CN103641169B - A kind of Bi 2s 3-MoS 2the synthetic method of nano-heterogeneous structure - Google Patents
A kind of Bi 2s 3-MoS 2the synthetic method of nano-heterogeneous structure Download PDFInfo
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- CN103641169B CN103641169B CN201310559429.XA CN201310559429A CN103641169B CN 103641169 B CN103641169 B CN 103641169B CN 201310559429 A CN201310559429 A CN 201310559429A CN 103641169 B CN103641169 B CN 103641169B
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- heterogeneous structure
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Abstract
The invention discloses a kind of Bi
2s
3-MoS
2the synthetic method of nano-heterogeneous structure, concrete grammar is as follows: (1) obtain solution: by Na
2moO
4, Na
2s, reductive agent and soluble bismuth salt are dissolved in deionized water, dissolve and obtain solution; (2) after solution stirring step (1) obtained, move into stainless steel cauldron, sealing, after isothermal reaction, is cooled to room temperature, obtains reaction product; (3) be separated above-mentioned reaction product, washing, drying, obtain Bi
2s
3-MoS
2nanometer sheet.The inventive method technique is simple, and with low cost, the product purity prepared is high, productive rate is high, and has important application in the fields such as photochemistry, catalysis, lithium electricity, is expected to for large-scale industrial production.
Description
Technical field
The present invention relates to field of nanometer material technology, specifically a kind of Bi
2s
3-MoS
2the synthetic method of nano-heterogeneous structure.
Background technology
Bi
2s
3be a kind of layered semiconductor, there is the very strong trend to the growth of C axle, therefore Bi
2s
3be easy to the one-dimensional crystal structure forming a kind of high length-diameter ratio, and its direct band gap is about 1.3eV, has good photovoltaic effect, thermoelectricity capability and rectifying effect; Compared with block, nanostructure Bi
2s
3absorbing wavelength and fluorescent emission generation blue shift, and can also nonlinear optical response be produced, there is more excellent photoelectric catalytically active.Have broad application prospects in luminescent material, nonlinear optical material, photocatalyst material, thermoelectric-cooled technology and photoelectron etc.; And molybdenumdisulphide is as important transient metal sulfide, it has the laminate structure of similar graphite flake layer, is very strong covalent linkage in layer, and interlayer is then very weak Van der Waals Er Sili, and layer and layer are easy to peel off, and have good tribological property; Along with the rise of nanotechnology, various nano molybdenum disulfide particle, because of its special size and interfacial effect, causes the extensive concern of people, is widely used in the fields such as solid lubrication, lithium electricity, air-sensitive.
Relevant Bi
2s
3-MoS
2the report of matrix material is less, particularly to Bi
2s
3-MoS
2the control of nano-heterogeneous structure, synthesis Bi
2s
3-MoS
2nano heterogeneous composite property obtains certain lifting, particularly photochemical catalysis, lithium electrically and tribological property etc.; The present invention participates in hydro-thermal reaction with Bi salt, has synthesized Bi
2s
3-MoS
2nano-heterogeneous structure, and productive rate is high, pattern is homogeneous, has a good application prospect.
Summary of the invention
The object of the present invention is to provide a kind of with low cost, technique is simple and productive rate is high Bi
2s
3-MoS
2the preparation method of nano-heterogeneous structure.
Above-mentioned purpose is achieved by the following technical solution: (1) obtain solution: take Na in proportion
2moO
4, Na
2s, reductive agent and soluble bismuth salt, be dissolved in deionized water, dissolves and obtain solution; (2) solution stirring step (1) obtained is even, and after fully dissolving, move into stainless steel cauldron, sealing, after isothermal reaction, naturally cools to room temperature, obtain reaction product; (3) the above-mentioned reaction product of centrifugation, washing, after drying, obtains Bi
2s
3-MoS
2nanometer sheet.
In preparation process of the present invention, all reagent is commerical prod, does not need to prepare again.
Described soluble bismuth salt is bismuth-containing inorganic salt or bismuth-containing organic salt, as Bi
2(SO
4)
3,bi (NO)
3, bismuth acetate or Oxalic acid bismuth salt.
In described reaction raw materials, Bi element is 1:0.6 ~ 1:2.5 with the ratio of the amount of substance of Mo element.
In described reaction raw materials, Bi element is 1:2.5 ~ 1:10 with the ratio of the amount of substance of S element.
Described reductive agent is oxammonium hydrochloride or sodium borohydride, and reductive agent is 2-6 with the ratio of the amount of Mo elemental substance.
The temperature of described isothermal reaction is 120 DEG C ~ 280 DEG C, reaction 24 ~ 48h.
The temperature of described drying is 60-100 DEG C, and time of drying is 10-12 h.
The cost of the inventive method is inexpensive, and production technique is simple and easy to control, and productive rate, up to 95%, is applicable to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the Bi that the present invention obtains
2s
3-MoS
2field emission scanning electron microscope (SEM) photo of nano-heterogeneous structure and transmission electron microscope (TEM) photo, wherein a, b are product S EM figure, and c is that product TEM schemes.
Fig. 2 is the Bi that the present invention obtains
2s
3-MoS
2the EDS spectrogram of nano-heterogeneous structure.Here mainly preparation method is protected.
Embodiment
The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
Embodiment 1:
By 0.22g Na
2moO
4, 0.3 g Na
2s, 0.28g NH
2oHHCl and 0.2gBi (NO
3)
3be dissolved in the deionized water of 60 mL, after dissolving completely, stir, then mixed solution is transferred in the stainless steel cauldron of 100 ml, be placed in vacuum drying oven in 280 DEG C of insulation 24h, be cooled to room temperature; Reaction product is after centrifugation, and washing, finally obtains the powder product of grey black, i.e. Bi at 80 DEG C of drying 11 h
2s
3-MoS
2nano-heterogeneous structure.
Embodiment 2:
0.22g Na
2moO
4, 0.3 g Na
2s, 0.3g sodium borohydride and 0.2g Bi
2(SO
4)
3be dissolved in the deionized water of 80 mL, after dissolving completely, stir, then mixed solution is transferred in the stainless steel cauldron of 100 ml, be placed in vacuum drying oven in 120 DEG C of insulation 48h, be cooled to room temperature; Reaction product is after centrifugation, and washing, finally obtains the powder product of grey black, i.e. Bi at 60 DEG C of drying 12 h
2s
3-MoS
2nano-heterogeneous structure.
Embodiment 3:
0.22g Na
2moO
4, 0.4 gNa
2s, 0.28g NH
2oHHCl and 0.4g Bi (Ac)
3be dissolved in the deionized water of 60 mL, after dissolving completely, stir, then mixed solution is transferred in the stainless steel cauldron of 100 ml, be placed in vacuum drying oven in 200 DEG C of insulation 30h, be cooled to room temperature; Reaction product is after centrifugation, and washing, finally obtains the powder product of grey black, i.e. Bi at 100 DEG C of drying 10 h
2s
3-MoS
2nano-heterogeneous structure.
Embodiment 4:
0.22g Na
2moO
4, 0.3 g Na
2s, 0.28g NH
2oHHCl and 0.5g Bi
2(SO
4)
3be dissolved in the deionized water of 80 mL, stir after dissolving completely, then mixed solution is transferred in the stainless steel cauldron of 100 ml, be placed in vacuum drying oven in 240 DEG C of insulation 28h, be cooled to room temperature; Reaction product is after centrifugation, and washing, finally obtains the powder product of grey black, i.e. Bi at 90 DEG C of drying 10 h
2s
3-MoS
2nano-heterogeneous structure.
Fig. 1 a and 1b is the SEM of product, and product is flower-shaped heterojunction structure, and Fig. 1 c is the TEM of product, can significantly see bar-shaped be assembled into flower-like structure together with; Fig. 2 is the EDS figure of product, can find out in sample main containing Mo, Bi and S element clearly, product mainly Bi is described from figure
2s
3and MoS
2.
Claims (6)
1. a Bi
2s
3-MoS
2the synthetic method of nano-heterogeneous structure, is characterized in that, comprises the steps:
(1) obtain solution: take Na in proportion
2moO
4, Na
2s, reductive agent and soluble bismuth salt, be dissolved in deionized water, dissolves and obtain solution;
(2) solution stirring step (1) obtained is even, and after fully dissolving, move into stainless steel cauldron, sealing, after isothermal reaction, naturally cools to room temperature, obtain reaction product;
(3) the above-mentioned reaction product of centrifugation, washing, after drying, obtains Bi
2s
3-MoS
2nanometer sheet;
Described reductive agent is oxammonium hydrochloride or sodium borohydride, and reductive agent is 2 ~ 6 with the ratio of the amount of Mo elemental substance.
2. a kind of Bi according to claim 1
2s
3-MoS
2the synthetic method of nano-heterogeneous structure, is characterized in that, described soluble bismuth salt is the organic salt of bismuth-containing inorganic salt or bismuth-containing, is specially Bi
2(SO
4)
3, Bi (NO)
3, bismuth acetate or Oxalic acid bismuth salt.
3. a kind of Bi according to claim 1
2s
3-MoS
2the synthetic method of nano-heterogeneous structure, is characterized in that, in described reaction raw materials, Bi element is 1:0.6 ~ 1:2.5 with the ratio of the amount of substance of Mo element.
4. a kind of Bi according to claim 1
2s
3-MoS
2the synthetic method of nano-heterogeneous structure, is characterized in that, in described reaction raw materials, Bi element is 1:2.5 ~ 1:10 with the ratio of the amount of substance of S element.
5. a kind of Bi according to claim 1
2s
3-MoS
2the synthetic method of nano-heterogeneous structure, is characterized in that, the temperature of described isothermal reaction is 120 DEG C ~ 280 DEG C, reaction 24 ~ 48h.
6. a kind of Bi according to claim 1
2s
3-MoS
2the synthetic method of nano-heterogeneous structure, is characterized in that, the temperature of described drying is 60-100 DEG C, and time of drying is 10-12 h.
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CN104491888B (en) * | 2014-12-18 | 2017-03-15 | 中国科学院上海硅酸盐研究所 | It is based on MoS2/Bi2S3Multi-functional diagnosis and treatment agent of PEG nanometer sheet and its preparation method and application |
CN105463566B (en) * | 2015-11-25 | 2018-04-10 | 中国科学技术大学 | A kind of epitaxial growth MoSe2‑XnSemThe liquid phase process of hetero nano structure |
CN106925302B (en) * | 2017-03-22 | 2019-07-09 | 湖南大学 | Molybdenum disulfide-antimony trisulfide composite material and preparation method and application |
CN107572489B (en) * | 2017-08-07 | 2020-01-03 | 中国科学技术大学 | Zinc selenide ultrathin nanobelt and anion exchange method for preparing same |
CN108878159A (en) * | 2018-05-23 | 2018-11-23 | 江苏大学 | 2D/1D structure molybdenum disulfide/bismuth sulfide nano composite material and preparation method thereof |
CN108675267B (en) * | 2018-06-14 | 2021-11-26 | 西南大学 | Universal method for preparing nano metal sulfide and compound thereof in one step |
CN110180560B (en) * | 2019-05-28 | 2022-02-15 | 广州大学 | Nano-rod bismuth-doped molybdenum sulfide sphere multiphase Fenton catalyst and preparation method and application thereof |
CN110289416B (en) * | 2019-06-26 | 2022-02-01 | 中南大学 | Preparation method of bismuth-molybdenum bimetallic sulfide as negative electrode material of sodium-ion battery |
CN110380042B (en) * | 2019-08-08 | 2021-01-15 | 山东大学 | Anode material of aluminum secondary battery, battery and preparation method |
CN115784304B (en) * | 2022-12-01 | 2023-07-18 | 浙大宁波理工学院 | Shuttle Bi composed of nano-sheets 2 S 3 Crystal synthesis method |
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CN101345290A (en) * | 2008-09-05 | 2009-01-14 | 中国科学院化学研究所 | Cadmium sulfide/organic semiconductor heterojunction nanowire and preparation method thereof |
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CN102814185A (en) * | 2011-07-21 | 2012-12-12 | 温州大学 | Preparation method of silver sulfide-zinc sulfide semiconductor nanometer heterojunction |
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CN101345290A (en) * | 2008-09-05 | 2009-01-14 | 中国科学院化学研究所 | Cadmium sulfide/organic semiconductor heterojunction nanowire and preparation method thereof |
US20120024362A1 (en) * | 2011-05-31 | 2012-02-02 | Primestar Solar, Inc. | Refractive index matching of thin film layers for photovoltaic devices and methods of their manufacture |
CN102814185A (en) * | 2011-07-21 | 2012-12-12 | 温州大学 | Preparation method of silver sulfide-zinc sulfide semiconductor nanometer heterojunction |
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