CN110212237A - A method of reducing lithium ion battery thermal runaway under confined space - Google Patents
A method of reducing lithium ion battery thermal runaway under confined space Download PDFInfo
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- CN110212237A CN110212237A CN201910551692.1A CN201910551692A CN110212237A CN 110212237 A CN110212237 A CN 110212237A CN 201910551692 A CN201910551692 A CN 201910551692A CN 110212237 A CN110212237 A CN 110212237A
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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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
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Abstract
The present invention relates to a kind of methods for reducing lithium ion battery thermal runaway under confined space, specifically, it is related to a kind of positive/negative electrode material by constructing with excellent thermostability, the safe charge and discharge of lithium ion battery are carried out by electronics conversion reaction, by low internal rate of side reactions, the risk of lithium ion battery thermal runaway under confined space is effectively reduced.This method realizes the integrated novel organic lithium ion battery of positive and negative pole material, it has many advantages, such as that thermal safety more more stable than conventional lithium ion battery positive electrode, more simple and environmentally-friendly preparation process and device are easy;The organic material used makes it not only can be used as positive electrode due to the electron-transfer reaction of carbonyl functional group, but also can be used as negative electrode material, and not only there are also excellent thermostabilities simultaneously for environmental protection.It is effective to promote thermal decomposition temperature, it is obviously improved the thermal runaway temperature of lithium ion battery, the inorganic positive electrode of tradition that security performance is used considerably beyond commercial Li-ion battery.
Description
Technical field
The invention belongs to cell safety technical fields, are related to a kind of reduction lithium ion battery thermal runaway under confined space
Method is converted specifically, being related to a kind of positive/negative electrode material by constructing with excellent thermostability by electronics
Reaction carries out the safe charge and discharge of lithium ion battery, and by low internal rate of side reactions, lithium ion battery is effectively reduced in confined space
The risk of lower thermal runaway.
Background technique
It is a series of important that undersea detection equipment is able to carry out underwater long-time information gathering, information countermeasure, defence strike etc.
Task greatly extends the underwater fight capability in China.The energy is the key that realize underwater kit long time continuous working, is
Execute the key core of diversification task.
For lithium ion battery compared to electrical source of power such as conventional lead acid, ni-mh and zinc-silver oxide cells, it is close that it has higher energy
Degree and power density, it has also become unmanned autonomous navigation device (AUV) etc. equips major impetus energy form.Traditional lithium-ion battery
Self structure does not have pressure-bearing characteristic, to avoid the battery in deep-marine-environment from bearing high pressure and fail, need to be stored in thicker shell
In the closed pressure resistant battery flat of body protection.Undersea detection is equipped in the task of execution, due to environment particularity, is generally required short
When high-power operation, therefore lithium ion battery generally requires to be large current discharge, however the anode that traditional commerce lithium battery uses
Material is due to fault of construction, in heavy-current discharge, often generates a large amount of heat, and aggravate the side reaction of inside battery,
Causing thermal runaway leads to the safety accidents such as explosive combustion.Conventional lithium ion battery positive electrode, can not due to structure limitation at present
Meet the safety being large current discharge in confined space under water.Thus, design it is a kind of can have it is heat-staple safely controllable
It is extremely necessary that positive and negative pole material, which reduces thermal runaway risk of the lithium ion battery under confined space,.
Summary of the invention
Technical problem solved by the present invention is in view of the defects existing in the prior art, the purpose of the present invention is to provide one
The method that kind reduces lithium ion battery thermal runaway under confined space, the method are enriched by preparation high concentration free radical
Three-dimensional carbon-based structure material can not only promote material conductivity, while single electron system can be dropped by intermolecular force
The internal resistance of low inside battery effectively improves the safety that lithium battery is large current discharge under confined space under water.
The technical scheme is that a kind of method for reducing lithium ion battery thermal runaway under confined space, including with
Lower step:
Step 1: organic acid hydrate is added to after being added in polar liquid and stirs evenly to form suspension, when stirring
Between >=5h, suspension is ultrasonically treated after stirring, the time of ultrasonic treatment is≤3h;
Step 2: the suspension after ultrasonic treatment in step (1) is stirred again, and mixing time is >=20h;
Step 3: organic salt is added in the pure polar liquid without organic acid hydrate and stirs to form suspension
Liquid, mixing time >=5h carry out suspension to be ultrasonically treated≤3h, wherein
Step 4: the suspension after ultrasonic treatment in step (3) is slowly added into step (1) after ultrasonic treatment
In suspension, time≤20min, mixing temperature carries out at ultrasound the mixing suspension after adding between 10~15 DEG C
Reason, sonication treatment time >=2h, to mixing suspension stirring >=48h after mixed by step (3) and step (1);
Step 5: the obtained mixed solution of step (4) being centrifugated, revolving speed >=12000rpm, and centrifugation time >=
8min;
Step 6: being centrifuged resulting product for step (5), is alternately cleaned with low boiling point solvent and deionized water, when cleaning
Between >=15min;
Step 7: the product obtained after step (6) are alternately cleaned is dried, drying temperature >=60 DEG C, dry
Time >=12h, obtain dried powder;
Step 8: dried powder obtained by step (7) is passed through into 200 DEG C or more high-temperature calcinations under inert gas atmosphere, is obtained
Obtain the organic positive/negative material of ball-type;
Step 9: spherical organic positive/negative material obtained by step (8) is slowly added into polar liquid, saturating to be formed
Bright mixed solution;
Step 10: conductive carbon medium is slowly added to be stirred in transparent mixed solution obtained by step (9), when stirring
Between for >=18h, suspension is ultrasonically treated after stirring, the processing time is≤3h;
Step 11: mixing suspension obtained by step (10) being poured into low boiling point solvent and is stirred, and mixing time >=
4h;
Step 12: mixing suspension obtained by step (11) is distilled under low pressure, place is dried after distillation
Reason, drying temperature >=30 DEG C, drying time >=12h;Obtain final product.
A further technical solution of the present invention is: organic acid hydrate in the step 1: polar liquid mass ratio is
1:8~1:10.
A further technical solution of the present invention is: organic salt and polar liquid mass ratio in the step 3 be 1:40~
1:60.
A further technical solution of the present invention is: the polar liquid is deionized water, and purity >=analysis is pure
(99.5%).
A further technical solution of the present invention is: the low boiling point solvent is ethyl alcohol or acetone.
A further technical solution of the present invention is: the inert gas is argon gas, helium or nitrogen.
A further technical solution of the present invention is: the conductive carbon medium is graphene, carbon nanotube, conductive carbon black
One or more of (Super P), acetylene black and gas-phase growth of carbon fibre (VGCF), when ingredient is more than more than one, each group
Point ratio is equal.
A further technical solution of the present invention is: the high-temperature calcination time in the step 8 is that 36 hours or 48 are small
When.
A further technical solution of the present invention is: obtaining product is positive electrode rose when the high-temperature calcination time is 36 small
Rare two lithiums of red acid, that is, Li2C6O6。
A further technical solution of the present invention is: obtaining product is negative electrode material rose when the high-temperature calcination time is 36 small
Rare four lithiums of red acid, that is, Li4C6O6。
Invention effect
The technical effects of the invention are that: the technical effect of this method are as follows:
1. the present invention provides a kind of method for reducing lithium ion battery thermal runaway under confined space, the method passes through
Pattern control and chemical synthesis prepare organic anode and organic cathode material, utilize electron-transfer reaction and carbonyl function
The unique redox reaction of group, realizes the integrated novel organic lithium ion battery of positive and negative pole material, it has than traditional lithium
Ion battery positive electrode have higher thermal runaway temperature, more stable thermostability, more simple and environmentally-friendly preparation process and
The advantages that device is easy;
2. making in the method the present invention provides a kind of method for reducing lithium ion battery thermal runaway under confined space
Organic material makes it not only can be used as positive electrode due to the electron-transfer reaction of carbonyl functional group, but also can make
For negative electrode material, not only there are also excellent thermostabilities simultaneously for environmental protection.For lithium ion battery for a long time under confined space due to
The accumulation of heat easily causes the risks such as thermal runaway, and organic positive electrode of preparation can effectively promote thermal decomposition temperature, significantly
The thermal runaway temperature of lithium ion battery is promoted, the tradition that security performance is used considerably beyond commercial Li-ion battery is inorganic just
Pole material.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of final product made from embodiment 1.
Fig. 2 is transmission electron microscope (TEM) figure of final product made from embodiment 1.
Fig. 3 is thermogravimetric curve (TG) figure of final product made from embodiment 1.
Specific embodiment
Referring to Fig. 1-Fig. 3, the purpose of the present invention is what is be achieved through the following technical solutions.
A method of lithium ion battery thermal runaway under confined space is reduced, the method comprises the following steps:
(1) organic acid hydrate is added in polar liquid and is stirred evenly to form suspension, mixing time >=5h,
Suspension is carried out to be ultrasonically treated≤3h;Organic acid hydrate: polar liquid mass ratio is 1:8~1:10
Wherein, organic acid hydrate is rhodizonic acid dihydrate (H2C6O6·2H2O), polar liquid be go from
Sub- water, purity >=analysis are pure;
(2) by suspension stirring >=20h after ultrasonic treatment in step (1);
Magnetic stirring apparatus progress can be used in stirring;
(3) organic salt is added in polar liquid and is stirred and form suspension, mixing time >=5h carries out suspension
Ultrasonic treatment≤3h;Organic salt and polar liquid mass ratio are 1:40~1:60.
Wherein, the organic salt is lithium carbonate (Li2CO3);
(4) suspension after ultrasonic treatment in step (3) is slowly added into the suspension in step (1) after ultrasonic treatment
In liquid, the time≤20min, mixing temperature is between 10~15 DEG C, ultrasonic treatment >=2h after adding, to mixed liquor stirring >=
48h;
(5) the obtained mixed solution of step (4) is centrifugated, revolving speed >=12000rpm, centrifugation time >=8min;
(6) step (5) products therefrom low boiling point solvent and deionized water is centrifuged alternately to clean, scavenging period >=
15min;
Wherein, the low boiling point solvent is ethyl alcohol or acetone;
(7) step (6) products therefrom is dry in vacuum drying oven, drying temperature >=60 DEG C, drying time >=12h;
(8) dried powder obtained by step (7) is passed through into 200 DEG C or more high-temperature calcinations 36 hours under inert gas atmosphere
Or it (is calcined within 36 hours as two lithium of positive electrode rhodizonic acid, Li with obtaining the organic positive/negative material of ball-type for 48 hours2C6O6;
Calcining in 48 hours is four lithium of negative electrode material rhodizonic acid, Li4C6O6);
The inert gas is argon gas, helium or nitrogen.
(9) spherical organic positive/negative material obtained by step (8) is slowly added into polar liquid transparent mixed to be formed
Close solution.
(10) conductive carbon medium is slowly added in transparent mixed solution obtained by step (9), mixing time >=18h, to outstanding
Supernatant liquid carries out being ultrasonically treated≤3h;
Wherein, the conductive carbon medium is graphene, carbon nanotube, conductive carbon black (Super P), acetylene black and gas phase
One or more of grown carbon fiber (VGCF),
(11) mixing suspension obtained by step (10) is poured into low boiling point solvent, mixing time >=4h;
(12) mixed liquor obtained by step (11) is distilled under low pressure, and dry in vacuum drying oven, drying temperature >=30
DEG C, drying time >=12h;Obtain final product.
It is specifically explained by the following examples:
Embodiment 1
3.5g rhodizonic acid dihydrate (0.017mol) is added in 40mL deionized water and is stirred evenly to be formed
Solution A;1.05g lithium carbonate (0.014mol) is added in 60mL deionized water again and is stirred to form solution B.Then will
Solution B is slowly added into solution A and adds in 20 minutes, ultrasound 2 hours after adding, and stirs 36 hours.By gained
The mixed solution arrived is centrifuged 8 minutes under the revolving speed of 10000~12000rpm, with 40mL ethyl alcohol and acetone alternately cleaning 3-5 times
And it is 12 hours dry in 60 DEG C of vacuum drying ovens.Gained powder is finally passed through into 200 DEG C of high-temperature calcinations 24 hours under an ar atmosphere
To obtain ball-type Li2C6O6.Wherein, tem study, the diameter of final product is between 100nm~200nm.
By 2g spherical shape Li2C6O6It is slowly added into deionized water (40mL) to form transparent mixed solution.Then will
200mg redox graphene (rGO) is slowly added to ultrasound 3 hours and stirring 18 hours in transparent mixed solution.By the mixing
Object is poured into ethyl alcohol (600mL) and is stirred 4 hours.Finally, alcohol mixture is distilled under low pressure, pressure when low-pressure distillation
It should be 0.1~0.2 atmospheric pressure;And 12 hours are dried in 30 DEG C of vacuum drying oven to obtain final product Li2C6O6/rGO.It is right
Final product obtained carries out following analysis detection:
(1) it scanning electron microscope analysis: is detected using the HITACHIS-4800 type scanning electron microscope of Hitachi, Ltd
Method is as follows: electron beam is emitted from electron gun, after being accelerated in accelerating field, is passed through electromagnetic lens and is pooled
The electron beam that one diameter is 5mm;Under scanning coil effect, diameter is that the electron beam of 5mm does raster-like on final product surface
Scanning, accelerated high energy electron are beaten after final product and final product interaction, secondary electron, the backscattered electron of generation
Deng;Then signal is sent to and shows pipe, on the screen by secondary electron, backscattered electron for generating in detector acquisition procedure etc.
It shows to get SEM picture is arrived, condition: 5000 times, voltage 8kV.As a result as shown in Figure 1, obtained particle is a kind of
Similar to the ball shape structure particle that diameter is about between 100~200nm, and even particle distribution, particle size consistency
It is good.Wherein, tem study, the diameter of final product is between 100nm~200nm.
(2) tem study: using FEI Co., U.S. TECNAI G2T20 type transmission electron microscope, point
Analysis method is as follows: showing final product interior tissue form and structure using the electron beam imaging through final product on film;Cause
While final product microstructure form obtains observation, it is (same that it can also carry out Identification On Crystal to observed region for this
Position analysis);Analysis condition: amplification 105Times.Fig. 2 is the transmission electron microscope figure of final product, scale 200nm;It can send out
Existing spherical particles are combined on the surface of graphene by intermolecular force, and partial size has stronger in 200nm or so
Absorption and fixed function.
(3) using the carbon content of thermogravimetric subsidiary cladding, accurately to understand effective carbon-coated content.It can also study
Such as physical phenomenon of fusing, evaporation, distillation and absorption substance;For understanding the decomposition of substance, dehydration, dissociation, oxidation, going back
The processes such as original have good help.Fig. 3 is as positive electrode Li2C6O6Thermal decomposition temperature at 350 DEG C or so, and as negative
The Li of pole material4C6O6Thermal decomposition temperature at 400 DEG C or so.
Claims (10)
1. a kind of method for reducing lithium ion battery thermal runaway under confined space, which comprises the following steps:
Step 1: organic acid hydrate being added to after being added in polar liquid and stir evenly to form suspension, and mixing time >=
5h is ultrasonically treated suspension after stirring, and the time of ultrasonic treatment is≤3h;
Step 2: the suspension after ultrasonic treatment in step (1) is stirred again, and mixing time is >=20h;
Step 3: organic salt being added in the pure polar liquid without organic acid hydrate and is stirred forms suspension, stirs
>=5h is mixed the time, suspension is carried out to be ultrasonically treated≤3h;
Step 4: the suspension after ultrasonic treatment in step (3) is slowly added into the suspension in step (1) after ultrasonic treatment
In, time≤20min, mixing temperature is ultrasonically treated the mixing suspension after adding between 10~15 DEG C, at ultrasound
Time >=2h is managed, to mixing suspension stirring >=48h after mixed by step (3) and step (1);
Step 5: the obtained mixed solution of step (4) is centrifugated, revolving speed >=12000rpm, centrifugation time >=8min;
Step 6: being centrifuged resulting product for step (5), is alternately cleaned with low boiling point solvent and deionized water, and scavenging period >=
15min;
Step 7: the product obtained after step (6) are alternately cleaned is dried, drying temperature >=60 DEG C, drying time
>=12h, obtains dried powder;
Step 8: dried powder obtained by step (7) is passed through into 200 DEG C or more high-temperature calcinations under inert gas atmosphere, obtains ball
The organic positive/negative material of type;
Step 9: spherical organic positive/negative material obtained by step (8) is slowly added into polar liquid, transparent mixed to be formed
Close solution;
Step 10: conductive carbon medium is slowly added to be stirred in transparent mixed solution obtained by step (9), and mixing time is >=
18h is ultrasonically treated suspension after stirring, and the processing time is≤3h;
Step 11: mixing suspension obtained by step (10) being poured into low boiling point solvent and is stirred, mixing time >=4h;
Step 12: mixing suspension obtained by step (11) being distilled under low pressure, is dried after distillation, dry
Temperature >=30 DEG C, drying time >=12h;Obtain final product.
2. a kind of method for reducing lithium ion battery thermal runaway under confined space as described in claim 1, which is characterized in that
Organic acid hydrate in the step 1: polar liquid mass ratio is 1:8~1:10.
3. a kind of method for reducing lithium ion battery thermal runaway under confined space as described in claim 1, which is characterized in that
Organic salt and polar liquid mass ratio in the step 3 are 1:40~1:60.
4. a kind of method for reducing lithium ion battery thermal runaway under confined space as described in claim 1, which is characterized in that
The polar liquid is deionized water, and purity >=analysis is pure (99.5%).
5. a kind of method for reducing lithium ion battery thermal runaway under confined space as described in claim 1, which is characterized in that
The low boiling point solvent is ethyl alcohol or acetone.
6. a kind of method for reducing lithium ion battery thermal runaway under confined space as described in claim 1, which is characterized in that
The inert gas is argon gas, helium or nitrogen.
7. a kind of method for reducing lithium ion battery thermal runaway under confined space as described in claim 1, which is characterized in that
The conductive carbon medium is graphene, carbon nanotube, conductive carbon black (Super P), acetylene black and gas-phase growth of carbon fibre
One or more of (VGCF), when ingredient is more than more than one, each component ratio is equal.
8. a kind of method for reducing lithium ion battery thermal runaway under confined space as described in claim 1, which is characterized in that
The high-temperature calcination time in the step 8 is 36 hours or 48 hours.
9. a kind of method for reducing lithium ion battery thermal runaway under confined space as claimed in claim 8, which is characterized in that
When the high-temperature calcination time is 36 small, obtaining product is the i.e. Li of two lithium of positive electrode rhodizonic acid2C6O6。
10. a kind of method for reducing lithium ion battery thermal runaway under confined space as claimed in claim 8, feature exist
In when the high-temperature calcination time is 36 small, obtaining product is the i.e. Li of four lithium of negative electrode material rhodizonic acid4C6O6。
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