CN103641169A

CN103641169A - Synthetic method of Bi2S3-MoS2 nanometer heterostructure

Info

Publication number: CN103641169A
Application number: CN201310559429.XA
Authority: CN
Inventors: 唐华; 唐国钢; 张杜; 王瑜琪; 李长生
Original assignee: Jiangsu University
Current assignee: Jiangsu University
Priority date: 2013-11-12
Filing date: 2013-11-12
Publication date: 2014-03-19
Anticipated expiration: 2033-11-12
Also published as: CN103641169B

Abstract

The invention discloses a synthetic method of Bi2S3-MoS2 nanometer heterostructure, which particularly comprises the following steps: (1) preparing a solution, that is, dissolving Na2MoO4, Na2S, a reducing agent, and soluble bismuth salt in deionized water to obtain the solution; (2) stirring the solution obtained in step (1), transferring the solution into a stainless steel reaction vessel, sealing the reaction vessel, performing a constant temperature reaction, cooling to room temperature to obtain a reaction product; (3) separating the reaction product, washing, and drying to obtain Bi2S3-MoS2 nanometer sheets. The method of the invention is simple in process, and low in cost; the prepared product is high in purity, and high in yield, and has important application in fields of photochemistry, catalysis, lithium batteries, and the like. The method of the invention is expected to be used in large-scale industrial production.

Description

A kind of Bi 2s 3-MoS 2the synthetic method of nano-heterogeneous structure

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, so Bi ₂s ₃be easy to form a kind of one-dimensional crystal structure of high length-diameter ratio, and its direct band gap is about 1.3eV, there is good photovoltaic effect, thermoelectricity capability and rectifying effect; Compare nanostructure Bi with block ₂s ₃absorbing wavelength and fluorescent emission generation blue shift, and can also produce nonlinear optical response, there is more excellent photoelectric catalytically active.At aspects such as luminescent material, nonlinear optical material, photocatalyst material, thermoelectric-cooled technology and photoelectrons, have broad application prospects; And molybdenumdisulphide is as important transient metal sulfide, it has the laminate structure of similar graphite flake layer, in layer, is very strong covalent linkage, and interlayer is very weak Van der Waals Er Sili, and layer is easy to peel off with layer, has good tribological property; Along with the rise of nanotechnology, various nano molybdenum disulfide particles, because of its special size and interfacial effect, cause people's extensive concern, are 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, synthetic Bi ₂s ₃-MoS ₂nano heterogeneous composite property has obtained 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, and pattern 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 in proportion Na ₂moO ₄, Na ₂s, reductive agent and soluble bismuth salt, be dissolved in deionized water, dissolves and obtain solution; (2) solution stirring step (1) being obtained is even, after fully dissolving, moves into stainless steel cauldron, and sealing, after isothermal reaction, naturally cools to room temperature, obtains reaction product; (3) the above-mentioned reaction product of centrifugation, washing, after being dried, 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 ℃～280 ℃, reaction 24 ~ 48h.

Described dry temperature is 60-100 ℃, and be 10-12 h time of drying.

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 makes ₂s ₃-MoS ₂the field emission scanning electron microscope of nano-heterogeneous structure (SEM) photo and transmission electron microscope (TEM) photo, wherein a, b are product S EM figure, c is product TEM figure.

Fig. 2 is the Bi that the present invention makes ₂s ₃-MoS ₂the EDS spectrogram of nano-heterogeneous structure.Here be mainly protection preparation method.

Embodiment

By embodiment, further describe the present invention below, as known by the technical knowledge, the present invention also can describe by other the scheme that does not depart from the technology of the present invention feature, and therefore changes within the scope of the present invention all or that be equal in the scope of the invention are 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 ℃ of insulation 24h, be cooled to room temperature; Reaction product is after centrifugation, and washing, is finally dried the product powder that 11 h obtain grey black, i.e. Bi at 80 ℃ 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 ℃ of insulation 48h, be cooled to room temperature; Reaction product is after centrifugation, and washing, is finally dried the product powder that 12 h obtain grey black, i.e. Bi at 60 ℃ 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 ℃ of insulation 30h, be cooled to room temperature; Reaction product is after centrifugation, and washing, is finally dried the product powder that 10 h obtain grey black, i.e. Bi at 100 ℃ 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, after dissolving completely, stir, then mixed solution is transferred in the stainless steel cauldron of 100 ml, be placed in vacuum drying oven in 240 ℃ of insulation 28h, be cooled to room temperature; Reaction product is after centrifugation, and washing, is finally dried the product powder that 10 h obtain grey black, i.e. Bi at 90 ℃ ₂s ₃-MoS ₂nano-heterogeneous structure.

Fig. 1 a and 1b are the SEM of product, and product is flower-shaped heterojunction structure, the TEM that Fig. 1 c is 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 clearly in sample and mainly contain Mo that Bi and S element illustrate that product is mainly Bi from figure ₂s ₃and MoS ₂.

Claims

1. a Bi ₂s ₃-MoS ₂the synthetic method of nano-heterogeneous structure, is characterized in that, comprises the steps:

(1) obtain solution: take in proportion Na ₂moO ₄, Na ₂s, reductive agent and soluble bismuth salt, be dissolved in deionized water, dissolves and obtain solution;

(2) solution stirring step (1) being obtained is even, after fully dissolving, moves into stainless steel cauldron, and sealing, after isothermal reaction, naturally cools to room temperature, obtains reaction product;

(3) the above-mentioned reaction product of centrifugation, washing, after being dried, obtains Bi ₂s ₃-MoS ₂nanometer sheet.

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, 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.

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 isothermal reaction is 120 ℃～280 ℃, reaction 24 ~ 48h.

7. a kind of Bi according to claim 1 ₂s ₃-MoS ₂the synthetic method of nano-heterogeneous structure, is characterized in that, described dry temperature is 60-100 ℃, and be 10-12 h time of drying.