CN108807960A - A kind of height ratio capacity lithium ion battery silicon cathode material preparation method - Google Patents
A kind of height ratio capacity lithium ion battery silicon cathode material preparation method Download PDFInfo
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- CN108807960A CN108807960A CN201810744970.0A CN201810744970A CN108807960A CN 108807960 A CN108807960 A CN 108807960A CN 201810744970 A CN201810744970 A CN 201810744970A CN 108807960 A CN108807960 A CN 108807960A
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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Abstract
The present invention provides a kind of height ratio capacity lithium ion battery silicon cathode material preparation methods, include the following steps：Step 1）The preparation of carbon nano tube compound material Ce-808/CNT, step 2）Stober methods synthesize nanosized SiO_2, step 3）Mg thermal reductions prepare nanoscale silica flour, step 4）Product processing：Reaction finishes, and removes reaction column；By the brown powder in reaction column down in a beaker, with spoon by its crushed into powder shape.Although the high side reaction of magnesiothermic reduction temperature is more in the present invention, impurity can be disposed by acid.The control of pattern can be carried out under high temperature, generates elemental silicon, has size uniform, the uniform feature of pore-size distribution, and good pattern contributes to performance boost, and it is accurate that structure imitates analysis result.
Description
Technical field
The invention belongs to the preparing technical fields of height ratio capacity lithium ion battery silicon cathode material, and in particular to a kind of high ratio
Capacity silicium cathode material preparation method.
Background technology
The energy is the material base that we depend on for existence and development.Traditional fossil fuel such as coal, oil and natural
The energy such as gas are faced with the problems such as reserves decline and high pollution, cannot be satisfied future society to efficient, cleaning, economy, safety
The requirement of energy system.So the exploitation of new energy and its technology is extremely urgent.Ion battery is managed as a new generation's " green two
Primary cell " has many advantages, such as that big open-circuit voltage height, energy density, long lifespan, pollution-free and self discharge are small, lithium ion battery quilt
It is considered optimal energy storage and the tool of conversion.
Currently, the positive electrode of commercial lithium ion battery mainstream mainly has LiCoO2And LiFePO4;Negative material is main
It is graphite, theoretical specific capacity is 372 mAh/g.The history for having more than 20 years with the use of upper electrode material, is assembled into full battery
Energy density be 120-200 Wh/Kg, by optimize battery preparation technique come improve battery performance be difficult to making a breakthrough property into
Exhibition.Therefore, the electrode material for exploring novel height ratio capacity has become the key of lithium ion battery development.Because of positive electrode can
Inverse specific capacity room for promotion is smaller, so the reversible specific capacity for promoting negative material at present is to improve lithium ion battery energy density
Key.Although commercialized graphite type material capacity is twice of existing positive electrode capacity, calculated by simulating, in cathode
In the case that material reversible capacity is no more than 1200 mAh/g, the capacity for improving existing negative material is close to the energy of entire battery
Degree still has larger contribution.
Silicon is a kind of environmentally friendly and widely distributed substance.Since its theoretical specific capacity is up to 4212 mAh/g
（Li22Si5）, decuple graphite（LiC6, 372 mAh/g）, therefore it is considered as most possible substitution lithium ion battery tradition
One of material of graphite cathode.However, the enormousness that the height ratio capacity of silicon is brought when but forming alloy along with same lithium changes
（About 300%）, this huge volume change can cause electrode is serious to burst apart and crush.So many researchers of industry taste
Many kinds of strategies have been tried, to evade deterioration of the silicium cathode material in charge and discharge cycles, such as reduced grain size, prepare activity/inertia
Composite material prepares silicon thin film, synthesizing one-dimensional silicon nanostructure, using other adhesives etc..In addition, industry is also to silicium cathode
Mechanism studied, understand that how lithium ion is in silicon from crystal structure, phase transformation, deformation, kinetics etc.
Electrochemical intercalation and abjection are carried out in the charge and discharge cycles of cathode.Although up to the present, close to the silicium cathode of theoretical capacity
The large-scale commercial production of material has not been achievable, but industry has been expected to develop and has been higher by 3 to 5 times than graphite in specific capacity
Silicium cathode material.
The failure of silicium cathode is largely because huge volume expansion during silicon embedding and removing and causes
Caused by Si particles are cracked and are ruptured.In order to reduce the volume expansion of silicium cathode, SiOx materials are developed, compared to
Pure Si materials, volume expansion are substantially reduced, and are a kind of silicium cathode materials of better performances with C composite, and at present
A kind of more silicon materials of practical application, but the material still has the problem of silicium cathode fails, research in actual use
It was found that failure has close relationship with Li+ insertion speed and Arrays Aluminum Films in Acid Solution, the more microstructure crucially with Si cathode.
SiO really described in us is not pure SiO but the compound of many oxide of Si and Si.In production
SiO is to utilize Si and SiO2Pyroreaction forms in a vacuum, but SiO is thermodynamically unstable, in 1000-1400
Disproportionated reaction can occur at DEG C, generate Si and Si2O3, STEM observations are it has also been found that heterogeneous in amorphous Si Ox be dispersed with
Amorphous nano Si.Additionally due to the effect of high temperature, Si is crystallized there is also some, therefore we actually use in SiOx
Si has the form of a variety of Si.Theoretical research finds that the embedding lithium dynamic characteristics of SiOx and Si materials simultaneously differ, and Li is embedded into
In SiOx, multiple compounds, such as Li can be formed2O, Li2Si2O5, Li2SiO3, Li4SiO4Deng, and this process is irreversible
, these lithium silicon compounds can become the buffer strip of Si negative electrode volume expansions, inhibit the volume expansion of silicium cathode, but this slow
Punching effect is limited, and the cycle performance of SiOx materials cannot be completely secured.
Invention content
In view of this, there is provided a kind of height ratio capacity lithium ion battery silicon cathode materials to prepare for the main object of the present invention
Method.
The technical solution adopted by the present invention is：
A kind of height ratio capacity silicium cathode material preparation method, includes the following steps：
Step 1）The preparation of carbon nano tube compound material Ce-808/CNT, specifically comprises the following steps：
1A:It is 1 to weigh molar ratio:Organic solvent n,N-Dimethylformamide and water is added in 1 trimesic acid and ammonium ceric nitrate
Mixed solvent, the two ratio be 5:1；
1B:Mixed solution is placed in the oil bath pan that temperature is 100 DEG C and is reacted 30 minutes, grey powder is obtained；
1C:Grey powder is washed with n,N-Dimethylformamide and absolute methanol respectively, and it is multiple that carbon nanotube is obtained after dry
Condensation material Ce-808/CNT；
Step 2）Stober methods synthesize nanosized SiO_2:
Ethyl alcohol, ammonium hydroxide are sequentially added into there-necked flask successively, deionized water after tepidarium water bath with thermostatic control, under mechanical stirring will
Ethyl orthosilicate is added drop-wise to dropwise in above-mentioned solution, product washed repeatedly with deionized water until filtrate be in neutrality, 80 DEG C of vacuum
Dry 24 h obtain nanoscale SiO2；
Step 3）Mg thermal reductions prepare nanoscale silica flour：
SiO2 powders and magnesium powder are pressed 3:5 ratio, which is respectively charged into, to be put into stainless steel reaction column, is had to during filling column
It keeps sample powder to lay upwards uniform, prevents from toppling, be marked in the upward side, by reaction column steel wire bundle
Good, high-temperature calcination can be carried out by being fixed, and stainless steel reaction column is placed in the pipe reaction stove of argon gas atmosphere protection, then
650 DEG C are warming up to the speed of 5 DEG C/min, reaction a period of time；
Step 4）Product processing：Reaction finishes, and removes reaction column；By the brown powder in reaction column down in a beaker,
With spoon by its crushed into powder shape.
In step 2, specially：
2A:Configure solution A：Concentrated ammonia liquor ethanol distillation water is mixed in a certain ratio, is placed in 100ml beakers, uses magnetic agitation
Device stirs evenly, rotating speed：1100rpm, the whirlpool estimated in beaker reach bottom；Concentrated ammonia liquor is volatile, and burning is sealed with plastic foil
Rim of a cup；
Configure B liquid：Ethyl orthosilicate and ethyl alcohol are placed in by a certain percentage in 100ml beakers, magnetic agitation is uniformly mixed about 1-2
Minute；
2B:B is rapidly added in A by ethyl orthosilicate with suction pipe absorption is a certain amount of, tries not that B solution contact walls of beaker is allowed to stir,
Solution becomes milky suspended things from water white transparency in beaker after stirring a period of time, can gradually become cloudy, use ParafilmTM
Beaker mouth, the reaction was continued at room temperature 2 hours；
2C:Nanometer grade silica white powder obtained；
Obtained solution is divided equally in four centrifuge tubes, centrifugation, rotating speed 7000/5min；
It is washed with ethyl alcohol, product deionized water and ethyl alcohol are washed repeatedly up to filtrate is in neutrality, and 80 DEG C of 24 h of vacuum drying are obtained
To nanoscale SiO2.
In step 4, further include removal of impurities processing, including
Gained powder is handled with concentrated hydrochloric acid：Powder is poured into the beaker equipped with 200ml water, the stirring of magneton blender is put into,
It is directly instilled wherein with the concentrated hydrochloric acid of 11.9mol/L simultaneously, in magnetic agitation in processing procedure until there is no bubble generation
It is stirred continuously on device；Magnetic agitation was by 24 hours always；Become coffee-like turbid solution；Then with 2 M HF and 25% HAC volumes
Than 1:9 70 DEG C of processing 2h of mixed acid；It is washed repeatedly with deionized water until filtrate is in neutrality, 80 DEG C of vacuum drying obtain pure
Porous nano grade silica flour.
Although the high side reaction of magnesiothermic reduction temperature is more in the present invention, impurity can be disposed by acid.It can be real under high temperature
The control of row pattern generates elemental silicon, has size uniform, the uniform feature of pore-size distribution, good pattern contributes to performance
It is promoted, structure imitates the accurate of analysis result.
Description of the drawings
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the SEM figures of porous silicon in the present invention；
Fig. 2 is the electrochemistry cycle schematic diagram that current density is porous Si under 0.5A/g in the present invention.
Specific implementation mode
Below in conjunction with attached drawing and specific embodiment, the present invention will be described in detail, herein illustrative examples of the invention
And explanation is used for explaining the present invention, but it is not as a limitation of the invention.
Magnesium reduction process control pattern prepares elementary silicon
Nano-silicon negative material is prepared by the method for magnesiothermic reduction, regulates and controls silicium cathode material by regulating and controlling the pattern of presoma
The nanostructure of material prepares the Si-C composite material with nanostructure in combination with carbon-coated method, in silicon material
On the basis of expecting high power capacity performance, the cycle performance of silicium cathode material is improved.In addition, originally having studied the nano material of complex topography
Controllable preparation, the silicium cathode material to prepare different nanostructures provides template, and this patent includes mainly following aspect:
In terms of thermodynamics and kinetics, the mechanism of magnesium reduction process is inquired into, is inquired into using nano silicon dioxide as raw material system
The feasibility of standby silicon nano material, it is desirable to by designing magnesiothermic reduction subtraction unit, regulate and control experiment parameter, obtain good silicon nanometer
Material.
This patent attempts by Stober legal system prepared silicon dioxide nanospheres, then as presoma, also by magnesium heat
Former method prepares the good silicon nanosphere of pattern, carries out carbon coating to material by high molecular material pyrolysismethod, while studying difference
Influence of the carbon coating amount for silicium cathode materials chemistry performance.
This patent is wished to be prepared the silica of hollow nanostructures using the iron oxide of different nanostructures as template, be led to
It crosses magnesium reduction process and prepares the nano-silicon negative material of different hollow structures, while studying hollow structure to silicon materials electrochemistry
The influence of energy.
Thus：The present invention provides a kind of height ratio capacity silicium cathode material preparation methods, include the following steps：
Step 1）The preparation of carbon nano tube compound material Ce-808/CNT, specifically comprises the following steps：
1A:It is 1 to weigh molar ratio:Organic solvent n,N-Dimethylformamide and water is added in 1 trimesic acid and ammonium ceric nitrate
Mixed solvent, the two ratio be 5:1；
1B:Mixed solution is placed in the oil bath pan that temperature is 100 DEG C and is reacted 30 minutes, grey powder is obtained；
1C:Grey powder is washed with n,N-Dimethylformamide and absolute methanol respectively, and it is multiple that carbon nanotube is obtained after dry
Condensation material Ce-808/CNT；
Step 2）Stober methods synthesize nanosized SiO_2:
Ethyl alcohol, ammonium hydroxide are sequentially added into there-necked flask successively, deionized water after tepidarium water bath with thermostatic control, under mechanical stirring will
Ethyl orthosilicate is added drop-wise to dropwise in above-mentioned solution, product washed repeatedly with deionized water until filtrate be in neutrality, 80 DEG C of vacuum
Dry 24 h obtain nanoscale SiO2；
Step 3）Mg thermal reductions prepare nanoscale silica flour：
By SiO2Powder and magnesium powder press 3:5 ratio, which is respectively charged into, to be put into stainless steel reaction column, is had to during filling column
It keeps sample powder to lay upwards uniform, prevents from toppling, be marked in the upward side, by reaction column steel wire bundle
Good, high-temperature calcination can be carried out by being fixed, and stainless steel reaction column is placed in the pipe reaction stove of argon gas atmosphere protection, then
650 DEG C are warming up to the speed of 5 DEG C/min, reaction a period of time；
Step 4）Product processing：Reaction finishes, and removes reaction column；By the brown powder in reaction column down in a beaker,
With spoon by its crushed into powder shape.
In step 2, specially：
2A:Configure solution A：Concentrated ammonia liquor ethanol distillation water is mixed in a certain ratio, is placed in 100ml beakers, uses magnetic agitation
Device stirs evenly, rotating speed：1100rpm, the whirlpool estimated in beaker reach bottom；Concentrated ammonia liquor is volatile, and burning is sealed with plastic foil
Rim of a cup；
Configure B liquid：Ethyl orthosilicate and ethyl alcohol are placed in by a certain percentage in 100ml beakers, magnetic agitation is uniformly mixed about 1-2
Minute；
2B:B is rapidly added in A by ethyl orthosilicate with suction pipe absorption is a certain amount of, tries not that B solution contact walls of beaker is allowed to stir,
Solution becomes milky suspended things from water white transparency in beaker after stirring a period of time, can gradually become cloudy, use ParafilmTM
Beaker mouth, the reaction was continued at room temperature 2 hours；
2C:Nanometer grade silica white powder obtained；
Obtained solution is divided equally in four centrifuge tubes, centrifugation, rotating speed 7000/5min；
It is washed with ethyl alcohol, product deionized water and ethyl alcohol are washed repeatedly up to filtrate is in neutrality, and 80 DEG C of 24 h of vacuum drying are obtained
To nanoscale SiO2。
In step 4, further include removal of impurities processing, including
Gained powder is handled with concentrated hydrochloric acid：Powder is poured into the beaker equipped with 200ml water, the stirring of magneton blender is put into,
It is directly instilled wherein with the concentrated hydrochloric acid of 11.9mol/L simultaneously, in magnetic agitation in processing procedure until there is no bubble generation
It is stirred continuously on device；Magnetic agitation was by 24 hours always；Become coffee-like turbid solution；Then with 2 M HF and 25% HAC volumes
Than 1:9 70 DEG C of processing 2h of mixed acid；It is washed repeatedly with deionized water until filtrate is in neutrality, 80 DEG C of vacuum drying obtain pure
Porous nano grade silica flour.
With reference to Fig. 2, the present invention also provides a kind of paintings of metal organic frame-carbon nano tube compound material (Ce-808/CNT)
Layer diaphragm is used for the electrochemical property test of lithium-sulfur cell：
Specific experiment step：Electrode for battery testing is by silicon, Si active materials（70wt%）, Super P carbon blacks
（10wt%）With sodium alginate adhesive（20wt%）It is made.The load capacity of active material is controlled in about 1mg/cm2.It weighs
Afterwards, using Si powder as working electrode and as the lithium piece to electrode, in the glove box full of argon gas（Mbraun,
Labstar）（<The H of 0.1ppm2O and<The O of 0.1ppm2）Middle assembling CR2032 type button cells.Electrolyte is in ethylene carbonate
（EC）And dimethyl carbonate（DMC）（1：1v / v）With 3% vinylene carbonate（VC）Mixture in 1M LiPF6In.?
CHI660D electrochemical workstations（CHI instruments）On recorded in 0.05 to 3.0V voltage range with the sweep speed of 0.1mV/s
Cyclic voltammetry（CV）It measures.Cycle performance test carries out under the current density of 0.5 A/g.
The technical solution disclosed in the embodiment of the present invention is described in detail above, specific implementation used herein
Example is expounded the principle and embodiment of the embodiment of the present invention, and the explanation of above example is only applicable to help to understand
The principle of the embodiment of the present invention；Meanwhile for those of ordinary skill in the art, embodiment, is being embodied according to the present invention
There will be changes in mode and application range, in conclusion the content of the present specification should not be construed as the limit to the present invention
System.
Claims (3)
1. a kind of height ratio capacity lithium ion battery silicon cathode material preparation method, which is characterized in that include the following steps：
Step 1）The preparation of carbon nano tube compound material Ce-808/CNT, specifically comprises the following steps：
1A:It is 1 to weigh molar ratio:Organic solvent n,N-Dimethylformamide and water is added in 1 trimesic acid and ammonium ceric nitrate
Mixed solvent, the two ratio be 5:1；
1B:Mixed solution is placed in the oil bath pan that temperature is 100 DEG C and is reacted 30 minutes, grey powder is obtained；
1C:Grey powder is washed with n,N-Dimethylformamide and absolute methanol respectively, and it is multiple that carbon nanotube is obtained after dry
Condensation material Ce-808/CNT；
Step 2）Stober methods synthesize nanosized SiO_2:
Ethyl alcohol, ammonium hydroxide are sequentially added into there-necked flask successively, deionized water after tepidarium water bath with thermostatic control, under mechanical stirring will
Ethyl orthosilicate is added drop-wise to dropwise in above-mentioned solution, product washed repeatedly with deionized water until filtrate be in neutrality, 80 DEG C of vacuum
Dry 24 h obtain nanoscale SiO2；
Step 3）Mg thermal reductions prepare nanoscale silica flour：
SiO2 powders and magnesium powder are pressed 3:5 ratio, which is respectively charged into, to be put into stainless steel reaction column, is had to during filling column
It keeps sample powder to lay upwards uniform, prevents from toppling, be marked in the upward side, by reaction column steel wire bundle
Good, high-temperature calcination can be carried out by being fixed, and stainless steel reaction column is placed in the pipe reaction stove of argon gas atmosphere protection, then
650 DEG C are warming up to the speed of 5 DEG C/min, reaction a period of time；
Step 4）Product processing：Reaction finishes, and removes reaction column；By the brown powder in reaction column down in a beaker,
With spoon by its crushed into powder shape.
2. height ratio capacity silicium cathode material preparation method according to claim 1, which is characterized in that in step 2, specifically
For：
2A:Configure solution A：Concentrated ammonia liquor ethanol distillation water is mixed in a certain ratio, is placed in 100ml beakers, uses magnetic agitation
Device stirs evenly, rotating speed：1100rpm, the whirlpool estimated in beaker reach bottom；Concentrated ammonia liquor is volatile, and burning is sealed with plastic foil
Rim of a cup；
Configure B liquid：Ethyl orthosilicate and ethyl alcohol are placed in by a certain percentage in 100ml beakers, magnetic agitation is uniformly mixed about 1-2
Minute；
2B:B is rapidly added in A by ethyl orthosilicate with suction pipe absorption is a certain amount of, tries not that B solution contact walls of beaker is allowed to stir,
Solution becomes milky suspended things from water white transparency in beaker after stirring a period of time, can gradually become cloudy, use ParafilmTM
Beaker mouth, the reaction was continued at room temperature 2 hours；
2C:Nanometer grade silica white powder obtained；
Obtained solution is divided equally in four centrifuge tubes, centrifugation, rotating speed 7000/5min；
It is washed with ethyl alcohol, product deionized water and ethyl alcohol are washed repeatedly up to filtrate is in neutrality, and 80 DEG C of 24 h of vacuum drying are obtained
To nanoscale SiO2.
3. height ratio capacity silicium cathode material preparation method according to claim 1, which is characterized in that in step 4, also wrap
Removal of impurities processing is included, including
Gained powder is handled with concentrated hydrochloric acid：Powder is poured into the beaker equipped with 200ml water, the stirring of magneton blender is put into,
It is directly instilled wherein with the concentrated hydrochloric acid of 11.9mol/L simultaneously, in magnetic agitation in processing procedure until there is no bubble generation
It is stirred continuously on device；Magnetic agitation was by 24 hours always；Become coffee-like turbid solution；Then with 2 M HF and 25% HAC volumes
Than 1:9 70 DEG C of processing 2h of mixed acid；It is washed repeatedly with deionized water until filtrate is in neutrality, 80 DEG C of vacuum drying obtain pure
Porous nano grade silica flour.
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| CN109867796A (en) * | 2019-01-31 | 2019-06-11 | 沈阳工业大学 | The preparation method of Ce-Li-MOF lithium ion battery negative material and its application in terms of preparing lithium ion battery |
| CN110890557A (en) * | 2019-11-27 | 2020-03-17 | 西北大学 | Perovskite type catalyst for oxygen reduction reaction, preparation method and application |
| CN113594459A (en) * | 2021-07-26 | 2021-11-02 | 常州烯源谷新材料科技有限公司 | Composite negative electrode material with multilayer structure and preparation method and application thereof |
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