CN119503865A - A preparation method of perovskite nanocrystal, radiation-resistant perovskite vulcanized silicone rubber and preparation method thereof - Google Patents
A preparation method of perovskite nanocrystal, radiation-resistant perovskite vulcanized silicone rubber and preparation method thereof Download PDFInfo
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 68
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 54
- 239000002159 nanocrystal Substances 0.000 title claims description 28
- 230000005855 radiation Effects 0.000 title claims description 19
- 238000002360 preparation method Methods 0.000 title abstract description 21
- 239000003446 ligand Substances 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 9
- 239000002841 Lewis acid Substances 0.000 claims abstract description 8
- 150000007517 lewis acids Chemical class 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 7
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims abstract description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 239000006229 carbon black Substances 0.000 claims description 16
- 239000003431 cross linking reagent Substances 0.000 claims description 16
- 239000000654 additive Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- 229920001971 elastomer Polymers 0.000 claims description 14
- 239000005060 rubber Substances 0.000 claims description 13
- 230000000996 additive effect Effects 0.000 claims description 11
- -1 aminosiloxane Chemical class 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000012763 reinforcing filler Substances 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 150000004820 halides Chemical class 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 230000003471 anti-radiation Effects 0.000 claims description 2
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims description 2
- NJGCRMAPOWGWMW-UHFFFAOYSA-N octylphosphonic acid Chemical compound CCCCCCCCP(O)(O)=O NJGCRMAPOWGWMW-UHFFFAOYSA-N 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 abstract description 7
- 230000032683 aging Effects 0.000 abstract description 4
- 239000002210 silicon-based material Substances 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 238000005303 weighing Methods 0.000 description 9
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 229920013822 aminosilicone Polymers 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000003878 thermal aging Methods 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical group [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000003566 sealing material Substances 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- QWANGZFTSGZRPZ-UHFFFAOYSA-N aminomethylideneazanium;bromide Chemical compound Br.NC=N QWANGZFTSGZRPZ-UHFFFAOYSA-N 0.000 description 1
- NMVVJCLUYUWBSZ-UHFFFAOYSA-N aminomethylideneazanium;chloride Chemical compound Cl.NC=N NMVVJCLUYUWBSZ-UHFFFAOYSA-N 0.000 description 1
- QHJPGANWSLEMTI-UHFFFAOYSA-N aminomethylideneazanium;iodide Chemical compound I.NC=N QHJPGANWSLEMTI-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 description 1
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- KHDSWONFYIAAPE-UHFFFAOYSA-N silicon sulfide Chemical compound S=[Si]=S KHDSWONFYIAAPE-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
-
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/006—Compounds containing lead, with or without oxygen or hydrogen, and containing two or more other elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/34—Three-dimensional structures perovskite-type (ABO3)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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Abstract
The application discloses a preparation method of perovskite nanocrystalline, irradiation-resistant perovskite vulcanized silicone rubber and a preparation method thereof, and belongs to the technical field of organic silicon materials. The preparation method of the perovskite nanocrystalline comprises the following steps of (1) adding AX and BX 2 into a solvent A for full dissolution to obtain a mixed solution, (2) adding a ligand into the mixed solution, carrying out ultrasonic treatment until the ligand is fully dissolved to obtain a uniform precursor solution, wherein the ligand is Lewis acid and aminosilane, (3) adding the precursor solution into the solvent B for stirring reaction, and (4) centrifuging the product obtained in the step (3), wherein the obtained precipitate is ABX 3 perovskite nanocrystalline. The perovskite nanocrystalline prepared by the method can improve the irradiation resistance and the ageing resistance of the vulcanized silicone rubber, can be widely applied to the fields of aerospace, nuclear industry, chemical industry, medical protection and the like, and has good social benefit and economic benefit.
Description
Technical Field
The application relates to a preparation method of perovskite nanocrystalline, irradiation-resistant perovskite vulcanized silicone rubber and a preparation method thereof, and belongs to the technical field of organic silicon materials.
Background
With the continuous development of aerospace, medical and health and nuclear industry technologies, the requirements on the safety coefficient of equipment are also higher and higher. In order to better ensure the safety, a large amount of high polymer elastomer is used as a sealing material in a spacecraft surface material temperature control coating adhesive, and in atomic energy equipment such as wires and cables, electric instruments and the like in nuclear power and nuclear energy industries. The sealing rubber material can be seriously aged in the environment of high-energy rays, the mechanical property is seriously reduced, and immeasurable loss is caused to the life and financial safety of people. Therefore, preparing a silicone rubber sealing material with excellent irradiation resistance is critical to improving the safety and stability of the device.
In order to improve the irradiation resistance of silicone rubber, it is a common approach to use methyl phenyl silicone rubber instead of traditional dimethyl silicone rubber and to use rare earth oxide as an irradiation resistant additive. However, phenyl-containing silicone rubber is difficult to process and cure, and has poor rebound resilience and mechanical strength. Chinese patent CN101775219B discloses a radiation-resistant addition type room temperature vulcanized liquid silicone rubber and a preparation method thereof, and describes that rare earth oxide can be used for improving radiation resistance of silicone rubber. However, the compatibility of rare earth oxide and silicon rubber is poor, and more complex reaction conditions are required to improve the irradiation resistance of the silicon rubber.
Disclosure of Invention
In order to solve the problems, the application provides a preparation method of perovskite nanocrystalline, irradiation-resistant perovskite vulcanized silicone rubber and a preparation method thereof, wherein the perovskite nanocrystalline is used as an irradiation-resistant additive and the proportion of each component is limited, so that the obtained silicone rubber has excellent irradiation resistance, heat resistance, ageing resistance, excellent mechanical properties and wide application range, and meanwhile, the preparation process of the irradiation-resistant perovskite room temperature vulcanized rubber is simpler and more efficient.
According to an aspect of the present application, there is provided a method for preparing perovskite nanocrystals, comprising the steps of:
(1) Adding AX and BX 2 into a solvent to be fully dissolved to obtain a mixed solution;
(2) Adding a ligand into the mixed solution, and performing ultrasonic treatment until the ligand is fully dissolved to obtain a uniform precursor solution, wherein the ligand is Lewis acid and aminosilane;
(3) Adding the precursor solution into a solvent, and stirring for reaction;
(4) Centrifuging the product obtained in the step (3), wherein the obtained precipitate is ABX 3 perovskite nanocrystalline, the ABX 3 perovskite nanocrystalline is lead halide perovskite nanocrystalline, A is at least one of Cs +,CH3NH3 +,NH2-CH＝NH2 +, B is Pb 2+, and X is at least one of Cl -,Br-,I-.
Specifically, the solvent in the step (1) may be any solvent capable of dissolving AX and BX 2, and is preferably at least one of N, N-dimethylformamide and dimethyl sulfoxide;
Step (2) uses Lewis acid and aminosilane as ligands together, so that the stability of perovskite nanocrystals can be improved;
the solvent in the step (3) is a solvent with smaller polarity, so that the precursor solution can be precipitated and crystallized, and the solvent specifically comprises one or more of acetone, butanone, cyclohexanone, toluene, methylene dichloride, chloroform, n-hexane and ethyl acetate.
Specifically, AX is one or more of cesium chloride, cesium bromide, cesium iodide, methyl amine chloride, methyl amine bromide, methyl amine iodide, formamidine hydrochloride, formamidine hydrobromide and formamidine hydroiodide, and BX 2 is one or more of lead chloride, lead bromide and lead iodide.
Specifically, the ABX 3 perovskite nanocrystals are one or more of CsPbBr3、CsPbCl3、CsPbI3、CsPbBrXI3-X(0≤x≤3)、CsPbBrXCl3-X(0≤x≤3)、CH3NH3PbI3、CH(NH2)2PbI3、CH3NH3PbBrXI3-X(0≤x≤3).
Optionally, the molar ratio of AX to BX 2 in step (1) is 1:1.
Alternatively, the lewis acid in step (2) is one of poly (maleic anhydride-alt-1-octadecene), oleic acid or octylphosphonic acid, preferably poly (maleic anhydride-alt-1-octadecene).
Specifically, poly (maleic anhydride-alt-1-octadecene) is used as a polymer polydentate ligand, one end of the ligand is provided with a plurality of anhydrides which can coordinate with the surface of perovskite nanocrystals at the same time to play a good role in stabilizing and passivating defects, the octadecene long chain at the other end is used as a hydrophobic carbon chain to effectively prevent the damage of water in the environment to the perovskite nanocrystals, and meanwhile, poly (maleic anhydride-alt-1-octadecene) can also enhance the effective adhesion of aminopropyl triethoxysilane on the surface of the perovskite nanocrystals to play a good synergistic effect.
Optionally, aminosiloxane refers to a siloxane compound with a-NH 2 group, and the amino group can repair halogen vacancies to improve the photostability of perovskite nanocrystals;
The aminosilicone is selected from the group consisting of aminopropyl triethoxysilane, 3-aminopropyl trimethoxysilane, N-aminoethyl-3-aminopropyl triethoxysilane, preferably aminopropyl triethoxysilane; the amino siloxane can enable the surface of the perovskite nanocrystalline to have a large number of silica groups, endow the perovskite nanocrystalline with functionality, and the perovskite nanocrystalline is used in silicon rubber, and the silica groups on the surface of the perovskite nanocrystalline are subjected to hydrolytic condensation with a cross-linked network of the silicon rubber to form a three-dimensional cross-linked network, so that the compatibility of the perovskite nanocrystalline and the silicon rubber is improved, the dispersibility of the perovskite nanocrystalline is increased, the overall performance of the material is more uniform, and the radiation resistance and the thermal aging resistance of the overall material are improved.
Optionally, the mass ratio of the Lewis acid to the aminosilicone is 1 (1-20).
Specifically, if the aminosilicone is too small, the compatibility of the obtained nanocrystal and the silicone rubber is poor, and if the aminosilicone is too large, the crystal structure of the perovskite is damaged, so that the irradiation resistance of the silicone rubber is affected.
The mass ratio of the total amount of AX and BX 2 to the total amount of ligand is 1 (1-20), preferably 1 (8-14);
Specifically, too small a ligand amount may cause defects on the perovskite surface to be poorly passivated and to be deliquesced more easily in air, so that stability may be poor and compatibility with silicone rubber may be poor, and if too much ligand amount, a thicker organic layer may be formed, resulting in uneven particle size of nanocrystals affecting irradiation resistance.
Optionally, the time of the ultrasonic treatment in the step (2) is 2-20 minutes.
Optionally, the stirring process in the step (3) is carried out for 5-15 minutes under the condition of the rotating speed of 300-1000 rpm.
The stirring process of the step (3) is rapid stirring, and after the precursor solution is added into the solvent, perovskite nanocrystals can be immediately separated out and crystallized to obtain the perovskite nanocrystals, and the rapid stirring is beneficial to obtaining the perovskite nanocrystals with more uniform particle size, and meanwhile, the probability of agglomeration of the perovskite nanocrystals is reduced.
The too short reaction time leads to less number of silicon ethoxy groups on the surface of the perovskite nanocrystalline and reduces the compatibility with silicon rubber, and the too long reaction time leads to the too large growth of the perovskite nanocrystalline and uneven grain size.
Optionally, the centrifugation in the step (4) is performed at a rotational speed of 500-15000 rpm for 2-30 minutes by a high-speed centrifuge.
According to a further aspect of the present application, there is provided an irradiation-resistant perovskite vulcanized silicone rubber prepared from the following components:
100 parts of base adhesive, 2-60 parts of radiation-resistant additive, 10-60 parts of reinforcing filler, 1-10 parts of cross-linking agent and 0.2-5 parts of catalyst;
The radiation-resistant additive is ABX 3 perovskite nanocrystalline prepared by the method.
Optionally, the cross-linking agent is a silane coupling agent containing at least three siloxy groups;
Specifically, the cross-linking agent is at least one of tetraethyl silicate, polyethyl silicate or methyltriethoxysilane, and preferably tetraethyl silicate.
The silicon oxygen group of the cross-linking agent and the silicon oxygen group on the surface of the perovskite nanocrystalline are condensed with the hydroxyl in the base rubber under the action of a catalyst to generate a silicon oxygen bond (Si-O-Si), ethanol is removed, and a cross-linking network is formed along with the progress of the reaction, so that the system is solidified, and the silicon rubber is obtained.
Optionally, the reinforcing filler is at least one of white carbon black, carbon black and calcium carbonate, preferably the reinforcing filler is white carbon black, the average particle size of the white carbon black is 10-30 nanometers, and the specific surface area is 70-320 m 2/g,SiO2, and the content of the white carbon black is not less than 99.8%.
Specifically, the reinforcing filler white carbon black is preferably gas phase white carbon black, if the amount of the white carbon black is too large, the hardness of the silicone rubber becomes poor, the elasticity becomes poor, if the amount of the white carbon black is too small, the mechanical strength becomes too low, the ideal reinforcing effect cannot be achieved, the amount of the cross-linking agent is too large, the brittleness becomes hard, the elasticity becomes low, the mechanical property of the rubber is poor, if the amount of the cross-linking agent is too small, the vulcanization rate becomes too high, the aging resistance of the silicone rubber is affected, and if the amount of the cross-linking agent is too small, the rubber cannot be vulcanized.
Too few radiation-resistant additives can lead to poor improvement of radiation resistance and thermal aging resistance of the silicone rubber, too many radiation-resistant additives can lead to agglomeration of the radiation-resistant additives in the silicone rubber, and can also reduce the dispersibility of the white carbon black, thereby influencing the mechanical properties of the silicone rubber. In addition, as the surface of the radiation-resistant additive contains the silicon ethoxy group, the dispersibility of the white carbon black in the base rubber can be improved, so that the radiation-resistant additive and the white carbon black are uniformly dispersed in the base rubber, and the silicon rubber with better performance is obtained under the crosslinking action of the crosslinking agent.
Optionally, the base gum is hydroxyl terminated polysiloxane with a molecular weight of 5000-30000.
Specifically, the base gum is one of alpha, omega-dihydroxypolydimethylsiloxane, alpha, omega-dihydroxypoly (dimethyl, diphenyl) siloxane, alpha, omega-dihydroxypoly (dimethyl, methylphenyl) siloxane and alpha, omega-dihydroxypolymethyltrifluoropropyl siloxane. The base rubber contains dihydroxyl groups, and can react with a cross-linking agent under the action of a catalyst, and after dealcoholization, the base rubber is hydrolyzed and condensed to form a cross-linked network.
Optionally, the catalyst is at least one of dibutyl tin dilaurate or stannous octoate, preferably dibutyl tin dilaurate, and is used for catalyzing hydroxyl groups in the base rubber and a cross-linking agent to perform condensation cross-linking reaction, so as to remove small molecular ethanol and form dealcoholized room temperature vulcanized silicone rubber.
According to still another aspect of the present application, there is provided a method for preparing the silicone rubber as described above, comprising the steps of:
(1) Fully mixing the base adhesive, the anti-radiation additive and the reinforcing filler, wherein the mixing process is carried out in a three-dimensional mixer;
(2) Adding a cross-linking agent and a catalyst into the mixture in the step (1), and uniformly mixing to obtain a silicone rubber base material;
(3) Pouring the silicon rubber base material into a polytetrafluoroethylene mould for vulcanization, and obtaining the irradiation-resistant perovskite vulcanized silicon rubber.
The beneficial effects that can be produced by the present application include, but are not limited to:
1. The irradiation-resistant perovskite vulcanized silicone rubber provided by the application uses the perovskite nanocrystalline as an irradiation-resistant additive of the vulcanized silicone rubber, has good absorption effect on high-energy rays, and converts the high-energy rays into visible light to be emitted, so that the silicone rubber has excellent irradiation resistance and thermal aging resistance, and the perovskite nanocrystalline is used as the irradiation-resistant additive of the vulcanized silicone rubber, so that the preparation process of the vulcanized silicone rubber is simpler and more efficient.
2. According to the irradiation-resistant perovskite vulcanized silicone rubber provided by the application, aminopropyl triethoxysilane is used as a ligand to prepare perovskite nanocrystals, a large amount of silicon ethoxy groups are arranged on the surface of the obtained perovskite nanocrystals, the silicon ethoxy groups on the surface of the perovskite, the silicon oxy groups of the cross-linking agent and the hydroxyl groups in the base rubber are subjected to condensation reaction under the action of a catalyst to generate silicon-oxygen-silicon bonds (Si-O-Si), ethanol is removed, and a cross-linked network is formed along with the progress of the reaction, so that a system is solidified, and the perovskite nanocrystals and the silicon rubber have better compatibility, so that the prepared vulcanized silicone rubber is more uniform, and the irradiation resistance and the heat-aging resistance of the whole material are improved.
3. According to the irradiation-resistant perovskite vulcanized silicone rubber provided by the application, the ratio between the halides AX and BX 2 and the ligand is limited, so that the obtained perovskite nanocrystalline can keep good stability, meanwhile, the compatibility of the nanocrystalline and the silicone rubber is improved, and the nanocrystalline is distributed more uniformly in the silicone rubber, so that the irradiation-resistant performance of the silicone rubber is better.
4. According to the irradiation-resistant perovskite vulcanized silicone rubber provided by the application, the proportion of the white carbon black and the cross-linking agent in the material components is limited, so that the tensile strength change, the elongation at break and the hardness of the vulcanized silicone rubber before and after irradiation are improved, and the irradiation-resistant ageing resistance of the obtained vulcanized silicone rubber material is more excellent.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application. In the drawings:
fig. 1 is an XRD diffractogram of the perovskite nanocrystals prepared according to example 1 of the present application.
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. The reagents or materials used in the present invention may be purchased in conventional manners, and unless otherwise indicated, they may be used in conventional manners in the art or according to the product specifications. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred methods and materials described in this patent are illustrative only.
The molecular weight of poly (maleic anhydride-alt-1-octadecene) used in the following examples was 1370-3650 and the average molecular weight was 1980.
Example 1
The preparation method of the perovskite nanocrystalline comprises the following steps:
(1) Adding AX and BX 2 into the solvent A for fully dissolving to obtain a mixed solution;
(2) Adding a ligand into the mixed solution, and performing ultrasonic treatment until the ligand is fully dissolved to obtain a uniform precursor solution;
(3) Adding the precursor solution into the solvent B, and stirring for reaction;
(4) And (3) centrifuging the product obtained in the step (3), wherein the obtained precipitate is ABX 3 perovskite nanocrystalline.
The perovskite nanocrystalline 1# -10# and D1# -D8# are prepared according to the preparation method, and specifically are as follows:
perovskite nanocrystalline 1#
(1) Weighing 0.4mmol of CsBr and 0.4mmol of PbBr 2, placing in a beaker, and weighing 10mL of N, N-Dimethylformamide (DMF) into the beaker to completely dissolve the solute;
(2) Weighing 0.2g of poly (maleic anhydride-alt-1-octadecene) and 2g of aminopropyl triethoxysilane into a beaker in the step (1), and carrying out ultrasonic treatment for 10 minutes to fully mix and dissolve the poly (maleic anhydride-alt-1-octadecene) and the aminopropyl triethoxysilane to obtain a uniform precursor solution;
(3) 1mL of the precursor solution is added into toluene solution with the stirring speed of 600 revolutions per minute, and the mixture is stirred for 10 minutes to obtain bright green solution;
(4) Centrifuging the product obtained in the step (3) at a rotating speed of 10000 revolutions per minute by a high-speed centrifuge for 10 minutes, discarding the supernatant, and collecting the precipitate to obtain the CsPbBr 3 perovskite nanocrystalline.
XRD characterization is carried out on perovskite nanocrystalline 1# and the characterization result is shown in figure 1.
The XRD spectrum can show that the diffraction peak of the perovskite nanocrystalline can be well corresponding to a standard card, and no impurity phase appears, thus indicating that the pure-phase perovskite nanocrystalline is prepared.
Perovskite nanocrystalline 2#
(1) Weighing 0.4mmol of CsBr and 0.4mmol of PbBr 2, placing in a beaker, and weighing 10mL of N, N-Dimethylformamide (DMF) into the beaker to completely dissolve the solute;
(2) Weighing 0.2g of poly (maleic anhydride-alt-1-octadecene) and 2g of aminopropyl triethoxysilane into a beaker in the step (1), and carrying out ultrasonic treatment for 2 minutes to fully mix and dissolve the poly (maleic anhydride-alt-1-octadecene) and the aminopropyl triethoxysilane to obtain a uniform precursor solution;
(3) 1mL of the precursor solution is added into toluene solution with the stirring speed of 300 revolutions per minute, and the mixture is stirred for 15 minutes to obtain bright green solution;
(4) Centrifuging the product obtained in the step (3) for 30 minutes at a rotation speed of 500 revolutions per minute by a high-speed centrifuge, discarding the supernatant, and collecting the precipitate to obtain the CsPbBr 3 perovskite nanocrystalline.
Perovskite nanocrystalline 3#
(1) Weighing 0.4mmol of CsBr and 0.4mmol of PbBr 2, placing in a beaker, and weighing 10mL of N, N-Dimethylformamide (DMF) into the beaker to completely dissolve the solute;
(2) Weighing 0.2g of poly (maleic anhydride-alt-1-octadecene) and 2g of aminopropyl triethoxysilane into a beaker in the step (1), and carrying out ultrasonic treatment for 20 minutes to fully mix and dissolve the poly (maleic anhydride-alt-1-octadecene) and the aminopropyl triethoxysilane to obtain a uniform precursor solution;
(3) 1mL of precursor solution is added into toluene solution with the stirring speed of 1000 revolutions per minute, and the mixture is stirred for 5 minutes to obtain bright green solution;
(4) And (3) centrifuging the product obtained in the step (3) by a high-speed centrifuge at a rotation speed of 15000 rpm for 2 minutes, discarding the supernatant, and collecting the precipitate to obtain the CsPbBr 3 perovskite nanocrystalline.
Perovskite nanocrystalline 4#
The difference from perovskite nanocrystalline 1# is that AX, BX 2 are CsCl, pbCl 2, respectively, and the remainder are the same as perovskite nanocrystalline 1 #.
Perovskite nanocrystalline 5#
Compared with perovskite nanocrystalline 1#, the difference is that AX and BX 2 are CsI and PbI 2 respectively, and the rest is the same as perovskite nanocrystalline 1 #.
Perovskite nanocrystalline 6#
The difference compared to perovskite nanocrystalline 1# is that AX is CH 3NH3 Br, and 0.2g of poly (maleic anhydride-alt-1-octadecene) and 2g of aminopropyl triethoxysilane are substituted for 0.6g of poly (maleic anhydride-alt-1-octadecene) and 6g of aminopropyl triethoxysilane, the remainder being identical to perovskite nanocrystalline 1 #.
Perovskite nanocrystalline 7#
The difference compared to perovskite nanocrystalline 1# is that AX is CH (NH 2)2 Br, ligand 0.2g poly (maleic anhydride-alt-1-octadecene) and 2g aminopropyl triethoxysilane are replaced with 0.1g poly (maleic anhydride-alt-1-octadecene) and 2.5g aminopropyl triethoxysilane, the remainder being the same as perovskite nanocrystalline 1 #.
Perovskite nanocrystalline 8#
The difference compared to perovskite nanocrystalline 1# is that 0.2g of the ligand poly (maleic anhydride-alt-1-octadecene) and 2g of aminopropyl triethoxysilane are replaced with 1.5g of poly (maleic anhydride-alt-1-octadecene) and 0.7g of aminopropyl triethoxysilane, the remainder being identical to perovskite nanocrystalline 1 #.
Perovskite nanocrystalline 9#
The difference is that the ligand aminopropyl triethoxysilane is 3-aminopropyl trimethoxysilane compared with perovskite nanocrystalline 1# and the rest is the same as perovskite nanocrystalline 1 #.
Perovskite nanocrystalline 10#
The difference compared to perovskite nanocrystalline 1# is that the ligand poly (maleic anhydride-alt-1-octadecene) is oleic acid, the remainder being the same as perovskite nanocrystalline 1 #.
Perovskite nanocrystalline D1#, and preparation method thereof
The difference compared with perovskite nanocrystalline 1# is that no aminopropyl triethoxysilane ligand is contained, only poly (maleic anhydride-alt-1-octadecene) ligand is contained, and the rest is the same as perovskite nanocrystalline 1 #.
Perovskite nanocrystalline D2#, and preparation method thereof
The difference compared to perovskite nanocrystalline 1# is that poly (maleic anhydride-alt-1-octadecene) ligand is not contained, only aminopropyl triethoxysilane ligand is present, and the remainder is identical to perovskite nanocrystalline 1 #.
Example 2
The preparation method of the vulcanized silicone rubber No. 1 comprises the following steps:
(1) Adding 100 parts of alpha, omega-dihydroxypolydimethylsiloxane (molecular weight 10000), 1#10 parts of perovskite nanocrystalline and 30 parts of fumed silica into a mixing box, and fully mixing in a three-dimensional mixer;
(2) Adding 3 parts of ethyl orthosilicate and 1.5 parts of dibutyl tin dilaurate into a mixing box, and uniformly mixing again;
(3) Pouring the mixed raw materials in the step (2) into a polytetrafluoroethylene mould, and vulcanizing at room temperature to obtain vulcanized silicone rubber No. 1.
The following vulcanized silicone rubbers 2# -11# and d1# -d7# were prepared according to the same preparation method as the vulcanized silicone rubber 1#, with the specific differences shown in table 1:
table 1 silicon sulfide rubber material proportion (parts by weight)
The newly added 11# adopts calcium carbonate reinforcing filler, and the rest components are the same as the 1# vulcanized silicone rubber.
The vulcanizing time of the silicone rubber is approximately within 12-72 hours, so long as the vulcanizing of the silicone rubber can be completed.
Experimental example
Performance test of the vulcanized silicone rubber product with irradiation resistance obtained in example 2 above:
1. Irradiation performance
The irradiation source is Co 60-gamma ray irradiation, the total irradiation dose of the sample is 500Kgy in the air, and the irradiation dose rate is 30Gy/min.
2. Mechanical property test
Tensile strength and elongation as per GB/T528-1998, and hardness as per GB/T531-1999.
The results are shown in Table 2.
TABLE 2 irradiation resistance of irradiation-resistant vulcanized silicone rubber
From the results, the silicon rubber obtained by the formula and the preparation method provided by the application has smaller changes in tensile strength, elongation at break and hardness before and after irradiation, and has better mechanical property and excellent irradiation resistance after irradiation.
In this specification, each embodiment is described in a progressive manner, and identical and similar parts of each embodiment are all referred to each other, and each embodiment mainly describes differences from other embodiments. In particular, for system embodiments, since they are substantially similar to method embodiments, the description is relatively simple, as relevant to see a section of the description of method embodiments.
The foregoing is merely exemplary of the present application and is not intended to limit the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the application are to be included in the scope of the claims of the present application.
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