CN110182848A - A kind of high-temperature stability 1T phase molybdenum disulfide nano structure and its preparation method and application - Google Patents
A kind of high-temperature stability 1T phase molybdenum disulfide nano structure and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of high-temperature stability 1T phase molybdenum disulfide nano structure and its preparation method and application, which includes: (1) by substrate progress Muffle furnace heat treatment, obtains the substrate of functionalization；(2) substrate of functionalization, catalyst and carbon source are subjected in tube furnace thermal response, obtain carbon nano tube modified carbon cloth；(3) carbon nano tube modified carbon cloth, molybdate and sulfur-containing compound are subjected to solvent thermal reaction in a solvent, the CNT-CFC of molybdenum disulfide must have been loaded.Preparation method step of the invention is simple, at low cost, yield is high, meets environmental requirement；Overcome 1T phase MoS2Can not high-temperature stable limitation, make by solvent-thermal method obtain 1T phase MoS2The crystal form of its metallicity 1T phase still can be maintained well after the high annealing by 300-700 DEG C or so；And the 1T phase MoS with high-temperature stability of preparation2Nanostructure has excellent storage lithium performance, having broad application prospects in lithium ion battery.
Description
Technical field
The present invention relates to the synthesis technical fields of 1T phase molybdenum disulfide nano material, more particularly to one kind to have high-temperature stable
The preparation method and applications of the 1T phase molybdenum disulfide nano structure of property.
Background technique
Two-dimentional (2D) stratified material is and blocky since it is widely studied with high-specific surface area and excellent characteristic
But above-mentioned characteristic is not present in form.In recent years, MoS2Due to its in nature rich reserves and show one's talent, it can be with
As the negative electrode material of lithium ion battery, there is the up to theoretical capacity of 667mAh g-1, but obtained battery capacity is fast
Speed decays and electrode reaction rate is slow, hinders MoS2Practical application in lithium ion battery.In addition to this, it due also to
Hydrogen storage material, in terms of have potential application and attract attention.
MoS2There are two types of crystal structures for tool, are the cylindrical 2H phase of triangular prism and octahedral 1T phase respectively.2H phase has half
Conducting and thermodynamic stability is form common in nature；And 1T phase has metallicity and metastable state property, in nature
In be not present.With 2H-MoS2It compares, 1T-MoS2With higher conductivity and broader ion diffusion admittance is provided, this is advantageous
Electron-transport and ion diffusion in electrochemical energy storage.In addition to this, 1T-MoS2There is higher catalytic activity in layer, thus
Enhance electro-catalysis H2-producing capacity.However, 1T phase is unstable, it is very easy to be transformed into 2H phase, especially in heating anneal condition
Under.
1T phase MoS2Stabilization become retain its excellent characteristics key.Therefore, 1T-MoS is probed into2Antihunt means and structure
Build stable nanostructure, it will help improve the storage lithium ability and cycle performance of lithium ion battery.1T phase MoS2Stablize system
There are many Preparation Method, mainly there is alkali metal intercalation stripping method, electron beam and low-temperature solvent thermal method etc., but the 1T phase obtained
Molybdenum disulfide is highly unstable, is easy to be converted to the molybdenum disulfide of 2H phase.The generally acknowledged method that can stablize 1T phase mainly has alkali golden
Belong to ion insertion, hydrated ion intercalation, graphene intercalation etc., but the 1T phase obtained still can turn after heating anneal processing
Become 2H phase.
It is compound to disclose a kind of hydro-thermal method synthesis 1T phase molybdenum disulfide/graphene nano by publication CN108404936A
Material, comprising the following steps: step A: graphene oxide is dissolved in into water and is ultrasonically formed homogeneous solution；Step B: to obtained by step A
Solution is added molybdenum source, sulphur source and reducing agent and stirs to dissolution, and solution is transferred to reaction kettle and carries out hydro-thermal reaction；Step C: step
B is cooled to room temperature after reaction, is obtained 1T phase molybdenum disulfide/graphene after product water and ethanol washing, centrifugation, drying and is received
Nano composite material.Its main technical schemes is to synthesize 1T phase MoS by the hydro-thermal method that graphene assists2.But this method obtains
1T phase molybdenum disulfide be not array structure, and its 1T phase is very unstable, and temperature, which slightly increases, will be converted to more stable 2H
Phase limits its scope of application (such as high temperature, high pressure particular surroundings).
Summary of the invention
The present invention is to solve the above problem in the prior art, proposes a kind of high-temperature stability 1T phase molybdenum disulfide nano knot
Structure and its preparation method and application.
The preparation method of high-temperature stability 1T phase molybdenum disulfide nano structure provided by the invention carries out heat to substrate first
Processing improves substrate surface wettability, then can grow carbon nanotube in substrate surface by tube furnace thermal response, then
Metallicity 1T molybdenum disulfide can be grown in the carbon nanotube of substrate surface by a step solvent thermal reaction；And preparation method
Step is simple, at low cost, yield is high, meets environmental requirement.
The preparation method of high-temperature stability 1T phase molybdenum disulfide nano structure provided by the invention overcomes 1T phase MoS2Nothing
The limitation of method high-temperature stable makes the 1T phase MoS obtained by solvent-thermal method2By 300-700 DEG C or so high annealing it
The crystal form of its metallicity 1T phase still can be maintained well afterwards, it is intended to simplify the preparation work for obtaining stable 1T phase molybdenum disulfide
Skill expands the temperature range of 1T phase molybdenum disulfide application.
To achieve the above object, the invention adopts the following technical scheme:
The first aspect of the invention is to provide a kind of preparation method of high-temperature stability 1T phase molybdenum disulfide, including as follows
Step:
(1) substrate is subjected to Muffle furnace heat treatment, obtains the substrate of functionalization；
(2) substrate of functionalization, catalyst and carbon source are subjected in tube furnace thermal response, obtain carbon nano tube modified carbon
Cloth (CNT-CFC)；
(3) carbon nano tube modified carbon cloth (CNT-CFC), molybdate and sulfur-containing compound are subjected to solvent heat in a solvent
Reaction, must load the CNT-CFC (MoS of molybdenum disulfide2/CNT-CFC)。
Further, the temperature of the heat treatment of Muffle furnace described in step (1) is 300~500 DEG C, and the time is 0.5~4h.
Further, the temperature of the heat treatment of tube furnace described in step (2) is 300~750 DEG C, and the time is 0.5~4h.
Further, catalyst described in step (2) is Co (NO3)2·6H2O, the catalyst Co (NO3)2·6H2O's
Dosage are as follows: to the catalyst Co (NO that 1.0~1.8g is added in the mixed liquor of every 10ml dehydrated alcohol and every 10ml ethylene glycol3)2·
6H2O, it is 1.13cm that the mixed liquor of acquisition, which can impregnate 6 areas,2Carbon cloth disk.
Further, carbon source described in step (2) is the mixed liquor of ethyl alcohol 10ml and ethylene glycol 10ml.
Further, molybdate described in step (3) includes one or more of sodium molybdate, potassium molybdate and molybdenum ammonium.
Further, sulfur-containing compound described in step (3) includes thiocarbamide and/or L-cysteine.
It is further preferred that the mass ratio of the material of molybdate described in step (3) and sulfur-containing compound is 1:2~8.
Further, solvent described in step (3) includes one or more of water, n,N dimethylformamide and ethyl alcohol
Mixture.
Further, the volume of solvent described in step (3) and the mass ratio of the material of molybdate are 50~80mL:1mol.
Further, the temperature of solvent thermal reaction described in step (3) be 180~240 DEG C, the time be 8~for 24 hours.
The second aspect of the invention is to provide a kind of high-temperature stability 1T phase curing of method preparation as described above
Molybdenum nanostructure.
Further, the high-temperature stability 1T phase molybdenum disulfide nano structure is in the high annealing by 300-700 DEG C
The crystal form of its metallicity 1T phase still can be maintained well later.
The third aspect of the invention is to provide a kind of high-temperature stability 1T phase molybdenum disulfide nano knot as described above
Application of the structure in lithium ion battery.
It will be using the MoS of above method preparation2Obtained MoS after/CNT-CFC and its annealing2/ CNT-CFC-A is applied in lithium
In ion battery, after showing that the material by annealing front and back is assembled into lithium ion battery through test result, in 0.5mAcm-2Electric current is close
It can be realized 755mAh g under degree-1With 1391mAh g-1Stabilization capacity.
The present invention by adopting the above technical scheme, compared with prior art, has the following technical effect that
(1) preparation method step provided by the invention is simple, at low cost, yield is high, meets environmental requirement；
(2) 1T phase MoS is overcome2Can not high-temperature stable limitation, make by solvent-thermal method obtain 1T phase MoS2Passing through
Still the crystal form of its metallicity 1T phase can be maintained after 300-700 DEG C or so of high annealing well；
(3) and preparation the 1T phase MoS with high-temperature stability2Nanostructure have excellent storage lithium performance, lithium from
Having broad application prospects in sub- battery.
Detailed description of the invention
Fig. 1 is MoS obtained by the embodiment of the present invention 12/ CNT-CFC and MoS2The SEM photograph of/CNT-CFC-A；
Fig. 2 is MoS obtained by the embodiment of the present invention 12/ CNT-CFC-A and MoS2The Raman map of/CNT-CFC；
Fig. 3 is the cycle performance test chart of the lithium ion half-cell of the embodiment of the present invention 2.
Specific embodiment
The present invention provides a kind of high-temperature stability 1T phase MoS2Preparation method, comprising the following steps:
(1) substrate is heat-treated, obtains the substrate of functionalization；
(2) substrate of functionalization, catalyst and carbon source are subjected in tube furnace thermal response, obtain CNT-CFC.
(3) CNT-CFC, molybdate and sulfur-containing compound are subjected to solvent thermal reaction in a solvent, obtain MoS2/CNT-CFC。
In step of the present invention (1), substrate is heat-treated, obtains the substrate of functionalization.The substrate is preferably carbon cloth；
The present invention does not have particular/special requirement to the shape and area of the substrate, can be set according to actual needs shape and the face of substrate
Product；The present invention does not have particular/special requirement to the source of the substrate, using the substrate in source known to those skilled in the art, such as
Commercially available carbon cloth；Specifically in the present invention, the model of the commercially available carbon cloth is preferably WOS1002.
It is preferred that substrate is successively washed and dried first, then it is heat-treated.In the present invention, the washing is excellent
It is selected as supersound washing；The supersound washing preferably successively includes that ultrasonic acetone is washed, ultrasonic ethyl alcohol is washed and ultrasound washing；The ultrasound
Acetone is washed, ultrasonic ethyl alcohol is washed and the time of ultrasound washing independent preferably 10~20min, more preferably 15min；The ultrasound
Acetone is washed, ultrasonic ethyl alcohol is washed and the frequency of ultrasound washing independent preferably 35~53Hz, more preferably 40~50Hz；The present invention
Pass through the impurity such as dust, organic matter existing for washing removal substrate surface.After the washing, the present invention is preferably by substrate drying.
The present invention does not have particular/special requirement to the temperature and time of the drying, can be dry complete by the water of substrate surface.
After the drying, the substrate after drying is heat-treated by the present invention, obtains the substrate of functionalization.In the present invention
In, the temperature of the heat treatment is preferably 300~500 DEG C, and more preferably 450 DEG C；The time of the heat treatment is preferably 0.5~
4h, more preferably 1h；The heat treatment is preferably aerobic calcination processing；The present invention does not have the specific method for carrying out aerobic calcining
Particular/special requirement, using aerobic method for calcinating well known to those skilled in the art, in a specific embodiment of the present invention, preferably
Substrate is subjected to aerobic calcining in air.In the present invention, heat treatment can increase the hydroxyl group of substrate surface, increase base
The wettability at bottom makes the 1T phase MoS with high-temperature stability2More easily generated in substrate surface.
In step of the present invention (2), after obtaining the substrate of functionalization, the substrate of the functionalization is immersed in and urges by the present invention
In agent solution, rear take out is placed on diamond heating area, and carbon source is placed on nozzle, and can get after heat treatment grown carbon pipe
Carbon cloth CNT-CFC.In the present invention, the temperature of the heat treatment is preferably 300~750 DEG C, and more preferably 700 DEG C；The heat
The time of processing is preferably 0.5~4h, more preferably 2h；The heat treatment is preferably argon gas calcination processing；In the present invention, hot
Processing can be such that carbon nanotube grows in substrate surface.
In step of the present invention (2), the catalyst is Co (NO3)2·6H2O, the catalyst Co (NO3)2·6H2O's
Dosage are as follows: to the catalyst Co (NO that 1.0~1.8g is added in the mixed liquor of every 10ml dehydrated alcohol and every 10ml ethylene glycol3)2·
6H2O, it is 1.13cm that the mixed liquor of acquisition, which can impregnate 6 areas,2Carbon cloth disk.Preferably, to every 10ml dehydrated alcohol and often
Catalyst Co (the NO of 1.2~1.7g is added in the mixed liquor of 10ml ethylene glycol3)2·6H2O is configured to catalyst mixed liquid, can soak
Steeping 6 areas is 1.13cm2Carbon cloth disk；It is highly preferred that the mixed liquor of every 10ml dehydrated alcohol and every 10ml ethylene glycol
The middle catalyst Co (NO that 1.4~1.6g is added3)2·6H2O is configured to catalyst mixed liquid, and can impregnate 6 areas is 1.13cm2
Carbon cloth disk.
In step of the present invention (3), after obtaining CNT-CFC, the present invention is by it with molybdate and sulfur-containing compound in solvent
Middle carry out solvent thermal reaction obtains a kind of 1T phase MoS with high-temperature stability2.In the present invention, the molybdate preferably wraps
Include the mixture of one or more of sodium molybdate, potassium molybdate and ammonium molybdate；When the molybdate is mixture, the present invention is to mixed
The mass ratio for closing various molybdates in object does not have particular/special requirement, using arbitrary proportion；The molybdate is preferably hydrated molybdenum
Hydrochlorate；The sulfur-containing compound preferably includes thiocarbamide and/or L-cysteine；The substance of the molybdate and sulfur-containing compound
Amount is than being preferably 1:2~8, more preferably 1:3~4.
In the present invention, the solvent preferably includes one or more of water, n,N-Dimethylformamide and ethyl alcohol
The mixture of mixture, more preferably water and n,N dimethylformamide；In the water and the mixture of n,N dimethylformamide
The volume ratio of water and n,N-Dimethylformamide is preferably 1:1~2, more preferably 1:1.5；The volume and molybdate of the solvent
The mass ratio of the material be preferably 50~80mL:lmo1, more preferably 70mL:lmol.
In the present invention, the temperature of the solvent thermal reaction is preferably 180~240 DEG C, and more preferably 190~200 DEG C；Institute
The time for stating solvent thermal reaction is preferably 8~for 24 hours, more preferably 14~20h, most preferably 16~18h.The present invention is to solvent heat
Reacting the device used does not have particular/special requirement, specific such as hydro-thermal reaction using device well known to those skilled in the art
Kettle.
The present invention preferably mixes molybdate, sulfur-containing compound and solvent, then water is added in gained mixed solution and substrate
Solvent thermal reaction is carried out in thermal response kettle.The present invention preferably mixes under agitation, and the revolving speed of the stirring is preferably
100~300rpm, more preferably 200rpm；The time of the stirring is preferably 20~40min, and more preferably the 3min present invention is logical
Crossing stirring is completely dissolved molybdate and sulfur-containing compound.
In a specific embodiment of the present invention, preferably molybdate is dissolved in a small amount of water, obtains molybdate solution, then
Sulfur-containing compound is added in molybdate solution and is dissolved, solvent is eventually adding, obtains mixed solution.
The present invention can generate metallicity 1T molybdenum disulfide in the substrate surface with carbon pipe by a step solvent thermal reaction,
And reaction temperature is low, low energy consumption.
After the solvent thermal reaction, the present invention preferably by reaction solution cooled to room temperature, is then successively separated, is washed
It washs and dries.The method that the present invention uses separation does not have particular/special requirement, uses separation method well known to those skilled in the art
, specific as filtered；Washing of the present invention is preferably washed, and the present invention does not have special want to the specific method of washing
It asks, the solvent for being attached to nanotube surface and unreacted raw material can be removed clean；The present invention is to the drying
Temperature and time does not have particular/special requirement, can be complete by the solvent seasoning of nanotube surface.
Invention provides the 1T phase MoS described in a kind of above scheme with high-temperature stability2Answering in lithium ion battery
With.The present invention is to the 1T phase MoS with high-temperature stability2Concrete application method in lithium ion battery does not have special want
It asks, is applied using method well known to those skilled in the art.1T phase MoS provided by the invention with high-temperature stability2
It is strong to store up lithium ability, and electric conductivity is good, is flexible electrode, there is wide application in lithium ion battery.
Below with reference to embodiment to the 1T phase MoS provided by the invention with high-temperature stability2And preparation method thereof and answer
With being described in detail, for a better understanding of the present invention, but following embodiments are not intended to limit the scope of the invention.
Embodiment 1
(1) carbon cloth (CFC) is cut into the disk that area is 1.13cm, distinguishes supersound washing 15min with acetone, ethyl alcohol, water,
Then it dries；
(2) by the 450 DEG C of calcination processing 1h in air of the carbon cloth after drying, the carbon cloth of functionalization is obtained；
(3) carbon cloth of the carbon cloth of functionalization is packed into quartz boat and is placed on diamond heating area, will fill volume ratio is
The ethyl alcohol of 1:5 and the quartz boat of ethylene glycol mixture are placed at tube furnace entrance low temperature, will be in tube furnace 1h under the conditions of argon gas
It is rapidly heated to 700 DEG C, and keeps the temperature 0.5h at such a temperature, then cool to room temperature；
(4) carbon cloth of acquisition is cleaned into 15min with deionized water and EtOH Sonicate respectively, then dried, CNT- is made
CFC；
(5) sodium molybdate dihydrate 0.46mmol and L-cysteine 1.46mmol are dissolved in the mixed of 80mL water and DMF
In bonding solvent (volume ratio of water and DMF are 1:1.5), stirring 30min is made it dissolve；
(6) gained reaction solution is added to the polytetrafluoroethylliner liner that volume is 100mL, is put into a piece of CNT- in liner
CFC is transferred in hydrothermal reaction kettle the insulation reaction 12h at 200 DEG C, then natural cooling, separates, washs, is dried to obtain length
There is the 1T phase MoS with high-temperature stability2Carbon cloth.
Using SEM to the MoS of acquisition2/ CNT-CFC and MoS2/ CNT-CFC-A is analyzed, can from Fig. 1 a and Fig. 1 b
To after hydro-thermal reaction, MoS2Nanometer sheet and CNT composite material form the nano tubular structure that diameter is about 100nm, and attached
Mesh is formed on CFC.It can clearly be seen that the MoS of small size vertical-growth in SEM figure at high resolutions2(~
15nm, Fig. 1 b), these nano tubular structures are by MoS2Array, CNT and organic matter composition.Fig. 1 c and Fig. 1 d show MoS2/CNT-
In high-temperature annealing process, organic matter is carbonized CFC, the MoS of small size2It is independent to be changed into the large scale that diameter is about 300nm
The 1T phase MoS of formula2(MoS2/CNT-CFC-A)。
It is further analyzed using Raman spectrum in MoS2It whether there is 1T phase MoS in/CNT-CFC-A sample2.Fig. 2 is
MoS2/ CNT-CFC-A and MoS2/ CNT-CFC is in 100-550cm-1The amplification Raman spectrogram at place.In MoS2/ CNT-CFC-A and
MoS2Have in/CNT-CFC positioned at 380cm-1(E12g)、408cm-1(A1g) and 450cm-1(2LA (M)) belongs to MoS2Typical case
Raman characteristic peak.Wherein 2LA (M) corresponds to second-order Raman scattering, and A1g corresponds to the Relative Vibration mode of S atom edgewise,
E12g corresponds to Mo atom and S atom along interlayer opposite direction vibration mode.
In addition, in 178cm-1And 229cm-1Place occurs belonging to the raman characteristic peak of J1 and J2 respectively.According to previous report
The phenomenon that road, J1 the and J2 raman characteristic peak for belonging to 1T phase slightly weakens and J3 raman characteristic peak almost disappears is because of 1T-
MoS2And 2H-MoS2The result coexisted.Therefore, in MoS2/ CNT-CFC-A and MoS2J1 and J2 Raman present in/CNT-CFC
Characteristic peak shows there is 1T phase MoS in both samples2, while showing MoS2/ CNT-CFC-A inhibits in high annealing
1T phase MoS2To 2H phase transition.
Compared with the 1T phase molybdenum disulfide prepared by the publication CN108404936A, 1T phase two manufactured in the present embodiment
Molybdenum sulfide nanostructure has array structure and high temperature resistant, greatly expands the application range of 1T phase molybdenum disulfide, and find
It is with excellent storage lithium performance.
Embodiment 2
(1) carbon cloth (CFC) is cut into the disk that area is 1.13cm, distinguishes supersound washing 15min with acetone, ethyl alcohol, water,
Then it dries；
(2) by the 450 DEG C of calcination processing 1h in air of the carbon cloth after drying, the carbon cloth of functionalization is obtained；
(3) carbon cloth of the carbon cloth of functionalization is packed into quartz boat and is placed on diamond heating area, will fill volume ratio is
The ethyl alcohol of 1:5 and the quartz boat of ethylene glycol mixture are placed at tube furnace entrance low temperature, will be in tube furnace 1h under the conditions of argon gas
It is rapidly heated to 700 DEG C, and keeps the temperature 0.5h at such a temperature, then cool to room temperature；
(4) carbon cloth of acquisition is cleaned into 15min with deionized water and EtOH Sonicate respectively, then dried, CNT- is made
CFC；
(5) sodium molybdate dihydrate 0.46mmol and L-cysteine 1.46mmol are dissolved in the mixed of 80mL water and DMF
In bonding solvent (volume ratio of water and DMF are 1:1.5), stirring 30min is made it dissolve；
(6) gained reaction solution is added to the polytetrafluoroethylliner liner that volume is 100mL, is put into a piece of CNT- in liner
CFC is transferred in hydrothermal reaction kettle the insulation reaction 18h at 220 DEG C, then natural cooling, separates, washs, is dried to obtain length
There is the 1T phase MoS with high-temperature stability2Carbon cloth.
Embodiment 3
Using two kinds of materials in embodiment 1 as half-cell electrode, it is assembled into button lithium ion half-cell, to half-cell
Cyclical stability is tested, and acquired results are as shown in Figure 3；
Fig. 3 shows MoS2/ CNT-CFC and MoS2/ CNT-CFC-A is in 0.5mA cm-2It is able to realize under current density
3.16mA h cm-2With 3.79mA h cm-2(755mA h g-1With 1391mA h g-1) stabilization capacity.The above test result table
Bright MoS2There is outstanding chemical property, after high annealing, the storage lithium energy of material before annealing with CNT composite material
Power significantly increases.
As seen from the above embodiment, preparation method step of the present invention is simple, at low cost, yield is high, meets environmental requirement, and
The 1T phase MoS with high-temperature stability of preparation2Nanocomposite has excellent storage lithium performance.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (13)
1. a kind of preparation method of high-temperature stability 1T phase molybdenum disulfide, which comprises the steps of:
(1) substrate is subjected to Muffle furnace heat treatment, obtains the substrate of functionalization；
(2) substrate of functionalization, catalyst and carbon source are subjected in tube furnace thermal response, obtain carbon nano tube modified carbon cloth
(CNT-CFC)；
(3) that carbon nano tube modified carbon cloth (CNT-CFC), molybdate and sulfur-containing compound are carried out solvent heat in a solvent is anti-
It answers, the CNT-CFC (MoS of molybdenum disulfide must have been loaded2/CNT-CFC)。
2. the preparation method of high-temperature stability 1T phase molybdenum disulfide according to claim 1, which is characterized in that step (1)
Described in Muffle furnace heat treatment temperature be 300~500 DEG C, the time be 0.5~4h.
3. the preparation method of high-temperature stability 1T phase molybdenum disulfide according to claim 1, which is characterized in that step (2)
Described in tube furnace heat treatment temperature be 300~750 DEG C, the time be 0.5~4h.
4. the preparation method of high-temperature stability 1T phase molybdenum disulfide according to claim 1, which is characterized in that step (2)
Described in catalyst be Co (NO3)2·6H2O, the catalyst Co (NO3)2·6H2The dosage of O are as follows: to every 10ml dehydrated alcohol
With the catalyst Co (NO that 1.0~1.8g is added in the mixed liquor of every 10ml ethylene glycol3)2·6H2The mixed liquor of O, acquisition can impregnate
6 areas are 1.13cm2Carbon cloth disk.
5. the preparation method of high-temperature stability 1T phase molybdenum disulfide according to claim 1, which is characterized in that step (2)
Described in carbon source be ethyl alcohol and ethylene glycol mixed liquor, volume ratio be 1:6~1:2.
6. the preparation method of high-temperature stability 1T phase molybdenum disulfide according to claim 1, which is characterized in that step (3)
Described in molybdate include one or more of sodium molybdate, potassium molybdate and molybdenum ammonium.
7. the preparation method of high-temperature stability 1T phase molybdenum disulfide according to claim 1, which is characterized in that step (3)
Described in sulfur-containing compound include thiocarbamide and/or L-cysteine.
8. the preparation method of high-temperature stability 1T phase molybdenum disulfide described according to claim 1 or 6 or 7, which is characterized in that step
Suddenly the mass ratio of the material of molybdate described in (3) and sulfur-containing compound is 1:2~8.
9. the preparation method of high-temperature stability 1T phase molybdenum disulfide according to claim 1, which is characterized in that step (3)
Described in solvent include water, N, the mixture of one or more of N-dimethylformamide and ethyl alcohol.
10. the preparation method of high-temperature stability 1T phase molybdenum disulfide according to claim 1, which is characterized in that step (3)
Described in solvent volume and molybdate the mass ratio of the material be 50~80mL:1mol.
11. the preparation method of high-temperature stability 1T phase molybdenum disulfide according to claim 1, which is characterized in that step (3)
Described in solvent thermal reaction temperature be 180~240 DEG C, the time be 8~for 24 hours.
12. a kind of high-temperature stability 1T phase molybdenum disulfide nano knot prepared such as any one of claim 1~11 the method
Structure.
13. a kind of high-temperature stability 1T phase molybdenum disulfide nano structure answering in lithium ion battery as claimed in claim 12
With.
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