CN115260502A - Preparation method of organic silicon-perovskite composite material - Google Patents
Preparation method of organic silicon-perovskite composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920002545 silicone oil Polymers 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 239000003446 ligand Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000000945 filler Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000001556 precipitation Methods 0.000 claims abstract description 3
- -1 cesium halide Chemical class 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 14
- 229910052792 caesium Inorganic materials 0.000 claims description 14
- 150000004820 halides Chemical class 0.000 claims description 14
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 11
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 11
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 11
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 11
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000005642 Oleic acid Substances 0.000 claims description 11
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 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 11
- 125000003396 thiol group Chemical class [H]S* 0.000 claims description 11
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 11
- 229920002554 vinyl polymer Polymers 0.000 claims description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims description 4
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 4
- 239000002798 polar solvent Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000004965 Silica aerogel Substances 0.000 claims description 2
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 2
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 claims description 2
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 229910021485 fumed silica Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000001723 curing Methods 0.000 abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 238000005424 photoluminescence Methods 0.000 abstract description 6
- 239000011247 coating layer Substances 0.000 abstract description 5
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000013008 moisture curing Methods 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 1
- OGFYGJDCQZJOFN-UHFFFAOYSA-N [O].[Si].[Si] Chemical compound [O].[Si].[Si] OGFYGJDCQZJOFN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- NCMHKCKGHRPLCM-UHFFFAOYSA-N caesium(1+) Chemical compound [Cs+] NCMHKCKGHRPLCM-UHFFFAOYSA-N 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
- 238000013329 compounding Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical group [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001029 thermal curing Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/14—Macromolecular compounds
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a preparation method of an organic silicon-perovskite composite material, which comprises the following steps: (1) Preparing a perovskite dispersion by adopting a ligand-assisted precipitation method; (2) Adding silicone oil and filler into the perovskite dispersion liquid in the step (1) and mixing; (3) Curing the mixture in the step (2) by ultraviolet light to obtain an organic silicon-perovskite composite material; the preparation method does not add a photoinitiator. According to the invention, perovskite is used for initiating organosilicon polymerization to form a coating layer, and the prepared organosilicon-perovskite composite material has the advantages of excellent water resistance, high stability, high photoluminescence intensity, adjustable luminescence wavelength, good weather resistance, high elasticity, good tensile property and the like.
Description
Technical Field
The invention relates to the field of preparation of fluorescent photoluminescent elastomers, in particular to a preparation method of a water-resistant fluorescent organic silicon-perovskite composite material.
Background
In recent years, perovskite materials have attracted extensive research interest due to their wide application prospects in the fields of solar photoelectric conversion, OLEDs, LEDs, and the like, but the practical applications of the materials are greatly limited due to the extreme sensitivity of the materials to water, heat, ultraviolet, and solvents.
Flexible materials have a wide range of applications, and the preparation of flexible and stretchable luminescent materials is a future trend. In order to improve the stability and maintain good stretchability, he et al prepares highly stable perovskite luminescent organogel which has excellent water-resistant function and high stretchability (adv. Mater.2019,31,1902928), but the preparation process of the method is complex and is not suitable for industrial production. In addition, researchers have prepared relatively stable luminescent perovskite-polymer composites by embedding perovskites into organic polymer gels (Nanophotonics 2018, 1949. However, the perovskite material prepared by the method has certain stability and flexibility under the condition of not too large humidity, but when the perovskite material meets water, the crystal structure of the perovskite material is damaged, so that the preparation of the perovskite flexible material with high stability and simple preparation process is a difficult point and a hot point of research on the material at present.
The organosilicon takes silicon-oxygen-silicon as a main chain, has unique physical and chemical properties, is a good packaging material, and is prepared by thermal curing or moisture curing of traditional organosilicon polymers, however, the curing methods have the following defects: (1) the curing temperature is higher; (2) longer curing time; and (3) water, oxygen and the like exist in the curing process. Research (J.Phys.D: appl.Phys.54074005) discloses that amphiphilic organosilicon copolymer is introduced into perovskite as passivator to prepare high-quality perovskite thin film with small size, high coverage rate, high defect density and enhanced photoluminescence quantum yield, but the method comprises a plurality of steps of introducing specific chain segments or groups into the synthesized hydrogen-terminated siloxane macromolecule prepolymer, and has the defects of complex preparation process and unsuitability for batch production. In addition, studies (ACS appl. Mater. Interfaces 2021,13,8138-8146) disclose the introduction of a thermally stable hydrophobic silicone resin layer with a network structure on the surface of perovskite to improve the stability of perovskite. However, the method can affect the photoluminescence performance of the perovskite material due to the introduction of the resin.
In consideration of environmental protection and energy conservation, the photocuring is gradually blended into a curing system of the organic silicon, has the characteristics of high efficiency, less pollution, simplicity, energy conservation and the like, and can avoid the risk of long moisture curing time or even no curing. However, the addition of a photoinitiator, such as CN201510996415.3, is required for the current silicone curing, which may affect the photoluminescence performance of the perovskite material to some extent.
Disclosure of Invention
The invention provides a preparation method of an organic silicon-perovskite composite material, which comprises the following steps:
(1) Preparing a perovskite dispersion by adopting a ligand-assisted precipitation method;
(2) Adding silicone oil and filler into the perovskite dispersion liquid in the step (1) and mixing to obtain a mixture;
(3) Curing the mixture in the step (2) by ultraviolet light to obtain an organic silicon-perovskite composite material;
the preparation method does not add a photoinitiator.
Specifically, the preparation method of the perovskite dispersion liquid in the step (1) comprises the following steps:
step 1) preparing a perovskite precursor by taking cesium halide, lead halide, a polar solvent and a ligand;
and 2) dropwise adding the perovskite precursor into a poor solvent until a supersaturated solution is formed, precipitating perovskite particles, centrifuging, removing a supernatant, and re-dispersing the residual solid in the poor solvent to obtain a perovskite dispersion liquid.
Specifically, the molar ratio of the lead halide to the cesium halide in the step 1) is 1:1, the lead halide is one or more of lead chloride, lead bromide and lead iodide, and the cesium halide is one or more of cesium chloride, cesium bromide and cesium iodide.
The perovskite precursor is a saturated solution.
The ligand in the step 1) is the combination of oleic acid and oleylamine, and the total addition amount of the oleic acid and the oleylamine is 4-7 times of the total mass of the lead halide and the cesium halide; preferably, 6 times; the volume ratio of the oleic acid to the oleylamine is 5-15; preferably, 10:1.
specifically, the polar solvent in the step 1) is N, N-dimethylformamide.
Specifically, the silicone oil in the step (2) is a combination of mercapto silicone oil and vinyl silicone oil;
specifically, the volume ratio of the mercapto silicone oil to the vinyl silicone oil is 1.3 to 6, preferably 2:1;
specifically, the addition amount of the mercapto silicone oil and the vinyl silicone oil is 0.5 times or more, preferably 3 times the total mass of the lead halide and the cesium halide.
Specifically, the filler in the step (2) is one or more of gas silicon and silica aerogel, preferably gas silicon, and the adding amount of the filler is 1-5% of the total mass of the lead halide and the cesium halide.
Specifically, in the organic silicon-perovskite composite material in the step (3), the perovskite nano particles account for 0.1-20% by mass; preferably, it is 0.5 to 10%, more preferably, it is 1 to 5%.
Wherein, in the step 1), the reaction formula of forming perovskite by cesium halide and lead halide is as follows:
AX+BX 2 ＝ABX 3
wherein the lead halide is BX 2 Cesium halide is AX and perovskite is ABX 3 (ii) a Wherein A is cesium ion; b is lead ion; x is a halogen ion.
Specifically, the poor solvent in step 2) is selected from one or more of acetone, butanone, pentanone, cyclohexanone, toluene, xylene, chlorobenzene, chloroform, dichloromethane and ethyl acetate, and preferably is toluene.
Specifically, the wavelength of the ultraviolet light is 365-405nm, and the curing time is 1-30 minutes.
The invention provides an organic silicon-perovskite composite material, which is formed by coating organic silicon elastomer on the surface of perovskite.
The invention has the following beneficial effects:
(1) The perovskite can generate electrons and holes under the irradiation of ultraviolet light without adding extra photoinitiators, curing agents and the like, and can be used as a photocatalyst to promote the polymerization reaction of mercapto silicone oil and vinyl silicone oil, so that an organic silicon coating layer is formed on the surface of the perovskite, and the influence of the curing agents, the photoinitiators and the like on the photoluminescence effect of the perovskite composite material is avoided;
(2) By forming the organic silicon coating layer on the surface of the perovskite, the coating layer is an elastomer, the prepared composite material is a flexible material, has high elasticity and excellent tensile property, is suitable for various occasions, and is beneficial to expanding the application range of the perovskite material;
(3) The organic silicon-perovskite composite material prepared by compounding the organic silicon with the perovskite material by utilizing the good characteristics of the organic silicon has high photoluminescence intensity and adjustable luminescence wavelength, and the perovskite organic silicon coating layer formed at the same time can ensure that the perovskite has excellent water resistance and greatly improves the stability of the perovskite material.
Drawings
Fig. 1 is a display of the organosilicon-perovskite prepared in example 1 in an unstretched state.
Fig. 2 is a graph of the effect of the organo-silicon-perovskite prepared in example 1 in a tensile state.
Fig. 3 is a graphical representation of the organosilicon-perovskite prepared in example 1 after 1 month soaking in water.
Fig. 4 is a scanning electron micrograph of the organosilicon-perovskite prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to the following specific examples and drawings, and the present invention is not limited to the following examples. Variations and advantages that may occur to those skilled in the art may be incorporated into the invention without departing from the spirit and scope of the inventive concept, and the scope of the appended claims is intended to be protected. The procedures, conditions, reagents, experimental methods and the like for carrying out the present invention are general knowledge and common general knowledge in the art, except for the contents specifically mentioned below, and the present invention is not particularly limited.
Example 1
Preparing an organic silicon-perovskite composite material:
weighing PbBr 2 And CsBr of 0.4mmol respectively are put into a glass bottle, then 10mL of N, N-Dimethylformamide (DMF) is added for ultrasonic dissolution, 1mL of oleic acid and 100ul of oleylamine are added, and magnetic stirring is carried out for 15min, so as to obtain the perovskite precursor.
Adding the perovskite precursor into 10mL of toluene, stirring for 15min, taking out a stirrer, centrifuging for 6min at 8000rpm, removing supernatant, adding 10mL of toluene, and performing ultrasonic dispersion to obtain perovskite dispersion;
taking 1mL of the perovskite dispersion, adding 2mL of mercapto silicone oil and 1mL of vinyl silicone oil, then opening an ultraviolet lamp (with the wavelength of 365 nm) for curing for 20min, and measuring the tensile property after curing.
Example 2
Preparing an organic silicon-perovskite composite material:
example 2 differs from example 1 in that the lead halide is added differently, and in example 2 the lead halide is PbCl 2 。
Example 3
Preparing an organic silicon-perovskite composite material:
example 3 differs from example 1 in that the cesium halide added in example 3 is different, and in example 3 the cesium halide is CsI.
Example 4
Preparing an organic silicon-perovskite composite material:
example 4 differs from example 1 in the ratio of oleic acid and oleylamine added, with the oleylamine and oleic acid addition volumes in example 4 being 185ul and 915ul.
Example 5
Preparing an organic silicon-perovskite composite material:
example 5 differs from example 1 in the total amount of oleic acid and oleylamine added, and the volumes of oleylamine and oleic acid added in example 4 were 57ul and 571ul, respectively.
Example 6
Preparing an organic silicon-perovskite composite material:
example 6 differs from example 1 in the ratio of mercapto silicone oil and vinyl silicone oil added, and the volumes of mercapto silicone oil and vinyl silicone oil added in example 6 are 429ul and 2571ul.
Example 7
Preparing an organic silicon-perovskite composite material:
example 7 differs from example 1 in the total amount of mercapto silicone oil and vinyl silicone oil added, 0.2mL of mercapto silicone oil and 0.1mL of vinyl silicone oil added in example 7.
Example 8
Preparing an organic silicon-perovskite composite material:
example 8 is different from example 1 in the wavelength of ultraviolet light for ultraviolet light curing, and the wavelength of ultraviolet light curing in example 8 is 405nm.
Comparative example 1
Comparative example 1 differs from example 1 in that in comparative example 1 a photoinitiator, 1-propanone, was added.
Test results for the organosilicon-perovskite composites prepared in examples 1-8:
| test item | Elongation of stretching | Luminous intensity |
| Example 1 | 400％ | 100％ |
| Example 2 | 400％ | 72％ |
| Example 3 | 400％ | 71％ |
| Example 4 | 400％ | 73％ |
| Example 5 | 400％ | 73％ |
| Example 6 | 301％ | 93％ |
| Example 7 | 220％ | 96％ |
| Example 8 | 392％ | 91％ |
| Comparative example 1 | 400％ | 30％ |
Fig. 1 illustrates that the transparency of the organosilicon-perovskite prepared by the method is better, fig. 2 illustrates that the organosilicon-perovskite prepared by the method has better tensile property and higher luminous intensity, fig. 3 further illustrates that the organosilicon-perovskite composite material prepared by the method has excellent water resistance, and fig. 4 illustrates that the surface compactness of the organosilicon-perovskite prepared by the method is better. In addition, the test results in the above table further show that the organic silicon perovskite prepared by the method of the present invention has good tensile property and good elasticity.
Claims (10)
1. A preparation method of an organic silicon-perovskite composite material is characterized by comprising the following steps:
(1) Preparing a perovskite dispersion liquid by adopting a ligand-assisted precipitation method;
(2) Adding silicone oil and filler into the perovskite dispersion liquid in the step (1) and mixing to obtain a mixture;
(3) Curing the mixture obtained in the step (2) by ultraviolet light to obtain an organic silicon-perovskite composite material;
the preparation method does not add a photoinitiator.
2. The method of preparing an organosilicon-perovskite composite material according to claim 1, wherein the perovskite dispersion in (1) is prepared by a method comprising the steps of:
step 1) preparing a perovskite precursor by taking cesium halide, lead halide, a polar solvent and a ligand;
and 2) dropwise adding the perovskite precursor into a poor solvent until a supersaturated solution is formed, precipitating perovskite particles, centrifuging, removing a supernatant, and re-dispersing the residual solid in the poor solvent to obtain a perovskite dispersion liquid.
3. The method of claim 1, wherein the filler in (2) is at least one of fumed silica and silica aerogel.
4. The method for preparing an organosilicon-perovskite composite material according to claim 1, wherein the ultraviolet light curing in the step (3) has a wavelength of 365 to 405nm and a curing time of 1 to 30 minutes.
5. The method for preparing an organosilicon-perovskite composite material according to claim 1, wherein the silicone oil in (2) is a combination of mercapto silicone oil and vinyl silicone oil, and the volume ratio of mercapto silicone oil to vinyl silicone oil is 1.3-6.
6. The method of claim 2, wherein in step 1) the molar ratio of lead halide to cesium halide is 1:1, the lead halide is at least one of lead chloride, lead bromide, and lead iodide, and the cesium halide is at least one of cesium chloride, cesium bromide, and cesium iodide.
7. The method of preparing an organosilicon-perovskite composite material according to claim 2, wherein the polar solvent in step 1) is N, N-dimethylformamide.
8. The method of claim 2, wherein the poor solvent in step 2) is selected from one or more of acetone, butanone, pentanone, cyclohexanone, toluene, xylene, chlorobenzene, chloroform, dichloromethane, and ethyl acetate.
9. The method for preparing an organosilicon-perovskite composite material as claimed in claim 2, wherein the ligand in step 1) is a combination of oleic acid and oleylamine, and the volume ratio of oleic acid to oleylamine is 5-15: 1, the sum of the addition amount of the oleic acid and the oleylamine is 4 to 7 times of the total mass of the lead halide and the cesium halide.
10. An organosilicon-perovskite composite material produced by the production method according to any one of claims 1 to 9.
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