CN109659477A - Rodlike silica composite diaphragm of fiber and preparation method thereof - Google Patents
Rodlike silica composite diaphragm of fiber and preparation method thereof Download PDFInfo
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- CN109659477A CN109659477A CN201910034190.1A CN201910034190A CN109659477A CN 109659477 A CN109659477 A CN 109659477A CN 201910034190 A CN201910034190 A CN 201910034190A CN 109659477 A CN109659477 A CN 109659477A
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- Prior art keywords
- diaphragm
- composite diaphragm
- porous polyolefin
- ceramic
- fiber
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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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
-
- 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
-
- 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
- H01M50/411—Organic material
-
- 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
- H01M50/431—Inorganic material
-
- 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
- H01M50/44—Fibrous material
-
- 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 invention belongs to technical field of lithium ion, and in particular to a kind of rodlike silica composite diaphragm of fiber and preparation method thereof.Wherein, the rodlike silica composite diaphragm of this fiber includes: porous polyolefin class diaphragm and the ceramic layer for being sprayed on porous polyolefin class membrane surface.Solve the problems, such as that ceramic particle is unevenly distributed；Ceramic particle can be contacted preferably with porous polyolefin class membrane surface simultaneously, more uniform and fine and close, make the composite diaphragm to be formed imbibition rate with higher and wetability, it is ensured that the charge and discharge under big multiplying power are realized in the quick transmission of lithium ion.In addition, ceramic layer has excellent thermal stability, the heat resistance of composite diaphragm can be improved.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of rodlike silica composite diaphragm of fiber and its
Preparation method.
Background technique
Battery diaphragm is the important component of battery.Commercial li-ion battery diaphragm has the following problems at present: (1)
It is heated easily to shrink, cause lithium battery positive and negative anodes short-circuit；(2) compatibility of battery diaphragm and polarity electrolyte is poor, electrolyte wetting
Property is poor；(3) porosity is lower, causes electrolyte retention poor.
In order to overcome the above problems, one layer of ceramic particle is generally coated in membrane surface using ceramic coated technology.But it makes pottery
The generally spherical particle of porcelain particle has characteristics that (1) surface can be high, is in thermodynamic instability state, easily reunites；
(2) ceramic grain surface has hydrophilic radical, and polarity is higher, is difficult to disperse in organic media.Due to the characteristic of ceramic particle, warp
The composite diaphragm for crossing paint-on technique acquisition is easy to that there are ceramic particles to disperse non-uniform phenomenon on diaphragm.
Summary of the invention
The object of the present invention is to provide a kind of composite diaphragms and preparation method thereof, by the way that ceramic layer is sprayed porous polyolefin
The surface of class diaphragm solves the problems, such as that ceramic particle is unevenly distributed.
In order to solve the above-mentioned technical problems, the present invention provides a kind of composite diaphragms, comprising: porous polyolefin class diaphragm and
It is sprayed on the ceramic layer of porous polyolefin class membrane surface.
Further, the ceramic layer includes: several ceramic particles for being stacked each other on porous polyolefin class membrane surface；Its
Described in ceramic particle be fiber club shaped structure.
Further, the ulking thickness of the ceramic particle is 0.1-10 microns；The length of the ceramic particle is 10 microns,
Diameter is 100-400 nanometers.
Further, the porous polyolefin class diaphragm be one of PP diaphragm, PE diaphragm, PP/PE/PP composite diaphragm or
It is several.
Further, the aperture of the porous polyolefin class diaphragm is 0.01-0.05 microns, porosity 30-50%.
Further, the porosity of the composite diaphragm is 45-65%.
Another aspect, the present invention also provides a kind of preparation methods of composite diaphragm, comprising: prepares the rodlike titanium dioxide of fiber
Silicon particle；The rodlike silica dioxide granule of fiber is dissolved in the mixed liquor that binder and solvent are formed, forms ceramic particle；It will pottery
Porcelain particle disperses to obtain dispersion liquid in mixed liquor；By dispersion liquid electrostatic spraying on the surface of porous polyolefin class diaphragm；And
Vacuum drying obtains the composite diaphragm.
Further, the mass ratio of the binder and solvent is 1:20-50；The solid content of the dispersion liquid is 0.1-
10%.
Further, the binder is Kynoar, carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, polytetrafluoro
One or more of ethylene, polyacrylic acid formicester.
Further, the solvent is N, N- dimethyl pyrrolidone, n,N-Dimethylformamide, ethyl alcohol, acetone, deionization
One or more of water.
The invention has the advantages that composite diaphragm of the invention is by spraying porous polyolefin class diaphragm for ceramic layer
Surface solves the problems, such as that ceramic particle is unevenly distributed；Simultaneously ceramic particle can preferably with porous polyolefin class diaphragm
Surface contact, makes the composite diaphragm to be formed imbibition rate with higher and wetability, it is ensured that the quick transmission of lithium ion, it is real
The now charge and discharge under big multiplying power.In addition, ceramic layer has excellent thermal stability, the heat resistance of composite diaphragm can be improved.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the surface topography schematic diagram of composite diaphragm of the invention.
In figure: porous polyolefin class diaphragm 1, ceramic particle 2.
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.These attached drawings are simplified schematic diagram, only with
Illustration illustrates basic structure of the invention, therefore it only shows the composition relevant to the invention.
Fig. 1 is the surface topography schematic diagram of composite diaphragm of the invention.
Embodiment 1
See that Fig. 1, the present embodiment 1 provide a kind of composite diaphragm, comprising: porous polyolefin class diaphragm and be sprayed on porous poly-
The ceramic layer of olefines membrane surface.
Optionally, see that Fig. 1, the ceramic layer include: several ceramics for being stacked each other on 1 surface of porous polyolefin class diaphragm
Particle 2；Wherein the ceramic particle 2 is fiber club shaped structure, and ulking thickness is 0.1-10 microns, preferably 5 microns, 8 micro-
Rice；The length of the ceramic particle is 10 microns, and diameter is 100-400 nanometers, preferably 150 nanometers, 250 nanometers.
Optionally, the porosity of the composite diaphragm be 45-65%, preferably 50%.
Further, optionally, the porous polyolefin class diaphragm is PP diaphragm (polypropylene single-layer septum), PE diaphragm (gathers
Ethylene diaphragm), one or more of PP/PE/PP composite diaphragm.Wherein, the aperture of the porous polyolefin class diaphragm is
0.01-0.05 microns, preferably 0.03 micron；Porosity is 30-50%, preferably 35%, 45%.
In general, being mixed with binder since ceramic particle is largely that round or partial size is smaller and being coated in porous gather
After olefines membrane surface, easily blocking diaphragm hole to block lithium ion transport influences the charge-discharge performance of lithium ion battery
And cycle performance.Therefore, this composite diaphragm has excellent under the premise of keeping superior heat-stability and electrolyte wetability
Dimensional structure, more preferably comprehensive battery performance.Both having solved traditional paint-on technique easily causes ceramic particle unevenly distributed on diaphragm
The problem of, and improve the phenomenon that spherical ceramic easily blocks porous polyolefin class diaphragm hole.
In conclusion the composite diaphragm of the present embodiment 1 is by solving the surface of ceramic layer spraying porous polyolefin class diaphragm
The problem of ceramic particle of having determined is unevenly distributed；Ceramic particle can preferably connect with porous polyolefin class membrane surface simultaneously
Touching, it is more uniform and fine and close, make the composite diaphragm to be formed imbibition rate with higher and wetability, it is ensured that lithium ion it is fast
Speed transmission, realizes the charge and discharge under big multiplying power.In addition, ceramic layer has excellent thermal stability, composite diaphragm can be improved
Heat resistance.
Embodiment 2
On the basis of embodiment 1, the present embodiment 2 additionally provides a kind of preparation method of composite diaphragm, including walks as follows
It is rapid:
Step S1 prepares the rodlike silica dioxide granule of fiber；The rodlike silica dioxide granule of fiber is dissolved in bonding by step S2
In the mixed liquor that agent and solvent are formed, ceramic particle is formed；Step S3 is dispersed ceramic particle in mixed liquor
Liquid；Step S4, by dispersion liquid electrostatic spraying on the surface of porous polyolefin class diaphragm；And step S5, vacuum drying, obtain institute
State composite diaphragm (being also the rodlike silica composite diaphragm of fiber or lithium ion battery Ceramic Composite diaphragm in this application).Its
In, the process conditions of the electrostatic spraying (being also electrostatic spinning) are: the ejection rate of dispersion liquid is 0.1-2mL/h, outer processing
Making voltage is 10-30kV, and receiving distance is 10-20cm, and spray time is 1-12 hours, thick with the accumulation for controlling ceramic particle
Degree.
Optionally, the mass ratio of the binder and solvent is 1:20-50；The solid content of the dispersion liquid is 0.1-
10%.
Optionally, the binder is Kynoar, carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, polytetrafluoro
One or more of ethylene, polyacrylic acid formicester.
Optionally, the solvent is N, N- dimethyl pyrrolidone, n,N-Dimethylformamide, ethyl alcohol, acetone, deionization
One or more of water.
Specific structure and embodiment about composite diaphragm is referring to the related content of embodiment 1, and details are not described herein.
Embodiment 3
On the basis of embodiment 2, the present embodiment 3 provides the first the optional embodiment for preparing composite diaphragm,
Concrete operations include the following steps:
Step S1: it first combines using sol-gel method and electrostatic spinning technique and prepares silica dioxide gel fiber；Then
Full ceramic silica silicon nanofiber will be obtained after silica dioxide gel fiber calcination；It is rodlike that fiber is finally obtained after grinding
Silica dioxide granule.
Step S2: first mixing binder with solvent 1:20 in mass ratio, stirring to dissolution；It adds in step S1 and obtains
The rodlike SiO 2-ceramic particle of fiber；It is finally placed under room temperature mechanical stirring 8-12 hours, the ceramics tentatively dispersed
Particle.
Step S3: the further ultrasonic disperse 20-30min of the ceramic particle tentatively dispersed obtained in step S2 makes to make pottery
Porcelain particle is uniformly dispersed, and obtains the dispersion liquid that solid content is 0.1%.
Step S4: dispersion liquid obtained in step S3 is added in the syringe with stainless steel syringe needle, then by quiet
Electrospray obtains the equally distributed Ceramic Composite diaphragm of ceramic particle on the surface of porous polyolefin class diaphragm.Electrostatic spinning
Process conditions are: the ejection rate of dispersion liquid is 0.2mL/h, external working voltage 20kV, and receiving distance is 10cm, when spraying
Between be 4 hours.
Step S5: Ceramic Composite diaphragm made from step S4 is put into vacuum drying oven, in 60-80 DEG C of at a temperature of drying
Lithium ion battery Ceramic Composite diaphragm is finally made to completely remove remaining solvent in 6-12h.
Embodiment 4
On the basis of embodiment 2, the present embodiment 4 provides second of optional embodiment for preparing composite diaphragm,
Concrete operations include the following steps:
Step S1: it first combines using sol-gel method and electrostatic spinning technique and prepares silica dioxide gel fiber；Then
Full ceramic silica silicon nanofiber will be obtained after silica dioxide gel fiber calcination；It is rodlike that fiber is finally obtained after grinding
Silica dioxide granule.
Step S2: first mixing binder with solvent 1:25 in mass ratio, stirring to dissolution；It adds in step S1 and obtains
The rodlike SiO 2-ceramic particle of fiber；It is finally placed under room temperature mechanical stirring 8-12 hours, the ceramics tentatively dispersed
Particle.
Step S3: the further ultrasonic disperse 20-30min of the ceramic particle tentatively dispersed obtained in step S2 makes to make pottery
Porcelain particle is uniformly dispersed, and obtains the dispersion liquid that solid content is 0.2%.
Step S4: dispersion liquid obtained in step S3 is added in the syringe with stainless steel syringe needle, then by quiet
Electrospray obtains the equally distributed Ceramic Composite diaphragm of ceramic particle on the surface of porous polyolefin class diaphragm.Electrostatic spinning
Process conditions are: the ejection rate of dispersion liquid is 0.2mL/h, external working voltage 20kV, and receiving distance is 10cm, when spraying
Between be 4 hours.
Step S5: Ceramic Composite diaphragm made from step S4 is put into vacuum drying oven, in 60-80 DEG C of at a temperature of drying
Lithium ion battery Ceramic Composite diaphragm is finally made to completely remove remaining solvent in 6-12h.
Embodiment 5
On the basis of embodiment 2, the present embodiment 5 provides the third the optional embodiment for preparing composite diaphragm,
Concrete operations include the following steps:
Step S1: it first combines using sol-gel method and electrostatic spinning technique and prepares silica dioxide gel fiber；Then
Full ceramic silica silicon nanofiber will be obtained after silica dioxide gel fiber calcination；It is rodlike that fiber is finally obtained after grinding
Silica dioxide granule.
Step S2: first mixing binder with solvent 1:50 in mass ratio, stirring to dissolution；It adds in step S1 and obtains
The rodlike SiO 2-ceramic particle of fiber；It is finally placed under room temperature mechanical stirring 8-12 hours, the ceramics tentatively dispersed
Particle.
Step S3: the further ultrasonic disperse 20-30min of the ceramic particle tentatively dispersed obtained in step S2 makes to make pottery
Porcelain particle is uniformly dispersed, and obtains the dispersion liquid that solid content is 0.3%.
Step S4: dispersion liquid obtained in step S3 is added in the syringe with stainless steel syringe needle, then by quiet
Electrospray obtains the equally distributed Ceramic Composite diaphragm of ceramic particle on the surface of porous polyolefin class diaphragm.Electrostatic spinning
Process conditions are: the ejection rate of dispersion liquid is 0.2mL/h, external working voltage 20kV, and receiving distance is 10cm, when spraying
Between be 4 hours.
Step S5: Ceramic Composite diaphragm made from step S4 is put into vacuum drying oven, in 60-80 DEG C of at a temperature of drying
Lithium ion battery Ceramic Composite diaphragm is finally made to completely remove remaining solvent in 6-12h.
Embodiment 6
Due to length, is only listed in embodiment 3-5 and prepare some embodiments of composite diaphragm, the system of the application
Preparation Method contains numerous embodiments, and main component dosage is as shown in table 1, specific operation process referring to embodiment 3 phase
Hold inside the Pass, details are not described herein.
Main component and dosage in 1 preparation method of table
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (10)
1. a kind of composite diaphragm characterized by comprising
Porous polyolefin class diaphragm and the ceramic layer for being sprayed on porous polyolefin class membrane surface.
2. composite diaphragm according to claim 1, which is characterized in that
The ceramic layer includes: several ceramic particles for being stacked each other on porous polyolefin class membrane surface；Wherein
The ceramic particle is fiber club shaped structure.
3. composite diaphragm according to claim 2, which is characterized in that
The ulking thickness of the ceramic particle is 0.1-10 microns；And
The length of the ceramic particle is 10 microns, and diameter is 100-400 nanometers.
4. composite diaphragm according to claim 1, which is characterized in that
The porous polyolefin class diaphragm is one or more of PP diaphragm, PE diaphragm, PP/PE/PP composite diaphragm.
5. composite diaphragm according to claim 1, which is characterized in that
The aperture of the porous polyolefin class diaphragm is 0.01-0.05 microns, porosity 30-50%.
6. composite diaphragm according to claim 1, which is characterized in that
The porosity of the composite diaphragm is 45-65%.
7. a kind of preparation method of composite diaphragm characterized by comprising
Prepare the rodlike silica dioxide granule of fiber；
The rodlike silica dioxide granule of fiber is dissolved in the mixed liquor that binder and solvent are formed, forms ceramic particle；
Ceramic particle is dispersed to obtain dispersion liquid in mixed liquor；
By dispersion liquid electrostatic spraying on the surface of porous polyolefin class diaphragm；And
Vacuum drying obtains the composite diaphragm.
8. preparation method according to claim 7, which is characterized in that
The mass ratio of the binder and solvent is 1:20-50；
The solid content of the dispersion liquid is 0.1-10%.
9. preparation method according to claim 7, which is characterized in that
The binder is Kynoar, carboxymethyl cellulose, polyvinyl alcohol, ethyl cellulose, polytetrafluoroethylene (PTFE), polypropylene
One or more of sour formicester.
10. preparation method according to claim 7, which is characterized in that
The solvent is N, one of N- dimethyl pyrrolidone, N,N-dimethylformamide, ethyl alcohol, acetone, deionized water
Or it is several.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910034190.1A CN109659477A (en) | 2019-01-15 | 2019-01-15 | Rodlike silica composite diaphragm of fiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910034190.1A CN109659477A (en) | 2019-01-15 | 2019-01-15 | Rodlike silica composite diaphragm of fiber and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109659477A true CN109659477A (en) | 2019-04-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910034190.1A Pending CN109659477A (en) | 2019-01-15 | 2019-01-15 | Rodlike silica composite diaphragm of fiber and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111725468A (en) * | 2020-06-15 | 2020-09-29 | 长春工业大学 | Silicon dioxide inorganic nanoparticle reinforced polyolefin diaphragm and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102218871A (en) * | 2011-04-14 | 2011-10-19 | 万向电动汽车有限公司 | Preparation method of modified diaphragm for lithium-ion secondary battery as well as product and preparation device thereof |
| CN104409674A (en) * | 2014-12-08 | 2015-03-11 | 清华大学 | Composite diaphragm material and preparation method and application thereof |
| WO2015084951A1 (en) * | 2013-12-04 | 2015-06-11 | Cornell University | Ceramic-polymer hybrid nanostructures, methods for producing and applications thereof |
| CN106159163A (en) * | 2016-08-31 | 2016-11-23 | 合肥国轩高科动力能源有限公司 | A kind of power lithium-ion battery ceramic coating membrane and preparation method |
-
2019
- 2019-01-15 CN CN201910034190.1A patent/CN109659477A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102218871A (en) * | 2011-04-14 | 2011-10-19 | 万向电动汽车有限公司 | Preparation method of modified diaphragm for lithium-ion secondary battery as well as product and preparation device thereof |
| WO2015084951A1 (en) * | 2013-12-04 | 2015-06-11 | Cornell University | Ceramic-polymer hybrid nanostructures, methods for producing and applications thereof |
| CN104409674A (en) * | 2014-12-08 | 2015-03-11 | 清华大学 | Composite diaphragm material and preparation method and application thereof |
| CN106159163A (en) * | 2016-08-31 | 2016-11-23 | 合肥国轩高科动力能源有限公司 | A kind of power lithium-ion battery ceramic coating membrane and preparation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111725468A (en) * | 2020-06-15 | 2020-09-29 | 长春工业大学 | Silicon dioxide inorganic nanoparticle reinforced polyolefin diaphragm and application thereof |
| CN111725468B (en) * | 2020-06-15 | 2022-05-17 | 长春工业大学 | Silicon dioxide inorganic nanoparticle reinforced polyolefin diaphragm and application thereof |
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