CN109449357A - A kind of lithium battery diaphragm, preparation method and electrostatic spinning apparatus - Google Patents
A kind of lithium battery diaphragm, preparation method and electrostatic spinning apparatus Download PDFInfo
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- CN109449357A CN109449357A CN201811311216.4A CN201811311216A CN109449357A CN 109449357 A CN109449357 A CN 109449357A CN 201811311216 A CN201811311216 A CN 201811311216A CN 109449357 A CN109449357 A CN 109449357A
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- Prior art keywords
- spinneret
- lithium battery
- pole piece
- battery diaphragm
- 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
- H01M50/411—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
- H01M50/44—Fibrous material
-
- 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
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a kind of lithium battery diaphragms, in parts by weight, including 93~96 parts of N, N- dimethylformamide, 10~13 parts of polyacrylonitrile, 1~2 part of lanthana acid lithium；1) by N, N- dimethylformamide and polyacrylonitrile powder mixing, solution is made；2) in N, lanthana acid lithium powder is added in the mixed solution of N- dimethylformamide and polyacrylonitrile, is stirred for uniformly using blender；3) mixed solution is placed in electrostatic spinning apparatus, the unidirectional spinneret of progress sequence first carries out transverse reciprocating spinneret, after reaching the end, then carries out longitudinally reciprocal spinneret, until returning to starting point；Then continue spinneret next time, fiber tool is made to have three layers；The technological parameter of electrostatic spinning apparatus are as follows: 15~20KV of electrostatic pressure, 0.2~0.71ml/h of jet velocity, receiving distance is 16cm；4) after spinneret fiber after molding being dried in vacuo 5h at 45 DEG C, that is, preparation is completed.Its structural strength is big, imbibition ability is strong, ionic conductivity is high, and prepares fast and easy.
Description
Technical field
The present invention relates to lithium batteries, and in particular to a kind of lithium battery diaphragm, preparation method and electrostatic spinning apparatus.
Background technique
The battery core of lithium ion battery is mainly made of positive electrode, negative electrode material, diaphragm and electrolyte.Its septation is electricity
The important component of core, it can separate battery plus-negative plate, and have electronic isolation and ionic conductivity.The performance of diaphragm
It determines the interfacial structure of battery, the retentivity of electrolyte and internal resistance of battery etc., and then influences the capacity of battery, cyclicity
The key characteristics such as energy, charging and discharging currents density.In addition, diaphragm also has large effect to the safety of battery.So diaphragm
The superiority and inferiority of performance directly affects the comprehensive performance of battery.The diaphragm synthesis of general polyacrylonitrile system is simple, heat resistance is high, no
The advantages that easy firing, stability are good.But due to the presence of this highly polar group of-CN, lead to PAN and metal electrode compatibility
Difference makes that serious passivation phenomenon occurs between gel polymer electrolyte and metal lithium electrode, causes battery internal resistance can be by
It is cumulative big, influence the use of battery.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of lithium battery diaphragm, preparation method and electrostatic spinning apparatus,
Structural strength is big, imbibition ability is strong, ionic conductivity is high, and prepares fast and easy.
In order to solve the above-mentioned technical problems, the present invention provides a kind of lithium battery diaphragm, in the formula of diaphragm, according to weight
Number meter, including
93~96 parts of N, N- dimethylformamide
10~13 parts of polyacrylonitrile
1~2 part of lanthana acid lithium.
Preferably, the fiber overlapping that the diaphragm is obtained by multilayer by electrostatic spinning forms.
Preferably, the diameter of the fiber is 150nm~500nm.
Preferably, the direction of fiber described in single layer is that continuous transverse-connection longitudinal direction or continuous longitudinal direction-connection are lateral.
A kind of preparation method of lithium battery diaphragm, comprising the following steps:
1) by N, N- dimethylformamide and polyacrylonitrile powder mixing, solution is made；
2) in N, lanthana acid lithium powder is added in the mixed solution of N- dimethylformamide and polyacrylonitrile, using blender
It is stirred for uniformly；
3) mixed solution being placed in electrostatic spinning apparatus, the unidirectional spinneret of progress sequence first carries out transverse reciprocating spinneret,
After reaching the end, then longitudinally reciprocal spinneret is carried out, until returning to starting point；Then continue spinneret next time, fiber is made to have 3
Layer；The technological parameter of electrostatic spinning apparatus are as follows: 15~20KV of electrostatic pressure, 0.2~0.71ml/h of jet velocity, receiving distance is
16cm；
4) after spinneret fiber after molding being dried in vacuo 5h at 45 DEG C, that is, preparation is completed.
Electrostatic spinning apparatus used in a kind of preparation method of lithium battery diaphragm, including it is spinneret pump, syringe, laterally driven
Pole piece, zigzag tread patterns pole piece and receiver board, the syringe are vertically arranged on spinneret pump, and the receiver board is horizontally set on syringe
Lower section, the laterally driven pole piece and zigzag tread patterns pole piece are arranged between syringe and receiver board, and the syringe is outer added with height
Voltage source, the reception plate earthing are circumscribed with laterally driven voltage on the laterally driven pole piece, on the zigzag tread patterns pole piece
It is circumscribed with zigzag tread patterns voltage.
Preferably, the laterally driven pole piece and zigzag tread patterns pole piece are mutually perpendicular to.
Compared with prior art, the beneficial effects of the present invention are:
1, lithium battery diaphragm of the invention has high mechanical tensile strength, can keep battery structure for a long time
Stability, improve the service life of battery；With high porosity, battery electrolyte can be preferably absorbed, lithium is made
The resistance of battery is extremely low；With good ionic conductivity and specific discharge capacity, makes lithium ion more easily by battery diaphragm, increase
It is powered on the power in pond.
2, the present invention is by by N, N- dimethylformamide, polyacrylonitrile and lanthana acid lithium, make its when fiber is at silk more
What is added is reliable and stable；Using specific electrostatic pressure, jet velocity and distance is received, the nano-scale fiber of even thickness can be manufactured
Silk；By reciprocal spinneret laterally, longitudinal, keeps fiber architecture regular, improve its structural strength, imbibition ability.
3, the present invention is between syringe and receiver board by increasing voltage, makes what fiber filament was more easier to fall on receiver board
On；By the way that laterally driven pole piece and zigzag tread patterns pole piece are arranged above receiver board, keep filametntary drop point controllable, so as to
Fiber filament is stacked on vertical and horizontal direction as needed, increases the structural strength and imbibition ability of diaphragm.
Detailed description of the invention
It, below will be in embodiment technical description for the clearer technical solution illustrated in technology of the embodiment of the present invention
Required attached drawing is briefly described, it should be apparent that, the accompanying drawings in the following description is only some realities of the invention
Example is applied, for those of ordinary skill in the art, without creative efforts, additionally it is possible to according to these attached drawings
Obtain other attached drawings.
Fig. 1 is the structural schematic diagram of lithium battery diaphragm；
Fig. 2 is the structural schematic diagram of electrostatic spinning apparatus.
Wherein, 1- spinneret pumps, 2- syringe, the laterally driven pole piece of 3-, 4- zigzag tread patterns pole piece, 5- receiver board.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Whole description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment during this is practical, those of ordinary skill in the art are obtained all without creative labor
Other embodiments shall fall within the protection scope of the present invention.
Embodiment 1
A kind of lithium battery diaphragm is disclosed in embodiment 1, according to number poidometer, formula is as shown in table 1.
The formula table of 1. embodiment 1 of table
| Component | Content (parts by weight) |
| N, N- dimethylformamide | 93 |
| Polyacrylonitrile | 10 |
| Lanthana acid lithium | 1 |
Embodiment 2
A kind of lithium battery diaphragm is disclosed in embodiment 2, according to number poidometer, formula is as shown in table 2.
The formula table of 2. embodiment 2 of table
| Component | Content (parts by weight) |
| N, N- dimethylformamide | 93 |
| Polyacrylonitrile | 10 |
| Lanthana acid lithium | 2 |
Embodiment 3
A kind of lithium battery diaphragm is disclosed in embodiment 3, according to number poidometer, formula is as shown in table 3.
The formula table of 3. embodiment 3 of table
| Component | Content (parts by weight) |
| N, N- dimethylformamide | 93 |
| Polyacrylonitrile | 11 |
| Lanthana acid lithium | 1 |
Embodiment 4
A kind of lithium battery diaphragm is disclosed in embodiment 4, according to number poidometer, formula is as shown in table 4.
The formula table of 4. embodiment 4 of table
| Component | Content (parts by weight) |
| N, N- dimethylformamide | 93 |
| Polyacrylonitrile | 13 |
| Lanthana acid lithium | 1 |
Embodiment 5
A kind of lithium battery diaphragm is disclosed in embodiment 5, according to number poidometer, formula is as shown in table 5.
The formula table of 5. embodiment 5 of table
Embodiment 6
A kind of lithium battery diaphragm is disclosed in embodiment 6, according to number poidometer, formula is as shown in table 6.
The formula table of 6. embodiment 6 of table
| Component | Content (parts by weight) |
| N, N- dimethylformamide | 94 |
| Polyacrylonitrile | 10 |
| Lanthana acid lithium | 1 |
Embodiment 7
A kind of lithium battery diaphragm is disclosed in embodiment 7, according to number poidometer, formula is as shown in table 7.
The formula table of 7. embodiment 7 of table
| Component | Content (parts by weight) |
| N, N- dimethylformamide | 95 |
| Polyacrylonitrile | 10 |
| Lanthana acid lithium | 1 |
Embodiment 8
A kind of lithium battery diaphragm is disclosed in embodiment 8, according to number poidometer, formula is as shown in table 8.
The formula table of 8. embodiment 8 of table
1~embodiment of above-described embodiment 8 is all made of method of electrostatic spinning and prepares lithium battery diaphragm.The diameter of its fiber is about
150nm~500nm.
Shown in referring to Fig.1, the machine direction of single layer is continuous transverse-continuously longitudinal direction or continuous longitudinal direction-continuous transverse, more
Layer fiber is overlapping together, becomes lithium battery diaphragm.Its high mechanical strength, ionic conductivity are high, specific discharge capacity is high, have
Excellent electrochemical stability and cycle performance.
Since there is polyacrylonitrile highly polar group-CN to be easy to happen so it is poor with metal lithium electrode compatibility
Passivation phenomenon, and N, N- dimethylformamide can alleviate this phenomenon just, and keep it more reliable and more stable when fiber is at silk.
The addition of lanthana acid lithium then substantially increases the ionic conductivity and specific discharge capacity of lithium battery diaphragm.
1~embodiment of above-described embodiment 8 is tested for the property, table 9 can be obtained.
1) tensile strength: diaphragm should have good mechanical property, to maintain the structural integrity of lithium battery for a long time, prolong
The service life of long battery.
2) porosity: the hole of diaphragm is directly affected the mouth imbibition ability of film, and then imbibition ability is strong for porosity height.
3) ionic conductivity: ionic conductivity is the precondition that diaphragm forms charge, has ionic conductivity just to can guarantee
Ion in electrolyte sufficiently passes through, charge required for being formed.Conductivity height is just able to achieve the target by big electric current.
4) specific discharge capacity: specific discharge capacity is the physical quantity for measuring lithium battery discharging efficiency.
The performance comparison of each embodiment of table 9.
Prepare lithium battery diaphragm in 1~embodiment of above-described embodiment 8 the preparation method comprises the following steps:
1) by N, N- dimethylformamide and polyacrylonitrile powder mixing, solution is made；
2) in N, lanthana acid lithium powder is added in the mixed solution of N- dimethylformamide and polyacrylonitrile, using blender
It is stirred for uniformly；
3) mixed solution being placed in electrostatic spinning apparatus, the unidirectional spinneret of progress sequence first carries out transverse reciprocating spinneret,
After reaching the end, then longitudinally reciprocal spinneret is carried out, until returning to starting point；Then continue spinneret next time, fiber is made to have 3
Layer；The technological parameter of electrostatic spinning apparatus are as follows: 15~20KV of electrostatic pressure, 0.2~0.71ml/h of jet velocity, receiving distance is
16cm；
4) after spinneret fiber after molding being dried in vacuo 5h at 45 DEG C, that is, preparation is completed.
Referring to shown in Fig. 2, above-mentioned electrostatic spinning apparatus, including spinneret pump 1, syringe 2, laterally driven pole piece 3, zigzag tread patterns
Pole piece 4 and receiver board 5.Syringe 2 is vertically arranged on spinneret pump 1.Spinneret pump 1 can needle cylinder 2 carry out spinneret, control simultaneously
The spinneret amount of syringe 2.It is outer added with high voltage power supply U1 on syringe 2, the solution in syringe 2 can be made to charge.5 level of receiver board is put
It sets, is grounded.The fiber filament that syringe 2 sprays can be fallen on receiver board 5 under the action of electric field U1.Laterally driven 3 He of pole piece
Zigzag tread patterns pole piece 4 is respectively positioned between syringe 2 and receiver board 5, and laterally driven source piece 3 and zigzag tread patterns pole piece 4 mutually hang down
Directly.The laterally driven voltage U3 of driving fiber filament horizontal swing is connected between the laterally driven pole piece 3 of two panels.Two panels zigzag tread patterns
The zigzag tread patterns voltage U2 of driving fiber filament longitudinal oscillation is connected between pole piece 4.By changing laterally driven voltage U3 and indulging
To driving voltage U2, fiber filament can be made to swing along predetermined direction, keep fiber filament more uniform reliable.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to consistent with principles disclosed herein and novel point
Widest scope.
Claims (7)
1. a kind of lithium battery diaphragm, which is characterized in that in the formula of diaphragm, in parts by weight, including
93~96 parts of N, N- dimethylformamide
10~13 parts of polyacrylonitrile
1~2 part of lanthana acid lithium.
2. lithium battery diaphragm as described in claim 1, which is characterized in that the diaphragm is obtained by multilayer by electrostatic spinning
Fiber overlapping composition.
3. lithium battery diaphragm as claimed in claim 2, which is characterized in that the diameter of the fiber is 150nm~500nm.
4. lithium battery diaphragm as claimed in claim 2, which is characterized in that the direction of fiber described in single layer is continuous transverse-company
It is lateral to connect longitudinal or continuous longitudinal direction-connection.
5. a kind of preparation method of lithium battery diaphragm described in claim 1-4 any one, which is characterized in that including following step
It is rapid:
1) by N, N- dimethylformamide and polyacrylonitrile powder mixing, solution is made；
2) in N, lanthana acid lithium powder is added in the mixed solution of N- dimethylformamide and polyacrylonitrile, using blender by its
It stirs evenly；
3) mixed solution is placed in electrostatic spinning apparatus, the unidirectional spinneret of progress sequence first carries out transverse reciprocating spinneret, reaches
After the end, then longitudinally reciprocal spinneret is carried out, until returning to starting point；Then continue spinneret next time, fiber tool is made to have three layers；It is quiet
The technological parameter of electric spinning device are as follows: 15~20KV of electrostatic pressure, 0.2~0.71ml/h of jet velocity, receiving distance is 16cm；
4) after spinneret fiber after molding being dried in vacuo 5h at 45 DEG C, that is, preparation is completed.
6. electrostatic spinning apparatus used in a kind of preparation method of lithium battery diaphragm described in claim 5, which is characterized in that
Including spinneret pump, syringe, laterally driven pole piece, zigzag tread patterns pole piece and receiver board, the syringe is vertically arranged on spinneret pump,
The receiver board is horizontally set below syringe, and the laterally driven pole piece and zigzag tread patterns pole piece are arranged at syringe and reception
Between plate, the syringe is outer added with high voltage power supply, the reception plate earthing, is circumscribed on the laterally driven pole piece laterally driven
Voltage is circumscribed with zigzag tread patterns voltage on the zigzag tread patterns pole piece.
7. electrostatic spinning apparatus used in the preparation method of lithium battery diaphragm as claimed in claim 6, which is characterized in that institute
It states laterally driven pole piece and zigzag tread patterns pole piece is mutually perpendicular to.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811311216.4A CN109449357A (en) | 2018-11-06 | 2018-11-06 | A kind of lithium battery diaphragm, preparation method and electrostatic spinning apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811311216.4A CN109449357A (en) | 2018-11-06 | 2018-11-06 | A kind of lithium battery diaphragm, preparation method and electrostatic spinning apparatus |
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| Publication Number | Publication Date |
|---|---|
| CN109449357A true CN109449357A (en) | 2019-03-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811311216.4A Pending CN109449357A (en) | 2018-11-06 | 2018-11-06 | A kind of lithium battery diaphragm, preparation method and electrostatic spinning apparatus |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110158164A (en) * | 2019-05-23 | 2019-08-23 | 天津工业大学 | Polyacrylonitrile nanofiber film and preparation method thereof, flexible piezoelectric nano generator and preparation method thereof |
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|---|---|---|---|---|
| US20050003277A1 (en) * | 2003-07-01 | 2005-01-06 | Samsung Sdi Co., Ltd. | Negative electrode for lithium secondary battery, method of preparing same, and lithium secondary battery comprising same |
| CN104538577A (en) * | 2015-01-28 | 2015-04-22 | 中国科学院宁波材料技术与工程研究所 | Composite diaphragm and preparation method thereof |
| CN107699965A (en) * | 2017-09-07 | 2018-02-16 | 浙江大学 | Right-angled intersection stacks nanofiber array preparation method |
| CN108365152A (en) * | 2017-12-27 | 2018-08-03 | 清华大学 | A kind of composite diaphragm for lithium battery |
-
2018
- 2018-11-06 CN CN201811311216.4A patent/CN109449357A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050003277A1 (en) * | 2003-07-01 | 2005-01-06 | Samsung Sdi Co., Ltd. | Negative electrode for lithium secondary battery, method of preparing same, and lithium secondary battery comprising same |
| CN104538577A (en) * | 2015-01-28 | 2015-04-22 | 中国科学院宁波材料技术与工程研究所 | Composite diaphragm and preparation method thereof |
| CN107699965A (en) * | 2017-09-07 | 2018-02-16 | 浙江大学 | Right-angled intersection stacks nanofiber array preparation method |
| CN108365152A (en) * | 2017-12-27 | 2018-08-03 | 清华大学 | A kind of composite diaphragm for lithium battery |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110158164A (en) * | 2019-05-23 | 2019-08-23 | 天津工业大学 | Polyacrylonitrile nanofiber film and preparation method thereof, flexible piezoelectric nano generator and preparation method thereof |
| CN110158164B (en) * | 2019-05-23 | 2020-11-03 | 天津工业大学 | Polyacrylonitrile nanofiber membrane and preparation method thereof, flexible piezoelectric nano generator and preparation method thereof |
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Application publication date: 20190308 |