CN106450185B - MoS2Nanoneedle/carbon nanotube composite negative pole material preparation method - Google Patents
MoS2Nanoneedle/carbon nanotube composite negative pole material preparation method Download PDFInfo
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- CN106450185B CN106450185B CN201610875853.9A CN201610875853A CN106450185B CN 106450185 B CN106450185 B CN 106450185B CN 201610875853 A CN201610875853 A CN 201610875853A CN 106450185 B CN106450185 B CN 106450185B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- 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
- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 MoS2Nanoneedle is epitaxially grown in the preparation method of carbon nanotube composite negative pole material.By using chemical vapour deposition technique, MoS is prepared2Nanoneedle/carbon nano tube compound material.MoS2It is combined with carbon nanotube in interface coherence, improves the bond strength of the two, guarantee that active material configuration is stablized in charge and discharge process, and accelerate the transmission of electronics in electrochemical reaction process;MoS2Nanoneedle prevents nano active substance from reuniting in charge and discharge process in being uniformly distributed for carbon nanotube;Flexible carrier carbon nanotube can alleviate volume change of the active material in charge and discharge process, ensure electrode structure stability.The advantage of the invention is that the preparation process of composite material is simple, yield is big, is suitble to large-scale industrial production.The MoS of the method preparation2Nanoneedle/carbon nano tube compound material has stable cycle performance and excellent high rate performance, is a kind of ideal lithium ion battery negative material, can be widely applied to the fields such as portable electronic device, electric car and aerospace.
Description
Technical field
The invention belongs to new energy materials and electrochemical field, and in particular to a kind of MoS2Nanoneedle/carbon nanotube is novel
Can charging-discharging lithium ion battery composite negative pole material preparation method.
Technical background
Lithium ion battery have many advantages, such as energy density it is high, it is environmental-friendly, have extended cycle life, in the convenient electricity such as mobile communication
It is widely applied in sub- equipment.With its high performance advantage, the main development for becoming power battery becomes lithium ion battery
Gesture has become hot spot and China's new-energy automobile industrialization of international competition using lithium ion battery as the electric car of power
Main way.Graphite material is now widely used lithium ion battery negative material, has the advantages that good cycle, but
Its specific capacity is lower, and (theoretical capacity is 372mAh g-1).Lithium ion battery of new generation, especially power lithium-ion battery is to electrode
Material specific capacity and in terms of put forward higher requirements.Therefore, research and development have specific capacity high and cyclicity
The excellent novel anode material of energy is of great significance for lithium ion battery of new generation, especially power lithium-ion battery technology
With specific application value.
MoS2Material, theoretical capacity are up to 667mAh g-1, resourceful, low toxicity is low in cost, receives in recent years
The extensive concern of researchers.But MoS2Along with biggish volume change during removal lithium embedded, so that active particle is sent out
Fecula, active material falls off from collection liquid surface and loses electrical contact, so as to cause capacity sharp-decay.In addition, MoS2Material
The electronic conductance of material is poor, causes electrochemical reaction dynamics slower, and electrode ladder high rate performance is not fully up to expectations.Currently, changing
Kind MoS2The method of chemical property specifically includes that reduction particle size, shortens lithium ion diffusion path, accelerates electrochemical reaction
Dynamics;Special appearance is synthesized, the volume change during removal lithium embedded is buffered.Another kind is effectively improved MoS2Chemical property
Method is to be compounded to form compound with compliant conductive matrix, the electronic conductance of composite material not only can be improved, but also can buffer and fill
Volume change in discharge process.
Representative MoS in document2The research work of base electrode material includes:
(1) Tsinghua University Wang Xun teaches research group and uses mixed solution method, by regulating and controlling the type of alcohol in solution,
The MoS of different scale and pattern is prepared2Material.Synthesize monodispersed MoS when alcohols material used is ethyl alcohol2Nanometer
Piece tests the discovery of its chemical property as lithium ion battery negative material: cyclical stability and ladder high rate performance compared with
Difference.In 100mAg-1Low current under, capacity sharp-decay, circulation 50 times after, reversible capacity only has 606mAh g-1;With
Current density is gradually increased, and capacity attenuation is very fast, and when electric current is restored to initial current, capacity can not be restored to initial value
(Adv.Mater.,2014, 26,964-969)。
(2) Shandong University Yang Jian teaches research group and uses solvent-thermal method, using the intermediate in reaction process as mould
Plate prepares the hollow MoS that nanometer sheet is assembled into2Nano particle.Electrochemical property test shows: in 100mA g-1Electric current it is close
After lower circulation 80 times of degree, electrode shows 902mAh g-1Reversible capacity;In 1000mA g-1High current density under, electrode
780mAh g can still be shown-1Reversible capacity (ACS Appl.Mater.Interfaces, 2013,5,1003-
1008).But the preparation process technological parameter controllability is poor.
(3) Zhejiang University Chen Weixiang teaches research group and uses liquid phase method, assists synthesizing using L-cysteine
Flaky molybdenum disulfide/graphene composite nano material, then under certain atmosphere, 800 DEG C of annealing 2h obtain final sample.It will
A series of molybdenum disulfide/graphene composite nano material of obtained different ratios is carried out as the negative electrode material of lithium ion battery
Performance test, as a result, it has been found that first discharge specific capacity highest is close in electric current when the ratio of molybdenum disulfide and graphene is 1:2
Degree is 100mA g-1When, reach 1571mAh g-1, and after 100 circulations, specific discharge capacity is still up to 1187mAh g-1
(ACS Nano,2011,6, 4720-4728).But the preparation process complex process, energy consumption is high.
At present for lithium ion battery negative material MoS2Research to be concentrated mainly on nanosizing, Composite and design special
Different pattern.Prepare the pure MoS of nanoscale2Material, due to volume change biggish in charge and discharge process and poor electronics
Conductance, and nano material is easy so that activity MoS2Reunite in charge and discharge process, cyclical stability and high rate performance
It still needs further improvement;Prepare the MoS of special appearance2Organic formwork or organic surface active agent, preparation process are used mostly
Complexity, low yield;It prepares compound and mostly uses solvent-thermal method, surface cladding process, but such preparation method complex technical process, it is multiple
Between polymer component together by physisorption, binding force is weaker.
Summary of the invention
The purpose of the present invention is to provide a kind of MoS2Nanoneedle/carbon nanotube composite negative pole material preparation method.
The present invention provides a kind of MoS2Nanoneedle/carbon nanotube composite negative pole material preparation method, it is characterized in that adopting
Be grown on carbon nanotube matrix in a manner of extension with nanoscale is prepared with a step chemical vapour deposition technique
MoS2, specific process step are as follows:
(1) molybdenum source of certain molar weight, sulphur source and carbon nanotube are uniformly mixed in protective atmosphere, it will be mixed
Powder afterwards is placed in sealing device;Wherein, wherein the amount of molybdenum source substance is controlled in 3 × 10-4~1 × 10-2Mol, sulphur source object
The amount of matter is controlled 2 × 10- 3~1 × 10- 1The amount of mol, carbon nanotube material are controlled 5 × 10-4~4 × 10-3mol;
(2) protective gas that certain flow is passed through in tube furnace will be installed on obtained in step (1), in certain temperature
Lower heat treatment certain time.Wherein, gas flow control is controlled in 10~100sccm, heat treatment time in 1~8h;
Wherein protective atmosphere described in step (1) is high-purity argon gas or high pure nitrogen;The molybdenum source is molybdenum oxide, molybdenum
Sour ammonium or phosphomolybdic acid;The sulphur source is sulphur powder, thiocarbamide, thioacetamide or carbon disulfide;The sealing device is stainless
Steel seal pipe or quartz glass seals pipe;
Temperature in step (2) is that protective gas is high-purity argon gas or high pure nitrogen;The certain temperature, refers to heat
The temperature of processing is 600~900 DEG C.
The invention discloses a kind of MoS2Nanoneedle is epitaxially grown in the preparation method of carbon nanotube composite negative pole material.It is logical
It crosses using chemical vapour deposition technique, prepares MoS2Nanoneedle/carbon nano tube compound material.MoS2With carbon nanotube in interface
Coherence combines, and improves the bond strength of the two, guarantees that active material configuration is stablized in charge and discharge process, and accelerate electrochemical reaction
The transmission of electronics in the process;MoS2Nanoneedle prevents nano active substance in charge and discharge process in being uniformly distributed for carbon nanotube
Reunite;Flexible carrier carbon nanotube can alleviate volume change of the active material in charge and discharge process, ensure electrode knot
Structure stability.Final MoS2Nanoneedle/carbon nano tube compound material shows stable cycle performance and excellent high rate performance.
The advantage of the invention is that the preparation process of composite material is simple, yield is big, is suitble to large-scale industrial production.This
The MoS of method preparation2Nanoneedle/carbon nano tube compound material has stable cycle performance and excellent high rate performance, is one
The ideal lithium ion battery negative material of kind, can be widely applied to portable electronic device, electric car and aerospace etc.
Field.
Detailed description of the invention
Fig. 1 is the MoS of embodiment 12Nanoneedle/carbon nano tube compound material field emission scanning electron microscope figure.
Fig. 2 is the MoS of embodiment 12Nanoneedle/carbon nano tube compound material transmission electron microscope picture.
Fig. 3 is the MoS of embodiment 12Nanoneedle/carbon nano tube compound material cycle performance figure.
Fig. 4 is the MoS of embodiment 12Nanoneedle/carbon nano tube compound material high rate performance figure.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, but is not limited to protection scope of the present invention:
Embodiment 1:
The molybdenum trioxide of 0.1g, the thiocarbamide of 0.5g and the carbon nanotube of 0.012g are uniformly mixed in an ar atmosphere, it will
Powder after mixing is placed in stainless steel seal pipe.Stainless steel seal pipe obtained above is placed in tube furnace and is passed through air-flow
Amount is that the Ar gas of 10sccm finally obtains MoS in 600 DEG C of heat treatment 8h2Nanoneedle/carbon nano tube compound material.
By the MoS of 75wt.% obtained2Nanoneedle/carbon nano tube compound material, the acetylene black of 15wt.% and
The sodium carboxymethylcellulose of 15wt.% is uniformly mixed, and slurry is made, is coated uniformly on copper foil, circle is stamped into after vacuum drying
Shape electrode plates are to electrode, 1mol L with lithium metal-1LiPF6/ EC+DEC+DMC (volume ratio 1:1:1) is electrolyte,
Celgard 2400 is diaphragm, is assembled into button cell.Constant current charge-discharge test is carried out to battery, charging/discharging voltage range is
0.01~3.0V, the results showed that, with preferable chemical property: 0.1A g-1Current density under, circulation 20 times after it is compound
Material has up to 1030mAh g-1Reversible specific capacity;Even if in 2A g-1High current density under, composite material still table
Reveal 750mAh g-1Reversible specific capacity, high rate performance is excellent.
Embodiment 2:
The phosphomolybdic acid of 0.4g, the sulphur powder of 0.55g and the carbon nanotube of 0.024g are uniformly mixed in an ar atmosphere, it will
Powder after mixing is placed in quartz glass seals pipe.Quartz glass seals pipe obtained above is placed in tube furnace and is passed through
Throughput is the N of 40sccm2Gas finally obtains MoS in 800 DEG C of heat treatment 3h2Nanoneedle/carbon nano tube compound material.
By the MoS of 75wt.% obtained2Nanoneedle/carbon nano tube compound material, the acetylene black of 15wt.% and
The sodium carboxymethylcellulose of 15wt.% is uniformly mixed, and slurry is made, is coated uniformly on copper foil, circle is stamped into after vacuum drying
Shape electrode plates are to electrode, 1mol L with lithium metal-1LiPF6/ EC+DEC+DMC (volume ratio 1:1:1) is electrolyte,
Celgard 2400 is diaphragm, is assembled into button cell.Constant current charge-discharge test is carried out to battery, charging/discharging voltage range is
0.01~3.0V, the results showed that, with preferable chemical property: 0.1A g-1Current density under, circulation 20 times after it is compound
Material has up to 870mAh g-1Reversible specific capacity;Even if in 2A g-1High current density under, composite material still shows
640mAh g out-1Reversible specific capacity, high rate performance is excellent.
Embodiment 3:
In N2By the ammonium molybdate of 0.1g in atmosphere, the carbon nanotube mixing of the thioacetamide and 0.018g of 0.3g is equal
It is even, the powder after mixing is placed in stainless steel seal pipe.Stainless steel seal pipe obtained above is placed in tube furnace and is led to
Enter the N that throughput is 80sccm2Gas finally obtains MoS in 700 DEG C of heat treatment 5h2Nanoneedle/carbon nano tube compound material.
By the MoS of 75wt.% obtained2Nanoneedle/carbon nano tube compound material, the acetylene black of 15wt.% and
The sodium carboxymethylcellulose of 15wt.% is uniformly mixed, and slurry is made, is coated uniformly on copper foil, circle is stamped into after vacuum drying
Shape electrode plates are to electrode, 1mol L with lithium metal- 1LiPF6/ EC+DEC+DMC (volume ratio 1:1:1) is electrolyte,
Celgard 2400 is diaphragm, is assembled into button cell.Constant current charge-discharge test is carried out to battery, charging/discharging voltage range is
0.01~3.0V, the results showed that, with preferable chemical property: 0.1A g-1Current density under, circulation 20 times after it is compound
Material has up to 950mAh g-1Reversible specific capacity;Even if in 2A g-1High current density under, composite material still shows
700mAh g out-1Reversible specific capacity, high rate performance is excellent.
Claims (5)
1. a kind of MoS2Nanoneedle/carbon nanotube composite negative pole material preparation method, it is characterized in that using a step chemical vapor deposition
Area method is prepared with nanoscale and the MoS that is epitaxially grown on carbon nanotube matrix2Nanoneedle, specific process step are as follows:
(1) molybdenum source of certain molar weight, sulphur source and carbon nanotube are uniformly mixed in protective atmosphere, after mixing
Powder is placed in sealing device;Wherein, the amount of molybdenum source substance is controlled 3 × 10-4~1 × 10-2Mol, the amount control of sulphur source substance
2 × 10-3~1 × 10-1The amount of mol, carbon nanotube material are controlled 5 × 10-4~4 × 10-3mol;
(2) sealing device described in step (1) is passed through to the protective gas of certain flow in tube furnace, in certain temperature
Lower heat treatment certain time;Wherein, gas flow control is controlled in 10~100sccm, heat treatment time in 1~8h;
Protective atmosphere described in step (1) is high-purity argon gas or high pure nitrogen;
Sealing device described in step (1) is stainless steel seal pipe or quartz glass seals pipe.
2. MoS according to claim 12Nanoneedle/carbon nanotube composite negative pole material preparation method, it is characterised in that:
Molybdenum source described in step (1) is molybdenum oxide, ammonium molybdate or phosphomolybdic acid.
3. MoS according to claim 12Nanoneedle/carbon nanotube composite negative pole material preparation method, it is characterised in that:
Sulphur source described in step (1) is sulphur powder, thiocarbamide, thioacetamide or carbon disulfide.
4. MoS according to claim 12Nanoneedle/carbon nanotube composite negative pole material preparation method, it is characterised in that:
Protective gas in step (2) is high-purity argon gas or high pure nitrogen.
5. MoS according to claim 12Nanoneedle/carbon nanotube composite negative pole material preparation method, it is characterised in that:
Certain temperature described in step (2) refers to that the temperature of heat treatment is 600~900 DEG C.
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CN107934939A (en) * | 2017-11-14 | 2018-04-20 | 中山大学 | A kind of controllable MoS of the number of plies2The preparation method of/carbon nano tube compound material |
CN107892330B (en) * | 2017-12-01 | 2019-06-25 | 东华大学 | A kind of preparation method of piece heap molybdenum disulfide nano tube |
CN109904408B (en) * | 2019-01-09 | 2021-01-01 | 哈尔滨工业大学(深圳) | MoS2Preparation method and application of composite material with nanosheet embedded in carbon substrate |
CN110380028B (en) * | 2019-07-08 | 2022-09-09 | 武汉理工大学 | CNT/MoS 2 Lithium ion battery cathode material and preparation method thereof |
GB2615511A (en) * | 2021-12-07 | 2023-08-16 | Oxlid Ltd | Electrochemical cell |
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