CN112811462A - Tin sulfide (SnS) @ niobium disulfide (NbS)2) Core-shell heterojunction and preparation method and application thereof - Google Patents
Tin sulfide (SnS) @ niobium disulfide (NbS)2) Core-shell heterojunction and preparation method and application thereof Download PDFInfo
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- 239000011258 core-shell material Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- AFNRRBXCCXDRPS-UHFFFAOYSA-N tin(ii) sulfide Chemical compound [Sn]=S AFNRRBXCCXDRPS-UHFFFAOYSA-N 0.000 title claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims abstract description 34
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims abstract description 14
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 13
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000004729 solvothermal method Methods 0.000 claims abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 3
- 239000004094 surface-active agent Substances 0.000 claims abstract description 3
- 229910020042 NbS2 Inorganic materials 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 28
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 26
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 11
- 239000012300 argon atmosphere Substances 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000007872 degassing Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- 238000004073 vulcanization Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 3
- WOJGNYNEEVGGGM-UHFFFAOYSA-N O.O.O.O.O.[Sn] Chemical compound O.O.O.O.O.[Sn] WOJGNYNEEVGGGM-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 16
- 239000000047 product Substances 0.000 description 12
- 239000004065 semiconductor Substances 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 5
- 230000005669 field effect Effects 0.000 description 5
- 239000012456 homogeneous solution Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 238000000370 laser capture micro-dissection Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000002207 thermal evaporation Methods 0.000 description 2
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 chalcogenide compounds Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J1/00—Photometry, e.g. photographic exposure meter
- G01J1/42—Photometry, e.g. photographic exposure meter using electric radiation detectors
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- 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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- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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Abstract
The invention discloses tin sulfide (SnS) @ niobium disulfide (NbS)2) A preparation method and application of a core-shell heterojunction belong to the technical field of functional nano material preparation. The SnS @ NbS is synthesized by taking niobium pentachloride, tin tetrachloride pentahydrate and carbon disulfide as raw materials and oleylamine as a solvent, a reducing agent and a surfactant through a solvothermal method2A core-shell heterojunction; and (4) dripping the ethanol solution of the heterojunction on the interdigital electrode to prepare the corresponding photoelectric detector.
Description
Technical Field
The invention relates to SnS @ NbS2A preparation method and application of a core-shell heterojunction, belonging to the technical field of functional nano-material preparation.
Technical Field
Layered metal chalcogenide compounds, LMCs) is a typical two-dimensional material that has received much attention due to its great potential in the next generation of electronic and optoelectronic fields. Compared with the currently mainly researched n-type semiconductor LMCs (such as molybdenum disulfide (MoS)2) And tungsten disulfide (WS)2) Etc.), tin sulfide (SnS) is a few natural p-type semiconductor with an indirect bandgap of 1.1eV and a direct bandgap of 1.3 eV. In recent years, the SnS is widely researched due to the low processing cost, no toxicity, abundant earth reserves, good stability and excellent electronic, optical and photoelectric properties. Currently, the SnS has been successfully applied in the fields of solar cells, batteries, photodetectors, and the like.
Similar to many semiconductor LCMs, the performance of SnS-based electronic/optoelectronic devices can be affected by contact resistance. For semiconductor LMCs, a metal/semiconductor heterojunction is constructed, the Fermi level pinning effect can be effectively weakened, the Schottky barrier is adjusted, and then the contact resistance is reduced. Semiconductor and noble metals (such as gold (Au) and platinum (Pt)) are combined to construct a metal/semiconductor heterojunction, which reduces the contact resistance, but the method is expensive. Since the electrical properties of LCMs are closely related to their composition or crystalline phase, LCMs are capable of constructing heterostructures containing metallic and semiconducting LMCs (e.g., NbS)2/WS2And 1T/2H Mo1-xWxS2Metal/semiconductor heterojunctions, etc.), reducing their contact resistance. The method is convenient, effective and low in cost. Therefore, the construction of the metal LMC and semiconductor SnS heterostructure has great significance for various photoelectric devices based on SnS.
Disclosure of Invention
In order to solve the technical problem, the invention provides SnS @ NbS2A preparation method of the core-shell heterojunction, namely, metallic NbS2Combined with SnS to construct SnS @ NbS2The core-shell heterojunction reduces the contact resistance of SnS and is applied to the photoelectric detector.
The technical scheme proposed for solving the technical problems is as follows: tin sulfide (SnS) @ niobium disulfide (NbS)2) The preparation method of the core-shell heterojunction comprises the following steps:
(1) dissolving niobium pentachloride and tin tetrachloride pentahydrate in a molar ratio of 2: 8-4: 6 in oleylamine, and degassing at high temperature;
(2) further heating the solution, then injecting carbon disulfide for vulcanization, wherein the vulcanization temperature is 300-350 ℃, and obtaining SnS @ NbS2A core-shell heterojunction;
(3) the obtained SnS @ NbS in the step (2) is treated2And adding a mixed solution of ethanol, isopropanol and n-hexane into the core-shell heterojunction for washing, washing with a washing solution, and dispersing in the dispersion liquid.
Preferably, SnS @ NbS in the step (1)2The preparation method of the core-shell heterojunction adopts niobium pentachloride and stannic chloride pentahydrate as raw materials and synthesizes the raw materials by a solvothermal method.
Preferably, in the step (1), oleylamine is used as a solvent, a reducing agent and a surfactant.
Preferably, in the step (1), the degassing temperature is 100-150 ℃, and the degassing time is 10-20 min.
Preferably, the method comprises the following steps: in the step (2), carbon disulfide is used as a sulfur source, and the reaction time is 15 min-3 h.
Preferably, in the step (3), the washing solution is one or more of ethanol, isopropanol or n-hexane, and the dispersion solution is ethanol, methanol or a volatile water solvent.
Preferably, 0.23mmol × 0.3 niobium pentachloride and 0.23mmol × 0.7 tin pentahydrate tetrachloride are dissolved in 20ml oleylamine, degassed at 100 deg.C for 15 minutes under argon atmosphere, heated to 300 deg.C, and 8mmol of carbon disulfide are injected into the solution via syringe and vulcanized for 1 hour to obtain SnS @ NbS2The shape of the core-shell heterojunction is optimal.
The technical scheme proposed for solving the other technical problem is as follows: SnS @ NbS prepared according to any one of the methods described above2A core-shell heterojunction.
The technical scheme proposed for solving the other technical problem is as follows: the SnS @ NbS2The application of the core-shell heterojunction can be applied to a photoelectric detector or a logic switch.
It is preferable thatSnS @ NbS2And (3) dripping the dispersion liquid of the core-shell heterojunction on the surface of the electrode, and drying to obtain the electrode applied to the photoelectric detector.
The invention has the beneficial effects that:
1. in the invention, SnS @ NbS is prepared by a solvothermal method2Compared with the common chemical vapor deposition method, the core-shell heterojunction has the advantages of lower temperature, low energy consumption and easy mass production.
2. SnS @ NbS prepared by the invention2The precursor of the core-shell heterojunction is niobium pentachloride and stannic chloride pentahydrate, the molar ratio is 4:6 to 2:8, and SnS @ NbS cannot be obtained if the molar ratio in the interval is not selected2A core-shell heterojunction.
3. The SnS @ NbS2 core-shell heterojunction prepared by the method has the vulcanization reaction temperature of 300-350 ℃, and cannot obtain the SnS @ NbS2 core-shell heterojunction when the vulcanization reaction temperature is lower than 300 ℃ or higher than 350 ℃.
4. SnS @ NbS of the invention2The core-shell heterojunction is a metal/semiconductor heterojunction, has lower contact resistance, can reach the performance of a noble metal/semiconductor heterojunction, and has lower cost.
5. SnS @ NbS of the invention2The core-shell heterogeneous material has excellent photoelectric properties and can be used for photoelectric detectors.
6. Niobium pentachloride 0.23mmol × 0.3 and tin pentahydrate 0.23mmol × 0.7 were dissolved in 20ml oleylamine, degassed at 100 deg.C for 15 minutes under argon atmosphere, then heated to 300 deg.C, 8mmol of carbon disulfide were injected into the solution via syringe and vulcanized for 1 hour to obtain SnS @ NbS2The shape of the core-shell heterojunction is optimal.
Drawings
FIG. 1 shows SnS @ NbS in example 12Scanning electron microscopy of core-shell heterojunctions.
FIG. 2 is SnS @ NbS in example 12Core-shell heterojunction powder X-ray diffraction pattern.
FIG. 3 is SnS @ NbS in example 22Scanning electron microscopy of core-shell heterojunctions.
FIG. 4 is SnS @ NbS in example 32Scanning electron microscope image of core-shell heterojunction。
FIG. 5 is a graph showing that SnS @ NbS is used in example 42And the source-drain current-source-drain voltage curve of the back gate type thin film field effect transistor of the core-shell heterojunction when the grid voltage is not applied.
FIG. 6 is a diagram of the SnS @ NbS-based device in example 42And the source-drain current-source-drain voltage curve of the back gate type thin film field effect transistor of the core-shell heterojunction when different gate voltages are applied.
FIG. 7 is a graph showing that SnS @ NbS is used in example 52Current-time curve of core-shell heterojunction photodetector versus 405nm laser.
FIG. 8 is a graph showing that SnS @ NbS is used in example 52Response-recovery time diagram of core-shell heterojunction photodetector to 405nm laser.
FIG. 9 is a scanning electron micrograph of the product of comparative example 1.
FIG. 10 is a scanning electron micrograph of the product of comparative example 2.
Detailed Description
For a better understanding of the present invention, the technical solutions of the present invention will be described in detail below by way of specific embodiments with reference to the accompanying drawings.
Example 1: SnS @ NbS2Preparation method of core-shell heterogeneity
Niobium pentachloride (0.23 mmol. times.0.3) and tin tetrachloride pentahydrate (0.23 mmol. times.0.7) were dissolved in 20ml oleylamine and degassed at 100 ℃ for 15 minutes under an ultra-high purity argon atmosphere to remove air and impurities while strictly mixing. Subsequently, the mixture was heated to 300 ℃ and 8mmol of carbon disulphide was injected into the solution via syringe. After 1 hour, the reaction was stopped, and the heating source was removed and cooled to room temperature. Adding excessive mixture (volume ratio is 1: 3) of ethanol and isopropanol into the synthesized solution for washing, and then centrifuging the solution in a centrifuge at the rotating speed of 8500 r/min for 5 minutes to separate out the synthesized SnS @ NbS2Core-shell heterogeneity. The obtained heterojunction was then dispersed in n-hexane and the centrifuge tube was sonicated to obtain a macroscopically homogeneous solution. Next, a mixture of excess ethanol and isopropanol was added again, followed by centrifugation under the same conditions. After rapid removal of the supernatant, the procedure was repeated three times. Finally, the sample is putThe product is washed with ethanol and dispersed in ethanol.
For the product SnS @ NbS of example 12Core-shell heterojunctions were analyzed, NbS as shown in FIG. 12Uniformly wrapping the SnS core surface; SnS @ NbS2The X-ray powder diffraction pattern of the core-shell heterojunction is shown in FIG. 2, which illustrates SnS @ NbS2SnS and NbS exist in the nuclear shell heterojunction at the same time2。
Example 2: SnS @ NbS2Preparation method of core-shell heterogeneity
Niobium pentachloride (0.23 mmol. times.0.2) and tin tetrachloride pentahydrate (0.23 mmol. times.0.8) were dissolved in 20ml oleylamine and degassed at 120 ℃ for 15 minutes under an ultra-high purity argon atmosphere to remove air and impurities while strictly mixing. Subsequently, the mixture was heated to 300 ℃ and 8mmol of carbon disulphide was injected into the solution via syringe. After 1 hour, the reaction was stopped, and the heating source was removed and cooled to room temperature. Adding excessive mixture (volume ratio is 1: 3) of ethanol and isopropanol into the synthesized solution for washing, and then centrifuging the solution in a centrifuge at the rotating speed of 8500 r/min for 5 minutes to separate out the synthesized SnS @ NbS2A core-shell heterojunction. The obtained heterojunction was then dispersed in n-hexane and the centrifuge tube was sonicated to obtain a macroscopically homogeneous solution. Next, a mixture of excess ethanol and isopropanol was added again, followed by centrifugation under the same conditions. After rapid removal of the supernatant, the procedure was repeated three times. Finally, the sample was washed with ethanol and dispersed in ethanol.
Using example 2, similar products to those of example 1, SnS @ NbS, were likewise obtained2Core-shell heterojunctions, FIG. 3, but in contrast to example 1, SnS @ NbS2NbS in core-shell heterojunction2The shell cannot completely wrap the SnS core, so that the appearance and the property of the core-shell mechanism are influenced.
Example 3: SnS @ NbS2Preparation method of core-shell heterogeneity
Niobium pentachloride (0.23 mmol. times.0.4) and tin tetrachloride pentahydrate (0.23 mmol. times.0.6) were dissolved in 20ml oleylamine and degassed at 100 ℃ for 15 minutes under an ultra-high purity argon atmosphere to remove air and impurities while strictly mixing. Subsequently, the mixture was heated to 350 deg.C8mmol of carbon disulphide was injected into the solution via syringe. After 15 minutes, the reaction was stopped and the heat source was removed and cooled to room temperature. Adding excessive mixture (volume ratio is 1: 3) of ethanol and isopropanol into the synthesized solution for washing, and then centrifuging the solution in a centrifuge at the rotating speed of 8500 r/min for 5 minutes to separate out the synthesized SnS @ NbS2Core-shell heterogeneity. The obtained heterojunction was then dispersed in n-hexane and the centrifuge tube was sonicated to obtain a macroscopically homogeneous solution. Next, a mixture of excess ethanol and isopropanol was added again, followed by centrifugation under the same conditions. After rapid removal of the supernatant, the procedure was repeated three times. Finally, the sample was washed with ethanol and dispersed in ethanol.
Using example 3, similar products to those of example 1, SnS @ NbS, can likewise be obtained2Core-shell heterology, FIG. 4, but in contrast to example 1, SnS @ NbS2NbS in core-shell heterojunction2Too much shell wrapping affects the appearance and properties of the core-shell structure.
Example 4: SnS @ NbS2Electrical properties of core-shell heterozygotes
A100-mesh square-hole copper mesh is used as a mask plate, a gold (50 nm)/chromium (30nm) source electrode and a drain electrode are deposited on the surface of a silicon dioxide (300 nm)/silicon substrate through a thermal evaporation method, the channel length is about 11 mu m, and silicon is used as a grid electrode. SnS @ NbS in example 12And the heterojunction ethanol solution is dripped on the channel to connect the source electrode and the drain electrode to form the back grid type field effect transistor. The prepared device was then placed in a low temperature probe station, which was connected to a semiconductor parameter instrument at 77K and 5X 10-5The electrical properties of the sample were measured under the condition of Torr vacuum.
The electrical properties of the device of example 4 were analyzed, as shown in FIG. 5, based on SnS @ NbS2A source-drain current-source-drain voltage curve of the back gate type thin film field effect transistor of the core-shell heterojunction when no grid voltage is applied; based on SnS @ NbS, as shown in FIG. 62The source-drain current-source-drain voltage curve of the back gate type thin film field effect transistor of the core-shell heterojunction when different gate voltages are applied; the result shows that SnS @ NbS2The core-shell heterojunction exhibits metallicityConductive properties of, SnS and NbS2With a lower contact resistance therebetween.
Example 5: based on SnS @ NbS2Photoelectric detector of core-shell heterojunction
Gold (15nm) was deposited on the surface of a silicon dioxide (300 nm)/silicon substrate by thermal evaporation, using a shaped shadow mask to obtain interdigitated electrodes with a line pitch of 10 μm. SnS @ NbS in example 12The heterojunction ethanol solution is dripped on the electrode to form a layer of film on the interdigital part, and the successful preparation based on SnS @ NbS is obtained after the solvent is dried2The core-shell heterojunction photodetector was then tested for its response to 405nm laser light.
The above test results were analyzed, as shown in FIG. 7, based on SnS @ NbS2The current change diagram of the photoelectric detector of the core-shell heterojunction is that the light source closing current is recovered along with the reduction of the current of the photoelectric detector irradiated by the 405nm laser. As shown in fig. 8, the response time and recovery time of the photocurrent were 1.12 seconds and 1.01 seconds, respectively, and the response-recovery process was fast. Thus, it can be said that SnS @ NbS2The core-shell heterojunction can be used for preparing a photoelectric detector.
Comparative example 1:
niobium pentachloride (0.23 mmol. times.0.5) and tin tetrachloride pentahydrate (0.23 mmol. times.0.5) were dissolved in 20ml oleylamine and degassed at 100 ℃ for 15 minutes under an ultra-high purity argon atmosphere to remove air and impurities while strictly mixing. Subsequently, the mixture was heated to 300 ℃ and 8mmol of carbon disulphide was injected into the solution via syringe. After 1 hour, the reaction was stopped, and the heating source was removed and cooled to room temperature. The resulting solution was washed by adding an excess of a mixture of ethanol and isopropanol (volume ratio 1: 3) and then centrifuged at 8500 rpm in a centrifuge for 5 minutes to separate the resulting product. The product obtained was then dispersed in n-hexane and the centrifuge tube was sonicated to obtain a macroscopically homogeneous solution. Next, a mixture of excess ethanol and isopropanol was added again, followed by centrifugation under the same conditions. After rapid removal of the supernatant, the procedure was repeated three times. Finally, the sample was washed with ethanol and dispersed in ethanol.
Using comparative example 1, it was not possible to obtain a product SnS @ NbS similar to that of example 12Core-shell heterogeneity, fig. 9.
Comparative example 2:
niobium pentachloride (0.23 mmol. times.0.3) and tin tetrachloride pentahydrate (0.23 mmol. times.0.7) were dissolved in 20ml oleylamine and degassed at 100 ℃ for 15 minutes under an ultra-high purity argon atmosphere to remove air and impurities while strictly mixing. Subsequently, the mixture was heated to 270 ℃ and 8mmol of carbon disulphide was injected into the solution via syringe. After 3 hours, the reaction was stopped and the heat source was removed and cooled to room temperature. The resulting solution was washed by adding an excess of a mixture of ethanol and isopropanol (volume ratio 1: 3) and then centrifuged at 8500 rpm in a centrifuge for 5 minutes to separate the resulting product. The product obtained was then dispersed in n-hexane and the centrifuge tube was sonicated to obtain a macroscopically homogeneous solution. Next, a mixture of excess ethanol and isopropanol was added again, followed by centrifugation under the same conditions. After rapid removal of the supernatant, the procedure was repeated three times. Finally, the sample was washed with ethanol and dispersed in ethanol.
Using comparative example 2, it was not possible to obtain a product SnS @ NbS similar to that of example 12Core-shell heterogeneity, fig. 10.
The invention is not limited to the specific technical solutions described in the above embodiments, and all technical solutions formed by equivalent substitutions are within the scope of the invention as claimed.
Claims (10)
1. Tin sulfide (SnS) @ niobium disulfide (NbS)2) The preparation method of the core-shell heterojunction is characterized by comprising the following steps: the method comprises the following steps:
(1) dissolving niobium pentachloride and tin tetrachloride pentahydrate in a molar ratio of 2: 8-4: 6 in oleylamine, and degassing at high temperature;
(2) further heating the solution, then injecting carbon disulfide for vulcanization, wherein the vulcanization temperature is 300-350 ℃, and obtaining SnS @ NbS2A core-shell heterojunction;
(3) the obtained SnS @ NbS in the step (2) is treated2Ethanol and isopropyl are added into the core-shell heterojunctionAnd washing with a mixed solution of alcohol and n-hexane, washing with a washing solution, and dispersing in the dispersion liquid.
2. The SnS @ NbS of claim 12The preparation method of the core-shell heterojunction is characterized by comprising the following steps: SnS @ NbS in the step (1)2The preparation method of the core-shell heterojunction adopts niobium pentachloride and stannic chloride pentahydrate as raw materials and synthesizes the raw materials by a solvothermal method.
3. The SnS @ NbS of claim 12The preparation method of the core-shell heterojunction is characterized by comprising the following steps: in the step (1), oleylamine is used as a solvent, a reducing agent and a surfactant.
4. The SnS @ NbS of claim 12The preparation method of the core-shell heterojunction is characterized by comprising the following steps: in the step (1), the degassing temperature is 100-150 ℃, and the degassing time is 10-20 min.
5. The SnS @ NbS of claim 12The preparation method of the core-shell heterojunction is characterized by comprising the following steps: in the step (2), carbon disulfide is used as a sulfur source, and the reaction time is 15 min-3 h.
6. The SnS @ NbS of claim 12The preparation method of the core-shell heterojunction is characterized by comprising the following steps: in the step (3), the washing solution is one or more of ethanol, isopropanol or n-hexane, and the dispersion liquid is ethanol, methanol or a volatile solvent of water.
7. The SnS @ NbS of claim 12The preparation method of the core-shell heterojunction is characterized by comprising the following steps: niobium pentachloride 0.23mmol × 0.3 and tin pentahydrate 0.23mmol × 0.7 were dissolved in 20ml oleylamine, degassed at 100 deg.C for 15 minutes under argon atmosphere, then heated to 300 deg.C, 8mmol of carbon disulfide were injected into the solution via syringe and vulcanized for 1 hour to obtain SnS @ NbS2The shape of the core-shell heterojunction is optimal.
8. SnS @ NbS prepared according to any one of claims 1-72A core-shell heterojunction.
9. The SnS @ NbS of claim 82The application of the core-shell heterojunction is characterized in that: the heterojunction can be applied to a photodetector or a logic switch.
10. The SnS @ NbS of claim 82The application of the core-shell heterojunction is characterized in that: SnS @ NbS2And (3) dripping the dispersion liquid of the core-shell heterojunction on the surface of the electrode, and drying to obtain the electrode applied to the photoelectric detector.
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