CN109346723A - The preparation method of the lithium ion battery of molybdenum disulfide nano sheet array structure based on molybdenum foil load - Google Patents
The preparation method of the lithium ion battery of molybdenum disulfide nano sheet array structure based on molybdenum foil load Download PDFInfo
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Abstract
The present invention relates to a kind of MoS based on molybdenum foil load2The preparation method of the lithium ion battery of nano-chip arrays structure belongs to new energy materials and its device preparation technical field.The present invention is with MoO3MoS is directly grown on molybdenum foil by simple step chemical vapour deposition technique for evaporation source with S powder2Nano-chip arrays structure, and it is directly used as the anode material of lithium ion battery；The direct-assemblings such as complexed metal lithium foil cathode, diaphragm, electrolyte are at lithium ion battery.The lithium ion battery anode material prepared using this technology, MoS2Nano-chip arrays structure yield is big, purity is high, good crystallinity, regular appearance；MoS2It is incorporated on molybdenum foil to nano-chip arrays close structure；And synthesis growth conditions is stringent controllable, equipment and simple process, at low cost.Lithium ion battery is prepared using this technology, process is simple, it is environmental-friendly, pollution-free, without post-processing；And this new type lithium ion battery specific capacity is high, charge and discharge cycles stability is stablized.
Description
Technical field
The present invention relates to a kind of preparations of the lithium ion battery of molybdenum disulfide nano sheet array structure based on molybdenum foil load
Method belongs to new energy materials and its device preparation technical field.
Background technique
Lithium ion battery has many advantages, such as density is big, specific power is high, is widely used, it is considered to be next
For mixed motivity type automobile or the ideal functionality device of electric vehicle, anode material therein is the commercialized key of lithium ion battery
One of material.Currently, commercialized anode material is mainly graphite material, but its theoretical specific capacity only has 372mAh/
g.Further, since its problems such as there are safety and cycle lives, constrain it in extensive energy storage and electric car field
Extensive use.Therefore, seek the anode material that a kind of specific capacity is high, good cycle and high rate performance are excellent, for mentioning
High-lithium ion battery performance has great importance.
Molybdenum disulfide (MoS2) it is used as a kind of typical class graphene transient metal sulfide, because of its unique excellent electricity
The performances such as, calorifics, mechanics receive significant attention in fields such as new energy, electronic device and photoelectric conversions.MoS2Theoretical hold
Measure higher, about 670mAh/g；And it has many advantages, such as relatively low volume change, rich reserves and at low cost.But make
For lithium ion battery anode material, MoS2Poor electric conductivity inhibit charge its lithium ion energy storage position and external circuit it
Between transfer ability, and then influence the performance of its specific capacity and high rate performance.Recent studies indicate that relative to block material
Material, MoS2Nano structural material is conducive to improve the high rate performance and stable circulation performance of lithium ion battery, because of nanostructure
There is material big specific surface area and high mechanical strength can effectively shorten when as lithium ion battery anode material
The diffusion path of lithium ion promotes its insertion and abjection；Surface area that can be bigger with exposed material, thus provide more lithiums from
The channel of son insertion and abjection；The cyclical stability that lithium ion battery can be improved is effectively prevented from volume in charge and discharge process
Expansion and structure destroy (H.Hwang, et al.MoS2nanoplates consisting of disordered
graphene-like layers for high rate lithium battery anode materials.Nano
Letters,2011,11:4826-4830)。
However, the electrode material as lithium ion battery, traditional method be all by electrode material and polymer bonding agent,
The mixing such as conductive black, is then uniformly coated in conductive current collector.This Fabrication Technology of Electrode will increase the series connection of electrode
Resistance, the diffusion for inhibiting electrolyte and coming into full contact with for electrolyte and active material is interfered, thus reduces the multiplying power of lithium battery
Performance and cycle performance.In order to overcome these disadvantages, there is document to propose and directly grow into active material nano array structure
As the method for electrode on collector matrix, this unique self-supporting electrode can promote the electric conductivity of electrode entirety, thus
Promote charge-discharge performance (S.Chen, et the al.Self-supported Li of battery4Ti5O12nanosheet arrays for
lithium ion batteries with excellent rate capability and ultralong cycle
life.Energy Environmental Science,2014,7:1924-1930)；In addition, nano structural material is directly grown
On a current collector, the mechanical strength that electrode can be improved is effectively prevented from reunion and shape of the active material in charge and discharge process
Cash as, and then promoted lithium ion battery cyclical stability；Also, the excellent collector matrix of electric conductivity is directly as electricity
Pole, assembly operation is easier, cheap.In short, in conjunction with MoS2Class graphene stratiform architectural characteristic, develop a kind of high
Effect, easy method directly grow MoS on collector matrix2Nano-chip arrays structural material, and be used as in lithium ion
The anode of battery will have Important Project value.
Therefore, the invention proposes a kind of MoS based on molybdenum foil load2The system of the lithium ion battery of nano-chip arrays structure
Preparation Method.The present invention is using molybdenum trioxide and sulphur powder as evaporation source, by simple step chemical vapour deposition technique, directly in molybdenum foil
On grow high-purity, high density, high crystalline MoS2Nano-chip arrays structure, and it is directly used as lithium ion battery
Anode material；Complexed metal lithium foil cathode, diaphragm, electrolyte, direct-assembling is at lithium ion in the glove box of argon gas filling
Battery.The lithium ion battery anode material prepared using the method, MoS2The yield of nano-chip arrays structure is big, purity is high, ties
Crystalline substance is good, regular appearance；MoS2It is incorporated on molybdenum foil to nano-chip arrays close structure；And synthesis growth conditions it is stringent controllable,
It is equipment and simple process, low in cost.Lithium ion battery is prepared using the method, preparation process is simple, it is environmental-friendly, without dirt
Dye is not necessarily to post-processing；And this new type lithium ion battery proposed by the present invention, specific capacity is big, battery first time specific discharge capacity
Up to 1041mAh/g, also there is good cyclical stability and high rate performance, be a kind of lithium-ion electric with excellent properties
Pond.
Summary of the invention
It is an object of the invention to propose a kind of MoS based on molybdenum foil load2The lithium ion battery of nano-chip arrays structure
Preparation method.This technology passes through essence using molybdenum trioxide and sulphur powder as evaporation source using simple step chemical vapour deposition technique
The synthesis technologic parameter of true control directly grows vertical, ultra-thin MoS on molybdenum foil2Nano-chip arrays structure (nanometer
Wall)；Then, by this anode material for being directly used as lithium ion battery with height-oriented, ordering growth nano structural material
Expect (self-supporting anode is constituted together with molybdenum foil), metallic lithium foil is assembled with electrolyte, diaphragm and battery case and made as cathode
At high performance lithium ion battery.The MoS prepared using the method2Nano-chip arrays structure anode material, MoS2Nano-chip arrays
The yield of structure is big, density is high, with high purity, good crystallinity, regular appearance；MoS2It is incorporated in molybdenum to nano-chip arrays close structure
On foil；And synthesis growth conditions is stringent controllable, equipment and simple process, low in cost.Lithium ion battery is prepared using the method,
Preparation process is simple, it is environmental-friendly, pollution-free, without post-processing, it is economic and environment-friendly；And this new type lithium ion proposed by the present invention
Battery, specific capacity is big, and battery first time specific discharge capacity also has good cyclical stability and multiplying power up to 1041mAh/g
Performance is a kind of lithium ion battery with excellent properties.
MoS proposed by the present invention based on molybdenum foil load2The preparation method of the lithium ion battery of nano-chip arrays structure,
It is characterized in that, the battery uses and grows vertical, ultra-thin MoS on molybdenum foil2Nano-chip arrays structure is as self-supporting sun
Pole directly assembles with metallic lithium foil cathode, diaphragm, electrolyte, battery case；The self-supporting anode is with molybdenum trioxide
With sulphur powder be evaporation source, by simple step chemical vapour deposition technique, the high-purity directly grown on molybdenum foil, high density,
High crystalline, vertical, ultra-thin MoS2Nano-chip arrays structure.
MoS proposed by the present invention based on molybdenum foil load2The preparation method of the lithium ion battery of nano-chip arrays structure, packet
Include following steps and content:
(1) in vacuum tube furnace, pretreated molybdenum foil is tipped upside down on equipped with the pure MoO of analysis3The aluminium oxide ceramics of powder
On crucible, and the central heating region of tube furnace is placed it in, then will be placed equipped with the alumina ceramic crucible for analyzing pure S powder
Distance is equipped with MoO above air-flow3At the crucible 14-20cm of powder.
(2) before heating, 0.02Pa first is evacuated to whole system hereinafter, being then passed through height into system with vacuum pump
Pure argon is as carrier gas and protects gas, remaining oxygen in removal system.When heating, added with the heating rate of 10-20 DEG C/min
Heat arrives 600-700 DEG C, then keeps the temperature 0.5-1.5 hours；In entire heating process, it is continually fed into 100-150 standard cube li
The high-purity argon gas of rice (sccm) per minute, until the MoS that cooled to room temperature loads to get molybdenum foil2Nano-chip arrays structure
Sample.
(3) in vacuum glove box, by the MoS of obtained molybdenum foil load2Nano-chip arrays structure sample be used as lithium from
The anode of sub- battery analyzes pure metal lithium foil as cathode, and assembled with electrolyte, diaphragm and battery case etc..In group
Before dress, 10 first are evacuated to entire vacuum glove box-3Pa lays equal stress on hereinafter, being then passed through high-purity argon gas thereto as protection gas
It is multiple multiple, to the air in removal system.In an assembling process, the MoS first loaded obtained molybdenum foil2Nanometer sheet battle array
Array structure sample is directly placed into battery case, electrolyte is then added, then be sequentially placed into diaphragm and metallic lithium foil, is covered outer
Battery is finally sealed by shell.
(4) outer packing is carried out to battery.
In the above preparation method, in the step (1) molybdenum foil pretreating process are as follows: by molybdenum foil successively in 0.5-
Dilute hydrochloric acid, acetone and the EtOH Sonicate of 2.5mol/L cleans 10 minutes, then dries spare.Wherein, hydrochloric acid, acetone and ethyl alcohol are equal
For ommercially available AR.
In the above preparation method, molybdenum foil is commercially available common conductive metals in the step (1), with a thickness of 0.05-
0.15mm, size and shape are consistent with commercial li-ion battery case.
In the above preparation method, evaporation source MoO in the step (1)3Powder and S powder are ommercially available AR, are used
Amount is respectively 100-140mg and 500-600mg.
In the above preparation method, in the step (1) sample and raw material setting are as follows: in vacuum tube furnace,
Pretreated molybdenum foil is tipped upside down on equipped with the pure MoO of analysis3On the alumina ceramic crucible of powder, and place it in tube furnace
Heating region is entreated, then distance above air-flow will be placed on equipped with the alumina ceramic crucible for analyzing pure S powder and MoO is housed3Powder
At crucible 14-20cm.
In the above preparation method, carrier gas and protection gas are high-purity argon gas in the step (2), and purity exists
99.99vol.% or more, flow are 100-150 sccm (sccm).
In the above preparation method, heating process in the step (2) are as follows: heated with the heating rate of 10-20 DEG C/min
To 600-700 DEG C, 0.5-1.5 hours then are kept the temperature, finally naturally cools to room temperature.
In the above preparation method, in the step (3), the MoS of obtained molybdenum foil load2Nano-chip arrays structure sample
Product directly as lithium ion battery anode, without carrying out any post-processing.
In the above preparation method, in the step (3), the metallic lithium foil as cathode is ommercially available AR.
In the above preparation method, in the step (3), electrolyte is made of electrolyte and organic solvent.Wherein, it is electrolysed
Matter is lithium hexafluoro phosphate (LiPF6), lithium perchlorate (LiClO4), LiBF4 (LiBF4) one kind；Organic solvent is carbonic acid
Vinyl acetate (EC), the mixed solution of EC and dimethyl carbonate (DMC), the mixed solution of EC and diethyl carbonate (DEC), EC, DMC
With one kind of the mixed solution of methyl ethyl ester (EMC).
In the above preparation method, in the step (3), the diaphragm in lithium battery is polyethylene porous membrane, polypropylene is more
One kind of pore membrane, polyvinylidene fluoride porous film, cellulose laminated film.
In the above preparation method, according to solid and gel electrolyte in the step (3), then electrolyte is played simultaneously
With the effect of diaphragm, solid electrolyte material can be LiPON compound (LiPON), Li at this time0.5La0.5TiO3Or polymer
One kind of electrolyte.
In the above preparation method, in the step (3), battery case is high insulating rigid material.
In the above preparation method, in the step (3), the argon gas as protection gas is high-purity gas, and purity exists
99.99vol.% or more.
In the above preparation method, in the step (3), before assembling, 10 first are evacuated to entire vacuum glove box- 3Then Pa is hereinafter, being passed through high-purity argon gas as protection gas thereto and being repeated as many times, to the air in removal system.
In the above preparation method, in the step (3), lithium ion battery sealing after must do so without leakage, it is air tight,
Leakproof.
In the above preparation method, in the step (4), prepared lithium ion battery is button, pillar, case in appearance
One kind of formula or All-solid film batteries.
One of the advantages of the present invention is: the MoS prepared using this technology2In nano-chip arrays structure anode material, MoS2
The yield of nano-chip arrays structure is big, density is high, with high purity, good crystallinity, regular appearance；MoS2Nano-chip arrays close structure
Ground is incorporated on molybdenum foil；And synthesis growth conditions is strictly controllable, equipment and simple process, product yield is high, production process cleaning
Environmental protection, it is low in cost.
The two of advantages of the present invention are: lithium ion battery is prepared using this technology, preparation process is simple, it is environmental-friendly,
It is pollution-free, without post-processing, it is economic and environment-friendly；And this new type lithium ion battery proposed by the present invention, specific capacity is big, battery first
Secondary specific discharge capacity also has good cyclical stability and high rate performance up to 1041mAh/g, is a kind of with excellent properties
Lithium ion battery.
Detailed description of the invention
Fig. 1 is the MoS of the load of molybdenum foil obtained by the embodiment of the present invention 12The x-ray diffraction pattern of nano-chip arrays structure
Fig. 2 is the MoS of the load of molybdenum foil obtained by the embodiment of the present invention 12The stereoscan photograph of nano-chip arrays structure
Fig. 3 is the MoS based on molybdenum foil load obtained by the embodiment of the present invention 12The lithium-ion electric of nano-chip arrays structure
The structural schematic diagram in pond
Fig. 4 is the MoS based on molybdenum foil load obtained by the embodiment of the present invention 12The lithium-ion electric of nano-chip arrays structure
The charging and discharging curve in pond
Specific embodiment
Below with reference to embodiment, technical scheme is described further.
The present invention proposes a kind of MoS based on molybdenum foil load2The preparation method of the lithium ion battery of nano-chip arrays structure,
It is characterized in that, the battery is used grows vertical, ultra-thin MoS on molybdenum foil2Nano-chip arrays structure is as self-supporting
Anode directly assembles with metallic lithium foil cathode, diaphragm, electrolyte, battery case；The self-supporting anode is with three oxidations
Molybdenum and sulphur powder are evaporation source, the high-purity directly grown on molybdenum foil, highly dense by simple step chemical vapour deposition technique
Degree, high crystalline, vertical, ultra-thin MoS2Nano-chip arrays structure；Include the following steps and content:
(1) in vacuum tube furnace, 10 points will be successively cleaned by ultrasonic with the dilute hydrochloric acid, acetone and ethyl alcohol of 0.5-2.5mol/L
The drying molybdenum foil of the pretreated 0.05-0.15mm thickness of clock, which is tipped upside down on, analyzes pure MoO equipped with 100-140mg3The aluminium oxide of powder is made pottery
On porcelain crucible, and the central heating region of tube furnace is placed it in, the aluminium oxide of pure S powder then will be analyzed equipped with 500-600mg
Ceramic crucible is placed on distance above air-flow and MoO is housed3At the crucible 14-20cm of powder.
(2) before heating, 0.02Pa first is evacuated to whole system hereinafter, being then passed through into system pure with vacuum pump
High-purity argon gas of the degree in 99.99vol.% or more as carrier gas and protects gas, remaining oxygen in removal system.When heating, with
The heating rate of 10-20 DEG C/min is heated to 600-700 DEG C, then keeps the temperature 0.5-1.5 hours；In entire heating process, hold
The continuous high-purity argon gas for being passed through 100-150 sccm (sccm), until cooled to room temperature is negative to get molybdenum foil
The MoS of load2Nano-chip arrays structure sample, it is spare.
(3) preparation of lithium-ion battery module.Electrolyte in lithium ion battery is made of electrolyte and organic solvent,
Middle electrolyte is lithium hexafluoro phosphate (LiPF6), lithium perchlorate (LiClO4), LiBF4 (LiBF4) one kind；Organic solvent
For ethylene carbonate (EC), the mixed solution of EC and dimethyl carbonate (DMC), the mixed solution of EC and diethyl carbonate (DEC),
One kind of the mixed solution of EC, DMC and methyl ethyl ester (EMC).Diaphragm in lithium ion battery be polyethylene porous membrane,
One kind of polypropylene porous film, polyvinylidene fluoride porous film, cellulose laminated film.According to solid and gel electrolyte, then
Play the effect of electrolyte and diaphragm simultaneously, at this time solid electrolyte material can for LiPON compound (LiPON),
Li0.5La0.5TiO3Or one kind of polymer dielectric.The shell of lithium ion battery is high insulating rigid material.
(4) battery assembly.In vacuum glove box, by the MoS of obtained molybdenum foil load2Nano-chip arrays structure sample
Anode as lithium ion battery analyzes pure metal lithium foil as cathode, and carry out group with electrolyte, diaphragm and battery case etc.
Dress.Before assembling, 10 first are evacuated to entire vacuum glove box-3Then Pa hereinafter, be passed through high-purity argon gas as guarantor thereto
It protects gas and is repeated as many times, to the air in removal system.In an assembling process, the MoS first loaded obtained molybdenum foil2
Nano-chip arrays structure sample is directly placed into battery case, electrolyte is then added, then be sequentially placed into diaphragm and metallic lithium foil,
Shell is covered, is finally sealed battery.Lithium ion battery after sealing must do so without leakage, air tight, leakproof.
(5) outer packing is carried out to battery.Final prepared lithium ion battery is button in appearance, pillar, box or complete
Solid-state thin-film battery.
The MoS of obtained molybdenum foil load2Nano-chip arrays structure sample is black thin film sample in appearance.X-ray is spread out
Penetrate analysis shows, this material be high-purity, the good MoS of crystallinity2Phase (see Fig. 1).Under a scanning electron microscope, in molybdenum
Foil surface is it is observed that ultra-thin MoS highdensity, vertical-growth, in a crisscross manner2Nano-chip arrays structure (nm wall), receives
Rice piece thickness about 10nm (see Fig. 2).
Cyclic charging and discharging test shows that obtained this lithium ion battery specific capacity is big, battery first time electric discharge specific volume
It measures up to 1041mAh/g, and also there is good cyclical stability and high rate performance.
In short, the MoS based on molybdenum foil load can be prepared with this technology2The high performance lithium of nano-chip arrays structure from
Sub- battery.
Embodiment 1: in vacuum tube furnace, pure MoO will be analyzed equipped with 120mg3The alumina ceramic crucible of powder is placed on
Tube furnace center heating region, then the molybdenum foil (thickness 0.08mm) of Φ 19mm size is buckled on this crucible.Then it will be equipped with
The alumina ceramic crucible that 550mg analyzes pure S powder is placed on air-flow upstream distance equipped with MoO3At the crucible 16cm of powder.It is heating
Before, being first just evacuated to 0.02Pa to whole system with vacuum pump, (purity exists hereinafter, being then passed through high-purity argon gas into system
99.99vol.% or more), and be so repeated 3 times.Then tube furnace is raised to 650 DEG C with the rate of 15 DEG C/min, and keeps the temperature 60
Minute.In entire heating process, it is continually fed into the high-purity argon gas of 100 sccms (sccm), until nature
It is cooled to room temperature the MoS to get molybdenum foil load2Nano-chip arrays structure sample.
The MoS that resulting molybdenum foil is loaded2Nano-chip arrays structure sample directly as lithium ion battery anode, 0.8
The metallic lithium foil of × 0.6cm size is as cathode, 1mol/L LiPF6(solvent volume is than EC and DEC for 1:1) is as electrolysis
Liquid, polyethylene porous membrane are that diaphragm, button cell shell etc. are placed into vacuum glove box structural schematic diagram group as shown in Figure 3
Dress up button cell.
Before assembling, 10 first are evacuated to entire vacuum glove box-3Then Pa hereinafter, be passed through high-purity argon gas work thereto
It for protection gas and is repeated as many times, to the air in removal system.In an assembling process, obtained molybdenum foil is loaded first
MoS2Nano-chip arrays structure sample is directly placed into battery case, electrolyte is then added, then be sequentially placed into diaphragm and metal
Lithium foil, covers shell.Battery is sealed.Finally carry out outer packing.
X-ray diffraction analysis shows, the MoS of synthesized this molybdenum foil load2Nano-chip arrays structural material is high-purity
Degree, the good six sides MoS of crystallinity2Phase (see Fig. 1).Under a scanning electron microscope, on molybdenum foil surface it is observed that high density
Vertical-growth, ultra-thin MoS2Nano-chip arrays structure (nm wall), nanometer sheet thickness about 10nm (see Fig. 2).
The MoS that prepared button is loaded based on molybdenum foil2The lithium ion battery of nano-chip arrays structure, in 0.01-3V electricity
Cyclic charging and discharging test is carried out under pressure, 0.1A/g current density, charge-discharge performance is good (see Fig. 4), and specific capacity is big, battery first
Secondary specific discharge capacity also has good cyclical stability and high rate performance up to 1041mAh/g, is a kind of high performance lithium
Ion battery.
Claims (3)
1. the MoS based on molybdenum foil load2The preparation method of the lithium ion battery of nano-chip arrays structure, which is characterized in that the electricity
Pond uses and grows vertical, ultra-thin MoS on molybdenum foil2Nano-chip arrays structure is as self-supporting anode, directly and lithium metal
Foil cathode, diaphragm, electrolyte, battery case assemble；The self-supporting anode be using molybdenum trioxide and sulphur powder as evaporation source,
It is the high-purity directly grown on molybdenum foil, high density, high crystalline, vertical, super by simple step chemical vapour deposition technique
Thin MoS2Nano-chip arrays structure；The following steps are included:
(1) in vacuum tube furnace, the molybdenum foil of pretreated 0.05-0.15mm thickness is tipped upside down on and is analyzed equipped with 100-140mg
Pure MoO3On the alumina ceramic crucible of powder, and the central heating region of tube furnace is placed it in, then 500-600mg will be housed
The alumina ceramic crucible for analyzing pure S powder is placed on distance above air-flow and MoO is housed3At the crucible 14-20cm of powder；
(2) before heating, 0.02Pa first is evacuated to whole system hereinafter, being then passed through purity into system with vacuum pump
The high-purity argon gas of 99.99vol.% or more is as carrier gas and protects gas, remaining oxygen in removal system；When heating, with 10-20
DEG C/heating rate of min is heated to 600-700 DEG C, then keep the temperature 0.5-1.5 hours；In entire heating process, it is continually fed into
The high-purity argon gas of 100-150 sccm (sccm) is loaded until cooled to room temperature to get molybdenum foil
MoS2Nano-chip arrays structure sample；
(3) in vacuum glove box, by the MoS of obtained molybdenum foil load2Nano-chip arrays structure sample is used as lithium ion battery
Anode, analyze pure metal lithium foil as cathode, and assembled with electrolyte, diaphragm and battery case etc.；Before assembling, first
10 are evacuated to entire vacuum glove box-3Pa is used as protection gas and is repeated as many times hereinafter, being then passed through high-purity argon gas thereto,
To the air in removal system；In an assembling process, the MoS first loaded obtained molybdenum foil2Nano-chip arrays structure
Sample is directly placed into battery case, electrolyte is then added, then be sequentially placed into diaphragm and metallic lithium foil, covers shell, finally
Battery is sealed；
(4) outer packing is carried out to battery.
2. preparation method described in accordance with the claim 1, which is characterized in that MoO in the step (1)3Powder and S powder are commercially available
Analytical reagents, molybdenum foil is commercially available common conductive metals, with a thickness of 0.05-0.15mm；The pretreating process of molybdenum foil are as follows: by molybdenum foil
It successively cleans 10 minutes, then dries spare in the dilute hydrochloric acid of 0.5-2.5mol/L, acetone and EtOH Sonicate；Sample and raw material
Setting are as follows: in vacuum tube furnace, pretreated molybdenum foil is tipped upside down on equipped with the pure MoO of analysis3The aluminium oxide ceramics of powder
On crucible, and the central heating region of tube furnace is placed it in, then will be placed equipped with the alumina ceramic crucible for analyzing pure S powder
Distance is equipped with MoO above air-flow3At the crucible 14-20cm of powder；High-purity argon gas purity exists in the step (2) and (3)
99.99vol.% or more；Heating process in the step (2) are as follows: 600-700 is heated to the heating rate of 10-20 DEG C/min
DEG C, 0.5-1.5 hours then are kept the temperature, finally naturally cools to room temperature, and in entire heating process, be continually fed into 100-150
The high-purity argon gas of sccm (sccm).
3. preparation method described in accordance with the claim 1, which is characterized in that by electrolyte and there is electrolyte in the step (3)
Solvent composition, wherein electrolyte is one kind of lithium hexafluoro phosphate, lithium perchlorate, LiBF4；Organic solvent is carbonic acid second
Enester (EC), the mixed solution of EC and dimethyl carbonate (DMC), the mixed solution of EC and diethyl carbonate (DEC), EC, DMC and
One kind of the mixed solution of methyl ethyl ester (EMC)；Diaphragm is polyethylene porous membrane, polypropylene porous film, polyvinylidene fluoride
One kind of alkene perforated membrane, cellulose laminated film；According to solid and gel electrolyte, then electrolyte and diaphragm are played simultaneously
Effect, solid electrolyte material can be LiPON compound (LiPON), Li at this time0.5La0.5TiO3Or polymer dielectric it
It is a kind of；Battery case is high insulating rigid material；Prepared lithium ion battery is button in appearance, pillar, box or complete solid
One kind of state hull cell.
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| CN113484341A (en) * | 2021-07-01 | 2021-10-08 | 南京工业大学 | Method for preparing TEM sample based on hybrid lead-based perovskite nanosheets |
| CN115020118A (en) * | 2022-07-20 | 2022-09-06 | 兰州大学 | Preparation method of composite electrode material, super capacitor and battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109950509A (en) * | 2019-04-09 | 2019-06-28 | 武汉轻工大学 | A kind of MoO2/MoS2Combination electrode material and preparation method thereof |
| CN109950509B (en) * | 2019-04-09 | 2021-08-20 | 武汉轻工大学 | MoO (MoO)2/MoS2Composite electrode material and preparation method thereof |
| CN111514916A (en) * | 2020-05-12 | 2020-08-11 | 刘志国 | Method for preparing nitrogen-doped molybdenum-based chalcogenide catalytic material for hydrogen evolution by water electrolysis |
| CN113484341A (en) * | 2021-07-01 | 2021-10-08 | 南京工业大学 | Method for preparing TEM sample based on hybrid lead-based perovskite nanosheets |
| CN115020118A (en) * | 2022-07-20 | 2022-09-06 | 兰州大学 | Preparation method of composite electrode material, super capacitor and battery |
| CN115020118B (en) * | 2022-07-20 | 2024-04-09 | 兰州大学 | Preparation method of composite electrode material, supercapacitor and battery |
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