CN106486658A - A kind of solid phase reaction prepares the method for silicon nano material and its application - Google Patents
A kind of solid phase reaction prepares the method for silicon nano material and its application Download PDFInfo
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- CN106486658A CN106486658A CN201510551123.9A CN201510551123A CN106486658A CN 106486658 A CN106486658 A CN 106486658A CN 201510551123 A CN201510551123 A CN 201510551123A CN 106486658 A CN106486658 A CN 106486658A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- 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 provides method and its application that a kind of solid phase prepares silicon nano power.Specifically in a mild condition, with micron order silica flour and Si oxide as silicon source, silicon/metal alloy is prepared with micron order silica flour with metal or its alloy reaction first, then silicon nano power is synthesized with Si oxide.The present invention can cause the reaction thoroughly to carry out by controlling ratio between Si oxide and silicon/metal alloy under appropriate reaction temperature and reaction time, it is not necessary to using the hydrofluoric acid reagent of severe toxicity, while can achieve magnanimity to prepare nano silicon material.
Description
Technical field
The present invention relates to the preparation of silicon nano power and application, prepare the process of high performance silicon nano powder more particularly to a kind of Si oxide and silicon/metal alloy reaction, prepared silicon nano power can be used as lithium ion battery negative material.
Background technology
Based on important application on function electronic equipment, the preparation of silicon nano material causes extensive concern.Meanwhile, silicon nano material is due to high theoretical capacity in lithium ion battery applications（～4200
mAh g-1）With low discharge potential (<0.5 V, Li/Li+) it is considered as the material for replacing traditional negative pole best.
Traditionally, silicon materials are mainly prepared using solid phase reduction silica.For example higher than 2000 DEG C carbon thermal reduction silica (document 1, Nagamori, M.,
Malinsky, I. &Claveau, A. Metall.Trans. B17,503–514 (1986))；Magnesiothermic reduction when 650 DEG C（Document 2, Bao Z,
Weatherspoon M R, Shian S, et al., Nature, 446: 172-175,(2007)）With more than electrochemical reduction (document 3, Cho S K, the Fan F R under the conditions of 850 DEG C
F, Bard A J., AngewandteChemie, 124: 12912-12916 (2012)).In the recent period, in order to synthesize the nano silicon material that can apply to lithium cell cathode material, substantial amounts of synthetic method is developed.For example, by chemical vapour deposition technique, it is 3 in pressure
400 DEG C of pyrolysis SiH4/H2 in the reactor of Torr（50%）And PH3/H2（100ppm）Gaseous mixture, and prepare silicon nanowires under auxiliary of the Woelm Alumina for template, the nano wire illustrates long cycle life（After 1100 circle charge and discharge circulations, capacity is 1029 mAh/g）With high high rate performance（Under 10 multiplying powers, capacity is～956 mAh g-1）（Document 4, Cho J H, Picraux
S T. Nano letters, 13: 5740-5747（2013））.Silicon nano material better performances prepared by this technology, but method is expensive.For silicon nano material preparation in organic solvent, Heath et al. method that sodium reduction silicon tetrachloride prepared silicon nanocluster in organic phase in reported first in 1992, the method need in the steel bomb 385 DEG C to react 3 to 7 days（Document 5, Heath J R.,
Science, 258: 1131-1133 (1992)）.Subsequently, Jaephil Cho et al. has synthesized nano silicon particles using similar preparation method, and the particle presents high charging capacity after further carbon coating（3535 mAh g-1）And capacity keeps 96% after circulating 40 circles（Document 6, Kim H, Seo M,
Park M H, et al. Angew. Chem. Inter. Ed., 49: 2146-2149 (2010)）.In the recent period, the molten salt system that Yitai Qian et al. sets up reduces silicon tetrachloride under cryogenic to prepare nano silicon particles, in 3A
Under the current density of g-1, circulation 500 is enclosed capacity and keeps 1183mAh
g-1.（Document 7, N.
Lin, Y. Han, L. B. Wang, J. B. Zhou, J. Zhou, Y. C. Zhu and Y. T. Qian, Angew.
Chem. Int. Ed., 54：3822-3825（2015））Brian A. Korgel et al. is prepared for silicon nanowires by pyrolysis phenylsilane in organic phase at 490 DEG C, and after carbon coating is carried out further, after 30 circle of silicon nanowires circulation, reversible capacity still reaches 1500 mAh g-1（Document 8, Chan C K, Patel R N, O ' Connell
M J, et al., ACS nano, 4: 1443-1450 (2010)）.Takeshi
The magnesium in the bismuth metal of melting in removal silication magnesium alloy such as Wada to prepare porous silica material, under the current density of 1A g-1, enclose, and capacity keeps 100%. by 1000 mAh g-1 charge and discharge cycles 1500 of constant volume amount（Document 9, T. Wada, T. Ichitsubo, K. Yubuta, H. Segawa, H. Yoshida,
H. Kato,NanoLett., 14: 4505-4510(2014)）Compared with above method, the reaction of the present invention needs raw material cheap, does not use harmfulness reagent such as hydrofluoric acid, simple to operate and yield is high.In the method for preparing nano-silicon negative material that is reported at present, problem encountered mainly has equipment cost high, and gross production rate is relatively low, and reaction raw materials are expensive, it is desirable to have malicious reagent such as silane, hydrofluoric acid etc..Therefore, develop the eco-friendly synthetic method of silicon nano power, the scale to silicon nano material is prepared and silicon is significant as the practical application of high-performance lithium ion negative material.
Content of the invention
The application provides a kind of method of synthesis silicon nano power, as ion cathode material lithium, with excellent chemical property.Documents report that required raw material is cheap, and preparation flow environmental protection, yield are higher, low production cost, produces beneficial to amplifying.Therefore, it is an object of the invention to provide a kind of method for simply efficiently preparing high performance silicon nano material.Silicon/metal alloy is prepared using low-cost commercialization micron order silica flour and commercialization metal reaction, then nano silicon material is prepared by the reaction with Si oxide.The silicon nano power body is applied to lithium cell negative pole energy effectively solving silicon as the actual application problem of high-performance lithium ion negative material.
The first aspect of the invention provides a kind of method for preparing silicon nano power, and methods described comprises the steps.
1) by micron order silica flour and metal ball milling mixing under the conditions of vacuum or inert gas shielding, calcine under the conditions of vacuum or inert gas shielding, obtain silicon/metal alloy.
2) by step 1）Silicon/the metal alloy of acquisition is heated with Si oxide after ball milling mixing under the conditions of vacuum or inert gas shielding under the conditions of vacuum or inert gas shielding.
Wherein described inert gas includes the gas not with raw material reaction such as argon gas, hydrogen and argon hydrogen gaseous mixture；Metal is selected from lithium, sodium, magnesium, aluminium or its respective alloy or its combination；Si oxide includes the mixture containing Si oxide such as silicon monoxide, silica and silicon powder, diatomite, soil.
In a preferred embodiment, in step 2）Also include the step of washing, diluting salt pickling, removal of impurities, filtration and/or drying afterwards.
In a preferred embodiment, the metal is magnesium, and Si oxide is silicon powder.
In a preferred embodiment, step 1）Middle magnesium is 2.1 with the mol ratio of micron order silica flour:1.
In a preferred embodiment, step 1）Middle Ball-milling Time is preferably 3 hours；Rotational speed of ball-mill is preferably 250 to 350 rpms；Ball milling pearl and material quality ratio preferably 15:1 to 25:1.
In a preferred embodiment, step 1）In calcining heat be preferably 700 degrees Celsius.
In a preferred embodiment, step 1）In calcination time be 5 to 10 hours.
In a preferred embodiment, step 2）Middle silicon/metal alloy is 1.1 with Si oxide mol ratio:1.
In a preferred embodiment, step 2）Middle Ball-milling Time is preferably 3 hours；Rotational speed of ball-mill is preferably 250 to 350 rpms；Ball milling pearl and material quality ratio preferably 15 to 25.
In a preferred embodiment, step 2）In heating-up temperature be preferably 650 to 900 degrees Celsius.
In a preferred embodiment, step 2）In heat time be preferably 9 to 13 hours.
The second aspect of the invention provide the present invention the on one side described in the silicon nano power for preparing of method.
The third aspect of the invention provides purposes of the silicon nano power described in second aspect of the present invention as lithium ion battery negative material.
Specifically, the technical scheme is that：
A kind of method that Si oxide prepares silicon nano power with silicon/metal alloy reaction, in a mild condition, with cheap commercialization micron order silica flour and Si oxide as silicon source, silicon/metal alloy is prepared through silica flour with metal or its alloy reaction, then silicon nano power is synthesized through Si oxide and silicon/metal alloy；It is characterized in that, reaction using Si oxide silica/metal alloy, be initial silicon source from cheap commodity micron order silica flour and Si oxide, silicon/metal alloy is prepared through silica flour with metal or its alloy reaction, then nano-silicon is prepared by Si oxide silica/metal alloy.The serial reaction can cause the reaction thoroughly to carry out by control silicon/metal alloy and the ratio of Si oxide under appropriate reaction temperature and reaction time, it is to avoid using the hydrofluoric acid reagent of severe toxicity, accessory substance such as magnesia is readily washed off.Two kinds of raw materials all can generate silicon, prepare silicon nano material compared to magnesiothermic reduction, greatly save the consumption of magnesium, it is possible to achieve more preferable economic worth.As preparation process is simple, it is easy to amplify production, achievable magnanimity prepares nano silicon material.
Raw material is as follows：Silicon source, selected from micron order silica flour and the technical grade Si oxide of commercialization.
Metal, from one or more in lithium, sodium, magnesium, aluminium, or its corresponding metal alloy；Si oxide includes：The mixture containing Si oxide such as silicon monoxide, silica and silicon powder, diatomite, soil.
Comprise the following steps that：A, above-mentioned silica flour is mixed by equivalent proportion with metal, 5-25 hours are calcined at 500 to 1000 degrees Celsius in argon hydrogen shield, prepare corresponding silicon/metal alloy.
B, the silicon/metal alloy of above-mentioned preparation and Si oxide are blended in argon atmosphere or isolation air under conditions of be heated to 650 to 900 degrees Celsius, keep 1 hour to 3 days.Question response terminates, and through washing, diluting salt pickling, after removing impurity, filtration drying obtains the silicon nano power body of pure phase to head product.
Silicon nano power prepared by segmentation scheme described in the inventive method can reach the yield of 95% even more high.
Preferably, the metal selects magnesium powder, and Si oxide selects silicon powder；Preferably, magnesium metal is Mg with the mol ratio of silica flour:Si=2.1:1；Preferably, magnesium silicide is Mg2Si with the mol ratio of silicon powder:Silicon powder=1.1:1；Preferably, the reaction time is 10 to 30 hours；Preferably, reaction temperature is 500 to 700 degrees Celsius.
The reaction can apply to carry out in vacuum drying oven or the stove with inert gas protection device.
Described silicon nano power body has preferable loose structure, the micro-nano structure of mostly even mesoporous shape.
The silicon nano power body can be assembled into lithium ion battery as negative pole, when the powder is used for lithium ion battery negative material, show the cyclical stability of higher lithium storage content, high coulombic efficiency and length.
The cyclical stability of the high lithium storage content of lithium ion battery and length be by the structures shape of the material, wherein nano silicon particles contribute high lithium storage content, and the micro-nano structure of even mesoporous shape is that silicon grain provides volumetric expansion and the space that shrinks and lithium ion transport passage.
The present invention has the advantages that：
Compared with the technology such as existing carbon heat, magnesiothermic reduction silica, the present invention achieves the preparation of nano-silicon under the conditions of relatively mild, while improve the utilization rate of magnesium, reducing preparation cost, and the hydrofluoric acid reagent without using severe toxicity, and yield is higher；Compared with the technology such as existing reduction silicon tetrachloride, the present invention is relatively low to equipment requirement, materials safety, simple to operate；Compared with the technology such as existing organic liquid phase reduction, raw material of the present invention is cheap nontoxic.
The initial silicon source of the present invention is from multiple cheap commercialization micron order silica flours, Si oxide；Metal, such as magnesium powder, preparation flow environmental protection, produce beneficial to amplifying.
The inventive method obtain silica flour be nano-structured particles, with preferable pattern, particle be the micro-nano structure size range of even mesoporous shape in 25～100nm, aperture is mainly distributed as 10-30 nm.
Silicon nanoparticle material prepared by the present invention, during for lithium ion battery negative, shows the lithium storage content far above graphite cathode.
The silicon nano power of present invention synthesis is compound with carbon to be assembled into lithium ion battery as negative pole, and its lithium storage content can be higher than 1000mAh/g, and capacity is graphite negative electrodes（372mAh/g）As many as nearly 3 times, and with longer cycle life.
Description of the drawings
Fig. 1 is the X-ray diffraction pattern of the product that embodiment 1 is obtained.
Fig. 2 is the scanning electron microscope (SEM) photograph of the product that embodiment 1 is obtained.
Fig. 3 is the X-ray diffraction pattern of the product that embodiment 2 is obtained.
Fig. 4 is the scanning electron microscope (SEM) photograph of the product that embodiment 2 is obtained.
The transmission electron microscope picture of the product that Fig. 5 embodiment 2 is obtained.
Fig. 6 is charge and discharge cycles figure of the silicon nano power body that obtains of embodiment 2 when current density is for 0.1C.
Fig. 7 is charge and discharge cycles figure of the silicon nano power body that obtains of embodiment 2 when current density is for 1C.
Specific embodiment
Technical scheme is clearly and detailedly described with reference to embodiment.It is understood that described embodiment is only the part of the present invention, rather than whole embodiment.Based on the embodiment in the present invention, the every other embodiment obtained under the premise of creative work is not made by the technical work personnel of this area.Belong to protection scope of the present invention.
The chemical reagent adopted in the embodiment of the present invention is purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
Embodiment 1 ：Magnesium silicide is prepared as raw material with metal magnesium powder and silica flour
Take 28g silica flour mix with 50g metal magnesium powder after, under the protection atmosphere of argon gas load 1.5L stainless steel cauldron in.Stainless steel cauldron is put in electric furnace 700 degrees Celsius are heated to, and kept for 10 hours.
Using X light powder diffraction instrument（Philips X’ Pert Super diffract meter）X light diffracting analysis are carried out, Fig. 1 is the x-ray diffraction spectrum of the embodiment gained powder.As seen from the figure, in x-ray diffraction spectra, 2 θ have apparent diffraction maximum in the range of 10-80 °, and all diffraction maximums all can the index Mg that is cube2Si
(JCPDS NO. 34-0458).Program yield is more than 95%.
The scanning electron microscope (SEM) photograph of product（Fig. 2）Show structure of the product for submicron order.
Embodiment 2 ：Silicon nano power is prepared from magnesium silicide
Magnesium silicide 21g prepared by Example 1 is uniform with 15g silicon powder mixed grinding, is put in ventable stainless steel cauldron, and connection argon gas is simultaneously followed bad.The stainless steel kettle is put in electric furnace and is heated to 650 degrees Celsius of holding 10h.Sample is taken out after natural cooling, through pickling, after washing, be put in 50 degrees Celsius of drying in vacuum drying oven.Program yield is more than 95%.
Fig. 3 is the x-ray diffraction spectrum of the embodiment gained powder.Spectrogram shows the powder for pure silicon phase (JPCDS 77-2111).
Fig. 4 is the scanning electron microscope (SEM) photograph of the embodiment gained powder, shows the powder for micron-sized nanoparticle agglomerates body.
Fig. 5 is the transmission electron microscope picture of the embodiment gained powder, shows that prepared nanoparticle agglomerates body has pore passage structure, and pore size is 10 nanometers to 30 nanometers.The particle size distribution of powder is 25 nanometers to 100 nanometers.
Embodiment 3 ：The application in the battery of obtained silicon nano power
Product in above-described embodiment 2 is dressed up CR2016 button cell respectively（Shenzhen Poxon Machinery Technology Co., Ltd.）, with lithium piece be to electrode, polyolefin porous membrane (Celgard
2500) it is barrier film, with the ethylene carbonate of LiPF6（EC）And dimethyl carbonate（DMC）（Volume ratio 1:1）Mixed solution as electrolyte, CR2016 battery is completed in the glove box of argon gas atmosphere.Silicon electrode is mixed using the silicon nano power body in the embodiment of 60 wt%, the sodium carboxymethylcellulose adhesive of 20 wt%, 20% conductive black, water, and the substrate of electrode film is metal copper foil.It is to carry out electric performance test at 25 DEG C in test temperature.Fig. 6-7 is the electrochemical lithium storage performance map of the silicon nano power body of 2 gained of above-described embodiment.As illustrated, circulating under the current density of 0.1C, after 94 circles, reversible specific capacity is 2050mAh/g, and circulation 1550 under the current density of 1C is enclosed, and reversible specific capacity keeps 1020 mAh/g.
As a result show, the present invention can be raw material using cheap commodity silica flour and Si oxide, prepare silicon/metal alloy through silica flour with metal or its alloy reaction, then prepare nano-silicon by Si oxide silica/metal alloy.By controlling reaction temperature, the factor such as reaction time, yield is improved.When this material is used for lithium ion battery negative material, lithium storage content and the preferable cyclical stability far above graphite cathode is shown, can be used as potential next generation's high performance lithium ionic cell cathode material.
Claims (10)
1. a kind of method for preparing silicon nano power, methods described comprise the steps：
By micron order silica flour and metal ball milling mixing under the conditions of vacuum or inert gas shielding, calcine under the conditions of vacuum or inert gas shielding, obtain silicon/metal alloy；
By step 1）Silicon/the metal alloy of acquisition is heated with Si oxide after vacuum or inert gas shielding condition ball milling mixing are uniform under the conditions of vacuum or inert gas shielding；
Wherein described inert gas includes the gas not with raw material reaction such as argon gas, hydrogen and argon hydrogen gaseous mixture；Metal is selected from lithium, sodium, magnesium, aluminium or its respective alloy or its combination；Si oxide includes the mixture containing Si oxide such as silicon monoxide, silica and silicon powder, diatomite, soil.
2. method according to claim 1, wherein in step 2）Also include the step of washing, diluting salt pickling, removal of impurities, filtration and/or drying afterwards.
3. method according to claim 1, wherein described inert gas are argon hydrogen gaseous mixture, and metal is magnesium, and Si oxide is silicon powder.
4. method according to claim 1, wherein Ball-milling Time are 1 to 240 hours；During ball milling, rotating speed is 100 to 2000 rpms；Ball milling pearl is 1 with material quality ratio:50 to 50:1.
5. method according to claim 1, wherein step 1）Calcining heat is 500 to 1200 degrees Celsius；Calcination time is 5 to 240 hours.
6. method according to claim 3, wherein step 1）Middle magnesium is 1 with the mol ratio of micron order silica flour:1 to 4:1.
7. method according to claim 1, wherein step 2）Middle silicon/metal alloy is 1 with silicon powder mol ratio:2 to 2:1.
8. method according to claim 1, wherein step 2）Heating-up temperature is 650 to 1200 degrees Celsius；Heat time is 1 to 120 hours.
9. the silicon nano power that prepared by the method according to any one of claim 1-8.
10. silicon nano power according to claim 9 is used as the purposes of lithium ion battery negative material.
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| CN107086294A (en) * | 2017-04-24 | 2017-08-22 | 广东烛光新能源科技有限公司 | A kind of preparation method of nano silica-base material |
| CN107093737A (en) * | 2017-04-24 | 2017-08-25 | 广东烛光新能源科技有限公司 | A kind of preparation method of nano silica-base material |
| CN110311120A (en) * | 2019-07-10 | 2019-10-08 | 洛阳联创锂能科技有限公司 | A kind of lithium ion battery negative electrode material of SiClx containing magnesia and preparation method thereof |
| CN111477849A (en) * | 2020-04-14 | 2020-07-31 | 厦门理工学院 | Preparation method of porous Si/SiC/C material and negative electrode material |
| CN112599778A (en) * | 2020-12-15 | 2021-04-02 | 广东凯金新能源科技股份有限公司 | Silicon-carbon-based negative electrode material and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107093737B (en) * | 2017-04-24 | 2019-11-05 | 广东烛光新能源科技有限公司 | A kind of preparation method of nano silica-base material |
| CN110311120A (en) * | 2019-07-10 | 2019-10-08 | 洛阳联创锂能科技有限公司 | A kind of lithium ion battery negative electrode material of SiClx containing magnesia and preparation method thereof |
| CN110311120B (en) * | 2019-07-10 | 2022-02-08 | 洛阳联创锂能科技有限公司 | Magnesium-containing silicon oxide negative electrode material for lithium ion battery and preparation method thereof |
| CN111477849A (en) * | 2020-04-14 | 2020-07-31 | 厦门理工学院 | Preparation method of porous Si/SiC/C material and negative electrode material |
| CN111477849B (en) * | 2020-04-14 | 2021-08-17 | 厦门理工学院 | Preparation method of porous Si/SiC/C material and negative electrode material |
| CN112599778A (en) * | 2020-12-15 | 2021-04-02 | 广东凯金新能源科技股份有限公司 | Silicon-carbon-based negative electrode material and preparation method thereof |
| CN112599778B (en) * | 2020-12-15 | 2022-04-01 | 广东凯金新能源科技股份有限公司 | Silicon-carbon-based negative electrode material and preparation method thereof |
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