CN103165871B - A kind of lithium ion battery and negative material thereof, and preparation method thereof - Google Patents
A kind of lithium ion battery and negative material thereof, and preparation method thereof Download PDFInfo
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- CN103165871B CN103165871B CN201110415096.4A CN201110415096A CN103165871B CN 103165871 B CN103165871 B CN 103165871B CN 201110415096 A CN201110415096 A CN 201110415096A CN 103165871 B CN103165871 B CN 103165871B
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Abstract
The invention discloses a kind of lithium ion battery cathode material and its preparation method, it comprises the following steps: (1) under the effect of catalyst, by containing hydrogen silicone oil, cross-linking agent and MgB2Mixing, carries out cross-linking and curing reaction under an inert atmosphere, cured product is crushed to mean diameter D50It it is 12 ��m-18 ��m; Described MgB2Consumption is described containing hydrogen silicone oil and the 5wt%-8wt% of cross-linking agent gross mass; (2) cured product described in roasting in an inert atmosphere, to obtain final product. The invention also discloses and a kind of adopt this lithium ion battery negative material as the lithium ion battery of negative pole. The lithium ion battery negative material technique of the present invention is simple, and the specific capacity of the lithium ion battery negative material prepared is high, good cycling stability.
Description
Technical field
The present invention relates to battery electrode material field, particularly relate to a kind of lithium ion battery cathode material and its preparation method, the invention still further relates to a kind of lithium ion battery containing this negative material.
Background technology
In order to meet the electronic equipment requirement to lithium ion battery high-energy-density, high-specific-power, it is necessary to explore novel high-capacity electrode material. What the research of current non-carbons negative pole was more has the materials such as tinbase, antimonio and silicon-base alloy, and wherein silicon is owing to having bigger theoretical capacity (4200mAh g-1) and attract wide attention. The same with other alloy materials, irreversible capacity loss is big, cycle performance is poor shortcoming that silicon currently also exists first as negative material, its reason be mainly silicon with the alloying of lithium, removal alloying process in bigger change in volume, reduce the electrical contact of material, even make active material come off from matrix and cause losing efficacy. In order to make silica-base material practical early, scholars studies from all many-sides and improves its chemical property.
Some glass with lithium ion conduction performance or pottery also can as the compound parent of silicon to cushion its bulk effect. Such as, Chinese Academy of Sciences's silicate institute synthesizes silica-based containing lithium glass state oxide composite, the preparation of this material is undertaken in two steps: to aoxidize sub-silicon for presoma, lithium metal is as reducing agent, wet method high-energy-milling in-situ reducing is adopted to prepare different from lithium phase composite materials, and by this intermedium further with glassy oxide and conduct electricity and equal carry out compound, prepare glassy state composite negative pole material. But, siliceous glass or ceramic applications are in lithium cell cathode material, and it is still in urgent need to be improved in electrode process and cycle life etc.
Summary of the invention
The technical problem to be solved is the shortcoming in order to overcome existing siliceous combination electrode material cyclical stability difference, it is provided that a kind of lithium ion battery cathode material and its preparation method, and a kind of lithium ion battery containing this negative material. The lithium ion battery negative material technique of the present invention is simple, and the specific capacity of the lithium ion battery negative material prepared is high, good cycling stability.
The present invention solves above-mentioned technical problem by the following technical programs.
The preparation method that the invention provides a kind of lithium ion battery negative material, it comprises the following steps:
(1) by containing hydrogen silicone oil, cross-linking agent and MgB2Mixing, under the effect of catalyst, carries out the cross-linking and curing reaction of described containing hydrogen silicone oil under an inert atmosphere, cured product is crushed to mean diameter D50It it is 12 ��m-18 ��m; Described MgB2Consumption is described containing hydrogen silicone oil and the 5wt%-8wt% of cross-linking agent gross mass;
(2) cured product described in roasting in an inert atmosphere, to obtain final product.
In the present invention, the roasting of step (2) is made without after terminating pulverizing, and can obtain described lithium ion battery negative material.
In step (1), the various containing hydrogen silicone oils that described containing hydrogen silicone oil can use for this area, it is preferred that for Methyl Hydrogen Polysiloxane Fluid and/or ethyl containing hydrogen silicone oil. The hydrogen content of described containing hydrogen silicone oil is preferably at more than 1.58wt%. Described Silicon Containing Hydrogen oil viscosity is preferably 15.00-40.00mm2��s-1��
In step (1), described cross-linking agent can for this area for organosilicon crosslinked various cross-linking agent, it is advantageous to be divinylbenzene.
The consumption of described containing hydrogen silicone oil and described cross-linking agent is the conventional amount used of this area, and the mass ratio of described containing hydrogen silicone oil and described cross-linking agent is preferably 1: 1.2-1: 1.8.
In step (1), described catalyst can the organosilicon crosslinked various catalyst of catalysis for this area, it is preferred that for H2PtCl6��6H2O or Pd (PPh3)4��
The consumption of described catalyst is the conventional amount used of this area, it is preferred that for the 5wt ��-10wt �� of described containing hydrogen silicone oil and cross-linking agent gross mass.
In step (1), the condition of described stirring and method are condition and the method for this area routine.
In step (1), described mixing preferably carries out ultrasonic when. Described ultrasonic condition and method are condition and the method for this area routine. Described ultrasonic frequency is preferably 30-50KHz. The described ultrasonic time is preferably 20-40min.
In step (1), described inert atmosphere is the inert atmosphere that this area is conventional, it is preferred that for N2Or Ar2��
In step (1), the condition of described crosslinking curing and method are condition and the method for this area routine. The temperature of described crosslinking curing is preferably 130 DEG C-180 DEG C. The time of described crosslinking curing, reactant consumption is complete to be as the criterion to detect, it is preferred that for 5-8 hour.
In step (1), described pulverizing is preferably and carries out dry ball milling after mechanical activation comminution. Described mechanical activation comminution and the condition of dry ball milling and method are all condition and the method for this area routine.
In a better embodiment in the present invention, carry out step (1) as follows: by described containing hydrogen silicone oil and described cross-linking agent mix and blend, add described catalyst, after stirring, at the described ultrasonic described MgB of lower addition2, carry out crosslinking curing under an inert atmosphere, carry out described pulverizing.
In step (1), described catalyst preferably adds with the solution form containing this catalyst. The solvent of described solution is solvent commonly used in the art, it is preferred that for ethanol and/or isopropanol. Described catalyst mass body volume concentrations in described solution is preferably 0.005-0.010g/L.
In step (2), described roasting is method and the condition of this area routine. The holding temperature of described roasting is preferably 1000 DEG C. The temperature retention time of described roasting is preferably 2-5 hour. The temperature increasing schedule of described roasting is preferably: rise to 400 DEG C from room temperature in 80-90 minute; It is warming up to 600 DEG C from 400 in 60-80 minute; 600 DEG C are incubated 60-80 minute; It is warming up to 900 DEG C from 600 DEG C in 60-80 minute; It is warming up to 1000 DEG C from 900 DEG C in 60-80 minute.
Present invention also offers the lithium ion battery negative material that a kind of above-mentioned preparation method obtains.
Present invention also offers a kind of lithium ion battery, its negative material is described lithium ion battery negative material.
Meeting on the basis of this area general knowledge, above-mentioned each optimum condition, can combination in any, obtain the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material are all commercially.
The actively progressive effect of the present invention is in that:
Obtained the lithium ion battery negative material of a kind of specific capacity height, good cycle by the preparation method of the present invention, after its reversible capacity circulates more than 600mAh/g, 0.5C discharge and recharge 100, capability retention is more than 93%. And the preparation method operation of the present invention is simple, is more conducive to industrialized production.
Accompanying drawing explanation
Fig. 1 is the cyclic curve figure of the 0.5C rate charge-discharge of embodiment 5.
Detailed description of the invention
Mode by the examples below further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments. The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or selects according to catalogue.
Methyl Hydrogen Polysiloxane Fluid is purchased from Dongyang City sky Chemical Co., Ltd., its hydrogen content (%) >=1.58, viscosity (25 DEG C): 15.00-40.00mm2��s-1;
Divinylbenzene is purchased from Shanghai Hai Qu Chemical Co., Ltd.;
H2PtCl6.6H2O is purchased from Chemical Reagent Co., Ltd., Sinopharm Group;
Pd(PPh3)4Purchased from Shanghai He Bao Chemical Co., Ltd.;
MgB2Purchased from Beijing Sen Mao chemical materials company limited;
All the other commodity are common commercial goods.
Embodiment 1
80g Methyl Hydrogen Polysiloxane Fluid and 96g divinylbenzene are mixed, drips containing 0.88gH after stirring2PtCl6��6H2The alcoholic solution of O (mass body volume concentrations is 0.005g/L), is stirred for uniformly, being added thereto to the MgB of 8.8g under 30KHz is ultrasonic2, ultrasonic 20 minutes, N2Under atmosphere at 130 DEG C crosslinking curing 7 hours. After cured product mechanical activation comminution, dry ball milling is to particle diameter D50It it is 15 ��m, at N2In atmosphere, roasting at 1000 DEG C, obtains lithium ion battery negative material; During roasting, concrete temperature increasing schedule is as follows: 90 minutes from room temperature to 400 DEG C; Within 60 minutes, it is warming up to 600 DEG C from 400 DEG C; 600 DEG C are incubated 60 minutes; It is warming up to 900 DEG C from 600 DEG C in 60 minutes; It is warming up to 1000 DEG C from 900 DEG C in 60 minutes; 1000 DEG C are incubated 5 hours.
Electrochemical property test method:
For checking the performance of the silicon-carbon composite cathode material of lithium ion battery utilizing the present embodiment to prepare, prepare lithium ion battery with this cell negative electrode material.
Wherein negative material: Super-P conductive agent: SBR binding agent: the weight ratio of CMC thickening agent is 93: 2: 2.5: 2.5, and add appropriate N-Methyl pyrrolidone mixing, it is coated on copper foil of affluxion body after stirring and dries 12 hours under vacuo. Being assembled into button cell with lithium sheet in vacuum glove box after taking-up, electrolyte is containing 1MLiPF6EC-DEC (volume ratio is 1: 1) solution. Carrying out under electro-chemical test constant temperature, voltage 0.005-2.0V, electric current density is 15mA/g. Test result shows that the reversible specific capacity first of the silicon-carbon composite cathode material of preparation is 652mAh g-1, initial coulomb efficiency is 86%.
Use LiCoO2For positive active material, with negative material: Super-P conductive agent: SBR binding agent: the weight ratio of CMC thickening agent for 93: 2: 2.5: 2.5 for negative electrode active material, with containing 1MLiPF6EC-DEC (volume ratio is 1: 1) solution be electrolyte, be assembled into the full battery of 053048A type (design battery capacity is 780mAh), with 0.5C constant current charge-discharge, the capability retention after circulating at 100 times is 94%.
Embodiment 2
80g Methyl Hydrogen Polysiloxane Fluid and 120g divinylbenzene are mixed, drips after stirring containing 1.6gPd (PPh3)4The aqueous isopropanol of (mass body volume concentrations is 0.006g/L), is stirred for uniformly, being added thereto to the MgB of 10.2g under 40KHz is ultrasonic2, ultrasonic 30min, Ar2Under atmosphere at 150 DEG C crosslinking curing 6 hours. After cured product mechanical activation comminution, dry ball milling is to particle diameter D50It it is 12 ��m, at N2Roasting at 1000 DEG C in atmosphere, obtains lithium ion battery negative material, and during roasting, concrete temperature increasing schedule is as follows: 80 minutes from room temperature to 400 DEG C; Within 60 minutes, it is warming up to 600 DEG C from 400 DEG C; 600 DEG C are incubated 80 minutes; Within 80 minutes, it is warming up to 900 DEG C from 600 DEG C; Within 80 minutes, it is warming up to 1000 DEG C from 900 DEG C; 1000 DEG C are incubated 4 hours.
The reversible capacity first recording the silicon-carbon composite cathode material of preparation according to the electrochemical test method identical with embodiment 1 is 633mAh g-1, coulombic efficiency is 87% first, and under 0.5C multiplying power, the capability retention after 100 circulations is 93%.
Embodiment 3
120g Methyl Hydrogen Polysiloxane Fluid and 216g divinylbenzene are mixed, drips containing 3.36gH after stirring2PtCl6��6H2The alcoholic solution of O (mass body volume concentrations is 0.005g/L), is stirred for uniformly, being added thereto to the MgB of 26.88g under 50KHz is ultrasonic2, ultrasonic 32min, Ar2Under atmosphere at 180 DEG C crosslinking curing 5 hours. After cured product mechanical activation comminution, dry ball milling is to particle diameter D50It it is 16 ��m, at N2Roasting at 1000 DEG C in atmosphere, obtains lithium ion battery negative material, and during roasting, concrete temperature increasing schedule is as follows: 90 minutes from room temperature to 400 DEG C; Within 60 minutes, it is warming up to 600 DEG C from 400 DEG C; 600 DEG C are incubated 60 minutes; Within 60 minutes, it is warming up to 900 DEG C from 600 DEG C; Within 60 minutes, it is warming up to 1000 DEG C from 900 DEG C; 1000 DEG C are incubated 5 hours.
The reversible capacity first recording the silicon-carbon composite cathode material of preparation according to the electrochemical test method identical with embodiment 1 is 647mAh g-1, coulombic efficiency is 88% first, and the capability retention after lower 100 circulations of 0.5C multiplying power is 93%.
Embodiment 4
120g Methyl Hydrogen Polysiloxane Fluid and 180g divinylbenzene are mixed, drips containing 1.8gH after stirring2PtCl6��6H2The alcoholic solution of O (mass body volume concentrations is 0.010g/L), is stirred for uniformly, being added thereto to 18gMgB under 40KHz is ultrasonic2, ultrasonic 40min, N2Under atmosphere at 130 DEG C crosslinking curing 8 hours. After cured product mechanical activation comminution, dry ball milling is to particle diameter D50It it is 18 ��m, at Ar2Roasting at 1000 DEG C in atmosphere, obtains lithium ion battery negative material, and during roasting, concrete temperature increasing schedule is as follows: 90 minutes from room temperature to 400 DEG C; Within 60 minutes, it is warming up to 600 DEG C from 400; 600 DEG C are incubated 80 minutes; Within 60 minutes, it is warming up to 900 DEG C from 600 DEG C; Within 80 minutes, it is warming up to 1000 DEG C from 900 DEG C; 1000 DEG C are incubated 5 hours.
The reversible capacity first recording the silicon-carbon composite cathode material of preparation according to the electrochemical test method identical with embodiment 1 is 651mAh g-1, coulombic efficiency is 87% first, and the capability retention after lower 100 circulations of 0.5C multiplying power is 95%.
Embodiment 5
120g Methyl Hydrogen Polysiloxane Fluid and 192g divinylbenzene are mixed, drips after stirring containing 2.5gPd (PPh3)4The aqueous isopropanol of (mass body volume concentrations is 0.006g/L), is stirred for uniformly, being added thereto to the MgB of 24.8g under 40KHz is ultrasonic2, ultrasonic 35min, Ar2Under atmosphere at 150 DEG C crosslinking curing 6 hours. After cured product mechanical activation comminution, dry ball milling is to particle diameter D50It it is 12 ��m, at N2Roasting at 1000 DEG C in atmosphere, obtains lithium ion battery negative material, and during roasting, concrete temperature increasing schedule is as follows: 80 minutes from room temperature to 400 DEG C; Within 80 minutes, it is warming up to 600 DEG C from 400 DEG C; 600 DEG C are incubated 60 minutes; Within 60 minutes, it is warming up to 900 DEG C from 600 DEG C; Within 80 minutes, it is warming up to 1000 DEG C from 900; 1000 DEG C are incubated 3 hours.
The reversible capacity first recording the silicon-carbon composite cathode material of preparation according to the electrochemical test method identical with embodiment 1 is 638mAh g-1, coulombic efficiency is 90% first, the capability retention 94% after lower 100 circulations of 0.5C multiplying power.
Claims (16)
1. a preparation method for lithium ion battery negative material, it comprises the following steps:
(1) by containing hydrogen silicone oil, cross-linking agent and MgB2Mixing, under the effect of catalyst, carries out cross-linking and curing reaction under an inert atmosphere, cured product is crushed to mean diameter D50It it is 12 ��m-18 ��m; Described MgB2Consumption is described containing hydrogen silicone oil and the 5wt%-8wt% of cross-linking agent gross mass;
(2) cured product described in roasting in an inert atmosphere, to obtain final product;
Described containing hydrogen silicone oil is Methyl Hydrogen Polysiloxane Fluid and/or ethyl containing hydrogen silicone oil; Described cross-linking agent is divinylbenzene; The mass ratio of described containing hydrogen silicone oil and described cross-linking agent is 1:1.2-1:1.8.
2. preparation method as claimed in claim 1, it is characterised in that the hydrogen content of described containing hydrogen silicone oil is at more than 1.58wt%.
3. preparation method as claimed in claim 1, it is characterised in that described Silicon Containing Hydrogen oil viscosity is 15.00-40.00mm2��s-1��
4. the preparation method as described in any one of claims 1 to 3, it is characterised in that described catalyst is H2PtCl6��6H2O or Pd (PPh3)4��
5. the preparation method as described in any one of claims 1 to 3, it is characterised in that the consumption of described catalyst is the 5wt ��-10wt �� of described containing hydrogen silicone oil and cross-linking agent gross mass.
6. the preparation method as described in any one of claims 1 to 3, it is characterised in that described be blended in ultrasonic under carry out; Described inert atmosphere is N2Or Ar2; The temperature of described crosslinking curing is 130 DEG C-180 DEG C; The time of described crosslinking curing is 5-8 hour; Described pulverizing is for carrying out dry ball milling after mechanical activation comminution.
7. preparation method as claimed in claim 6, it is characterised in that described ultrasonic frequency is 30-50KHz.
8. preparation method as claimed in claim 6, it is characterised in that the described ultrasonic time is 20-40min.
9. the preparation method as described in any one of claims 1 to 3, it is characterized in that, step (1) is undertaken by operations described below: by described containing hydrogen silicone oil and described cross-linking agent mix and blend, add described catalyst, after stirring, at the ultrasonic described MgB of lower addition2, carry out crosslinking curing under an inert atmosphere, carry out described pulverizing.
10. the preparation method as described in any one of claims 1 to 3, it is characterised in that described catalyst adds with the solution form containing this catalyst.
11. preparation method as claimed in claim 10, it is characterised in that the solvent of described solution is ethanol and/or isopropanol.
12. preparation method as claimed in claim 10, it is characterised in that described catalyst mass body volume concentrations in described solution is 0.005-0.010g/L.
13. the preparation method as described in any one of claims 1 to 3, it is characterised in that the holding temperature of described roasting is 1000 DEG C; The temperature retention time of described roasting is 2-5 hour.
14. the preparation method as described in any one of claims 1 to 3, it is characterised in that the temperature increasing schedule of described roasting is: rise to 400 DEG C from room temperature in 80-90 minute; It is warming up to 600 DEG C from 400 in 60-80 minute; 600 DEG C, it is incubated 60-80 minute; It is warming up to 900 DEG C from 600 DEG C in 60-80 minute; It is warming up to 1000 DEG C from 900 DEG C in 60-80 minute.
15. the lithium ion battery negative material that the preparation method described in any one of claim 1-14 prepares.
16. a lithium ion battery, it is characterised in that its negative material is lithium ion battery negative material as claimed in claim 15.
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| CN1758466A (en) * | 2004-07-30 | 2006-04-12 | 信越化学工业株式会社 | Si-C-O composite, making method, and non-aqueous electrolyte secondary cell negative electrode material |
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| JP2000223126A (en) * | 1999-02-02 | 2000-08-11 | Mitsubishi Paper Mills Ltd | Electrode and its manufacture |
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| CN1758466A (en) * | 2004-07-30 | 2006-04-12 | 信越化学工业株式会社 | Si-C-O composite, making method, and non-aqueous electrolyte secondary cell negative electrode material |
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Effective date of registration: 20210202 Address after: 200131 building 10, No. 860, Xinyang Road, Lingang New District, China (Shanghai) pilot Free Trade Zone, Pudong New Area, Shanghai Patentee after: Shanghai Shanshan New Material Co.,Ltd. Address before: 201209 No. 3158 Golden Sea Road, Shanghai, Pudong New Area Patentee before: SHANGHAI SHANSHAN TECH Co.,Ltd. |