CN111725406B - Ultraviolet photoelectric detector of lead-free perovskite single crystal and preparation method thereof - Google Patents
Ultraviolet photoelectric detector of lead-free perovskite single crystal and preparation method thereof Download PDFInfo
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Abstract
The invention disclosesAn ultraviolet photoelectric detector of lead-free perovskite single crystal and a preparation method thereof. This ultraviolet photoelectric detector of leadless perovskite single crystal includes from the bottom up in proper order: the lead-free perovskite single crystal comprises A, B, X, and the molecular structural formula of the lead-free perovskite single crystal is ABX 4 Wherein A is MA (CH) 3 NH 3 ) B is In, Bi or Sb, and X is Cl, I or Br. The detector replaces Pb element In the traditional perovskite material with elements such as In and Bi, and the synthesized novel perovskite material solves the problem caused by the biological toxicity of lead In the traditional perovskite; can maintain good performance in the air and humidity environment, and has better stability than the traditional perovskite material.
Description
Technical Field
The invention belongs to the technical field of semiconductor photoelectric detection, and particularly relates to an ultraviolet photoelectric detector of lead-free perovskite single crystal and a preparation method thereof.
Background
Organic-inorganic hybrid perovskite material APbX 3 [A＝(CH 3 NH 3 ) + (MA + )、CH(NH 2 ) 2+ (FA + )、Cs + ；X＝I - 、Br - 、Cl - ]Has high light absorption performance, and can detect secondary X - Various electromagnetic waves from rays to a near infrared region have low-cost solution processing performance, good photoelectron yield and long carrier life, and the unique advantages enable the semiconductor to have extremely wide application prospects in the fields of detection imaging, optical communication and biomedical sensing, thereby becoming one of the most concerned photoelectron materials at present.
At present, the perovskite thin film material with microcrystalline or polycrystalline morphology researched at home and abroad has very good performance after research and development in recent years, but the problems of grain boundary, pore, surface defect state and the like existing in the material affect the important photoelectric properties such as carrier mobility and the like. Compared with the single crystal perovskite, the single crystal perovskite further reduces the crystal boundary, greatly reduces the defect state density, further improves the mobility of electrons and holes, has wider absorption spectrum, longer carrier service life and higher stability, and becomes a powerful competitor in the field of photoelectric detection.
The traditional lead-based perovskite single crystal can have serious ion migration under the action of an electric field, so that a hysteresis phenomenon is generated, and the detection precision is influenced. ABX of conventional perovskite structure 3 The structure is mainly constructed on the basis of Sn (II), and the strong reducibility of Sn (II) cannot ensure that the single crystal stably exists in the atmospheric environment, so that the production and use conditions of the single crystal are limited. Furthermore, the toxicity of the heavy metal lead in lead-based perovskites has also caused new problems to be encountered in the large-scale commercial use of devices. Under the requirement of an environment-friendly concept, the novel lead-free perovskite material becomes an excellent choice for an environment-friendly and high-performance detector.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide the ultraviolet photoelectric detector of the lead-free perovskite single crystal, which overcomes the defects of intrinsic instability and biotoxicity of a lead-containing perovskite structure.
The second purpose of the invention is to provide a preparation method of the ultraviolet photoelectric detector of lead-free perovskite single crystal.
The first purpose of the invention is realized by the following technical scheme:
an ultraviolet photoelectric detector of lead-free perovskite single crystal, from bottom to top sequentially comprises: the lead-free perovskite single crystal is composed of A, B, X, and the molecular structural formula of the lead-free perovskite single crystal is ABX 4 Wherein A is MA (CH) 3 NH 3 ) B is In, Bi or Sb, and X is Cl, I or Br.
Preferably, the lead-free perovskite single crystal material is MAInI 4 、MAInBr 4 、MAInCl 4 、MABiI 4 、MABiBr 4 、MABiCl 4 、MASbI 4 、MASbBr 4 And MASbCl 4 One kind of (1).
Preferably, the substrate is a glass substrate for fixing the lead-free perovskite single crystal.
Preferably, the electrode is a gate electrode, and the electrode material is gold.
Preferably, the diameter of the conductive gold wire is 0.1-0.5 mm.
The second purpose of the invention is realized by the following technical scheme:
a preparation method of an ultraviolet photoelectric detector of lead-free perovskite single crystal comprises the following steps:
(1) preparation of ABX 4 Lead-free perovskite precursor solution: mixing a solute AX: BX 3 The molar ratio is 9-10: 1, dissolving the precursor solution in a mixed solution of halogen acid and anhydrous acetonitrile to form a lead-free perovskite precursor solution;
(2) preparation of ABX 4 Lead-free perovskite single crystal: heating the lead-free perovskite precursor solution obtained in the step (1) at 60-70 ℃ for 1-2 hours until the solution is clear and completely dissolved, then continuously heating at 60-70 ℃ for 4-5 hours for crystallization, and finally rapidly cooling to room temperature at the speed of 2-5 ℃/h until lead-free perovskite single crystals are generated;
(3)ABX 4 preparing a lead-free perovskite single crystal ultraviolet photoelectric detector: washing the lead-free perovskite single crystal grown in the step (2) by isopropanol or ethyl acetate, and then annealing the lead-free perovskite crystal in air at 373K for 1-2 hours; plating a layer of gold electrode on the surface of the lead-free perovskite single crystal by using a grid electrode template; lead-free perovskite single crystal is fixed on a substrate, and two ends of an electrode are led out by conductive gold wires and silver colloid, so that wiring test is facilitated.
Preferably, the hydrohalic acid in step (1) is at least one of hydrochloric acid, hydrobromic acid or hydroiodic acid.
Preferably, the mass concentration of the hydrohalic acid solution is 36-45%.
The method in the step (2) is an optimized crystal growth method, wherein the control of the crystal growth temperature is particularly critical, and the improvement of crystallinity and crystallization quality are facilitated.
Preferably, the electrode is subjected to electrode evaporation by using a grid template, and the thickness of the metal electrode is 100-300 nm.
In the ultraviolet photoelectric detector of the lead-free perovskite single crystal, the preparation method of the Au gate electrode is a conventional method, and the Au gate electrode can be prepared according to the existing preparation method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the novel perovskite material synthesized by using elements such as In, Bi and the like to replace Pb element In the traditional perovskite material solves the problem caused by the biological toxicity of lead In the traditional perovskite material; can maintain good performance in the air and humidity environment, and has better stability than the traditional perovskite material.
(2) According to the invention, a series of perovskite materials with 0D structures are grown through reasonable design of B-site ions and X-site ions in the perovskite; studies have shown that 0D perovskite materials possess numerous advantages: the super-large Stokes displacement can overcome the problem of reabsorption, higher quantum efficiency can ensure higher light efficiency, and the lead-free perovskite single crystal photoelectric detector synthesized by the 0D perovskite single crystal material has higher stability, higher sensitivity and faster response rate in the aspects of light stability and fluorescence effect.
(3) The invention solves the problem of difficult control of the appearance of the single crystal and realizes the growth of the large-size single crystal.
Based on ABX 3 A preparation method of a perovskite single crystal detector. The single crystal detector mainly comprises a perovskite single crystal, an electrode, conductive silver colloid, a gold wire lead and a glass substrate; the single crystal is positioned on the glass substrate, the gold electrode is evaporated on the surface of the single crystal by an evaporation method, and then the conductive gold wire is connected with the electrode by silver colloid for testing; wherein the lead-free perovskite single crystal is (CH) 3 NH 3 ) + (MA + ) As A site ions, B site Pb In the traditional perovskite is replaced by non-toxic metal In, Sb or Bi to form MABX with 0D structure 4 (B is In, Bi or Sb), and X is Cl - 、Br - 、I - ) The perovskite-like material solves the problems of high manufacturing cost, low detection sensitivity and the like of the traditional photoelectric conversion material device, and the MABX is designed 4 As a main material body, the ultra-low detection lower limit and high-sensitivity detection are realized, the lead-free material also solves the toxicity problem of heavy metal lead in lead-based perovskite, the development requirements of environmental friendliness and environmental protection are met, and meanwhile, the device has better stability in air and humidity environments, so that the perovskite-like single crystal detector has wide application prospect in the field of photoelectric detection
Drawings
FIG. 1 shows ABX 4 A lead-free perovskite single crystal structure diagram;
FIG. 2 is a structural diagram of a lead-free perovskite photodetector,
the solar cell comprises a substrate, a grid electrode, a conductive gold wire, a conductive silver colloid, a grid electrode, a conductive metal wire, a conductive perovskite monocrystal, a conductive silver colloid, a grid electrode, a conductive silver colloid, a conductive silver wire, a conductive perovskite monocrystal, a conductive silver colloid, a grid electrode, a conductive silver colloid, a glass, a grid electrode, a grid;
FIG. 3 shows MAInCl in example 1 4 The change curve of the current along with the voltage of the ultraviolet photoelectric detector in a dark state and an illumination environment;
FIG. 4 shows MAInCl in example 2 4 The change curve of the current along with the voltage of the ultraviolet photoelectric detector in a dark state and an illumination environment;
FIG. 5 shows the MABiI in example 3 4 The change curve of the current along with the voltage of the ultraviolet photoelectric detector in a dark state and an illumination environment;
FIG. 6 is MASbCl in example 4 4 The change curve of the current along with the voltage of the ultraviolet photoelectric detector in a dark state and an illumination environment;
FIG. 7 shows MAInCl in example 1 4 The response speed test result of the ultraviolet photoelectric detector;
FIG. 8 shows MAInCl in example 2 4 The response speed test result of the ultraviolet photoelectric detector;
FIG. 9 shows MABiI in example 3 4 The response speed test result of the ultraviolet photoelectric detector;
FIG. 10 is MASbCl in example 4 4 And testing the response speed of the ultraviolet photoelectric detector.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The process of the present invention is a conventional process unless otherwise specified. The raw material can be obtained from open commercial way if no special description is provided, wherein the mass concentration of the hydrohalide acid solution is 36-45%, the diameter of the conductive gold wire is 0.1-0.5 mm, and the ABX shown in figure 1 4 The structure of lead-free perovskite single crystal and fig. 2 is the structure of lead-free perovskite photoelectric detector.
Example 1 preparation of MAInCl 4 Single crystal perovskite ultraviolet photoelectric detector
1) Preparation of MAInCl 4 Precursor solution
0.023g MACl and 0.007g InCl were weighed by a high precision electronic balance 3 Then mixing and dissolving the two in a mixed solution of 1mL hydrochloric acid with the mass concentration of 36% and 0.5mL anhydrous acetonitrile;
2) preparation of MAInCl 4 (Single Crystal)
Adding MAInCl 4 Placing the precursor solution on a heating table, heating at 60 ℃ for 1h until the solution is clear and completely dissolved, and properly adding a hydrochloric acid solvent to promote complete dissolution if the solution is not completely dissolved; then continuously heating for 5 hours at 60 ℃ for crystal growth to improve the crystallization quality, wherein the crystal growth is too fast due to too high temperature, so that the crystal quality is influenced, and the crystal growth speed is too slow due to too low temperature, so that the growth of large-size single crystals is not facilitated; finally, rapidly reducing the temperature to room temperature at the speed of 5 ℃/h until a single crystal with the size of about 3mm is generated to be made into a device;
3)MAInCl 4 preparation of single crystal devices
After the grown single crystal is cleaned by isopropanol or ethyl acetate solution, a layer of gold electrode with the thickness of about 100nm is plated on the surface of the crystal by using a special grid electrode template. After the electrodes are plated, the single crystal is fixed on a glass substrate, and two ends of the electrodes are led out by using conductive gold wires with the diameter of 0.1mm and silver colloid, so that the wiring test is convenient.
FIG. 3 shows MAInCl in example 1 4 Ultraviolet photoelectric detector in darkThe current change curve along with the voltage under the state and illumination environment has the sensitivity of 1803.38A/W.
FIG. 7 shows MAInCl in example 1 4 The response speed test result of the ultraviolet photoelectric detector shows that the rising time is 1.1 mu s, the falling time is 1.0 mu s, and the ultraviolet photoelectric detector has quick response to ultraviolet light.
Both fig. 3 and fig. 7 were tested at 365nm, which is in the uv region.
Example 2 preparation of MAInCl 4 Single crystal perovskite ultraviolet photoelectric detector
1) Preparation of MAInCl 4 Precursor solution
0.023g of MACl and 0.007g of InCl were weighed by a high-precision electronic balance 3 Then mixing and dissolving the two in a mixed solution of 1mL of hydrochloric acid with the mass concentration of 45% and 0.5mL of anhydrous acetonitrile;
2) preparation of MAInCl 4 (Single Crystal)
Adding MAInCl 4 Placing the precursor solution on a heating table, heating at 70 ℃ for 2h until the solution is clear and completely dissolved, and properly adding a hydrochloric acid solvent to promote complete dissolution if the solution is not completely dissolved; then continuously heating for 4 hours at 70 ℃ for crystal growth to improve the crystallization quality, wherein the crystal growth is too fast due to too high temperature, so that the crystal quality is influenced, and the crystal growth speed is too slow due to too low temperature, so that the growth of large-size single crystals is not facilitated; finally, rapidly reducing the temperature to room temperature at the speed of 2 ℃/h until a single crystal with the size of about 4mm is generated to be made into a device;
3)MAInCl 4 preparation of single crystal devices
After the grown single crystal is cleaned by isopropanol or ethyl acetate solution, a layer of gold electrode with the thickness of about 300nm is plated on the surface of the crystal by using a special grid electrode template. After the electrodes are plated, the single crystal is fixed on a glass substrate, and two ends of the electrodes are led out by using conductive gold wires with the diameter of 0.5mm and silver colloid, so that the wiring test is convenient.
FIG. 4 shows MAInCl in example 1 4 The current variation curve of the ultraviolet photoelectric detector along with the voltage under the dark state and the illumination environment has the sensitivity of 1821.16A/W.
FIG. 8 shows M in example 1AInCl 4 The response speed test result of the ultraviolet photoelectric detector shows that the rising time is 1.2 mu s, the falling time is 1.1 mu s, and the ultraviolet photoelectric detector has quick response to ultraviolet light.
Both fig. 4 and fig. 8 were tested at 365nm, which is in the uv region.
Example 3 preparation of MABiI 4 Single crystal perovskite ultraviolet photoelectric detector
1) Configuring a MABiI 4 Precursor solution
0.048g MAI and 0.017g BiI are weighed by a high-precision electronic balance 3 Then mixing and dissolving the mixture in a mixed solution of 1mL of hydriodic acid with the mass concentration of 36 percent and 0.5mL of anhydrous acetonitrile;
2) preparation of MABiI 4 (Single Crystal)
Mixing MABiI 4 The precursor solution is placed on a heating table and heated for 2 hours at 60 ℃ until the solution is clear and completely dissolved, and if the solution is not completely dissolved, a hydriodic acid solvent is properly added to promote the complete dissolution of the solution; then continuously heating at 60 ℃ for 5h for crystal growth to improve the crystallization quality, wherein the excessive high temperature can cause the excessive high growth of the crystal, thereby affecting the crystal quality, and the excessive low temperature can cause the excessive low growth speed of the crystal, thereby being not beneficial to the growth of large-size single crystals, and finally rapidly reducing the temperature to the room temperature at the speed of 5 ℃/h until the single crystals with the size of about 3mm are generated to be made into devices;
3)MABiI 4 preparation of single crystal devices
Cleaning the grown single crystal with isopropanol or ethyl acetate solution, and plating a gold electrode layer with the thickness of about 100nm on the surface of the crystal by using a special grid electrode template; after the electrodes are plated, the single crystal is fixed on a glass substrate, and two ends of the electrodes are led out by using conductive gold wires with the diameter of 0.1mm and silver colloid, so that the wiring test is convenient.
FIG. 5 shows MABiI in example 3 4 The current variation curve of the ultraviolet photoelectric detector along with the voltage under the dark state and the illumination environment has the sensitivity of 945.96A/W.
FIG. 9 shows MABiI in example 3 4 The response speed test result of the ultraviolet photoelectric detector shows that the rising time is 0.2 mu s, the falling time is 0.1 mu s, and the ultraviolet photoelectric detector shows rapid ultraviolet lightAnd (6) responding.
Both fig. 5 and fig. 9 were tested at 365nm, which is in the uv region.
Example 4 preparation of MASbCl 4 Perovskite ultraviolet photoelectric detector of crystal
1) Configuring MASbCl 4 Precursor solution
0.023g of MACl and 0.007g of SbCl were weighed by a high-precision electronic balance 3 Then mixing and dissolving the two into a mixed solution of 1mL hydrochloric acid with the mass concentration of 36% and 0.5mL anhydrous acetonitrile;
2) preparation of MASbCl 4 (Single Crystal)
Mixing MASbCl 4 Placing the precursor solution on a heating table, heating at 60 ℃ for 2h until the solution is clear and completely dissolved, and properly adding a hydrochloric acid solvent to promote complete dissolution if the solution is not completely dissolved; then continuously heating for 5 hours at 60 ℃ for crystal growth to improve the crystallization quality, wherein the crystal growth is too fast due to too high temperature, so that the crystal quality is influenced, and the crystal growth speed is too slow due to too low temperature, so that the growth of large-size single crystals is not facilitated; finally, rapidly reducing the temperature to room temperature at the speed of 5 ℃/h until a single crystal with the size of about 3mm is generated to be made into a device;
3)MASbCl 4 preparation of single crystal devices
Cleaning the grown single crystal with isopropanol, and plating a gold electrode layer with the thickness of about 100nm on the surface of the crystal by using a special grid electrode template; after the electrodes are plated, the single crystal is fixed on a glass substrate, and two ends of the electrodes are led out by using conductive gold wires with the diameter of 0.1mm and silver colloid, so that the wiring test is convenient.
FIG. 6 is MASbCl in example 4 4 The current variation curve of the ultraviolet photoelectric detector along with the voltage under the dark state and the illumination environment has the sensitivity of 2153.89A/W.
FIG. 10 is MASbCl in example 4 4 The response speed test result of the ultraviolet photoelectric detector shows that the rising time is 0.3 mu s, the falling time is 0.4 mu s, and the ultraviolet photoelectric detector has quick response to ultraviolet light.
Both fig. 6 and fig. 10 were tested at 365nm, which is in the uv region.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. The ultraviolet photoelectric detector of the lead-free perovskite single crystal is characterized by sequentially comprising the following components from bottom to top: the lead-free perovskite single crystal is composed of A, B, X, and the molecular structural formula of the lead-free perovskite single crystal is ABX 4 Wherein A is MA, B is In, Bi or Sb, and X is Cl, I or Br;
the lead-free perovskite single crystal material is specifically MAInI 4 、MAInBr 4 、MAInCl 4 、MABiI 4 、MABiBr 4 、MABiCl 4 、MASbI 4 、MASbBr 4 And MASbCl 4 One of (1);
the preparation method of the ultraviolet photoelectric detector of the lead-free perovskite single crystal comprises the following steps:
(1) preparation of ABX 4 Lead-free perovskite precursor solution: mixing a solute AX: BX 3 The molar ratio is 9-10: 1, dissolving the precursor solution in a mixed solution of halogen acid and anhydrous acetonitrile to form a lead-free perovskite precursor solution;
(2) preparation of ABX 4 Lead-free perovskite single crystal: heating the lead-free perovskite precursor solution obtained in the step (1) at 60-70 ℃ for 1-2 hours until the solution is clear and completely dissolved, then continuously heating at 60-70 ℃ for 4-5 hours for crystallization, and finally rapidly cooling to room temperature at the speed of 2-5 ℃/h until lead-free perovskite single crystals are generated;
(3)ABX 4 preparing a lead-free perovskite single crystal ultraviolet photoelectric detector: washing the lead-free perovskite single crystal grown in the step (2) by isopropanol or ethyl acetate, and then annealing the lead-free perovskite single crystal in air at 373K for 1-2 hours; plating a layer of gold electrode on the surface of the lead-free perovskite single crystal by using a grid electrode template; lead-free calcium titaniumThe mineral single crystal is fixed on the substrate, and two ends of the electrode are led out by using conductive gold wires and silver colloid, so that the wiring test is convenient.
2. The ultraviolet photodetector for lead-free perovskite single crystal as claimed in claim 1, wherein the substrate is a glass substrate, and the substrate is used for fixing the lead-free perovskite single crystal.
3. The lead-free perovskite single crystal ultraviolet photodetector as claimed in claim 1, wherein the electrode is a gate electrode and the electrode material is gold.
4. The ultraviolet photodetector for lead-free perovskite single crystal according to claim 1, wherein the diameter of the conductive gold wire is 0.1-0.5 mm.
5. The ultraviolet photodetector of lead-free perovskite single crystal as claimed in claim 1, wherein the hydrohalic acid in the step (1) is at least one of hydrochloric acid, hydrobromic acid or hydroiodic acid.
6. The ultraviolet photodetector for lead-free perovskite single crystal as claimed in claim 1, wherein the mass concentration of the hydrohalide acid solution is 36 to 45%.
7. The ultraviolet photodetector of lead-free perovskite single crystal according to claim 1, wherein the electrode is subjected to electrode evaporation by using a grid template, and the thickness of the metal electrode is 100 to 300 nm.
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