CN114836817B - All-inorganic CsPbBr 3-x I x Single crystal and method for producing same - Google Patents
All-inorganic CsPbBr 3-x I x Single crystal and method for producing same Download PDFInfo
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- CN114836817B CN114836817B CN202210600863.7A CN202210600863A CN114836817B CN 114836817 B CN114836817 B CN 114836817B CN 202210600863 A CN202210600863 A CN 202210600863A CN 114836817 B CN114836817 B CN 114836817B
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- 239000013078 crystal Substances 0.000 title claims abstract description 67
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 50
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 48
- 239000002243 precursor Substances 0.000 claims description 39
- 239000002904 solvent Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- 239000012046 mixed solvent Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 abstract description 38
- 238000013508 migration Methods 0.000 abstract description 6
- 230000005012 migration Effects 0.000 abstract description 6
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 239000000376 reactant Substances 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 description 35
- 238000001035 drying Methods 0.000 description 23
- 238000001914 filtration Methods 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 7
- 238000001514 detection method Methods 0.000 description 5
- 238000003384 imaging method Methods 0.000 description 5
- 230000004044 response Effects 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- -1 iodide ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
- C30B7/06—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using non-aqueous solvents
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides an all-inorganic CsPbBr 3‑x I x The method is to grow all-inorganic perovskite CsPbBr with different components in low-temperature solution by adopting a heating crystallization method and adjusting parameters such as temperature, reactant proportion, solution concentration and the like in an organic solvent 3‑x I x And (3) single crystals. The preparation method overcomes the problems of low-temperature growth of perovskite single crystals with high bulk resistivity and low ion migration, and has the characteristics of short single crystal growth time, low growth temperature, low equipment requirement, relatively simple process, capability of obtaining perovskite single crystals with higher quality and the like.
Description
Technical Field
The invention belongs to the technical field of perovskite single crystal X-ray detection, and relates to an all-inorganic CsPbBr 3-x I x Single crystals and methods of making the same.
Background
The preparation of X-ray detectors with high sensitivity and low cost without breaking new materials is always an important point in the research fields of X-ray detection and imaging, and is one of the fields of preferential development and main research directions in recent years.
Current detectors based on perovskite single crystals have some problems. For example, all-inorganic perovskite CsPbBr 3 The single crystal resistivity is low, serious ion migration exists, for an X-ray detector which needs to work at a high electric field, the serious ion migration can affect the stability of the detector, and the low bulk resistivity can reduce the signal to noise ratio of the detector, and finally the sensitivity and imaging spatial resolution of the detector are reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an all-inorganic CsPbBr 3-x I x Single crystal and preparation method thereof, which solves the problems of all inorganic calcium in the prior artThe resistivity of the titanium ore monocrystal is low, and the ion migration efficiency is affected.
In order to achieve the purpose, the invention is realized by adopting the following technical scheme:
all-inorganic CsPbBr 3-x I x A method for producing a single crystal comprising the steps of:
step 1, csI and PbBr are processed 2 Adding the mixture into a solvent, and stirring and reacting to obtain a precursor solution;
step 2, placing the precursor solution into a vessel, sealing the vessel, placing the sealed vessel into a heating box, and precipitating CsPbBr in the precursor solution along with the temperature rise of the heating box 3-x I x The heating temperature of the single crystal and the heating box is 30-200 ℃.
The invention further improves that:
preferably, in step 1, csI and PbBr 2 The mixing mole ratio of x is 1.01-2.99.
Preferably, in step 1, the concentration of the precursor solution is 0.1 to 2mol/L.
Preferably, in step 1, the stirring temperature is 5 to 50 ℃.
Preferably, in step 2, the precursor solution is filtered through a filter cartridge before being placed in the vessel.
Preferably, the pore size of the filter element is 0.1-1.6 microns.
Preferably, in the step 2, the temperature rising rate is 0.1-5 ℃/h, and the temperature rising range is 30-200 ℃.
Preferably, in step 2, csPbBr is precipitated from the precursor solution 3-x I x In the single crystal process, the vessel does not vibrate.
Preferably, in the step 1, the solvent is a mixed solvent of dimethyl sulfoxide and N, N-dimethylformamide.
An all-inorganic CsPbBr prepared by any one of the above preparation methods 3-x I x And (3) single crystals.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides an all-inorganic CsPbBr 3-x I x The preparation method of monocrystal includes heating and crystallizing in organic solvent, and through regulating temperature, reactant proportion, solution concentration and other parameters, different components of all-inorganic perovskite CsPbBr are grown in low temperature solution 3-x I x And (3) single crystals. The preparation method overcomes the problems of low-temperature growth of perovskite single crystals with high bulk resistivity and low ion migration, and has the characteristics of short single crystal growth time, low growth temperature, low equipment requirement, relatively simple process, capability of obtaining perovskite single crystals with higher quality and the like.
Furthermore, the response speed of the single crystal device can be optimized by changing the proportion of iodide ions in the single crystal growth solution in the preparation process, the response speed of the single crystal device can be improved by increasing ions, the bulk resistivity of the single crystal is improved, the ion mobility in the single crystal is reduced, and the replacement of the traditional all-inorganic single crystal material for X-ray detection can be possibly realized.
Further, the stirring temperature is limited, so that all solutes can be uniformly dissolved in the solvent.
Further, the precursor solution is filtered through the filter element, impurities and undissolved solutes in the precursor solution are filtered, and the crystallization quality of the single crystal is improved.
Furthermore, the precursor solution needs to control the vessel not to vibrate in the process of separating out the single crystal, and the whole crystallization process of the single crystal is in a quiet environment to prevent the single crystal from cracking.
Further, two organic solvents are selected as the mixed solvent so that the single crystal can be precipitated from the solvent with an increase in temperature.
The invention also discloses an all-inorganic CsPbBr 3-x I x The perovskite monocrystal grown by low-temperature solution has good environmental stability, and the anion part adopts different halogens, so that the halogen has high stability, weak ion migration and improved resistivity, and meanwhile, the perovskite monocrystal has all-inorganic CsPbBr 3-x I x The atomic number of the whole single crystal is increased, and the density of the grown single crystal is higher than that of single halogen grown single crystal, thereby the single crystal is more convenient to useThe absorption capacity of X-ray shooting becomes strong, the photoelectric stability is high, and the quality and the performance of the grown crystal are high. The detector prepared based on the single crystal has extremely high light detection performance and excellent X-ray imaging performance, such as imaging resolution higher than 10lp/mm, response time shorter than us and sensitivity higher than 10 6 μC Gy air -1 cm -2 The minimum detectable dose is less than 10nGy s-1 . The all-inorganic perovskite monocrystal can be applied to the fields of high-sensitivity X-ray imaging, optical fiber communication, biomedical sensing, environment detection and the like, and is hopeful to be applied to the fields of X-ray detectors and the like which need to work under a high electric field.
Drawings
Fig. 1 is CsPbBr growth in low temperature solution 2.9 I 0.1 A schematic flow chart of the single crystal.
FIG. 2 is CsPbBr prepared in the example 2.9 I 0.1 Photo of perovskite single crystal.
FIG. 3 is CsPbBr prepared in the example 2.9 I 0.1 XRD pattern of perovskite single crystal powder.
FIG. 4 is CsPbBr prepared in the example 2.9 I 0.1 X-ray response plot of perovskite single crystal detector.
Detailed Description
The invention is described in further detail below with reference to the attached drawing figures and to specific examples:
the invention discloses a CsPbBr 3-x I x The perovskite monocrystal and low-temperature solution preparation method comprises the following steps:
(1) CsI and PbBr 2 Adding the mixture into a solvent according to a molar ratio x 1, and stirring and reacting to obtain a precursor solution, wherein the concentration of the precursor solution is 0.1-2 mol/L; stirring for 0.1-24 h at 5-50deg.C until completely dissolved to obtain clear precursor solution.
The solvent is a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF).
(2) Filtering the precursor solution by adopting a filter element with the aperture of 0.1-1.6 microns and a syringe, filtering the solution into a clean crystallization dish, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying box.
(3) Controlling the temperature of a drying box, and growing CsPbBr by adopting a temperature-rising crystallization method 3-x I x (x is more than or equal to 0.01 and less than or equal to 2.99), specifically, the temperature rising range of the drying oven is 30-200 ℃, and the temperature rising speed is 0.1-5 ℃/h.
CsPbBr prepared by the preparation method 3-x I x And (3) single crystals.
Further analysis is described below in connection with specific examples.
Example 1
(1) CsI and PbBr in a molar ratio of 0.6:1 were used 2 Adding the mixture into 100mL of mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1:1, and reacting for 24 hours under stirring at 25 ℃ to obtain clear 1.0mol/L precursor solution;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 0.8 micron and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying oven is controlled to be 65-90 ℃, the temperature is increased at the heating rate of 0.8 ℃/hour, and CsPbBr is grown 2.2 I 0.6 Perovskite single crystals.
CsPbBr growth by the temperature-rising crystallization method of this example 2.9 I 0.1 The flow chart of perovskite single crystal is shown in figure 1, and the single crystal growth temperature is adjusted according to the actual situation.
This example CsPbBr 2.9 I 0.1 A photograph of a perovskite single crystal is shown in fig. 2, and it can be seen that the single crystal has a regular shape.
This example CsPbBr 2.9 I 0.1 As shown in FIG. 3, the XRD spectrum of the perovskite single crystal only shows diffraction peaks of crystal faces such as (101), (121), (040), (202), (222), (321), (123), (242) and the like, which indicates that the three-dimensional single crystal has obvious orientation and good single crystal lattice.
This example CsPbBr 2.4 I 0.6 The response of the perovskite single crystal detector to X-rays at a bias of 40V is shown in FIG. 4, which shows that the single crystal detector is evident from the X-raysAnd (5) responding.
Example 2
(1) CsI and PbBr in a molar ratio of 0.01:1 are used 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1:1, and reacting for 24 hours under stirring at 30 ℃ to obtain a clear precursor solution of 0.1 mol/L;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 1.2 microns and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying box is controlled to be 30-200 ℃, the temperature is increased at the heating rate of 0.1 ℃/hour, and CsPbBr is grown 2.99 I 0.01 Perovskite single crystals.
Example 3
(1) CsI and PbBr in a molar ratio of 0.1:1 were used 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1:1, and reacting for 24 hours under stirring at 25 ℃ to obtain a clear precursor solution of 0.3 mol/L;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 1.6 microns and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying box is controlled to be 40-70 ℃, the temperature is increased at the heating rate of 0.5 ℃/hour, and CsPbBr is grown 2.9 I 0.1 Perovskite single crystals.
Example 4
(1) CsI and PbBr in a molar ratio of 0.2:1 were used 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1:1, and reacting for 18h under stirring at 20 ℃ to obtain a clear precursor solution of 0.5 mol/L;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 0.5 micron and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying box is controlled to be 60-100 ℃, the temperature is increased at the heating rate of 1 ℃/hour, and CsPbBr is grown 2.8 I 0.2 Calcium titaniumAnd (3) ore single crystals.
Example 5
(1) CsI and PbBr in a molar ratio of 0.3:1 were used 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1:1, and reacting for 12 hours under stirring at 15 ℃ to obtain a clear precursor solution of 0.8 mol/L;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 0.1 micron and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying box is controlled to be 30-100 ℃, the temperature is increased at the heating rate of 2 ℃/hour, and CsPbBr is grown 2.7 I 0.3 Perovskite single crystals.
Example 6
(1) CsI and PbBr in a molar ratio of 0.4:1 were used 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1:1, and reacting for 0.1h under stirring at 10 ℃ to obtain a clear 1mol/L precursor solution;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 0.3 micron and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying box is controlled to be 70-150 ℃, the temperature is increased at the heating rate of 3 ℃/hour, and CsPbBr is grown 2.6 I 0.4 Perovskite single crystals.
Example 7
(1) CsI and PbBr in a molar ratio of 0.5:1 were used 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1:1, and stirring and reacting for 10 hours at 5 ℃ to obtain a clear precursor solution of 1.2 mol/L;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 0.8 micron and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying box is controlled to be 50-200 ℃, the temperature is increased at the heating rate of 4 ℃/hour, and CsPbBr is grown 2.5 I 0.5 Perovskite single crystal。
Example 8
(1) CsI and PbBr in a molar ratio of 0.7:1 were used 2 Adding the mixture into 100mL of mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1.5:1, and stirring and reacting for 24h at 20 ℃ to obtain clear 1.5mol/L precursor solution;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 1 micron and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying box is controlled to be 120-200 ℃, the temperature is increased at the heating rate of 2.5 ℃/h, and CsPbBr is grown 2.3 I 0.7 Perovskite single crystals.
Example 9
(1) CsI and PbBr in a molar ratio of 0.9:1 were used 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1:1, and reacting for 24 hours under stirring at 30 ℃ to obtain a clear precursor solution of 1.8 mol/L;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 1.4 microns and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying box is controlled to be 30-60 ℃, the temperature is increased at the heating rate of 3.5 ℃/h, and CsPbBr is grown 2.1 I 0.9 Perovskite single crystals.
Example 10
(1) CsI and PbBr in a molar ratio of 0.99:1 were used 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the solvent ratio is 1:1, and reacting for 24 hours under stirring at 5 ℃ to obtain a clear 2mol/L precursor solution;
(2) Filtering the precursor solution into a clean crystallization dish by using a filter element with the aperture of 1.6 microns and a syringe, sealing the crystallization dish, and transferring the crystallization dish into a quiet drying oven;
(3) The temperature of the drying box is controlled to be 90-180 ℃, the temperature is increased at the temperature rising rate of 5 ℃/hour, and CsPbBr is grown 2.01 I 0.99 Perovskite single crystal。
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (6)
1. All-inorganic CsPbBr 3-x I x A method for producing a single crystal, comprising the steps of:
step 1, csI and PbBr are processed 2 Adding the mixture into a solvent, and stirring and reacting to obtain a precursor solution;
the solvent is a mixed solvent of dimethyl sulfoxide and N, N-dimethylformamide;
the concentration of the precursor solution is 0.1-2 mol/L;
step 2, placing the precursor solution into a vessel, sealing the vessel, placing the sealed vessel into a heating box, and precipitating CsPbBr in the precursor solution along with the temperature rise of the heating box 3-x I x A single crystal;
in the step 2, the heating rate is 0.1-5 ℃/h, the heating range of the heating box is 65-90 ℃, 30-200 ℃, 40-70 ℃, 60-100 ℃, 30-100 ℃, 70-150 ℃, 50-200 ℃, 120-200 ℃, 30-60 ℃ or 90-180 ℃;
in step 2, csPbBr is separated out from the precursor solution 3-x I x In the single crystal process, the vessel does not vibrate.
2. An all-inorganic CsPbBr according to claim 1 3-x I x A method for producing a single crystal, characterized in that in step 1, csI and PbBr 2 The mixing mole ratio of x is 1.01-2.99.
3. An all-inorganic CsPbBr according to claim 1 3-x I x The preparation method of the single crystal is characterized in that in the step 1, the stirring temperature is 5-50 ℃.
4. According to claim 1Is an all-inorganic CsPbBr 3-x I x The preparation method of the monocrystal is characterized in that in the step 2, the precursor solution is filtered through a filter element before being placed in a vessel.
5. An all-inorganic CsPbBr according to claim 4 3-x I x The preparation method of the monocrystal is characterized in that the pore diameter of the filter element is 0.1-1.6 microns.
6. An all-inorganic CsPbBr prepared by the preparation method of any one of claims 1 to 5 3-x I x And (3) single crystals.
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