CN110311120A - A kind of lithium ion battery negative electrode material of SiClx containing magnesia and preparation method thereof - Google Patents
A kind of lithium ion battery negative electrode material of SiClx containing magnesia and preparation method thereof Download PDFInfo
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- CN110311120A CN110311120A CN201910621840.2A CN201910621840A CN110311120A CN 110311120 A CN110311120 A CN 110311120A CN 201910621840 A CN201910621840 A CN 201910621840A CN 110311120 A CN110311120 A CN 110311120A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
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- 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
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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 relates to lithium battery material field, specifically a kind of lithium ion battery negative electrode material of SiClx containing magnesia and preparation method thereof.It mainly include raw material preparation, magnesium silicide preparation and the preparation of the negative electrode material of SiClx containing magnesia.Preparation method in the present invention can realize batch production, be easy to industrial application, have the excellent chemical properties such as specific capacity height, good cycle using the lithium ion battery that preparation method provided by the invention obtains negative electrode material preparation.
Description
Technical field
The present invention relates to lithium battery material field, specifically a kind of lithium ion battery negative electrode material of SiClx containing magnesia
And preparation method thereof.
Background technique
As lithium ion battery is in the extensive use of the mobile electronic devices such as mobile phone, laptop and and environmental improvement
Demand to electric car is badly in need of the cathode material of lithium ion battery of exploitation high capacity at present.
Silicon based anode material is because its specific capacity with superelevation receives significant attention, and by recent two decades, people are unremitting
Research, become at present most industrialization promotion application high-capacity cathode material.Wherein, SiOx material is because in cycle life
The more practical potentiality of the advantage of aspect, therefore be also to promote and apply fastest high capacity type negative electrode material at present.SiOx material
Expect that existing greatest problem is that first charge discharge efficiency is lower, only 68%~69%, it can be mentioned by the modified first charge discharge efficiency in carbon coating surface
75%~76% is risen to, but still is not able to satisfy the demand of lithium ion battery for electric vehicle.
People determine that suitable magnesium, which is added, can promote first charge discharge efficiency by largely studying, the method for being currently fed Mg, one
Kind is that Mg metal is added while the preparation of SiOx material, incorporates magnesium in a gaseous form wherein during SiOx formation,
Such as the description of patent CN201710193442 " Si composite oxide and preparation method thereof for lithium secondary battery cathode material ";
Another main stream approach is after the production of SiOx material, before carbon coating processing, with the alkoxide or silicic acid of metal Mg or MgO and Mg
The forms such as salting liquid are added, such as CN201210553245.8 " a kind of lithium ion battery silicon oxide/carbon negative electrode material and its preparation
Method ", CN201610863902.7 " a kind of compound, preparation method and cathode and lithium ion using compound preparation
Battery ", CN201711318537 " a kind of lithium ion battery negative material and preparation method thereof ", CN201680058576 are " non-aqueous
Electrolyte secondary battery negative electrode active material, non-aqueous electrolyte secondary battery, negative electrode material for nonaqueous electrode secondary battery
Manufacturing method and non-aqueous electrolyte secondary battery manufacturing method ", CN201480027925 " the secondary electricity of nonaqueous electrolyte
Pond negative electrode material and its manufacturing method and lithium ion secondary battery " etc..
The above method the addition because of Mg cause wherein silicon crystal grain it is oversized, and process is not easy to control, causes material
Cycle performance is poor;Or the various problems such as industrialization is not easy because process is more complex, although cause plus Mg after first charge discharge efficiency have substantially
Degree is promoted, but industrial application is still not implemented because cycle performance is poor.
Summary of the invention
The present invention is intended to provide a kind of lithium ion battery negative electrode material of SiClx containing magnesia and preparation method thereof, this method can
It realizes batch production, is easy to industrial application, the lithium ion of negative electrode material preparation is obtained using preparation method provided by the invention
Battery has the excellent chemical properties such as specific capacity height, good cycle.
In order to solve the above technical problems, the technical solution adopted by the present invention are as follows: a kind of lithium ion battery, which is used, contains magnesia
The preparation method of silicium cathode material, it is characterised in that: the following steps are included:
1) silicon powder and magnesium powder, are weighed according to the mass ratio of 1:1.7-1.75;
2) inert gas shielding type mixing machine, is added in silicon powder weighed in step 1) and magnesium powder to mix, by what is mixed
Rotary funace is added in material, and rotary funace is evacuated to 0.05Pa hereinafter, being warming up to the heating speed of 10 DEG C/min
It 550-650 DEG C, is cooled to room temperature after keeping the temperature 3-5h, obtains magnesium silicide;
3) silicon monoxide powder, is weighed, the ratio of magnesium silicide obtained is 100:2-10 in silicon monoxide powder and step 2, will be weighed
To silicon monoxide powder and step 2 in magnesium silicide be added inert gas shielding type mixing machine mixed;After the completion of mixing
Material be added to CVD chemical vapor deposition stove, be evacuated to 0.05Pa after sealing hereinafter, and with the heating speed of 10 DEG C/min
After being warming up to 500 DEG C~1000 DEG C keep the temperature 1~5h, after be passed through carbon source carry out gas phase carbon coating, carbon coating amount be 3%~5%, cladding
900 DEG C~1000 DEG C of temperature;It is cooled to room temperature taking-up after the completion of carbon coating, carries out crushing and classification processing, obtains lithium ion battery
With the negative electrode material of SiClx containing magnesia.
Preferably, 99.9% or more silicon powder purity in step 1), granularity D50≤8 μm, 99.9% or more the purity of magnesium powder,
Maximum particle diameter is no more than 300 μm;The purity of silicon monoxide powder in step 3) is not less than 99.9%, granularity D50≤5 μm.
Preferably, the ratio that weighs of silicon powder and magnesium powder is 1:1.73 in step 1).
Preferably, the carbon source in step 3) is acetylene or methane.
A kind of lithium ion battery negative electrode material of SiClx containing magnesia is prepared using any one of the above preparation method.
Beneficial effect
In preparation method of the invention, magnesium elements are added in the form of magnesium silicide, rather than with gaseous metal in the prior art or
The forms such as alkoxide or silicate solutions are added, so that production process of the invention is convenient for control, it can be achieved that batch production, is easy to produce
Industry application.
The magnesium in the negative electrode material of SiClx containing magnesia prepared through the invention exists in the form of magnesium silicide, after carbon coating
It will not lead to the oversized of silicon crystal grain because of the addition of magnesium, silicon crystal grain is closely sized to conventional SiOx negative electrode material, for circulation
Performance influences little.In addition, the capacity for the first time and capacity retention ratio of the lithium battery of negative electrode material preparation through the invention all connect
It is bordering on the lithium battery of routine SiOx preparation in the prior art, but is greatly improved in first charge discharge efficiency.To make life of the present invention
The negative electrode material of production becomes at present the lithium ion battery high-capacity cathode material of most industrialization prospect.
Specific embodiment
Cathode material preparation method of the invention is described in detail below by way of three embodiments.
The preparation method of the lithium ion battery of embodiment one negative electrode material of SiClx containing magnesia, it is characterised in that: including with
Lower step:
1) silicon powder and magnesium powder, are weighed according to the mass ratio of 1:1.7, wherein 99.9% or more silicon powder purity, granularity D50≤8 μm,
99.9% or more the purity of magnesium powder, maximum particle diameter are no more than 300 μm.
2) inert gas shielding type mixing machine, is added in silicon powder weighed in step 1) and magnesium powder to mix, will be mixed
Rotary funace is added in good material, and rotary funace is evacuated to 0.05Pa hereinafter, heating up with the heating speed of 10 DEG C/min
To 550 DEG C, it is cooled to room temperature after keeping the temperature 3h, obtains magnesium silicide;
3) silicon monoxide powder, is weighed, purity is not less than 99.9%, granularity D50≤5 μm.It is made in silicon monoxide powder and step 2
Magnesium silicide ratio be 100:2, by the silicon monoxide powder and step 2 that weigh magnesium silicide be added inert gas shielding
Type mixing machine is mixed;Material after the completion of mixing is added to CVD chemical vapor deposition stove, is evacuated to after sealing
0.05Pa hereinafter, and keep the temperature 1h after being warming up to 500 DEG C DEG C with the heating speed of 10 DEG C/min, after be passed through carbon source and carry out gas-phase carbon packet
It covers, carbon source is acetylene, and carbon coating amount is 3%%, 900 DEG C of temperature of plate;It is cooled to room temperature taking-up after the completion of carbon coating, is crushed
Classification processing, obtains the lithium ion battery negative electrode material of SiClx containing magnesia of embodiment one.
The preparation method of the lithium ion battery of embodiment two negative electrode material of SiClx containing magnesia, it is characterised in that: including with
Lower step:
1) silicon powder and magnesium powder, are weighed according to the mass ratio of 1:1.73, wherein 99.9% or more silicon powder purity, granularity D50≤8 μm,
99.9% or more the purity of magnesium powder, maximum particle diameter are no more than 300 μm.
2) inert gas shielding type mixing machine, is added in silicon powder weighed in step 1) and magnesium powder to mix, will be mixed
Rotary funace is added in good material, and rotary funace is evacuated to 0.05Pa hereinafter, heating up with the heating speed of 10 DEG C/min
To 600 DEG C, it is cooled to room temperature after keeping the temperature 4h, obtains magnesium silicide;
3) silicon monoxide powder, is weighed, purity is not less than 99.9%, and granularity D50≤5 μm, silicon monoxide powder is made with step 2
Magnesium silicide ratio be 100:6.Inert gas shielding is added in magnesium silicide in the silicon monoxide powder and step 2 that weigh
Type mixing machine is mixed;Material after the completion of mixing is added to CVD chemical vapor deposition stove, is evacuated to after sealing
0.05Pa hereinafter, and keep the temperature 3h after being warming up to 700 DEG C with the heating speed of 10 DEG C/min, after be passed through carbon source and carry out gas-phase carbon packet
It covers, carbon source is acetylene or methane.Carbon coating amount 4%, 950 DEG C of temperature of plate;It is cooled to room temperature taking-up after the completion of carbon coating, is carried out
Crushing and classification processing, obtains the lithium ion battery negative electrode material of SiClx containing magnesia of embodiment two.
The preparation method of the lithium ion battery of embodiment three negative electrode material of SiClx containing magnesia, it is characterised in that: including with
Lower step:
1) silicon powder and magnesium powder, are weighed according to the mass ratio of 1:1.75, wherein 99.9% or more silicon powder purity, the μ of granularity D50≤8
M, 99.9% or more the purity of magnesium powder, maximum particle diameter are no more than 300 μm.
2) inert gas shielding type mixing machine, is added in silicon powder weighed in step 1) and magnesium powder to mix, will be mixed
Rotary funace is added in good material, and rotary funace is evacuated to 0.05Pa hereinafter, heating up with the heating speed of 10 DEG C/min
To 650 DEG C, it is cooled to room temperature after keeping the temperature 3-5h, obtains magnesium silicide;
3) silicon monoxide powder, is weighed, purity is not less than 99.9%, and granularity D50≤5 μm, silicon monoxide powder is made with step 2
Magnesium silicide ratio be 100:10.Inert gas shielding is added in magnesium silicide in the silicon monoxide powder and step 2 that weigh
Type mixing machine is mixed;Material after the completion of mixing is added to CVD chemical vapor deposition stove, is evacuated to after sealing
0.05Pa hereinafter, and keep the temperature 5h after being warming up to 1000 DEG C with the heating speed of 10 DEG C/min, after be passed through carbon source and carry out gas-phase carbon packet
It covers, carbon source is methane.Carbon coating amount be 5%, 1000 DEG C of temperature of plate;It is cooled to room temperature taking-up after the completion of carbon coating, is crushed
Classification processing, obtains the lithium ion battery negative electrode material of SiClx containing magnesia of embodiment three.
Otide containing lighium silicium cathode material prepared by above three embodiments is normal by comparative test and in the prior art
Rule SiOx negative electrode material compares, material characterization method:
(1) characterizing method of the Si microcrystalline grain size of material is using X-ray diffractometer, is 10 ° to 2-Theta range
~90 ° are scanned, and are then 26 °~30 ° to 2-Theta range and are fitted to obtain the half-peak breadth at Si (111) peak, using thanking
Si microcrystalline grain size is calculated in happy formula.
(2) capacity for the first time of material and first charge discharge efficiency test are characterized using button cell, are lithium metal to electrode
Piece, charge-discharge magnification are 0 .1C, and charging/discharging voltage range is the .5V of 0 .005V~1.
(3) the cycle performance use of material is characterized with the mixed button cell of graphite, with graphite by material according to
Material of the present invention: after the mixing of graphite=1:9 (mass ratio) ratio, pole piece is made in coating on copper foil, using metal lithium sheet as to electricity
Pole is assembled into button cell.
The ratio of the charging capacity that (4) 50 weeks capacity retention ratios are the 50th week and the 1st week charging capacity.
The experimental results are shown inthe following table:
As seen from the above table, the negative electrode material and comparative example prepared through the invention Si microcrystalline grain size, for the first time capacity and
It is not much different in terms of 50 weeks capacity retention ratios, but is greatly improved in first charge discharge efficiency, and preparation method of the invention can batch
Industrialization production, and then the lithium ion battery that negative electrode material produced by the invention can be made to become at present most industrialization prospect is used
High-capacity cathode material.
Claims (5)
1. a kind of lithium ion battery preparation method of the negative electrode material of SiClx containing magnesia, it is characterised in that: the following steps are included:
1) silicon powder and magnesium powder, are weighed according to the mass ratio of 1:1.7-1.75;
2) inert gas shielding type mixing machine, is added in silicon powder weighed in step 1) and magnesium powder to mix, by what is mixed
Rotary funace is added in material, and rotary funace is evacuated to 0.05Pa hereinafter, being warming up to the heating speed of 10 DEG C/min
It 550-650 DEG C, is cooled to room temperature after keeping the temperature 3-5h, obtains magnesium silicide;
3) silicon monoxide powder, is weighed, the ratio of magnesium silicide obtained is 100:2-10 in silicon monoxide powder and step 2, will be weighed
To silicon monoxide powder and step 2 in magnesium silicide be added inert gas shielding type mixing machine mixed;After the completion of mixing
Material be added to CVD chemical vapor deposition stove, be evacuated to 0.05Pa after sealing hereinafter, and with the heating speed of 10 DEG C/min
After being warming up to 500 DEG C~1000 DEG C keep the temperature 1~5h, after be passed through carbon source carry out gas phase carbon coating, carbon coating amount be 3%~5%, cladding
900 DEG C~1000 DEG C of temperature;It is cooled to room temperature taking-up after the completion of carbon coating, carries out crushing and classification processing, obtains lithium ion battery
With the negative electrode material of SiClx containing magnesia.
2. a kind of preparation method of the lithium ion battery according to claim 1 with the negative electrode material of SiClx containing magnesia, feature
Be: 99.9% or more silicon powder purity in step 1), granularity D50≤8 μm, 99.9% or more the purity of magnesium powder, maximum particle diameter is not
More than 300 μm;The purity of silicon monoxide powder in step 3) is not less than 99.9%, granularity D50≤5 μm.
3. a kind of preparation method of the lithium ion battery according to claim 1 with the negative electrode material of SiClx containing magnesia, feature
Be: the ratio that weighs of silicon powder and magnesium powder is 1:1.73 in step 1).
4. a kind of preparation method of the lithium ion battery according to claim 1 with the negative electrode material of SiClx containing magnesia, feature
Be: the carbon source in step 3) is acetylene or methane.
5. a kind of lithium ion battery negative electrode material of SiClx containing magnesia, it is characterised in that: using any one in claim 1-4
Kind preparation method preparation.
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Cited By (8)
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CN111029538A (en) * | 2019-10-31 | 2020-04-17 | 合肥国轩高科动力能源有限公司 | Carbon-coated silicon composite silicate material and preparation method and application thereof |
CN111342030A (en) * | 2020-03-28 | 2020-06-26 | 兰溪致德新能源材料有限公司 | Multi-element composite high-first-efficiency lithium battery negative electrode material and preparation method thereof |
CN112186145A (en) * | 2020-09-08 | 2021-01-05 | 合肥国轩高科动力能源有限公司 | Magnesium reduced carbon coated silica material and preparation method and application thereof |
CN113471440A (en) * | 2021-07-09 | 2021-10-01 | 惠州亿纬锂能股份有限公司 | Silica material, preparation method and application thereof |
CN113735572A (en) * | 2021-08-24 | 2021-12-03 | 王立卓 | Preparation method of magnesium-containing silicon monoxide |
CN113764651A (en) * | 2021-08-24 | 2021-12-07 | 复旦大学 | High-capacity lithium ion battery negative electrode active material, negative electrode plate and lithium ion battery |
CN114122341A (en) * | 2020-08-31 | 2022-03-01 | 贝特瑞新材料集团股份有限公司 | Silicon-based composite material, preparation method thereof and lithium ion battery |
CN114497484A (en) * | 2022-01-04 | 2022-05-13 | 广东东岛新能源股份有限公司 | Silica-based composite anode material and preparation method thereof |
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CN111029538A (en) * | 2019-10-31 | 2020-04-17 | 合肥国轩高科动力能源有限公司 | Carbon-coated silicon composite silicate material and preparation method and application thereof |
CN111029538B (en) * | 2019-10-31 | 2022-05-10 | 合肥国轩高科动力能源有限公司 | Carbon-coated silicon composite silicate material and preparation method and application thereof |
CN111342030A (en) * | 2020-03-28 | 2020-06-26 | 兰溪致德新能源材料有限公司 | Multi-element composite high-first-efficiency lithium battery negative electrode material and preparation method thereof |
CN111342030B (en) * | 2020-03-28 | 2022-03-15 | 兰溪致德新能源材料有限公司 | Multi-element composite high-first-efficiency lithium battery negative electrode material and preparation method thereof |
CN114122341A (en) * | 2020-08-31 | 2022-03-01 | 贝特瑞新材料集团股份有限公司 | Silicon-based composite material, preparation method thereof and lithium ion battery |
CN112186145A (en) * | 2020-09-08 | 2021-01-05 | 合肥国轩高科动力能源有限公司 | Magnesium reduced carbon coated silica material and preparation method and application thereof |
CN112186145B (en) * | 2020-09-08 | 2022-06-07 | 合肥国轩高科动力能源有限公司 | Magnesium reduced carbon coated silica material and preparation method and application thereof |
CN113471440A (en) * | 2021-07-09 | 2021-10-01 | 惠州亿纬锂能股份有限公司 | Silica material, preparation method and application thereof |
CN113735572A (en) * | 2021-08-24 | 2021-12-03 | 王立卓 | Preparation method of magnesium-containing silicon monoxide |
CN113764651A (en) * | 2021-08-24 | 2021-12-07 | 复旦大学 | High-capacity lithium ion battery negative electrode active material, negative electrode plate and lithium ion battery |
CN113735572B (en) * | 2021-08-24 | 2022-11-08 | 王立卓 | Preparation method of magnesium-containing silicon monoxide |
CN114497484A (en) * | 2022-01-04 | 2022-05-13 | 广东东岛新能源股份有限公司 | Silica-based composite anode material and preparation method thereof |
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CN110311120B (en) | 2022-02-08 |
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