CN110104675B - Lead iodide nano material and preparation method and application thereof - Google Patents
Lead iodide nano material and preparation method and application thereof Download PDFInfo
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- CN110104675B CN110104675B CN201910305048.6A CN201910305048A CN110104675B CN 110104675 B CN110104675 B CN 110104675B CN 201910305048 A CN201910305048 A CN 201910305048A CN 110104675 B CN110104675 B CN 110104675B
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- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 26
- 229910052710 silicon Inorganic materials 0.000 claims description 26
- 239000010703 silicon Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 229920002799 BoPET Polymers 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 abstract description 19
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000002135 nanosheet Substances 0.000 description 25
- 235000012431 wafers Nutrition 0.000 description 25
- 239000002904 solvent Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000010410 layer Substances 0.000 description 10
- 239000007791 liquid phase Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000004044 response Effects 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 239000002055 nanoplate Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000005240 physical vapour deposition Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- -1 transition metal chalcogenides Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 239000002346 layers by function Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002060 nanoflake Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 125000002346 iodo group Chemical group I* 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- RQQRAHKHDFPBMC-UHFFFAOYSA-L lead(ii) iodide Chemical compound I[Pb]I RQQRAHKHDFPBMC-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/16—Halides
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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Abstract
The invention discloses a preparation method of a lead iodide nano material, which comprises the following steps: placing a target substrate in a cuvette; putting the small vessel into a large vessel filled with deionized water; and transferring the supersaturated aqueous solution of lead iodide onto the target substrate, sealing the large vessel, and standing until the water on the target substrate is completely volatilized to obtain the two-dimensional lead iodide nano material. The preparation method is simple, can obtain the high-quality two-dimensional lead iodide nano material in a short time in an environment-friendly manner at a lower temperature by using very simple equipment, improves the preparation efficiency and yield, and has low preparation cost. The invention also discloses a two-dimensional lead iodide nano material prepared by the preparation method and application thereof, wherein the two-dimensional lead iodide nano material has a layered structure, smooth surface and high crystal quality. The ultraviolet detector prepared by the two-dimensional lead iodide nano material has excellent detection performance.
Description
Technical Field
The invention relates to the technical field of two-dimensional nano materials, in particular to a lead iodide nano material and a preparation method and application thereof.
Background
With the development of miniaturization and multi-functionalization of chips, optical and electronic devices are included, which puts higher demands on materials. New two-dimensional materials such as graphene, transition metal chalcogenides, etc. have many unique properties not found in conventional materials and thus have received much attention from both academic and industrial areas.
Lead iodide (PbI)2) The material is a two-dimensional layered material, the forbidden band width is 2.38-2.5 eV due to different layers, and although single-layer lead iodide is an indirect band gap semiconductor like a bulk silicon material, other layers of lead iodide are direct band gap semiconductor materials, so that the material can be used for preparing optoelectronic devices, such as an ultraviolet detector.
There are two-dimensional PbI2The synthesis method of the nano-sheet comprises mechanical stripping, Physical Vapor Deposition (PVD), a hydrothermal method and a liquid phase growth method. Although mechanical exfoliation can produce high quality PbI2The nano-sheet, however, is difficult to control in size, is not suitable for large-scale preparation, and requires extensive experience in the preparation process. The PVD method can prepare PbI with higher quality in large area2Nano meterFlakes, but the manufacturing equipment is complex, expensive, and requires higher temperatures.
Compared with the traditional mechanical stripping and PVD methods, the liquid phase growth method generally does not need high temperature, does not involve vacuum and complex equipment, and is easier to operate. Patent specification CN107739047A discloses a preparation method of monodisperse high-purity lead iodide, which comprises the steps of mixing a lead acetate aqueous solution with a potassium iodide solution, reacting for 8-16 hours at 80-120 ℃, and drying to obtain a lead iodide thin film material. The disadvantages of this process are the high temperatures required for the reaction, the complex operating procedures and the long time required.
Another literature reports PbI by saturation at 100 deg.C2The solution is directly dripped on a target substrate to obtain PbI with different thicknesses2Nanoflakes (Ricchardo Frisenda et al, Nanotechnology, vol.2017 28, 455703), although this process enables the preparation of lead iodide nanomaterials, the PbI obtained2The surface of the nano material is rough and has low quality.
The liquid phase method can prepare PbI2However, the chemical reaction process and the solvent volatilization process are difficult to control, and the shape regularity, the shape controllability and the crystal quality of the prepared crystal still need to be improved. It is well known that for semiconductor materials, surface roughness, crystal structure defects can significantly affect the performance of optoelectronic devices.
Disclosure of Invention
Aiming at the defects in the field, the invention provides the preparation method of the lead iodide nano material, which has the advantages of low cost, simplicity and environmental protection, can be used for preparing the two-dimensional lead iodide nano material on any target substrate under the condition of being close to room temperature, and has smooth surface and high crystal quality.
A preparation method of a lead iodide nano material comprises the following steps:
(1) placing a target substrate in a cuvette;
(2) putting the small vessel into a large vessel filled with deionized water;
(3) and transferring the supersaturated aqueous solution of lead iodide onto the target substrate, sealing the large vessel, and standing until the water on the target substrate is completely volatilized to obtain the two-dimensional lead iodide nano material.
In order to enable the two-dimensional lead iodide nano material to grow more uniformly, the invention adopts two technologies to control the volatilization of the solvent, namely the small vessel in the steps (1) and (2) is placed in a big vessel filled with water, the height of the water level in the big vessel is smaller than that of the small vessel, and the big vessel is sealed in the step (3), so that a relatively closed environment for stabilizing the volatilization of the solvent is created for the growth of the two-dimensional lead iodide nano material. The basic principle is as follows:
due to PbI2Can be dissolved in water and the solubility of which depends on the temperature, hot PbI2The reduction of the solution temperature leads to PbI2The solubility in water decreases; thus, as the solvent evaporates, the supersaturation of the solution increases, and thus PbI2The crystal starts to grow. Maintaining a stable atmosphere and a slow growth rate during liquid phase growth is useful for obtaining high quality PbI2The crystal is critical. In order to inhibit the rapid evaporation of the water solvent, the present invention adopts two simple control methods, i.e., adding water to the boat to increase the partial pressure and inhibit PbI2The evaporation rate of the solvent, while covering the growth system to isolate the crystal growth environment from the atmosphere to some extent.
Preferably, when the two-dimensional lead iodide nano material is kept stand, the temperature in the large vessel is 20-50 ℃, the low temperature is kept, a relatively closed environment for stabilizing solvent volatilization is created for the growth of the two-dimensional lead iodide nano material, the appearance control and the surface smoothness of the generated two-dimensional lead iodide nano material are facilitated, and the crystal quality is improved. More preferably, the temperature in the large vessel is 30 ℃ on standing. The two-dimensional lead iodide nano material generated at the temperature has the most regular shape, the most smooth surface and the best crystal quality.
The target substrate of step (1) of the present invention may be a substrate of any material because of low temperature growth, including commonly used silicon wafers, glass, flexible carbon films, and other flexible substrate materials.
Preferably, the target substrate is a silicon wafer, glass, a PET film or a copper mesh carbon film.
The length of the standing time depends on the amount of the supersaturated aqueous solution of lead iodide transferred onto the target substrate, and is related to factors such as the size, the dimensional thickness, the solvent volatilization speed, etc. of the prepared lead iodide sample.
The invention also provides a two-dimensional lead iodide nano material prepared by the preparation method of the lead iodide nano material.
The microscopic morphology of the two-dimensional lead iodide nano material is a hexagonal nanosheet.
Preferably, the microscopic morphology of the two-dimensional lead iodide nanomaterial is a regular hexagon nanosheet.
The invention also provides application of the two-dimensional lead iodide nanomaterial as a photosensitive functional layer.
The invention also provides application of the two-dimensional lead iodide nano material in an ultraviolet detector.
The ultraviolet detector takes a two-dimensional lead iodide nano material as a photosensitive functional layer, and realizes ultraviolet detection by a device structure of a conventional field effect transistor. The preparation of field effect transistors and the substrates, source and drain electrodes, gates, insulating layers, etc. involved are prior art.
Compared with the prior art, the invention has the main advantages that:
(1) the preparation method of the two-dimensional lead iodide nano material is simple, the high-quality two-dimensional lead iodide nano material can be obtained in a short time in an environment-friendly manner at a lower temperature by using very simple equipment, the preparation efficiency and the yield are improved, and the preparation cost is low.
(2) The two-dimensional lead iodide nano material has a layered structure, regular appearance, smooth surface and high crystal quality.
(3) The ultraviolet detector prepared by the two-dimensional lead iodide nano material has excellent detection performance.
Drawings
FIG. 1 is a schematic structural diagram of a two-dimensional layered lead iodide nanomaterial of the present invention;
fig. 2 is a schematic view of a preparation method of a lead iodide nanomaterial of the present invention, in which: 1-big vessel, 2-small vessel, 3-target substrate, 4-lead iodide supersaturated aqueous solution and 5-sealing cover;
FIG. 3 is an atomic force microscope photograph of two-dimensional lead iodide nanosheets prepared in example 1;
fig. 4 is an atomic force microscope photograph of the two-dimensional lead iodide nanosheet prepared in example 2;
fig. 5 is an atomic force microscope photograph of two-dimensional lead iodide nanosheets prepared on silicon wafer of example 3;
fig. 6 is an optical microscope photograph of two-dimensional lead iodide nanosheets prepared on different target substrates of example 3;
FIG. 7 is an X-ray photoelectron spectroscopy (XPS), XRD and Raman spectra of two-dimensional lead iodide nanoplates prepared on a silicon wafer of example 3;
fig. 8 is a schematic structural diagram of a lead iodide ultraviolet detector of an application example;
FIG. 9 is a photograph showing an application example of a lead iodide UV detector;
FIG. 10 is a performance characterization diagram of a lead iodide ultraviolet detector of an application example; FIG. 10a is a graph of the corresponding output in light and dark; FIG. 10b is the corresponding transfer curve of a lead iodide UV detector in the dark and under light; FIGS. 10c and 10d are graphs of the photo-response behavior of a lead iodide UV detector; FIG. 10d shows the result of the measurement of the ultraviolet intensity of lead iodideds-a t-plot;
fig. 11 is an atomic force microscope photograph of two-dimensional lead iodide nanosheets prepared in comparative example 1;
fig. 12 is an atomic force microscope photograph of two-dimensional lead iodide nanosheets prepared in comparative example 2;
FIG. 13 is a graph showing the results of the surface roughness of the two-dimensional lead iodide nanosheets prepared in example 3 and comparative examples 1-2.
Detailed Description
The invention is further described with reference to the following drawings and specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out under conventional conditions or conditions recommended by the manufacturers.
The two-dimensional lead iodide nano material contains lead element and iodine element, the atomic structure of the two-dimensional lead iodide nano material is planar, and the single-layer two-dimensional lead iodide is a sandwich structure consisting of iodine-lead-iodine three atomic layers, as shown in figure 1. The single-layer two-dimensional lead iodide is piled into two-dimensional lead iodide nano materials with different layers and different thicknesses, and the chemical structural formula of the material is PbI2。
Referring to fig. 2, a method for preparing a lead iodide nanomaterial in each of the following examples and comparative examples is shown, in which a large vessel 1 is sealed by a sealing cover 5, a proper amount of water is contained in the large vessel 1, a small vessel 2 is also contained in the large vessel 1, the water in the large vessel 1 does not overflow the small vessel 2, a target substrate 3 is contained in the small vessel 2, and a supersaturated aqueous solution 4 of lead iodide is dropped on the target substrate 3. And standing the structural device at a certain temperature to completely volatilize the solvent of the lead iodide supersaturated aqueous solution 4 to obtain the two-dimensional lead iodide nano material.
Due to PbI2Can be dissolved in water, the solubility depends on the temperature, hot PbI2The reduction of the solution temperature leads to PbI2The solubility in water decreases and the supersaturation of the solution gradually increases as the solvent evaporates, so that PbI2The crystal starts to grow. Maintaining a stable atmosphere and a slow growth rate during liquid phase growth is useful for obtaining high quality PbI2The crystal is critical. In order to inhibit the rapid evaporation of the water solvent, the present invention employs two simple control methods, i.e., adding water to a large culture dish to increase its partial pressure in the growth system to inhibit PbI2The evaporation rate of the solvent and the covering of the growth system to isolate the crystal growth environment from the atmosphere to some extent.
Example 1
1. Cutting a silicon wafer with a 300nm oxide layer into a plurality of square small blocks of 1cm × 1cm, and cleaning for later use;
2. placing the processed silicon wafer into a small uncovered culture dish, and then placing the small uncovered culture dish into a large culture dish with a small amount of deionized water;
3. the large culture dish is insulated at 20 ℃;
4. sucking 50 mu L of supersaturated aqueous solution of 2mg/mL lead iodide powder by using a pipette and dropping the supersaturated aqueous solution on the silicon wafer substrate;
5. covering the large culture dish, standing for about 10 minutes, and waiting for complete volatilization of the solvent to obtain the two-dimensional lead iodide nanosheets shown in figure 3.
The meandering in the photograph of fig. 3 is a phenomenon in which the metal probe jumps due to the rough particles on the surface of the sample.
Example 2
1. Cutting a silicon wafer with a 300nm oxide layer into a plurality of square small blocks of 1cm × 1cm, and cleaning for later use;
2. placing the processed silicon wafer into a small uncovered culture dish, and then placing the small uncovered culture dish into a large culture dish with a small amount of deionized water;
3. the large culture dish is insulated at 50 ℃;
4. sucking 50 mu L of supersaturated aqueous solution of 2mg/mL lead iodide powder by using a pipette and dropping the supersaturated aqueous solution on the silicon wafer substrate;
5. covering the large culture dish, standing for about 10 minutes, and waiting for complete volatilization of the solvent to obtain the two-dimensional lead iodide nanosheets shown in fig. 4.
The meandering in the photograph of fig. 4 is a phenomenon in which the metal probe jumps due to the rough particles on the surface of the sample.
Example 3
1. Cutting a silicon wafer with a 300nm oxide layer into a plurality of square small blocks of 1cm × 1cm, and cleaning for later use;
2. placing the processed silicon wafer into a small uncovered culture dish, and then placing the small uncovered culture dish into a large culture dish with a small amount of deionized water;
3. the large culture dish is insulated at 30 ℃;
4. sucking 50 mu L of supersaturated aqueous solution of 2mg/mL lead iodide powder by using a pipette and dropping the supersaturated aqueous solution on the silicon wafer substrate;
5. covering the large culture dish, standing for about 10 minutes, and waiting for the solvent to be completely volatilized to obtain the two-dimensional lead iodide nanosheets on the silicon wafer as shown in FIG. 5.
6. And respectively using glass, a PET film and a copper mesh carbon film as target substrates, repeating the steps, preserving heat at 30 ℃, and volatilizing the solvent to respectively obtain two-dimensional lead iodide nanosheets on the glass, the PET film and the copper mesh carbon film. Optical microscope photographs of the two-dimensional lead iodide nanosheets prepared on different substrates are shown in fig. 6.
The XPS test results of the two-dimensional lead iodide nanosheets on the silicon wafer of this example are shown in fig. 7a and 7b, and it was confirmed that PbI was present in X-ray photoelectron spectroscopy (XPS)2Composition of nano-flakes. As can be seen from the figure, Pb4f7/2And Pb4f5/2Has a binding energy of 138.0eV and 142.9eV, respectively, and I3d5/2And I3d3/2The binding energies of (a) and (b) are 618.9eV and 630.4eV, respectively.
The XRD test result of the two-dimensional lead iodide nanosheet on the silicon wafer of this example is shown in fig. 7c, and only the diffraction peak of the (00L) crystal plane can be observed (L ═ 1,2,3,4), which is very consistent with the standard JCPDS card (No.01-073-1-Kα2Peak separation, indicating growing PbI2Has high crystal quality.
The Raman test results of the two-dimensional lead iodide nanosheets on the silicon wafer of this example are shown in fig. 7d, where the Raman peaks are clear and the symmetric profile illustrates PbI2Has high quality. At 75cm-1Of (E)gPeak sum located at about 105cm-1The Eu peak at (A) is an in-plane (a plane composed of the a and b axes, also referred to as ab plane) vibration mode, A1gThe peak is located at 95cm-1A is2uLocated at about 113cm-1And represents the vibration of the I atom perpendicular to the ab plane (along the c-axis and perpendicular to the ab plane). Raman spectral characterization confirmed the composition of our samples, further validating the XRD results.
Application example
An ultraviolet detector was prepared using the two-dimensional lead iodide nanosheets on the silicon wafer prepared in example 3. The structure of the ultraviolet detector is schematically shown in fig. 8, and the physical photograph is shown in fig. 9. The invention characterizes the performance of the prepared lead iodide ultraviolet detector, the wavelength of incident light is 375nm ultraviolet light, and the characterization result is shown in figure 10.
FIG. 10a is a graph of the corresponding output curves in light and dark, at source-drain voltage VdsAt 5V, laser irradiation increased the current from 1.1nA in the dark to 63.7 nA. FIG. 10b is the corresponding transfer curve for the device in darkness and light, with back gate voltage VgGradually increase of IdsGradual decrease indicates PbI2The channel has the properties of a p-type semiconductor. FIGS. 10c and 10d show PbI at 375nm laser pulses2The photo-response behavior of the photodetector, with a rise time of 14.1ms and a decay time of 31.0 ms. Further, I in FIG. 10ddsThe-t curve shows a stable optical response over the repetition period of the laser pulse, indicating good photodetector stability.
The following parameters can be obtained by characterization: the photoresponsiveness (photoresponsiveness) was 0.51A W-1The external quantum effect (external quantum effect) is 168.9%, the response time comprises a rise time of 14.1ms and a decay time of 31.0ms, and the performance parameters show that the lead iodide ultraviolet detector has outstanding responsivity and response speed, can meet the requirements of practical application, and is suitable for arc detectors, flame detectors and the like.
Comparative example 1
1. Cutting a silicon wafer with a 300nm oxide layer into a plurality of square small blocks of 1cm × 1cm, and cleaning for later use;
2. placing the treated silicon wafer in a culture dish;
3. sucking 50 mu L of supersaturated aqueous solution of 2mg/mL lead iodide powder by using a pipette and dropping the supersaturated aqueous solution on the silicon wafer substrate;
4. and (3) adjusting the temperature of the lead iodide growth culture dish to rise from 30 ℃ to 150 ℃, and waiting for the solvent to be completely volatilized to obtain the two-dimensional lead iodide nanosheet.
As shown in fig. 11, the two-dimensional lead iodide nanosheet of the present comparative example has a rough surface and low crystal quality, which indicates that the lead iodide prepared by the existing liquid phase method has a rough surface.
Comparative example 2
1. Cutting a silicon wafer with a 300nm oxide layer into a plurality of square small blocks of 1cm × 1cm, and cleaning for later use;
2. placing the processed silicon wafer into a small uncovered culture dish, and then placing the small uncovered culture dish into a large culture dish with a small amount of deionized water;
3. sucking 50 mu L of supersaturated aqueous solution of 2mg/mL lead iodide powder by using a pipette and dropping the supersaturated aqueous solution on the silicon wafer substrate;
4. covering the large culture dish, adjusting the temperature of the lead iodide growth culture dish to rise from 30 ℃ to 150 ℃, and waiting for the solvent to be completely volatilized to obtain the two-dimensional lead iodide nanosheet.
As shown in fig. 12, the two-dimensional lead iodide nanosheet of the present comparative example has a rough surface, which indicates that temperature instability can cause solvent volatilization instability, thereby affecting the crystal quality of the prepared lead iodide.
Fig. 13a, 13d are atomic force microscope photographs of two-dimensional lead iodide nanoplates of comparative example 1, with line scan results as shown in fig. 13 g; fig. 13b, 13e are atomic force microscope photographs of two-dimensional lead iodide nanoplates of comparative example 2, with line scan results as shown in fig. 13 g; fig. 13c and 13f are atomic force microscope photographs of two-dimensional lead iodide nanoplates on a silicon wafer of example 3, with the line scan results shown in fig. 13 g. Therefore, the two-dimensional lead iodide nanosheet prepared by the preparation method disclosed by the invention is regular in shape, smooth in surface and high in crystal quality.
Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the above description of the present invention, and equivalents also fall within the scope of the invention as defined by the appended claims.
Claims (3)
1. A preparation method of a lead iodide nano material comprises the following steps:
(1) placing a target substrate in a cuvette;
(2) putting the small vessel into a large vessel filled with deionized water;
(3) transferring the supersaturated aqueous solution of lead iodide onto the target substrate, sealing the large vessel, and standing until the water on the target substrate is completely volatilized to obtain a two-dimensional lead iodide nano material;
and when standing, the temperature in the large vessel is 20-50 ℃.
2. The method of claim 1, wherein the temperature of the inside of the large vessel is 30 ℃ at rest.
3. The method of claim 1, wherein the target substrate is a silicon wafer, glass, a PET film, or a copper mesh carbon film.
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