CN106064831A - A kind of nano-particle embeds perovskite nano wire and forms the preparation method of composite - Google Patents
A kind of nano-particle embeds perovskite nano wire and forms the preparation method of composite Download PDFInfo
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- CN106064831A CN106064831A CN201610329937.2A CN201610329937A CN106064831A CN 106064831 A CN106064831 A CN 106064831A CN 201610329937 A CN201610329937 A CN 201610329937A CN 106064831 A CN106064831 A CN 106064831A
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 53
- 239000002070 nanowire Substances 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 17
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000018417 cysteine Nutrition 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 8
- -1 halogen acids Chemical class 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- QEZYDNSACGFLIC-UHFFFAOYSA-N CN.[I] Chemical compound CN.[I] QEZYDNSACGFLIC-UHFFFAOYSA-N 0.000 claims description 5
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 5
- 229940071870 hydroiodic acid Drugs 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 229940046892 lead acetate Drugs 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- GBMPPHPJKKUMPS-UHFFFAOYSA-N [Br].CN Chemical compound [Br].CN GBMPPHPJKKUMPS-UHFFFAOYSA-N 0.000 claims description 2
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 claims description 2
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 2
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims 1
- 229920002125 Sokalan® Polymers 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 claims 1
- RAJISUUPOAJLEQ-UHFFFAOYSA-N chloromethanamine Chemical compound NCCl RAJISUUPOAJLEQ-UHFFFAOYSA-N 0.000 claims 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 claims 1
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 claims 1
- 235000019260 propionic acid Nutrition 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 238000009396 hybridization Methods 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 34
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 239000007788 liquid Substances 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 6
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000002114 nanocomposite Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- KQNKJJBFUFKYFX-UHFFFAOYSA-N acetic acid;trihydrate Chemical compound O.O.O.CC(O)=O KQNKJJBFUFKYFX-UHFFFAOYSA-N 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of nano-particle and embed the preparation method of perovskite nano wire formation composite.Concrete grammar includes: first prepare pattern rule, the nano-particle of size uniformity；Then being dispersed in the aqueous solution of cysteine by pretreated nano-particle, the inorganic salt adding lead to this solution can prepare nanoparticle embedding perovskite presoma nano wire；At room temperature, add halogen acids and the mixed solution of halogen methylamine salt to presoma nano wire, ultimately form organic/inorganic hybridization material.It is ingenious that the method possesses design, and reaction condition is gentle, simple to operate, and productivity is high and is prone to the feature being prepared on a large scale, and makes the present invention have broad application prospects in preparation novel hybride field of nanometer material technology based on perovskite.
Description
Technical field
The invention belongs to material chemistry technical field, be specifically related to a kind of nano-particle and embed the preparation of perovskite nano wire
Method.
Background technology
In recent years, hybrid perovskite material caused the research enthusiasm of researcher, and nearest research worker is to system
Standby nano composite material based on perovskite creates great interest, and this possesses its composition of composition due to nano composite material
The peculiar property that single nano material does not has.
Synthesizing research field based on perovskite nano composite material, owing to perovskite material preparation condition is received with majority
The synthesis condition difference of rice grain is difficult to more greatly use " one kettle way " synthesis, and with stepwise synthesis then existing document report is all
Mode through simple physical mixing realizes, and composite two phase material as time went on prepared by this method is easy to
Separate, cause the performance being combined to be greatly attenuated, and the serious agglomeration of nano material self also makes nano material the most of the same race
When physical mixed it is difficult to ensure that the uniformity of mixing, and then greatly have impact on combined efficiency, it is impossible to really embody composite wood
The advantage of material.So the synthesis of nano composite material based on perovskite material is still a challenge at present.
Summary of the invention
It is an object of the invention to provide a kind of nano-particle and embed the preparation method of perovskite nano wire formation composite.
The method is capable of nano-particle and embeds perovskite nano wire and then form the nano composite material of integration, overcomes physics
The material split-phase problem that mixing is easily caused, it is ensured that the stability of composite life-time service, the method has simultaneously
Reaction condition is gentle, simple to operate, it is easy to the feature being prepared on a large scale.
The present invention provides a kind of nano-particle to embed perovskite nano wire and forms the preparation method of composite, technical scheme
As follows:
Step 1: prepare pattern rule, the nano-particle of size uniformity；
Step 2: nano-particle is carried out surface process；
Step 3: be dispersed in the aqueous solution of cysteine by pretreated nano-particle, adds the nothing of lead to this solution
Machine salt room temperature can prepare nano-particle embedding hybrid perovskite presoma nano wire；
Step 4: nano-particle embeds hybrid perovskite presoma nano wire at halogen acids and halogen methylamine salt
In the presence of room temperature situ converting be nano-particle embed hybrid perovskite nano wire.
Accompanying drawing explanation
Fig. 1 be the size prepared by the embodiment of the present invention 1 be the nano-particle transmission electron microscope picture of 23 nanometers.
Fig. 2 be the size prepared by the embodiment of the present invention 1 be 23 nanometers nano-particle through surface process after transmission
Electronic Speculum figure.
Fig. 3 be the size prepared by the embodiment of the present invention 1 be 23 nanometers nano-particle embed hybrid calcium titanium
The transmission electron microscope picture of ore deposit presoma nano wire.
Fig. 4 be the size prepared by the embodiment of the present invention 1 be 23 nanometers nano-particle embed hybrid calcium titanium
The transmission electron microscope picture of ore deposit nano wire.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated.These embodiments are interpreted as being merely to illustrate
The present invention rather than limit the scope of the invention.After having read the content that the present invention records, based on the present invention
Various changes or amendment that the present invention is made by principle fall into claims of the present invention limited range equally.
Embodiment 1:
Accurately weigh 50mg Polyethylene Glycol to be dissolved in 15mL chloroform, then addition 30mL is dispersed with 5mg size in this solution
It is the chloroformic solution of the nano-particle of 23 nanometers, 24h is stirred at room temperature；Add hexamethylene centrifugal receiving of modifying of Polyethylene Glycol surface
Rice grain, is scattered in this nano-particle in the 20mL deionized water dissolved with 12mg (0.1mmol) cysteine molecule, then to this
Adding the deionized water solution of the lead acetate trihydrate of the 0.1M of 1mL in solution, reaction system produces a large amount of nano-particle and embeds
Hybrid perovskite presoma nano wire, centrifugal obtain white solid, after that product is dispersed in 10mL isopropanol is molten
In liquid.Finally take the isopropanol dispersion liquid of this presoma nano wire of 1mL, be rapidly added with vigorous stirring and be dissolved with 0.5g iodine first
The 30mL aqueous isopropanol of amine and 50uL hydroiodic acid, room temperature reaction 2h, it is centrifuged and obtains hybrid composite.
Embodiment 2:
Accurately weigh 50mg polyvinylpyrrolidone to be dissolved in 15mL chloroform, then addition 30mL is dispersed with in this solution
The chloroformic solution of the nano-particle of 5mg a size of 2 nanometer, is stirred at room temperature 24h；Add hexamethylene and be centrifuged to obtain polyvinylpyrrolidone
Surface modify nano-particle, this nano-particle is scattered in 20mL dissolved with 6mg (0.05mmol) cysteine molecule go from
In sub-water, then adding the deionized water solution of the lead chloride of the 0.1M of 10mL in this solution, reaction system produces a large amount of nanometers
The hybrid perovskite presoma nano wire that granule embeds, centrifugal obtains white solid, after product is dispersed in 10mL
In aqueous isopropanol.Finally take the isopropanol dispersion liquid of this presoma nano wire of 1mL, be rapidly added with vigorous stirring and be dissolved with
0.5g iodine methylamine and 50uL hydrobromic 30mL aqueous isopropanol, room temperature reaction 2h, it is centrifuged and obtains hybrid composite wood
Material.
Embodiment 3:
Accurately weigh 50mg polymine to be dissolved in 15mL chloroform, then addition 30mL is dispersed with 5mg chi in this solution
The chloroformic solution of the very little nano-particle being 23 nanometers, is stirred at room temperature 24h；Add hexamethylene centrifugal that polymine surface is modified
Nano-particle, this nano-particle is scattered in the 20mL deionized water dissolved with 12mg (0.1mmol) cysteine molecule, then
Adding the deionized water solution of the plumbi nitras of the 0.1M of 1mL in this solution, reaction system produces what a large amount of nano-particle embedded
Hybrid perovskite presoma nano wire, centrifugal obtains white solid, after product is dispersed in 10mL aqueous isopropanol
In.Finally take the isopropanol dispersion liquid of this presoma nano wire of 1mL, be rapidly added with vigorous stirring and be dissolved with 0.5g iodine methylamine
With the 30mL aqueous isopropanol of 50uL hydroiodic acid, room temperature reaction 2h, it is centrifuged and obtains hybrid composite.
Embodiment 4:
Accurately weigh 50mg polymine to be dissolved in 15mL chloroform, then addition 30mL is dispersed with 5mg chi in this solution
The chloroformic solution of the very little nano-particle being 60 nanometers, is stirred at room temperature 24h；Add hexamethylene centrifugal that polymine surface is modified
Nano-particle, this nano-particle is scattered in the 20mL deionized water dissolved with 72mg (0.6mmol) cysteine molecule, then
Adding the deionized water solution of the lead acetate trihydrate of the 0.1M of 300 μ L in this solution, reaction system produces a large amount of nanometers
The hybrid perovskite presoma nano wire that grain embeds, centrifugal obtains white solid, after that product is dispersed in 10mL is different
In propanol solution.Finally take the isopropanol dispersion liquid of this presoma nano wire of 1mL, be rapidly added with vigorous stirring and be dissolved with
0.5g bromine methylamine and the 30mL aqueous isopropanol of 50uL hydroiodic acid, room temperature reaction 2h, it is centrifuged and obtains hybrid composite wood
Material.
Embodiment 5:
Accurately weigh 50mg Polyethylene Glycol to be dissolved in 15mL chloroform, then addition 30mL is dispersed with 5mg size in this solution
It is the chloroformic solution of the nano-particle of 23 nanometers, 24h is stirred at room temperature；Add hexamethylene centrifugal receiving of modifying of Polyethylene Glycol surface
Rice grain, is scattered in this nano-particle in the 20mL deionized water dissolved with 24mg (0.2mmol) cysteine molecule, then to this
Solution adds the deionized water solution of the lead sulfate of the 0.1M of 1mL, reaction system produce that a large amount of nano-particle embed organic/
Inorganic hybridization perovskite presoma nano wire, centrifugal obtains white solid, after product is dispersed in 10mL aqueous isopropanol.?
After take the isopropanol dispersion liquid of this presoma nano wire of 1mL, be rapidly added with vigorous stirring be dissolved with 0.5g iodine methylamine and
The 30mL aqueous isopropanol of 50uL hydroiodic acid, room temperature reaction 2h, it is centrifuged and obtains hybrid composite.
Embodiment 6:
Accurately weigh 50mg polymine to be dissolved in 15mL chloroform, then addition 30mL is dispersed with 5mg chi in this solution
The chloroformic solution of the very little nano-particle being 36 nanometers, is stirred at room temperature 24h；Add hexamethylene centrifugal that Polyethylene Glycol surface is modified
Nano-particle, is scattered in this nano-particle in the 20mL deionized water dissolved with 48mg (0.4mmol) cysteine molecule, then to
Adding the deionized water solution of the lead acetate trihydrate of the 0.1M of 1mL in this solution, it is embedding that reaction system produces a large amount of nano-particle
The hybrid perovskite presoma nano wire entered, centrifugal obtains white solid, after product is dispersed in 10mL isopropanol
In solution.Finally take the isopropanol dispersion liquid of this presoma nano wire of 1mL, be rapidly added with vigorous stirring and be dissolved with 0.5g iodine
Methylamine and the aqueous isopropanol of 50uL hydrochloric acid, room temperature reaction 2h, it is centrifuged and obtains hybrid composite.
Claims (7)
1. nano-particle embeds perovskite nano wire and forms a preparation method for composite, and it comprises the following steps: first
Prepare pattern rule, the nano-particle of size uniformity；Then nano-particle is carried out surface process；Again by surface treated
Nano-particle is dispersed in the aqueous solution of cysteine, to this solution add lead inorganic salt can room temperature to prepare nano-particle embedding
Enter hybrid perovskite presoma nano wire；Last formation organic/inorganic in the presence of halogen acids and halogen methylamine salt
Hybrid material.
A kind of nano-particle the most according to claim 1 embeds perovskite nano wire and forms the preparation method of composite,
It is characterized in that: the nanoparticle size used between 2 nanometers to 60 nanometers.
A kind of nano-particle the most according to claim 1 embeds perovskite nano wire and forms the preparation method of composite,
It is characterized in that: the reagent that nano-particle carries out surface process is polyacrylic acid (PAA), polymine (PEI), 3-sulfydryl
One in propanoic acid, polyvinylpyrrolidone (PVP) and Polyethylene Glycol (PEG).
A kind of nano-particle the most according to claim 1 embeds perovskite nano wire and forms the preparation method of composite,
It is characterized in that: the inorganic salt of the lead used is the one in plumbi nitras, lead acetate, lead chloride and lead sulfate.
A kind of nano-particle the most according to claim 1 embeds perovskite nano wire and forms the preparation method of composite,
It is characterized in that: the cysteine used changes from 20: 1 to 1 with the mol ratio of lead (II) ion: 20.
A kind of nano-particle the most according to claim 1 embeds perovskite nano wire and forms the preparation method of composite,
It is characterized in that: the halogen acids used includes the one in hydrochloric acid, hydrobromic acid and hydroiodic acid.
A kind of nano-particle the most according to claim 1 embeds perovskite nano wire and forms the preparation method of composite,
It is characterized in that: the halogen methylamine salt used includes the one in chloromethane amine, bromine methylamine and iodine methylamine.
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| CN106064831B CN106064831B (en) | 2017-11-03 |
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Cited By (4)
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| CN106809875A (en) * | 2017-03-07 | 2017-06-09 | 南京工业大学 | A kind of preparation method of perovskite-based multi-wavelength infrared electro response nano material |
| CN109306265A (en) * | 2017-07-28 | 2019-02-05 | Tcl集团股份有限公司 | Perovskite quantum dot of polymer overmold and preparation method thereof |
| CN109980095A (en) * | 2017-12-27 | 2019-07-05 | 南京工业大学 | A kind of effective perovskite film layer, device and preparation method for promoting efficiency of luminescent device |
| CN115172520A (en) * | 2022-07-08 | 2022-10-11 | 陕西师范大学 | Method for improving efficiency and stability of all-inorganic perovskite solar cell |
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| CN115172520A (en) * | 2022-07-08 | 2022-10-11 | 陕西师范大学 | Method for improving efficiency and stability of all-inorganic perovskite solar cell |
| CN115172520B (en) * | 2022-07-08 | 2023-09-22 | 陕西师范大学 | Method for improving efficiency and stability of all-inorganic perovskite solar cell |
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| CN106064831B (en) | 2017-11-03 |
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