CN108346786A - The preparation method and product of nano-silicon/carbon composite and nano silicon dioxide/carbon composite - Google Patents
The preparation method and product of nano-silicon/carbon composite and nano silicon dioxide/carbon composite Download PDFInfo
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- CN108346786A CN108346786A CN201810065659.3A CN201810065659A CN108346786A CN 108346786 A CN108346786 A CN 108346786A CN 201810065659 A CN201810065659 A CN 201810065659A CN 108346786 A CN108346786 A CN 108346786A
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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
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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
- 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
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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 nano-silicon/carbon composite, and using rice husk as raw material, using magnesium powder as reducing agent, high temperature reduction is carried out under inert gas shielding, nano-silicon/carbon composite is prepared through one-step method；The temperature of the high temperature reduction is 600~900 DEG C, and the time is 1~10h.The invention also discloses a kind of preparation methods of nano silicon dioxide/carbon composite, and using rice husk as raw material, carbonization under inert gas protection obtains nano silicon dioxide/carbon composite；The temperature of the carbonization is 400~900 DEG C, and the time is 1~10h.The present invention each provides the preparation method of nano-silicon/carbon composite and nano silicon dioxide/carbon composite, using rice husk as raw material, is prepared through one-step method, and the preparation process is simple, without environmental pressure.
Description
Technical field
The present invention relates to field of lithium ion battery, and in particular to silicon/carbon, silicon/carbon dioxide with nanostructure are compound
Material and preparation method thereof.
Background technology
The rapid development of science and technology, the application of electronic equipment increase, have all shifted electrochmical power source onto more and more important
On position.In all kinds of electrochmical power sources, lithium ion battery is easy to carry since its is small, and charging and discharging capacity is high and stable etc.
Series of advantages so that it is using extremely wide.In the lithium ion battery applied at present, negative material is mostly carbon materials
Material, the stability of such as graphite, graphite is fine, but its lower theoretical specific capacity (372mAh/g) so that its application with development by
To limitation and influence.It is found in research, the theoretical lithium storage content of the semi-conducting materials such as silicon, tin is far above graphite, but its stability
Can be poor, there is more violent volume change during lithium ion deintercalation, destroy the microstructure of material, further influences its electricity
Pond performance causes its application to be obstructed.To solve this problem, researcher does a lot of work, this is also field of lithium ion battery
A big research hotspot.
In the research of lithium ion battery negative material, the research of silica-base material is of great interest, the theoretical specific volume of silicon materials
Higher, safety non-pollution is measured, but since removal lithium embedded causes volume change so that specific capacity is anxious during electrochemical property test
It falls sharply low, it is carbon material is compound with silicon materials, it is desirable to be able to have complementary advantages, improve the electrochemistry of material to solve this phenomenon
Performance.
In the document delivered, have it is several with silicon and carbon, the silica and compound obtained material of carbon be used as lithium from
The example of sub- cell negative electrode material.
As 103000902 A of Publication No. CN Chinese patent literature in disclose a kind of silicon/carbon composite, the material
Silicon/carbon composite is made by spraying cracking process respectively using silica flour and citric acid as silicon source and carbon source in material.For another example Publication No.
A kind of preparation method of silicon/carbon dioxide composite material is disclosed in the Chinese patent literature of 105633406 A of CN, respectively with
Sodium metasilicate and glucose are silicon source and carbon source, use sodium chloride for template, and it is compound to obtain silicon/carbon dioxide by the dry method of heat
Object.
But it is the combination product that two kinds of substances are formed using complex method in above-mentioned document, preparation method is cumbersome, former material
The production cost of material is also higher.
The Chinese patent literature of 104009210 A of Publication No. CN discloses a kind of porous silicon/carbon composite material, preparation
Method and purposes obtain having silicon/carbon of porous structure compound using rice husk as raw material using the method for metallothermic reduction and purifying
Material.This method first carries out high temperature cabonization to rice husk, and it is reducing agent to be followed by metal or carbon, is obtained through high temperature or ball-milling treatment
Silicon/carbon composite.But this method flow is complicated, and needed further in post-processing because reducing silica is not complete
Using hydrofluoric acid treatment, more serious problem of environmental pollution can be caused.
Invention content
In view of the above technical problems, the present invention each provides nano-silicon/carbon composite and nano silicon dioxide/carbon is multiple
The preparation method of condensation material is prepared using rice husk as raw material through one-step method, and the preparation process is simple, without environmental pressure.
Nano-silicon/the carbon composite being prepared and nano silicon dioxide/carbon composite are used separately as negative electrode of lithium ion battery,
It is suitable with using the performance of two kinds of composite materials being prepared in prior art.
Specific technical solution is as follows：
A kind of preparation method of nano-silicon/carbon composite, using rice husk as raw material, using magnesium powder as reducing agent, inert gas
Protection is lower to carry out high temperature reduction, and nano-silicon/carbon composite is prepared through one-step method；
The temperature of the high temperature reduction is 600~900 DEG C, and the time is 1~10h.
Product after the high temperature reduction also needs to be post-processed, specially：
Product is subjected to pickling, washing and drying process.
The present invention is high for silica-base material charging and discharging capacity, but volume change is apparent when removal lithium embedded, and special capacity fade is tight
Weight；Though and carbon material specific capacity is low, the characteristics of stable cycle performance, prepares silicon/carbon composite, can both obtain high
Specific capacity can enhance its cyclical stability again.In addition, it is raw material to choose carbon containing simultaneously and silicon biological material-rice husk, make
For carbon source and silicon source, cost is reduced；Raw material restores and then through pickling processes under the conditions of inert gas high temperature through magnesium powder
Fall magnesium oxide, obtains nano-silicon/carbon composite.It takes one-step method to prepare in experimentation, reduces experimental implementation complexity.
In post-processing, the purpose of pickling is the oxide of demagging, therefore can select common hydrochloric acid solution or sulfuric acid
Solution etc..
Preferably, the rice husk needs to be pre-processed before use, specially：
Rice husk washs successively through water, acetone, ethyl alcohol, deionized water, for use after drying.
Preferably, the rice husk and the mass ratio of magnesium powder are 1~2:1.
Further preferably, the rice husk and the mass ratio of magnesium powder are 2:1；
The temperature of the high temperature reduction is 700 DEG C, time 6h, and heating rate is 2 DEG C/min, and inert atmosphere is Ar gas.
After tested, under above-mentioned special reducing process, the element silicon in rice husk is fully reduced to elemental silicon, is not necessarily into one
Step processing.
Rice is maintained on from macroscopic view to nanoscale through nano-silicon/carbon composite that above-mentioned one-step method is prepared
The primary morphology and structure of shell remain the porous structure feature of rice husk, and wherein silicone content is 36% (mass percent), carbon
Content is 57%, remaining is oxygen component, is negative electrode of lithium ion battery silicon/comparatively ideal silicon carbon ratio of carbon material.
Nano-silicon/the carbon composite prepared in this way is the lithium ion battery that assembles of battery cathode, have compared with
High specific capacity and preferable stable cycle performance.
The invention also discloses a kind of preparation methods of nano silicon dioxide/carbon composite, using rice husk as raw material, lazy
Property gas shield under carbonization obtain nano silicon dioxide/carbon composite；
The temperature of the carbonization is 400~900 DEG C, and the time is 1~10h.
It comprises the concrete steps that：Directly rice husk is placed in tube furnace, high temperature cabonization under inert gas environment.
Rice husk itself is biomass castoff, and yield is big and at low cost；Contain carbon element silicon in rice husk simultaneously, disclosure satisfy that
The idea that two kinds of elements of carbon silicon are provided with same raw material simultaneously.
Preferably, the rice husk needs to be pre-processed before use, specially：
Rice husk washs successively through water, acetone, ethyl alcohol, deionized water, for use after drying.
Preferably, the time of the carbonization is 6h, heating rate is 2 DEG C/min, and inert atmosphere is Ar gas；It is further excellent
The temperature of choosing, the carbonization is 900 DEG C.
The more of original rice husk are completely maintained through nano silicon dioxide/carbon composite that above-mentioned one-step method is prepared
Scale topography and porous structure, are conducive to the chemical property for improving it as lithium ion battery negative material, dioxy in sample
SiClx content is 25% (mass percent), and carbon content 53%, remaining is the oxygen ingredient contained by rice husk carbonizing product.
Nano silicon dioxide/the carbon composite prepared in this way is the lithium ion battery that battery cathode assembles,
With higher specific capacity and preferable stable cycle performance.
Compared with prior art, the invention has the advantages that：
1, raw materials of the present invention are the rice husk in biological material, the feature which has yield big, at low cost；
In addition, rice husk itself simultaneously contain two kinds of essential elements of carbon and silicon, can by a kind of raw material provide two kinds needed for element.
2, preparation method is simple used in the present invention, and nonhazardous is pollution-free.
3, the silicon/carbon of nanostructure and silicon/carbon dioxide composite material being prepared respectively using the present invention as lithium from
The negative material of sub- battery, the specific capacity that electrochemical property test obtains is high, and good cycling stability has extended cycle life.
Description of the drawings
Fig. 1 is scanning electron microscopic picture of the nano-silicon/carbon composite of the preparation of embodiment 1 under different amplification；
Fig. 2 is the transmission electron microscope picture of nano-silicon/carbon composite prepared by embodiment 1；
Fig. 3 is the high-resolution-ration transmission electric-lens picture of nano-silicon/carbon composite prepared by embodiment 1；
Fig. 4 is the scanning electron microscopic picture that silicon/carbon dioxide composite material is prepared in embodiment 2~4 respectively；
Fig. 5 is the transmission electron microscope picture that silicon/carbon dioxide composite material is prepared in embodiment 2~4 respectively；
Fig. 6 is the constant current charge and discharge cycle performance and coulombic efficiency curve of battery 1；
Fig. 7 is charge-discharge performance curve of the battery 1 under different multiplying；
Fig. 8 is the constant current charge and discharge cycle performance of battery 2,3,4 and the coulombic efficiency curve of battery 4；
Fig. 9 is charge-discharge performance curve of the battery 2,3,4 under different multiplying.
Specific implementation mode
Embodiment 1
(1) by the rice husk cleaned up and magnesium powder in mass ratio 2:1 is placed in tube furnace.
(2) after leading to argon gas 3h, magnesiothermic reduction 6h, natually cooled to room temperature, heating rate at 700 DEG C in argon gas protection
For 2 DEG C/min.
(3) sample will be obtained and is placed in 12h in 0.1M hydrochloric acid, and remove the oxide of sample surfaces, centrifuge washing is dried to obtain
Silicon/carbon composite.
The scanning electron microscope (SEM) photograph of nano-silicon/carbon composite manufactured in the present embodiment is as shown in Figure 1, that surface can be seen in the figure is thick
Rough sample, and there is fine particle shape in surface sample.
The transmission electron microscope picture of nano-silicon/carbon composite manufactured in the present embodiment in figure in edge as shown in Fig. 2, can see
To there are porous structures.
The high-resolution-ration transmission electric-lens figure of nano-silicon/carbon composite manufactured in the present embodiment is as shown in figure 3, lattice fringe d
=0.232nm corresponds to (100) crystal face of Si, it was demonstrated that the silicon compound in rice husk is successfully reduced to nano silicon particles.
Embodiment 2
(1) rice husk cleaned up is placed in tube furnace.
(2) after leading to argon gas 3h, high temperature 6h, heating rate are 2 DEG C/min, natural cooling at 400 DEG C in argon gas protection
It is down to room temperature, obtains silicon/carbon dioxide composite material.
Embodiment 3~4
Preparation process and all same in embodiment 2, differ only in and carburizing temperature are replaced with to 600 DEG C and 900 DEG C respectively.
The scanning electron microscope (SEM) photographs of three kinds of nano silicon dioxide/carbon composites that embodiment 2~4 is prepared respectively as shown in figure 4,
In figure, (A), (B), (C) are respectively the scanning electron microscopic picture to sample prepared at 400 DEG C, 600 DEG C, 900 DEG C.Three width figures pair
It than observation, is increased with temperature, the grain shape that the surface formation of sample is prepared is more regular, and distribution is more uniform.Grain diameter
Within the scope of 100~150nm.
The transmission electron microscope picture for nano silicon dioxide/carbon composite that embodiment 2~4 is prepared respectively is as shown in figure 5, figure
In, (A), (B), (C) they are respectively the transmission electron microscope picture to sample prepared at 400 DEG C, 600 DEG C, 900 DEG C, transmission electron microscope picture
The property that piece is shown is consistent with scan image.
Application examples
Materials A is ground into 1h in agate mortar, weighs 40mg and with mass ratio 70:15:15 with conductive agent acetylene black and
Binder PVDF is mixed, and is dried in vacuum overnight at 80 DEG C；Pasty slurry is made later, magneton, which is added, after ultrasonic 1h is stirred overnight,
After be applied on foam copper, be dried in vacuo 12h after, tabletting.
When materials A is nano-silicon/carbon composite that embodiment 1 is prepared, the negative electrode of lithium ion battery that is prepared into
Piece is denoted as 1；
When materials A is nano silicon dioxide/carbon composite that embodiment 2 is prepared, the lithium-ion electric that is prepared into
Pond negative plate is denoted as 2；
When materials A is nano silicon dioxide/carbon composite that embodiment 3 is prepared, the lithium-ion electric that is prepared into
Pond negative plate is denoted as 3；
When materials A is nano silicon dioxide/carbon composite that embodiment 4 is prepared, the lithium-ion electric that is prepared into
Pond negative plate is denoted as 4；
Anode plate for lithium ionic cell is assembled with positive plate-lithium piece in the glove box full of argon gas respectively respectively, is obtained
CR2025 type button cells.The use of electrolyte is with LiPF6For solute, with volume ratio for 1:1:1 ethylene carbonate (EC), carbon
Dimethyl phthalate (DMC) and methyl ethyl carbonate (EMC) are solvent, the use of diaphragm are Celgard 2300.
The button cell of assembling is tested, does not test battery 1,2,3,4 respectively using battery system in constant current and not
Charge-discharge performance under same multiplying, charging/discharging voltage ranging from 0.01~3V.
Battery 1 under the constant current of 100mA/g charge-discharge performance and coulombic efficiency as shown in fig. 6, first circle charge and discharge
Specific capacity is respectively 508.56mAh/g and 852.80mAh/g, and coulombic efficiency 59.64%, after cycle 100 is enclosed, specific discharge capacity is still
510mAh/g, the coulombic efficiency after stablizing are maintained at 98% or more.Illustrate silicon/carbon composite tool that embodiment 1 is prepared
There are higher specific capacity and preferable stable cycle performance.
Charge-discharge performance of the battery 1 under different multiplying is as shown in fig. 7, in 100mA/g, 200mA/g, 500mA/g,
10 circles are recycled under the current density of 1A/g, 2A/g, 3A/g successively, finally return 100mA/g.Still there is about specific capacity when 3A/g
245mAh/g, after returning to 100mA/g, specific capacity goes back up to 670mA/g or more.
The constant current charge-discharge cycle performance of battery 2,3,4 as shown in figure 8, it can be seen from the figure that after 100 circle of cycle,
Battery 2, battery 3, battery 4, specific capacity are stablized in 385mAh/g, 525mAh/g, 616mAh/g respectively.
The comparison of charge-discharge performance of the battery 2,3,4 under different multiplying is as shown in figure 9, different temperatures is prepared
The multiplying power property of three kinds of samples be consistent with cycle performance figure.Temperature is higher, obtains what sample was tested as negative material
Specific capacity value is higher.
Claims (10)
1. a kind of preparation method of nano-silicon/carbon composite, which is characterized in that using rice husk as raw material, using magnesium powder as reducing agent,
High temperature reduction is carried out under inert gas shielding, and nano-silicon/carbon composite is prepared through one-step method；
The temperature of the high temperature reduction is 600~900 DEG C, and the time is 1~10h.
2. the preparation method of nano-silicon/carbon composite according to claim 1, which is characterized in that the rice husk and magnesium
The mass ratio of powder is 1~2:1.
3. the preparation method of nano-silicon/carbon composite according to claim 2, which is characterized in that the rice husk and magnesium
The mass ratio of powder is 2:1；
The temperature of the high temperature reduction is 700 DEG C, time 6h, and heating rate is 2 DEG C/min, and inert gas is Ar gas.
4. the preparation method of nano-silicon/carbon composite according to claim 1, which is characterized in that the rice husk makes
It need to be pre-processed before, specially：
Rice husk washs successively through water, acetone, ethyl alcohol, deionized water, for use after drying.
5. the preparation method of nano-silicon/carbon composite according to claim 1, which is characterized in that after high temperature reduction
Product also needs to be post-processed, specially：
Product is subjected to pickling, washing and drying process.
6. nano-silicon/carbon composite prepared by a kind of method according to Claims 1 to 5 any claim.
7. a kind of preparation method of nano silicon dioxide/carbon composite, which is characterized in that using rice husk as raw material, in indifferent gas
The lower carbonization of body protection obtains nano silicon dioxide/carbon composite；
The temperature of the carbonization is 400~900 DEG C, and the time is 1~10h.
8. the preparation method of nano silicon dioxide/carbon composite according to claim 7, which is characterized in that the rice
Shell needs to be pre-processed before use, specially：
Rice husk washs successively through water, acetone, ethyl alcohol, deionized water, for use after drying.
9. the preparation method of nano silicon dioxide/carbon composite according to claim 7, which is characterized in that the carbon
The time of change is 6h, and heating rate is 2 DEG C/min, and inert gas is Ar gas.
10. nano silicon dioxide/carbon composite wood prepared by a kind of method according to claim 7~9 any claim
Material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113809296A (en) * | 2021-09-08 | 2021-12-17 | 生态环境部华南环境科学研究所 | Porous silicon-carbon composite material capable of reducing carbon emission and preparation method thereof |
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| CN113809296B (en) * | 2021-09-08 | 2022-08-30 | 生态环境部华南环境科学研究所 | Porous silicon-carbon composite material and preparation thereof |
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Application publication date: 20180731 |