CN113122250A - Preparation method of white-light perovskite quantum sheet - Google Patents
Preparation method of white-light perovskite quantum sheet Download PDFInfo
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- CN113122250A CN113122250A CN202110295041.8A CN202110295041A CN113122250A CN 113122250 A CN113122250 A CN 113122250A CN 202110295041 A CN202110295041 A CN 202110295041A CN 113122250 A CN113122250 A CN 113122250A
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- manganese
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000011572 manganese Substances 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- -1 salt compound Chemical class 0.000 claims abstract description 6
- 150000001412 amines Chemical class 0.000 claims abstract description 5
- 239000006184 cosolvent Substances 0.000 claims abstract description 5
- 239000002096 quantum dot Substances 0.000 claims description 11
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 7
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 7
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 7
- 239000005642 Oleic acid Substances 0.000 claims description 7
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 7
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 7
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 6
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 6
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 5
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 5
- HYZQBNDRDQEWAN-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;manganese(3+) Chemical compound [Mn+3].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O HYZQBNDRDQEWAN-LNTINUHCSA-N 0.000 claims description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 4
- IYSGJCJSRBFZSZ-UHFFFAOYSA-N carbon monoxide;manganese;5-methylcyclopenta-1,3-diene Chemical group [Mn].[O+]#[C-].[O+]#[C-].[O+]#[C-].C[C-]1C=CC=C1 IYSGJCJSRBFZSZ-UHFFFAOYSA-N 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- MTZQAGJQAFMTAQ-UHFFFAOYSA-N ethyl benzoate Chemical compound CCOC(=O)C1=CC=CC=C1 MTZQAGJQAFMTAQ-UHFFFAOYSA-N 0.000 claims description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 150000002632 lipids Chemical class 0.000 claims description 4
- 229940071125 manganese acetate Drugs 0.000 claims description 4
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical compound COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 claims description 4
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 3
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 3
- 229940057995 liquid paraffin Drugs 0.000 claims description 3
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 3
- 229960002446 octanoic acid Drugs 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 2
- RUFPHBVGCFYCNW-UHFFFAOYSA-N 1-naphthylamine Chemical compound C1=CC=C2C(N)=CC=CC2=C1 RUFPHBVGCFYCNW-UHFFFAOYSA-N 0.000 claims description 2
- OAVRWNUUOUXDFH-UHFFFAOYSA-H 2-hydroxypropane-1,2,3-tricarboxylate;manganese(2+) Chemical compound [Mn+2].[Mn+2].[Mn+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O OAVRWNUUOUXDFH-UHFFFAOYSA-H 0.000 claims description 2
- JYLNVJYYQQXNEK-UHFFFAOYSA-N 3-amino-2-(4-chlorophenyl)-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(CN)C1=CC=C(Cl)C=C1 JYLNVJYYQQXNEK-UHFFFAOYSA-N 0.000 claims description 2
- PNKUSGQVOMIXLU-UHFFFAOYSA-N Formamidine Chemical compound NC=N PNKUSGQVOMIXLU-UHFFFAOYSA-N 0.000 claims description 2
- 239000005639 Lauric acid Substances 0.000 claims description 2
- 239000005802 Mancozeb Substances 0.000 claims description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- 229910021569 Manganese fluoride Inorganic materials 0.000 claims description 2
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 2
- DEIHRWXJCZMTHF-UHFFFAOYSA-N [Mn].[CH]1C=CC=C1 Chemical compound [Mn].[CH]1C=CC=C1 DEIHRWXJCZMTHF-UHFFFAOYSA-N 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- RJYMRRJVDRJMJW-UHFFFAOYSA-L dibromomanganese Chemical compound Br[Mn]Br RJYMRRJVDRJMJW-UHFFFAOYSA-L 0.000 claims description 2
- CTNMMTCXUUFYAP-UHFFFAOYSA-L difluoromanganese Chemical compound F[Mn]F CTNMMTCXUUFYAP-UHFFFAOYSA-L 0.000 claims description 2
- NAAXGLXYRDSIRS-UHFFFAOYSA-L dihydrogen phosphate;manganese(2+) Chemical compound [Mn+2].OP(O)([O-])=O.OP(O)([O-])=O NAAXGLXYRDSIRS-UHFFFAOYSA-L 0.000 claims description 2
- QFEOTYVTTQCYAZ-UHFFFAOYSA-N dimanganese decacarbonyl Chemical group [Mn].[Mn].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] QFEOTYVTTQCYAZ-UHFFFAOYSA-N 0.000 claims description 2
- ZQHKAIDDHTYINE-UHFFFAOYSA-J disodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate;manganese(2+) Chemical compound [Na+].[Na+].[Mn+2].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O ZQHKAIDDHTYINE-UHFFFAOYSA-J 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 235000006748 manganese carbonate Nutrition 0.000 claims description 2
- 239000011656 manganese carbonate Substances 0.000 claims description 2
- 229940093474 manganese carbonate Drugs 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- 235000014872 manganese citrate Nutrition 0.000 claims description 2
- 239000011564 manganese citrate Substances 0.000 claims description 2
- 229940097206 manganese citrate Drugs 0.000 claims description 2
- 235000014012 manganese gluconate Nutrition 0.000 claims description 2
- 239000011683 manganese gluconate Substances 0.000 claims description 2
- 229940072543 manganese gluconate Drugs 0.000 claims description 2
- FLFJVPPJGJSHMF-UHFFFAOYSA-L manganese hypophosphite Chemical compound [Mn+2].[O-]P=O.[O-]P=O FLFJVPPJGJSHMF-UHFFFAOYSA-L 0.000 claims description 2
- 229940099596 manganese sulfate Drugs 0.000 claims description 2
- 235000007079 manganese sulphate Nutrition 0.000 claims description 2
- 239000011702 manganese sulphate Substances 0.000 claims description 2
- OXHQNTSSPHKCPB-IYEMJOQQSA-L manganese(2+);(2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Mn+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O OXHQNTSSPHKCPB-IYEMJOQQSA-L 0.000 claims description 2
- LSKJZEDMESDBLU-UHFFFAOYSA-L manganese(2+);6-methylheptanoate Chemical compound [Mn+2].CC(C)CCCCC([O-])=O.CC(C)CCCCC([O-])=O LSKJZEDMESDBLU-UHFFFAOYSA-L 0.000 claims description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 2
- OXOKTPUZOHPXSA-UHFFFAOYSA-L manganese(2+);n-propyl-n-[2-(2,4,6-trichlorophenoxy)ethyl]imidazole-1-carboxamide;dichloride Chemical class Cl[Mn]Cl.C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl.C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl.C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl.C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl OXOKTPUZOHPXSA-UHFFFAOYSA-L 0.000 claims description 2
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 claims description 2
- OHZZTXYKLXZFSZ-UHFFFAOYSA-I manganese(3+) 5,10,15-tris(1-methylpyridin-1-ium-4-yl)-20-(1-methylpyridin-4-ylidene)porphyrin-22-ide pentachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mn+3].C1=CN(C)C=CC1=C1C(C=C2)=NC2=C(C=2C=C[N+](C)=CC=2)C([N-]2)=CC=C2C(C=2C=C[N+](C)=CC=2)=C(C=C2)N=C2C(C=2C=C[N+](C)=CC=2)=C2N=C1C=C2 OHZZTXYKLXZFSZ-UHFFFAOYSA-I 0.000 claims description 2
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 2
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 claims description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 2
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 2
- QWYFOIJABGVEFP-UHFFFAOYSA-L manganese(ii) iodide Chemical compound [Mn+2].[I-].[I-] QWYFOIJABGVEFP-UHFFFAOYSA-L 0.000 claims description 2
- UNFXNHYYYBGDFV-UHFFFAOYSA-N manganese;pentane-2,4-dione;dihydrate Chemical compound O.O.[Mn].CC(=O)CC(C)=O.CC(=O)CC(C)=O UNFXNHYYYBGDFV-UHFFFAOYSA-N 0.000 claims description 2
- 229940095102 methyl benzoate Drugs 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 238000005191 phase separation Methods 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000000703 high-speed centrifugation Methods 0.000 abstract 1
- 229910001437 manganese ion Inorganic materials 0.000 abstract 1
- 230000005012 migration Effects 0.000 abstract 1
- 238000013508 migration Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 239000012452 mother liquor Substances 0.000 description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000005424 photoluminescence Methods 0.000 description 4
- 238000000103 photoluminescence spectrum Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
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- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000012296 anti-solvent Substances 0.000 description 2
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 2
- 229910000024 caesium carbonate Inorganic materials 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
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- 239000010413 mother solution Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000000527 sonication Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 241000155258 Plebejus glandon Species 0.000 description 1
- 235000005811 Viola adunca Nutrition 0.000 description 1
- 240000009038 Viola odorata Species 0.000 description 1
- 235000013487 Viola odorata Nutrition 0.000 description 1
- 235000002254 Viola papilionacea Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- UCAGLBKTLXCODC-UHFFFAOYSA-N carzenide Chemical compound NS(=O)(=O)C1=CC=C(C(O)=O)C=C1 UCAGLBKTLXCODC-UHFFFAOYSA-N 0.000 description 1
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- 150000004820 halides Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/664—Halogenides
- C09K11/665—Halogenides with alkali or alkaline earth metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
Abstract
The invention discloses a preparation method of a white-light perovskite quantum sheet, which comprises the following steps: firstly, dissolving a salt compound containing A, adding a cosolvent, and obtaining a precursor containing A after complete dissolution and cooling; then mixing a high-boiling-point solvent and a compound containing B and X, heating in a vacuum environment, respectively injecting an acid substance and an amine substance into the solution, simultaneously cooling, injecting the prepared precursor containing A, and cooling the solution in a water bath to terminate the reaction; separating and purifying the obtained solution by high-speed centrifugation to obtain a quantum plate solution; and further regulating the doping ratio of the quantum plate to manganese ions by using a manganese-containing compound doped quantum plate solution to obtain the white-light perovskite quantum plate. The perovskite white photon sheet prepared by the method is a single component, so that the problems of change of luminescent color, poor stability and the like caused by serious ion migration and phase separation in the multi-component perovskite are effectively solved, and the production cost is reduced.
Description
Technical Field
The invention relates to a preparation method of a perovskite quantum sheet, in particular to a preparation method of a white-light perovskite quantum sheet.
Background
The perovskite material as a new photoelectric material can be processed and prepared by a solution method, the synthesis method is simple, the cost is low, full-color light emission (380 nm-780 nm) can be realized by regulating and controlling the structure and the components thereof, and the light emission has the advantages of narrow spectrum, pure chromaticity, high light-emitting efficiency and the like. Recently, researchers have found that wide-spectrum white light emission can be realized by adopting metal-doped perovskite quantum dots, which indicates that perovskite materials have application potential and prospect as white light sources. The white light source is a surface light source, can be processed into a flexible streamline shape, and has the advantage of adjustable color temperature. The perovskite white light reported at present is generally realized by the following two ways: a. blue LED chip + red phosphor powder + green perovskite coating, b. And the process for preparing the multilayer luminescent layer is complex and the cost is high.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of a white-light perovskite quantum sheet, which can realize the white-light emission of single-component perovskite, reduce the toxicity of materials and increase the stability of the materials.
The technical scheme is as follows: the preparation method of the white-light perovskite quantum plate comprises the following steps:
(1) dissolving a salt compound containing A in a solvent, adding a cosolvent, stirring and heating, reacting until a clear solution is obtained, and cooling to room temperature to obtain a precursor containing A for later use;
(2) mixing a compound containing B and X with a solvent, heating in a vacuum environment, and keeping the temperature constant;
(3) injecting an acid substance and an amine substance into the solution after constant temperature, simultaneously cooling, injecting a precursor containing A, reacting, and cooling the solution in water bath to terminate the reaction;
(4) adding the solution after the reaction is stopped into a lipid solvent, centrifuging, dissolving the precipitate into an organic weak-polarity solvent, centrifuging again, and taking out the centrifuged supernatant to obtain a quantum tablet solution;
(5) doping quantum slice solution with manganese or manganese-containing compound to obtain white perovskite quantum slice;
wherein A is one or more of formamidine, methylamine or cesium, B is one or more of Pb, Sn, Ge or Cu, and X is one or more of Cl, Br or I.
Keeping the temperature in the step (2) for 20min-60min to remove water and oxygen in the reaction system.
Further, in the step (1), the temperature is increased to 100-140 ℃. In the step (2), the solvent is a solvent with a boiling point higher than 100-120 ℃. In the step (2), the heating temperature is 100-120 ℃. In the step (3), the temperature is reduced to 80-90 ℃. In the step (4), the lipid solvent is one or more of methyl acetate, ethyl benzoate or methyl benzoate. In the step (3), the acid is one or more of caproic acid, caprylic acid, lauric acid or oleic acid, and the amine is one or more of butylamine, octylamine, dodecylamine, hexadecylamine, octadecylamine, oleylamine, tert-butylamine, n-butylamine, aniline or naphthylamine.
In the step (2), the solvent is one or more of liquid paraffin, silicone oil or octadecene. The manganese-containing compound in the step (5) is one or more of manganese bromide, manganese chloride, manganese iodide, manganese acetate, manganese oxide, manganese tetra-p-chlorophenylporphyrin, manganese nitrate, manganese dihydrogen phosphate, manganese carbonyl, manganous oxide, cyclopentadienyl manganese tricarbonyl, manganese hypophosphite, manganese carbonate, MnTMPyP pentachloride, manganese acetate, manganese sulfate, disodium manganese ethylenediamine tetraacetate, 2-methylcyclopentadienyl manganese tricarbonyl, bis (trifluoromethanesulfonyl) manganese imine, bis (2, 4-pentanedione) manganese dihydrate, manganese acetylacetonate, sodium permanganate, manganese fluoride, manganese acetylacetonate, manganese isooctanoate, manganese citrate, mancozeb, prochloraz manganese salt, manganese gluconate or 2-methylcyclopentadienyl manganese tricarbonyl. In the step (1), the cosolvent is an acid substance.
The preparation principle is as follows: lead halide perovskite ABX3In (2), the change of A site cation, B cation and X site halide ion can cause the change of perovskite optical property, and finally influences the absorption and luminescence behavior in the whole visible spectrum. When Mn is present2+Incorporation of ABX3In middle, it will partially replace ABX3B-site ions in the crystal lattice. Excited state electrons are accessible from ABX3Transfer of conduction band to Mn2+And relaxation back to Mn in the form of optical radiation2+Thereby showing Mn2+The characteristic orange-red color emits light, producing a large stokes shift of the fluorescent emission. The quantum sheet synthesized by the invention can generate two luminescence peaks which are perovskite ABX respectively under an ultraviolet lamp3Perovskite quantum plate dominant blue light (about 470nm) and Mn2+Orange-red light (about 600nm), by adjusting Mn2+The doping proportion can realize the continuous adjustment of white light with different color temperatures and single component. In addition, Mn is advantageous for increasing the fluorescence quantum yield due to charge transfer inside the material2+Doping can effectively improve the luminous efficiency of the quantum plate.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages:
the single-component perovskite avoids the problems of ion exchange and phase separation in the multi-component perovskite, and the realization of white light of the multi-component perovskite is seriously restricted by the anion exchange and the phase separation between the perovskites; the single-component white perovskite has extremely wide luminescence spectrum, covers 430-700nm, and particularly can adjust the short-wave cut-off wavelength to more than 450nm, thereby avoiding the damage of blue-violet light to human eyes and realizing eye-protecting white light emission; the preparation scheme uses low-price manganese as an orange light source, and has rich raw materials and low cost.
Drawings
FIG. 1 is a Photoluminescence (PL) spectrum of a perovskite quantum plate of the present invention;
FIG. 2 is a CIE coordinate diagram of a perovskite quantum plate of the present invention;
FIG. 3 is a transmission electron micrograph of a perovskite quantum plate of the present invention;
FIG. 4 is a graph of PL spectra of a multicomponent perovskite over time;
FIG. 5 is a graph of the PL spectrum of a single component perovskite as a function of time.
Detailed Description
Objects, advantages and features of the present invention will be illustrated and explained by the following non-limiting description of preferred embodiments. These embodiments are merely exemplary of the technical solutions of the present invention, and any technical solution formed by replacing or converting the equivalent thereof falls within the scope of the present invention. The technical solution of the present invention is further illustrated by the following examples.
Example 1
(1) Cs-OA: 0.40g of cesium carbonate, 1mL of oleic acid and 10mL of octadecene were mixed in a three-necked flask, heated and stirred at 120 ℃ for 30min until a clear solution was obtained, and then cooled to room temperature to obtain a Cs-OA precursor.
(2) 5mL ODE and 0.069g PbBr2Mix and place in a 100mL three-neck flask. The solution was then heated to 120 ℃ and evacuated for 1h to remove water and oxygen from the reaction system.
(3) 0.5mL of OLA and 0.5mL of OA were injected into the above solution while the temperature was reduced to 90 ℃ and 0.4mL of Cs-OA was injected. After one minute of reaction, the three-necked flask was cooled in a water bath to terminate the reaction.
(4) Centrifuging the resultant solution at 15000rpm for 5min, collecting precipitate, and adding ABenzene and methyl acetate (ratio 1: 2) are purified and separated to obtain CsPbBr3Quantum plate mother liquor. The synthesis mother liquor is divided into two parts: CsPbBr3Quantum plate mother liquor of 22+Doping with excess CsPbBr3Quantum plate mother liquor.
(5) 2mL of liquid is taken respectively, and 20 mu L of mother liquor of No. I is doped into the liquid of No. II each time, so that the proportion of blue to orange-red yellow is regulated and controlled. When 160 mu L of mother solution is added, the sample emits white light, and the single-component CsPbBr is obtained3White quantum dots. As shown in fig. 1, is a Photoluminescence (PL) spectrum of a perovskite quantum plate; as shown in fig. 2, is a CIE coordinate diagram of a perovskite quantum plate; FIG. 3 shows a transmission electron micrograph of a perovskite quantum plate of the present invention. FIG. 5 shows the PL spectrum of a single-component perovskite as a function of time.
Example 2
(1) Cs-OA: 0.40g of cesium carbonate, 1mL of oleic acid and 10mL of liquid paraffin were mixed in a three-necked flask, heated and stirred at 100 ℃ for 30min until a clear solution was obtained, and then cooled to room temperature to obtain a Cs-OA precursor.
(2) 5mL ODE and 0.069g PbBr2Mix and place in a 100mL three-neck flask. Then, the solution was heated to 100 ℃ and evacuated for 1 hour to remove water and oxygen from the reaction system.
(3) 0.5mL of octylamine and 0.5mL of caprylic acid were injected into the above solution while cooling to 80 ℃ and injecting 0.4mL of Cs-OA. After one minute of reaction, the three-necked flask was cooled in a water bath to terminate the reaction.
(4) Centrifuging the synthesized solution at 15000rpm for 5min, collecting precipitate, adding toluene and methyl acetate (ratio 1: 2), purifying and separating to obtain CsPbBr3Quantum plate mother liquor. The synthesis mother liquor is divided into two parts: CsPbBr3Quantum plate mother liquor of 22+Doping with excess CsPbBr3Quantum plate mother liquor.
(5) 2mL of liquid is taken respectively, and 20 mu L of mother liquor of No. I is doped into the liquid of No. II each time, so that the proportion of blue to orange-red yellow is regulated and controlled. When 160 mu L of mother solution is added, the sample emits white light, and the single-component CsPbBr is obtained3White quantum dots.
Comparative example 1
(1) Red CsPbI3And (3) synthesis of quantum dots:
184.4mg of PbI2And 10mL of ODE were mixed in a 100mL three-necked flask, and after evacuating the system, the solution was heated to 120 ℃ and maintained for 1 hour to remove water and oxygen from the reaction system.
② preheating oleic acid, oleylamine and oleylamine iodine to 80 ℃, sequentially adding 1mL of oleic acid, oleylamine and oleylamine iodine into the three-neck flask in the step (1), and reacting for 30min at the temperature of 120 ℃.
Thirdly, the system is continuously heated to 260 ℃ and kept warm for 1 min. When the temperature is increased to 240 ℃, the temperature is difficult to rise, and N needs to be filled in the temperature2And the temperature rise is accelerated.
Fourthly, injecting 1mL of cesium oleate with the temperature of 100 ℃, cooling in a cold water bath after 1min to obtain CsPbI3Perovskite quantum dot mother liquor.
(2) Green CsPbBr3And (3) synthesis of quantum dots:
taking 36.7mg of PbBr2100. mu.L of Cs-OA was dissolved in 2mL of N, N-dimethylformamide by sonication to obtain a mixed solution.
And secondly, adding 491 mu L of oleic acid, 21 mu L of dodecylamine and 5.3mg of p-carboxylbenzenesulfonamide into the mixed solution, fully stirring, and uniformly mixing to obtain a precursor solution of the perovskite quantum dot.
③ adding 250 mu L of isopropanol into 10mL of toluene to obtain a mixed anti-solvent of isopropanol and toluene.
Fourthly, adding 250 mu L of precursor solution of perovskite quantum into the mixed anti-solvent which is stirred at high speed, and obtaining CsPbBr after mixing3Perovskite quantum dot mother liquor.
(3) Blue CsPbBr3And (3) synthesis of quantum chips:
first, 0.146g of PbBr was added28mL of ODE, 1mL of OLA and 1mL of OA are sequentially added into a 100mL three-neck flask, and N is filled after a vacuum pump exhausts for 5min2. The solution was then warmed to 120 ℃ and held for 30min until complete dissolution.
② cooling to 30 ℃, injecting 1mL Cs-OA, injecting 1mL isopropanol after 30s, then heating to 70 ℃, and reacting for 10 min.
③ the reaction was stopped by placing the three-necked flask in a water bath to cool, and the product was diluted with toluene in a 2:1 ratio.
Separating and purifying: the mother liquor was mixed with methyl acetate in a ratio of 1: 2, and taking out the precipitate after centrifugation. 1mL of toluene was added to the precipitate and dissolved by sonication. Centrifuging again, taking supernatant to obtain blue CsPbBr3Quantum tablets.
(4) Mixing red and green quantum dots and blue quantum chips in different proportion to synthesize white light.
FIG. 4 is a graph showing the change in PL spectra over time for the multicomponent perovskite of comparative example 1; compared with example 1, in comparative example 1, no matter how the proportion is changed in the practical process, ion exchange occurs after different quantum dots/sheets are mixed, and the ion exchange causes the change of the luminescent color, so that white light is difficult to generate. The luminescent color of the mixed solution is extremely unstable.
Claims (10)
1. The preparation method of the white-light perovskite quantum plate is characterized by comprising the following steps of:
(1) dissolving a salt compound containing A in a solvent, adding a cosolvent, stirring and heating, reacting until a clear solution is obtained, and cooling to room temperature to obtain a precursor containing A for later use;
(2) mixing a compound containing B and X with a solvent, heating in a vacuum environment, and keeping the temperature constant;
(3) injecting an acid substance and an amine substance into the solution after constant temperature, simultaneously cooling, injecting a precursor containing A, reacting, and cooling the solution in water bath to terminate the reaction;
(4) adding the solution after the reaction is stopped into a lipid solvent, centrifuging, dissolving the precipitate into an organic weak-polarity solvent, centrifuging again, and taking out the centrifuged supernatant to obtain a quantum tablet solution;
(5) doping quantum slice solution with manganese or manganese-containing compound to obtain white perovskite quantum slice;
wherein A is one or more of formamidine, methylamine or cesium, B is one or more of Pb, Sn, Ge or Cu, and X is one or more of Cl, Br or I.
2. The method for preparing a white-light perovskite quantum chip as claimed in claim 1, wherein in the step (1), the heating is carried out to raise the temperature to 100-140 ℃.
3. The method for preparing a white-light perovskite quantum plate as claimed in claim 1, wherein the solvent in the step (2) is a solvent having a boiling point of 100 ℃ to 120 ℃.
4. The method for preparing a white-light perovskite quantum plate as claimed in claim 1, wherein the heating temperature in the step (2) is 100 ℃ to 120 ℃.
5. The method for preparing the white-light perovskite quantum plate as claimed in claim 1, wherein in the step (3), the temperature is reduced to 80-90 ℃.
6. The method for preparing the white-light perovskite quantum tablet as claimed in claim 1, wherein the lipid solvent in the step (4) is one or more of methyl acetate, ethyl benzoate and methyl benzoate.
7. The method for preparing the white-light perovskite quantum dot according to claim 1, wherein the acid in the step (3) is one or more of caproic acid, caprylic acid, lauric acid or oleic acid, and the amine is one or more of butylamine, octylamine, dodecylamine, hexadecylamine, octadecylamine, oleylamine, tert-butylamine, n-butylamine, aniline or naphthylamine.
8. The method for preparing the white-light perovskite quantum chip as claimed in claim 1, wherein the solvent in the step (2) is one or more of liquid paraffin, silicone oil or octadecene.
9. The method of preparing a white perovskite quantum plate according to claim 1, the manganese-containing compound in the step (5) is one or more of manganese bromide, manganese chloride, manganese iodide, manganese acetate, manganese oxide, manganese tetra-p-chlorophenylporphyrin, manganese nitrate, manganese dihydrogen phosphate, manganese carbonyl, manganous oxide, cyclopentadienyl manganese tricarbonyl, manganese hypophosphite, manganese carbonate, MnTMPyP pentachloride, manganese acetate, manganese sulfate, disodium manganese ethylenediamine tetraacetate, 2-methylcyclopentadienyl manganese tricarbonyl, bis (trifluoromethanesulfonyl) manganese imine, bis (2, 4-pentanedione) manganese dihydrate, manganese acetylacetonate, sodium permanganate, manganese fluoride, manganese acetylacetonate, manganese isooctanoate, manganese citrate, mancozeb, prochloraz manganese salt, manganese gluconate or 2-methylcyclopentadienyl manganese tricarbonyl.
10. The method for preparing the white-light perovskite quantum plate as claimed in claim 1, wherein the cosolvent in the step (1) is an acid substance.
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