CN113945502A - Porosity testing tool and testing method thereof - Google Patents
Porosity testing tool and testing method thereof Download PDFInfo
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- CN113945502A CN113945502A CN202111234932.9A CN202111234932A CN113945502A CN 113945502 A CN113945502 A CN 113945502A CN 202111234932 A CN202111234932 A CN 202111234932A CN 113945502 A CN113945502 A CN 113945502A
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- 238000003825 pressing Methods 0.000 claims abstract description 59
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical group [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 16
- 229910052753 mercury Inorganic materials 0.000 claims description 16
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- 238000004140 cleaning Methods 0.000 claims description 6
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
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- 239000013543 active substance Substances 0.000 description 6
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
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- 229910052744 lithium Inorganic materials 0.000 description 1
- BDKWOJYFHXPPPT-UHFFFAOYSA-N lithium dioxido(dioxo)manganese nickel(2+) Chemical compound [Mn](=O)(=O)([O-])[O-].[Ni+2].[Li+] BDKWOJYFHXPPPT-UHFFFAOYSA-N 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
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- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- AWRQDLAZGAQUNZ-UHFFFAOYSA-K sodium;iron(2+);phosphate Chemical compound [Na+].[Fe+2].[O-]P([O-])([O-])=O AWRQDLAZGAQUNZ-UHFFFAOYSA-K 0.000 description 1
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Images
Classifications
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- 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
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a porosity testing tool and a porosity testing method. The porosity testing tool comprises: liquid nitrogen quenching part, pressurizing part and porosity testing part. The liquid nitrogen quenching component is internally provided with a chamber for storing liquid nitrogen and placing a sample to be detected, wherein the sample to be detected comprises an electrode plate and/or a battery diaphragm; the pressurizing component is used for applying pressure to the sample to be tested; and the porosity testing part is used for testing the pores in the sample to be tested after liquid nitrogen quenching. The sample to be measured (electrode plate and/or battery diaphragm) is subjected to cold quenching treatment, so that the sample to be measured can be prevented from being decompressed and rebounded after being pressurized. On the one hand, the real state of the sample to be detected can be maintained, and the morphological change of the sample to be detected in the pressure state can be reflected really; on the other hand, the adverse effect of the rebound of the to-be-tested sample after pressure relief on the porosity test result can be inhibited, the error of the porosity test result can be reduced, and the porosity test accuracy is improved.
Description
Technical Field
The invention relates to the technical field of porosity testing, in particular to a porosity testing tool and a porosity testing method.
Background
In the development process of secondary batteries such as lithium ion power batteries and the like, the selection of a battery diaphragm plays a significant role in the design of a battery core, and the porosity is a key parameter in the selection of the battery diaphragm. Based on the level of a single battery cell, the selection of a battery diaphragm directly influences the infiltration of electrolyte on a pole piece, influences the interface of the pole piece and further influences the cycle capacity and the service life of the battery cell; in addition, the porosity of the pole piece directly affects the design of the compacted density of the pole piece and the liquid injection coefficient of the battery cell, and further affects the cycle performance of the battery cell. Based on the module level, the electric core in the circulation process is influenced by initial pretightening force and the expansion of the electric core, and the porosity of the pole piece and the battery diaphragm can be changed, so that the distribution of electrolyte is influenced, and then the conditions of lithium precipitation, black spots, purple spots and the like under different conditions appear in the circulation process. Therefore, it is necessary to clearly study the porosity change of the pole piece and the battery diaphragm under the pressure state, so as to provide reference for the pretightening force and the module design and optimize the design scheme.
The methods commonly used at present for testing the porosity include mercury intrusion method, gas adsorption method (BET method), weighing method, theoretical calculation method and the like. The principle of the mercury intrusion method is that mercury is pressed into pores of a porous body by using the characteristic that mercury does not infiltrate the surface of a solid body at a certain pressure so as to overcome the resistance of a capillary tube, the smaller the pore diameter, the larger the pressure is, and the corresponding pore size can be obtained according to the pressure. The quantity of mercury in the inlet hole under different external pressures is measured, namely the corresponding pore volume, so that a curve of pore volume change along with the size of the pore diameter, and the pore size distribution and the porosity of the porous material can be calculated.
The mercury pressing method or the BET method needs to apply pressure to the pole piece or the diaphragm to compress the pole piece or the diaphragm, and then the porosity test is carried out through a mercury pressing instrument or a nitrogen adsorption desorption instrument, the pressure relief operation in the method can cause the rebound of the pole piece or the diaphragm, the porosity obtained by the test deviates from the value under the actual pressure state, and the rebound of the pole piece or the diaphragm made of different materials has difference, so that a larger error can be caused even if the comparison of the relative porosity is carried out, and the evaluation of the design scheme has deviation, thereby causing misjudgment or miskilling.
The prior document (publication number CN106684330A) provides a measurement and calculation method for porosity of a pole piece, which includes the following steps: firstly, selecting raw materials to prepare slurry; measuring the density and solid content of the slurry; calculating the comprehensive true density according to the density of the slurry, the solid content of the slurry and the density of the selected solvent; coating the slurry on the surface of the pole piece according to the required compaction density of the pole piece, and compacting the surface of the pole piece; and calculating the porosity of the pole piece according to the compacted density and the comprehensive true density. The method is only suitable for porosity test of the bare electrode slice which is not originally assembled into the battery cell, cannot be used for characterization under a certain pressure state, and cannot be used for characterization of the diaphragm.
However, at present, no effective evaluation means is available for testing the porosity under the pressure state, and the porosity is tested after pressure compression and pressure relief mostly by adopting theoretical calculation or qualitative method, so that large errors exist, particularly rebound (rebound) of a pole piece and a battery diaphragm after pressure relief, and the actual porosity of the porosity obtained by testing under the non-pressure state exists.
On the basis, a porosity testing device for secondary batteries such as lithium ion batteries or sodium ion batteries is researched and developed, and meanwhile, a porosity testing method and a porosity testing system capable of effectively improving the porosity testing accuracy and reducing the measurement error are researched and developed, so that the method and the system have important significance for providing effective data and theoretical support for battery development, module design and battery simulation.
Disclosure of Invention
The invention mainly aims to provide a porosity testing tool and a porosity testing method, and aims to solve the problem that the electrode plate or a diaphragm is rebounded due to pressure relief after pressure is applied to the electrode plate or the diaphragm in the existing mercury intrusion porosimeter method testing and gas adsorption (BET) testing processes, so that the porosity testing accuracy is poor.
In order to achieve the above object, one aspect of the present invention provides a porosity testing tool, including: liquid nitrogen quenching part, pressurizing part and porosity testing part. The liquid nitrogen quenching component is internally provided with a chamber for storing liquid nitrogen and placing a sample to be detected, wherein the sample to be detected comprises an electrode plate and/or a battery diaphragm; the pressurizing component is used for applying pressure to the sample to be tested; and the porosity testing part is used for testing the pores in the sample to be tested after liquid nitrogen quenching.
Further, the pressing member includes: the device comprises a first tool fixing plate, a second tool fixing plate, a mechanical sensor fixing pressing plate, a movable pressing plate, a mechanical sensor, a torque wrench and at least two guide posts. The first tool fixing plate is provided with at least two first positioning holes and a first middle positioning hole; the second fixture fixing plate is provided with at least two second positioning holes and a second middle positioning hole; the mechanical sensor fixing pressure plate is provided with at least two third positioning holes; the movable pressing plate is provided with at least two fourth positioning holes, and the first fixture fixing plate, the second fixture fixing plate, the mechanical sensor fixing pressing plate and the movable pressing plate are arranged in parallel; the mechanical sensor is arranged between the fixed pressing plate and the movable pressing plate of the mechanical sensor; the torque wrench comprises a lead screw and a wrench which are vertically arranged, and the lead screw acts on the mechanical sensor through a first middle positioning hole and a second middle positioning hole; the first fixture fixing plate is fixedly arranged with the guide post through the first positioning hole, the second fixture fixing plate is fixedly arranged with the guide post through the second positioning hole and the mechanical sensor fixing pressing plate is fixedly arranged with the guide post through the third positioning hole, the guide post is inserted into the fourth positioning hole, and the movable pressing plate can move up and down along the guide post so as to apply pressure to a sample to be tested.
Further, the chamber is formed by a bottom surface and a side wall arranged around the bottom surface, a liquid nitrogen inlet and a liquid nitrogen outlet are arranged on the side wall, and the height of the liquid nitrogen inlet is lower than that of the liquid nitrogen outlet.
Furthermore, the movable pressing plate comprises a bearing part and a pressing part, the bearing part is provided with a fourth positioning hole, and the pressing part can extend into the cavity and be in contact with a sample to be tested.
Further, the porosity testing tool also comprises a crushing device, wherein the crushing device is used for crushing the sample to be tested subjected to liquid nitrogen cold quenching; preferably, the porosity testing component is a mercury intrusion gauge.
In order to achieve the above object, another aspect of the present invention further provides a porosity testing method, where the porosity testing tool provided in the present application is adopted, and the porosity testing method includes: placing a sample to be detected in a cavity of a liquid nitrogen cold quenching component, and applying pressure to the surface of the sample to be detected by adopting a pressurizing component, wherein the sample to be detected comprises an electrode plate and/or a battery diaphragm; introducing liquid nitrogen into the chamber, and performing cold quenching treatment on the sample to be detected to obtain a cold quenched sample; and (3) carrying out porosity test on the cold quenching sample by adopting a porosity test part, and obtaining porosity data of the sample to be tested.
Further, the temperature of the liquid nitrogen is-194 ℃ to-198 ℃, and the time of cold quenching treatment is 3-5 min.
Further, the porosity testing method further comprises the following steps: and applying pressure to the surface of the sample to be detected by adopting a torque wrench, wherein the applied pressure is 1000-20000N, and the pressure application time is 5-15 min.
Further, the porosity testing method further comprises the following steps: and (3) monitoring the pressure applying step in real time by adopting a mechanical sensor, and performing cold quenching treatment when the change of the applied pressure is less than or equal to 5N.
Further, the porosity testing method further comprises the following steps: before a sample to be detected is placed in a cavity of a liquid nitrogen cold quenching component, soaking and/or cleaning the sample to be detected by adopting a solvent; preferably, the soaking time is 10-30 min; preferably, the solvent is selected from one or more of the group consisting of dimethyl carbonate, ethyl methyl carbonate, dimethyl ether, propylene carbonate and ethanol.
By applying the technical scheme of the invention, the cavity is arranged in the liquid nitrogen quenching component, so that the liquid nitrogen quenching component can store liquid nitrogen and provide a proper space for liquid nitrogen quenching treatment; meanwhile, a sample to be detected is placed in the chamber and is subjected to cold quenching by liquid nitrogen. And then, applying pressure to the sample to be measured after cold quenching by adopting a pressurizing component so as to compress the sample to be measured. And then, a porosity testing part is used for testing the pores in the sample to be tested which is subjected to liquid nitrogen quenching, so that a porosity testing result can be obtained.
The sample to be detected (the electrode plate and/or the battery diaphragm) is subjected to cold quenching treatment, so that the sample to be detected can be restrained from rebounding after being subjected to pressure application and pressure relief, and the shape and the gap distribution of the sample to be detected in a pressure state can be maintained. On the one hand, the real state of the sample to be detected can be maintained, and the morphological change of the sample to be detected in the pressure state can be reflected really; on the other hand, the adverse effect of the rebound of the to-be-tested sample after pressure relief on the porosity test result can be inhibited, the error of the porosity test result can be reduced, and the porosity test accuracy is improved. In addition, effective data support is provided for selection of electrode plates and/or battery separators, cell design, module design and cell simulation.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a schematic structural diagram of a porosity testing tool according to embodiment 1 of the present invention;
fig. 2 shows SEM images of samples to be measured before and after the cold quenching treatment in example 1 of the present invention, in which fig. 2a) is an SEM image of a battery separator under no pressure, and fig. 2b) is an SEM image of a battery separator after being frozen by liquid nitrogen under a pressure of 3000N.
Wherein the figures include the following reference numerals:
100. a liquid nitrogen cold quenching component; 110. a chamber; 111. a liquid nitrogen inlet; 112. a liquid nitrogen outlet;
200. a pressing member; 210. a first fixture fixing plate; 220. a second fixture fixing plate; 230. the mechanical sensor fixes the pressing plate; 240. a movable pressing plate; 250. a mechanical sensor; 260. a torque wrench; 261. a lead screw; 262. a wrench; 270. and a guide post.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background art, the existing mercury porosimeter method test and gas adsorption method (BET) test have a problem that pressure relief after applying pressure to an electrode sheet or a diaphragm causes the electrode sheet or the diaphragm to rebound, resulting in poor accuracy of porosity test. In order to solve the technical problem, the application provides a porosity test fixture, and the porosity test fixture comprises: liquid nitrogen quenching part 100, pressurizing part 200 and porosity testing part. A chamber 110 is arranged in the liquid nitrogen quenching component 100 and is used for storing liquid nitrogen and placing a sample to be detected, wherein the sample to be detected comprises an electrode plate and/or a battery diaphragm; the pressurizing member 200 is used for applying pressure to a sample to be measured; and the porosity testing part is used for testing the pores in the sample to be tested after liquid nitrogen quenching.
A chamber 110 is arranged in the liquid nitrogen quenching component 100, so that the liquid nitrogen quenching component can store liquid nitrogen and provide a proper space for liquid nitrogen quenching treatment; meanwhile, a sample to be measured is placed in the chamber 110 and is subjected to cold quenching using liquid nitrogen. And then, applying pressure to the sample to be measured after the cold quenching by using a pressure component 200 to compress the sample to be measured. And then, a porosity testing part is used for testing the pores in the sample to be tested which is subjected to liquid nitrogen quenching, so that a porosity testing result can be obtained.
The sample to be detected (the electrode plate and/or the battery diaphragm) is subjected to cold quenching treatment, so that the sample to be detected can be restrained from rebounding after being subjected to pressure application and pressure relief, and the shape and the gap distribution of the sample to be detected in a pressure state can be maintained. On the one hand, the real state of the sample to be detected can be maintained, and the morphological change of the sample to be detected in the pressure state can be reflected really; on the other hand, the adverse effect of the rebound of the to-be-tested sample after pressure relief on the porosity test result can be inhibited, the error of the porosity test result can be reduced, and the porosity test accuracy is improved. In addition, effective data support is provided for selection of electrode plates and/or battery separators, cell design, module design and cell simulation.
The pressing member 200 may be of any type commonly used in the art as long as it can perform the above-described function, and the specific structure is not particularly limited. In a preferred embodiment, the pressing member 200 includes: the tool comprises a first tool fixing plate 210, a second tool fixing plate 220, a mechanical sensor fixing pressing plate 230, a movable pressing plate 240, a mechanical sensor 250, a torque wrench 260 and at least two guide posts 270. The first tool fixing plate 210 is provided with at least two first positioning holes and a first middle positioning hole; the second fixture fixing plate 220 is provided with at least two positioning holes and a second middle positioning hole; the mechanical sensor fixing pressure plate 230 is provided with at least two third positioning holes; the movable pressing plate 240 is provided with at least two fourth positioning holes, and the first tool fixing plate 210, the second tool fixing plate 220, the mechanical sensor fixing pressing plate 230 and the movable pressing plate 240 are arranged in parallel; the mechanical sensor 250 is arranged between the mechanical sensor fixed pressing plate 230 and the movable pressing plate 240; the torque wrench 260 comprises a lead screw 261 and a wrench 262 which are vertically arranged, wherein the lead screw 261 acts on the mechanical sensor 250 through a first middle positioning hole and a second middle positioning hole; the first fixture fixing plate 210 passes through the first positioning hole, the second fixture fixing plate 220 passes through the second positioning hole, the mechanical sensor fixing pressing plate 230 passes through the third positioning hole and is fixedly arranged with the guide post 270, the guide post 270 is inserted into the fourth positioning hole, and the movable pressing plate 240 can move up and down along the guide post 270 to apply pressure to a sample to be measured.
By adopting the pressurizing part 200, pressure can be applied to the sample to be measured, so that the sample to be measured is compressed and deformed. Specifically, when an operator twists the wrench 262, the screw 261 vertically disposed with the wrench 262 can convert the rotation force into a force that is applied to the first fixture fixing plate 210, the movable pressing plate 240, and the mechanical sensor 250 vertically in sequence, and is finally applied to the surface of the sample to be measured, so that the sample to be measured is compressed and deformed. In the process of applying the pressure, the mechanical sensor 250 can convert the pressure value applied to the sample to be measured into an electric signal, so that an operator can read the pressure value conveniently.
In the process of applying the pressure, the guide post 270, the first positioning hole, the second positioning hole and the third positioning hole enable the lead screw 261 to pass through the first middle positioning hole to maintain a vertical position relation with the first tool fixing plate 210; at the same time, the movable platen 240 can move up and down along the guide posts 270 to apply pressure to the surface of the sample to be measured.
In a preferred embodiment, the chamber 110 is formed of a bottom surface and a sidewall disposed therearound, a liquid nitrogen inlet 111 and a liquid nitrogen outlet 112 are disposed on the sidewall, and the liquid nitrogen inlet 111 is lower in height than the liquid nitrogen outlet 112. Liquid nitrogen can enter from a liquid nitrogen inlet 111 and exit from a liquid nitrogen outlet 112. Compared with other arrangement modes, the liquid nitrogen inlet 111 is lower than the liquid nitrogen outlet 112, so that liquid nitrogen is sequentially and gradually filled upwards from the bottom of the chamber 110 after entering the chamber 110, and the liquid level of the liquid nitrogen is favorably adjusted to be adaptive to the placement position of a sample to be detected.
The liquid nitrogen quenching component 100, the pressurizing component 200 and the porosity testing component in the porosity testing tool can be three independent components, or the liquid nitrogen quenching component 100 and the pressurizing component 200 are assembled into a whole, and the porosity testing component is an independent component, or the three are connected together to form a whole. When the three parts are connected together to form a whole, optionally, the liquid nitrogen quenching part 100 and the pressurizing part 200 are firstly assembled into a whole, and then the upper end opening of the liquid nitrogen quenching part 100 is communicated with the sample testing area of the porosity testing part through the sample conveying device to be tested.
In a preferred embodiment, the movable platen 240 includes a receiving portion provided with a fourth positioning hole and a pressing portion capable of extending into the chamber 110 and contacting with the sample to be tested. The fourth positioning hole of the bearing part can play a role of fixing the guide post 270, and the movable pressing plate 240 can move up and down along the guide post 270 in the process of applying pressure; meanwhile, the pressure applying part can protrude into the chamber 110 and come into contact with the sample to be measured, thereby applying pressure to the sample to be measured.
In a preferred embodiment, the porosity testing tool further comprises a crushing device, and the crushing device is used for crushing the sample to be tested which is subjected to liquid nitrogen quenching. After the crushing device crushes the sample to be tested which is subjected to liquid nitrogen cold quenching, the subsequent porosity testing component can conveniently test the porosity.
The porosity test member may employ a test apparatus commonly used in the art. In a preferred embodiment, the porosity testing component is a mercury intrusion gauge.
The second aspect of the present application further provides a method for testing porosity, where, by using the porosity testing tool provided by the present application, the method for testing porosity includes: placing a sample to be detected in a cavity 110 of a liquid nitrogen cold quenching component 100, and applying pressure to the surface of the sample to be detected by adopting a pressurizing component 200, wherein the sample to be detected comprises an electrode plate and/or a battery diaphragm; introducing liquid nitrogen into the chamber 110, and performing cold quenching treatment on the sample to be detected to obtain a cold quenched sample; and (3) carrying out porosity test on the cold quenching sample by adopting a porosity test part, and obtaining porosity data of the sample to be tested.
A chamber 110 is arranged in the liquid nitrogen quenching component 100, so that the liquid nitrogen quenching component can store liquid nitrogen and provide a proper space for liquid nitrogen quenching treatment; meanwhile, a sample to be measured is placed in the chamber 110 and is subjected to cold quenching using liquid nitrogen. And then, applying pressure to the sample to be measured after the cold quenching by using a pressure component 200 to compress the sample to be measured. And then, a porosity testing part is used for testing the pores in the sample to be tested which is subjected to liquid nitrogen quenching, so that a porosity testing result can be obtained.
The sample to be detected (the electrode plate and/or the battery diaphragm) is subjected to cold quenching treatment, so that the sample to be detected can be restrained from rebounding after being subjected to pressure application and pressure relief, and the shape and the gap distribution of the sample to be detected in a pressure state can be maintained. On the one hand, the real state of the sample to be detected can be maintained, and the morphological change of the sample to be detected in the pressure state can be reflected really; on the other hand, the adverse effect of the rebound of the to-be-tested sample after pressure relief on the porosity test result can be inhibited, the error of the porosity test result can be reduced, and the porosity test accuracy is improved. The method is particularly suitable for testing the porosity of the electrode plate and the battery diaphragm.
In a preferred embodiment, the temperature of the liquid nitrogen is-194 ℃ to-198 ℃, and the time of the cold quenching treatment is 3-5 min. The temperature of the liquid nitrogen and the time of the cold quenching treatment include but are not limited to the ranges, and the limitation of the temperature and the time to the cold quenching treatment in the ranges is favorable for further inhibiting the adverse effect of the rebound of the pressure-relieved sample to be tested on the porosity test result, so that the porosity test accuracy is improved; meanwhile, the temperature is favorable for avoiding the electrode plate and the diaphragm from being fractured due to embrittlement, and the integrity of a sample to be tested is favorably maintained.
In a preferred embodiment, the method for testing porosity further comprises: the torque wrench 260 is used for applying pressure to the surface of the sample to be tested, the applied pressure is 1000-20000N, and the pressure application time is 5-15 min. The applied pressure and the applied pressure time include, but are not limited to, the above ranges, and the limitation of the applied pressure and the applied pressure time within the above ranges is beneficial to causing the sample to be tested to generate compression deformation, and avoiding the yield limit of the sample to be tested from being exceeded to seriously damage the internal original pore structure, thereby avoiding the inaccurate porosity test data caused by the internal original pore structure.
In a preferred embodiment, the method for testing porosity further comprises: and (3) monitoring the pressure applying step in real time by using a mechanical sensor 250, and performing cold quenching treatment when the pressure change is less than or equal to 5N. By monitoring the pressure application step in real time using the mechanical sensor 250, the operator can observe the pressure value in real time, facilitating the applied pressure. When the pressure changes within the range, the pressure is basically in a stable state, and the cold quenching treatment can be closer to the real state of the sample to be tested, so that the porosity testing accuracy can be further improved.
In a preferred embodiment, the method for testing porosity further comprises: before the sample to be tested is placed in the chamber 110 of the liquid nitrogen quenching component 100, the sample to be tested is subjected to soaking treatment and/or cleaning treatment by using a solvent. The soaking treatment and the cleaning treatment are suitable for electrode plates or battery diaphragms obtained by disassembling lithium ion batteries or sodium ion batteries serving as samples to be detected. The soaking treatment and the cleaning treatment can remove electrolyte and other electrode active substances (namely impurities which interfere the porosity test) adsorbed on the surfaces of the electrode slice and the battery diaphragm obtained by disassembling and in the internal pores of the electrode slice and the battery diaphragm, and reduce the interference of redundant electrolyte and electrode active substances on the porosity test, thereby improving the accuracy of the porosity test. In order to further remove the electrolyte and other electrode active substances adsorbed on the surfaces of the electrode plates and the battery separator and in the internal pores of the electrode plates and the battery separator, the soaking treatment time is preferably 10-30 min.
In order to improve the elution efficiency, a solvent which has high lithium salt solubility and is volatile is selected for elution, so that on one hand, electrolyte and other electrode active substances (namely impurities which interfere the porosity test) are adsorbed on the surfaces of electrode plates and battery separators obtained by cleaning and disassembling and in the internal pores of the electrode plates and the battery separators, and on the other hand, the volatile solvent can reduce the influence of the solvent on the accuracy of the porosity test to the maximum extent; preferably, the solvent includes, but is not limited to, one or more of the group consisting of dimethyl carbonate, ethyl methyl carbonate, dimethyl ether, propylene carbonate and ethanol.
In an alternative embodiment, the electrode sheet includes one or more of the group consisting of, but not limited to, an aluminum foil, a copper foil, an aluminum foil with a surface remaining the positive electrode active material and/or the conductive binder, and a copper foil with a surface remaining the negative electrode active material and/or the conductive binder; the positive active material includes, but is not limited to, one or more of the group consisting of a nickel-cobalt-manganese ternary material, a nickel-lithium manganate cobalt-free material and a lithium iron phosphate material, or one or more of the group consisting of sodium cobaltate, sodium ferrite, sodium manganate, sodium nickelate, vanadium pentoxide, sodium iron phosphate and sodium vanadium phosphate; the negative active material includes, but is not limited to, one or more of the group consisting of graphite, silicon, and silicon monoxide.
In an alternative embodiment, the battery separator includes, but is not limited to, a polyethylene film (PE), a polypropylene film (PP), a Polyethylene (PE)/polyvinylidene fluoride (PVDF) composite film, a polypropylene (PP)/polyvinylidene fluoride (PVDF) composite film, a Polyethylene (PE)/Al composite film2O3Ceramic composite film and polypropylene/Al2O3One or more of the group consisting of ceramic composite membranes.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
A method of testing porosity comprising:
taking a fresh diaphragm (which refers to a diaphragm which is not assembled into a battery and has a thickness of 14 μm, wherein the thickness of the PE base film is 9 μm, and Al2O3The thickness of the ceramic layer is 3 μm, and the thickness of the double-side coated PVDF is 1 μm respectively) is taken as a sample to be measured, and the sample is soaked for 20min, cleaned and dried by adopting dimethyl carbonate (DMC). And folding the fresh diaphragm in half, and ensuring the flatness of the diaphragm.
As shown in the structural schematic diagram of the porosity testing tool shown in fig. 1, a folded sample to be tested is placed in a cavity 110 of a liquid nitrogen quenching component 100, pressure is applied through a torque wrench 260, a pressure value is observed, when the applied pressure reaches 3000N and is kept for 5min, the porosity testing tool displays pressure 2542N, pressurization is continued, the pressure reaches 3050N, pressure is maintained for 15min, a pressure sensor displays pressure 2997N, a pressure change value is less than or equal to 5N, and cold quenching treatment is started.
Introducing liquid nitrogen with the temperature of-196 ℃ into a chamber 110 of the liquid nitrogen cold quenching component 100 through a liquid nitrogen inlet 111, performing cold quenching treatment on a sample to be detected, wherein the time of the cold quenching treatment is 5min, and discharging redundant liquid nitrogen through a liquid nitrogen outlet 112 and recovering the liquid nitrogen. The diaphragm after cold quenching is taken out and crushed by a crushing device through pressure relief of a torque wrench 260, and then is put into a mercury intrusion porosimeter (manufactured by Macmer Raitk (Shanghai) instruments, Inc., model number AutoPore9500) for porosity test. The porosity of the membrane was found to be 37.87% at 3000N pressure. Sampling the diaphragm after the cold quenching treatment, performing SEM characterization, and observing the shape and structure change of the diaphragm under the pressure state, wherein SEM images before and after the cold quenching treatment are respectively shown in figures 2a) and 2 b).
The initial porosity (i.e., porosity without applied pressure) of the fresh diaphragm was measured using the mercury porosimeter (AutoPore9500) as described above, with a test result of 41.35% (manufacturer supplied 41.5% porosity for new shanghai enjie material).
Example 2
The difference from example 1 is that: the applied pressure was 1000N.
Example 3
The difference from example 1 is that: the applied pressure was 5000N.
Example 4
The difference from example 1 is that: the applied pressure was 7000N.
Example 5
The difference from example 1 is that: the applied pressure was 10000N.
Example 6
The difference from example 1 is that: the applied pressure was 15000N.
Example 7
The difference from example 1 is that: the time of cold quenching treatment is 3 min.
Example 8
The difference from example 1 is that: the time of cold quenching treatment is 10 min.
Example 9
The difference from example 1 is that: the pressure application time is 5 min.
Example 10
The difference from example 1 is that: the pressure application time is 1 min.
Example 11
The difference from example 1 is that: the time for soaking the sample to be tested is 10 min.
Comparative example 1
The difference from example 1 is that: and (3) not performing cold quenching treatment on the sample to be tested, and directly placing the sample to be tested into a mercury intrusion instrument for porosity test after applying pressure.
The porosity test data of the separator measured in all examples and comparative examples of the present application are shown in table 1.
TABLE 1
| Porosity test data (%) | |
| Example 1 | 37.87 |
| Example 2 | 39.20 |
| Example 3 | 36.88 |
| Example 4 | 36.32 |
| Example 5 | 35.89 |
| Example 6 | 35.43 |
| Example 7 | 37.86 |
| Example 8 | 36.55 |
| Example 9 | 38.30 |
| Example 10 | 39.21 |
| Example 11 | 37.88 |
| Comparative example 1 | 39.94 |
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
comparing example 1 with comparative example 1, it can be seen that the porosity measured in example 1 is 37.87%, while the sample to be tested in comparative example 1 is not cold quenched, and the sample is directly put into a mercury porosimeter after pressure is applied for porosity measurement, and the porosity is 39.94%, the data measured in comparative example 1 is significantly larger, and the error is 5.47%.
As can be seen from comparison of examples 1 to 6, the pressure applied to the sample to be tested in example 1 was 3000N, example 2 was 1000N, example 3 was 5000N, and the pressures applied to the sample to be tested in examples 4 to 6 were 7000N, 10000N, and 15000N, respectively, in this order. As can be seen from the test results in table 1, the test results of the porosity of the sample to be tested show a gradually decreasing trend with increasing applied pressure. This indicates that, as the applied pressure increases, the compression set of the sample to be tested is large, and the hole portion in the sample to be tested is compressed, so that the test result shows a tendency to gradually decrease.
The porosity can be increased due to the rebound, and as can be seen from the comparison of the example 1 and the comparative example 1, the rebound of the battery diaphragm can be well inhibited by performing liquid nitrogen quenching treatment on the sample to be tested, so that the test process is closer to the real state of the sample to be tested, and the porosity test accuracy is improved.
Comparing examples 1, 7 and 8, it can be seen that the time of the cold quenching process includes, but is not limited to, the preferred range of the present application, and that limiting the time to the preferred range of the present application is advantageous to further suppress the rebound of the sample to be tested after pressure relief from adversely affecting the porosity test result, thereby further improving the accuracy of the porosity test.
Comparing examples 1, 9 and 10, it can be seen that the pressing time includes, but is not limited to, the preferred range of the present application, and it is limited to the preferred range of the present application, which is favorable for causing the sample to be tested to generate compression deformation, and avoiding exceeding the yield limit of the sample to be tested and seriously damaging the original internal pore structure, thereby avoiding the inaccurate porosity test data caused by the compression deformation.
Comparing examples 1 and 11, it can be seen that the time of the soaking treatment, including but not limited to the preferred range of the present application, is limited to the preferred range of the present application, which is beneficial for further removing the electrolyte and other electrode active substances adsorbed in the surface of the electrode sheet and the battery separator and the internal pores thereof, and reducing the interference of the redundant electrolyte and electrode active substances on the porosity test, thereby improving the accuracy of the porosity test.
It is noted that the terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those described or illustrated herein.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a porosity test fixture, its characterized in that, porosity test fixture includes:
the device comprises a liquid nitrogen cold quenching component (100), wherein a chamber (110) is arranged inside the liquid nitrogen cold quenching component (100) and is used for storing liquid nitrogen and placing a sample to be detected, and the sample to be detected comprises an electrode plate and/or a battery diaphragm;
the pressurizing component (200), the said pressurizing component (200) is used for exerting the pressure to the said sample to be measured;
and the porosity testing component is used for testing the pores in the sample to be tested after liquid nitrogen quenching.
2. The porosity test fixture according to claim 1, wherein the pressing member (200) comprises:
the fixture comprises a first fixture fixing plate (210), wherein the first fixture fixing plate (210) is provided with at least two first positioning holes and a first middle positioning hole;
the second fixture fixing plate (220), the second fixture fixing plate (220) is provided with at least two second positioning holes and a second middle positioning hole;
the mechanical sensor fixing pressing plate (230) is provided with at least two third positioning holes;
the movable pressing plate (240) is provided with at least two fourth positioning holes, and the first fixture fixing plate (210), the second fixture fixing plate (220), the mechanical sensor fixing pressing plate (230) and the movable pressing plate (240) are arranged in parallel;
a mechanical sensor (250), the mechanical sensor (250) disposed between the mechanical sensor stationary platen (230) and the movable platen (240);
the torque wrench (260) comprises a lead screw (261) and a wrench (262) which are vertically arranged, and the lead screw (261) acts on the mechanical sensor (250) through the first middle positioning hole and the second middle positioning hole;
the first tool fixing plate (210) passes through the first positioning hole, the second tool fixing plate (220) passes through the second positioning hole, the mechanical sensor fixing pressing plate (230) passes through the third positioning hole and the guide columns (270) are fixedly arranged, the guide columns (270) are inserted into the fourth positioning hole, and the movable pressing plate (240) can move up and down along the guide columns (270) so as to apply pressure to the sample to be tested.
3. The porosity test tool according to claim 2, wherein the chamber (110) is formed by a bottom surface and a side wall arranged around the bottom surface, a liquid nitrogen inlet (111) and a liquid nitrogen outlet (112) are arranged on the side wall, and the liquid nitrogen inlet (111) is lower than the liquid nitrogen outlet (112).
4. The porosity testing tool according to claim 3, wherein the movable pressing plate (240) comprises a receiving portion and a pressing portion, the receiving portion is provided with the fourth positioning hole, and the pressing portion can extend into the chamber (110) and contact with the sample to be tested.
5. The porosity testing tool according to any one of claims 1 to 4, further comprising a crushing device, wherein the crushing device is used for crushing a sample to be tested which is subjected to liquid nitrogen quenching;
preferably, the porosity testing component is a mercury intrusion gauge.
6. A porosity testing method, characterized in that, the porosity testing tool of any claim 1 to 5 is adopted, and the porosity testing method comprises the following steps:
placing a sample to be detected in a chamber (110) of a liquid nitrogen cold quenching component (100), and applying pressure to the surface of the sample to be detected by adopting a pressurizing component (200), wherein the sample to be detected comprises an electrode plate and/or a battery diaphragm;
introducing liquid nitrogen into the chamber (110), and performing cold quenching treatment on the sample to be detected to obtain a cold quenched sample;
and carrying out porosity test on the cold quenching sample by adopting a porosity test part, and obtaining the porosity data of the sample to be tested.
7. The porosity testing method according to claim 6, wherein the temperature of the liquid nitrogen is-194 ℃ to-198 ℃, and the time of the cold quenching treatment is 3-5 min.
8. The method for testing porosity according to claim 6 or 7, further comprising: and applying pressure to the surface of the sample to be detected by adopting a torque wrench (260), wherein the applied pressure is 1000-20000N, and the pressure application time is 5-15 min.
9. The method for testing porosity as claimed in claim 8, further comprising: and (3) monitoring the pressure applying step in real time by adopting a mechanical sensor (250), and performing cold quenching treatment when the change of the applied pressure is less than or equal to 5N.
10. The method for testing porosity according to any one of claims 7 to 9, further comprising: before the sample to be detected is placed in a chamber (110) of the liquid nitrogen quenching component (100), soaking and/or cleaning treatment is carried out on the sample to be detected by adopting a solvent;
preferably, the soaking time is 10-30 min;
preferably, the solvent is selected from one or more of the group consisting of dimethyl carbonate, ethyl methyl carbonate, dimethyl ether, propylene carbonate and ethanol.
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