CN114836817A - All-inorganic CsPbBr 3-x I x Single crystal and method for producing the same - Google Patents
All-inorganic CsPbBr 3-x I x Single crystal and method for producing the same Download PDFInfo
- Publication number
- CN114836817A CN114836817A CN202210600863.7A CN202210600863A CN114836817A CN 114836817 A CN114836817 A CN 114836817A CN 202210600863 A CN202210600863 A CN 202210600863A CN 114836817 A CN114836817 A CN 114836817A
- Authority
- CN
- China
- Prior art keywords
- single crystal
- cspbbr
- precursor solution
- inorganic
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 81
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- 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 40
- 239000002904 solvent Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- 239000012046 mixed solvent Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000013508 migration Methods 0.000 abstract description 5
- 230000005012 migration Effects 0.000 abstract description 5
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 239000000376 reactant Substances 0.000 abstract description 2
- -1 regulating temp Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 40
- 238000001035 drying Methods 0.000 description 23
- 238000001914 filtration Methods 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 230000004044 response Effects 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000003384 imaging method Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 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
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011259 mixed solution Substances 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
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- 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 A single crystal and its preparing process includes such steps as heating for crystallizing in organic solvent, regulating temp, reactant ratio and solution concentration to grow different components of inorganic perovskite CsPbBr in low-temp solution 3‑x I x And (3) single crystal. The preparation method overcomes the problems of high bulk resistivity and low ion migration perovskite single crystal growth at low temperature in the prior art, and has the characteristics of short single crystal growth time, low growth temperature, low equipment requirement, relatively simple process, capability of obtaining high-quality perovskite single crystal 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 A single crystal and a method for producing the same.
Background
The continuous development of new materials to obtain high sensitivity and low cost for preparing the X-ray detector has been the focus of the research field of X-ray detection and imaging, and is one of the prior development field and main research direction in recent years.
There are several problems with current perovskite single crystal based detectors. For example, fully inorganic perovskites CsPbBr 3 The resistivity of the single crystal is low, and serious ion migration exists, so that the demand is highFor an X-ray detector to work in a high electric field, severe ion migration affects the stability of the detector, and low volume resistivity reduces the signal-to-noise ratio of the detector, and finally reduces the sensitivity and the imaging spatial resolution of the detector.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an all-inorganic CsPbBr 3-x I x A single crystal and a preparation method thereof are used for solving the problems that the resistivity of an all-inorganic perovskite single crystal is low and the ion transfer efficiency is influenced in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
all-inorganic CsPbBr 3-x I x A method for producing a single crystal, comprising the steps of:
The invention is further improved in that:
preferably, in step 1, CsI and PbBr 2 The mixing molar ratio of x to 1, x is more than or equal to 0.01 and less than or equal to 2.99.
Preferably, in the step 1, the concentration of the precursor solution is 0.1-2 mol/L.
Preferably, in the step 1, the stirring temperature is 5-50 ℃.
Preferably, in step 2, the precursor solution is filtered through a filter element before being placed in the vessel.
Preferably, the pore size of the filter element is 0.1 to 1.6 microns.
Preferably, in the step 2, the heating rate is 0.1-5 ℃/h, and the heating range is 30-200 ℃.
Preferably, in step 2, CsPbBr is precipitated from the precursor solution 3-x I x In the process of single crystal, the vessel is not vibratedAnd (6) moving.
Preferably, in step 1, the solvent is a mixed solvent of dimethyl sulfoxide and N, N-dimethylformamide.
All-inorganic CsPbBr prepared by any one of the preparation methods 3-x I x And (3) single crystal.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides an all-inorganic CsPbBr 3-x I x A process for preparing single crystal features that the full-inorganic perovskite CsPbBr with different components is grown in low-temp solution by heating crystallization in organic solvent and regulating temp, reactant ratio and solution concentration 3-x I x And (3) single crystal. The preparation method overcomes the problems of high bulk resistivity and low ion migration perovskite single crystal growth at low temperature in the prior art, and has the characteristics of short single crystal growth time, low growth temperature, low equipment requirement, relatively simple process, capability of obtaining high-quality perovskite single crystal 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 increase of the ions can improve the response speed of the single crystal device, improve the volume resistivity of the single crystal and reduce the ion mobility in the single crystal, and the substitution of the traditional all-inorganic single crystal material for X-ray detection can be realized.
Further, the stirring temperature is limited, and all solutes can be uniformly dissolved in the solvent.
Furthermore, the precursor solution is filtered through the filter element, impurities and undissolved solute in the precursor solution are filtered, and the crystallization quality of the single crystal is improved.
Furthermore, in the process of precipitating the single crystal from the precursor solution, the vessel needs to be controlled not to vibrate, and the whole crystallization process of the single crystal is in a quiet environment, so that the crystallized single crystal is prevented from cracking.
Further, two organic solvents are selected as the mixed solvent so that a 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 single crystal, perovskite single crystal grown by low temperature solution, has good environmental stability, because the anion part adopts different halogen, the halogen stability is high, the ion migration is weak, the resistivity is improved, and simultaneously the all-inorganic CsPbBr crystal is prepared 3-x I x The integral atomic number of the single crystal is increased, the density of the grown single crystal is higher than that of the single halogen grown single crystal, the absorption capacity of X-ray photography is enhanced, the photoelectric stability is high, and the grown crystal has high quality and excellent performance. 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 lowest detectable dose is less than 10nGy s-1 . The all-inorganic perovskite single crystal can be applied to the fields of high-sensitivity X-ray imaging, optical fiber communication, biomedical sensing, environmental detection and the like, and is expected 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 growth of CsPbBr in a cryogenic solution 2.9 I 0.1 Schematic flow diagram of single crystal.
FIG. 2 is CsPbBr prepared in example 2.9 I 0.1 Photographs of perovskite single crystals.
FIG. 3 is CsPbBr prepared in example 2.9 I 0.1 XRD pattern of perovskite single crystal powder.
FIG. 4 is CsPbBr prepared in example 2.9 I 0.1 X-ray response diagram of perovskite single crystal detector.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
the invention discloses CsPbBr 3-x I x The preparation method of the perovskite single crystal and the low-temperature solution comprises the following steps:
(1) mixing CsI and PbBr 2 Adding the mixture into a solvent according to a molar ratio x:1, and stirringStirring 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 5-50 ℃, and stirring until the precursor is completely dissolved to obtain a 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 crystallizing dish, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box.
(3) Controlling the temperature of the drying oven, and growing CsPbBr by heating crystallization 3-x I x (x is more than or equal to 0.01 and less than or equal to 2.99), and specifically, the temperature rise range of the drying oven is 30-200 ℃, and the temperature rise speed is 0.1-5 ℃/h.
CsPbBr prepared by the preparation method 3-x I x And (3) single crystal.
Further analysis is described below in connection with specific examples.
Example 1
(1) Mixing CsI and PbBr at a molar ratio of 0.6:1 2 Adding the mixture into 100mL of mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the ratio of the solvent is 1:1, and reacting for 24 hours at the temperature of 25 ℃ under stirring to obtain clear 1.0mol/L precursor solution;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 0.8 micron and a syringe, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box;
(3) controlling the temperature of the drying oven to be 65-90 ℃, increasing the temperature at a heating rate of 0.8 ℃/hour, and growing CsPbBr 2.2 I 0.6 A perovskite single crystal.
This example of temperature-rising crystallization method for CsPbBr growth 2.9 I 0.1 The perovskite single crystal is prepared by adjusting the growth temperature of the perovskite single crystal according to the actual conditions as shown in FIG. 1.
This example CsPbBr 2.9 I 0.1 The perovskite single crystal was photographed as shown in FIG. 2, and the regular shape of the single crystal was observed.
This example CsPbBr 2.9 I 0.1 The XRD spectrum of the perovskite single crystal is shown in fig. 3, and the XRD spectrum of the crystal shows only diffraction peaks of crystal planes such as (101), (121), (040), (202), (222), (321), (123), and (242), indicating that the three-dimensional single crystal has a significant orientation and a good single crystal lattice.
This example CsPbBr 2.4 I 0.6 The response graph of the perovskite single crystal detector to X-rays under 40V bias is shown in FIG. 4, and the obvious response of the single crystal detector to the X-rays can be seen.
Example 2
(1) Mixing CsI and PbBr at a molar ratio of 0.01:1 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the ratio of the solvent is 1:1, and reacting for 24 hours at the temperature of 30 ℃ under stirring to obtain a clear 0.1mol/L precursor solution;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 1.2 microns and a syringe, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box;
(3) controlling the temperature of the drying oven to be 30-200 ℃, increasing the temperature at a heating rate of 0.1 ℃/hour, and growing CsPbBr 2.99 I 0.01 A perovskite single crystal.
Example 3
(1) Mixing CsI and PbBr at a molar ratio of 0.1:1 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the ratio of the solvent is 1:1, and reacting for 24 hours at 25 ℃ under stirring to obtain a clear 0.3mol/L precursor solution;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 1.6 microns and a syringe, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box;
(3) the temperature of the drying oven 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 A perovskite single crystal.
Example 4
(1) Mixing CsI and PbBr at a molar ratio of 0.2:1 2 Adding into mixed solution of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF)In the agent, the solvent ratio is 1:1, and the clear 0.5mol/L precursor solution is obtained after the reaction is carried out for 18 hours under the stirring at the temperature of 20 ℃;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 0.5 micron and a syringe, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box;
(3) the temperature of the drying oven 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 A perovskite single crystal.
Example 5
(1) Mixing CsI and PbBr at a molar ratio of 0.3:1 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the ratio of the solvent is 1:1, and reacting for 12 hours at 15 ℃ under stirring to obtain a clear 0.8mol/L precursor solution;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 0.1 micron and a syringe, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box;
(3) controlling the temperature of the drying oven to be 30-100 ℃, increasing the temperature at a heating rate of 2 ℃/hour, and growing CsPbBr 2.7 I 0.3 A perovskite single crystal.
Example 6
(1) Mixing CsI and PbBr at a molar ratio of 0.4:1 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the ratio of the solvent is 1:1, and reacting for 0.1h at 10 ℃ under stirring to obtain a clear 1mol/L precursor solution;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 0.3 micron and a syringe, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box;
(3) controlling the temperature of the drying oven to be 70-150 ℃, increasing the temperature at a heating rate of 3 ℃/hour, and growing CsPbBr 2.6 I 0.4 A perovskite single crystal.
Example 7
(1) Mixing CsI and PbBr at a molar ratio of 0.5:1 2 Adding into mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF)Wherein the solvent ratio is 1:1, and the clear 1.2mol/L precursor solution is obtained after stirring and reacting for 10 hours at the temperature of 5 ℃;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 0.8 micron and a syringe, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying oven;
(3) the temperature of the drying oven 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 A perovskite single crystal.
Example 8
(1) Mixing CsI and PbBr at a molar ratio of 0.7:1 2 Adding the mixture into 100mL of mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the ratio of the solvent is 1.5:1, and stirring and reacting for 24 hours at 20 ℃ to obtain clear 1.5mol/L precursor solution;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 1 micron and an injector, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box;
(3) the temperature of the drying oven is controlled to be 120-200 ℃, the temperature is increased at the heating rate of 2.5 ℃/hour, and CsPbBr is grown 2.3 I 0.7 A perovskite single crystal.
Example 9
(1) Mixing CsI and PbBr at a molar ratio of 0.9:1 2 Adding the mixture into a mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), wherein the ratio of the solvent is 1:1, and reacting for 24 hours at 30 ℃ under stirring to obtain a clear 1.8mol/L precursor solution;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 1.4 microns and a syringe, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box;
(3) controlling the temperature of the drying oven to be 30-60 ℃, increasing the temperature at a heating rate of 3.5 ℃/hour, and growing CsPbBr 2.1 I 0.9 A perovskite single crystal.
Example 10
(1) Mixing CsI and PbBr at a molar ratio of 0.99:1 2 Adding into mixed solvent of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF)Wherein the solvent ratio is 1:1, and the clear precursor solution with the concentration of 2mol/L is obtained after the reaction is carried out for 24 hours under the stirring at the temperature of 5 ℃;
(2) filtering the precursor solution into a clean crystallizing dish by using a filter element with the aperture of 1.6 microns and a syringe, sealing the crystallizing dish, and transferring the crystallizing dish into a quiet drying box;
(3) the temperature of the drying oven is controlled to be 90-180 ℃, the temperature is raised at the rate of 5 ℃/hour, and CsPbBr is grown 2.01 I 0.99 A perovskite single crystal.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. All-inorganic CsPbBr 3-x I x A method for producing a single crystal, characterized by comprising the steps of:
step 1, CsI and PbBr are added 2 Adding the mixture into a solvent, and stirring for reaction 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 separating out CsPbBr from the precursor solution along with the rise of the temperature of the heating box 3-x I x The heating temperature range of the heating box for the single crystal is 30-200 ℃.
2. The all-inorganic CsPbBr of 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 molar ratio of x to 1, x is more than or equal to 0.01 and less than or equal to 2.99.
3. The all-inorganic CsPbBr of claim 1 3-x I x The preparation method of the single crystal is characterized in that in the step 1, the concentration of the precursor solution is 0.1-2 mol/L.
4. The all-inorganic CsPbBr of 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 ℃.
5. The all-inorganic CsPbBr of claim 1 3-x I x The preparation method of the single crystal is characterized in that in the step 2, the precursor solution is filtered by a filter element before being placed in a vessel.
6. The all-inorganic CsPbBr of claim 4 3-x I x The preparation method of the single crystal is characterized in that the aperture of the filter element is 0.1-1.6 microns.
7. The all-inorganic CsPbBr of claim 1 3-x I x The preparation method of the single crystal is characterized in that in the step 2, the heating rate is 0.1-5 ℃/hour, and the heating range is 30-200 ℃.
8. The all-inorganic CsPbBr of claim 1 3-x I x The preparation method of the single crystal is characterized in that in the step 2, CsPbBr is precipitated from the precursor solution 3-x I x During the single crystal process, the vessel does not vibrate.
9. The all-inorganic CsPbBr of claim 1 3-x I x The method for preparing the single crystal is characterized in that in the step 1, the solvent is a mixed solvent of dimethyl sulfoxide and N, N-dimethylformamide.
10. An all-inorganic CsPbBr prepared by the preparation method of any one of claims 1 to 9 3-x I x And (3) single crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210600863.7A CN114836817B (en) | 2022-05-30 | 2022-05-30 | All-inorganic CsPbBr 3-x I x Single crystal and method for producing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210600863.7A CN114836817B (en) | 2022-05-30 | 2022-05-30 | All-inorganic CsPbBr 3-x I x Single crystal and method for producing same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114836817A true CN114836817A (en) | 2022-08-02 |
| CN114836817B CN114836817B (en) | 2024-02-27 |
Family
ID=82571376
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210600863.7A Active CN114836817B (en) | 2022-05-30 | 2022-05-30 | All-inorganic CsPbBr 3-x I x Single crystal and method for producing same |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114836817B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115404537A (en) * | 2022-08-26 | 2022-11-29 | 华中科技大学 | Preparation method of all-inorganic tin-based perovskite B-gamma CsSnI3 single crystal |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104911705A (en) * | 2015-05-18 | 2015-09-16 | 陕西师范大学 | Method for growing ABX3 perovskite single crystals in low-temperature solution |
| CN107611191A (en) * | 2017-08-24 | 2018-01-19 | 宁波大学 | A kind of inorganic perovskite solar cell and preparation method thereof |
| CN107829139A (en) * | 2017-11-07 | 2018-03-23 | 西北工业大学 | The inversion solution growth method of full-inorganic perovskite monocrystalline |
| CN108691012A (en) * | 2018-06-22 | 2018-10-23 | 福州大学 | Caesium lead halide perovskite crystal material and its preparation method and application of the one kind with high photoelectric respone efficiency, ambient-temp-stable |
| WO2019165909A1 (en) * | 2018-02-28 | 2019-09-06 | 湖北大学 | Gan/cspbbrxi3-x heterojunction-based light-responsive led preparation method therefor and use thereof |
| CN110611004A (en) * | 2019-09-24 | 2019-12-24 | 湖南大学 | All-inorganic halogen perovskite single crystal X-ray detector and preparation method thereof |
| CN111286779A (en) * | 2020-03-16 | 2020-06-16 | 山东科技大学 | Method for growing large-size perovskite single crystal by using ternary mixed solvent |
| CN111321467A (en) * | 2020-03-11 | 2020-06-23 | 中物院成都科学技术发展中心 | Preparation method of inorganic perovskite crystal and product thereof |
-
2022
- 2022-05-30 CN CN202210600863.7A patent/CN114836817B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104911705A (en) * | 2015-05-18 | 2015-09-16 | 陕西师范大学 | Method for growing ABX3 perovskite single crystals in low-temperature solution |
| CN107611191A (en) * | 2017-08-24 | 2018-01-19 | 宁波大学 | A kind of inorganic perovskite solar cell and preparation method thereof |
| CN107829139A (en) * | 2017-11-07 | 2018-03-23 | 西北工业大学 | The inversion solution growth method of full-inorganic perovskite monocrystalline |
| WO2019165909A1 (en) * | 2018-02-28 | 2019-09-06 | 湖北大学 | Gan/cspbbrxi3-x heterojunction-based light-responsive led preparation method therefor and use thereof |
| CN108691012A (en) * | 2018-06-22 | 2018-10-23 | 福州大学 | Caesium lead halide perovskite crystal material and its preparation method and application of the one kind with high photoelectric respone efficiency, ambient-temp-stable |
| CN110611004A (en) * | 2019-09-24 | 2019-12-24 | 湖南大学 | All-inorganic halogen perovskite single crystal X-ray detector and preparation method thereof |
| CN111816719A (en) * | 2019-09-24 | 2020-10-23 | 湖南大学 | All-inorganic halogen perovskite single crystal X-ray detector and preparation method thereof |
| CN111321467A (en) * | 2020-03-11 | 2020-06-23 | 中物院成都科学技术发展中心 | Preparation method of inorganic perovskite crystal and product thereof |
| CN111286779A (en) * | 2020-03-16 | 2020-06-16 | 山东科技大学 | Method for growing large-size perovskite single crystal by using ternary mixed solvent |
Non-Patent Citations (2)
| Title |
|---|
| FANGBAO WANG 等: "Low-Temperature Solution Growth and Characterization of Halogen (Cl, I)-Doped CsPbBr3 Crystals", 《CRYST. GROWTH DES.》, pages 1638 - 1645 * |
| ZEHAN LIU等: "High Temperature CsPbBrxI3−x Memristors Based on Hybrid Electrical and Optical Resistive Switching Effects", 《ACS APPL. MATER. INTERFACES》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115404537A (en) * | 2022-08-26 | 2022-11-29 | 华中科技大学 | Preparation method of all-inorganic tin-based perovskite B-gamma CsSnI3 single crystal |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114836817B (en) | 2024-02-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Holtzberg et al. | Chemistry of the group VB pentoxides. VI. The polymorphism of Nb2O5 | |
| CN109468131B (en) | Organic-inorganic perovskite scintillator for nuclear radiation detection and preparation method thereof | |
| CN110676342B (en) | Perovskite material-based X-ray detector and preparation method thereof | |
| CN114836817A (en) | All-inorganic CsPbBr 3-x I x Single crystal and method for producing the same | |
| CN111058085B (en) | Growing method of perovskite single crystal | |
| CN110846715A (en) | Large size zero dimension Cs4PbBr6/CsPbBr3Perovskite scintillation crystal and preparation method thereof | |
| CN115595660A (en) | Large-area halide perovskite single crystal heterojunction, growth method thereof and application of large-area halide perovskite single crystal heterojunction in nuclear radiation detector | |
| CN111816719A (en) | All-inorganic halogen perovskite single crystal X-ray detector and preparation method thereof | |
| CN111286779A (en) | Method for growing large-size perovskite single crystal by using ternary mixed solvent | |
| CN112853466A (en) | Method for growing copper-based lead-free perovskite single crystal by low-temperature solvent method | |
| CN111321467A (en) | Preparation method of inorganic perovskite crystal and product thereof | |
| CN113130769A (en) | Two-dimensional layered perovskite single crystal, wide-spectrum photoelectric detector and preparation method thereof | |
| CN113373501A (en) | EuCl3Helper Cs3Cu2X5Method for growing perovskite single crystal | |
| CN111933730B (en) | Nuclear radiation detector based on leadless perovskite monocrystal and preparation method thereof | |
| CN113970779A (en) | Microstructure scintillation screen formed by perovskite filled microporous panel and preparation method | |
| CN112210816B (en) | Perovskite single crystal sheet, method for promoting growth of perovskite single crystal sheet and application of perovskite single crystal sheet | |
| CN114921853B (en) | Perovskite single crystal with ordered domain structure, preparation method and radiation detector | |
| CN114197044B (en) | Perovskite single crystal growth method and device | |
| CN113046830B (en) | Mixed solvent-based all-inorganic perovskite Cs 3 Sb 2 Cl 9 Single crystal growth method of (2) | |
| CN111994947B (en) | 125-type cesium-lead-bromine perovskite nanosheet and aqueous phase preparation method of monocrystal thereof | |
| CN113604867B (en) | Method for efficiently preparing perovskite microcrystal by microwave method | |
| CN115678546A (en) | Thallium-doped Cs 3 Cu 2 I 5 Scintillator microcrystalline powder and preparation method and application thereof | |
| CN112853487B (en) | Epitaxial growth method of large-area metal halide perovskite single crystal array for nuclear radiation detection imaging | |
| CN114645327B (en) | Perovskite single crystal and growth method thereof | |
| CN115433999A (en) | Method for growing all-inorganic non-lead perovskite single crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |