CN112142100A - Perovskite polycrystalline thin sheet and preparation method and application thereof - Google Patents

Perovskite polycrystalline thin sheet and preparation method and application thereof Download PDF

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CN112142100A
CN112142100A CN202011052773.6A CN202011052773A CN112142100A CN 112142100 A CN112142100 A CN 112142100A CN 202011052773 A CN202011052773 A CN 202011052773A CN 112142100 A CN112142100 A CN 112142100A
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perovskite
powder
solution
polycrystalline
perovskite polycrystalline
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刘生忠
杨周
贾珊珊
肖英锐
胡明昕
刘渝城
张云霞
步诺
莫莉红
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Shaanxi Normal University
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    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G21/00—Compounds of lead
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    • C—CHEMISTRY; METALLURGY
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    • C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
    • C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
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    • C01P2002/34—Three-dimensional structures perovskite-type (ABO3)
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    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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    • C01—INORGANIC CHEMISTRY
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract

The invention discloses a perovskite polycrystalline flake and a preparation method and application thereof2Powder of PbX2The powder and the AX powder are capable of reacting to produce a perovskite precursor, which is insoluble in the organic solvent, such that the perovskite precursor is capable of being separated from the process solution by a centrifugation process; the preparation process is different from the preparation process of the existing in-situ hot pressing method, and the perovskite powder prepared by the solution methodThe raw materials are more uniform, so that the precursor can fully react, the raw material utilization rate can be 80%, and the waste of the raw materials is avoided.

Description

Perovskite polycrystalline thin sheet and preparation method and application thereof
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of semiconductor photoelectric materials, and particularly relates to a perovskite polycrystalline thin sheet and a preparation method and application thereof.
[ background of the invention ]
The lead-halogen perovskite material has excellent photoelectric properties and is widely applied to devices such as solar cells, LEDs, lasers, ray detectors and the like. At present, perovskite materials have high sensitivity when being used as ray detectors, and are widely concerned by people. However, most of the high-performance devices reported at present are single crystals with small areas, and in order to further realize large-scale application of perovskite materials, the development of a preparation technology of large-area perovskite materials becomes a problem to be solved in current research. Meanwhile, the performance of the perovskite ray detector is in a positive correlation with the thickness of the perovskite material, and the development of a preparation technology of the perovskite thick film is a problem to be solved urgently.
At present, a slow cooling growth method, an inverse temperature gradient growth method, an anti-solvent assisted growth method and other growing single crystals are generally adopted as a ray detector, but huge raw material waste is easily caused in the growth process, and the grown crystals are generally small. Therefore, it is necessary to develop a method for preparing a crystal rapidly, with high operability, high material utilization rate, and good device performance.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art and provides a perovskite polycrystalline thin sheet, a preparation method and application thereof, so as to solve the problem that the prior art is lack of a perovskite thick film preparation method.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of a perovskite polycrystalline thin sheet comprises the following steps:
step 1, dissolving AX powder in lower alcohol, and stirring and dissolving to obtain a solution B; adding PbX into the solution B2Powder is evenly stirred to generate a perovskite precursor in the solution, the solution containing the perovskite precursor is centrifugally processed to obtain a centrifugal product, and the centrifugal product is dried to obtain perovskite powder; a is Cs2+、CH3NH3 2+Or CH (NH)2)2 2+X is halogen, the lower alcohol is compatible with AX powder and is insoluble with perovskite precursor;
and 2, preparing the perovskite powder into a perovskite polycrystalline sheet by an in-situ hot pressing method.
The invention is further improved in that:
preferably, in step 1, AX powder is dissolved in a lower alcohol and stirred at 60-90 ℃ to obtain a solution B.
Preferably, the lower alcohol is iso-n-butanol, ethyl propanol, iso-propanol or iso-butanol.
Preferably, in step 1, the mixing ratio of AX powder and lower alcohol is (1-10) g:10 mL.
Preferably, in step 1, PbX is added to the solution B2And (3) uniformly stirring the powder, and then centrifuging the powder for 3 to 5 times.
Preferably, in the step 1, the drying temperature is 40-150 ℃ and the drying time is 6-18 h.
Preferably, in step 2, the in-situ hot pressing method specifically comprises: adding the perovskite powder into a die, heating and pressurizing to obtain the perovskite polycrystalline sheet.
Preferably, the heating temperature is 80-250 ℃, the pressure is 0.1-40MPa, and the heating and pressurizing time is 1-12 h.
The perovskite polycrystalline thin slice prepared by the preparation method is APbX3And has a thickness of 10 μm to 5 mm.
Preferably, the perovskite polycrystalline thin slice is applied to a perovskite detector, and the sensitivity of the perovskite polycrystalline thin slice is less than or equal to 5.14 multiplied by 104μC Gyair -1cm-2。
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of perovskite polycrystalline flake, which comprises the steps of firstly dissolving AX powder in an organic solvent through a solution compatible with the AX powder by a solution method, and then adding PbX into the solution2Powder of PbX2The powder and the AX powder are capable of reacting to produce a perovskite precursor, which is insoluble in the organic solvent, such that the perovskite precursor is capable of being separated from the process solution by a centrifugation process; the preparation process is different from the preparation process of the existing in-situ hot pressing method, the perovskite powder prepared by the solution method has more uniform raw materials, the precursor is subjected to sufficient reaction, the raw material utilization rate can be 80 percent, and the waste of the raw materials is avoided. In the process of preparing perovskite materials by adopting a chemical method, such as a spin-coating method and a solution method for growing crystals, only a part of solution is effectively utilized, and the problems of large solution waste and raw material waste exist. The perovskite powder is prepared by the step method, and the perovskite polycrystalline thin slice with high quality and controllable thickness is obtained under the condition of heating and pressurizing.
Further, stirring at 60-90 deg.C ensures that AX powder can be sufficiently dissolved in lower alcohol.
Furthermore, through multiple times of centrifugation, the perovskite precursors can be separated from the solution as much as possible.
The invention also discloses a perovskite polycrystalline slice which is fast in grain growth and high in grain purity, and the polycrystalline slice obtained by the method has carrier mobility and carrier collection efficiency equivalent to those of single crystal materials and can be used for preparing ray detectors with different structures.
The invention also discloses application of the perovskite polycrystalline thin sheet, which can be used for preparing high-quality perovskite photoelectric devices.
[ description of the drawings ]
FIG. 1 shows an example of a perovskite multi-wafer used as an X-ray detector.
FIG. 2 is a scanning electron micrograph of a perovskite polycrystalline plate according to example 1 of the present invention;
fig. 3 shows the response of the detector described in example 1 of the present invention to X-rays.
[ detailed description ] embodiments
The invention is described in further detail below with reference to the accompanying drawings:
in the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention; the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance; furthermore, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly and encompass, for example, both fixed and removable connections; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
A method of making a composite perovskite polycrystalline sheet comprising the steps of:
step 1, perovskite powder is prepared through a solution method.
Dissolving AX powder in lower alcohol at a mixing ratio of (1-10) g:10 mL; preferably, the lower alcohol is n-butanol, ethyl propanol, isopropanol or isobutanol, and is dissolved by stirring at 60 deg.C-90 deg.C to obtain solution B, and PbX powder is poured into solution B, wherein PbX and AX are mixed at a ratio of PbX to AXExample is APbX3Stirring until PbX completely reacts with the solution, centrifuging for several times to obtain calcium-titanium ore powder, drying the centrifuged product for 6-18h at 40-120 deg.C to obtain perovskite powder, wherein A in AX powder is Cs2+、CH3NH3 2+Or CH (NH)2)2 2+X is halogen, in particular Cl-、Br-And I-. In the step, the organic solvent provides a solvent place for the perovskite powder, so that the perovskite powder is uniform and is prepared for the crystallization in the next step.
Step 2, preparing perovskite polycrystalline slice
Putting perovskite powder into a die, pressurizing and heating for 1-12h at the pressure of 0.1-40MPa and the heating temperature of 80-250 ℃ to realize the reaction between the raw materials, pressing the raw materials into sheets, and obtaining the perovskite polycrystalline sheet with the target thickness by controlling the pressure of a press in the pressing process, wherein the thickness of the perovskite polycrystalline sheet is 10 mu m-5 mm.
And 3, uniformly spreading the electron transport layer or the hole transport layer on the surface of the wafer through spin coating.
And 4, covering the metal electrode on the surface of the transmission layer or the wafer through evaporation.
In the above step, as a detector, a metal electrode on the upper surface or the lower surface of the perovskite polycrystalline thin film is necessary, and a hole transport layer or an electron transport layer may be provided between the upper surface of the perovskite polycrystalline thin film and the upper metal electrode or between the lower surface of the perovskite polycrystalline thin film and the lower metal electrode as required to promote the transport of electrons, and then the metal electrode is deposited on the upper surface or the lower surface.
Example 1
1. First 1g of CH2NH3The I powder was dissolved in 10mL of isopropanol, stirred at 80 ℃ until dissolved, and 2g of PbI was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times to obtain perovskite solid powderAnd drying at 60 ℃ for 12h to obtain the perovskite powder.
2. Putting perovskite powder into a round die, pressing for 5 hours in a high-temperature and high-pressure mode (10MPa, 150 ℃), and pressing the raw materials into sheets to obtain perovskite polycrystalline sheets;
3. taking out the cooled wafer, and respectively evaporating gold with the thickness of 50nm and 100nm on two surfaces to be used as electrodes;
4. the prepared X-ray detector was tested for sensitivity under different conditions.
Referring to fig. 1, the perovskite polycrystalline wafer prepared by the present example is used as an X-ray detector, referring to fig. 2, the gold phase diagram of the perovskite polycrystalline wafer prepared by the present example is shown, it can be seen from the diagram that the grains of the perovskite polycrystalline wafer prepared by the method are uniform, the size is about 20 μm, fig. 3 is a test of the sensitivity of the perovskite polycrystalline wafer, it can be seen from the diagram that the sensitivity of the perovskite polycrystalline wafer can reach 5.14 × 104μC Gyair -1cm-2。
Example 2
1. First 1g of CH2NH3Br powder was dissolved in 10mL of isopropanol, stirred at 80 ℃ until dissolved, and 2g of PbBr was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 80 ℃ for 12h to obtain the perovskite powder.
2. Putting perovskite powder into a round die, pressing for 8 hours in a high-temperature and high-pressure mode (10MPa, 150 ℃), and pressing the raw materials into sheets to obtain perovskite polycrystalline sheets;
3. taking out the cooled wafer, spin-coating an electron transport layer (PCBM solution with the concentration of 20 mg/mL) on one surface of the wafer, and not processing the other surface of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 3
1. 1.5g CsBr powder was dissolved in 10mL isopropanol, stirred at 80 ℃ until dissolved, and 2g PbBr was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 100 ℃ for 12h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (10MPa, 150 ℃, 1h) to obtain perovskite polycrystalline sheets;
3. taking out the cooled wafer, and respectively spin-coating electron transport layers (PCBM solution with the concentration of 20 mg/mL) on two surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 4
1. 1.5g CsCl powder was dissolved in 10mL isopropanol, stirred to dissolve at 80 deg.C, and 2g PbCl was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 40 ℃ for 12h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (10MPa, 150 ℃, 12h) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and an electron transport layer (PCBM solution at 20 mg/mL) was spin-coated on one surface and a hole transport layer (Spiro solution at 0.09 mg/mL) was spin-coated on the other surface;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 5
1. First 1g of CH (NH)2)2The I powder was dissolved in 10mL of isopropanol, stirred at 80 ℃ until dissolved, and 2g of PbI was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 50 ℃ for 12h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (10MPa, 150 ℃, 10h) to obtain perovskite polycrystalline sheets;
3. taking out the cooled wafer, spin-coating a hole transport layer (0.09mg/mL of Spiro solution) on one surface of the wafer, and not processing the other surface;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 6
1. First 1g of CH (NH)2)2Br powder was dissolved in 10mL of isopropanol, stirred at 80 ℃ until dissolved, and 2g of PbBr was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 80 ℃ for 12h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (10MPa, 150 ℃ and 2 hours) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 7
1. First 2g of CH2NH3Dissolving the powder I in 10mL of n-butanol, stirring at 60 deg.C to dissolve, and adding 2g of PbI2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 80 ℃ for 6h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (0.1MPa, 150 ℃ and 3 hours) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 8
1. First 3g of CH2NH3Br powder was dissolved in 10mL of ethylene propylene alcohol, stirred at 90 ℃ until dissolved, and 2g of PbBr was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 70 ℃ for 18h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (1MPa, 2000 ℃, 6h) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 9
1. 4g CsBr powder was dissolved in 10mL isopropanol, stirred at 70 ℃ until dissolved, and 2g PbBr was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 90 ℃ for 10h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (10MPa, 150 ℃, 10h) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 10
1.5g CsCl powder was dissolved in 10mL of isobutanol, the solution was stirred at 65 ℃ until dissolved, and 2g CsBr was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and centrifuging at 110 deg.CDrying at the temperature of 8 ℃ for 8h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (15MPa, 100 ℃ and 8 hours) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 11
1. First 6g of CH (NH)2)2Dissolving the powder I in 10mL of n-butanol, stirring at 75 deg.C to dissolve, and adding 2g of PbI2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 45 ℃ for 12h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (20MPa, 90 ℃ and 7 hours) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 12
1. First 7g of CH (NH)2)2Br powder was dissolved in 10mL of ethylene propylene alcohol, stirred at 85 ℃ until dissolved, and 2g of PbBr was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 55 ℃ for 16h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (25MPa, 80 ℃ and 6 hours) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 13
1. First 8g of CH2NH3Cl powder was dissolved in 10mL of isopropanol, stirred at 80 ℃ until dissolved, and 2g of PbBr was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 75 ℃ for 17h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (30MPa, 150 ℃, 11h) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 14
1. 9g CsCl powder was dissolved in 10mL isobutanol, stirred to dissolve at 85 deg.C, and 2g PbCl was added2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 105 ℃ for 15h to obtain the perovskite powder.
2. Putting perovskite powder into a circular die, and pressing the raw material into sheets in a high-temperature and high-pressure mode (35MPa, 200 ℃ and 10 hours) to obtain perovskite polycrystalline sheets;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
Example 15
1. First 10g of CH (NH)2)2Dissolving Cl powder in 10mL n-butanol, stirring at 65 deg.C to dissolve, and adding 2g PbCl2Pouring the powder into the solution, stirring for 2h, centrifuging for 3 times, and drying at 95 ℃ for 14h to obtain the perovskite powder.
2. Putting perovskite powder into a round die, pressing the raw material into a sheet shape in a high-temperature and high-pressure mode (40MPa, 250 ℃ and 9 hours) to obtain a perovskite polycrystalline sheet;
3. the cooled wafer was taken out, and a hole transport layer (0.09mg/mL of Spiro solution) was spin-coated on both surfaces of the wafer;
4. taking out the spin-coated wafer, and respectively evaporating gold with the thickness of 50nm and the thickness of 100nm on two sides to be used as electrodes;
5. the prepared X-ray detector was tested for sensitivity under different conditions.
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. A preparation method of a perovskite polycrystalline slice is characterized by comprising the following steps:
step 1, dissolving AX powder in lower alcohol, and stirring and dissolving to obtain a solution B; adding PbX into the solution B2Powder is evenly stirred to generate a perovskite precursor in the solution, the solution containing the perovskite precursor is centrifugally processed to obtain a centrifugal product, and the centrifugal product is dried to obtain perovskite powder; a is Cs2+、CH3NH3 2+Or CH (NH)2)2 2+X is halogen, the lower alcohol is compatible with AX powder and is insoluble with perovskite precursor;
and 2, preparing the perovskite powder into a perovskite polycrystalline sheet by an in-situ hot pressing method.
2. The method for producing a perovskite polycrystalline flake according to claim 1, wherein in step 1, AX powder is dissolved in a lower alcohol and stirred at 60 to 90 ℃ to obtain a solution B.
3. The method of claim 1, wherein the lower alcohol is iso-n-butanol, ethyl propanol, iso-propanol or iso-butanol.
4. The method for producing a perovskite polycrystalline flake according to claim 1, wherein in the step 1, the mixing ratio of the AX powder and the lower alcohol is (1-10) g:10 mL.
5. The method for preparing a perovskite polycrystalline flake according to claim 1, wherein in the step 1, PbX is added to the solution B2And (3) uniformly stirring the powder, and then centrifuging the powder for 3 to 5 times.
6. The method for preparing a perovskite polycrystalline flake according to claim 1, wherein in the step 1, the drying temperature is 40 to 150 ℃ and the drying time is 6 to 18 hours.
7. The method for producing a perovskite polycrystalline thin sheet according to any one of claims 1 to 6, wherein in the step 2, the in-situ hot pressing method is specifically: adding the perovskite powder into a die, heating and pressurizing to obtain the perovskite polycrystalline sheet.
8. The method for producing a perovskite polycrystalline flake according to claim 5, wherein the heating temperature is 80 to 250 ℃, the pressure is 0.1 to 40MPa, and the heating and pressing time is 1 to 12 hours.
9. The perovskite polycrystalline thin sheet prepared by the preparation method according to claim 1, wherein the perovskite polycrystalline thin sheet is APbX3And has a thickness of 10 μm to 5 mm.
10. Use of a perovskite polycrystalline flake according to claim 9 in a perovskite detector, wherein the perovskite polycrystalline flake has a sensitivity of 5.14 x 10 or less4μC Gyair -1cm-2。
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113130765A (en) * 2021-04-13 2021-07-16 吉林大学 Based on inorganic CsPbI2Br powder perovskite solar cell and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106340587A (en) * 2015-07-09 2017-01-18 清华大学 Perovskite film preparation method and perovskite solar cell
US20170162809A1 (en) * 2014-08-19 2017-06-08 Wuhan University Perovskite thin-film photovoltaic cell and preparation method thereof
CN109742238A (en) * 2018-12-28 2019-05-10 陕西师范大学 A kind of lead halogen perovskite polycrystalline thin slice and preparation method thereof
CN109935694A (en) * 2017-12-19 2019-06-25 国家纳米科学中心 A kind of perovskite thin film and the preparation method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170162809A1 (en) * 2014-08-19 2017-06-08 Wuhan University Perovskite thin-film photovoltaic cell and preparation method thereof
CN106340587A (en) * 2015-07-09 2017-01-18 清华大学 Perovskite film preparation method and perovskite solar cell
CN109935694A (en) * 2017-12-19 2019-06-25 国家纳米科学中心 A kind of perovskite thin film and the preparation method and application thereof
CN109742238A (en) * 2018-12-28 2019-05-10 陕西师范大学 A kind of lead halogen perovskite polycrystalline thin slice and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JOYDEEP DHAR ET AL.: "Investigation of Ion-Mediated Charge Transport in Methylammonium Lead Iodide Perovskite", 《THE JOURNAL OF PHYSICAL CHEMISTRY C》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113130765A (en) * 2021-04-13 2021-07-16 吉林大学 Based on inorganic CsPbI2Br powder perovskite solar cell and preparation method thereof

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