CN110255606A - A kind of radial full-inorganic perovskite nano material and preparation method thereof - Google Patents
A kind of radial full-inorganic perovskite nano material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of radial full-inorganic perovskite nano materials, including center and by center along the nano wire of the radial growth of two-dimensional directional；Center is made of the perovskite nano particle that multiple partial sizes are 30~80nm, and the partial size at center is 100~200nm；The diameter of nano wire is 30~80nm, and length is 2~20 μm；Its structural formula is CsPbX3, X is selected from Cl, Br or I.Preparation method, comprising: (1) cesium carbonate, oleic acid and octadecylene are mixed to get solution I；(2) lead halide, oleic acid and oleyl amine are mixed to get solution II；Volume ratio≤1:10 of oleic acid and oleyl amine；(3) solution I is mixed with solution II, sufficiently obtains radial full-inorganic perovskite material after reaction.The full-inorganic perovskite nano material with completely new pattern that the invention discloses a kind of, radial, regular appearance and uniqueness are expected to be used for the fields such as solar battery and photocatalysis.
Description
Technical field
The present invention relates to perovskite material and its preparation field more particularly to a kind of radial full-inorganic perovskite nanometer materials
Material and preparation method thereof.
Background technique
Lead halogen perovskite nano material (Lead halide perovskite nanomaterials) has width in view of it
The physical characteristics such as spectral region, high absorption coefficient, high carrier mobility, shallow defect level are shining and display device, the sun
Energy photovoltaic cell, photodetector etc. have shown tempting application prospect.
Zero dimension perovskite material is unstable, while surface defect is more, is easy to make electrons and holes in surface recombination, be unfavorable for
Electrons and holes efficiently separate.The stability and efficiently separating for electrons and holes of control for how improving perovskite material become
The direction that everybody pays close attention to, wherein a peacekeeping multidimensional perovskite material becomes a kind of feasible method.
One peacekeeping multidimensional perovskite material has carrier diffusion distance, and structural stability is good etc..One-dimensional material more has
Conducive to the generation, separation and transmission of charge, is conducive to efficiently separating for light induced electron and hole, can be widely used for solar battery
And the photoelectric fields such as LED.
Currently, the pattern of a common peacekeeping multidimensional perovskite material is mostly nanometer threadiness or nano-sheet.Such as apply for public affairs
A kind of synthetic method of inorganic perovskite nano wire is disclosed in the Chinese patent literature that cloth number is 108502918 A of CN, is wrapped
It includes: step 1, cesium carbonate being added in mixed liquor A, 15-35min is stirred at 110~160 DEG C, then naturally cools to room
Temperature forms the precursor solution of caesium；Mixed solution A is made of oleic acid and octadecylene, wherein volume ratio oleic acid: octadecylene=1:
8；In the precursor solution of caesium, the molar concentration of caesium is 0.12~0.25M；Step 2, lead bromide is added in mixed solution B,
15~35min is stirred at 90~130 DEG C, is then cooled to room temperature under water bath condition, is formed the precursor solution of lead bromide；
Mixed solution B is made of oleyl amine, oleic acid and octadecylene, wherein volume ratio oleyl amine: oleic acid: octadecylene=1:1:8, lead bromide
In precursor solution, the molar concentration of lead bromide is 0.09~0.15M；Step 3, the precursor solution of caesium is heated to 60~
It 100 DEG C, is transferred in reaction kettle after cooled to room temperature, the precursor solution of lead bromide is added, and at room temperature at ultrasound
15~35min is managed, mixed solution D is obtained；The precursor solution of volume ratio lead bromide: precursor solution=7:1~16:1 of caesium；
Step 4, by mixed solution D, 30~90h is reacted in 80~150 DEG C, obtains reactant solution E through Temperature fall；By reactant
Solution E washs after centrifugal treating, obtains final product.
A kind of perovskite nanometer sheet is disclosed in the Chinese patent literature that for another example application publication number is 109810704 A of CN
Material and its preparation method and application, the wherein preparation method of perovskite nanometer sheet material, comprising: (1) by cesium carbonate powder with
Octadecylene and oleic acid mixing are heated to 100~130 DEG C under inert gas protection and keep the temperature a period of time until cesium carbonate powder
Dissolution, rises to 140~160 DEG C of 10~60min of reaction for system temperature later, obtains oleic acid caesium presoma；By bromination iron powder
Mixed with octadecylene, oleic acid and oleyl amine, under room temperature stirring until powder dissolve, backward mixed solution in addition bromination lead powder
End is heated to 100~120 DEG C under inert gas protection and maintains a period of time until the dissolution of lead bromide powder, obtains iron lead
Mixed liquor；(2) iron lead mixed liquor is warming up to 120~140 DEG C, oleic acid caesium presoma is heated to 80~100 DEG C, later and iron
Lead mixed liquor mixes, and is insulation reaction 5s~5min at 120~140 DEG C, is centrifugated after cooling, and gained precipitating is calcium titanium
Mine nanometer sheet material.
And the perovskite nano material of different-shape have the characteristics that it is different, be expected to be applied to different application fields, because
This, it is necessary to develop the perovskite nano material of new pattern.
Summary of the invention
The full-inorganic perovskite nano material and preparation method thereof with completely new pattern that the invention discloses a kind of, should be completely without
Machine perovskite nano material is radial, regular appearance and uniqueness, is expected to improve light induced electron and diffusion length of holes, and
Its stability is improved, the fields such as solar battery and photocatalysis are widely used in.
Specific technical solution is as follows:
A kind of radial full-inorganic perovskite nano material, including center, and by center along the radial life of two-dimensional directional
Long nano wire；
The center is made of multiple perovskite nano particles, and the partial size at the center is 100~200nm, single calcium titanium
The partial size of mine nano particle is 30~80nm；
The diameter of the nano wire is 30~80nm, and length is 2~20 μm；
The quantity of the nano wire is 10~40；
The structural formula of the radial full-inorganic perovskite nano material is CsPbX3, X is selected from Cl, Br or I.
Full-inorganic perovskite nano material prepared by the present invention has radial nanowire structure, has biggish
Specific surface area is conducive to the transmission of carrier；In addition, every nano wire does not exist due in the full-inorganic perovskite nano material
Same direction, contact point only have center, and electrons and holes can be transmitted by center to all directions, and electrons and holes are not easy
It meets and compound, to improve the photoelectric properties of material.
The invention also discloses the preparation methods of the radial full-inorganic perovskite nano material, include the following steps:
(1) cesium carbonate, oleic acid are mixed with octadecylene, is heated to being completely dissolved, obtain solution I；
(2) lead halide, oleic acid are mixed with oleyl amine, is heated to being completely dissolved, obtain solution II；
Volume ratio≤1:10 of the oleic acid and oleyl amine；
(3) solution I is mixed with solution II, is heated at 150~220 DEG C, sufficiently obtained after reaction described radial
Full-inorganic perovskite material.
In the existing preparation process for preparing full-inorganic perovskite nano material, the preparation of lead halide precursor solution is mostly
Using oleic acid and oleyl amine as ligand, using octadecylene as solvent, by adjusting the proportion of oleic acid and oleyl amine, or additional halogen is selectively added
The mode of element regulates and controls the pattern of product.In the present invention, inventor is had been surprisingly found that in test, is prepared in step (2)
When lead halide precursor solution, octadecylene is not added, but (the body of oleic acid and oleyl amine when being in excess in the oleyl amine of oleic acid significantly is added
Product ratio≤1:10), the radial full-inorganic perovskite nano material with unique morphology can be prepared.At this point, oleyl amine rises
To the dual function of ligand and solvent.
In the present invention, other than the volume ratio of oleic acid and oleyl amine, in step (3), the control of reaction temperature is for product
Pattern also functions to vital effect.
It is found through experiment that when reaction temperature is controlled at 150~160 DEG C, the product being prepared, with unilateral radial calcium titanium
Based on mine structure, i.e., nano wire is by center along two-dimensional directional (along plane), the radial growth of one direction.
When reaction temperature control at 160~200 DEG C, the product being prepared, based on the radial perovskite structure of bilateral,
I.e. nano wire is by center along the radial symmetric growth of two-dimensional directional.
In step (1):
Preferably, in the solution I, the concentration of cesium carbonate is 0.05~0.1mol/L；
Preferably, the molar ratio of the cesium carbonate and oleic acid is 1:2~6.
In step (1), >=100 DEG C are heated to, is preferably heated to 110~130 DEG C.
In step (2):
In the solution II, the concentration of lead halide is 0.015~0.05mol/L.
In step (2), >=100 DEG C are heated to, is preferably heated to 110~130 DEG C.
Preferably, the volume ratio of the oleic acid and oleyl amine is 1:10~20.
In step (3):
Preferably, the volume ratio of the solution I and the solution II is 1:10~30.
Preferably, the time of the reaction be 12~for 24 hours.
Compared with prior art, the present invention has the advantage that
The present invention uses organic synthesis method, passes through the volume ratio and reaction temperature to oleic acid in preparation process and oleyl amine
Optimization, obtain a kind of unique radial full-inorganic perovskite nano material of pattern.
Detailed description of the invention
Fig. 1 is the XRD spectrum that embodiment 1 prepares product；
Fig. 2 is the SEM photograph that embodiment 1 prepares product；
Fig. 3 is the TEM photo that embodiment 1 prepares product；
Fig. 4 is the SEM photograph that comparative example 1 prepares product；
Fig. 5 is the SEM photograph that comparative example 2 prepares product；
Fig. 6 is the SEM photograph that embodiment 2 prepares product；
Fig. 7 is the SEM photograph that embodiment 5 prepares product.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
(1) under an inert atmosphere by 0.1g cesium carbonate (0.3mmol), 0.3mL (1mmol) oleic acid and 3.75mL octadecylene,
Sufficiently reaction dissolution, obtains solution I at 120 DEG C of temperature；
(2) 69mg (0.188mmol) lead bromide, 0.5mL (1.5mmol) oleic acid are mixed with 10mL (0.03mol) oleyl amine,
Under an inert atmosphere, it sufficiently dissolves at 120 DEG C of temperature, obtains solution II；
(3) II temperature of solution is increased to 160 DEG C, 0.4mL solution I is injected in solution II (10.5mL), continued anti-
It should stir；
(4) reaction solution is obtained after keeping identical constant temperature to be stirred to react 12h, is most obtained most through centrifugation, separation, washing afterwards
Final product.
Fig. 1 is the XRD spectrum that the present embodiment prepares product, and observation XRD spectrum can confirm that product group becomes CsPbBr3, from
Diffraction peak intensity judges in XRD, and mainly growing crystal face is (100) and (200).
Fig. 2 is the SEM figure that the present embodiment prepares product, as seen from the figure, obtained radial full-inorganic perovskite nanometer material
Material includes center, and by center along 20 or so nano wires of the radial symmetric growth of two-dimensional directional, medium particle diameter is
150nm or so is made of multiple perovskite nano particles, and the partial size of single perovskite nano particle is 50nm or so, single to receive
The diameter of rice noodles is 50nm or so, and unilateral length is 20 μm or so.The ingredient of the perovskite nano particle and nano wire is
CsPbBr3。
Fig. 3 is the TEM figure that the present embodiment prepares product, and You Tujian, main interplanar distance is 0.75nm, is met
CsPbBr3The interplanar distance of perovskite material (100) also illustrates that prepared radial perovskite structural material mainly grows crystalline substance
Face is (100).
Comparative example 1
(1) under an inert atmosphere by 0.1g cesium carbonate (0.3mmol), 0.3mL (1mmol) oleic acid and 3.75mL octadecylene,
Sufficiently reaction dissolution, obtains solution I at 120 DEG C of temperature；
(2) 69mg (0.188mmol) lead bromide, 0.5mL (1.5mmol) oleic acid, 0.5mL (1.5mmol) oleyl amine are dissolved in
In 5mL octadecylene, under an inert atmosphere, is sufficiently dissolved at 120 DEG C of temperature, obtain solution II；
(3) II temperature of solution is increased to 160 DEG C, 0.4mL solution I is injected in solution II, stirring that the reaction was continued；
(4) reaction solution is obtained after keeping identical constant temperature to be stirred to react 12h, is most obtained after centrifugation, separation, washing afterwards
Product.
Fig. 4 is the SEM figure that this comparative example prepares product, and as seen from the figure, the product being prepared is in large grained, partial size
It is 10~30 μm, there is no linear structure presence.
Comparative example 2
(1) under an inert atmosphere by 0.1g cesium carbonate (0.3mmol), 0.3mL (1mmol) oleic acid and 3.75mL octadecylene,
The sufficiently reaction dissolution of 120 DEG C of temperature, obtains solution I；
(2) by 69mg (0.188mmol) lead bromide, 0.5mL (1.5mmol) oleic acid and 10mL (0.03mol) oleyl amine, lazy
Property atmosphere under, the sufficiently dissolution of 120 DEG C of temperature obtains solution II；
(3) II temperature of solution is increased to 160 DEG C, 0.4mL solution I is injected in solution II, stirring that the reaction was continued；
(4) reaction solution is obtained after keeping identical constant temperature to be stirred to react 3h, is most obtained after centrifugation, separation, washing afterwards
Product.
Fig. 5 is the SEM figure that this comparative example prepares product, it can be seen from the figure that product is some little particle perovskite knots
Structure, partial size are 0.2~1 μm, and there are also a small amount of perovskite nanowire structure, length is 10 μm or so.
Embodiment 2
(1) by 0.1g (0.3mmol) cesium carbonate, 0.35mL (1.1mmol) oleic acid and 3.75mL octadecylene in inert atmosphere
Under, the sufficiently reaction dissolution of 120 DEG C of temperature obtains solution I；
(2) by 69mg (0.188mmol) lead bromide, 0.5mL (1.5mmol) oleic acid in 10mL (0.03mol) oleyl amine,
Under inert atmosphere, the sufficiently dissolution of 120 DEG C of temperature obtains solution II；
(3) II temperature of solution is increased to 150 DEG C, 0.4mL solution I is injected in solution II, stirring that the reaction was continued；
(4) reaction solution is obtained after keeping identical constant temperature to be stirred to react 12h, is most obtained after centrifugation, separation, washing afterwards
Product.
Fig. 6 is the SEM figure that the present embodiment prepares product, it can be seen from the figure that the product being prepared at 150 DEG C
CsPbBr3With unilateral radial perovskite structure, it is made of 10 or so perovskite nano wires, the diameter of single nano-wire
For 80nm or so, length is 10 μm or so.
Embodiment 3
(1) by 0.1g (0.3mmol) cesium carbonate, 0.35mL (1.1mmol) oleic acid and 3.75mL octadecylene in inert atmosphere
Under, the sufficiently reaction dissolution of 120 DEG C of temperature obtains solution I；
(2) by 69mg (0.188mmol) lead bromide, 0.5mL (1.5mmol) oleic acid in 5mL (0.015mol) oleyl amine,
Under inert atmosphere, the sufficiently dissolution of 120 DEG C of temperature obtains solution II；
(3) II temperature of solution is increased to 180 DEG C, 0.4mL solution I is injected in solution II, stirring that the reaction was continued；
(4) reaction solution is obtained after keeping identical constant temperature to be stirred to react 12h, is most obtained after centrifugation, separation, washing afterwards
Product.
After tested, the present embodiment prepares the almost the same of the pattern of product and embodiment 1.
Embodiment 4
(1) under an inert atmosphere by 0.1g (0.3mmol) cesium carbonate, 0.3mL (1mmol) oleic acid and 3.75mL octadecylene,
The sufficiently reaction dissolution of 120 DEG C of temperature, obtains solution I；
(2) by 69 (0.188mmol) mg lead bromides, 0.5mL (1.5mmol) oleic acid in 10mL (0.03mol) oleyl amine,
Under inert atmosphere, the sufficiently dissolution of 120 DEG C of temperature obtains solution II；
(3) II temperature of solution is increased to 220 DEG C, 0.4mL solution I is injected in solution II, stirring that the reaction was continued；
(4) reaction solution is obtained after keeping identical constant temperature to be stirred to react 12h, is most obtained after centrifugation, separation, washing afterwards
Product.
After tested, the present embodiment prepares the almost the same of the pattern of product and embodiment 1.
Embodiment 5
(1) by 0.1g (0.3mmol) cesium carbonate, 0.35mL (1.1mmol) oleic acid and 3.75mL octadecylene in inert atmosphere
Under, the sufficiently reaction dissolution of 120 DEG C of temperature obtains solution I；
(2) by 87mg (0.188mmol) lead iodide, 0.5mL (1.5mmol) oleic acid in 10mL (0.03mol) oleyl amine,
Under inert atmosphere, the sufficiently dissolution of 120 DEG C of temperature obtains solution II；
(3) II temperature of solution is increased to 160 DEG C, 0.4mL solution I is injected in solution II, stirring that the reaction was continued；
(4) reaction solution is obtained after keeping identical constant temperature to be stirred to react 12h, is most obtained after centrifugation, separation, washing afterwards
Product.
Fig. 7 is diluted CsPbI manufactured in the present embodiment3The SEM of radial perovskite structural material schemes, and You Tujian is obtained
It is consistent with the structure and morphology prepared in embodiment 1 to the radial perovskite structure.
Embodiment 6
(1) by 0.1g (0.3mmol) cesium carbonate, 0.35mL (1.1mmol) oleic acid and 3.75mL octadecylene in inert atmosphere
Under, the sufficiently reaction dissolution of 120 DEG C of temperature obtains solution I；
(2) by 52mg (0.188mmol) lead chloride, the positive trioctylphosphine oxide (TOPO) of 1mL, 0.5mL (1.5mmol) oleic acid in 10mL
In (0.03mol) oleyl amine, under an inert atmosphere, the sufficiently dissolution of 120 DEG C of temperature obtains solution II；
(3) II temperature of solution is increased to 160 DEG C, 0.4mL solution I is injected in solution II, stirring that the reaction was continued；
(4) reaction solution is obtained after keeping identical constant temperature to be stirred to react 12h, is most obtained after centrifugation, separation, washing afterwards
Product.
After tested, it is CsPbCl that the present embodiment, which prepares product,3, pattern is almost the same with embodiment 1.
Embodiment 7
(1) by 0.1g (0.3mmol) cesium carbonate, 0.35mL (1.1mmol) oleic acid and 3.75mL octadecylene in inert atmosphere
Under, the sufficiently reaction dissolution of 120 DEG C of temperature obtains solution I；
(2) by 69mg (0.188mmol) lead bromide, 0.5mL (1.5mmol) oleic acid in 10mL (0.03mol) oleyl amine,
Under inert atmosphere, the sufficiently dissolution of 120 DEG C of temperature obtains solution II；
(3) II temperature of solution is increased to 160 DEG C, 0.4mL solution I is injected in solution II, stirring that the reaction was continued；
(4) it keeps identical constant temperature to be stirred to react and obtains reaction solution afterwards for 24 hours, then obtained most after centrifugation, separation, washing
Final product.
After tested, the present embodiment prepares the almost the same of the pattern of product and embodiment 1.
Claims (10)
1. a kind of radial full-inorganic perovskite nano material, which is characterized in that be in along two-dimensional directional including center, and by center
The nano wire of radial growth；
The center is made of multiple perovskite nano particles, and the partial size at the center is 100~200nm, and single perovskite is received
The partial size of rice grain is 30~80nm；
The diameter of the nano wire is 30~80nm, and length is 2~20 μm；
The structural formula of the radial full-inorganic perovskite nano material is CsPbX3, X is selected from Cl, Br or I.
2. radial full-inorganic perovskite nano material according to claim 1, which is characterized in that the nano wire is in
The heart is along the radial symmetric growth of two-dimensional directional；
The quantity of the nano wire is 10~40.
3. a kind of preparation method of radial full-inorganic perovskite nano material according to claim 1 or 2, feature exist
In including the following steps:
(1) cesium carbonate, oleic acid are mixed with octadecylene, is heated to being completely dissolved, obtain solution I；
(2) lead halide, oleic acid are mixed with oleyl amine, is heated to being completely dissolved, obtain solution II；
Volume ratio≤1:10 of the oleic acid and oleyl amine；
(3) solution I is mixed with solution II, is heated at 150~220 DEG C, sufficiently obtained after reaction it is described it is radial completely without
Machine perovskite material.
4. the preparation method of radial full-inorganic perovskite nano material according to claim 3, which is characterized in that step
(1) in:
In the solution I, the concentration of cesium carbonate is 0.05~0.1mol/L；
The molar ratio of the cesium carbonate and oleic acid is 1:2~6.
5. the preparation method of radial full-inorganic perovskite nano material according to claim 3, which is characterized in that step
(1) in, >=100 DEG C are heated to.
6. the preparation method of radial full-inorganic perovskite nano material according to claim 3, which is characterized in that step
(2) in, in the solution II, the concentration of lead halide is 0.015~0.05mol/L.
7. the preparation method of radial full-inorganic perovskite nano material according to claim 3, which is characterized in that step
(2) in, >=100 DEG C are heated to.
8. the preparation method of radial full-inorganic perovskite nano material according to claim 3, which is characterized in that step
(2) in, the volume ratio of the oleic acid and oleyl amine is 1:10~20.
9. the preparation method of radial full-inorganic perovskite nano material according to claim 3, which is characterized in that step
(3) in:
The volume ratio of the solution I and the solution II is 1:10~30.
10. the preparation method of radial full-inorganic perovskite nano material according to claim 3, which is characterized in that step
Suddenly in (3), the temperature of the reaction is 160~200 DEG C, the time is 12~for 24 hours.
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| CN114751446A (en) * | 2022-05-16 | 2022-07-15 | 浙江大学 | Stepped 113 type perovskite structure and preparation method and application thereof |
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| CN112808282A (en) * | 2021-01-20 | 2021-05-18 | 河南大学 | Cesium-lead-bromine perovskite @ silicon dioxide hollow mesoporous spherical core-shell structure, and preparation method and application thereof |
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| CN114057221A (en) * | 2021-12-20 | 2022-02-18 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing flower-like lead halide cesium perovskite structure nanowire |
| CN114057221B (en) * | 2021-12-20 | 2023-06-13 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing flower-like lead halide cesium perovskite structure nanowire |
| CN114479852A (en) * | 2022-02-10 | 2022-05-13 | 黑龙江大学 | Preparation method of ultralong controllable all-inorganic bromine-lead-cesium perovskite nanowire |
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| CN114735746A (en) * | 2022-05-16 | 2022-07-12 | 浙江大学 | Micron-sized three-dimensional 416-type perovskite structure and preparation method and application thereof |
| CN114751446A (en) * | 2022-05-16 | 2022-07-15 | 浙江大学 | Stepped 113 type perovskite structure and preparation method and application thereof |
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