CN105280901B - The preparation method of spherical porous silicon carbide composite particles - Google Patents

The preparation method of spherical porous silicon carbide composite particles Download PDF

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CN105280901B
CN105280901B CN201510609459.6A CN201510609459A CN105280901B CN 105280901 B CN105280901 B CN 105280901B CN 201510609459 A CN201510609459 A CN 201510609459A CN 105280901 B CN105280901 B CN 105280901B
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composite particles
sio
spherical porous
spherical
silicon carbide
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CN105280901A (en
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路密
杨行
陈海
肖彩霞
汤林斌
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Xiamen University of Technology
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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
    • H01M4/364—Composites as mixtures
    • 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
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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 present invention discloses a kind of preparation method of spherical porous silicon carbide composite particles, including：One Na is provided2SiO3Solution；One saccharide compound is dissolved in the Na2SiO3Solution, forms one first solution；First solution is spray-dried, spherical Na is formed2SiO3/ carbohydrate composite particles；By the spherical Na2SiO3/ carbohydrate composite particles add one suspension of charing process formation in the concentrated sulfuric acid, and further above-mentioned suspension is added in distilled water and dilutes and makes Na2SiO3Hydrolysis, which is obtained, includes spherical porous SiO2The suspension of/C composite particles；Filtering obtains spherical porous SiO2/ C composite particles；By a reducing agent and the spherical porous SiO2/ C composite particles are mixed, and heating makes spherical porous SiO2SiO in/C composite particles2Reduction, forms spherical porous Si/C composite particles.

Description

The preparation method of spherical porous silicon carbide composite particles
Technical field
The present invention relates to a kind of preparation method of spherical porous silicon carbide composite particles.
Background technology
Lithium ion battery is the secondary cell of new generation after lead-acid battery, nickel-cadmium cell and Ni-MH battery.In the whole world Today that the lasting in short supply and environment of petroleum resources constantly deteriorates is faced, lithium ion battery is due to capacity height, cycle life Length, small self discharge, memory-less effect, non-environmental-pollution and the advantages of have a safety feature, have become the weight of hi-tech development One of point, it is considered to be high power capacity, the choosing of the ideal of high power battery, are the environmentally friendly power supplys of 21 century.Chargeable lithium ion electricity Pond is since the nineteen ninety since commercialization, and its application is constantly expanded, from portable electrics such as mobile phone, notebook computers Sub- apparatus field will all be used widely to the numerous areas such as electric automobile and Aero-Space, the artificial satellite in future.Mesh Before, people have begun to be directed to study new rechargeable lithium ion batteries, are available for mixed power electric car, chargeable mixed Close the vehicles such as power car and pure electric vehicle to use, so as to reduce the dependence to oil and alleviate air pollution.Meet This application, the cycle performance that lithium ion battery must possess high power density, high energy density is become reconciled.Negative material conduct The important component of lithium ion battery, is the key of lithium-ion energy storage device development.Current commercial li-ion GND material Material is mainly graphite material, and graphite has layer structure, and volumetric expansion is small in charge and discharge process, be not easy powder that material occur Change, but the theoretical treatment capacity of graphite is smaller, only 400mAh/g.Silicon is due to maximum theoretical treatment capacity 4200mAh/g and widely paid close attention to, but be due to close-packed structure, silicon volumetric expansion in charge and discharge process is big, material Efflorescence is serious, and nano-silicon and thin film silicon cost of manufacture are high in addition, and these all govern its application in lithium ion battery.
Existing Si-C composite material can combine the advantage of above two material, so as to obtain the negative of high power capacity low bulk Pole material.However, existing Si-C composite material, typically carries out silica flour and graphite being formed after simply grinding, e.g., CN102403491A.However, the performance that above-mentioned preparation method obtains Si-C composite material needs further raising.
The content of the invention
The present invention provides a kind of preparation method of spherical porous silicon carbide composite particles, can solve the above problems.The ball The preparation method of the porous silicon carbide composite particles of shape, comprises the following steps：
One Na is provided2SiO3Solution；One saccharide compound is dissolved in the Na2SiO3Solution, forms one first solution； First solution is spray-dried, spherical Na is formed2SiO3/ carbohydrate composite particles；By the spherical Na2SiO3/ carbohydrate Composite particles add one suspension of charing process formation in the concentrated sulfuric acid, and the suspension includes spherical porous Na2SiO3Compound of/C Grain；The suspension is added in distilled water and diluted, makes spherical porous Na2SiO3Na in/carbon composite particles2SiO3Hydrolysis, shape The porous SiO of globulate2/ C composite particles；Filtering obtains spherical porous SiO2/ C composite particles；By a reducing agent with it is described spherical many Hole SiO2/ C composite particles are mixed, and heating makes spherical porous SiO2SiO in/C composite particles2Reduction, is formed spherical porous Si/C composite particles.
Further, the Na2SiO3The concentration of solution is 15wt% to 25wt%.
Further, it is described that saccharide compound is dissolved in the Na2SiO3The step of solution, includes：According to carbonization degree 15% ~ 25% is included in the saccharide compound of silicone content 5wt% ~ 15%.
Further, the saccharide compound includes monosaccharide and disaccharide, oligosaccharide and polysaccharide.
Further, the monose is glucose, fructose or its mixture, and disaccharide is sucrose, maltose, lactose or it is mixed Compound.
Further, the spray parameters are：Inlet amount is 1 ~ 10ml/min., and inlet temperature is 100 ~ 200 DEG C, pressure For 0.1 ~ 1MPa.
Further, filtering obtains spherical porous SiO2After/C composite particles, further comprising will be described spherical porous SiO2The step that/C composite particles are cleaned and dried.
Further, the reducing agent is magnesium powder, and described by reducing agent and the spherical porous SiO2/ C composite particles Mixing, and heating makes spherical porous SiO2SiO in/C composite particles2Reduction, the step of forming spherical porous Si/C composite particles Including：By excessive magnesium powder and the spherical porous SiO2/ C composite particles are mixed；Heating makes magnesium powder reduction described spherical porous SiO2SiO in/C composite particles2, form spherical porous Si/C composite particles；Above-mentioned spherical porous Si/C composite particles are added Cleaned in water；And filter and dry, obtain the spherical porous Si/C composite particles of high-purity.
Further, being heated to 600 ~ 700 DEG C makes magnesium powder reduce the spherical porous SiO2SiO in/C composite particles2, Form spherical porous Si/C composite particles.
Further, it is described by excessive magnesium powder and the spherical porous SiO2The step of/C composite particles are mixed includes：Will Theoretical amount 105wt% ~ 115wt% magnesium powder and the spherical porous SiO2/ C composite particles are mixed.
A kind of preparation method for spherical porous silicon carbide composite particles that the present invention is provided, can obtain high-purity, micron order Or even many sky Si/C composite particles of nanoscale.
Brief description of the drawings
Fig. 1 is the preparation method flow chart of spherical porous silicon carbide composite particles provided in an embodiment of the present invention.
Fig. 2 is the stereoscan photograph of the spherical porous silicon carbide composite particles obtained by the present embodiment 1.
Fig. 3 is the song of circulation first that the spherical porous silicon carbide composite particles obtained by the present embodiment 1 are assembled into button cell Line.
Fig. 4 is the cyclic curve that the spherical porous silicon carbide composite particles obtained by the present embodiment 1 are assembled into button cell.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.It is understood that this place is retouched The specific embodiment stated is used only for explaining the present invention, rather than limitation of the invention.It also should be noted that, in order to just Part related to the present invention rather than entire infrastructure are illustrate only in description, accompanying drawing.
Fig. 1 is refer to, a kind of preparation method of spherical porous silicon carbide composite particles comprises the following steps：
There is provided a Na by S12SiO3Solution；
S2, the Na is dissolved in by a saccharide compound2SiO3Solution, forms one first solution；
S3, first solution is spray-dried, and forms spherical Na2SiO3/ carbohydrate composite particles；
S4, by the spherical Na2SiO3/ carbohydrate composite particles add one suspension of charing process formation in the concentrated sulfuric acid, described Suspension includes spherical porous Na2SiO3/ C composite particles；
S5, the suspension is added in distilled water and diluted, makes spherical porous Na2SiO3In/carbon composite particles Na2SiO3Hydrolysis, forms spherical porous SiO2/ C composite particles；
S6, filtering obtains spherical porous SiO2/ C composite particles；
S7, by a reducing agent and the spherical porous SiO2/ C composite particles are mixed, and heating makes spherical porous SiO2/ C is multiple Close the SiO in particle2Reduction, forms spherical porous Si/C composite particles.
In step sl, the Na2SiO3The concentration of solution is 15wt% to 25wt%.It is preferred that, the 18wt% is arrived 22wt%.The Na2SiO3The concentration of solution is 20% or so.It is appreciated that when concentration it is too high, the Na2SiO3The viscosity of solution It is excessive, it is unfavorable for follow-up spraying treatment；And concentration is too low, it is unfavorable for forming composite particles.
In step s 2, the saccharide compound includes monosaccharide and disaccharide, oligosaccharide and polysaccharide.It is preferred that, the sugar Class compound is monose or disaccharide, and this is due to that monose or disaccharide are more beneficial for follow-up charing process.Further, the list Sugar can be glucose, fructose or its mixture.Disaccharide can be sucrose, maltose, lactose or its mixture.The carbohydrate Compound can be included in silicone content 5wt% ~ 15% according to carbonization degree 15% ~ 25% and add Na2SiO3In solution.It is preferred that, the carbohydrate Compound is preferred to be included in silicone content 8wt% ~ 12% according to carbonization degree 18% ~ 22% and adds Na2SiO3In solution.It is furthermore preferred that the sugar Class compound is preferred to be included in silicone content 10% according to carbonization degree 20% and adds Na2SiO3In solution.It is appreciated that by adding not The saccharide compound of same amount can control the ratio of carbon and silicon in earliest product.
In step s3, the spray parameters are：Inlet amount is 1 ~ 10ml/min, and inlet temperature is 100 ~ 200 DEG C, pressure For 0.1 ~ 1MPa.It is appreciated that micron order or nano level spherical Na can be obtained by the control of spray parameters2SiO3/ carbohydrate Composite particles.It is preferred that, the spray parameters are：Inlet amount is 2 ~ 5ml/min, and inlet temperature is 150 ~ 170 DEG C, and pressure is 0.3~0.5MPa.It is preferred that, the spray parameters are：Inlet amount is 3 ~ 4ml/min, and inlet temperature is 155 ~ 160 DEG C, and pressure is 0.3~0.5MPa。
In step s 4, in order to prevent spherical Na2SiO3Na in/carbohydrate composite particles2SiO3Produce in atmosphere rotten Reaction, should be by the spherical Na of acquisition2SiO3/ carbohydrate composite particles are transferred in the concentrated sulfuric acid immediately.It is appreciated that spherical Na2SiO3Saccharide compound in/carbohydrate composite particles can be dehydrated and carbonize by the concentrated sulfuric acid.Further, can suitably it heat To promote carbohydrate dehydration.
In step s 6, filtering obtains spherical porous SiO2After/C composite particles, may further include will be described spherical Porous SiO2/ C composite particles are cleaned and dried, to remove the impurity such as sodium ion and sulfate radical.
In the step s 7, the reducing agent is preferably magnesium powder, and described by reducing agent and the spherical porous SiO2/C Composite particles are mixed, and heating makes spherical porous SiO2SiO in/C composite particles2Reduction, forms compound of spherical porous Si/C The step of grain, includes：
S71, by excessive magnesium powder and the spherical porous SiO2/ C composite particles are mixed；
S72, heating makes magnesium powder reduce the spherical porous SiO2SiO in/C composite particles2, form spherical porous Si/C Composite particles；
Above-mentioned spherical porous Si/C composite particles are added to the water cleaning by S73；And
S74, filters and dries, obtain the spherical porous Si/C composite particles of high-purity.
It is described by excessive magnesium powder and the spherical porous SiO in step S712The step of/C composite particles are mixed includes：Will Theoretical amount 105wt% ~ 115wt% magnesium powder and the spherical porous SiO2/ C composite particles are mixed.It is preferred that, by theoretical amount 108wt% ~ 112wt% magnesium powder and the spherical porous SiO2/ C composite particles are mixed.It is furthermore preferred that by theoretical amount 109wt% ~ 111wt% magnesium powder and the spherical porous SiO2/ C composite particles are mixed.By excessive magnesium powder and the spherical porous SiO2/C Composite particles reaction is in order that SiO2Fully reduction, prevents residual Si O in final product2。
The step S72 is preferred to be carried out in inert atmosphere.In addition, heating makes magnesium powder reduce the SiO2Temperature be 600~700℃.It is preferred that, the heating makes magnesium powder reduce the SiO2Temperature be 640 ~ 760 DEG C.It is furthermore preferred that described add Heat makes magnesium powder reduce the SiO2Temperature be 655 ~ 765 DEG C.
In step S73, remaining magnesium powder can react and remove with water, and the MgO of generation can also be dissolved in the water And remove.
Embodiment 1：
Compound concentration is 20% Na2SiO3Solution, the sucrose of silicone content 10% is included according to carbonization degree 20%, is sprayed after dissolving Dry, wherein, spray parameters are：Inlet amount is 4ml/min., and inlet temperature is 160 DEG C, and pressure is 0.4MPa；The product of acquisition Appropriate dense H is added immediately2SO4Make char sucrose, mixed solution is slowly added into distilled water after certain time and dilutes acquisition SiO2/ C composite, powder is mixed in the case where inertia dries atmosphere with the magnesium powder of theoretical amount 110% after filtering, cleaning, drying After even, compacting under an inert atmosphere 600 DEG C of reactions be naturally cooling to after room temperature powder being dissolved in cause in distilled water it is remaining Magnesium powder is reacted and the MgO of generation dissolves, and spherical porous Si/C composite particles are obtained after filtering cleaning, drying.
Fig. 2 is refer to, Fig. 2 is the stereoscan photograph of the spherical porous Si/C composite particles obtained.Can from figure The maximum gauge for going out the spherical porous Si/C composite particles of acquisition is 20 ~ 30 microns, and minimum diameter can reach 100 nanometers of left sides It is right.That is, a diameter of 30 microns to 100 nanometers of spherical porous Si/C composite particles.
By spherical porous Si/C composite particles:SBR:CMC:Conductive agent is according to mass ratio 70:10:10:10 are fabricated to slurry, It is coated on copper foil, button cell is assembled into after drying and measures its chemical property.Fig. 3 is bent for the circulation first of button cell Line, as can be seen from the figure its reversible capacity is up to 1187 mAh/g.Fig. 4 is the cyclic curve of the material, can from figure Go out reversible capacity after 20 circulations and may also reach up 1079 mAh/g.
Note, above are only presently preferred embodiments of the present invention and institute's application technology principle.It will be appreciated by those skilled in the art that The invention is not restricted to specific embodiment described here, can carry out for a person skilled in the art it is various it is obvious change, Readjust and substitute without departing from protection scope of the present invention.Therefore, although the present invention is carried out by above example It is described in further detail, but the present invention is not limited only to above example, without departing from the inventive concept, also Other more equivalent embodiments can be included, and the scope of the present invention is determined by scope of the appended claims.

Claims (10)

1. a kind of preparation method of spherical porous silicon carbide composite particles, it is characterised in that comprise the following steps：
One Na is provided2SiO3Solution；
One saccharide compound is dissolved in the Na2SiO3Solution, forms one first solution；
First solution is spray-dried, spherical Na is formed2SiO3/ carbohydrate composite particles；
By the spherical Na2SiO3/ carbohydrate composite particles add one suspension of charing process formation, the suspension in the concentrated sulfuric acid Including spherical porous Na2SiO3/ C composite particles；
The suspension is added in distilled water and diluted, makes spherical porous Na2SiO3Na in/carbon composite particles2SiO3Hydrolysis, shape The porous SiO of globulate2/ C composite particles；
Filtering obtains spherical porous SiO2/ C composite particles；
By a reducing agent and the spherical porous SiO2/ C composite particles are mixed, and heating makes spherical porous SiO2/ C composite particles In SiO2Reduction, forms spherical porous Si/C composite particles.
2. the preparation method of spherical porous silicon carbide composite particles according to claim 1, it is characterised in that the Na2SiO3 The concentration of solution is 15wt% to 25wt%.
3. the preparation method of spherical porous silicon carbide composite particles according to claim 1, it is characterised in that described by carbohydrate Compound is dissolved in the Na2SiO3The step of solution, includes：According to carbonization degree 15%~25% be included in silicone content 5wt%~ 15% saccharide compound.
4. the preparation method of spherical porous silicon carbide composite particles according to claim 1, it is characterised in that the carbohydrate Compound includes monosaccharide and disaccharide and polysaccharide.
5. the preparation method of spherical porous silicon carbide composite particles according to claim 4, it is characterised in that the carbohydrate Compound is monosaccharide and disaccharide or its mixture, and the monose is glucose or fructose, and the disaccharide is sucrose, maltose or lactose.
6. the preparation method of spherical porous silicon carbide composite particles according to claim 1, it is characterised in that the spraying ginseng Number is：Inlet amount is 1~10ml/min., and inlet temperature is 100~200 DEG C, and pressure is 0.1~1MPa.
7. the preparation method of spherical porous silicon carbide composite particles according to claim 1, it is characterised in that filtering obtains ball The porous SiO of shape2After/C composite particles, further comprise the spherical porous SiO2What/C composite particles were cleaned and dried Step.
8. the preparation method of spherical porous silicon carbide composite particles according to claim 1, it is characterised in that the reducing agent For magnesium powder, and it is described by reducing agent and the spherical porous SiO2/ C composite particles are mixed, and heating makes spherical porous SiO2/ C is multiple Close the SiO in particle2Reduction, the step of forming spherical porous Si/C composite particles includes：
By excessive magnesium powder and the spherical porous SiO2/ C composite particles are mixed；
Heating makes magnesium powder reduce the spherical porous SiO2SiO in/C composite particles2, form spherical porous Si/C composite particles；
Above-mentioned spherical porous Si/C composite particles are added to the water cleaning；And
Filter and dry, obtain the spherical porous Si/C composite particles of high-purity.
9. the preparation method of spherical porous silicon carbide composite particles according to claim 8, it is characterised in that be heated to 600 ~700 DEG C make magnesium powder reduce the spherical porous SiO2SiO in/C composite particles2, form spherical porous Si/C composite particles.
10. the preparation method of spherical porous silicon carbide composite particles according to claim 8, it is characterised in that described to incite somebody to action Measure magnesium powder and the spherical porous SiO2The step of/C composite particles are mixed includes：By theoretical amount 105wt%~115wt% magnesium Powder and the spherical porous SiO2/ C composite particles are mixed.
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CN105762338A (en) * 2016-02-04 2016-07-13 天津大学 Method for preparing lithium battery silicon carbon anode material by utilizing magnesiothermic reduction
CN105826539A (en) * 2016-06-02 2016-08-03 南阳师范学院 WO<3-X>/C composite, preparation method and application of WO3-X/C composite
CN106784769A (en) * 2017-02-17 2017-05-31 南通市苏中纺织有限公司 The water sodium metasilicate silicon nanometer anode material of low temperature magnesium nine
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