CN109360923A - The preparation method of composite lithium ion battery ceramic diaphragm - Google Patents
The preparation method of composite lithium ion battery ceramic diaphragm Download PDFInfo
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- CN109360923A CN109360923A CN201811116455.4A CN201811116455A CN109360923A CN 109360923 A CN109360923 A CN 109360923A CN 201811116455 A CN201811116455 A CN 201811116455A CN 109360923 A CN109360923 A CN 109360923A
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- 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
- H01M10/60—Heating or cooling; Temperature control
- H01M10/65—Means for temperature control structurally associated with the cells
- H01M10/654—Means for temperature control structurally associated with the cells located inside the innermost case of the cells, e.g. mandrels, electrodes or electrolytes
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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
- H01M10/60—Heating or cooling; Temperature control
- H01M10/65—Means for temperature control structurally associated with the cells
- H01M10/658—Means for temperature control structurally associated with the cells by thermal insulation or shielding
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/463—Separators, membranes or diaphragms characterised by their shape
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2200/00—Safety devices for primary or secondary 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
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- General Chemical & Material Sciences (AREA)
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- General Physics & Mathematics (AREA)
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- Cell Separators (AREA)
Abstract
The invention proposes a kind of preparation methods of composite lithium ion battery ceramic diaphragm, comprising the following steps: 1) prepares nano-cellulose suspension；2) prepared by nano pulp: nano ceramic powder being put into styrene-butadiene latex solution and is dispersed, after dispersion liquid is warming up to 60~80 DEG C, silane coupling agent is added and carries out reacting 1~3h with hydrolysis sodium starch；3) spinning: by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2), mixed liquor is subjected to vacuum defoamation, spinning solution is obtained after deaeration, spinning solution is added in syringe, carry out electrostatic spinning, cellulose basement membrane is formed, then gained cellulose basement membrane is dried.The diaphragm that this method is prepared not only good heat-insulation effect, also has and the good wetability of electrolyte.
Description
Technical field
The invention belongs to battery diaphragm technical fields, and in particular to a kind of preparation method of composite lithium ion battery ceramic diaphragm.
Background technique
With the rapid development in lithium ion battery applications field, market proposes the performance of lithium ion battery more stringent
Requirement, requirement of the battery manufacturer to battery diaphragm be also higher and higher.Lithium battery diaphragm need to have following characteristic: 1, thickness is uniform
It is moderate and take into account mechanical strength and the internal resistance of cell；2, good permeability and the micropore uniformity；3, stronger imbibition, guarantor's liquid energy
Power；4, good chemical stability and electrochemical stability and thermal stability；5, higher security performance, good heat are self-closing
The effect of holes.The technology and production method of lithium ion battery separator also fall behind relatively at present, and there is also closed pore temperature height and rupture of membranes temperature
The problems such as low is spent, the safety of diaphragm is low.
Lithium ion battery has that energy density is high, specific power is big, cycle performance as a kind of high-energy green secondary cell
Good, memory-less effect, it is pollution-free the features such as, be widely used to Intelligent mobile equipment, hybrid vehicle, electric vehicle, the sun
The new energy fields such as energy electricity generation system, quickly grow.These fields do not require nothing more than battery with high-energy, power density, to electricity
The security requirement in pond is also higher and higher.And diaphragm is influence and determine lithium ion battery chemical property and safety important
Factor.Currently, the diaphragm material of commercial lithium-ion batteries mainly still uses polyethylene, microporous polypropylene membrane.However, poly- second
Alkene, polypropylene diaphragm are poor to electrolyte compatibility, there are imbibition rate and protect the low deficiency of liquid rate, electrolyte is easy to happen side
Leakage, there are hidden danger for the safety of battery.In addition, diaphragm currently on the market it is all simple play simple buffer action, in phase
Under same aperture, not any help of the raising to lithium ion conductivity.
Cellulose is that a kind of most wide, content is most high molecular material is distributed in nature.According to statistics, annual fine in the world
The yield of dimension element is 200,000,000,000 tons.Contain a large amount of good celluloses in cotton, flax, taro fiber crops and jute, wherein the fibre of cotton
Cellulose content highest is tieed up, up to 90% or more；In general timber, cellulose accounts for 40%~50%.Native cellulose is odorless, tasteless
White filiform.Cellulose output is abundant, and chemical stability is good, not soluble in water and common organic solvents, and has excellent
Thermal stability and good biodegradability.Therefore cellulose is widely used and develops.Cellulose is not only
It is important paper making raw material, is also widely used in plastics, weaving, explosive, electrician and Scientific Research Equipments etc..In recent years, many films
Investigation of materials person is devoted to research and development low cost, reproducible cellulosic material preparation High-performance diaphragm, especially with cellulose,
The lithium ion battery separator of raw material based on modified and enhancing cellulose, and and polyalkene diaphragm heat resistance, puncture,
Intensity, resistance sizes, high voltage withstanding property etc. are compared research.
Summary of the invention
The present invention proposes a kind of preparation method of composite lithium ion battery ceramic diaphragm, the diaphragm that this method is prepared not only every
Thermal effect is good, also has and the good wetability of electrolyte.
The technical scheme of the present invention is realized as follows:
A kind of preparation method of composite lithium ion battery ceramic diaphragm, comprising the following steps:
1) it prepares nano-cellulose suspension: after nano-cellulose, dispersing agent are mixed with water, adjusting pH to 9.0
Aromatic polyimide is added after~10.0 to be reacted, after reaction nano-cellulose suspension；
2) prepared by nano pulp: nano ceramic powder being put into styrene-butadiene latex solution and is dispersed, by dispersion liquid liter
Temperature carries out reacting 1~3h to after 60~80 DEG C, adding silane coupling agent with hydrolysis sodium starch；
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carries out vacuum defoamation, and spinning solution is obtained after deaeration, spinning solution is added in syringe, carries out electrostatic spinning, is formed fine
Plain basement membrane is tieed up, then gained cellulose basement membrane is dried.
Preferably, the dispersing agent in the step 1) is the mixture of isopropanol and dimethyl acetamide, the Nanowire
The mass ratio of element and the water is tieed up as 10~20:100, the mass ratio of the dispersing agent and the water is 1~5:1, described
The mass ratio of nano-cellulose and the aromatic polyimide is 6~12:1.
Preferably, the mass ratio of the nano ceramic powder in the step 2) and the styrene-butadiene latex solution is 10
The mass ratio of~20:100, the nano ceramic powder and the silane coupling agent is 100:4~8, the nano-ceramic powder
The last mass ratio with the hydrolysis sodium starch is 100:1~3.
Preferably, the silane coupling agent is KH550 or KH560.
Preferably, the electrostatic spinning in the step 3) specifically comprises the processes of: in voltage be 20~35kV, to receive distance be
10~20cm, flow be 2~4mL/h, spinning temperature be 40~60 DEG C, receive drum rotation speed be 10~25m/h under conditions of into
Row electrostatic spinning forms fiber basement membrane.
Preferably, dry specific steps are as follows: the fiber basement membrane that electrostatic spinning is formed is put into vacuum drying oven, 45~
Dry 10~12h at a temperature of 55 DEG C.
Beneficial effects of the present invention:
1) nano pulp of the invention is mainly by nano ceramic powder, silane coupling agent and hydrolysis sodium starch in butadiene-styrene rubber
Reaction is prepared in milk solution, not only makes nano ceramic powder dispersibility more preferable, also improves diaphragm and electrolyte
Wettability, the contact angle with electrolyte is less than 20 °.
2) preparation method of composite lithium ion battery ceramic diaphragm of the invention is by nano pulp and nano-cellulose suspension
It carries out spinning after mixing to be prepared, with very high heat-proof quality.
3) nano-cellulose suspension of the invention is prepared by nano-cellulose, dispersing agent and aromatic polyimide
It arrives, effectively improves the closed pore temperature and broken film temperature of diaphragm, have a safety feature.
4) present invention is prepared fiber base lithium battery diaphragm and can apply in lithium battery, the closed pore temperature of battery diaphragm
It is 145~165 DEG C, broken film temperature is at 252 DEG C or more, and at 1.0C, after 100 circulations, the lithium battery capacity of battery diaphragm is protected
95% or more holdup, the porosity of battery diaphragm reaches 70% or more.
Specific embodiment
Embodiment 1
A kind of preparation method of composite lithium ion battery ceramic diaphragm, comprising the following steps:
1) it prepares nano-cellulose suspension: after nano-cellulose, dispersing agent are mixed with water, adjusting pH to 9.5
Aromatic polyimide is added afterwards to be reacted, after reaction nano-cellulose suspension；Dispersing agent in step 1) is different
The mass ratio of the mixture of propyl alcohol and dimethyl acetamide, nano-cellulose and water is 15:100, the quality of dispersing agent and water
The ratio between be 3:1, the mass ratio of nano-cellulose and aromatic polyimide is 8:1.
2) prepared by nano pulp: nano ceramic powder being put into styrene-butadiene latex solution and is dispersed, by dispersion liquid liter
Temperature carries out reacting 2h to after 70 DEG C, adding silane coupling agent KH560 with hydrolysis sodium starch；Nano ceramic powder and fourth
The mass ratio of benzene latex solution is 16:100, and the mass ratio of nano ceramic powder and silane coupling agent is 100:6, nanometer pottery
Porcelain powder and the mass ratio of hydrolysis sodium starch are 100:2.
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carry out vacuum defoamation, after deaeration spinning solution, spinning solution is added in syringe, voltage be 25kV, receive away from
From for 16cm, flow 3mL/h, spinning temperature is 50 DEG C, receives under conditions of drum rotation speed is 15m/h and carries out electrostatic spinning,
Fiber basement membrane is formed, cellulose basement membrane is formed, then gained cellulose basement membrane is put into vacuum drying oven, dries at 50 °C
10h.
The closed pore temperature of the battery diaphragm of the present embodiment is 154 DEG C, contact angle of the broken film temperature at 256 DEG C, with electrolyte
It is 16 °；At 1.0C, after 100 circulations, 95% or more the lithium battery capacity conservation rate of battery diaphragm, the hole of battery diaphragm
Rate reaches 77%.
Embodiment 2
A kind of preparation method of composite lithium ion battery ceramic diaphragm, comprising the following steps:
1) it prepares nano-cellulose suspension: after nano-cellulose, dispersing agent are mixed with water, adjusting pH to 9.0
Aromatic polyimide is added afterwards to be reacted, after reaction nano-cellulose suspension；Dispersing agent in step 1) is different
The mass ratio of the mixture of propyl alcohol and dimethyl acetamide, nano-cellulose and water is 10:100, the quality of dispersing agent and water
The ratio between be 1:1, the mass ratio of nano-cellulose and aromatic polyimide is 6:1.
2) prepared by nano pulp: nano ceramic powder being put into styrene-butadiene latex solution and is dispersed, by dispersion liquid liter
Temperature carries out reacting 3h to after 60 DEG C, adding Silane coupling agent KH550 with hydrolysis sodium starch；Nano ceramic powder and fourth
The mass ratio of benzene latex solution is 10:100, and the mass ratio of nano ceramic powder and silane coupling agent is 100:8, nanometer pottery
Porcelain powder and the mass ratio of hydrolysis sodium starch are 100:1.
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carry out vacuum defoamation, after deaeration spinning solution, spinning solution is added in syringe, voltage be 20kV, receive away from
From for 10cm, flow 2mL/h, spinning temperature is 60 DEG C, receives under conditions of drum rotation speed is 10m/h and carries out electrostatic spinning,
Fiber basement membrane is formed, forms cellulose basement membrane, then gained cellulose basement membrane is put into vacuum drying oven, it is dry at a temperature of 45 DEG C
12h.
The closed pore temperature of the battery diaphragm of the present embodiment is 145 DEG C, contact angle of the broken film temperature at 253 DEG C, with electrolyte
It is 18 °；At 1.0C, after 100 circulations, 95% or more the lithium battery capacity conservation rate of battery diaphragm, the hole of battery diaphragm
Rate reaches 71%.
Embodiment 3
A kind of preparation method of composite lithium ion battery ceramic diaphragm, comprising the following steps:
1) it prepares nano-cellulose suspension: after nano-cellulose, dispersing agent are mixed with water, adjusting pH to 10.0
Aromatic polyimide is added afterwards to be reacted, after reaction nano-cellulose suspension；Dispersing agent in step 1) is different
The mass ratio of the mixture of propyl alcohol and dimethyl acetamide, nano-cellulose and water is 20:100, the quality of dispersing agent and water
The ratio between be 5:1, the mass ratio of nano-cellulose and aromatic polyimide is 12:1.
2) prepared by nano pulp: nano ceramic powder being put into styrene-butadiene latex solution and is dispersed, by dispersion liquid liter
Temperature carries out reacting 1h to after 80 DEG C, adding silane coupling agent KH560 with hydrolysis sodium starch；Nano ceramic powder and fourth
The mass ratio of benzene latex solution is 20:100, and the mass ratio of nano ceramic powder and silane coupling agent is 100:4, nanometer pottery
Porcelain powder and the mass ratio of hydrolysis sodium starch are 100:3.
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carry out vacuum defoamation, after deaeration spinning solution, spinning solution is added in syringe, voltage be 35kV, receive away from
From for 20cm, flow 4mL/h, spinning temperature is 40 DEG C, receives under conditions of drum rotation speed is 25m/h and carries out electrostatic spinning,
Fiber basement membrane is formed, forms cellulose basement membrane, then gained cellulose basement membrane is put into vacuum drying oven, it is dry at a temperature of 55 DEG C
10h.
The closed pore temperature of the battery diaphragm of the present embodiment is 165 DEG C, and broken film temperature is at 255 DEG C or more, with connecing for electrolyte
Feeler is 15 °；At 1.0C, after 100 circulations, 95% or more the lithium battery capacity conservation rate of battery diaphragm, battery diaphragm
Porosity reaches 74%.
Comparative example 1
A kind of preparation method of composite lithium ion battery ceramic diaphragm, comprising the following steps:
1) it prepares nano-cellulose suspension: after nano-cellulose is mixed with water, obtaining nano-cellulose suspension
Liquid；The mass ratio of nano-cellulose and water is 15:100.
2) prepared by nano pulp: nano ceramic powder being put into styrene-butadiene latex solution and is dispersed, by dispersion liquid liter
Temperature adds silane coupling agent KH560 and carries out reaction 2h to after 70 DEG C；Nano ceramic powder and styrene-butadiene latex solution
Mass ratio is 16:100, and the mass ratio of nano ceramic powder and silane coupling agent is 100:6.
3) spinning:, will by the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2)
Mixed liquor carry out vacuum defoamation, after deaeration spinning solution, spinning solution is added in syringe, voltage be 25kV, receive away from
From for 16cm, flow 3mL/h, spinning temperature is 50 DEG C, receives under conditions of drum rotation speed is 15m/h and carries out electrostatic spinning,
Fiber basement membrane is formed, cellulose basement membrane is formed, then gained cellulose basement membrane is put into vacuum drying oven, dries at 50 °C
10h.
The closed pore temperature of battery diaphragm is 116 DEG C, and broken film temperature is at 212 DEG C or more, at 1.0C, after 100 circulations, and electricity
95% or more the lithium battery capacity conservation rate of pond diaphragm, the porosity of battery diaphragm reaches 69%.
Composite lithium ion battery ceramic diaphragm is prepared at 200 DEG C in embodiment 1-3 and comparative example 1 and heats 6h, according to adding
The change in size of hot front and back diaphragm vertical and horizontal, calculates the shrinking percentage of diaphragm vertical and horizontal, the results are shown in Table 1.
Table 1
| Diaphragm sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 |
| Lateral percent thermal shrinkage (%) | 0.3 | 0.5 | 0.2 | 0.6 |
| Longitudinal percent thermal shrinkage (%) | 0.2 | 0.5 | 0.3 | 0.7 |
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of composite lithium ion battery ceramic diaphragm, which comprises the following steps:
1) nano-cellulose suspension is prepared: after nano-cellulose, dispersing agent are mixed with water, adjusting pH to 9.0~
Aromatic polyimide is added after 10.0 to be reacted, after reaction nano-cellulose suspension；
2) prepared by nano pulp: nano ceramic powder being put into styrene-butadiene latex solution and is dispersed, dispersion liquid is warming up to
After 60~80 DEG C, adds silane coupling agent and carry out reacting 1~3h with hydrolysis sodium starch；
3) spinning: the mixed liquor for mixing nano pulp of the nano-cellulose suspension of step 1) and step 2) will mix
Liquid carries out vacuum defoamation, and spinning solution is obtained after deaeration, spinning solution is added in syringe, carries out electrostatic spinning, forms cellulose
Basement membrane, then gained cellulose basement membrane is dried.
2. the preparation method of composite lithium ion battery ceramic diaphragm according to claim 1, which is characterized in that in the step 1)
Dispersing agent be isopropanol and dimethyl acetamide mixture, the mass ratio of the nano-cellulose and the water is 10~
The mass ratio of 20:100, the dispersing agent and the water is 1~5:1, and the nano-cellulose and the aromatic series polyamides are sub-
The mass ratio of amine is 6~12:1.
3. the preparation method of composite lithium ion battery ceramic diaphragm according to claim 1, which is characterized in that in the step 2)
The nano ceramic powder and the styrene-butadiene latex solution mass ratio be 10~20:100, the nano ceramic powder with
The mass ratio of the silane coupling agent is 100:4~8, and the nano ceramic powder and the mass ratio of the hydrolysis sodium starch are
100:1~3.
4. the preparation method of composite lithium ion battery ceramic diaphragm according to claim 3, which is characterized in that described silane coupled
Agent is KH550 or KH560.
5. the preparation method of composite lithium ion battery ceramic diaphragm according to claim 1, which is characterized in that in the step 3)
Electrostatic spinning specifically comprises the processes of: in voltage be 20~35kV, receiving distance is 10~20cm, and flow is 2~4mL/h, is spun
Silk temperature is 40~60 DEG C, receives under conditions of drum rotation speed is 10~25m/h and carries out electrostatic spinning, forms fiber basement membrane.
6. the preparation method of composite lithium ion battery ceramic diaphragm according to claim 1, which is characterized in that dry specific step
Suddenly are as follows: the fiber basement membrane that electrostatic spinning is formed is put into vacuum drying oven, dry 10~12h at a temperature of 45~55 DEG C.
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| CN201811116455.4A CN109360923A (en) | 2018-09-25 | 2018-09-25 | The preparation method of composite lithium ion battery ceramic diaphragm |
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| CN201811116455.4A CN109360923A (en) | 2018-09-25 | 2018-09-25 | The preparation method of composite lithium ion battery ceramic diaphragm |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114552122A (en) * | 2022-01-11 | 2022-05-27 | 惠州锂威电子科技有限公司 | Diaphragm, preparation method thereof and secondary battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114552122A (en) * | 2022-01-11 | 2022-05-27 | 惠州锂威电子科技有限公司 | Diaphragm, preparation method thereof and secondary battery |
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Application publication date: 20190219 |