CN110286075A - A kind of test method of lithium ion battery separator closed pore temperature - Google Patents
A kind of test method of lithium ion battery separator closed pore temperature Download PDFInfo
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- CN110286075A CN110286075A CN201910507345.9A CN201910507345A CN110286075A CN 110286075 A CN110286075 A CN 110286075A CN 201910507345 A CN201910507345 A CN 201910507345A CN 110286075 A CN110286075 A CN 110286075A
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- 239000011148 porous material Substances 0.000 title claims abstract description 57
- 238000010998 test method Methods 0.000 title claims abstract description 21
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 230000003252 repetitive effect Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- 230000009989 contractile response Effects 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 19
- 230000008859 change Effects 0.000 abstract description 11
- 239000012530 fluid Substances 0.000 abstract description 10
- 239000003792 electrolyte Substances 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 abstract description 3
- 230000035772 mutation Effects 0.000 abstract description 3
- -1 polyethylene Polymers 0.000 description 6
- 239000004698 Polyethylene Substances 0.000 description 5
- 239000004743 Polypropylene Substances 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 229920001155 polypropylene Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000013102 re-test Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000004801 process automation Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004260 weight control Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/0806—Details, e.g. sample holders, mounting samples for testing
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
- G01N2013/0208—Investigating surface tension of liquids by measuring contact angle
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
- G01N2013/0283—Investigating surface tension of liquids methods of calculating surface tension
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/086—Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention discloses the test methods of lithium ion battery separator closed pore temperature, comprising the following steps: (1) cuts out the diaphragm sample of default size；(2) preheating temperature is heated to diaphragm sample；(3) diaphragm sample is placed in pressure water instrument and is loaded in the sample cell of water, test temperature is gradually increased, at interval of the porosity of the diaphragm in 15s record sample cell, when the porosity of diaphragm sample is 0, thus as corresponding diaphragm closed pore temperature when the porosity for obtaining diaphragm sample is 0.It uses water as test fluid in the present invention, using the principle of pressure water instrument, sudden change of resistivity method is replaced by the mutation method of hydraulic pressure and water volume, does not need to influence test result using electrolyte, it is repeated and comparative good.
Description
Technical field
The invention belongs to technical field of lithium-ion battery, more particularly, to a kind of lithium ion battery separator closed pore temperature
Test method.
Background technique
Diaphragm is one of the four big key materials for forming lithium ion battery, and being mainly used for isolation positive and negative electrode material prevents
It forms internal short-circuit and allows lithium ion freely through.Therefore, the characteristic of diaphragm for lithium ion battery performance, such as times
Rate performance, cycle performance and security performance etc. have important influence.
Closed pore temperature is one of key property of diaphragm, and the overriding concern to guarantee safety applied to lithium ion battery
Index.In order to ensure passing freely through for lithium ion, can commercially use diaphragm all there is the microcellular structure largely penetrated through, electricity
Since violent electrochemical reaction can generate a large amount of Joule heat when the internal short-circuit of pond, when temperature reaches the closed pore temperature of diaphragm
When, diaphragm can hinder passing through for lithium ion by shrinking closed pore, so that the internal resistance of cell steeply rises and avoids further
The generation of thermal runaway, therefore, selecting has the diaphragm of suitable closed pore temperature significant to guarantee battery security.
Currently, generally testing the closed pore temperature of diaphragm using sudden change of resistivity method, Permeability gauge or scanning electron microscope.Wherein, it adopts
The test device used is disclosed with the patent of sudden change of resistivity method, such as Publication No. CN101221140A to fix diaphragm sample
And soaked with electrolyte, resistance variations of the re-test test device under Elevated Temperature Conditions, utilize sudden change of resistivity point later
Judge the closed pore temperature of diaphragm, although sudden change of resistivity method has feasibility, its limitation is fairly obvious, in addition, because of diaphragm
Closed pore temperature is at 130 DEG C -150 DEG C or so, and electrolyte can volatilize and decompose during being heated to target temperature, and electrolyte subtracts
It will also result in resistance increase less, test result produced bigger effect, so that the diaphragm closed pore temperature inaccuracy of test；Make
Diaphragm sample is tested with Permeability gauge, is merely able to reflect diaphragm resistance value, and the variation of membrane pore size can not be reacted, and it also requires
Internal resistance is measured using accurate internal resistance instrument, testing cost is high；Using scanning electron microscope, the degree for testing diaphragm closed pore is difficult to symbolize
Come, and testing efficiency is low.
Summary of the invention
A kind of it is an object of the invention to overcome the deficiencies of the prior art and provide structures simple, easy to operate, testing efficiency
The test method of high, test fluid environmental protection lithium ion battery separator closed pore temperature.
Technical scheme is as follows:
A kind of test method of lithium ion battery separator closed pore temperature, comprising the following steps:
(1) the diaphragm sample of default size is cut out；
(2) preheating temperature is heated to diaphragm sample；
(3) diaphragm sample is placed in pressure water instrument and is loaded in the sample cell of water, test temperature, interval note is gradually increased
The porosity for recording the diaphragm in sample cell illustrates that diaphragm has begun and closes when obvious contractile response occurs for diaphragm sample
Hole reaction, when the porosity of diaphragm sample is 0, corresponding test temperature is diaphragm closed pore temperature.
In the above-mentioned technical solutions, step described in repetitive operation (1)-(3) at least 3 times, and according to the closed pore obtained every time
Closed pore temperature of the average value of temperature as diaphragm sample.
In the above-mentioned technical solutions, the preheating temperature in the step (2) is 120 DEG C -200 DEG C.
In the above-mentioned technical solutions, diaphragm sample is heated using baking oven in the step (2).
In the above-mentioned technical solutions, baking oven 10min heating and continuous to diaphragm sample.
In the above-mentioned technical solutions, pass through the air pressure of the gas of diaphragm sample in the step (3) in pressure water instrument in 0-
It is gradually increased within the scope of 1500psi, the rate of pressurization is 2psi/s.
In the above-mentioned technical solutions, the interval time recorded in the step (3) is at interval of 15s.
In the above-mentioned technical solutions, in the step (3), if the closed pore of diaphragm measured by any 2 repetitive operations
When the difference of temperature is more than 3 DEG C, then this 2 times operations are accordingly to be regarded as unqualified test and need to retest.
In the above-mentioned technical solutions, the size range of the diaphragm sample is length: 40cm-60cm, width: 30cm-50cm.
It is a further object to provide a kind of pressure water instrument answering in measurement lithium ion battery separator closed pore temperature
With.
The advantages and positive effects of the present invention are:
1. water is used to replace passing by the mutation method of porosity using the principle of pressure water instrument as test fluid in the present invention
The closed pore temperature of the sudden change of resistivity method test diaphragm of system, does not need that electrolyte is used to influence test result as test fluid, surveys
Examination repeatability and it is comparative good.
2. water is as test fluid when being pressed into diaphragm, the range for applying hydraulic pressure is small and mild, makes when testing diaphragm sample
At deformation it is smaller so that testing the time of day closer to sample, sample may be reused.
3. the porosity and pore-size distribution of diaphragm can be calculated in the pressure water instrument used by hydraulic pressure and water volume, test
Sample it is full-featured.
4. test fluid is pollution-free, test process automation degree is high, and testing cost is low.
Detailed description of the invention
Fig. 1 is the temperature porosity change curve graph of the test diaphragm of embodiment 1.
Specific embodiment
Below in conjunction with specific embodiment, invention is further described in detail.It should be appreciated that described herein specific
Embodiment is used only for explaining the present invention, is not intended to limit the present invention, is never limited in protection scope of the present invention.
Embodiment 1
As shown in Figure 1, a kind of test method of lithium ion battery separator closed pore temperature of the invention, presses water instrument using PMI
It is tested, comprising the following steps:
(1) diaphragm sample is cut out into the diaphragm sample for 40cm*30cm, wherein using diaphragm sample made of PE material,
Weight is 1g；
(2) 120 DEG C of preheating temperature are heated to diaphragm sample by baking oven, continue 10min, wherein the heating temperature of baking oven
Range is 120 DEG C -200 DEG C, and heating rate is 1 DEG C/min；
(3) diaphragm sample is placed in pressure water instrument and is loaded in the sample cell of water, test temperature is gradually increased from 120 DEG C
(test temperature increases by 0.1 DEG C every time), the porosity of interval 15s record sample cell inner septum, when test temperature is improved to 125 DEG C
When, there is obvious contractile response in diaphragm sample, gradually starts closed pore, continues to improve test temperature, when test temperature is improved to 134
DEG C when, the porosity of diaphragm sample is 0, is illustrated at 134 DEG C, diaphragm complete closed pore, then 0 point of the porosity of diaphragm sample
The corresponding diaphragm closed pore temperature of Shi Zuowei.
(4) repetitive operation step (1)-(3) 3 times, and according to the average value of the closed pore temperature obtained every time as diaphragm sample
The closed pore temperature of product.
Further say, if the difference of initial closed pore temperature measured by any 2 repetitive operations is more than 3 DEG C,
This 2 times operations are accordingly to be regarded as unqualified test and need to retest.
It further says, passes through the air pressure of the gas of diaphragm sample in step (3) in pressure water instrument within the scope of 0-1500psi
It gradually increases, the rate of pressurization is 2psi/s.
Wherein, pressure water instrument is introduced and (presses water instrument using PMI in the present invention):
Pressure water instrument is the instrument using water or other non-compatibility fluid test sample pore structures, reuses water as test
When liquid, water is squeezed under the effect of the pressure in sample aperture, and the corresponding pressure of the water squeezed into different pore size follows
Washburn equation, thus through being calculated pore structure parameter (i.e. pore-size distribution, pore volume and distribution, porosity and distribution,
Pore specific surface area and Kong Qudu).
The Computing Principle that pressure water instrument measuring diaphragm obtains diaphragm porosity is, corresponding at various pressures to enter different pore size
Interior water volume is calculated according to the surface tension and contact angle of the data and test fluid of water volume and pressure according to formula
Diaphragm porosity:
φ=V* ρ * 100%
Wherein, φ represents diaphragm porosity；
V is accumulative water volume；ρ is bulk density；The aperture of diaphragm sample is calculated by pressure and water volume.
Herein it should be noted that the diaphragm sample of pressure water instrument measurement is 40cm*30cm for the size cut out, Weight control exists
0.8-1g can be put into multi-disc sample in pressure water instrument, control the diaphragm example weight being put into if weight is insufficient.
Test temperature is continuously improved to the test of diaphragm sample, by pressing the measurement of water instrument to obtain diaphragm porosity in test temperature
Change curve under degree, obtains temperature-porosity characterization.As seen in Figure 1, corresponding to the point in porosity for zero
Temperature is 134.2 DEG C, i.e., diaphragm sample is tested in the 134.2 DEG C closed pore temperatures for diaphragm sample, repetitive operation above-mentioned steps (1)-(3)
Product acquire average value according to obtained closed pore temperature, to obtain the closed pore temperature of more accurate diaphragm.
Diaphragm porosity is obtained by pressure water instrument measurement, and diaphragm closed pore temperature is obtained according to the variation of diaphragm porosity,
It can measure different types of diaphragm and obtain diaphragm closed pore temperature, using the applied widely of above-mentioned test method, and use
Water is as test fluid, using the principle of pressure water instrument, replaces traditional sudden change of resistivity method to test diaphragm by the mutation method of porosity
Closed pore temperature, do not need that electrolyte is used to influence test result as test fluid, test repeatability and it is comparative good.
Embodiment 2
On the basis of embodiment 1, dry to polyethylene wet process diaphragm, polypropylene respectively using the test method of embodiment 1
Method diaphragm, polyethylene/polypropylene meet the test that diaphragm carries out closed pore temperature, repeat to be averaged after being measured by sampling 6 times, obtain
The test data of three kinds of diaphragm samples, specific test data are shown in Tables 1 and 2:
Table 1: the closed pore temperature initial data of test diaphragm sample
Table 2: according to the closed pore temperature for the diaphragm sample that the initial data of table 1 acquires
As can be seen from Table 2, the closed pore temperature of polyethylene wet process diaphragm and polypropylene dry method diaphragm is higher, security performance compared with
Difference, and the closed pore temperature of polyethylene/polypropylene composite diaphragm is lower closed pore and can keep structure complete rapidly under the high temperature conditions
Whole property, security performance are relatively preferable.
Embodiment 3
In order to verify beneficial effects of the present invention, respectively using the present invention in test method and sudden change of resistivity method to poly- second
Alkene wet process diaphragm carries out the contrast test of closed pore temperature, and the test device and method that wherein sudden change of resistivity method uses are respectively referring to public affairs
The number of opening is the patent content of CN105738404A and CN101625271A.The data of test are shown in Table 3 and table 4:
Table 3: the initial data of closed pore temperature is tested
Table 4: using different test methods to the test result of diaphragm sample
As can be seen from Table 4, smaller using the panel data difference data of test method of the invention, repeatability is more preferable,
And it is simple and convenient in test process, it does not need using electrolyte and resistance meter, and available during the test
The porosity and pore-size distribution of diaphragm sample.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (10)
1. a kind of test method of lithium ion battery separator closed pore temperature, which comprises the following steps:
(1) the diaphragm sample of default size is cut out；
(2) preheating temperature is heated to diaphragm sample；
(3) diaphragm sample is placed in pressure water instrument and is loaded in the sample cell of water, test temperature, interval record sample is gradually increased
It is anti-to illustrate that diaphragm has begun generation closed pore when obvious contractile response occurs for diaphragm sample for the porosity of diaphragm in product pond
It answers, when the porosity of diaphragm sample is 0, corresponding test temperature is diaphragm closed pore temperature.
2. test method according to claim 1, it is characterised in that: step described in repetitive operation (1)-(3) at least 3 times,
And the closed pore temperature according to the average value of the closed pore temperature obtained every time as diaphragm sample.
3. test method according to claim 1, it is characterised in that: preheating temperature in the step (2) is 120 DEG C-
200℃。
4. test method according to claim 3, it is characterised in that: using baking oven to diaphragm sample in the step (2)
Heating.
5. test method according to claim 4, it is characterised in that: baking oven 10min heating and continuous to diaphragm sample.
6. test method according to claim 1, it is characterised in that: pass through diaphragm sample in pressure water instrument in the step (3)
The air pressure of the gas of product gradually increases within the scope of 0-1500psi.
7. test method according to claim 1, it is characterised in that: the interval time recorded in the step (3) is every
It is spaced 15s.
8. test method according to claim 1, it is characterised in that: in the step (3), if any 2 repetitions are grasped
When the difference of the closed pore temperature of diaphragm measured by making is more than 3 DEG C, then this 2 times operations are accordingly to be regarded as unqualified test and need again
Test.
9. test method according to claim 1, it is characterised in that: the size range of the diaphragm sample is length: 40cm-
60cm, width: 30cm-50cm.
10. pressing application of the water instrument in measurement lithium ion battery separator closed pore temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910507345.9A CN110286075A (en) | 2019-06-12 | 2019-06-12 | A kind of test method of lithium ion battery separator closed pore temperature |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910507345.9A CN110286075A (en) | 2019-06-12 | 2019-06-12 | A kind of test method of lithium ion battery separator closed pore temperature |
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| CN110286075A true CN110286075A (en) | 2019-09-27 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111766283A (en) * | 2020-06-23 | 2020-10-13 | 合肥国轩高科动力能源有限公司 | Diaphragm closed pore temperature testing method |
| CN113295297A (en) * | 2021-04-30 | 2021-08-24 | 中材锂膜有限公司 | Method for testing closed pore temperature of lithium battery diaphragm |
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| CN108242523A (en) * | 2016-12-27 | 2018-07-03 | 上海恩捷新材料科技股份有限公司 | A kind of battery isolating film |
| CN109326760A (en) * | 2018-08-10 | 2019-02-12 | 泰州衡川新能源材料科技有限公司 | It is a kind of for manufacturing the manufacturing method of lithium battery diaphragm |
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2019
- 2019-06-12 CN CN201910507345.9A patent/CN110286075A/en active Pending
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| CN102522528A (en) * | 2011-12-31 | 2012-06-27 | 宁波长阳科技有限公司 | Battery diaphragm and preparation method thereof |
| WO2014123973A1 (en) * | 2013-02-08 | 2014-08-14 | Schlumberger Canada Limited | Apparatus and methodology for measuring properties of microporous material at multiple scales |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111766283A (en) * | 2020-06-23 | 2020-10-13 | 合肥国轩高科动力能源有限公司 | Diaphragm closed pore temperature testing method |
| CN113295297A (en) * | 2021-04-30 | 2021-08-24 | 中材锂膜有限公司 | Method for testing closed pore temperature of lithium battery diaphragm |
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