CN105047914B - A kind of lithium ion battery negative material molybdenum disulfide/carbon and preparation method thereof - Google Patents
A kind of lithium ion battery negative material molybdenum disulfide/carbon and preparation method thereof Download PDFInfo
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- CN105047914B CN105047914B CN201510284228.2A CN201510284228A CN105047914B CN 105047914 B CN105047914 B CN 105047914B CN 201510284228 A CN201510284228 A CN 201510284228A CN 105047914 B CN105047914 B CN 105047914B
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- lithium ion
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- molybdenum disulfide
- battery negative
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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
- H01M4/58—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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/58—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
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- 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
The invention discloses a kind of lithium ion battery negative material molybdenum disulfide/carbon and preparation method thereof, the MoS of dry agaric shape has been prepared with thermal reduction2/ C composite, it is prepared into after half-cell and tests its chemical property and show its specific capacity height, stable cycle performance.This method is simple and reliable, good process repeatability, workable, can be widely popularized.Its preparation method includes several steps：1) it is raw material to take appropriate four thio ammonium molybdate, cetyl trimethylammonium bromide, silica nanosphere；2) sample is prepared with thermal reduction；3) required product is obtained after removing silica with hydrofluoric acid.
Description
Technical field
The present invention relates to a kind of lithium ion battery negative material and preparation method thereof, more particularly to a kind of lithium ion battery is born
Pole material molybdenum disulfide/carbon (MoS2/ C) and preparation method thereof.
Background technology
Achievement acquired by the progress of the mankind at this stage and the development of society largely depends on oil, coal
The traditional fossil energies such as charcoal.With the continuous consumption and not exclusively use of these non-regeneration energies, the whole world is faced with the energy
Crisis and serious problem of environmental pollution.The words such as Global Greenhouse Effect, disruption of ecological balance, haze were becoming familiar to the ear energy in recent years
In detail, how to solve these problems, the huge challenge of scientific technological advance is become.Therefore, the renewable new energy of cleaning is developed
Become study hotspot.Wherein the regenerative resource such as solar energy, wind energy and biological energy source has had a popularization in some places, but by
It is high to geographical factors dictate in it, to realize that whole world popularization has certain difficulty, so its development process is slow.
Secondary cell energy system using lithium ion battery as representative has high operating voltage, specific capacity height, self discharge effect
Should small, in light weight, small volume, memory-less effect and the excellent properties such as environment-friendly not only become at present it is most popular just
Formula electronic equipment power source is taken, while great concern is caused in electric automobile field.Therefore, countries in the world will be each from now on
Kind lithium ion battery used for electric vehicle also opens wide hair as industry of giving priority to for China's electrokinetic cell industry
Open up space.However, current lithium ion battery can not also meet Large-scale Mobile equipment high-energy-density, be capable of wanting for fast charging and discharging
Ask.This just makes the study hotspot of lithium ion battery be centered around raising battery energy density, strengthen battery cyclical stability and
Solve the problems, such as fast charging and discharging, so that lithium ion battery disclosure satisfy that the demand of Large-scale Mobile equipment, and then promote lithium ion
Battery industry is fast-developing.
Research wherein for negative material focuses primarily upon the following aspects：Relatively low electrode potential, higher ratio
Good compatible, the relatively low life of the battery part such as capacity and good cyclical stability and electrolyte and adhesive
Produce the environment friendly of cost and safety non-pollution.Graphite is due to good cycling stability at present, and operating voltage is higher, and material comes
Source is wide, low production cost and by extensively with for lithium ion battery negative material, and have been commercialized.But the ratio of graphite electrode
Capacity is relatively low (~372mAh/g), and which also limits the further development of lithium ion battery.Therefore, how the property prepared
Focus of the more preferable negative material of energy into Study on Li-ion batteries in recent years.
Molybdenum disulfide (MoS with typical layered structure2) possess and structure as graphite-phase：Layer in S-Mo-S atoms it
Between by stronger Covalent bonding together, and then combined between layers by weaker Van der Waals force.Just because of MoS2Interlayer is weaker
Bonding so that it can introduce external molecule, atom or ion without changing its layer by the method for intercalation in its interlayer
Interior structure, form composite.As lithium ion battery negative material, MoS2There is very high initial capacity (~670mAh/
G), its special layer structure is beneficial to Li+Insertion and abjection.However, due to itself low electrons/ions electrical conductivity and
Serious volumetric expansion make it that its cyclical stability is extremely low during removal lithium embedded.In addition, during cell reaction, MoS2With Li+
React and generate the Li of indissoluble2S, Li2S again catalytic electrolysis liquid decomposition so as to formed thickness polymeric layer cause it is irreversible
Capacitance loss, the reason for this is also its cyclical stability difference.Therefore how MoS is improved2Cyclical stability, into MoS2As
The key of lithium ion battery negative material research.
If by MoS2Combine to form composite with carbon material, high power capacity may be obtained and good circulation is stable
The electrode material of property.Cetyl trimethylammonium bromide (CTAB) is a kind of common cationic surfactant, is usually used in material
The controllable preparation of material, thus it is possible to vary the microscopic appearance of material, while it contains many carbons, carbon source can be served as, in Re Chu
Carbon is obtained after reason.Silica nanosphere is often used as template and prepares porous material, can increase the surface area of material.In lithium
In ion negative material, the increase of material surface area can increase the contact area of electrode and lithium ion in electrolyte and activity is inhaled
Attached, desorption center, so as to be advantageous to embedding de- lithium reaction, increase the lithium storage content of material.
The content of the invention
Goal of the invention：In order to overcome the deficiencies in the prior art, the present invention provides a kind of negative electrode of lithium ion battery material
Expect molybdenum disulfide/carbon (MoS2/ C) and preparation method thereof, this method is simple and reliable, good process repeatability, workable.
Technical scheme：To achieve the above object, the technical solution adopted by the present invention is：
A kind of lithium ion battery negative material molybdenum disulfide/carbon, raw material is by four thio ammonium molybdate, cetyl trimethyl bromine
Change ammonium, silica nanosphere and absolute ethyl alcohol composition.
Further, in the present invention, the four thio ammonium molybdate, cetyl trimethylammonium bromide and silica are received
The ratio between amount of material of rice ball three is 1:0.14~0.43:1.7~1.75；The absolute ethyl alcohol is 30ml.
Further, in the present invention, a diameter of 20nm of the silica nanosphere, content are>99wt%.
The method for preparing the lithium ion battery negative material molybdenum disulfide/carbon, comprises the following steps：
1) raw material is mixed, stirs to absolute ethyl alcohol and volatilize, residual powder is dried at 50~65 DEG C；
2) step 1) the dried powder is placed under atmosphere in tube furnace and is incubated 4h, be cooled to room temperature, obtain
To black powder；
3) by step 2) the black powder hydrofluoric acid treatment, filtration drying, product MoS is obtained2/ C composite.
Further, in the present invention, atmosphere described in step 2) is the mixed atmosphere of argon gas and hydrogen, the argon gas and
The volume ratio of hydrogen is 9.5:0.5.
Further, in the present invention, the temperature stabilization of insulating process described in step 2) is 700~800 DEG C.
Further, in the present invention, the mass concentration of hydrofluoric acid described in step 3) is 5~6%.
Beneficial effect：Lithium ion battery negative material molybdenum disulfide/carbon (MoS provided by the invention2/ C) and its preparation side
Method, compared with prior art, have the advantage that：
1. product is prepared using thermal reduction in the present invention, this method is simple and reliable, good process repeatability, operability
By force；
2. products obtained therefrom of the present invention carries out electrochemical property test after being assembled into half-cell, test result shows that the material has
There are high specific capacity and excellent cyclical stability.
Brief description of the drawings
Fig. 1 is the MoS being prepared2The thermogravimetric curve schematic diagram of/C composite；
Fig. 2 is the MoS being prepared2The scanning electron microscope image schematic diagram of/C composite；
Fig. 3 is the MoS being prepared2The images of transmissive electron microscope schematic diagram of/C composite, wherein illustration transmit for high power
Sem image；
Fig. 4 is the MoS being prepared2The MoS that/C composite is prepared2The cycle characteristics curve of/C composite
Charging and discharging curve schematic diagram；
Fig. 5 is the MoS being prepared2The CV curve synoptic diagrams of/C composite；
Fig. 6 is the MoS being prepared2/ C composite in 100mA g-1Current density under cycle characteristics curve show
It is intended to；
Fig. 7 is the MoS being prepared2The cycle characteristics curve synoptic diagram of/C composite under different multiplying.
Embodiment
The present invention is further described below in conjunction with the accompanying drawings.
A kind of lithium ion battery negative material molybdenum disulfide/carbon (MoS2/ C), reaction raw materials are by four thio ammonium molybdate, 16
Alkyl trimethyl ammonium bromide, silica nanosphere and absolute ethyl alcohol composition.Wherein, four thio ammonium molybdate, cetyl front three
The ratio between amount of material of base ammonium bromide and silica nanosphere three is 1:0.14~0.43:1.7~1.75；Absolute ethyl alcohol is
30ml.The a diameter of 20nm of silica nanosphere, content are>99wt%.
Medicine is as follows：
Four thio ammonium molybdate, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group, Shanghai；
Cetyl trimethylammonium bromide, analyze pure, Shanghai Ling Feng chemical reagent Co., Ltd, Shanghai；
Silica nanosphere, diameter 20nm, content：>99wt%, Nanjing Xian Feng Nono-material Science ＆ Technology Ltd., south
Capital；
Absolute ethyl alcohol, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group, Shanghai.
The method for preparing lithium ion battery negative material molybdenum disulfide/carbon, dry agaric is prepared with thermal reduction
The MoS of shape2/ C composite, it is prepared into after half-cell and tests its chemical property and show its specific capacity height, stable cycle performance.
Specifically include following steps：
1) all reaction raw materials are mixed, is stirred at room temperature to solvent absolute ethyl alcohol and volatilizees completely, residual powder is existed
It is dried at 50~65 DEG C；
2) the dried powder of step 1) is placed under the mixed atmosphere of argon gas and hydrogen in tube furnace with 700~800
DEG C insulation 4h, then naturally cools to room temperature, obtains black powder；
3) the black powder mass concentration for obtaining step 2) is 5~6% hydrofluoric acid treatment, removes SiO2, filtering
Dry, obtain final product MoS2/ C composite.
Embodiment 1
A kind of lithium ion battery negative material molybdenum disulfide/carbon (MoS2/ C), reaction raw materials are by four thio ammonium molybdate
(the ratio between amount of three's material is 1 by 0.250g, cetyl trimethylammonium bromide 0.050g, silica nanosphere 0.100g:
0.143:1.733) and absolute ethyl alcohol 30ml prepares MoS2/ C reaction raw materials；
1) by the MoS2The reaction raw materials of/C composite are stirred at room temperature until solvent volatilizees completely, by remaining powder
End is dried at 50~65 DEG C；
2) volume ratio that step 1) the dried powder is placed in argon gas and hydrogen is 9.5:0.5 mixed atmosphere
Under, with 700~800 DEG C of insulation 4h in tube furnace, naturally cool to room temperature and obtain black powder；
3) by the hydrofluoric acid treatment that the black powder concentration described in step 3 is 5~6%, SiO is removed2, after filtration drying
Obtain final product MoS2/ C composite.
The MoS being prepared as shown in Figure 1 for embodiment 12The thermogravimetric curve of/C composite.Can be with from thermogravimetric curve
Seeing at 50 DEG C or so has an obvious weightless process, and this is the evaporation of moisture in sample.It is second at 270 DEG C to 500 DEG C
Secondary weightless process, this is by MoS2Caused by the aerial oxidation of carbon.And have third time weightlessness at 650 DEG C to 1000 DEG C,
Corresponding to MoO3Distillation.According to this part MoO3Distillation caused by it is weightless be 42.9%, calculated the carbon content in material
For 33.4%.
Fig. 2 is the MoS that embodiment 1 is prepared2The scanning electron microscope image of/C composite.Material is found out from scan image
Material surface shows a kind of plate like structure of class, and overall pattern is similar to dry agaric.This of material is similar to drying
The pattern of agaric adds the surface area of material, is advantageous to more lithium ion insertions, so as to improve the lithium storage content of material.
Fig. 3 is the MoS that embodiment 1 is prepared2The images of transmissive electron microscope of/C composite, wherein illustration transmit for high power
Sem image.It can clearly be seen that the lamellar structure of material, measures to it and find that interlamellar spacing is 1.03nm from high power figure,
Compare MoS2Original 0.62nm increased.Lamella is unordered in a jumble simultaneously, and the accumulation number of plies is seldom, is individual layer or 2~3 layers, and piece
Layer size is smaller.
Fig. 4 is the MoS that embodiment 1 is prepared2The MoS that/C composite is prepared2The cycle characteristics of/C composite
The charging and discharging curve of curve.In discharge process first, the discharge curve of material is the curve of consecutive variations, without obvious electricity
Bit platform, because influence of the presence of carbon to material charge and discharge process.And in second and third time discharge curve,
Occurs an obvious potential plateau at~1.9V, the platform is first reduced into polysulfide corresponding to sulphur, then become again
Into Li2S reaction.Both have two potential plateaus, corresponding to Li in charging curve three times at~2.2 and 1.75V2S
It has been oxidized to the reaction of sulphur.
Fig. 5 is the MoS that embodiment 1 is prepared2The CV curves of/C composite.In first time is circulated, in~0.8V
There is a unconspicuous wide reduction peak at place, has a reduction peak at~0.45V, corresponds respectively to Li+Insert MoS2Interlayer,
Form LixMoS2And LixMoS2It is converted further into Mo and Li2S reaction.In second and third time circulate, oxidation peak
Position do not change, and~0.45V and~0.8V place reduction peak disappear, corresponding to multistep reaction generation Li2S。
Fig. 6 is the MoS that embodiment 1 is prepared2/ C composite in 100mA g-1Current density under circulation it is special
Linearity curve；Cycle-index by 0 increase to 100 times between, it is about stable that chemical property experiment measures the specific capacity of the product
In 800~1000mAh g-1Between, illustrate the product of the present invention through electrochemical property test, it was demonstrated that it has specific capacity high, follows
The characteristic of ring stable performance.
Fig. 7 is the MoS that embodiment 1 is prepared2The cycle characteristics curve of/C composite under different multiplying.From figure
It can be seen that passing through 200mA g respectively-1、400mA g-1、600mA g-1、800mA g-1With 1000mA g-1Gradually increase
It is recycled under current density after 150 times, material still can keep 560mAh g-1Specific capacity, and from 1000mA g-1
Return to 100mA g-1When, its reversible capacity can almost be promptly restored to initial 100mA g-1Capability value during circulation, and
There is no the decay of capacity in follow-up circulation.
Embodiment 2
As different from Example 1, reaction raw materials are the present embodiment：Four thio ammonium molybdate 0.250g, cetyl front three
(the ratio between amount of three's material is 1 by base ammonium bromide 0.100g, silica nanosphere 0.100g:0.286:And anhydrous second 1.733)
Alcohol 30ml, other are same as Example 1.
Embodiment 3
The present embodiment as different from Example 1, four thio ammonium molybdate 0.250g, cetyl trimethyl bromine in step 1
Change ammonium 0.150g, (the ratio between amount of three's material is 1 to silica nanosphere 0.100g:0.429:1.733) and absolute ethyl alcohol
30ml, other are same as Example 1.
Described above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
- A kind of 1. lithium ion battery negative material molybdenum disulfide/carbon, it is characterised in that：Raw material is by four thio ammonium molybdate, hexadecane Base trimethylammonium bromide, silica nanosphere and absolute ethyl alcohol composition；The four thio ammonium molybdate, cetyl trimethyl bromine It is 1 to change the ratio between ammonium and the amount of material of silica nanosphere three:0.14~0.43:1.7~1.75；The absolute ethyl alcohol is 30 ml；The preparation method of the lithium ion battery negative material molybdenum disulfide/carbon comprises the following steps：1）The raw material is mixed, stirs to absolute ethyl alcohol and volatilizees, residual powder is dried at 50 ~ 65 DEG C；2）By step 1）The dried powder is placed under atmosphere is incubated 4h in tube furnace, is cooled to room temperature, obtains black Color powder；3）By step 2）The black powder hydrofluoric acid treatment, filtration drying, obtains product MoS2/ C composite.
- 2. lithium ion battery negative material molybdenum disulfide/carbon according to claim 1, it is characterised in that：The titanium dioxide A diameter of 20 nm of silicon nanosphere, content are> 99 wt%.
- 3. lithium ion battery negative material molybdenum disulfide/carbon according to claim 1, it is characterised in that：Step 2）Middle institute Atmosphere is stated as argon gas and the mixed atmosphere of hydrogen, the volume ratio of the argon gas and hydrogen is 9.5:0.5.
- 4. lithium ion battery negative material molybdenum disulfide/carbon according to claim 1, it is characterised in that：Step 2）Middle institute The temperature stabilization for stating insulating process is 700 ~ 800 DEG C.
- 5. lithium ion battery negative material molybdenum disulfide/carbon according to claim 1, it is characterised in that：Step 3）Middle institute The mass concentration for stating hydrofluoric acid is 5 ~ 6%.
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| CN107248573A (en) * | 2017-06-26 | 2017-10-13 | 浙江工业大学 | Polyphosphazene is combined the preparation method of carbon composite electrode material for the molybdenum disulfide of carbon source |
| CN109830670B (en) * | 2019-03-04 | 2021-11-12 | 郑州大学 | Hollow sandwich type SiO for lithium ion battery cathode material2/C/MoS2Hybrid microspheres |
| CN111864209B (en) * | 2020-05-14 | 2021-11-30 | 清华大学 | Preparation method and application of lithium-sulfur battery positive electrode material |
| CN114520327B (en) * | 2020-11-20 | 2023-11-07 | 中国科学院大连化学物理研究所 | Preparation method and application of mesoporous molybdenum disulfide/carbon composite material |
| CN113173601B (en) * | 2021-04-25 | 2022-09-02 | 黑龙江大学 | Thin-layer MXene/hexagonal phase molybdenum disulfide composite material and preparation method and application thereof |
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| CN102208634B (en) * | 2011-05-06 | 2014-04-16 | 北京科技大学 | Porous silicon/carbon composite material and preparation method thereof |
| AU2012275046A1 (en) * | 2011-06-30 | 2014-01-23 | Cornell University | Hybrid materials and nanocomposite materials, methods of making same, and uses thereof |
| CN102500360B (en) * | 2011-11-15 | 2013-08-14 | 中国科学院上海硅酸盐研究所 | Method for preparing mesoporous tungsten oxide/carbon composite conductive materials |
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