CN109133175A - A kind of preparation method of nano-sheet tungsten disulfide electrode material - Google Patents
A kind of preparation method of nano-sheet tungsten disulfide electrode material Download PDFInfo
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- CN109133175A CN109133175A CN201811279158.1A CN201811279158A CN109133175A CN 109133175 A CN109133175 A CN 109133175A CN 201811279158 A CN201811279158 A CN 201811279158A CN 109133175 A CN109133175 A CN 109133175A
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- 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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
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- 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
Disodium tungstate (Na2WO4) dihydrate is added in deionized water a kind of preparation method of nano-sheet tungsten disulfide electrode material, and stirring to dissolution forms clear solution A, and adjusting pH value is 1.3~1.8, and the hydro-thermal reaction 8~for 24 hours at 150~180 DEG C obtains WO3·0.33H2O powder；1:(10~30 in molar ratio), by WO3·0.33H2After O powder is mixed with thioacetamide, is calcined under argon atmosphere protection, obtain nano-sheet tungsten disulfide material.WS obtained by the present invention2Nanometer sheet has better crystallinity degree, and the complete advantage of crystal development, atomic rule arrangement is quickly transmitted for sodium ion provides advantage, can be relieved the structure as caused by volume expansion in charge and discharge process and destroys；The good dispersion of product, soilless sticking phenomenon, big specific surface area are conducive to the contact of electrolyte, to generate excellent chemical property.
Description
Technical field
The present invention relates to WS2A kind of technical field of nano material preparation, and in particular to nano-sheet tungsten disulfide electrode
The preparation method of material.
Background technique
WS2Chemical property is stablized, and cannot dissolve, will not chemically react with soda acid in water and organic solvent.WS2
Also there is good heat resistance and oxidative resistance, decomposition temperature in an atmosphere is 510 DEG C, and 539 DEG C can quickly aoxidize, in vacuum
Middle decomposition temperature is 1150 DEG C.The layer structure of WS2 makes it have good anti-friction performance, is suitable for common lubrication incessantly
Condition for high temperature and pressure, vacuum, there are the conditions such as corrosivity to be equally also suitable.
Common preparation method includes: (1) hydro-thermal method.Preparing nano particle, cost is relatively low, non-environmental-pollution, reaction condition
It is easy the features such as reaching.But high-temperature and high-presure resistent steel and corrosion resistant liner are needed, and temperature and pressure control is stringent, safety
It can be poor.Jing Ren etc., which is reported, selects to use Disodium tungstate (Na2WO4) dihydrate as tungsten source, and thiocarbamide is as sulphur source hydro-thermal method one-step synthesis
WS2And its combination product (Ren J, Wang Z, Yang F, et al.Freestanding 3D single-wall carbon
nanotubes/WS2,nanosheets foams as ultra-long-life anodes for rechargeable
Lithium ion batteries [J] .ElectrochimicaActa, 2018.), but its synthesis temperature is higher, at 250 DEG C.
(2) chemical vapour deposition technique.This method is to be steamed under high temperature environment by the oxide and sulphur of tungsten or tungsten
Vapour reaction, the method for generating two-dimensional metallic disulphide.It during the preparation process, can be by controlling reaction temperature, carrier gas flux, pipe
The parameters such as interior pressure control the physicochemical properties of product.Wang et al. prepares stratiform WS2Make sodium-ion battery cathode material
Material, but material structure causes its chemical property poor there is serious agglomeration.(Wang X,Huang J,Li J,
et al.Controlling the layered structure of WS2,nanosheets to promote Na+,
insertion with enhanced Na-ion storage performance[J].ElectrochimicaActa,
2016,222.)
(3) high-energy ball milling method.Ball mill model, ball milling stone intensity, ball-milling medium, ball milling stone diameter, ratio of grinding media to material in this method
Product can all be impacted with ball milling temperature etc..The nanometer WS of this method preparation2Powder grain size is uneven, Er Qierong
It is easily introduced impurity.But be suitble to high-volume to synthesize, simple process, moreover it is possible to prepare refractory metal that commonsense method cannot synthesize and
Alloy nano-material.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano-sheet tungsten disulfide electrode material, this method is real
It is simple to test operating process, raw material is easy to get, and at low cost, reaction temperature is also easy to control, and low energy consumption, and the time used is short.
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of preparation method of nano-sheet tungsten disulfide electrode material, comprising the following steps:
Step 1: Disodium tungstate (Na2WO4) dihydrate is added in deionized water, and stirring to dissolution forms clear solution A, adjusts pH value
It is 1.3~1.8, the hydro-thermal reaction 8~for 24 hours at 150~180 DEG C obtains WO3·0.33H2O powder；
Step 2: 1:(10~30 in molar ratio), by WO3·0.33H2After O powder is mixed with thioacetamide, in argon gas
It is calcined under atmosphere protection, obtains nano-sheet tungsten disulfide material.
A further improvement of the present invention lies in that the concentration of clear solution A is 0.075~0.3mol/L.
A further improvement of the present invention lies in that the speed of stirring is 400~600r/min, 0.1~1h of time of stirring.
A further improvement of the present invention lies in that using the salt acid for adjusting pH value of 1~4mol/L for 1.3~1.8.
A further improvement of the present invention lies in that 700~900 DEG C of the temperature of calcining, the time is 2~3h.
A further improvement of the present invention lies in that calcining carries out in low temperature tube furnace.
Compared with prior art, the invention has the benefit that the present invention is using Disodium tungstate (Na2WO4) dihydrate as tungsten source, in hydro-thermal
Under the conditions of first synthesize tungstic oxide nano-powder, then using thioacetamide as sulphur source, pure phase WS is obtained by cryogenic vulcanization technique2
Nanometer sheet.WS obtained by the present invention2Nanometer sheet, has better crystallinity degree, the complete advantage of crystal development, and atomic rule arrangement is
Sodium ion quickly transmits and provides advantage, can be relieved the structure as caused by volume expansion in charge and discharge process and destroys；Product
Good dispersion, soilless sticking phenomenon, big specific surface area is conducive to the contact of electrolyte, to generate excellent electrochemistry
Energy.Simple process of the invention, technological parameter is easy to control, and raw material is easy to get, at low cost, and low energy consumption, time short product dispersion used
Property is preferable, can quickly prepare the WS of high-purity2Nanometer sheet uses WS made from this method2Nanometer sheet powder is in electrochemical field
In have wide researching value and application value.
Detailed description of the invention
Fig. 1 is WS prepared by embodiment 32X-ray diffraction (XRD) map of nanometer sheet；
Fig. 2 is WS prepared by embodiment 32Scanning electron microscope (SEM) photo of nanometer sheet.
Fig. 3 is WS prepared by embodiment 32The cycle performance figure of nanometer sheet.
Specific embodiment
Present invention will now be described in detail with reference to the accompanying drawings..
The present invention the following steps are included:
Step 1: by Disodium tungstate (Na2WO4) dihydrate be added 25~50mL deionized water in magnetic agitation to be completely dissolved to be formed it is transparent
Solution A, mixing speed are 400~600r/min, 0.1~1h of mixing time.Control solution concentration is 0.075~0.3mol/L.
Concentrated hydrochloric acid: being diluted to the clear solution B of 1~4mol/L, is added drop-wise in solution A with solution B by step 2, arrives solution
PH value is 1.3~1.8, and solution is transferred to 100mL ptfe autoclave and carries out homogeneous reaction, reaction temperature 150~180
DEG C, the reaction time 8~for 24 hours, after reaction, freeze-drying obtains the WO of white after centrifugation3·0.33H2O。
Step 3: by gained WO3·0.33H2O powder is as tungsten source, and thioacetamide is as sulphur source, in low temperature tube furnace
Under middle argon atmosphere protection, nano-sheet WS is obtained after calcining2Material.The molar ratio of tungsten source and sulphur source is 1:(10~30), tungsten
Source taken amount is 0.1~0.5g, and 700~900 DEG C of calcination temperature, soaking time is 2~3h.
Embodiment 1
Step 1: magnetic agitation in 0.618g Disodium tungstate (Na2WO4) dihydrate addition 25mL deionized water to be formed to being completely dissolved
Bright solution A, mixing speed 400r/min, mixing time 1h, solution concentration 0.075mol/L.
Concentrated hydrochloric acid: being diluted to the clear solution B of 1mol/L, is added drop-wise in solution A with solution B by step 2, arrives pH value of solution
Value be 1.3, by solution be transferred to 100mL ptfe autoclave carry out homogeneous reaction, 160 DEG C of reaction temperature, the reaction time
12h, after reaction, freeze-drying obtains WO after centrifugation3·0.33H2O。
Step 3: by gained WO3·0.33H2O powder is as tungsten source, and thioacetamide is as sulphur source, in low temperature tube furnace
Under middle argon atmosphere protection, nano-sheet WS is obtained after calcining2The molar ratio of material, tungsten source and sulphur source is 1:20, tungsten source taken amount
For 0.1g, 900 DEG C of calcination temperature, soaking time 2h.
Embodiment 2
Step 1: by 1.8g Disodium tungstate (Na2WO4) dihydrate be added 35mL deionized water in magnetic agitation to be completely dissolved to be formed it is transparent
Solution A, mixing speed 500r/min, mixing time 0.5h, solution concentration 0.155mol/L.
Concentrated hydrochloric acid: being diluted to the clear solution B of 3mol/L, is added drop-wise in solution A with solution B by step 2, arrives pH value of solution
Value be 1.5, by solution be transferred to 100mL ptfe autoclave carry out homogeneous reaction, 180 DEG C of reaction temperature, the reaction time
12h, after reaction, freeze-drying obtains WO after centrifugation3·0.33H2O。
Step 3: by gained WO3·0.33H2O powder is as tungsten source, and thioacetamide is as sulphur source, in low temperature tube furnace
Under middle argon atmosphere protection, nano-sheet WS is obtained after calcining2The molar ratio of material, tungsten source and sulphur source is 1:10, tungsten source taken amount
For 0.3g, 800 DEG C of calcination temperature, soaking time 3h.
Embodiment 3
Step 1: magnetic agitation in 0.825g Disodium tungstate (Na2WO4) dihydrate addition 25mL deionized water to be formed to being completely dissolved
Bright solution A, mixing speed 500r/min, mixing time 0.5h, solution concentration 0.10mol/L.
Concentrated hydrochloric acid: being diluted to the clear solution B of 2mol/L, is added drop-wise in solution A with solution B by step 2, arrives pH value of solution
Value be 1.5, by solution be transferred to 100mL ptfe autoclave carry out homogeneous reaction, 180 DEG C of reaction temperature, the reaction time
12h, after reaction, freeze-drying obtains WO after centrifugation3·0.33H2O。
Step 3: by gained WO3·0.33H2O powder is as tungsten source, and thioacetamide is as sulphur source, in low temperature tube furnace
Under middle argon atmosphere protection, nano-sheet WS is obtained after calcining2The molar ratio of material, tungsten source and sulphur source is 1:20, tungsten source taken amount
For 0.2g, 900 DEG C of calcination temperature, soaking time 2h.
Sample (WS is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2Nanometer sheet), referring to Fig. 1, find sample
The WS for the hexagonal crystal system for being 08-0237 with JCPDS number2Structure is consistent, illustrates that the WS of pure phase can be made in this method2。
The sample is observed with field emission scanning electron microscope (FESEM), referring to fig. 2, it can be seen that prepared
WS2Product is the preferable nanometer sheet of dispersibility, and nano-sheet is presented in even size distribution.
Using the sample as anode material of lithium-ion battery, cycle performance figure is referring to Fig. 3, in 100mA g-1Electric current it is close
After lower 100 circle of circulation of degree, capacity is maintained at 470mAh g almost without decaying-1, show excellent chemical property.
Embodiment 4
Step 1: magnetic agitation in 2.38g Disodium tungstate (Na2WO4) dihydrate addition 25mL deionized water to be formed to being completely dissolved
Bright solution A, mixing speed 600r/min, mixing time 1h, solution concentration 0.288mol/L.
Concentrated hydrochloric acid: being diluted to the clear solution B of 4mol/L, is added drop-wise in solution A with solution B by step 2, arrives pH value of solution
Value be 1.8, by solution be transferred to 100mL ptfe autoclave carry out homogeneous reaction, 180 DEG C of reaction temperature, the reaction time
For 24 hours, after reaction, freeze-drying obtains WO after centrifugation3·0.33H2O。
Step 3: by gained WO3·0.33H2O powder is as tungsten source, and thioacetamide is as sulphur source, in low temperature tube furnace
Under middle argon atmosphere protection, nano-sheet WS is obtained after calcining2The molar ratio of material, tungsten source and sulphur source is 1:15, tungsten source taken amount
For 0.5g, 900 DEG C of calcination temperature, soaking time 2h.
Embodiment 5
Step 1: magnetic agitation in 4.95g Disodium tungstate (Na2WO4) dihydrate addition 50mL deionized water to be formed to being completely dissolved
Bright solution A, mixing speed 500r/min, mixing time 1h, solution concentration 0.3mol/L.
Concentrated hydrochloric acid: being diluted to the clear solution B of 1mol/L, is added drop-wise in solution A with solution B by step 2, arrives pH value of solution
Value be 1.6, by solution be transferred to 100mL ptfe autoclave carry out homogeneous reaction, 170 DEG C of reaction temperature, the reaction time
10h, after reaction, freeze-drying obtains WO after centrifugation3·0.33H2O。
Step 3: by gained WO3·0.33H2O powder is as tungsten source, and thioacetamide is as sulphur source, in low temperature tube furnace
Under middle argon atmosphere protection, nano-sheet WS is obtained after calcining2The molar ratio of material, tungsten source and sulphur source is 1:20, tungsten source taken amount
For 0.4g, 900 DEG C of calcination temperature, soaking time is2.5h。
Embodiment 6
Step 1: magnetic agitation in 4.95g Disodium tungstate (Na2WO4) dihydrate addition 50mL deionized water to be formed to being completely dissolved
Bright solution A, mixing speed 500r/min, mixing time 1h.
Concentrated hydrochloric acid: being diluted to the clear solution B of 1mol/L, is added drop-wise in solution A with solution B by step 2, arrives pH value of solution
Value be 1.6, by solution be transferred to 100mL ptfe autoclave carry out homogeneous reaction, 150 DEG C of reaction temperature, the reaction time
For 24 hours, after reaction, freeze-drying obtains WO after centrifugation3·0.33H2O。
Step 3: by gained WO3·0.33H2O powder is as tungsten source, and thioacetamide is as sulphur source, in low temperature tube furnace
Under middle argon atmosphere protection, nano-sheet WS is obtained after calcining2The molar ratio of material, tungsten source and sulphur source is 1:30, tungsten source taken amount
For 0.4g, 700 DEG C of calcination temperature, soaking time 3h.
Embodiment 7
Step 1: magnetic agitation in 4.95g Disodium tungstate (Na2WO4) dihydrate addition 50mL deionized water to be formed to being completely dissolved
Bright solution A, mixing speed 500r/min, mixing time 1h.
Concentrated hydrochloric acid: being diluted to the clear solution B of 1mol/L, is added drop-wise in solution A with solution B by step 2, arrives pH value of solution
Value be 1.6, by solution be transferred to 100mL ptfe autoclave carry out homogeneous reaction, 180 DEG C of reaction temperature, the reaction time
8h, after reaction, freeze-drying obtains WO after centrifugation3·0.33H2O。
Step 3: by gained WO3·0.33H2O powder is as tungsten source, and thioacetamide is as sulphur source, in low temperature tube furnace
Under middle argon atmosphere protection, nano-sheet WS is obtained after calcining2The molar ratio of material, tungsten source and sulphur source is 1:25, tungsten source taken amount
For 0.4g, 750 DEG C of calcination temperature, soaking time 2h.
The present invention is prepared for the nano-sheet WS of high degree of dispersion using two-step method2Material utilizes WS obtained by the present invention2
Nanometer sheet has better crystallinity degree, and the complete advantage of crystal development, atomic rule arrangement is quickly transmitted for sodium ion to be provided favorably
Condition can be relieved the structure as caused by volume expansion in charge and discharge process and destroy；The good dispersion of product, soilless sticking phenomenon,
Big specific surface area is conducive to the contact of electrolyte, to generate excellent chemical property.The method of use is very simple, weight
Renaturation is high, and experimental implementation process is simple, and raw material is easy to get, and at low cost, reaction temperature is also easy to control, and low energy consumption, and the time used is short, instead
It should be not necessarily to Large expensive equipment, greatly saved energy consumption and production cost, and Product size prepared by the present invention is small, purity
Height has preferable application in electrochemical field.
Claims (6)
1. a kind of preparation method of nano-sheet tungsten disulfide electrode material, which comprises the following steps:
Step 1: Disodium tungstate (Na2WO4) dihydrate is added in deionized water, and stirring to dissolution forms clear solution A, and adjusting pH value is 1.3
~1.8, the hydro-thermal reaction 8~for 24 hours at 150~180 DEG C obtains WO3·0.33H2O powder；
Step 2: 1:(10~30 in molar ratio), by WO3·0.33H2After O powder is mixed with thioacetamide, in argon atmosphere
The lower calcining of protection, obtains nano-sheet tungsten disulfide material.
2. a kind of preparation method of nano-sheet tungsten disulfide electrode material according to claim 1, which is characterized in that thoroughly
The concentration of bright solution A is 0.075~0.3mol/L.
3. a kind of preparation method of nano-sheet tungsten disulfide electrode material according to claim 1, which is characterized in that stir
The speed mixed is 400~600r/min, 0.1~1h of time of stirring.
4. a kind of preparation method of nano-sheet tungsten disulfide electrode material according to claim 1, which is characterized in that adopt
It is 1.3~1.8 with the salt acid for adjusting pH value of 1~4mol/L.
5. a kind of preparation method of nano-sheet tungsten disulfide electrode material according to claim 1, which is characterized in that forge
700~900 DEG C of the temperature of burning, time are 2~3h.
6. a kind of preparation method of nano-sheet tungsten disulfide electrode material according to claim 1, which is characterized in that forge
Burning carries out in low temperature tube furnace.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109908889A (en) * | 2019-02-28 | 2019-06-21 | 陕西科技大学 | A kind of carbon cloth surfaces growth in situ WO3/WO3·0.33H2The preparation method of O self-supporting electrode material |
| CN110563040A (en) * | 2019-09-27 | 2019-12-13 | 天津大学 | Preparation method of tungsten disulfide nanosheet for electrocatalytic hydrogen evolution |
| CN110970607A (en) * | 2019-12-10 | 2020-04-07 | 肇庆市华师大光电产业研究院 | Preparation method of cobalt-doped tungsten trioxide/CNTs sodium ion battery cathode material |
-
2018
- 2018-10-30 CN CN201811279158.1A patent/CN109133175A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109908889A (en) * | 2019-02-28 | 2019-06-21 | 陕西科技大学 | A kind of carbon cloth surfaces growth in situ WO3/WO3·0.33H2The preparation method of O self-supporting electrode material |
| CN109908889B (en) * | 2019-02-28 | 2022-04-01 | 陕西科技大学 | WO for in-situ growth on surface of carbon cloth3/WO3·0.33H2Preparation method of O self-supporting electrode material |
| CN110563040A (en) * | 2019-09-27 | 2019-12-13 | 天津大学 | Preparation method of tungsten disulfide nanosheet for electrocatalytic hydrogen evolution |
| CN110970607A (en) * | 2019-12-10 | 2020-04-07 | 肇庆市华师大光电产业研究院 | Preparation method of cobalt-doped tungsten trioxide/CNTs sodium ion battery cathode material |
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