CN116023115A - Silicon aerogel-nanofiber composite membrane and preparation method thereof - Google Patents
Silicon aerogel-nanofiber composite membrane and preparation method thereof Download PDFInfo
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 127
- 239000012528 membrane Substances 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 82
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 32
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- 239000010703 silicon Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 79
- 239000004964 aerogel Substances 0.000 claims abstract description 42
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 32
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
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- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The application relates to the technical field of nanofiber materials, in particular to a silicon aerogel-nanofiber composite membrane and a preparation method thereof. The preparation method of the silicon aerogel-nanofiber composite membrane provided by the application comprises the following steps: adding water into the nanofiber, and stirring until the water is uniformly dispersed to obtain nanofiber water suspension; adding silicon aerogel particles into the nanofiber aqueous suspension, and stirring until the silicon aerogel particles are uniformly dispersed to obtain a mixed suspension; preparing the mixed suspension into a wet nanofiber composite membrane; and (3) carrying out gradient drying on the nanofiber composite membrane material, and then carrying out hot press molding to obtain the silica aerogel-nanofiber composite membrane. The silicon aerogel-nanofiber composite film prepared by the method has small thickness, compact structure and nanoscale porous structure.
Description
Technical Field
The application relates to the technical field of nanofiber materials, in particular to a silicon aerogel-nanofiber composite membrane and a preparation method thereof.
Background
The aerogel is a nano-scale porous solid material formed by replacing liquid phase in gel with gas in a certain drying mode through a sol-gel method, and the common aerogel is silicon aerogel. The silicon aerogel has a unique three-dimensional network pore structure, the average pore size is about 20 nanometers, the porosity is more than 90 percent, and the silicon aerogel is the material with the lowest heat conductivity at present.
The aerogel products in the market at present are mainly aerogel glass fiber mats, and the preparation method comprises the steps of forming sol by hydrolysis of a silicon source precursor, adopting the glass fiber mats as a reinforcing base material, and performing gum dipping, gel, aging, hydrophobic modification and drying. The aerogel glass fiber felt prepared by the method is filled with aerogel powder in gaps among fibers in the glass fiber felt, and the aerogel powder is fixed in the felt by the glass fiber network structure. Because the aerogel skeleton structure has poor strength and large brittleness, a large amount of aerogel powder breaks away from and escapes from the glass fiber mat when the aerogel skeleton structure is subjected to external force, and serious powder falling problems occur. In order to solve the powder falling problem, a technology of fixing aerogel powder by using nanofibers has been developed by researchers, for example, patent CN108035074a discloses a preparation method of a silica aerogel nanofiber composite membrane, specifically discloses a method of adding silica aerogel powder into a solvent to obtain a silica aerogel/organic solvent dispersion, then adding a polymer resin or powder, and finally obtaining a silica aerogel nanofiber composite material by an electrostatic spinning method. When the electrostatic spinning technology is adopted, the composite spinning solution is easy to block pinholes, the aerogel solid particles can change various spinning parameters such as viscosity, conductivity, surface tension and the like of a spinning solution system, the forming of nanofibers and the quality of nanofiber membranes are easily influenced, and the technical difficulties are multiple and the difficulty is high.
Based on the above analysis, it is important to provide a method of fixing aerogel that can improve the powder fall problem without affecting the quality of the nanofiber membrane.
Disclosure of Invention
The embodiment of the application provides a preparation method of a silicon aerogel-nanofiber composite membrane, which aims to solve the problems that in the related art, an aerogel nanofiber membrane is prepared by adopting electrostatic spinning, pinholes are blocked, and the quality of the nanofiber membrane is affected.
In a first aspect, the present application provides a method for preparing a silica aerogel-nanofiber composite membrane, comprising the steps of:
step S101, adding water into the nanofiber, and stirring until the water is uniformly dispersed to obtain nanofiber water suspension;
step S102, adding silicon aerogel particles into nanofiber aqueous suspension, and stirring until the silicon aerogel particles are uniformly dispersed to obtain mixed suspension;
step S103, preparing the mixed suspension into a wet nanofiber composite membrane;
step S104, carrying out gradient drying on the nanofiber composite membrane material, and then carrying out hot press molding to obtain the silicon aerogel-nanofiber composite membrane.
In some embodiments, the silica aerogel and nanofiber have a mass ratio of 1 to 20 on an oven dry mass basis: 1.
in some embodiments, the nanofibers are selected from aramid nanofibers. The aramid nanofibers are strong in hygroscopicity, expand in size after absorbing a large amount of water in a dispersing way, provide proton donors for the aramid nanofibers, generate a large amount of hydrogen bonds between the aramid nanofibers to be combined, and have strong film forming property; when the wet nanofiber composite membrane material is subjected to gradient drying, the expanded aramid nanofiber is dehydrated to cause that the weight of a single nanofiber is lighter and the diameter is smaller, the fibers are close to each other due to stronger hydrogen bond acting force, the number of pores in the nanofiber membrane is smaller, the size of the pores is smaller, the size of the whole membrane material is greatly contracted, the structure is more compact, aerogel particles uniformly embedded in the network structure of the nanofiber membrane are coated more tightly, the aerogel is not easy to separate, and the powder dropping amount is effectively reduced. In addition, the self-film forming and drying contractility of the aramid nanofiber is utilized to embed the silica aerogel particles into the composite film fiber network structure, the adhesive bonding is not needed, the process of adhesive curing and the like is not involved, the whole process is safe and pollution-free, the product is nontoxic and harmless, and the problems that the comprehensive performance of the composite material is reduced due to the fact that thermoplastic bonding fibers are introduced or resin impregnation or adhesive bonding and compounding are carried out when the aerogel composite material is prepared at present are avoided.
In some embodiments, the aramid nanofibers have a diameter of 3 to 20nm and a length of 2 to 10 μm.
In some embodiments, in step S101, the stirring speed is 500-1500 rpm and the stirring time is 20-60 min.
In some embodiments, in step S102, an ethoxypolydimethylsiloxane is also added to the nanofiber aqueous suspension in an amount of 0.2% to 1% by mass of the silica aerogel.
In some embodiments, in step S102, the stirring speed is 800-1800 rpm and the stirring time is 2-4 hours.
In some embodiments, in step S103, the mixed suspension is made into a wet nanofiber composite membrane by doctor blade coating or vacuum filtration.
In some embodiments, in step S104, the gradient drying process is as follows: drying is carried out at 40-50 ℃, 60-70 ℃, 80-90 ℃ and 100-110 ℃ in sequence, and the drying time at each temperature is 2-3 h.
In some embodiments, in step S104, the hot pressing conditions are: the pressure of the hot pressing line is 30-120 kN/m, and the hot pressing temperature is 220-280 ℃; the speed of the hot pressing roller is 2-6 m/min, and the hot pressing times are 1-2 times.
In some embodiments, the silica aerogel is prepared from an inorganic silica source or an organic silica source through hydrolysis, polycondensation, hydrophobic modification, normal pressure or supercritical drying, and the particle size of the silica aerogel is 0.2-500 μm.
In some preferred embodiments, the silicone source is one or a mixture of two of methyl orthosilicate, ethyl orthosilicate, methyltriethoxysilane, and dimethyldiethoxysilane.
In some preferred embodiments, the inorganic silicon source is one or a mixture of water glass and silicon tetrachloride.
In a second aspect, the present application further provides a silica aerogel-nanofiber composite membrane prepared by the above preparation method, wherein the temperature resistance of the silica aerogel-nanofiber composite membrane is not lower than 280 ℃, and the thickness of the silica aerogel-nanofiber composite membrane is 50-600 μm; UL94 horizontal burn test rating HB; the heat conductivity coefficient is 0.065-0.032W/m.K.
The silicon aerogel-nanofiber composite membrane prepared by the method can be applied to the field of light and refined electronic products.
According to the preparation method provided by the application, aerogel particles are added into the aqueous dispersion of the nanofibers, after being uniformly mixed, a wet nanofiber composite membrane material is obtained by adopting a mode of scraping a membrane or vacuum suction filtration, and after gradient drying, the nanofibers lose a large amount of adsorbed water, so that the diameter is reduced, the length is shortened, the composite membrane is contracted in size, a compact nanofiber membrane with certain strength is formed, and therefore the aerogel particles are firmly fixed in a nanofiber membrane network structure; the silicon aerogel particles have a nanoscale pore structure, and the nanofibers are mutually overlapped to form a nanoscale porous structure, so that the prepared composite film has the nanoscale porous structure.
The beneficial effects that technical scheme that this application provided brought include:
1. according to the preparation method provided by the application, firstly, the nano fibers are added with water for dispersion, then, silicon aerogel particles are directly added, and then, the moisture in the wet nano fiber composite membrane material is removed in a gradient drying mode, so that the quality of the nano fiber membrane is not affected, the high-efficiency heat insulation property of the silicon aerogel, the high-temperature resistance and flame retardance of the aramid nano fibers and the silicon aerogel are maintained, and the good mechanical strength and the appearance flatness of the nano fiber membrane are also ensured;
2. according to the method, micron-sized aerogel particles are uniformly and firmly embedded in the composite membrane fiber net, aerogel is not easy to separate and escape, the composite membrane is less in powder falling, and the problem of serious powder falling of the traditional aerogel composite material is solved;
3. the silicon aerogel-nanofiber composite membrane prepared by the method has small thickness, compact structure and nano-scale porous structure, solves the problems that the existing aerogel composite material has large thickness and cannot be applied to occasions with limited space or high requirements on material fineness, and greatly expands the application of the lightweight heat-insulating, high-temperature-resistant and flame-retardant composite membrane.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic flow chart of a preparation method of a silica aerogel-nanofiber composite membrane according to an embodiment of the present application;
FIG. 2 is a product diagram of the silica aerogel-nanofiber composite membrane prepared in example 1 of the present application;
FIG. 3 is a product graph of the silica aerogel-nanofiber composite membrane prepared in example 3 of the present application.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
The embodiment of the application provides a preparation method of a silicon aerogel-nanofiber composite membrane, which can solve the problems of pinhole blockage and nanofiber membrane quality influence existing in the preparation of an aerogel nanofiber membrane by adopting electrostatic spinning in the prior art.
Fig. 1 is a schematic flow chart of a preparation method of a silica aerogel-nanofiber composite membrane provided by the application, and referring to fig. 1, the preparation method provided by the application comprises the following steps:
step S101, adding water into nano fibers with the diameter of 3-20 nm, and stirring at the rotating speed of 500-1500 rpm until the nano fibers are uniformly dispersed to obtain nano fiber water suspension;
step S102, adding silicon aerogel particles with the particle size of 0.2-500 mu m into nanofiber water suspension, and stirring at the rotating speed of 800-1800 rpm until the particles are uniformly dispersed to obtain mixed suspension;
step S103, preparing the mixed suspension into a wet nanofiber composite membrane;
step S104, drying the nanofiber composite membrane material at 40-50 ℃, 60-70 ℃, 80-90 ℃ and 100-110 ℃ in sequence, and then performing hot press molding to obtain the silica aerogel-nanofiber composite membrane; the conditions of hot pressing are: the pressure of the hot pressing line is 30-120 kN/m, and the hot pressing temperature is 220-280 ℃; the speed of the hot pressing roller is 2-6 m/min, and the hot pressing times are 1-2 times.
The silica aerogel-nanofiber composite membrane provided by the application and the preparation method thereof are described in detail below with reference to examples.
Example 1:
example 1 provides a method for preparing a silica aerogel-nanofiber composite membrane, comprising the steps of:
(1) Adding water into 1 part of aramid nanofiber by mass, and stirring at 600rpm for 30min to obtain nanofiber aqueous suspension;
(2) Adding 5 parts by mass of silicon aerogel particles into the nanofiber aqueous suspension, and stirring at a rotating speed of 1200rpm for 2 hours to obtain a mixed suspension;
(3) Preparing the mixed suspension into a wet nanofiber composite membrane by adopting a vacuum suction filtration mode;
(4) And (3) drying the nanofiber composite membrane material at 40 ℃, 60 ℃, 80 ℃ and 100 ℃ in sequence, drying for 2 hours at each temperature, and then hot-pressing for 1 time according to the conditions of the line pressure of 40kN/m, the hot-pressing temperature of 255 ℃ and the hot-pressing roller speed of 3m/min to obtain the silica aerogel-nanofiber composite membrane.
The product diagram of the silica aerogel-nanofiber composite membrane prepared in example 1 is shown in fig. 2, and it can be seen from fig. 2 that the composite membrane has a flat appearance.
Example 2:
example 2 provides a method for preparing a silica aerogel-nanofiber composite membrane, comprising the steps of:
(1) Adding water into 1 part of aramid nanofiber by mass, and stirring at 800rpm for 40min to obtain nanofiber aqueous suspension;
(2) Adding 10 parts by mass of silicon aerogel particles into the nanofiber aqueous suspension, and stirring at a rotating speed of 1500rpm for 2.5 hours to obtain a mixed suspension;
(3) Preparing the mixed suspension into a wet nanofiber composite membrane by adopting a scraper coating mode;
(4) And (3) drying the nanofiber composite membrane material at 45 ℃, 60 ℃, 85 ℃ and 100 ℃ in sequence, drying for 3 hours at each temperature, and then hot-pressing for 2 times according to the conditions of the line pressure of 50kN/m, the hot-pressing temperature of 260 ℃ and the hot-pressing roller speed of 5m/min to obtain the silica aerogel-nanofiber composite membrane.
Example 3:
example 3 provides a method for preparing a silica aerogel-nanofiber composite membrane, comprising the steps of:
(1) Adding water into 4 parts of aramid nanofibers by mass, and stirring at 600rpm for 40min to obtain nanofiber aqueous suspension;
(2) Adding 36 parts by mass of silicon aerogel particles into the nanofiber aqueous suspension, and stirring at a rotating speed of 1800rpm for 3.5 hours to obtain a mixed suspension;
(3) Preparing the mixed suspension into a wet nanofiber composite membrane by adopting a scraper coating mode;
(4) And (3) drying the nanofiber composite membrane material at 50 ℃, 60 ℃, 90 ℃ and 110 ℃ in sequence, drying for 2 hours at each temperature, and then hot-pressing for 2 times according to the conditions of line pressure of 60kN/m, hot-pressing temperature of 250 ℃ and hot-pressing roller speed of 3m/min to obtain the silica aerogel-nanofiber composite membrane.
The product graph of the silica aerogel-nanofiber composite membrane prepared in example 3 is shown in fig. 3, and it can be seen from fig. 3 that the composite membrane has a flat appearance.
Example 4:
example 4 provides a method for preparing a silica aerogel-nanofiber composite membrane, comprising the steps of:
(1) Adding water into 1 part of aramid nanofiber by mass, and stirring at 600rpm for 40min to obtain nanofiber aqueous suspension;
(2) 15 parts of silicon aerogel particles and 0.015 part of ethoxy polydimethylsiloxane are added into the nanofiber water suspension, and the mixture is stirred for 3 hours at a rotating speed of 1500rpm to obtain a mixed suspension;
(3) Preparing the mixed suspension into a wet nanofiber composite membrane by adopting a vacuum suction filtration mode;
(4) And (3) drying the nanofiber composite membrane material at 50 ℃, 70 ℃, 85 ℃ and 105 ℃ in sequence, drying for 3 hours at each temperature, and then hot-pressing for 1 time according to the conditions of line pressure of 60kN/m, hot-pressing temperature of 260 ℃ and hot-pressing roller speed of 3m/min to obtain the silica aerogel-nanofiber composite membrane.
The composite films prepared in examples 1 to 4 were subjected to thickness measurement and performance test, and the results are shown in Table 1.
Table 1: results of thickness and Performance test of composite films prepared in examples 1-4
In Table 1, flame retardant ratings were made according to UL94 horizontal burn test standards.
As can be seen from table 1, the composite films prepared in examples 1 to 4 of the present application have high heat insulation properties and excellent high temperature resistance and flame retardance.
In the description of the present specification, reference to the terms "one embodiment/manner," "some embodiments/manner," "example," "a particular example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment/manner or example is included in at least one embodiment/manner or example of the present application. In this specification, the schematic representations of the above terms are not necessarily for the same embodiment/manner or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments/modes or examples. Furthermore, the various embodiments/modes or examples described in this specification and the features of the various embodiments/modes or examples can be combined and combined by persons skilled in the art without contradiction.
It should be noted that in this application, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element. In the present application, the meaning of "plurality" means at least two, for example, two, three, etc., unless explicitly specified otherwise.
The foregoing is merely a specific embodiment of the application to enable one skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The preparation method of the silica aerogel-nanofiber composite membrane is characterized by comprising the following steps of:
s101, adding water into the nanofiber, and stirring until the water is uniformly dispersed to obtain nanofiber water suspension;
s102, adding silicon aerogel particles into nanofiber aqueous suspension, and stirring until the silicon aerogel particles are uniformly dispersed to obtain mixed suspension;
s103, preparing the mixed suspension into a wet nanofiber composite membrane;
s104, carrying out gradient drying on the nanofiber composite membrane material, and then carrying out hot press molding to obtain the silicon aerogel-nanofiber composite membrane.
2. The method for preparing a silica aerogel-nanofiber composite membrane according to claim 1, wherein the mass ratio of the silica aerogel to the nanofiber is 1-20 in terms of absolute dry mass: 1.
3. the method for preparing a silica aerogel-nanofiber composite membrane according to claim 1, wherein the particle size of the silica aerogel is 0.2-500 μm.
4. The method for preparing a silica aerogel-nanofiber composite membrane according to claim 1, wherein the nanofiber is an aramid nanofiber.
5. The method for preparing a silica aerogel-nanofiber composite membrane according to claim 4, wherein the diameter of the aramid nanofiber is 3-20 nm.
6. The method of claim 1, wherein in step S103, the method of preparing the mixed suspension into the wet nanofiber composite membrane is a doctor blade.
7. The method of preparing silica aerogel-nanofiber composite membrane according to claim 1, wherein in step S103, the mode of preparing the mixed suspension into the wet nanofiber composite membrane is vacuum filtration.
8. The method for preparing a silica aerogel-nanofiber composite membrane according to claim 1, wherein the gradient drying process is as follows: drying at 40-50 deg.c, 60-70 deg.c, 80-90 deg.c and 100-110 deg.c successively.
9. The method of preparing a silica aerogel-nanofiber composite membrane according to claim 1, wherein in step S104, the hot pressing conditions are: the pressure of the hot pressing line is 30-120 kN/m, and the hot pressing temperature is 220-280 ℃; the speed of the hot pressing roller is 2-6 m/min, and the hot pressing times are 1-2 times.
10. The silica aerogel-nanofiber composite membrane produced by the production method according to any one of claims 1 to 9.
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Citations (6)
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US20210062429A1 (en) * | 2019-08-26 | 2021-03-04 | Hunan University | Aramid nanofiber-based insulation paper and preparation method thereof |
US20220238959A1 (en) * | 2019-11-08 | 2022-07-28 | South China University Of Technology | Functional coating material for lithium ion battery separator and preparation method therefor |
CN113308931A (en) * | 2021-05-28 | 2021-08-27 | 陕西科技大学 | Aramid nano paper and preparation method thereof |
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