CN105470459B - A kind of silicon-carbon composite cathode material and preparation method thereof - Google Patents
A kind of silicon-carbon composite cathode material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of silicon-carbon composite anode material for lithium ion battery and preparation method thereof.This method reduces silicon compound using sodium naphthalene solution in room temperature, obtains well dispersed silicon grain, then the macromolecule organic material containing reactive hydrogen atom is added in the reaction system so that the organic material is combined closely with silicon grain.Material is heat-treated afterwards, organic material is obtained the nano-silicon negative material that carbon closely coats through high temperature cabonization.
Description
Technical field
The present invention relates to a kind of silicon-carbon composite anode material for lithium ion battery and preparation method thereof, belong to lithium ion battery
Material Field.
Background technology
As fossil fuel continues to use so as to cause to peter out and caused by it the problems such as global warming, new energy
Industry is gradually subject to numerous researchers to pay close attention to.In numerous new technologies, lithium ion battery has a high-energy-density, low self-discharge and
The advantages that environmentally protective, thus the battery of digital product and electric automobile is widely used in, it is the research hotspot of new energy field.
At this stage, lithium ion battery negative material is mainly graphite series material, lithium titanate and other carbon materials.Stone
Ink is most widely used lithium ion battery negative material, it is derived from a wealth of sources, advantage of lower cost etc. with good cycle
Advantage, but its theoretical capacity is relatively low (372mAh/g), and from the raising for limiting lithium ion battery energy density；Although lithium titanate
With good cycle life, but its capacity is lower with respect to for graphite, greatly limit its application.So as product needs
Ask and further improve, finding the negative material of high-energy-density density becomes the common recognition of numerous researchers.
Silicon has very high theoretical capacity (4200mAh/g) as lithium ion battery negative material, is the reason for substituting graphite
Think material.But due to its volumetric expansion present in charge and discharge process, cause battery capacity decay quickly, cycle performance compared with
Difference.How on the premise of silicon materials capacity is kept the emphasis that its cycle performance is the investigation of materials is improved.The modification of silicon materials
Major way is that material is prepared into nano-scale particle, or by the filling of little particle silicon materials in the porous material or with other materials
Expect compound etc..
Patent CN 101244814A provide a kind of preparation method of Si-C composite material, by nano silica fume in this method
It is added in cold primer-oil, it is fully dispersed, ball-type native graphite is then added, and be sufficiently stirred and make dispersed, dry, carbon
Change.It is dispersed in by the technique nano-silicon in carbon, but nano silica fume can disperse not exclusively, to reunite, make in cold primer-oil
It into bulky grain, can not be evenly dispersed in cold primer-oil very much, cause in the material that subsequent treatment obtains nano silica fume in carbon
Exist in matrix still in the form of aggregate, to volumizing effect unobvious of the buffering silica flour in charge and discharge process.
103199252 A of patent CN disclose a kind of preparation method of the Si-C composite material containing oxygen silicon base.In the technique
The oxygen-containing silica-base material of nanoscale is mixed with graphite composite powder, it is dry, then this dried object and organic carbon source combination drying are obtained
The presoma of composite material, then carbonization crush.Obtained composite material is uniformly mixed with graphite composite powder again afterwards, obtains lithium
Ion battery silicon-carbon cathode material.Material is handled in this way and forms two buffer layer, can suppress silicon in charge and discharge process
Volumetric expansion, improve stable circulation performance.But the oxygen-containing silica-base material of nanoscale used in the material is generated in industry
Compare in generation and be difficult to realize, so as to can not possibly mass produce.
The method that 10318074 A of patent CN provide Si-C composite material.First by grinding silica flour system in this method
Standby silicon dispersion liquid, then adds carbon black, polyvinyl alcohol, graphite, stirs and form composite dispersion liquid.Spray drying, heat treatment.To heat
Product after processing adds pitch and carries out melting mechanical kneading, carries out high-temperature process afterwards.Although this method by multi-step at
Reason enables silica flour to be dispersed in as far as possible in the carbon as obtained by decomposing graphite and other carbon sources, but silica flour is worn into fine particle
Even nanoscale still has many difficulties, moreover silicon nature is more active, and in process of lapping, silicon is likely to and grinds
Grind solvent and certain reaction occurs, harmful effect is caused to final products performance.
Fine grinding is used for above-mentioned physical method, scattered obtained silica flour is extremely difficult to nanoscale on particle scale,
Real nano level silica flour is obtained, CVD is relatively effective means at this stage, but cost is excessive, it is difficult to is adopted by industrialization
With.Therefore, low cost synthesis nano silica fume is that silica-base material really is able to obtain large-scale application and the key of popularization.Patent
7214599 B2 of US provide a kind of method that nano silica fume is synthesized under temperate condition.The method is using sodium naphthalene solution in room temperature
Down just can be by SiCl4Elemental silicon is reduced into, this method raw material is easy to get, and cost is low, and obtained nano silica fume particle is in 10-
250nm or so, is evenly distributed.Then Yoojung Kwon etc. are added in the reaction system using this method synthesis nano silica fume
Tetrabutyl lithium, the Cl in silicon grain are reacted with tetrabutyl lithium so that the tetrabutyl can combine closely with silica flour.Then it is this material is high
Temperature processing, obtains carbon-coated nano silica-base material.Because silicon grain is nanoscale in the material, therefore the cycle life of material
And high rate performance is more satisfactory.But tetrabutyl lithium price is high, and activity is high, explosive, is not suitable for industry generation.
The shortcomings that in order to overcome above-mentioned existing nano-silicone wire/carbon material preparation technology, and since cost relation, material are general
Fine silica powder is all ground into by thick silicon.But this processing mode is difficult that micron order material is ground into required nanoscale material
Material, while in process of lapping, silica flour can inevitably occur necessarily to react with solvent, the final comprehensive performance for influencing material.At the same time
It is a problem all the time that how silica flour and other materials after grinding, which are uniformly dispersed,.Reunite and disperse inequality in the base and necessarily lead
Causing the cushion in design of material, the Volumetric expansion role in discharge and recharge reduces to silicon grain, therefore can not be fine
Ground solves the problems, such as that thus caused cycle performance declines.
The content of the invention
To solve the above-mentioned problems, the present invention provides a kind of preparation side of silicon-carbon composite cathode material of lithium ion battery
Method, comprises the following steps：
1) naphthalene is dissolved in organic solvent, then adds Na, stirred, form sodium naphthalene solution (blackish green)；
2) silicon-containing compound is added into the sodium naphthalene solution of above-mentioned preparation, makes silicon-containing compound reduce to obtain the outstanding of nano-silicon
Turbid (brown)；
3) high-molecular compound containing active hydrogen is added in the nano-silicon suspension of above-mentioned preparation, is removed after reaction
Organic solvent and naphthalene, it (is usually 2~10 small that then 400~1100 DEG C, which are heat-treated, under inert gas or hydrogen shield
When), finally the NaCl in the material after heat treatment is washed away, is dried to obtain the silicon-carbon composite cathode material of the present invention.
Another embodiment according to the present invention, the preparation method bag of above-mentioned silicon-carbon composite cathode material of lithium ion battery
Include following steps：
1) naphthalene is dissolved in organic solvent, then adds Na, stirred, form sodium naphthalene solution (blackish green)；
2) silicon-containing compound is added into the sodium naphthalene solution of above-mentioned preparation, makes silicon-containing compound reduce to obtain the outstanding of nano-silicon
Turbid (brown)；
3) high-molecular compound containing active hydrogen is added in the nano-silicon suspension of above-mentioned preparation, is removed after reaction
Organic solvent and naphthalene, then give birth to reaction after 400~900 DEG C of processing (when being usually 2~5 small) in inert gas or hydrogen
Into NaCl wash away, it is dry；
4) material prepared in step 3) is added into deionized water, and adds the organic molecule of 0~30wt%, carry out ball
Mill, is then spray-dried, and it (is usually 2~10 small that finally 400~1100 DEG C, which are heat-treated, under inert gas or hydrogen shield
When) obtain spherical silicon-carbon composite cathode material.
In the present invention, the organic solvent in the step 1) can be selected from glycol dimethyl ether and tetrahydrofuran.
In the present invention, the silicon-containing compound is SiCl4。
Above-mentioned steps 3) in, the high-molecular compound containing active hydrogen is added in nano-silicon brown suspension so that
Reactive hydrogen atom is reacted with the Cl on silicon nanoparticle, so that high-molecular compound is combined closely with silicon nanoparticle.
High-molecular compound of the present invention containing active hydrogen can be selected from phenolic resinoid, polyvinyl alcohol, polyethylene
At least one of polycarboxylic acid high-molecular compound such as butyral and polyacrylic acid, institute is hydrogeneous in such high-molecular compound
Atom can be reacted with the chlorine atom on silicon grain.
Above-mentioned steps 3) in, the high-molecular compound containing active hydrogen is added to the reaction time in nano-silicon suspension
For 1~10 it is small when, preferred reaction time for 3~5 it is small when.
Above-mentioned steps 3) and step 4) in, the inert gas is selected from least one of nitrogen, argon gas and helium.
Above-mentioned steps 3) or step 4) in, the temperature of the heat treatment is preferably 800~1000 DEG C；The heat treatment when
Between be preferably 3~5 it is small when.
In the step 4) of above-mentioned second of technical solution, the organic molecule is polyethyleneimine, polyethylene glycol or poly- carboxylic
The high-molecular compound of acids.
The present invention also provides a kind of silicon-carbon composite cathode material prepared using the above method.Wherein, silicon grain can be equal
It is dispersed in evenly in carbon base body.
The present invention also provides a kind of lithium rechargeable battery, includes silicon-carbon composite cathode material as described above.
In order to overcome defect existing in the prior art, the present invention provides a kind of silicon grain and is dispersed in carbon base body
Si-C composite material and preparation method thereof, and obtain following effect：
1) reduces SiCl using sodium naphthalene solution in room temperature4, well dispersed silicon grain is obtained, then will contain active hydrogen
The macromolecule organic material of atom is added in the reaction system, is carried out using the Cl atoms on reactive hydrogen atom and silicon grain anti-
Should so that the organic material is combined closely with silicon grain.Naphthalene in system is removed afterwards, material is heat-treated.So add
The organic material gone can be closely coated on obtained by reaction reduction around silicon nanoparticle through high temperature cabonization.
2) pattern more preferably materials in order to obtain, can be granulated using spray drying, to material after spray drying into
Row cladding, can further reduce material specific surface area, improve the performance of whole material.
Brief description of the drawings
Fig. 1：The circulation volume test chart of silicon-carbon composite cathode material prepared by embodiment 1；
Fig. 2：The circulation volume test chart of silicon-carbon composite cathode material prepared by embodiment 2；
Fig. 3：The SEM figures of silicon-carbon composite cathode material prepared by embodiment 2.
Embodiment
The present invention is described in detail in following specific embodiment, but the present invention is not restricted to following implementation
Example.
Embodiment 1：
95.232g naphthalenes are dissolved in 500ml glycol dimethyl ethers, 20.5356g sodium blocks is added, it is molten to be dissolved into green black
Liquid.It is stirred overnight, then by 30.35gSiCl4Be added in above-mentioned green dark solution, be vigorously stirred 4 it is small when.Then will dissolving
The ethylene glycol dimethyl ether solution of 25.29g polyvinyl butyrals is added in above-mentioned suspension, stirs 2h.Vacuum distillation, by second
Glycol dimethyl ether removes, and then adds hexamethylene and removes naphthalene.Obtain yellow-brown solid.By above-mentioned solid with the heating speed of 5min
Rate be raised to 800 DEG C insulation 5 it is small when, Temperature fall.Taking-up washes away the sodium chloride in product with distilled water, is dried to obtain final production
Product.
Embodiment 2：
95.232g naphthalenes are dissolved in 500ml glycol dimethyl ethers, 20.5356g sodium blocks is added, it is molten to be dissolved into green black
Liquid.Be stirred overnight, then 30.35gSiCl4 be added in above-mentioned green dark solution, be vigorously stirred 4 it is small when.Then will dissolving
The ethylene glycol dimethyl ether solution of 8.56g phenolic resin is added in above-mentioned suspension, stirs 2h.Vacuum distillation, by ethylene glycol
Dimethyl ether removes, and then adds hexamethylene and removes naphthalene.Obtain yellow-brown solid.By above-mentioned solid with the heating speed of 2 DEG C/min
Rate be raised to 450 DEG C insulation 5 it is small when, Temperature fall.Taking-up washes away the sodium chloride in product with distilled water, dry.Take the said goods
4.0g, and 0.4g polyethyleneimines are added in deionized water together, when planetary ball mill 1.5 is small, spray drying.By obtained material
Material is warming up to 900 DEG C, when insulation 3 is small with the speed of 5 DEG C/min in a nitrogen atmosphere, Temperature fall.The SEM of prepared material
Figure is shown in Fig. 3.
Button cell makes:Respectively activity is used as by the use of silicon-carbon composite cathode material of lithium ion battery prepared by Examples 1 and 2
Material, makes button cell, and making step is as follows：
1. dispensing and stirring：According to active material:Conductive agent:PVDF=8:1:1 ratio prepares slurry, and PVDF is used
The PVDF solution of 3% solid content, obtains thick paste slurry preferably after stirring；
2. slurry is coated on copper foil, pole piece is made；
3. pole piece dries drying, it is placed directly in air dry oven, when 120 DEG C of baking 3-4 are small, is then placed in vacuum drying
When case baking 8-14 is small；
4. assembled battery：It is anode with lithium piece, using polypropylene diaphragm, adds electrolyte, be assembled into button cell.
Tested using new prestige test cabinet, voltage range 0.01-2.0V, multiplying power evaluates the electrochemistry of material for 0.3C
Performance.The lithium ion battery test result that the material prepared respectively with Examples 1 and 2 makes is shown in Fig. 1 and Fig. 2.
Claims (8)
1. a kind of preparation method of silicon-carbon composite cathode material, comprises the following steps：
1) naphthalene is dissolved in organic solvent, then adds Na, stir sodium naphthalene solution；
2) silicon-containing compound is added into the sodium naphthalene solution of above-mentioned preparation, makes silicon-containing compound reduce to obtain the suspended of nano-silicon
Liquid；The silicon-containing compound is SiCl4；
3) high-molecular compound containing active hydrogen is added in the nano-silicon suspension of above-mentioned preparation, is removed after reaction organic
Solvent and naphthalene, then under inert gas or hydrogen shield 400~1100 DEG C be heat-treated, finally by the material after heat treatment
In NaCl wash away, be dried to obtain silicon-carbon composite cathode material；Above-mentioned steps 3) in, by the high-molecular compound containing active hydrogen
When the reaction time being added in nano-silicon suspension is 1~10 small；The high-molecular compound containing active hydrogen is selected from phenol
At least one of air aldehyde resin, polyvinyl alcohol, polyvinyl butyral resin and polyacrylic acid.
2. a kind of preparation method of silicon-carbon composite cathode material, comprises the following steps：
1) naphthalene is dissolved in organic solvent, then adds Na, stirred, form sodium naphthalene solution；
2) silicon-containing compound is added into the sodium naphthalene solution of above-mentioned preparation, makes silicon-containing compound reduce to obtain the suspended of nano-silicon
Liquid；The silicon-containing compound is SiCl4；
3) high-molecular compound containing active hydrogen is added in the nano-silicon suspension of above-mentioned preparation, is removed after reaction organic
Solvent and naphthalene, then wash away the NaCl for reacting generation after 400~900 DEG C of processing in inert gas or hydrogen, dry；Step
It is rapid 3) in, by the high-molecular compound containing active hydrogen be added to reaction time in nano-silicon suspension for 1~10 it is small when；
4) material prepared in step 3) is added into deionized water, and adds the organic molecule of 0~30wt%, carry out ball milling,
Then be spray-dried, finally under inert gas or hydrogen shield 400~1100 DEG C carry out being thermally treated resulting in silicon-carbon composite cathode
Material；
The high-molecular compound containing active hydrogen is selected from phenolic resinoid, polyvinyl alcohol, polyvinyl butyral resin and poly- third
At least one of olefin(e) acid.
3. the preparation method of silicon-carbon composite cathode material according to claim 1 or 2, it is characterised in that the step 1)
In organic solvent be selected from glycol dimethyl ether and tetrahydrofuran.
4. the preparation method of silicon-carbon composite cathode material according to claim 1 or 2, it is characterised in that the indifferent gas
Body is selected from least one of nitrogen, argon gas and helium.
5. the preparation method of silicon-carbon composite cathode material according to claim 1 or 2, it is characterised in that the heat treatment
Temperature be 800~1000 DEG C.
6. the preparation method of silicon-carbon composite cathode material according to claim 2, it is characterised in that the organic molecule is
The high-molecular compound of polyethyleneimine, polyethylene glycol or polycarboxylic acid.
A kind of 7. silicon-carbon Compound Negative prepared by preparation method of silicon-carbon composite cathode material according to claim 1 or 2
Pole material.
8. a kind of lithium rechargeable battery, includes silicon-carbon composite cathode material according to claim 7.
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| CN109546134A (en) * | 2018-12-11 | 2019-03-29 | 武汉大学 | The negative electrode material and sodium-ion battery a kind of sodium-ion battery cathode pre- sodium modification method and obtained |
| CN115159527B (en) * | 2022-05-16 | 2024-04-12 | 广东马车动力科技有限公司 | Hard carbon coated silicon nanoparticle composite microsphere negative electrode material and preparation method and application thereof |
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| CN102332571A (en) * | 2011-09-21 | 2012-01-25 | 广东达之邦新能源技术有限公司 | Silicon-carbon compound cathode material and manufacturing method thereof as well as lithium ion battery and cathode piece |
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| WO2003025260A1 (en) * | 2001-09-19 | 2003-03-27 | Evergreen Solar, Inc. | High yield method for preparing silicon nanocrystals with chemically accessible surfaces |
| CN102157731B (en) * | 2011-03-18 | 2015-03-04 | 上海交通大学 | Silicon and carbon compound anode material of lithium ion battery and preparation method of silicon and carbon compound anode material |
| US20120244436A1 (en) * | 2011-03-24 | 2012-09-27 | Leyden Energy, Inc. | Anodes of porous silicon particles |
| CN103682286B (en) * | 2013-12-18 | 2015-09-02 | 南京毕汉特威高分子材料有限公司 | Silicon/high molecular composite microsphere and silicon-carbon composite anode material for lithium ion battery and preparation method thereof |
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| CN102332571A (en) * | 2011-09-21 | 2012-01-25 | 广东达之邦新能源技术有限公司 | Silicon-carbon compound cathode material and manufacturing method thereof as well as lithium ion battery and cathode piece |
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| Title |
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| "Solution reduction synthesis of surface stabilized silicon nanoparticles";Richard K. Baldwin等;《ChemComm》;20020722;第1822-1823页 * |
| "Synthesis and electrochemical properties of lithium-electroactive surface-stabilized silicon quantum dots";Yoojung Kwon等;《Electrochimica Acta》;20070209;第52卷;第4663-4668页 * |
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Effective date of registration: 20230506 Address after: 1080 Greenwood Avenue, Lake Mary, Florida, USA Patentee after: Weihong Advanced Materials Co. Address before: 313000 No. 2198 Hongfeng Road, Huzhou Economic and Technological Development Zone, Zhejiang Province Patentee before: MICROVAST POWER SYSTEMS Co.,Ltd. |