming a light emitting layer 20 on the anode 10;
step S23: dispersing the composite material in a solvent to obtain a composite material solution, and disposing the composite material solution on the light-emitting layer 20 to obtain an electron transport layer 30;
Step S24: a cathode 40 is formed on the electron transport layer 30 to obtain a light emitting diode 100.
It can be understood that, when the light emitting diode 100 further includes the hole transport layer 50, the step S22 is: a hole transport layer 50 and a light emitting layer 20 are sequentially formed on the anode 10.
It can be understood that, when the light emitting diode 100 further includes the hole injection layer 60, the step S22 is: a hole injection layer 60 and a light emitting layer 20 are sequentially formed on the anode 10.
It can be understood that, when the light emitting diode 100 further includes the hole transport layer 50 and the hole injection layer 60, the step S22 is: a hole injection layer 60, a hole transport layer 50, and a light emitting layer 20 are sequentially formed on the anode 10.
It will be appreciated that when the light emitting diode 100 further includes other functional layers for the light emitting diode that help to improve the performance of the light emitting diode, such as an electron blocking layer, a hole blocking layer, an electron injection layer, an interface modification layer, etc., the manufacturing method further includes a step of forming the functional layers on the respective layers.
The application also relates to a preparation method of the light-emitting diode, which comprises the following steps:
step S31: providing a substrate having a cathode 40;
Step S32: dispersing the composite material in a solvent to obtain a composite material solution, and disposing the composite material solution on the cathode 40 to obtain an electron transport layer 30;
step S33: a light emitting layer 20 and an anode 10 are sequentially formed on the electron transport layer 30 to obtain a light emitting diode 100.
It can be understood that, when the light emitting diode 100 further includes the hole transport layer 50, the step S33 is: a light emitting diode 100 is obtained by sequentially forming the light emitting layer 20, the hole transport layer 50, and the anode 10 on the electron transport layer 30.
It can be understood that, when the light emitting diode 100 further includes the hole injection layer 60, the step S33 is: a light emitting diode 100 is obtained by sequentially forming the light emitting layer 20, the hole injection layer 60, and the anode 10 on the electron transport layer 30.
It can be understood that, when the light emitting diode 100 further includes the hole transport layer 50 and the hole injection layer 60, the step S33 is: a light emitting diode 100 is obtained by sequentially forming the light emitting layer 20, the hole transporting layer 50, the hole injecting layer 60, and the anode 10 on the electron transporting layer 30.
It will be appreciated that when the light emitting diode 100 further includes other functional layers for the light emitting diode that help to improve the performance of the light emitting diode, such as an electron blocking layer, a hole blocking layer, an electron injection layer, an interface modification layer, etc., the manufacturing method further includes a step of forming the functional layers on the respective layers.
In the above two methods for preparing light emitting diodes, the solvent may be one or more selected from, but not limited to, straight chain alcohols having 1 to 5C atoms, branched alcohols having 1 to 5C atoms, chlorobenzene, and dimethyl sulfoxide.
The preparation method of the two light emitting diodes further comprises the following steps: the prepared light-emitting diode 100 is subjected to heat treatment at 60-150 ℃ for 1 min-48 h. The heat treatment may accelerate forward aging of the light emitting diode 100, improving efficiency and lifetime of the light emitting diode 100.
In the preparation methods of the two light emitting diodes, the preparation methods of the anode 10, the light emitting layer 20, the electron transport layer 30, the cathode 40, the hole transport layer 50 and the hole injection layer 60 can be implemented by conventional techniques in the art, such as chemical methods or physical methods. Wherein, the chemical method comprises chemical vapor deposition, continuous ion layer adsorption and reaction, anodic oxidation, electrolytic deposition and coprecipitation. Physical methods include physical plating methods and solution methods, wherein the physical plating methods include: thermal evaporation plating, electron beam evaporation plating, magnetron sputtering, multi-arc ion plating, physical vapor deposition, atomic layer deposition, pulsed laser deposition, etc.; the solution method may be spin coating, printing, ink jet printing, knife coating, printing, dip-coating, dipping, spray coating, roll coating, casting, slit coating, bar coating, or the like.
The materials of the anode 10, the light-emitting layer 20, the cathode 40, the hole transport layer 50 and the hole injection layer 60 are described above, and are not described here again.
The substrate may be a rigid substrate or a flexible substrate. In some embodiments, the material of the substrate may be selected from, but not limited to, one or more of glass, silicon wafer, polycarbonate, polymethyl methacrylate, polyethylene terephthalate, polyethylene naphthalate, polyamide, and polyethersulfone.
The application also relates to a display device comprising the light emitting diode 100.
The present application will now be described in more detail by way of the following examples, which are intended to be illustrative of the application and not limiting thereof.
Example 1
ZnSO is added to 4 ·7H 2 O is dissolved in deionized water to prepare zinc salt solution with the concentration of 0.08M;
will K 2 S 2 O 8 Dissolving in deionized water to prepare persulfate solution with concentration of 0.02M;
15mL of a persulfate solution with a concentration of 0.02M is added to 20mL of a zinc salt solution with a concentration of 0.08M, and 5mL of 25% ammonia water and 3mg of nano alumina with an average particle diameter of 3-30 nm are added and mixed with stirring. Then the mixture is placed in a high-pressure reaction kettle for reaction for 2 hours at 300 ℃. And after the reaction is finished, cleaning and drying the product to obtain the composite material.
The composite material of the embodiment comprises mesoporous ZnO and nano alumina filled in mesopores of the mesoporous ZnO.
In the composite material of this example, the content of mesoporous ZnO was 96.8wt% and the content of nano alumina was 3.2wt%.
Example 2
ZnSO is added to 4 ·7H 2 O is dissolved in deionized water to prepare zinc salt solution with the concentration of 0.08M;
will K 2 S 2 O 8 Dissolving in deionized water to prepare persulfate solution with concentration of 0.02M;
15mL of a persulfate solution with a concentration of 0.02M was added to 18mL of a zinc salt solution with a concentration of 0.08M, and 7mL of 25% aqueous ammonia and 4mg of nano alumina with an average particle diameter of 3 to 30nm were added and mixed with stirring. Then the mixture is placed in a high-pressure reaction kettle for reaction for 2 hours at 300 ℃. And after the reaction is finished, cleaning and drying the product to obtain the composite material.
The composite material of the embodiment comprises mesoporous ZnO and nano alumina filled in mesopores of the mesoporous ZnO.
In the composite material of this example, the content of mesoporous ZnO was 95.8wt% and the content of nano alumina was 4.2wt%.
Example 3
ZnSO is added to 4 ·3H 2 O is dissolved in deionized water to prepare zinc salt solution with the concentration of 0.08M;
will K 2 S 2 O 8 Dissolving in deionized water to prepare persulfate solution with concentration of 0.02M;
18mL of a persulfate solution with a concentration of 0.02M was added to 22mL of a zinc salt solution with a concentration of 0.08M, and 7mL of 25% aqueous ammonia and 5mg of nano alumina with a particle size of 3 to 30nm were added and mixed with stirring. Then the mixture is placed in a high-pressure reaction kettle for reaction for 2 hours at 300 ℃. And after the reaction is finished, cleaning and drying the product to obtain the composite material.
The composite material of the embodiment comprises mesoporous ZnO and nano alumina filled in mesopores of the mesoporous ZnO.
In the composite material of this embodiment, the content of mesoporous ZnO is 95.2wt% and the content of nano alumina is 4.8wt%.
Example 4
This example is substantially the same as example 1 except that 1.5mg of nano alumina and 1.5mg of nano aluminum nitride are used in place of nano alumina in example 1.
Example 5
This example is essentially the same as example 1 except that 15mL of a 0.02M persulfate solution was added to 3.75mL of a 0.08M zinc salt solution.
In the composite material of this example, the content of mesoporous ZnO was 93.9wt% and the content of nano alumina was 6.1wt%.
Example 6
This example is essentially the same as example 1 except that 15mL of a 0.02M persulfate solution is added to 37.5mL of a 0.08M zinc salt solution in this example.
In the composite material of this embodiment, the content of mesoporous ZnO is 93.2wt% and the content of nano alumina is 6.8wt%.
Example 7
This example is essentially the same as example 1 except that 15mL of a 0.02M persulfate solution was added to 3mL of a 0.08M zinc salt solution.
In the composite material of this embodiment, the content of mesoporous ZnO is 92% and the content of nano alumina is 8%.
Example 8
This example is essentially the same as example 1 except that 15mL of a 0.02M persulfate solution was added to 40mL of a 0.08M zinc salt solution.
In the composite material of this embodiment, the content of mesoporous ZnO is 96%, and the content of nano alumina is 4%.
Comparative example
Weighing 3mmol of Zn (Ac) 2 ·2H 2 Placing the O alkane in a three-neck flask, adding 30ml of DMSO, and then stirring at 25 ℃ until the O alkane is completely dissolved to obtain zinc salt solution;
5.8mmol of tetramethylammonium hydroxide was dissolved in 10ml of ethanol to obtain a tetramethylammonium hydroxide solution;
slowly dripping a tetramethyl ammonium hydroxide solution into a zinc salt solution;
after the reaction is finished, adding ethyl acetate into the product for precipitation, centrifuging, discarding supernatant, adding absolute ethyl alcohol for dissolution, adding ethyl acetate for precipitation, and centrifuging; repeating the steps for 2 times to obtain the nano zinc oxide.
Device example 1
Providing a glass substrate;
depositing an ITO material on the glass substrate to obtain an ITO cathode 40 with the thickness of 100 nm;
dispersing the composite material in the embodiment 1 in ethanol to obtain a composite material solution, and spin-coating the composite material solution on the cathode 40 to obtain an electron transport layer 30 with a thickness of 70 nm;
spin-coating a CdZnSe/CdZnSe/ZnSe/CdZnS/ZnS quantum dot material with a light-emitting peak position of 630nm and a light-emitting peak width of 19nm on the electron transport layer to obtain a light-emitting layer 20 with a thickness of 20 nm;
spin-coating a TFB material on the light-emitting layer 20 to obtain a hole transport layer 50 having a thickness of 80 nm;
spin-coating a PEDOT: PSS material on the hole transport layer 50 to obtain a hole injection layer 60 having a thickness of 90 nm;
ag was vapor-deposited on the hole injection layer 60 to obtain an anode 10 having a thickness of 50nm, thereby obtaining a light emitting diode 100.
The light emitting diode 100 was heat treated at 120 deg.c for 15min.
Device examples 2 to 8
Device examples 2-8 are substantially identical to device example 1, except that the composite materials used in the preparation of device examples 2-8 are the composite materials of examples 2-8, respectively.
Device comparative example
The device comparative example was substantially the same as device example 1 except that the composite material used in the preparation of the device comparative example was nano zinc oxide of the comparative example.
External quantum efficiency EQE and lifetime t95@1000nit tests were performed on the light emitting diodes 100 of device examples 1 to 8 and device comparative examples. The test results are shown in the table one.
The test method of the external quantum efficiency EQE comprises the following steps:
the external quantum efficiency EQE is the ratio of the number of electron-hole pairs injected into the quantum dots to the number of outgoing photons, the unit is an important parameter for measuring the advantages and disadvantages of the electroluminescent device, and the EQE is obtained by measuring by an EQE optical test instrument. The specific calculation formula is as follows:
wherein ηe is light output coupling efficiency, ηr is the ratio of the number of carriers combined to the number of carriers injected, χ is the ratio of the number of excitons generating photons to the total number of excitons, K R For the rate of the radiation process, K NR Is the non-radiative process rate.
Test conditions: the process is carried out at room temperature, and the air humidity is 30-60%.
The test method of the service life T95@1000nit comprises the following steps:
the time required for the device to decrease in brightness to a certain proportion of the maximum brightness under constant current or voltage drive is defined as T95, and the lifetime is the measured lifetime. To shorten the test period, the device lifetime test is usually performed by accelerating the aging of the device at high brightness, and fitting the device lifetime at high brightness by an extended exponential decay brightness decay fitting formula, for example: the lifetime meter at 1000nit is T95@1000nit. The specific calculation formula is as follows:
Wherein T95 L T95 is the life at low brightness H For the actual life under high brightness, L H To accelerate the device to the highest brightness, L L For 1000nit, A is an acceleration factor, and the experiment obtains an A value of 1.7 by measuring the service lives of a plurality of groups of green QLED devices under rated brightness;
test conditions: the process is carried out at room temperature, and the air humidity is 30-60%.
Table one:
from Table one can see:
the light emitting diodes 100 of the device embodiments 1 to 6 have higher light emitting efficiency and longer lifetime than the light emitting diode of the device comparative example.
The light emitting diode 100 of device example 7 has lower light emitting efficiency and shorter lifetime than the light emitting diodes 100 of device examples 1 and 5 to 6, probably because the use of too low an amount of metal salt in the preparation of the composite material of the electron transport layer 30 of device example 7 results in too low a yield of mesoporous inorganic oxide particles, which is disadvantageous for purification, resulting in lower purity of the composite material.
The light emitting diode 100 of device example 8 has lower light emitting efficiency and shorter lifetime than the light emitting diodes 100 of device examples 1 and 5 to 6, probably because the electron transport layer 30 of the light emitting diode 100 of device example 8 is prepared with too high an amount of metal salt, which causes other side reactions, resulting in lower purity of the mesoporous inorganic oxide particles.
The composite material, the preparation method thereof, the light emitting diode and the display device provided by the embodiment of the application are described in detail, and specific examples are applied to the principle and the implementation mode of the application, and the description of the above examples is only used for helping to understand the method and the core idea of the application; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present application, the present description should not be construed as limiting the present application.
Claims (15)
1. A composite material characterized by: comprises mesoporous inorganic oxide particles and insulating materials filled in the mesopores of the mesoporous inorganic oxide particles.
2. The composite material of claim 1, wherein: the composite material consists of the mesoporous inorganic oxide particles and insulating materials filled in the mesopores of the mesoporous inorganic oxide particles.
3. The composite material of claim 1 or 2, wherein: in the composite material, the mass ratio of the mesoporous inorganic oxide particles to the insulating material is (92-97): (3-8).
4. The composite material of claim 1 or 2, wherein: the mesoporous inorganic oxide particles are selected from mesoporous ZnO and mesoporous TiO 2 Mesoporous SnO 2 Mesoporous Ta 2 O 3 Mesoporous ZrO 2 And one or more of mesoporous NiO; and/or
The average particle diameter of the mesoporous inorganic oxide particles is 20-400 nm.
5. The composite material of claim 1 or 2, wherein:
the insulating material is selected from inorganic insulating materials, and the inorganic insulating materials are selected from one or more of aluminum oxide and aluminum nitride; and/or
The average grain diameter of the insulating material is 3-30 nm.
6. A method of preparing a composite material comprising the steps of:
dissolving metal salt in water to obtain a metal salt solution;
dissolving persulfate in water to obtain persulfate solution;
mixing the metal salt solution with the persulfate solution to obtain a mixed solution;
and adding an insulating material and an alkaline solution into the mixed solution, and performing hydrothermal reaction to obtain the composite material.
7. The method of manufacturing according to claim 6, wherein:
the temperature of the hydrothermal reaction is 250-500 ℃; and/or
The hydrothermal reaction time is 10 min-5 h.
8. The method of manufacturing according to claim 6, wherein:
The metal salt is one or more selected from zinc salt, titanium salt, tin salt, nickel salt, tantalum salt and zirconium salt; and/or
The persulfate is selected from one or more of potassium persulfate, sodium persulfate, ammonium persulfate and sodium peroxodisulfate; and/or
The alkaline solution is selected from one or more of ammonia water, tetramethyl ammonium hydroxide, sodium hydroxide and potassium hydroxide; and/or
The insulating material is selected from inorganic insulating materials, and the inorganic insulating materials are selected from one or more of aluminum oxide and aluminum nitride.
9. The method of preparing as claimed in claim 8, wherein:
the zinc salt is selected from one or more of zinc acetate, zinc nitrate, zinc sulfate, zinc chloride, zinc fluoride, zinc bromide and zinc iodide; and/or
The titanium salt is selected from one or more of titanium nitrate, titanium sulfate and titanium chloride; and/or
The tin salt is selected from one or more of tin chloride, tin fluoride, tin bromide and tin iodide; and/or
The nickel salt is selected from one or more of nickel nitrate, nickel sulfate, nickel chloride, nickel fluoride, nickel bromide and nickel iodide; and/or
The tantalum salt is selected from one or more of tantalum pentabromide, tantalum pentachloride, tantalum carbonate, tantalum nitrate and tantalum bromide; and/or
The zirconium salt is one or more selected from zirconium chloride, zirconium acid, zirconium sulfate and zirconium bromide.
10. The method of manufacturing according to claim 6, wherein: the concentration of the metal salt solution is 0.01-1M; and/or
The concentration of the persulfate solution is 0.005-0.05M; and/or
The pH of the alkaline solution is 10-13.
11. The method of manufacturing according to claim 6, wherein: the molar ratio of the metal salt to the persulfate is (1-10): 1, a step of; and/or
The mass ratio of the metal salt to the insulating material is (10-200): 1.
12. the method of manufacturing according to claim 6, wherein:
the composite material comprises mesoporous inorganic oxide particles and insulating materials filled in mesopores of the mesoporous inorganic oxide particles, wherein the mass ratio of the mesoporous inorganic oxide particles to the insulating materials is (92-97): (3-8); and/or
The average grain diameter of the insulating material is 3-30 nm; and/or
The average grain diameter of the mesoporous inorganic semiconductor particles is 20-400 nm.
13. A light emitting diode comprising a stacked anode, a light emitting layer, an electron transport layer, and a cathode, characterized in that: the electron transport layer comprises the composite material according to any one of claims 1 to 5, or the electron transport layer comprises the composite material produced by the production method according to any one of claims 6 to 12.
14. A light emitting diode according to claim 13 wherein:
the anode is selected from Ca electrode, ba electrode, ca/Al electrode, liF/Ca electrode, liF/Al electrode, baF 2 Al electrode, csF/Al electrode, caCO 3 Al electrode, baF 2 a/Ca/Al electrode, an Al electrode, a Mg electrode, an Au-to-Mg electrode or an Ag-to-Mg electrode; or alternatively
The light-emitting layer is an organic light-emitting layer or a quantum dot light-emitting layer, and the material of the organic light-emitting layer is selected from 4,4' -bis (N-carbazole) -1,1' -biphenyl, tris [2- (p-tolyl) pyridine-C2, N) iridium (III), 4' -tris (carbazole-9-yl) triphenylamine, tris [2- (p-tolyl) pyridine-C2, N) iridium, diarylanthracene derivatives, stilbene aromatic derivatives, pyrene derivatives, fluorene derivatives, blue light-emitting TBPe fluorescent material, green light-emitting TTPX fluorescent material, orange light-emitting TBRb fluorescent materialOne or more of materials and DBP fluorescent materials capable of emitting red light, wherein the material of the quantum dot luminescent layer is selected from one or more of single-structure quantum dots and core-shell structure quantum dots, the material of the single-structure quantum dots, the material of the core-shell structure quantum dots and the material of the shell of the core-shell structure quantum dots are selected from one or more of II-VI compounds, III-V compounds and I-III-VI compounds, and the II-VI compounds are selected from one or more of CdS, cdSe, cdTe, znS, znSe, znTe, znO, hgS, hgSe, hgTe, cdSeS, cdSeTe, cdSTe, znSeS, znSeTe, znSTe, hgSeS, hgSeTe, hgSTe, cdZnS, cdZnSe, cdZnTe, cdHgS, cdHgSe, cdHgTe, hgZnS, hgZnSe, hgZnTe, cdZnSeS, cdZnSeTe, cdZnSTe, cdHgSeS, cdHgSeTe, cdHgSTe, hgZnSeS, hgZnSeTe and HgZnSte; the III-V compound is one or more selected from GaN, gaP, gaAs, gaSb, alN, alP, alAs, alSb, inN, inP, inAs, inSb, gaNP, gaNAs, gaNSb, gaPAs, gaPSb, alNP, alNAs, alNSb, alPAs, alPSb, inNP, inNAs, inNSb, inPAs, inPSb, gaAlNP, gaAlNAs, gaAlNSb, gaAlPAs, gaAlPSb, gaInNP, gaInNAs, gaInNSb, gaInPAs, gaInPSb, inAlNP, inAlNAs, inAlNSb, inAlPAs and InAlPSb; the I-III-VI compound is selected from CuInS 2 、CuInSe 2 AgInS 2 One or more of the following; or alternatively
The cathode is selected from a metal oxide electrode, a doped metal oxide electrode, a metal simple substance electrode, a graphene electrode or a carbon nano tube electrode, and the material of the metal oxide electrode is selected from SnO 2 、In 2 O 3 The material of the doped metal oxide electrode is selected from one or more of indium doped tin oxide, indium doped zinc tin oxide, fluorine doped tin oxide, antimony doped tin oxide, gallium doped tin oxide, aluminum doped zinc oxide, gallium doped zinc oxide, indium doped zinc oxide, magnesium doped zinc oxide, aluminum doped magnesium oxide, cadmium doped zinc oxide and indium doped cadmium oxide, and the material of the metal simple substance electrode is selected from one or more of nickel, platinum, gold, silver and iridium.
15. A display device, characterized in that: the display device comprising the light emitting diode according to any one of claims 13 to 14.
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