CN105932240A - Nano-silicon-carbon compound and preparation method and application thereof - Google Patents

Nano-silicon-carbon compound and preparation method and application thereof Download PDF

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Publication number
CN105932240A
CN105932240A CN201610310457.1A CN201610310457A CN105932240A CN 105932240 A CN105932240 A CN 105932240A CN 201610310457 A CN201610310457 A CN 201610310457A CN 105932240 A CN105932240 A CN 105932240A
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silicon
nano
carbon
containing biomass
anhydrous
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高标
苏建君
霍开富
付继江
张旭明
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Wuhan University of Science and Engineering WUSE
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/362Composites
    • H01M4/364Composites as mixtures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/38Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386Silicon or alloys based on silicon
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention belongs to the comprehensive technical field of biological waste resources, and in particular a nano-silicon-carbon compound and a preparation method and application thereof. The preparation method comprises the following steps: performing acid-cooking on silicon-containing biomass to remove inorganic ion impurities, cleaning and drying the silicon-containing biomass, and then grinding the biomass into powder; carbonizing the biomass in an inert atmosphere to obtain a compound product of silicon dioxide and carbon; and uniformly mixing the carbonized product, metal powder and anhydrous chloride metal salt, placing the mixture in a tubular furnace, and obtaining a nano-silicon-carbon compound material with silicon nano-particles uniformly distributed in the carbon by reaction in the inert atmosphere. The method disclosed by the invention is simple and easy to implement, the raw material is rich in source, the most important is that the added anhydrous chloride enables the reaction to be generated in an extremely low temperature; the preparation process of the super-thin nano-silicon has the features of being low in energy consumption, simple in process, small in pollution, high in product purity, and uniform in particle; and the obtained silicon nano-particle is uniform in particle size and distribution, and can be applied to the field of a negative electrode material of a lithium ion battery.

Description

Nano silicon-carbon complex and its preparation method and application
Technical field
The invention belongs to biological waste resource comprehensive technical field, particularly relate to a kind of nano silicon-carbon complex and Its preparation method and application.
Background technology
Lithium ion battery as the energy storage device of a kind of green, have that running voltage is high, energy density greatly, certainly put The advantages such as electricity rate is little, are widely used in all kinds of portable electric appts.The theoretical lithium storage content of silicon (Si) is up to 4200mAh/g, exceedes 10 times of commercialization mainstay material-graphite theoretical capacity, and the voltage platform of Si is slightly higher In graphite, being difficult to cause the phenomenon of surface analysis lithium when charging, security performance is better than graphite-like C negative material, Thus silicon is expected to substitute commercialization graphite and becomes the negative material of lithium ion battery of future generation.But, silicium cathode material It is obviously not enough to there are some in material: first, lithium ion (Li+) enter Si negative pole can form alloy phase volume Expanding up to 420%, the internal stress making material produce is up to 1-2GPa, causes Si active material efflorescence, electricity Pole material produces with collector and separates, and causes electrode cycle performance rapid attenuation;Secondly, the intrinsic conductivity of Si Low, for 6.7x10-4S/cm, limits the high rate performance under the conditions of its high current charge-discharge.It addition, Si deintercalation The expansion repeatedly of lithium process and contraction so that it is at LiPF6Electrolyte is difficult to form stable solid electrolyte circle Face (SEI) film.Compared to block Si material, nano Si, due to the reduction of absolute expansion volume, can reduce de- The stress destruction to material structure produced in process of intercalation, improves the electrochemistry cycle performance of Si material, meanwhile, Nano Si also can shorten the lithium ion deintercalation degree of depth and the evolving path, brings advantage kinetically.
The preparation about silicon-carbon composite electrode material in current document and patent all uses multistep processes to realize, first First synthesis silicon or carbon, loads another composition by physics and chemical method the most again, frequently with side Method has pyrolysismethod, ball-milling method, vapour deposition process and polymer-pyrolysis route etc., and the silicon-carbon that these methods obtain is combined Material homogeneity is poor, and cost is the highest, and damage ratio is more serious, it is impossible to realize large-scale production.
Can be at lower temperature (more than 650 DEG C) it addition, there is many documents report to utilize magnesium heat, aluminothermy etc. to react Silicon oxide reduction is generated silicon, but these methods exist pasc reaction, and silicon easily reunion etc. that is insufficient and that generate is asked Topic, needs follow-up removal step, therefore not only increases production cost, also make the product prepared Can be undesirable.
Summary of the invention
For above-mentioned technical problem, the present invention provides a kind of with silicon containing biomass as raw material, and ultralow temperature prepares nanometer Silico-carbo complex, this nano silicon-carbon complex mix homogeneously.
The present invention solves that the technical scheme that above-mentioned technical problem is taked is:
Nano silicon-carbon complex, prepares gained with silicon containing biomass for raw material ultralow temperature.
Concrete preparation method comprises the following steps:
(1) by silicon containing biomass Acid treatment, remove inorganic ion impurity, be dried after repeatedly cleaning;
(2) by (1) acid boil after silicon containing biomass grind into powder, 400-700 DEG C in an inert atmosphere Carbonization treatment 1-12h, obtains the silicon containing biomass after the complex of silicon dioxide and carbon, i.e. carbonization;
(3) according to silicon dioxide: metal dust: anhydrous chloride slaine mass ratio is 1:1-3:2-20 Amount, the silicon containing biomass after carbonization adds metal dust and anhydrous chloride slaine, after mix homogeneously Put in tube furnace and be heated to 150-300 DEG C with the programming rate of 1-30 DEG C/min, be incubated 1-12h, wait to produce Thing takes out after cooling to room temperature with the furnace;
(4) by after products therefrom chlorohydric acid pickling in (3), clean, filter, obtain after drying nano-silicon- Carbon combination product.
Wherein, in step (1), silicon containing biomass includes one or more in rice husk, Folium Bambusae or straw Mixing.
In step (3), anhydrous chloride slaine used is anhydrous zinc chloride, anhydrous ferric chloride or anhydrous chlorination One or more mixing in aluminum.
The application of this nano silicon-carbon complex is, is used for making lithium ion battery negative material.
Nano silicon-carbon complex that the present invention provides and its preparation method and application, by the siliceous biology after carbonization Matter is put in tube furnace under an inert atmosphere after uniformly mixing with appropriate metal dust, anhydrous chloride slaine Fully reaction (4Al+3SiO2+2AlCl3==3Si+6AlOCl), remove by-product i.e. by pickling subsequently Obtain superfine nano silicon.Anhydrous chloride fusing point owing to adding is low, and fusing point about 100 DEG C-400 DEG C, during reaction Melted inorganic salt can ensure that reaction fully carries out also to control reaction temperature, it addition, metal dust is at fused salt Middle meeting ionizing (Al=Al3++3e-) so that metal dust has the highest reactivity so that this super Thin nano-silicon have high yield, purity compared with high, specific surface area is big, evengranular feature, this is also this method Can (200 DEG C) occur under ultralow temperature major reason.
Nano silicon-carbon complex that the present invention provides and its preparation method and application, preparation method is simple, Raw material sources are extensive, it is most important that owing to adding anhydrous chloride so that reaction at very low temperature can Occur, the preparation technology of this superfine nano silicon has that energy consumption is low, technique simple, it is little to pollute, product purity relatively High, the granule feature such as uniformly, and the nano silicon particles uniform particle diameter obtained is evenly distributed, can apply to lithium from Sub-cell negative electrode material field.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the silicon-carbon complex that the embodiment of the present invention 1 prepares.
Fig. 2 is the EDS collection of illustrative plates of the silicon-carbon complex that the embodiment of the present invention 1 prepares.
Fig. 3 is the SEM Electronic Speculum figure of the silicon-carbon complex that the embodiment of the present invention 1 prepares.
Fig. 4 is the TEM collection of illustrative plates of the silicon-carbon complex that the embodiment of the present invention 1 prepares.
Detailed description of the invention
The present invention will be further described with embodiment below in conjunction with the accompanying drawings, and certain following embodiment should not be understood For limitation of the present invention.
Embodiment 1
(1) 5g rice husk Acid treatment is removed inorganic ion impurity, be dried after repeatedly cleaning;
(2) by (1) acid boil after rice husk grind into powder 600 DEG C of carbonization treatment 6h in an inert atmosphere Obtain black product;
(3) by the black product 2.1g in (2) and 1.2g aluminum and 10g aluminum chloride (AlCl3) mixing is all Even, then mixture is put in tube furnace and be heated to 200 DEG C of insulation 3h with the programming rate of 5 DEG C/min, Take out after product cools to room temperature with the furnace;
(4) by after products therefrom chlorohydric acid pickling in (3), clean, filter, obtain after drying nano-silicon- Carbon combination product.
From the XRD diffracting spectrum of Fig. 1, at the three strongest ones peak of 28.4 °, 47.3 ° and 56.1 ° and silicon (JCPDS No.27-1402) three strongest ones peak is corresponding, and substantially without dephasign;From the scanning electron microscope (SEM) photograph of Fig. 2, this reality Execute a diameter of 30-60nm of silicon nano that example prepares and dispersion is the most uniform;By Fig. 3's and Fig. 4 The silicon nano yardstick major part that the present embodiment knowable to transmission electron microscope picture prepares is at below 50nm;Therefore The present invention can industrially large-scale production and application.
Embodiment 2
(1) 5g Folium Bambusae Acid treatment is removed inorganic ion impurity, be dried after repeatedly cleaning;
(2) by (1) acid boil after Folium Bambusae grind into powder 400 DEG C of carbonization treatment 12h in an inert atmosphere Obtain black product;
(3) by the black product 2.8g in (2) and 2g magnesium and 20g zinc chloride (ZnCl2) mix homogeneously, Then mixture is put in tube furnace and be heated to 150 DEG C of insulation 12h with the programming rate of 3 DEG C/min, wait to produce Thing takes out after cooling to room temperature with the furnace;
(4) by after products therefrom chlorohydric acid pickling in (3), clean, filter, obtain after drying nano-silicon- Carbon combination product.
Embodiment 3
(1) 5g straw Acid treatment is removed inorganic ion impurity, be dried after repeatedly cleaning;
(2) by (1) acid boil after straw grind into powder 500 DEG C of carbonization treatment 9h in an inert atmosphere Obtain black product;
(3) by the black product 1.5g in (2) and 1.9g ferrum and 15g aluminum chloride (AlCl3) mixing is all Even, then mixture is put in tube furnace and be heated to 250 DEG C of insulation 6h with the programming rate of 10 DEG C/min, Take out after product cools to room temperature with the furnace;
(4) by after products therefrom chlorohydric acid pickling in (3), clean, filter, obtain after drying nano-silicon- Carbon combination product.
Embodiment 4
(1) 5g rice husk Acid treatment is removed inorganic ion impurity, be dried after repeatedly cleaning;
(2) by (1) acid boil after rice husk grind into powder 700 DEG C of carbonization treatment 1h in an inert atmosphere Obtain black product;
(3) by the black product 2.1g in (2) and 3g aluminum and 2g iron chloride (FeCl3) mix homogeneously, Then mixture is put in tube furnace and be heated to 300 DEG C of insulation 9h with the programming rate of 20 DEG C/min, wait to produce Thing takes out after cooling to room temperature with the furnace;
(4) by after products therefrom chlorohydric acid pickling in (3), clean, filter, obtain after drying nano-silicon- Carbon combination product.
Embodiment 5
(1) 5g rice husk Acid treatment is removed inorganic ion impurity, be dried after repeatedly cleaning;
(2) by (1) acid boil after rice husk grind into powder 550 DEG C of carbonization treatment 5h in an inert atmosphere Obtain black product;
(3) by the black product 2.1g in (2) and 1.2g aluminum and 25g aluminum chloride (AlCl3) mixing is all Even, then mixture is put in tube furnace and be heated to 200 DEG C of insulation 1h with the programming rate of 30 DEG C/min, Take out after product cools to room temperature with the furnace;
(4) by after products therefrom chlorohydric acid pickling in (3), clean, filter, obtain after drying nano-silicon- Carbon combination product.
Embodiment 6
(1) 5g rice husk Acid treatment is removed inorganic ion impurity, be dried after repeatedly cleaning;
(2) by (1) acid boil after rice husk grind into powder 650 DEG C of carbonization treatment 3h in an inert atmosphere Obtain black product;
(3) by the black product 2.1g in (2) and 2.5g magnesium and 15g aluminum chloride (AlCl3) mixing is all Even, then mixture is put in tube furnace and be heated to 200 DEG C of insulation 3h with the programming rate of 5 DEG C/min, Take out after product cools to room temperature with the furnace;
(4) by after products therefrom chlorohydric acid pickling in (3), clean, filter, obtain after drying nano-silicon- Carbon combination product.
This detailed description of the invention compared with prior art, has the positive effect that:
1. the present invention is fused into liquid phase after utilizing the heat absorption of anhydrous chlorination slaine, not only makes reactant be fully contacted, Improve reaction yield, also make metal dust ionized at liquid-phase fused salts, improve reactivity, significantly Reduce reaction temperature.
Reaction the most used in the present invention occurs under ultralow temperature, therefore effectively prevent the reunion of nano-silicon, The nano-silicon prepared is made to have less particle diameter.
It should be noted that it will be understood by those within the art that, can be to technical scheme Modifying or equivalent, without deviating from objective and the scope of technical solution of the present invention, it all should be contained at this In the middle of the right of invention.

Claims (5)

1. nano silicon-carbon complex, it is characterised in that prepare gained for raw material ultralow temperature with silicon containing biomass.
Nano silicon-carbon complex the most according to claim 1, it is characterised in that preparation method include with Lower step:
(1) by silicon containing biomass Acid treatment, remove inorganic ion impurity, be dried after repeatedly cleaning;
(2) by (1) acid boil after silicon containing biomass grind into powder, 400-700 DEG C in an inert atmosphere Carbonization treatment 1-12h, obtains the silicon containing biomass after the complex of silicon dioxide and carbon, i.e. carbonization;
(3) according to silicon dioxide: metal dust: anhydrous chloride slaine mass ratio is 1:1-3:2-20 Amount, the silicon containing biomass after carbonization adds metal dust and anhydrous chloride slaine, after mix homogeneously Put in tube furnace and be heated to 150-300 DEG C with the programming rate of 1-30 DEG C/min, be incubated 1-12h, treat product Take out after cooling to room temperature with the furnace;
(4) by after products therefrom chlorohydric acid pickling in (3), clean, filter, obtain after drying nano-silicon- Carbon combination product.
Nano silicon-carbon complex the most according to claim 2, it is characterised in that in described step (1) Silicon containing biomass includes one or more the mixing in rice husk, Folium Bambusae or straw.
Nano silicon-carbon complex the most according to claim 2, it is characterised in that in described step (3) Anhydrous chloride slaine used is one or both in anhydrous zinc chloride, anhydrous ferric chloride or anhydrous Aluminum chloride Above mixing.
5. according to the application of the nano silicon-carbon complex described in any one of claim 1 to 4, it is characterised in that For making lithium ion battery negative material.
CN201610310457.1A 2016-05-11 2016-05-11 Nano-silicon-carbon compound and preparation method and application thereof Pending CN105932240A (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106299327A (en) * 2016-10-10 2017-01-04 东莞市凯金新能源科技股份有限公司 A kind of preparation method of lithium ion battery anode material
CN106684336A (en) * 2016-12-25 2017-05-17 常州亚环环保科技有限公司 Preparation method for high-combination degree lithium battery carbon silicon anode material
CN110386604A (en) * 2019-08-09 2019-10-29 北方奥钛纳米技术有限公司 The preparation method of nano-silicon, silicon based anode material and preparation method thereof
CN110429264A (en) * 2019-08-13 2019-11-08 吉林大学 A method of preparing rice husk base negative electrode material
CN110867567A (en) * 2019-10-25 2020-03-06 湖北万润新能源科技发展有限公司 High-safety SiO synthesized by biomass siliconxPreparation method and application of @ C material
CN110943211A (en) * 2019-12-16 2020-03-31 安徽工业大学 Preparation method of high-performance Si/C negative electrode material
CN111009648A (en) * 2019-12-10 2020-04-14 华南农业大学 Silicon-carbon composite material and preparation method thereof
CN111082000A (en) * 2019-11-29 2020-04-28 湖北万润新能源科技发展有限公司 Preparation method for optimizing SiOx @ C performance by using pore-forming agent
CN111646472A (en) * 2020-05-22 2020-09-11 兰州理工大学 Method for in-situ preparation of porous silicon-carbon composite negative electrode material
CN113998702A (en) * 2021-10-13 2022-02-01 昆明理工大学 Method for preparing Si/C negative electrode material by using micro silicon powder as raw material
CN114014320A (en) * 2021-11-18 2022-02-08 兰州城市学院 Method for preparing carbon-silicon composite material by using algae biomass and application of carbon-silicon composite material in lithium ion battery
CN114735704A (en) * 2022-05-25 2022-07-12 安徽工业大学 Method for synthesizing nano silicon carbide at low temperature
CN116375035A (en) * 2023-03-15 2023-07-04 湖北斯诺新材料科技有限公司 Preparation method of three-dimensional porous silicon-carbon composite material and composite material thereof

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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106299327A (en) * 2016-10-10 2017-01-04 东莞市凯金新能源科技股份有限公司 A kind of preparation method of lithium ion battery anode material
CN106684336A (en) * 2016-12-25 2017-05-17 常州亚环环保科技有限公司 Preparation method for high-combination degree lithium battery carbon silicon anode material
CN106684336B (en) * 2016-12-25 2019-08-23 联动天翼新能源有限公司 A kind of preparation method of high conjugation lithium battery carbon silicium cathode material
CN110386604A (en) * 2019-08-09 2019-10-29 北方奥钛纳米技术有限公司 The preparation method of nano-silicon, silicon based anode material and preparation method thereof
CN110429264A (en) * 2019-08-13 2019-11-08 吉林大学 A method of preparing rice husk base negative electrode material
CN110429264B (en) * 2019-08-13 2022-03-08 吉林大学 Method for preparing rice hull-based negative electrode material
CN110867567A (en) * 2019-10-25 2020-03-06 湖北万润新能源科技发展有限公司 High-safety SiO synthesized by biomass siliconxPreparation method and application of @ C material
CN111082000A (en) * 2019-11-29 2020-04-28 湖北万润新能源科技发展有限公司 Preparation method for optimizing SiOx @ C performance by using pore-forming agent
CN111009648A (en) * 2019-12-10 2020-04-14 华南农业大学 Silicon-carbon composite material and preparation method thereof
CN111009648B (en) * 2019-12-10 2021-12-24 华南农业大学 Silicon-carbon composite material and preparation method thereof
CN110943211A (en) * 2019-12-16 2020-03-31 安徽工业大学 Preparation method of high-performance Si/C negative electrode material
CN111646472A (en) * 2020-05-22 2020-09-11 兰州理工大学 Method for in-situ preparation of porous silicon-carbon composite negative electrode material
CN113998702A (en) * 2021-10-13 2022-02-01 昆明理工大学 Method for preparing Si/C negative electrode material by using micro silicon powder as raw material
CN113998702B (en) * 2021-10-13 2023-10-13 昆明理工大学 Method for preparing Si/C anode material by taking micro silicon powder as raw material
CN114014320A (en) * 2021-11-18 2022-02-08 兰州城市学院 Method for preparing carbon-silicon composite material by using algae biomass and application of carbon-silicon composite material in lithium ion battery
CN114735704A (en) * 2022-05-25 2022-07-12 安徽工业大学 Method for synthesizing nano silicon carbide at low temperature
CN114735704B (en) * 2022-05-25 2024-01-05 安徽工业大学 Method for synthesizing nano silicon carbide at low temperature
CN116375035A (en) * 2023-03-15 2023-07-04 湖北斯诺新材料科技有限公司 Preparation method of three-dimensional porous silicon-carbon composite material and composite material thereof

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Application publication date: 20160907