CN109449410A - A kind of preparation method of nitrogen, sulphur codope tungsten disulfide anode material of lithium-ion battery - Google Patents

A kind of preparation method of nitrogen, sulphur codope tungsten disulfide anode material of lithium-ion battery Download PDF

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CN109449410A
CN109449410A CN201811280597.4A CN201811280597A CN109449410A CN 109449410 A CN109449410 A CN 109449410A CN 201811280597 A CN201811280597 A CN 201811280597A CN 109449410 A CN109449410 A CN 109449410A
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nitrogen
sulphur codope
ion battery
lithium
tungsten disulfide
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CN109449410B (en
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黄剑锋
罗晓敏
曹丽云
李嘉胤
王蓉
徐培光
王泽坤
王芳敏
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Shaanxi University of Science and Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581—Chalcogenides or intercalation compounds thereof
    • H01M4/5815—Sulfides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

A kind of preparation method of nitrogen, sulphur codope tungsten disulfide anode material of lithium-ion battery, magnetic agitation in tungsten hexachloride addition ethyl alcohol is formed into clear solution to being completely dissolved, then thioacetamide, melamine and trithiocyanuric acid is added, 4~48h of homogeneous reaction is carried out at 200~240 DEG C, obtains black powder；Black powder is calcined under argon atmosphere protection, obtains nitrogen, sulphur codope tungsten disulfide anode material of lithium-ion battery.The present invention successfully prepares the WS of nitrogen, sulphur codope with tungsten hexachloride, thioacetamide and carbon cloth raw material, the methods of the solvent heat assisted by melamine and trithiocyanuric acid and heat treatment2Electrode material.Operation of the present invention process is simple, and reaction temperature is also easy to control.Nitrogen, sulphur codope itself provides more active sites to electrode material, be conducive to the transmission of ion, electronics, to promote the chemical property of battery.

Description

A kind of preparation method of nitrogen, sulphur codope tungsten disulfide anode material of lithium-ion battery
Technical field
The present invention relates to WS2The technical field of nano material preparation, and in particular to a kind of nitrogen, sulphur codope tungsten disulfide sodium The preparation method of ion battery cathode material.
Background technique
WS2Nano material is because have unique two-dimensional nanostructure, and the tungsten disulfide crystal of conventional sheet is by S=W=S The elementary layer of composition is constituted.In elementary layer, each W atom is combined by strong covalent bond and two S, and atom passes through arrangement in crystal Net plane structure is formed, interplanar is combined by weaker Van der Waals force.Insoluble in acid, alkali, alcohol, there is certain reduction Property, there can be oxidizing species to react with the concentrated sulfuric acid of chloroazotic acid, nitric acid and heat etc..Specific surface area with higher, table simultaneously Face effect, quantum size effect and small-size effect are widely used in electricity material, nano-sensor, nano catalytic material, receive The multiple fields such as rice lubriation material are one of the popular new function materials of Abroad in Recent Years research.
Tungsten disulfide is conducive to battery in charge discharge process due to its unique layer structure and biggish interlamellar spacing The deintercalation of intermediate ion is a kind of good electrode material, but exists due to itself poorly conductive and in charge and discharge process Biggish volume expansion, cause the structural stability of material poor.According to progress both domestic and external, using carbon material as base Body is conducive to the transmission of electronics, and can alleviate volume expansion of the tungsten disulfide in charge and discharge process, effective to improve again Chemical property of the condensation material as lithium ion battery negative material.Such as Guowei Huang et al. is by tungsten disulfide and three-dimensional Compound (Huang G, Liu H, Wang S, the et al.Hierarchical architecture of WS2 of graphene oxide nanosheets on graphene frameworks with enhanced electrochemical properties for lithium storage and hydrogen evolution[J].Journal of Materials Chemistry A, 2015,3 (47): 24128-24138.) as lithium ion battery negative material, it is compound after tungsten disulfide its electrification It learns performance to be substantially improved, 100 circles is recycled under the current density of 100mA/g, capacity is maintained at 766mAh/g.But two sulphur Change tungsten material the problem of there is also poorly conductives itself, doping often can solve this problem, introduce defect in material, have Effect improves the active site of electrolyte contacts, the quantity of carrier is controlled, to promote the electric conductivity of material, to accelerate electronics Transmission promoted material chemical property.
Summary of the invention
The object of the present invention is to provide the preparations of a kind of nitrogen, sulphur codope tungsten disulfide anode material of lithium-ion battery Method.
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of preparation method of nitrogen, sulphur codope tungsten disulfide anode material of lithium-ion battery, comprising the following steps:
Step 1: by tungsten hexachloride be added ethyl alcohol in magnetic agitation to the clear solution to form yellow is completely dissolved, then Thioacetamide, melamine and trithiocyanuric acid is added, 4~48h of homogeneous reaction is carried out at 200~220 DEG C, washs, does It is dry, obtain black powder；
Step 2: black powder is calcined under argon atmosphere protection, obtains nitrogen, sulphur codope tungsten disulfide sodium ion electricity Pond negative electrode material.
A further improvement of the present invention lies in that the concentration of the clear solution of yellow is 0.025~0.1mol/L.
A further improvement of the present invention lies in that the speed of stirring is 600~1000r/min, the time is 5~15min.
A further improvement of the present invention lies in that the molar ratio of tungsten hexachloride and thioacetamide is 10:1；Tungsten hexachloride, three The mass ratio of poly cyanamid and trithiocyanuric acid is (7~10): (0.5~2): (0.5~2).
A further improvement of the present invention lies in that the temperature of calcining is 600~1000 DEG C, the time is 1~3h.
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 with tungsten hexachloride, thioacetamide and carbon cloth Raw material, the methods of the solvent heat assisted by melamine and trithiocyanuric acid and heat treatment successfully prepare nitrogen, sulphur is co-doped with Miscellaneous WS2Electrode material.Operation of the present invention process is simple, and reaction temperature is also easy to control, and it is total can quickly to prepare high-purity nitrogen, sulphur The WS of doping2Compound storage sodium electrode material.Nitrogen, sulphur codope itself provides more active sites to electrode material, favorably In the transmission of ion, electronics, to promote the chemical property of battery, nitrogen made from this method, the WS of sulphur codope are used2Electricity Pole material has wide researching value and application value in electrochemical field.
Detailed description of the invention
Fig. 1 is the WS of nitrogen prepared by embodiment 3, sulphur codope2X-ray diffraction (XRD) figure of combination electrode material Spectrum；
Fig. 2 is the WS of nitrogen prepared by embodiment 3, sulphur codope2Scanning electron microscope (SEM) photo of combination electrode material.
Fig. 3 is the WS of nitrogen prepared by embodiment 3, sulphur codope2The cycle performance figure of combination electrode material, current density For 100mA g-1。
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: magnetic agitation in tungsten hexachloride addition 30~60mL ethanol solution is formed into the clear of yellow to being completely dissolved Clear solution A, mixing speed are 600~1000r/min, 5~15min of mixing time.Control solution concentration be 0.025~ 0.1mol/L；
Step 2: being added thioacetamide in solution A, control molar ratio n (WCl6):n(CH3CSNH2)=10:1, then plus Enter melamine and trithiocyanuric acid, control mass ratio m (WCl6):m(C3H6N6):m(C3H3N3S3)=(7~10): (0.5~2): (0.5~2) stirs 0.5-3h, forms uniform mixed solution；
Step 3: above-mentioned solution is transferred to 100mL ptfe autoclave and carries out homogeneous reaction, reaction temperature is 200~220 DEG C, the reaction time is 4~48h, after reaction cooled to room temperature.
Step 4: opening reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifugated, weight It is -40~-70 DEG C that after backwashing, which washs 4~6 times and is placed on temperature, and vacuum degree is dry 8~12h in 10~40Pa freeze drier, i.e., Obtain black powder.
Step 5: black powder is put into magnetic boat, and in low temperature tube furnace under argon atmosphere protection, calcination temperature is 600~1000 DEG C, the time is 1~3h, obtains nitrogen, sulphur codope WS2Electrode material.
Embodiment 1
Step 1: magnetic agitation in 0.2975g tungsten hexachloride addition 30mL ethanol solution is formed into yellow to being completely dissolved Clear solution A, mixing speed 700r/min, mixing time 8min.Control solution concentration is 0.025mol/L；
Step 2: the addition 0.5625g thioacetamide in solution A, control molar ratio n (WCl6):n(CH3CSNH2)= 10:1, adds melamine and trithiocyanuric acid, control mass ratio m (WCl6):m(C3H6N6):m(C3H3N3S3)=10:1:1, 0.5h is stirred, uniform mixed solution is formed；
Step 3: above-mentioned solution is transferred to 100mL ptfe autoclave and carries out homogeneous reaction, reaction temperature is 200 DEG C, reaction time 12h, cooled to room temperature after reaction.
Step 4: opening reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifugated, weight It is -60 DEG C that after backwashing, which washs 4 times and is placed on temperature, and vacuum degree is that 8h is dried in 10Pa freeze drier to get black powder is arrived.
Step 5: black powder is put into magnetic boat, in low temperature tube furnace under argon atmosphere protection, 600 DEG C of calcining 1h After obtain nitrogen, sulphur codope WS2Electrode material.
Embodiment 2
Step 1: magnetic agitation in 0.595g tungsten hexachloride addition 40mL ethanol solution is formed into yellow to being completely dissolved Clear solution A, mixing speed 800r/min, mixing time 5min.Control solution concentration is 0.0375mol/L；
Step 2: the addition 1.127g thioacetamide in solution A, control molar ratio n (WCl6):n(CH3CSNH2)=10: 1, add melamine and trithiocyanuric acid, control mass ratio m (WCl6):m(C3H6N6):m(C3H3N3S3)=7:0.5:1, is stirred 1.5h is mixed, uniform mixed solution is formed；
Step 3: above-mentioned solution is transferred to 100mL ptfe autoclave and carries out homogeneous reaction, reaction temperature is 210 DEG C, reaction time 4h, cooled to room temperature after reaction.
Step 4: opening reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifugated, weight It is -40 DEG C that after backwashing, which washs 6 times and is placed on temperature, and vacuum degree is that 10h is dried in 35Pa freeze drier to get black powder is arrived.
Step 5: black powder is put into magnetic boat, in low temperature tube furnace under argon atmosphere protection, 700 DEG C of calcining 2h After obtain nitrogen, sulphur codope WS2Electrode material.
Embodiment 3
Step 1: magnetic agitation in 1.19g tungsten hexachloride addition 60mL ethanol solution is formed into yellow to being completely dissolved Clear solution A, mixing speed 700r/min, mixing time 8min.Control solution concentration is 0.05mol/L；
Step 2: the addition 2.25g thioacetamide in solution A, control molar ratio n (WCl6):n(CH3CSNH2)=10: 1, add melamine and trithiocyanuric acid, control mass ratio m (WCl6):m(C3H6N6):m(C3H3N3S3)=9:2:1, stirring 3h forms uniform mixed solution；
Step 3: above-mentioned solution is transferred to 100mL ptfe autoclave and carries out homogeneous reaction, reaction temperature is 200 DEG C, the reaction time is cooled to room temperature after reaction for 24 hours.
Step 4: opening reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifugated, weight It is -60 DEG C that after backwashing, which washs 5 times and is placed on temperature, and vacuum degree is that 12h is dried in 60Pa freeze drier to get black powder is arrived.
Step 5: black powder is put into magnetic boat, in low temperature tube furnace under argon atmosphere protection, 800 DEG C of calcining 3h After obtain nitrogen, sulphur codope WS2Electrode material.
Sample (the WS of nitrogen, sulphur codope is analyzed with Rigaku D/max2000PCX- x ray diffractometer x2Electrode material), Referring to Fig. 1, it is found that sample and JCPDS number the WS for the hexagonal crystal system for being 08-02372Structure is consistent, illustrates made from this method Product is pure phase.The sample is observed with field emission scanning electron microscope (FESEM), referring to fig. 2, it can be seen that made Preferably, nano-sheet is presented in even size distribution to standby product dispersibility.
Referring to Fig. 3, as anode material of lithium-ion battery, in 100mAg-1Current density under, circulation 100 circle after, The also surplus 485mAh g of capacity-1, its cyclical stability is preferable as can be seen from Figure 3.
Embodiment 4
Step 1: magnetic agitation in 2.38g tungsten hexachloride addition 60mL ethanol solution is formed into yellow to being completely dissolved Clear solution A, mixing speed 700r/min, mixing time 8min.Control solution concentration is 0.1mol/L；
Step 2: the addition 4.5g thioacetamide in solution A, control molar ratio n (WCl6):n(CH3CSNH2)=10:1, Add melamine and trithiocyanuric acid, control mass ratio m (WCl6):m(C3H6N6):m(C3H3N3S3)=10:1.5:2, stirring 0.5h forms uniform mixed solution；
Step 3: above-mentioned solution is transferred to 100mL ptfe autoclave and carries out homogeneous reaction, reaction temperature is 220 DEG C, reaction time 10h, cooled to room temperature after reaction.
Step 4: opening reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifugated, weight It is -70 DEG C that after backwashing, which washs 5 times and is placed on temperature, and vacuum degree is that 8h is dried in 20Pa freeze drier to get black powder is arrived.
Step 5: black powder is put into magnetic boat, in low temperature tube furnace under argon atmosphere protection, 1000 DEG C of calcinings Nitrogen, sulphur codope WS are obtained after 1.5h2Electrode material.
Embodiment 5
Step 1: magnetic agitation in 1.037g tungsten hexachloride addition 40mL ethanol solution is formed into yellow to being completely dissolved Clear solution A, mixing speed 700r/min, mixing time 8min.Control solution concentration is 0.065mol/L；
Step 2: the addition 1.965g thioacetamide in solution A, control molar ratio n (WCl6):n(CH3CSNH2)=10: 1, add melamine and trithiocyanuric acid, control mass ratio m (WCl6):m(C3H6N6):m(C3H3N3S3)=9:2:2, stirring 3h forms uniform mixed solution；
Step 3: above-mentioned solution is transferred to 100mL ptfe autoclave and carries out homogeneous reaction, reaction temperature is 200 DEG C, reaction time 12h, cooled to room temperature after reaction；
Step 4: opening reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifugated, weight It is -60 DEG C that after backwashing, which washs 4 times and is placed on temperature, and vacuum degree is that 8h is dried in 10Pa freeze drier to get black powder is arrived；
Step 5: black powder is put into magnetic boat, in low temperature tube furnace under argon atmosphere protection, 600 DEG C of calcining 2h After obtain nitrogen, sulphur codope WS2Electrode material.
Embodiment 6
Step 1: magnetic agitation in 1.037g tungsten hexachloride addition 40mL ethanol solution is formed into yellow to being completely dissolved Clear solution A, mixing speed 700r/min, mixing time 8min.Control solution concentration is 0.065mol/L；
Step 2: the addition 1.965g thioacetamide in solution A, control molar ratio n (WCl6):n(CH3CSNH2)=10: 1, add melamine and trithiocyanuric acid, control mass ratio m (WCl6):m(C3H6N6):m(C3H3N3S3)=10:2:0.5, is stirred 3h is mixed, uniform mixed solution is formed；
Step 3: above-mentioned solution is transferred to 100mL ptfe autoclave and carries out homogeneous reaction, reaction temperature is 220 DEG C, reaction time 48h, cooled to room temperature after reaction；
Step 4: opening reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifugated, weight It is -60 DEG C that after backwashing, which washs 4 times and is placed on temperature, and vacuum degree is that 8h is dried in 10Pa freeze drier to get black powder is arrived；
Step 5: black powder is put into magnetic boat, in low temperature tube furnace under argon atmosphere protection, 1000 DEG C of calcining 1h After obtain nitrogen, sulphur codope WS2Electrode material.
Embodiment 7
Step 1: magnetic agitation in 1.037g tungsten hexachloride addition 40mL ethanol solution is formed into yellow to being completely dissolved Clear solution A, mixing speed 700r/min, mixing time 8min.Control solution concentration is 0.065mol/L；
Step 2: the addition 1.965g thioacetamide in solution A, control molar ratio n (WCl6):n(CH3CSNH2)=10: 1, add melamine and trithiocyanuric acid, control mass ratio m (WCl6):m(C3H6N6):m(C3H3N3S3)=7:1:2, stirring 3h forms uniform mixed solution；
Step 3: above-mentioned solution is transferred to 100mL ptfe autoclave and carries out homogeneous reaction, reaction temperature is 215 DEG C, reaction time 30h, cooled to room temperature after reaction；
Step 4: opening reaction kettle, takes out product and successively uses dehydrated alcohol and deionized water to wash and be centrifugated, weight It is -60 DEG C that after backwashing, which washs 4 times and is placed on temperature, and vacuum degree is that 8h is dried in 10Pa freeze drier to get black powder is arrived；
Step 5: black powder is put into magnetic boat, in low temperature tube furnace under argon atmosphere protection, 600 DEG C of calcining 3h After obtain nitrogen, sulphur codope WS2Electrode material.
For the present invention using tungsten hexachloride as tungsten source, thioacetamide is sulphur source, obtains nitrogen, sulphur codope using solvent-thermal method WS2Electrode material.Preparation process is simple, and technological parameter is easy to control, and repeatability is high, and reaction is not necessarily to Large expensive equipment, greatly Energy consumption and production cost are saved, product dispersibility preferably, can quickly prepare the WS of high-purity nitrogen, sulphur codope2Electrode material Material, and nitrogen, sulphur codope itself provides more active sites to electrode material, be conducive to the transmission of ion, electronics, thus The chemical property for promoting battery, uses nitrogen made from this method, the WS of sulphur codope2Electrode material size is small, purity is high, There are wide researching value and application value in electrochemical field.

Claims (6)

1. the preparation method of a kind of nitrogen, sulphur codope tungsten disulfide anode material of lithium-ion battery, which is characterized in that including following Step:
Step 1: magnetic agitation in ethyl alcohol is added in tungsten hexachloride and is then added to the clear solution to form yellow is completely dissolved Thioacetamide, melamine and trithiocyanuric acid carry out 4~48h of homogeneous reaction at 200~220 DEG C, wash, dry, obtain To black powder；
Step 2: black powder is calcined under argon atmosphere protection, it is negative to obtain nitrogen, sulphur codope tungsten disulfide sodium-ion battery Pole material.
2. the preparation method of a kind of nitrogen according to claim 1, sulphur codope tungsten disulfide anode material of lithium-ion battery, It is characterized in that, the concentration of the clear solution of yellow is 0.025~0.1mol/L.
3. the preparation method of a kind of nitrogen according to claim 1, sulphur codope tungsten disulfide anode material of lithium-ion battery, It is characterized in that, the speed of stirring is 600~1000r/min, the time is 5~15min.
4. the preparation method of a kind of nitrogen according to claim 1, sulphur codope tungsten disulfide anode material of lithium-ion battery, It is characterized in that, the molar ratio of tungsten hexachloride and thioacetamide is 10:1；Tungsten hexachloride, melamine and trithiocyanuric acid Mass ratio is (7~10): (0.5~2): (0.5~2).
5. the preparation method of a kind of nitrogen according to claim 1, sulphur codope tungsten disulfide anode material of lithium-ion battery, It is characterized in that, the temperature of calcining is 600~1000 DEG C, the time is 1~3h.
6. the preparation method of a kind of nitrogen according to claim 1, sulphur codope tungsten disulfide anode material of lithium-ion battery, It is characterized in that, calcining carries out in low temperature tube furnace.
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