CN111807409A - Preparation method and application of semiconductor photoelectric material of silicon wafer-based bismuth sulfide nanoflower array - Google Patents
Preparation method and application of semiconductor photoelectric material of silicon wafer-based bismuth sulfide nanoflower array Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 63
- 239000010703 silicon Substances 0.000 title claims abstract description 63
- 239000002057 nanoflower Substances 0.000 title claims abstract description 40
- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000004065 semiconductor Substances 0.000 title description 6
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 235000012431 wafers Nutrition 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 230000035945 sensitivity Effects 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- ABEBSOCCFCCWFY-UHFFFAOYSA-N 3-[2-(4-methylphenyl)sulfanylethyl]oxadiazol-3-ium-5-olate Chemical compound C1=CC(C)=CC=C1SCC[N+]1=NOC([O-])=C1 ABEBSOCCFCCWFY-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 229960000583 acetic acid Drugs 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 239000007810 chemical reaction solvent Substances 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000012362 glacial acetic acid Substances 0.000 claims description 2
- 230000000640 hydroxylating effect Effects 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- FGHSTPNOXKDLKU-UHFFFAOYSA-N nitric acid;hydrate Chemical group O.O[N+]([O-])=O FGHSTPNOXKDLKU-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 3
- 150000004763 sulfides Chemical class 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002074 nanoribbon Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004098 selected area electron diffraction Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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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
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02367—Substrates
- H01L21/0237—Materials
- H01L21/02373—Group 14 semiconducting materials
- H01L21/02381—Silicon, silicon germanium, germanium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02568—Chalcogenide semiconducting materials not being oxides, e.g. ternary compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02587—Structure
- H01L21/0259—Microstructure
- H01L21/02601—Nanoparticles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention belongs to the technical field of chemical materials, and particularly relates to a preparation method and application of a silicon wafer-based bismuth sulfide nanoflower array. The method comprises the following steps: the bismuth sulfide nanoflower array can be assembled on the silicon wafer substrate through a simple hydrothermal method, and the silicon wafer substrate bismuth sulfide array structure is obtained through full and drying treatment. The bismuth sulfide nanometer flower crystal grown on the silicon chip has uniform appearance, the size of about 800nm and the chemical formula of Bi2S3The method has simple and convenient process and universality, and can be used for preparing other sulfides. The prepared bismuth sulfide nanoflower array has great application prospect in the fields of photoelectric detectors, field emission and the like.
Description
Technical Field
The invention belongs to the technical field of chemical material synthesis, and particularly relates to a preparation method of a silicon wafer-based bismuth sulfide nanoflower array semiconductor photoelectric material and application of the semiconductor photoelectric material in photoelectric detection.
Background
In recent years, the application of specially designed nano materials with various structures in a plurality of construction modules of nano devices and nano systems is more and more prominent, so people pay more and more attention to the research on the preparation process of the nano materials. The study of nanostructures also ranges from simple structures to the assembly of ordered structures, with the aim of achieving increased structural complexity and functionality. For example, a four-footed structure may be an important alternative structure for fiber and rod structures due to the multi-branched mechanical strengthening advantages, and multi-branched nanocrystals also have many advantages because they not only have all the performance characteristics of one-dimensional structural materials, but also have the advantages of hierarchical structures. However, developing a simple, novel hierarchical structure building method still has significant challenges.
Bismuth sulfide (Bi)2S3) Is a direct band gap semiconductor with a bandwidth Eg of 1.3 eV. The earliest reports on the photoconductive properties of bismuth sulfide were based on studies of mineral samples bismuthate in 1917. The importance of bismuth sulfide in the earliest batch of photoconductive materials was also described in 1920. Large-sized grain films of bismuth sulfide have been applied to electronic devices due to the forbidden band width of 1.25eV to 1.7 eV. Up to now, Bi2S3Nanoribbon, snowflake-shaped Bi2S3Nanorods, nanowires and nanoflowers have been successfully prepared by microwave ionic liquid methods, solvothermal methods, hydrothermal solutions and microemulsions. It can be seen, however, that most of the reactions of these methods are in solution, producing Bi2S3The nanomaterial is in a powder non-ordered form, and the existing form greatly limits Bi2S3And detecting the photoconductive characteristic of the nanostructure. Because of this, so far little can be seen about Bi2S3The photoelectric response nano structure is used for reporting of photoelectric devices, although the semiconductor material has good photoelectric effect, not to mention the specially constructed hierarchical structure.
The volume expansion phenomenon of different degrees not only destroys the structural stability of the electrode material and deteriorates the contact of the electrode material with an active material, but also further rapidly attenuates the capacity of the lithium ion battery. In order to better solve this problem, researchers have tried to combine a metallic negative electrode with a buffer system to eliminate the adverse effects of the volume expansion phenomenon, and sulfides have been receiving much attention as buffer materials due to their excellent mechanical and thermodynamic stability.
The invention provides a preparation method of a silicon chip-based bismuth sulfide nanoflower array with simple and convenient process and certain universality, the morphology is uniform and controllable, the crystallinity of the flaky bismuth sulfide forming the nanoflower is good, and the characterization of the photoelectric response performance of the nanoflower shows that the nanoflower has very high sensitivity to simulated sunlight. The light-induced conductivity makes it a reversible opto-electric switch, similar to an optical switch commonly used for electrical control. The array structure is shown to be used for creating a highly sensitive photoelectric detector, and an optical switch, and has a wide application prospect in the aspects of novel micro-nano electronic equipment and optoelectronic equipment.
Disclosure of Invention
Aiming at the defects in the existing synthesis technology of sulfide nano array structure materials, the invention provides a silicon chip-based bismuth sulfide nano flower array material which is simple and convenient to operate, safe and environment-friendly, a preparation method thereof and application in photoelectric detection.
The invention provides a preparation method of a silicon chip-based bismuth sulfide nanoflower array material, which comprises the following specific steps:
1. a preparation method of a silicon chip-based bismuth sulfide nanoflower array is characterized by comprising the following specific steps:
(1) cleaning, hydroxylating and surface sulfhydrylation modification of a silicon wafer, firstly cutting the silicon wafer into a set size, respectively carrying out ultrasonic treatment for 20mins by using acetone, ethanol and deionized water in sequence, blow-drying by using a blower with cold air, and then placing the silicon wafer into a concentrated sulfuric acid solution (30% H) prepared in advance2O2And concentrated H2SO4The volume ratio is 3: 7) and standing in an oven at 90 ℃ for 30mins, wherein the step is to hydroxylate the surface of the silicon wafer. After the completion of the reaction, the mixture was thoroughly washed with ionized water, blow-dried with nitrogen gas, and then placed in a 2 vol% 3-MPTES solution, and the dispersion solvent was dissolved in waterProduct ratio 9: 1, adding all silicon wafers into the mixed solution of ethanol and water, dropwise adding a plurality of drops of glacial acetic acid for catalytic reaction, and sealing and standing for 24 hours at room temperature. And finally, taking out the silicon wafer modified with the sulfydryl, washing with absolute ethyl alcohol, and blowing with nitrogen flow for later use.
(2) Growth of Bi on thiolated silicon substrates by hydrothermal method2S3The nano flower array: first, a reaction solution was prepared by mixing 10mL of 0.1M Bi (NO)3)3The solution was mixed with 60mL of 0.1M NH2CSNH2To the solution, 1M nitric acid solution was added dropwise with stirring to adjust the pH to 0.5. And then fixing the processed silicon wafer substrate with the front side facing downwards on a customized silicon wafer fixing device, placing the silicon wafer substrate into a 100mL polytetrafluoroethylene reaction kettle inner container, and adding 70mL prepared reaction solvent. Sealing and placing in an oven at 150 ℃ for reaction for 24 h.
(3) And washing and drying to obtain the silicon wafer-based bismuth sulfide nanoflower array material.
In the invention, the prepared silicon chip-based bismuth sulfide nanoflower array has bismuth sulfide nanoflower crystals grown on the silicon chip, uniform appearance, size of about 800nm and chemical formula of Bi2S3。
In the preparation method of the silicon wafer-based bismuth sulfide nanoflower array material, the soluble salt adopts hydrated nitrate (Bi (NO)3)3·5H2O), thiourea (NH)2CSNH2) The reagent is analytically pure, and all the water is deionized water; concentrated sulfuric acid and concentrated nitric acid, wherein the ethanol is commercial grade absolute ethanol, and the mass fraction is more than or equal to 99.8%.
The preparation method of the silicon wafer-based bismuth sulfide nanoflower array is characterized by comprising two steps, wherein the first step is modification of a substrate silicon wafer, and in the process, except soaking and drying processes, other steps are stored in a vacuum box and are not placed in the air for a long time; in the second step of the bismuth sulfide nanoflower array growth process, the front surface (the surface modified with sulfydryl) of the silicon wafer is ensured to face downwards, and bismuth sulfide and the like formed in the solution in the growth process are prevented from sinking on the silicon wafer. In the two-step operation process, all the silicon wafer cleaning processes are full soaking and light leaching, and all the drying processes are blown dry by using nitrogen flow. The invention also provides application of the silicon chip-based bismuth sulfide nanoflower array in photoelectric performance.
Compared with the prior art, the invention has the technical effects that:
1. the chemical modification method and the hydrothermal synthesis process are simple and convenient and have certain universality.
2. The silicon chip-based bismuth sulfide nanoflower array obtained by the invention has the advantages that bismuth sulfide nanoflower crystals grown on the silicon chip are uniform in appearance, about 800nm in size and Bi in chemical formula2S3. The structure not only has the size effect of a nano-sized structure, but also has higher specific surface area and multiple active sites; meanwhile, the structure also has the synergistic effect of a stepped structure, and the nano-sheet structure assembled in a flower shape can receive light sources in different directions, so that the sensitivity of the structural material to light can be increased.
3. The single particle layer array structure is densely and uniformly arranged in an array manner, and the utilization rate and efficiency of materials are utilized to the maximum extent. The possibility and optical switch for creating highly sensitive photodetectors have great application prospects in novel micro-nano electronic and optoelectronic devices.
Drawings
FIG. 1(a) shows Bi on a silicon wafer substrate2S3The distribution of the nano flower array can be seen as Bi2S3The nanoflowers are densely and uniformly distributed on the silicon wafer substrate. FIG. 1(b) is a view of preparing a silicon wafer-based Bi2S3And (3) characterizing the sensitivity of the nanoflower array to the light of the xenon lamp. When the lamp is switched on, the lamp current increases linearly to 4.4 μ a. Once the lamp is off, the current drops immediately. Showing very sensitive light detection, the on/off sensing is repeated many times without significant degradation.
FIG. 2 shows Bi grown on a silicon wafer2S3SEM image of the nanometer flower, and flower-shaped appearance characteristics can be seen from the image.
FIG. 3(a) is ultrasonic Bi prepared2S3Bi obtained from nanoflower2S3A projection electron microscope photograph of the lamellar structure, and (b) a corresponding selected area electron diffraction. The clear electron diffraction pattern illustrates Bi2S3Good crystallinity.
FIG. 4 shows the Bi-based silicon wafer prepared2S3An X-ray powder diffraction pattern of the nanoflower array. The one-to-one correspondence of diffraction peaks proves that Bi is in the fully-washed silicon wafer base2S3Other impurities are not present in the nanoflower array.
Claims (5)
1. A preparation method of a silicon chip-based bismuth sulfide nanoflower array is characterized by comprising the following specific steps:
(1) cleaning, hydroxylating and surface sulfhydrylation modification of a silicon wafer: firstly, cutting a silicon wafer into a set size, respectively carrying out ultrasonic treatment for 20mins by using acetone, ethanol and deionized water in sequence, drying the silicon wafer by using a blower with cold air, and then placing the silicon wafer into a concentrated sulfuric acid solution (30% H) prepared in advance2O2And concentrated H2SO4The volume ratio is 3: 7) and (3) standing in an oven at 90 ℃ for 30nins, wherein the step is to hydroxylate the surface of the silicon wafer. After the reaction is finished, fully washing with ionized water, drying by using nitrogen, and then putting into a 2 vol% 3-MPTES solution, wherein the volume ratio of a dispersion solvent is 9: 1, adding all silicon wafers into the mixed solution of ethanol and water, dropwise adding a plurality of drops of glacial acetic acid for catalytic reaction, and sealing and standing for 24 hours at room temperature. And finally, taking out the silicon wafer modified with the sulfydryl, washing with absolute ethyl alcohol, and blowing with nitrogen flow for later use.
(2) Growth of Bi on thiolated silicon substrates by hydrothermal method2S3The nano flower array: first, a reaction solution was prepared by mixing 10mL of 0.1M Bi (NO)3)3The solution was mixed with 60mL of 0.1M NH2CSNH2To the solution, 1M nitric acid solution was added dropwise with stirring to adjust the pH to 0.5. And then fixing the processed silicon wafer substrate with the front side facing downwards on a customized silicon wafer fixing device, placing the silicon wafer substrate into a 100mL polytetrafluoroethylene reaction kettle inner container, and adding 70mL prepared reaction solvent. Sealing and placing in an oven at 150 ℃ for reaction for 24 h.
(3) And washing and drying to obtain the silicon wafer-based bismuth sulfide nanoflower array material.
2. The method for preparing the silicon wafer-based bismuth sulfide nanoflower array material according to claim 1, wherein the soluble salt is nitrate hydrate (Bi (NO)3)3·5H2O), thiourea (NH)2CSNH2) The reagent is analytically pure, and all the water is deionized water; concentrated sulfuric acid and concentrated nitric acid, wherein the ethanol is commercial grade absolute ethanol, and the mass fraction is more than or equal to 99.8%.
3. The method for preparing a silicon wafer-based bismuth sulfide nanoflower array according to claim 1, wherein the method comprises two steps, wherein the first step is modification of a substrate silicon wafer, and in the process, except for the soaking and drying processes, the rest of the substrate silicon wafer is stored in a vacuum chamber and is not placed in the air for a long time; in the second step of the bismuth sulfide nanoflower array growth process, the front surface (the surface modified with sulfydryl) of the silicon wafer is ensured to face downwards, and bismuth sulfide and the like formed in the solution in the growth process are prevented from sinking on the silicon wafer. In the two-step operation process, all the silicon wafer cleaning processes are full soaking and light leaching, and all the drying processes are blown dry by using nitrogen flow.
4. The silicon wafer-based bismuth sulfide nanoflower array obtained by the production method according to claims 1 to 3.
5. The silicon wafer-based bismuth sulfide nanoflower array according to claim 4, wherein the application of the silicon wafer-based bismuth sulfide nanoflower array in a photodetector is realized by characterizing the sensitivity of the photoelectric response of the silicon wafer-based bismuth sulfide nanoflower array.
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| CN102965735A (en) * | 2012-11-16 | 2013-03-13 | 杭州师范大学 | Synthesis method of bismuth sulfide nanorod arrays with length-diameter ratios regulated and controlled by solvent hydrothermal method |
| CN106477629A (en) * | 2016-10-08 | 2017-03-08 | 江苏大学 | A kind of bismuth sulfide classifying nano flower electrode material for super capacitor and preparation method |
| CN111185196A (en) * | 2020-01-09 | 2020-05-22 | 南京工业大学 | Bamboo-leaf-shaped bismuth sulfide nano-sheet catalytic material and preparation method and application thereof |
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| CN106477629A (en) * | 2016-10-08 | 2017-03-08 | 江苏大学 | A kind of bismuth sulfide classifying nano flower electrode material for super capacitor and preparation method |
| CN111185196A (en) * | 2020-01-09 | 2020-05-22 | 南京工业大学 | Bamboo-leaf-shaped bismuth sulfide nano-sheet catalytic material and preparation method and application thereof |
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| YINGCHANG JIANG等: "Inducing nucleation and growth of chalcogenide nanostructures on silicon wafers" * |
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