CN110690393A - Preparation method of para-aramid nanofiber/PP non-woven fabric diaphragm - Google Patents
Preparation method of para-aramid nanofiber/PP non-woven fabric diaphragm Download PDFInfo
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- CN110690393A CN110690393A CN201910988637.9A CN201910988637A CN110690393A CN 110690393 A CN110690393 A CN 110690393A CN 201910988637 A CN201910988637 A CN 201910988637A CN 110690393 A CN110690393 A CN 110690393A
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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
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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
- H01M50/44—Fibrous material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a preparation method of a para-aramid nano-fiber/PP non-woven fabric diaphragm, and relates to the technical field of para-aramid nano-fiber/PP non-woven fabric diaphragms. According to the invention, a PP non-woven fabric is selected as a base material, para-aramid resin is used for preparing para-aramid slurry, the PP non-woven fabric is reinforced in a mode of coating the para-aramid slurry on the PP non-woven fabric to form a film, the bonding effect between the para-aramid slurry and the PP non-woven fabric is strong, and an integrated diaphragm can be formed; dissolving para-aramid resin in concentrated sulfuric acid, adding N-methyl pyrrolidone, and stirring at high speed to prepare para-aramid nanofiber slurry, wherein polymerization reaction is not involved, and the process is simple; the space is occupied by the pore-forming agent, the PP non-woven fabric pore caused by coating the para-aramid slurry is prevented from being blocked, and the porosity of the para-aramid nanofiber/PP non-woven fabric diaphragm is effectively improved.
Description
Technical Field
The invention relates to the technical field of a para-aramid nano-fiber/PP non-woven fabric diaphragm, in particular to a preparation method of the para-aramid nano-fiber/PP non-woven fabric diaphragm.
Background
In mobile phones, computers and electric vehicles, batteries that can be charged and discharged many times are mainly lithium ion batteries. The key of the charge and discharge of the lithium ion battery is the regular movement of lithium ions between the anode and the cathode; specifically, during charging, lithium ions are extracted from the positive electrode and inserted into the negative electrode through the electrolyte, and the negative electrode is in a lithium-rich state; the opposite is true during discharge. The lithium ion battery has the advantages that the lithium ion battery is provided with a diaphragm inside besides the anode, the cathode and the electrolyte, and the diaphragm has the functions of separating the anode and the cathode of the battery and preventing the two electrodes from contacting and short-circuiting, so that the diaphragm needs to have a certain thickness; and the diaphragm is provided with holes for providing a passage for lithium ions to move between the anode and the cathode.
The diaphragm is an important component of the lithium ion battery, the performance of the diaphragm determines the interface structure, internal resistance and the like of the battery, the characteristics of the lithium ion battery such as capacity, cycle and safety performance are directly influenced, and the diaphragm with excellent performance plays an important role in improving the comprehensive performance of the lithium ion battery.
At present, the diaphragm in the lithium ion battery is mainly a polyethylene film and a polypropylene film, the materials are easy to obtain, but the performance is slightly poor; the para-aramid fiber has the advantages of high strength, high modulus, high temperature resistance and the like, and can be used for reinforcing a composite film.
Disclosure of Invention
The invention provides a preparation method of a para-aramid nano-fiber/PP non-woven fabric diaphragm, which is used for reinforcing a para-aramid nano-fiber film compounded on a PP non-woven fabric.
The technical scheme adopted by the invention is a preparation method of a para-aramid nano-fiber/PP non-woven fabric diaphragm, which comprises the following steps:
s1, selecting PP non-woven fabric as a substrate material;
s2, preparing a pore-forming agent solution, dissolving benzoic acid in N-methyl pyrrolidone, wherein the concentration is 4-6mol/L, and the temperature of the N-methyl pyrrolidone is 60-80 ℃;
s3, immersing the PP non-woven fabric in the S1 into the pore-forming agent solution prepared in the S2, taking out the PP non-woven fabric after 4-8min, reducing the temperature of the PP non-woven fabric to be below 30 ℃, and cleaning the surface of the PP non-woven fabric to be flat and free of impurities;
s4, preparing para-aramid slurry, namely adding para-aramid resin with the viscosity of 5-8dL/g into concentrated sulfuric acid with the concentration of more than 98% for dissolving, adding N-methyl pyrrolidone, and stirring until a uniform solution is formed, wherein the stirring speed is 4000-;
s5, spraying atomized N-methyl pyrrolidone on the surface of the PP non-woven fabric cleaned in the S3, and then uniformly coating the para-aramid slurry prepared in the S4 on the surface of the PP non-woven fabric to obtain a prefabricated composite diaphragm, wherein the thickness of the slurry is 60-200 mu m;
s6, curing, namely putting the prefabricated composite diaphragm in the S5 into a coagulating bath consisting of N-methyl pyrrolidone and water for curing, wherein the volume ratio of the N-methyl pyrrolidone to the water in the coagulating bath is (8-10) to 1, and the coagulation time is 1-6 min;
s7, cleaning, namely washing the cured prefabricated composite diaphragm in the S6 by deionized water;
s8, pore-forming and hot-pressing, namely heating the cleaned prefabricated composite diaphragm in the S7 at the temperature of 100 ℃ and 125 ℃ for 5-10min, sublimating benzoic acid of the PP non-woven fabric layer, and leaving pores on the PP non-woven fabric layer; and carrying out hot-pressing shaping at the temperature of 100-.
In a certain embodiment, in S2, benzoic acid is dissolved in N-methylpyrrolidone at a temperature of 70 ℃ at a concentration of 5 mol/L; in S3, immersing PP non-woven fabric for 6min, taking out and reducing the temperature to 20 ℃; in S4, the volume ratio of concentrated sulfuric acid to N-methyl pyrrolidone is 1: (2-10); in S5, the thickness of the para-aramid pulp on the PP non-woven fabric is 100 mu m; in S6, the volume ratio of N-methyl pyrrolidone to water in the coagulation bath is 9:1, and the coagulation time is 4 min; heating at 120 deg.C for 8min in S8 to sublimate benzoic acid; pressing with hot pressing roller at 120 deg.C for 3 min; and the thickness of the para-aramid fiber layer in the finally prepared para-aramid nanofiber/PP non-woven fabric diaphragm is 10 mu m.
In the lithium ion battery diaphragm, the heat resistance of PP is better than that of PE, so that the diaphragm is widely applied, and the PP non-woven fabric with simple forming and excellent air permeability is used as a substrate material. And dissolving the para-aramid resin in concentrated sulfuric acid, dispersing in N-methyl pyrrolidone solvent, stirring at high speed to form uniform solution, dispersing the para-aramid nanofiber therein, and coating the prepared para-aramid slurry on a PP non-woven fabric for curing to form a film. When coating, the para-aramid slurry can permeate into the pores on the PP non-woven fabric, so that the bonding force between the para-aramid layer and the PP non-woven fabric layer can be enhanced, but the pores on a large number of PP non-woven fabric layers can be blocked, and finally the porosity of the membrane is reduced. In the invention, a pore-forming agent is used, and the pore-forming agent is firstly infiltrated into the PP non-woven fabric in a liquid state, and then is cooled and recrystallized to firstly occupy the pores on the PP non-woven fabric; after the para-aramid layer is compositely cured, the temperature is raised to recover the original pores on the PP non-woven fabric through sublimation of the pore-forming agent. Under the condition that the space occupied by the pore-forming agent is occupied, partial para-aramid slurry still enters the pores of the PP non-woven fabric layer, and once the para-aramid slurry enters the pores, the para-aramid slurry extends in filaments along the pores due to the spinnability of the para-aramid slurry, so that the para-aramid layer and the PP non-woven fabric layer are firmly compounded together. The para-aramid slurry contains N-methyl pyrrolidone, the coagulating bath also contains N-methyl pyrrolidone, atomized N-methyl pyrrolidone is sprayed on the surface of the PP non-woven fabric before the para-aramid slurry is coated, solutions with similar components are easily dissolved together when the solutions are contacted, and a gap is not generated between the para-aramid layer and the PP non-woven fabric layer. The para-aramid slurry is acidic, so that the dissolution of a pore-forming agent benzoic acid can be reduced, the occupation effect of the para-aramid slurry is kept, and the damage to the pore structure of the PP non-woven fabric layer and the reduction of the strength of the diaphragm caused by the damage to the pore structure before the para-aramid slurry is cured are avoided. In addition, the soaking time of the pore-forming agent solution is related to the thickness of the PP non-woven fabric, generally, the thickness is large, and the needed soaking time is long; experiments show that after the pore-forming agent solution is soaked for 4-8min, the pore-forming agent molecules uniformly and fully permeate into pores of the PP non-woven fabric and are in a dynamic balance process.
Compared with the prior art, the invention has the advantages that:
1) the PP non-woven fabric is reinforced in a mode that the para-aramid pulp is coated on the PP non-woven fabric to form a film, the bonding effect between the PP non-woven fabric and the PP non-woven fabric is strong, and an integrated diaphragm can be formed;
2) dissolving para-aramid resin in concentrated sulfuric acid, adding N-methyl pyrrolidone, and stirring at high speed to prepare para-aramid nanofiber slurry, wherein polymerization reaction is not involved, and the process is simple;
3) the space is occupied by the pore-forming agent, the PP non-woven fabric pore caused by coating the para-aramid slurry is prevented from being blocked, and the porosity of the para-aramid nanofiber/PP non-woven fabric diaphragm is effectively improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments.
A preparation method of a para-aramid nanofiber/PP non-woven fabric diaphragm comprises the following steps:
s1, selecting PP non-woven fabric as a substrate material;
s2, preparing a pore-forming agent solution, dissolving benzoic acid in N-methyl pyrrolidone, wherein the concentration is 4-6mol/L, and the temperature of the N-methyl pyrrolidone is 60-80 ℃;
s3, immersing the PP non-woven fabric in the S1 into the pore-forming agent solution prepared in the S2, taking out the PP non-woven fabric after 4-8min, reducing the temperature of the PP non-woven fabric to be below 30 ℃, and cleaning the surface of the PP non-woven fabric to be flat and free of impurities;
s4, preparing para-aramid slurry, namely adding para-aramid resin with the viscosity of 5-8dL/g into concentrated sulfuric acid with the concentration of more than 98% for dissolving, adding N-methyl pyrrolidone, and stirring until a uniform solution is formed, wherein the stirring speed is 4000-;
s5, spraying atomized N-methyl pyrrolidone on the surface of the PP non-woven fabric cleaned in the S3, and then uniformly coating the para-aramid slurry prepared in the S4 on the surface of the PP non-woven fabric to obtain a prefabricated composite diaphragm, wherein the thickness of the slurry is 60-200 mu m;
s6, curing, namely putting the prefabricated composite diaphragm in the S5 into a coagulating bath consisting of N-methyl pyrrolidone and water for curing, wherein the volume ratio of the N-methyl pyrrolidone to the water in the coagulating bath is (8-10) to 1, and the coagulation time is 1-6 min;
s7, cleaning, namely washing the cured prefabricated composite diaphragm in the S6 by deionized water;
s8, pore-forming and hot-pressing, namely heating the cleaned prefabricated composite diaphragm in the S7 at the temperature of 100 ℃ and 125 ℃ for 5-10min, sublimating benzoic acid of the PP non-woven fabric layer, and leaving pores on the PP non-woven fabric layer; and carrying out hot-pressing shaping at the temperature of 100-.
Example 1:
in S2, the benzoic acid is dissolved in N-methyl pyrrolidone with the temperature of 60 ℃ and the concentration of 4 mol/L; in S3, soaking PP non-woven fabric for 8min, taking out and reducing the temperature to 20 ℃; in S4, the viscosity of the para-aramid resin is 5dL/g, the concentration of concentrated sulfuric acid is 98%, and the volume ratio of the concentrated sulfuric acid to the N-methylpyrrolidone is 1: 4, the stirring speed is 4000 r/min; in S5, the thickness of the para-aramid pulp on the PP non-woven fabric is 60 mu m; in S6, the volume ratio of N-methyl pyrrolidone to water in the coagulation bath is 8:1, and the coagulation time is 1 min; heating at 125 deg.C for 8min in S8 to sublimate benzoic acid; pressing with hot pressing roller at 125 deg.C for 10 min; and the thickness of the para-aramid fiber layer in the finally prepared para-aramid nanofiber/PP non-woven fabric diaphragm is 10 mu m.
Example 2:
in S2, the benzoic acid is dissolved in N-methyl pyrrolidone with the temperature of 65 ℃ and the concentration is 5 mol/L; in S3, soaking PP non-woven fabric for 7min, taking out and reducing the temperature to 20 ℃; in S4, the viscosity of the para-aramid resin is 8dL/g, the concentration of concentrated sulfuric acid is 98%, and the volume ratio of the concentrated sulfuric acid to the N-methylpyrrolidone is 1: 6, the stirring speed is 4500 r/min; in S5, the thickness of the para-aramid pulp on the PP non-woven fabric is 140 mu m; in S6, the volume ratio of N-methyl pyrrolidone to water in the coagulation bath is 8:1, and the coagulation time is 4 min; heating at 120 deg.C for 5min in S8 to sublimate benzoic acid; pressing with hot-pressing roller at 120 deg.C for 15 min; and the thickness of the para-aramid fiber layer in the finally prepared para-aramid nanofiber/PP non-woven fabric diaphragm is 10 mu m.
Example 3:
in S2, the benzoic acid is dissolved in N-methyl pyrrolidone with the temperature of 70 ℃ and the concentration is 5 mol/L; in S3, immersing PP non-woven fabric for 6min, taking out and reducing the temperature to 20 ℃; in S4, the viscosity of the para-aramid resin is 5dL/g, the concentration of concentrated sulfuric acid is 98%, and the volume ratio of the concentrated sulfuric acid to the N-methylpyrrolidone is 1: 8, stirring at 4000 r/min; in S5, the thickness of the para-aramid pulp on the PP non-woven fabric is 100 mu m; in S6, the volume ratio of N-methyl pyrrolidone to water in the coagulation bath is 9:1, and the coagulation time is 4 min; heating at 120 deg.C for 8min in S8 to sublimate benzoic acid; pressing with hot pressing roller at 120 deg.C for 3 min; and the thickness of the para-aramid fiber layer in the finally prepared para-aramid nanofiber/PP non-woven fabric diaphragm is 10 mu m.
Example 4:
in S2, the benzoic acid is dissolved in N-methyl pyrrolidone with the temperature of 75 ℃ and the concentration of 5 mol/L; in S3, soaking PP non-woven fabric for 5min, taking out and reducing the temperature to 30 ℃; in S4, the viscosity of the para-aramid resin is 6dL/g, the concentration of concentrated sulfuric acid is 98%, and the volume ratio of the concentrated sulfuric acid to the N-methylpyrrolidone is 1: 4, the stirring speed is 4000 r/min; in S5, the thickness of the para-aramid pulp on the PP non-woven fabric is 180 mu m; in S6, the volume ratio of N-methyl pyrrolidone to water in the coagulation bath is 10:1, and the coagulation time is 4 min; heating at 110 deg.C for 10min in S8 to sublimate benzoic acid; pressing with hot-pressing roller at 110 deg.C for 20 min; and the thickness of the para-aramid fiber layer in the finally prepared para-aramid nanofiber/PP non-woven fabric diaphragm is 10 mu m.
Example 5:
in S2, the benzoic acid is dissolved in N-methyl pyrrolidone with the temperature of 80 ℃ and the concentration of 6 mol/L; in S3, soaking PP non-woven fabric for 4min, taking out and reducing the temperature to 30 ℃; in S4, the viscosity of the para-aramid resin is 7dL/g, the concentration of concentrated sulfuric acid is 98%, and the volume ratio of the concentrated sulfuric acid to the N-methylpyrrolidone is 1: 4, the stirring speed is 4000 r/min; in S5, the thickness of the para-aramid pulp on the PP non-woven fabric is 200 mu m; in S6, the volume ratio of N-methyl pyrrolidone to water in the coagulation bath is 10:1, and the coagulation time is 6 min; heating at 100 deg.C for 8min in S8 to sublimate benzoic acid; pressing with hot press roller at 100 deg.C for 10 min; and the thickness of the para-aramid fiber layer in the finally prepared para-aramid nanofiber/PP non-woven fabric diaphragm is 10 mu m.
Table 1 shows the longitudinal tensile strength and porosity of the para-aramid nanofiber/PP nonwoven membrane and the PP nonwoven prepared in examples 1 to 5; the thickness of the film after the PP non-woven fabric and the para-aramid layer are compounded is equal to test the thickness of the film. As can be seen from the table, the PP non-woven fabric prepared by the preparation method provided by the invention has obviously enhanced longitudinal tensile strength, and the higher porosity of the PP non-woven fabric is kept.
TABLE 1
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents and are included in the scope of the present invention.
Claims (7)
1. A preparation method of a para-aramid nano-fiber/PP non-woven fabric diaphragm, which is characterized in that,
comprises the following steps:
s1, selecting PP non-woven fabric as a substrate material;
s2, preparing a pore-forming agent solution, dissolving benzoic acid in N-methyl pyrrolidone, wherein the concentration is 4-6mol/L, and the temperature of the N-methyl pyrrolidone is 60-80 ℃;
s3, immersing the PP non-woven fabric in the S1 into the pore-forming agent solution prepared in the S2, taking out the PP non-woven fabric after 4-8min, reducing the temperature of the PP non-woven fabric to be below 30 ℃, and cleaning the surface of the PP non-woven fabric to be flat and free of impurities;
s4, preparing para-aramid slurry, namely adding para-aramid resin with the viscosity of 5-8dL/g into concentrated sulfuric acid with the concentration of more than 98% for dissolving, adding N-methyl pyrrolidone, and stirring until a uniform solution is formed, wherein the stirring speed is 4000-;
s5, spraying atomized N-methyl pyrrolidone on the surface of the PP non-woven fabric cleaned in the S3, and then uniformly coating the para-aramid slurry prepared in the S4 on the surface of the PP non-woven fabric to obtain a prefabricated composite diaphragm, wherein the thickness of the slurry is 60-200 mu m;
s6, curing, namely putting the prefabricated composite diaphragm in the S5 into a coagulating bath consisting of N-methyl pyrrolidone and water for curing, wherein the volume ratio of the N-methyl pyrrolidone to the water in the coagulating bath is (8-10) to 1, and the coagulation time is 1-6 min;
s7, cleaning, namely washing the cured prefabricated composite diaphragm in the S6 by deionized water;
s8, pore-forming and hot-pressing, namely heating the cleaned prefabricated composite diaphragm in the S7 at the temperature of 100 ℃ and 125 ℃ for 5-10min, sublimating benzoic acid of the PP non-woven fabric layer, and leaving pores on the PP non-woven fabric layer; and carrying out hot-pressing shaping at the temperature of 100-.
2. The preparation method of the para-aramid nanofiber/PP non-woven fabric membrane as claimed in claim 1, wherein in S2, benzoic acid is dissolved in N-methyl pyrrolidone at a temperature of 70 ℃ at a concentration of 5 mol/L.
3. The preparation method of the para-aramid nanofiber/PP non-woven fabric diaphragm as claimed in claim 1, wherein in S3, the PP non-woven fabric is immersed for 6min and then taken out and then the temperature is reduced to 20 ℃.
4. The preparation method of the para-aramid nanofiber/PP non-woven fabric membrane as claimed in claim 1, wherein in S4, the volume ratio of concentrated sulfuric acid to N-methylpyrrolidone is 1: (2-10).
5. The method for preparing the para-aramid nanofiber/PP nonwoven membrane separator as claimed in claim 1, wherein the thickness of the para-aramid pulp on the PP nonwoven fabric is 100 μm in S5.
6. The preparation method of the para-aramid nanofiber/PP non-woven fabric diaphragm as claimed in claim 1, wherein in S6, the volume ratio of N-methyl pyrrolidone to water in a coagulation bath is 9:1, and the coagulation time is 4 min.
7. The preparation method of the para-aramid nanofiber/PP non-woven fabric membrane as claimed in claim 1, wherein benzoic acid is sublimed by heating at 120 ℃ for 8min in S8; pressing with hot-pressing roller at 120 deg.C for 3 min.
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CN112813692A (en) * | 2020-12-30 | 2021-05-18 | 山东聚芳新材料股份有限公司 | Preparation method of para-aramid nanofiber modified polypropylene melt-blown nonwoven fabric |
CN115149211A (en) * | 2022-08-09 | 2022-10-04 | 四川大学 | Double-layer composite diaphragm, preparation method thereof and HNTs @ PI-PP double-layer composite diaphragm |
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