CN104319371B - A kind of preparation method of lithium ion battery SnS2/CNTs/PPy composite negative pole material - Google Patents
A kind of preparation method of lithium ion battery SnS2/CNTs/PPy composite negative pole material Download PDFInfo
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- CN104319371B CN104319371B CN201410618533.6A CN201410618533A CN104319371B CN 104319371 B CN104319371 B CN 104319371B CN 201410618533 A CN201410618533 A CN 201410618533A CN 104319371 B CN104319371 B CN 104319371B
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A kind of lithium ion battery SnS2The preparation method of/CNTs/PPy composite negative pole material comprises the steps: step 1: by SnCl4·5H2O and thioacetamide join in polyglycol solution, stir；Step 2: CNT is joined above-mentioned solution, and ultrasonic wave dispersion 60min；Step 3: solution step 2 obtained proceeds in the automatic reactor of polytetrafluoroethylene (PTFE), cools down with stove after isothermal holding；Step 4: solution centrifugal step 3 obtained separates, with deionized water and absolute ethanol washing, vacuum drying；Step 5: the SnS that step 4 is obtained2/ CNTs composite is dissolved in deionized water, stirs, and adds lauryl sodium sulfate, adds pyrrole monomer and oxidant, is stirred at room temperature reaction 4h；Step 6: solution centrifugal step 5 obtained separates, with deionized water and absolute ethanol washing, vacuum drying.Negative material capacity that the present invention obtains is high and good cycle, at field tool potential application foregrounds such as portable electric appts, electric automobile and Aero-Space.
Description
Technical field
The present invention relates to lithium ion battery negative material field, be specifically related to a kind of lithium ion battery SnS2The preparation method of/CNTs/PPy composite negative pole material.SnS2I.e. stannic disulfide, CNTs i.e. CNT (Carbon nanotubes), PPy i.e. polypyrrole.
Background technology
Along with microelectric technique and the development of new-energy automobile, power supply proposing the highest requirement, lithium ion battery becomes focus of concern by plurality of advantages such as charge efficiency height and energy density are high.Lithium ion battery is mainly made up of positive pole, negative pole, barrier film, electrolyte.Wherein, negative material, primarily as the main body of storage lithium, realizes embedding and the abjection of lithium ion in charge and discharge process, is the key component of whole battery.Commercial Li-ion battery negative pole mainly uses various material with carbon element at present, the specific capacity of graphite-based carbon negative material the most closely its theoretical capacity (372mAh/g), become the bottleneck limiting lithium battery capacity, the space making its capacity of raising is very limited, and it is urgent and necessary for finding a kind of novel secondary lithium ion battery negative material that can substitute graphite-based carbon negative material, that have more high power capacity and security.
As the negative material of a kind of high power capacity, SnS2The most also having attracted the extensive concern of field of lithium ion battery it is considered to be one of most potential negative material, its theoretical capacity is up to 645mAh g-1.There are six side CdI2The SnS of the layer structure of type2More active sites can be provided to accommodate lithium ion, and allow lithium ion to be inserted into Van der Waals gap.Thus, the material of this stratiform can minimize the Volume Changes of charge and discharge process, and the transmission for lithium ion provides convenient.But, SnS2There is Volume Changes (200%) huge in charge and discharge process and the problem of conductance rate variance as negative material, thus cause the internal resistance of electrode to increase suddenly, capacity rapid decrease, cycle performance is deteriorated.
In order to suppress huge Volume Changes huge, effective method is that the pattern of material is controlled the nano material for porous.China Patent No. CN101950804 of China Patent No. CN101609884 of Chinese patent CN 101609887, the Wu Feng etc. of Li Hui etc. and Mu Daobin etc. uses different Sn sources and method to synthesize the SnS of different shape2, improve SnS to a certain extent2Cycle performance.
For SnS2The problem of conductance rate variance, the method that main thinking and various conductive carbon materials carry out being combined.China Patent No. CN102412394 of Du Ning etc. has synthesized stratiform SnS2/SiO2Core-shell nanometer rod negative material；Huang Ying etc. China Patent No. CN103094562 use water heat transfer artificial gold/rare earth metal negative material；China Patent No. CN102142540 of Chen Weixiang has synthesized Graphene/SnS2The lithium ion cell electrode of composite nano materials；China Patent No. CN102522543 that Caoization waits by force has synthesized SnS2/ graphene composite negative pole nano-complex.
Make a general survey of domestic and international patent and publish knowable to scientific paper, current various SnS2The research of base negative pole is that comparison is positive, active, gets a good chance of becoming a new generation's cathode material for high capacity lithium ion battery.The above-mentioned various SnS related to2The synthesis of base lithium cell cathode material, but be all to suppress SnS from single direction2The Volume Changes that alloying/removal alloying process is huge, although cathode of lithium battery cycle performance can be improved, but increase rate is little.
Summary of the invention
The technical problem to be solved in the present invention is: lithium cell cathode material exists the problem that capacity is the highest and cycle performance is undesirable at present, proposes a kind of lithium ion battery SnS2The preparation method of/CNTs/PPy composite negative pole material, raising electrode cycle stability, and prepare the lithium ion battery negative material of high power capacity high stability, and then improve the overall performance of power lithium-ion battery.
In order to solve above-mentioned technical problem, the present invention proposes techniques below scheme: a kind of lithium ion battery SnS2The preparation method of/CNTs/PPy composite negative pole material, comprises the steps:
Step 1: by SnCl4·5H2O and thioacetamide (TAA) join in polyglycol solution, stir；
Step 2: a number of CNT is joined in above-mentioned solution, and ultrasonic wave dispersion 60min；
Step 3: solution step 2 obtained proceeds in the automatic reactor of polytetrafluoroethylene (PTFE), carries out isothermal holding, then cools down with stove；
Step 4: the solution that step 3 obtained uses the mode of centrifugation, respectively with deionized water and absolute ethanol washing 3 times, the product after separating is vacuum dried, and the buff powder obtained is SnS2/ CNTs composite；
Step 5: the SnS that step 4 is obtained2/ CNTs composite is dissolved in certain deionized water, after stirring, adds a number of lauryl sodium sulfate, is subsequently added a number of pyrrole monomer and a number of oxidant, and mixed solution is stirred at room temperature reaction 4h；
Step 6: the solution that step 5 obtained uses the mode of centrifugation, respectively with deionized water and absolute ethanol washing 3 times, the product after separating is vacuum dried, and the black powder obtained is lithium ion battery SnS2/ CNTs/PPy composite negative pole material.
Limiting further of technique scheme is: the SnCl that step 1 is selected4·5H2It is pure that O and TAA is analysis, and SnCl4·5H2The ratio of the amount of O and TAA material controls: SnCl4·5H2O:TAA=1:1.
Limiting further of technique scheme is: in step 2, and the quality adding CNTs is theoretical gained SnS2The 0.5%～10% of compound quality.
Limiting further of technique scheme is: in step 3, the condition of isothermal holding is as follows: holding temperature is 160 DEG C～200 DEG C, and temperature retention time is 14h～24h.
Limiting further of technique scheme is: in step 5, adds the quality of lauryl sodium sulfate by being taken SnS2The 0.1%-3% of/CNTs composite quality.
Limiting further of technique scheme is: the oxidant added in step 5 is FeCl3·6H2O, the amount of its material is 1:1 with the ratio of the amount of the material of pyrrole monomer.
Limiting further of technique scheme is: the vacuum drying condition described in step 6 is as follows: being dried in vacuum drying chamber, baking temperature controls at 60 DEG C～100 DEG C, and drying time controls at 6h～10h.
The present invention makes full use of 3D nano flower valvular structure SnS2High theoretical capacity and the feature of security, as storage lithium main body, introduce CNT, construct SnS2The three-dimensional structure of/CNT, utilizes the one-dimensional loose structure of CNT both to contribute to the embedding of lithium ion in charge and discharge process and moved out, the advantage that can construct again three-dimensional conductive network, prepares SnS2/ CNTs composite.Meanwhile, at SnS2Surface forms the clad of PPy, and the PPy of introducing is possible not only to improve electrical conductivity, it is also possible to suppress volumetric expansion further, synthesizes SnS2/ CNTs/PPy composite negative pole material, gives full play to SnS2, the cooperative effect of CNTs and PPy material, it is achieved have complementary advantages, to improve electrode cycle stability, and prepare the lithium ion battery negative material of high power capacity high stability, and then improve the overall performance of power lithium-ion battery.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the composite negative pole material of embodiment 1.
Fig. 2 is the circulation volume figure of the composite negative pole material of embodiment 1.
Detailed description of the invention
The present invention proposes a kind of lithium ion battery SnS2The preparation method of/CNTs/PPy composite negative pole material, wherein, SnS2I.e. stannic disulfide, CNTs i.e. CNT (Carbon nanotubes), PPy i.e. polypyrrole, this preparation method comprises the steps:
Step 1: by SnCl4·5H2O and thioacetamide (TAA) join in polyglycol solution, stir；
In step 1, the SnCl of selection4·5H2It is pure that O and TAA is analysis, and SnCl4·5H2The ratio of the amount of O and TAA material controls: SnCl4·5H2O:TAA=1:1；
Step 2: a number of CNT (CNTs) is joined in above-mentioned solution, and ultrasonic wave dispersion 60min；
In step 2, the quality adding CNTs is theoretical gained SnS2The 0.5%～10% of compound quality；
Step 3: solution step 2 obtained proceeds in the automatic reactor of polytetrafluoroethylene (PTFE), carries out isothermal holding, then cools down with stove；
In step 3, the condition of isothermal holding is as follows: holding temperature is 160 DEG C～200 DEG C, and temperature retention time is 14h～24h；
Step 4: the solution that step 3 obtained uses the mode of centrifugation, respectively with deionized water and absolute ethanol washing 3 times, the product after separating is vacuum dried, and the buff powder obtained is SnS2/ CNTs composite；
Step 5: the SnS that step 4 is obtained2/ CNTs composite is dissolved in certain deionized water, after stirring, adds a number of lauryl sodium sulfate, is subsequently added a number of pyrrole monomer and a number of oxidant, and mixed solution is stirred at room temperature reaction 4h；
In step 5, add the quality of lauryl sodium sulfate by being taken SnS2The 0.1%-3% of/CNTs composite quality, the oxidant of addition is FeCl3·6H2O, the amount of the material of the oxidant of addition is 1:1 with the ratio of the amount of the material of pyrrole monomer；
Step 6: the solution that step 5 obtained uses the mode of centrifugation, respectively with deionized water and absolute ethanol washing 3 times, the product after separating is vacuum dried, and the black powder obtained is SnS2/ CNTs/PPy composite negative pole material.
In step 6, described vacuum drying condition is as follows: being dried in vacuum drying chamber, baking temperature controls at 60 DEG C～100 DEG C, and drying time controls at 6h～10h.
Embodiment 1
Take 1.42g SnCl4·5H2The thioacetamide (TAA) of O and 0.60g passes through stirring and dissolving in 100ml polyethylene glycol (PEG 400).After TAA dissolves, 0.0070g CNT is dispersed in solution, ultrasonic wave dispersion 60min.Finally, above-mentioned solution is proceeded in the automatic reactor of polytetrafluoroethylene (PTFE), in 180 DEG C of baking ovens, heat 18h.Product deionized water and ethanol after cooling wash 3 times respectively, are vacuum dried 24h in 80 DEG C, i.e. obtain light yellow SnS2/ CNTs composite.
By above-mentioned SnS2/ CNTs composite is dissolved in 40ml deionized water, stirs 30min, after adding 8mg lauryl sodium sulfate stirring 30min, is sequentially added into pyrrole monomer and the 0.40gFeCl of 104 μ L3·6H2O, mixed solution is stirred at room temperature reaction 4h.The solution that obtains uses the mode of centrifugation, and respectively with deionized water and absolute ethanol washing 3 times, the product after separating is vacuum dried, and vacuum drying condition is 8h at 80 DEG C, and the black powder obtained is SnS2/ CNTs/PPy composite negative pole material.
The composite negative pole material obtained is carried out electrochemical property test, and result shows, at 100mA g-1Current density under, composite first charge-discharge capacity is respectively 626mAh g-1With 1200mAh g-1, first charge-discharge efficiency is 52%, and after 30 circulations, reversible capacity still can maintain 420mAh g-1, capability retention is 67%, and coulombic efficiency, close to 100%, has preferable chemical property.
Embodiment 2
The present embodiment difference from Example 1 is: described addition carbon nanotube mass is 0.0035g, 14h at heat-retaining condition is 180 DEG C in automatic reactor, and the quality adding lauryl sodium sulfate is 24mg, and the amount of pyrrole monomer is 82 μ L, adds FeCl3·6H2O mass is 0.32g, and it is 6h at 100 DEG C that product carries out vacuum drying condition.Other is the most same as in Example 1.
Composite negative pole material constant current charge-discharge test described in the present embodiment shows, chemical property is held essentially constant, and discharge capacity is 1184mAh g first-1, after circulating 30 times, reversible capacity can maintain 410mAh g-1。
Embodiment 3
The present embodiment difference from Example 1 is: described addition carbon nanotube mass is 0.0350g, 20h at heat-retaining condition is 160 DEG C in automatic reactor, and the quality adding lauryl sodium sulfate is 8mg, and the amount of pyrrole monomer is 109 μ L, adds FeCl3·6H2O mass is 0.42g, and it is 10h at 80 DEG C that product carries out vacuum drying condition.Other is the most same as in Example 1.
Composite negative pole material constant current charge-discharge test described in the present embodiment shows, chemical property is held essentially constant, and discharge capacity is 1250mAh g first-1, after circulating 30 times, reversible capacity can maintain 455mAh g-1。
Embodiment 4
The present embodiment difference from Example 1 is: described addition carbon nanotube mass is 0.0700g, 14h at heat-retaining condition is 200 DEG C in automatic reactor, and the quality adding lauryl sodium sulfate is 0.8mg, and the amount of pyrrole monomer is 137 μ L, adds FeCl3·6H2O mass is 0.53g, and it is 6h at 100 DEG C that product carries out vacuum drying condition.Other is the most same as in Example 1.
Composite negative pole material constant current charge-discharge test described in the present embodiment shows, chemical property is held essentially constant, and discharge capacity is 1258mAh g first-1, after circulating 30 times, reversible capacity can maintain 425mAh g-1。
Claims (7)
1. a lithium ion battery SnS2The preparation method of/CNTs/PPy composite negative pole material, it is characterised in that include as follows
Step:
Step 1: by SnCl4·5H2O and thioacetamide join in polyglycol solution, stir；
Step 2: a number of CNT is joined in above-mentioned solution, and ultrasonic wave dispersion 60min；
Step 3: solution step 2 obtained proceeds to, in the automatic reactor of polytetrafluoroethylene (PTFE), carry out isothermal holding, then
Cool down with stove；
Step 4: solution step 3 obtained uses the mode of centrifugation, respectively with deionized water and absolute ethanol washing 3
Secondary, the product after separating is vacuum dried, and the buff powder obtained is SnS2/ CNTs composite；
Step 5: the SnS that step 4 is obtained2/ CNTs composite is dissolved in certain deionized water, after stirring, adds
A number of lauryl sodium sulfate, is subsequently added a number of pyrrole monomer and a number of oxidant, mixes molten
Liquid is stirred at room temperature reaction 4h；
Step 6: solution step 5 obtained uses the mode of centrifugation, respectively with deionized water and absolute ethanol washing 3
Secondary, the product after separating is vacuum dried, and the black powder obtained is lithium ion battery SnS2/ CNTs/PPy is multiple
Close negative material.
A kind of lithium ion battery SnS the most according to claim 12The preparation method of/CNTs/PPy composite negative pole material, its
It is characterised by: the SnCl that step 1 is selected4·5H2It is pure that O and TAA is analysis, and SnCl4·5H2The ratio of the amount of O and TAA material
Control: SnCl4·5H2O:TAA=1:1.
A kind of lithium ion battery SnS the most according to claim 12The preparation method of/CNTs/PPy composite negative pole material, its
Being characterised by: in step 2, the quality adding CNTs is theoretical gained SnS2The 0.5%～10% of compound quality.
A kind of lithium ion battery SnS the most according to claim 12The preparation method of/CNTs/PPy composite negative pole material, its
Being characterised by: in step 3, the condition of isothermal holding is as follows: holding temperature is 160 DEG C～200 DEG C, and temperature retention time is 14h～24h.
A kind of lithium ion battery SnS the most according to claim 12The preparation method of/CNTs/PPy composite negative pole material, its
It is characterised by: in step 5, adds the quality of lauryl sodium sulfate by being taken SnS2/ CNTs composite quality
0.1%-3%.
A kind of lithium ion battery SnS the most according to claim 12The preparation method of/CNTs/PPy composite negative pole material, its
It is characterised by: the oxidant added in step 5 is FeCl3·6H2O, the amount of its material with the ratio of the amount of the material of pyrrole monomer is
1:1。
A kind of lithium ion battery SnS the most according to claim 12The preparation method of/CNTs/PPy composite negative pole material, its
It is characterised by: the vacuum drying condition described in step 6 is as follows: being dried in vacuum drying chamber, baking temperature controls 60
DEG C～100 DEG C, drying time controls at 6h～10h.
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| CN105185989B (en) * | 2015-08-07 | 2017-08-25 | 中南大学 | A kind of sodium-ion battery conducting polymer/SnSexNano flower anode material and preparation method thereof |
| CN105964276B (en) * | 2016-05-05 | 2019-04-12 | 国家纳米科学中心 | The SnS of carbon quantum dot load2Nanometer sheet, preparation method and application |
| CN106058198A (en) * | 2016-07-26 | 2016-10-26 | 陕西科技大学 | Method for preparing SnS2/CNTs (carbon nano-tubes) cathode materials for sodium-ion batteries in in-situ manner |
| CN106099064B (en) * | 2016-08-03 | 2019-12-06 | 常州大学 | Preparation method of SnS2/CNTs composite nano material and application of composite nano material as negative electrode material of sodium-ion battery |
| CN106129385B (en) * | 2016-09-09 | 2018-08-24 | 深圳职业技术学院 | A kind of lithium ion battery CA/Fe2O3The preparation method of/PPy composite negative pole materials |
| CN106848254B (en) * | 2017-03-20 | 2020-09-01 | 上海中聚佳华电池科技有限公司 | Sodium-ion battery negative electrode material, preparation method thereof and sodium-ion battery |
| CN107026265B (en) * | 2017-06-05 | 2019-05-17 | 深圳职业技术学院 | A kind of lithium ion battery SnS2The preparation method of/SnSb composite negative pole material |
| CN107394129A (en) * | 2017-06-20 | 2017-11-24 | 陕西科技大学 | A kind of preparation method of stannic disulfide carbon nano-tube combination electrode material |
| CN107742718B (en) * | 2017-10-18 | 2020-02-14 | 安徽工业大学 | Preparation method of sodium lithium titanate negative electrode material with multilevel structure |
| CN107732206B (en) * | 2017-10-18 | 2020-06-30 | 安徽工业大学 | Preparation method of bimetallic oxide composite negative electrode material with multilevel structure |
| CN110071279A (en) * | 2019-05-08 | 2019-07-30 | 陕西科技大学 | A kind of SnS2/ CNTs@rGO composite construction, preparation method and application |
| CN110844933B (en) * | 2019-11-29 | 2022-02-11 | 河北省科学院能源研究所 | Preparation method of stannous sulfide composite negative electrode material |
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| CN101609885B (en) * | 2009-07-20 | 2011-04-27 | 北京理工大学 | Method for improving chemical property of negative pole material SnS2 of lithium ion battery |
| JP2012012263A (en) * | 2010-07-02 | 2012-01-19 | Kansai Electric Power Co Inc:The | Core-shell structure useful as negative electrode active material for lithium secondary battery and method for producing the same |
| CN103915625B (en) * | 2014-04-09 | 2016-02-10 | 暨南大学 | A kind of preparation method of spherical artificial gold of nano bar-shape composition and application |
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