CN110611015A - Preparation method and application of two-dimensional lead iodide sheet - Google Patents
Preparation method and application of two-dimensional lead iodide sheet Download PDFInfo
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- CN110611015A CN110611015A CN201910892389.8A CN201910892389A CN110611015A CN 110611015 A CN110611015 A CN 110611015A CN 201910892389 A CN201910892389 A CN 201910892389A CN 110611015 A CN110611015 A CN 110611015A
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- lead iodide
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- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 238000004140 cleaning Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000004528 spin coating Methods 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 24
- 229910052710 silicon Inorganic materials 0.000 claims description 24
- 239000010703 silicon Substances 0.000 claims description 24
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 6
- -1 oxygen ion Chemical class 0.000 claims description 6
- 229920002799 BoPET Polymers 0.000 claims description 4
- 239000002346 layers by function Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 239000002135 nanosheet Substances 0.000 description 8
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010420 art technique Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
-
- 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
Abstract
The invention discloses a preparation method and application of a two-dimensional lead iodide thin sheet. The preparation method comprises the following steps: cleaning the substrate; dropwise adding a quantitative supersaturated lead iodide aqueous solution on the cleaned substrate; and putting the substrate on a spin coater for spin coating, drying, and obtaining the two-dimensional lead iodide sheet after the aqueous solution on the substrate is completely volatilized. The preparation method provided by the invention is simple to operate, low in cost and environment-friendly, the two-dimensional lead iodide thin slices can be quickly prepared with high yield, the prepared two-dimensional lead iodide thin slices are large in size, smooth in surface and high in crystallization quality, and the two-dimensional lead iodide thin slices can be processed and applied to a photoelectric detector.
Description
Technical Field
The invention relates to the technical field of two-dimensional nano materials, in particular to a preparation method and application of a lead iodide nano material.
Background
The two-dimensional material is a layered nano material with nano size (less than 100nm) only in one dimension, atoms are combined by chemical bonds in a two-dimensional plane, and electrons move freely in the plane. When the material is thinned to two-dimensional dimensions, it tends to exhibit numerous unique and superior characteristics not specific to bulk materials. The unique properties of these two-dimensional materials, such as force, electricity, light, heat, magnetism, etc., have received extensive attention from both academic and industrial areas.
Lead iodide is a layered material, and van der waals force bonds are formed between layers, and iodine and lead are ionically bonded together in the layers. The forbidden band width of the lead iodide is 2.2-2.55 eV, the forbidden band width can be increased along with the reduction of the number of layers of the material, the lead iodide has the characteristic of adjustable band gap, and can be used as a precursor of hybrid perovskite, so that the lead iodide has important application in the fields of photoelectric detectors, lasers, solar cells and the like. And due to the characteristics of high resistance and high carrier mobility of the lead iodide, the photoelectric detector prepared from the lead iodide crystal has low leakage current, strong weak light resolution capability, excellent detection efficiency and outstanding stability.
The two-dimensional lead iodide can be prepared by vapor deposition, liquid phase stripping and mechanical cleavage. The size distribution of the lead iodide prepared by the vapor deposition process is uniform (1-7 mu m), the yield of the two-dimensional lead iodide is high (Yaguang Wang et al, Science Bulletin, volume 62, 1654 in 2017), but the size of the prepared two-dimensional lead iodide is small, vapor deposition equipment is needed, and high temperature and high-purity gas atmosphere are required. The liquid phase peeling method is a method for preparing a two-dimensional material by thinning through the action of liquid phase on the surface of the material and the action of ultrasound, and the method is simple to operate and low in cost, but the material is broken when the ultrasound is used for thinning, so that the size of the material is reduced, and the yield of the two-dimensional material is low (Chaolang Tan et al, Chemical reviews, vol 117, 6225 2017). The mechanical cleavage mode is simple to operate, equipment is basically not depended on, other reagents are not introduced in the preparation process, the quality of the prepared two-dimensional material is high, the yield is low, and the size and the shape of the two-dimensional material are uncontrollable. The above three preparation processes are effective for the preparation of a variety of two-dimensional materials.
Two-dimensional lead iodide flakes can also be prepared using a solution process for their properties. The solution method does not need higher preparation temperature, complex equipment and high-purity gas atmosphere, and has simple operation and low cost. However, the traditional solution method for preparing the two-dimensional lead iodide has the problems of small size (dozens of microns), low yield of the two-dimensional nanosheets, rough crystalline surface, low crystalline quality and the like. For the semiconductor material of lead iodide, the lower the surface roughness, the smoother the surface, and the more beneficial the performance of the lead iodide photoelectric device is to be improved.
Disclosure of Invention
In order to overcome the defects of the traditional solution method for preparing the two-dimensional lead iodide, the invention aims to provide the preparation method of the two-dimensional lead iodide slice, which is simple to operate, low in cost and environment-friendly.
The technical scheme adopted by the invention is as follows:
a preparation method of a two-dimensional lead iodide thin sheet comprises the following specific steps:
(1) cleaning the substrate;
(2) dropwise adding a quantitative supersaturated lead iodide aqueous solution on the cleaned substrate;
(3) and (3) spin-coating the substrate obtained in the step (2) on a spin coater at a certain rotating speed, and then drying to obtain the two-dimensional lead iodide slice.
Further, in the step (1), the substrate is a silicon wafer, glass or a PET film.
Further, in the step (1), an oxygen ion cleaning process is adopted for cleaning.
Further, the power of the oxygen ion cleaning is 10W to 700W.
Further, the time for oxygen ion cleaning is 5s to 600 s.
Furthermore, in the step (2), the dosage of the supersaturated lead iodide aqueous solution is 5 to 800 μ L.
Furthermore, in the step (3), the spin coating speed is 100 r/min-3000 r/min.
Further, in the step (3), the spin coating time is 5s to 30 s.
Further, in the step (3), the drying temperature is 5 ℃ to 60 ℃.
The invention also provides application of the two-dimensional lead iodide thin sheet prepared by the method in a photoelectric detector.
Compared with the prior art, the invention has the main advantages that:
(1) the method for preparing the two-dimensional lead iodide thin sheet has the advantages of simple process operation, low cost, environmental protection and high efficiency.
(2) The preparation method can prepare the two-dimensional lead iodide thin sheet with large size (over hundred microns), regular shape, smooth surface and high crystallization quality in high yield.
(3) The two-dimensional lead iodide photoelectric detector can be prepared by using the two-dimensional lead iodide thin sheet provided by the invention for photoelectric detection, and the performance of the device is improved.
Drawings
Fig. 1 is a schematic flow chart of the invention for preparing two-dimensional lead iodide flakes, wherein: 1-substrate, 2-oxygen ion cleaning process, 3-supersaturated lead iodide aqueous solution, 4-cleaned substrate, 5-liquid transfer gun and 6-spin coater.
Fig. 2 is (a) an optical photograph, (b) an atomic force microscope thickness test, and (c) a surface roughness test chart of the two-dimensional lead iodide flakes prepared in example 1.
Fig. 3 is an XRD pattern of a two-dimensional lead iodide thin sheet prepared on a silicon wafer in example 3.
Fig. 4 is a statistical chart of the size distribution of two-dimensional lead iodide flakes prepared in example 5.
Fig. 5 is a schematic flow chart of a process for preparing lead iodide nanosheets by the conventional solution method in example 8.
Fig. 6 is an optical photograph, (a) an atomic force microscope thickness test, and (c) a surface roughness test chart of the lead iodide nanosheet prepared in example 8.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted that technical features or combinations of technical features described in the following embodiments should not be considered in isolation, and they may be combined with each other to achieve better technical effects. In the drawings of the embodiments described below, the same reference numerals appearing in the respective drawings denote the same features or components, and may be applied to different embodiments.
The two-dimensional lead iodide flakes of the following examples and application examples were prepared as shown in fig. 1, and the substrate 1 was cleaned by a plasma resist remover or plasma cleaner 2. A saturated aqueous solution 3 of lead iodide was prepared. A quantitative amount of lead iodide solution was dropped on the substrate 4 after the washing treatment using a pipette gun 5. Spin-coating with a spin coater 6 followed by drying, a two-dimensional lead iodide thin sheet was prepared.
Example 1
The silicon wafer with 285nm silicon dioxide is cut into a plurality of square small pieces with the size of 1cm multiplied by 1cm, and the square small pieces are cleaned and dried for standby. The cleaned silicon wafer was cleaned with a plasma resist remover 50W for 180 seconds, and 100. mu.L of a supersaturated aqueous solution of lead iodide (2mg/mL) was dropped on the treated silicon wafer. And spin-coating the silicon wafer with the lead iodide solution on a spin coater at the rotating speed of 300r/min for 30s, and then drying the sample at 25 ℃ to obtain the two-dimensional lead iodide thin sheet.
Example 2
The silicon wafer with 285nm silicon dioxide is cut into a plurality of square small pieces with the size of 1cm multiplied by 1cm, and the square small pieces are cleaned and dried for standby. The cleaned silicon wafer was cleaned with 180W plasma resist remover for 120 seconds, and 50. mu.L of supersaturated aqueous lead iodide solution (2mg/mL) was added dropwise to the treated silicon wafer. And spin-coating the silicon wafer with the lead iodide solution on a spin coater at the rotating speed of 300r/min for 30s, and then drying the sample at 25 ℃ to obtain the two-dimensional lead iodide thin sheet.
Example 3
The silicon wafer with 285nm silicon dioxide is cut into a plurality of square small pieces with the size of 1cm multiplied by 1cm, and the square small pieces are cleaned and dried for standby. The cleaned silicon wafer was cleaned with 400W plasma resist remover for 60 seconds, and 300. mu.L of supersaturated aqueous lead iodide solution (4mg/mL) was dropped on the treated silicon wafer. And spin-coating the silicon wafer with the lead iodide solution on a spin coater at the rotating speed of 1000r/min for 20s, and then drying the sample at 50 ℃ to obtain the two-dimensional lead iodide thin sheet.
Example 4
The silicon wafer with 285nm silicon dioxide is cut into a plurality of square small pieces with the size of 1cm multiplied by 1cm, and the square small pieces are cleaned and dried for standby. The cleaned silicon wafer was cleaned with 10W plasma cleaner for 500 seconds, and 150. mu.L of supersaturated aqueous lead iodide solution (1mg/mL) was dropped on the treated silicon wafer. And spin-coating the silicon wafer with the lead iodide solution on a spin coater at the rotating speed of 3000r/min for 10s, and then drying the sample at 20 ℃ to obtain the two-dimensional lead iodide slice.
Example 5
The glass is cut into square small pieces of 1cm multiplied by 1cm, and the small pieces are cleaned and dried for standby. The cleaned glass piece was cleaned with a plasma cleaner 700W for 100 seconds, and 150. mu.L of a supersaturated aqueous solution of lead iodide (2mg/mL) was dropped onto the treated glass piece. And spin-coating the silicon wafer with the lead iodide solution on a spin coater at the rotating speed of 1200r/min for 10s, and then drying the sample at 50 ℃ to obtain the two-dimensional lead iodide slice.
Example 6
Cutting the PET film into a plurality of square small pieces of 1cm multiplied by 1cm, and cleaning and drying the small pieces for later use. The washed PET film was washed with 300W for 120 seconds by a plasma washer, and 200. mu.L of a supersaturated aqueous solution of lead iodide (2mg/mL) was dropped onto the treated glass sheet. And spin-coating the silicon wafer with the lead iodide solution on a spin coater at the rotating speed of 1500r/min for 5s, and then drying the sample at 25 ℃ to obtain the two-dimensional lead iodide slice.
Example 7
The two-dimensional lead iodide nanoplates prepared in example 1 were used to prepare photodetectors. A two-dimensional lead iodide sheet is used as a photosensitive functional layer of a photoelectric detector, and the photoelectric detector realizes photoelectric detection by using a device structure of a conventional field effect transistor. The fabrication of field effect transistors and related substrates, source drain electrodes, gates, insulating layers, etc. may all employ prior art techniques.
Fig. 2 shows the results of the optical photograph, the corresponding atomic force microscope thickness test, and the surface roughness test of the two-dimensional lead iodide flake prepared in example 1. The two-dimensional lead iodide flake has a size of 188um, a thickness of 80nm and a root mean square roughness RMS of 0.9nm, and it is known that the surface is smooth and the crystal quality is also high.
The XRD pattern of the two-dimensional lead iodide thin sheet prepared on the silicon wafer in example 3 is shown in fig. 3. All diffraction peaks were consistent with the standard ratio of lead iodide to the card JCPDS 07-0235. And not only the shape of the diffraction peak is sharp, but also (003) (004) produces obvious diffraction peak broadening, which indicates that the two-dimensional lead iodide flake has excellent crystallinity.
The statistics of the size distribution of the two-dimensional lead iodide flakes prepared in this example 5 are shown in fig. 4. It can be seen that two-dimensional lead iodide with a size of over 100 μm can be prepared by the preparation method of the present invention, and the maximum size can be close to 300 μm.
Example 8
In order to embody the beneficial effects of the present invention, the present embodiment adopts a traditional solution method to prepare lead iodide nanosheets for comparison. As shown in fig. 5, the specific preparation process is as follows: cutting a silicon wafer with 285nm silicon dioxide into a plurality of square small pieces of 1cm multiplied by 1cm, and cleaning and drying the small pieces for later use; dripping 100 mu L of supersaturated lead iodide aqueous solution (2mg/mL) at 90 ℃ on a silicon wafer; and obtaining the lead iodide nanosheet after the solution is completely volatilized.
Fig. 6 is a result of a test performed on a lead iodide polygon prepared by a conventional solution method. As can be seen from the figure, the thickness of the lead iodide nanosheet is 576nm, the lead iodide nanosheet does not have two-dimensional thickness, the surface lines are surface concave-convex fluctuation, the fluctuation range can reach 234nm, and the root mean square roughness RMS is 61 nm. Therefore, the lead iodide nanosheet prepared by the traditional solution method is thick, difficult to achieve two-dimensional thickness, not large enough (dozens of micrometers) in size, large in surface undulation, not smooth enough and not high in crystallization quality. The method of the present invention can solve the above problems well.
Claims (10)
1. A preparation method of a two-dimensional lead iodide thin sheet is characterized by comprising the following specific steps:
(1) cleaning the substrate;
(2) dropwise adding a quantitative supersaturated lead iodide aqueous solution on the cleaned substrate;
(3) and (3) spin-coating the substrate obtained in the step (2) on a spin coater at a certain rotating speed, and then drying to obtain the two-dimensional lead iodide slice.
2. The method of claim 1, wherein in step (1), the substrate is a silicon wafer, glass or PET film.
3. The method for preparing two-dimensional lead iodide flakes according to claim 1, wherein in step (1), an oxygen ion cleaning process is used for cleaning.
4. The method of claim 3, wherein the power of the oxygen ion cleaning is 10W to 700W.
5. The method of claim 3, wherein the time for the oxygen ion cleaning is 5 to 600 seconds.
6. The method of claim 1, wherein the supersaturated aqueous solution of lead iodide used in step (2) is used in an amount of 5 to 800. mu.L.
7. The method of claim 1, wherein in the step (3), the spin coating speed is 100-3000 r/min.
8. The method for preparing a two-dimensional lead iodide flake according to claim 1, wherein in the step (3), the spin coating time is 5s to 30 s.
9. The method of claim 1, wherein the drying temperature in step (3) is 5 to 60 ℃.
10. Use of a two-dimensional lead iodide flake prepared according to claim 1, characterized in that the two-dimensional lead iodide flake is used as a light-sensitive functional layer of a photodetector.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114772633A (en) * | 2022-04-25 | 2022-07-22 | 深圳大学 | Corner double-layer lead iodide two-dimensional nano material and preparation method thereof |
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| JP2005268452A (en) * | 2004-03-17 | 2005-09-29 | Toshiba Corp | Radiation detector |
| CN108360067A (en) * | 2018-02-26 | 2018-08-03 | 深圳大学 | A kind of ultra-thin two-dimension PbI2The preparation method of monocrystalline |
| CN109355708A (en) * | 2018-10-29 | 2019-02-19 | 天津理工大学 | A kind of two-dimentional hydridization perovskite crystal growing method of space limitation |
| CN110104675A (en) * | 2019-04-16 | 2019-08-09 | 浙江大学 | A kind of lead iodide nano material and its preparation method and application |
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- 2019-09-20 CN CN201910892389.8A patent/CN110611015B/en active Active
Patent Citations (4)
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| JP2005268452A (en) * | 2004-03-17 | 2005-09-29 | Toshiba Corp | Radiation detector |
| CN108360067A (en) * | 2018-02-26 | 2018-08-03 | 深圳大学 | A kind of ultra-thin two-dimension PbI2The preparation method of monocrystalline |
| CN109355708A (en) * | 2018-10-29 | 2019-02-19 | 天津理工大学 | A kind of two-dimentional hydridization perovskite crystal growing method of space limitation |
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Non-Patent Citations (1)
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| MEAGAN V. KELSO1等: "Spin coating epitaxial films", 《SCIENCE》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114772633A (en) * | 2022-04-25 | 2022-07-22 | 深圳大学 | Corner double-layer lead iodide two-dimensional nano material and preparation method thereof |
| CN114772633B (en) * | 2022-04-25 | 2022-10-11 | 深圳大学 | Corner double-layer lead iodide two-dimensional nano material and preparation method thereof |
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