CN112390986B - Preparation method of sandwich structure reinforced and toughened electromagnetic shielding composite film - Google Patents

Preparation method of sandwich structure reinforced and toughened electromagnetic shielding composite film Download PDF

Info

Publication number
CN112390986B
CN112390986B CN202011189822.0A CN202011189822A CN112390986B CN 112390986 B CN112390986 B CN 112390986B CN 202011189822 A CN202011189822 A CN 202011189822A CN 112390986 B CN112390986 B CN 112390986B
Authority
CN
China
Prior art keywords
solution
mixed solution
composite film
electromagnetic shielding
preparing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202011189822.0A
Other languages
Chinese (zh)
Other versions
CN112390986A (en
Inventor
王珍
许姗姗
方长青
黄颖为
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian University of Technology
Original Assignee
Xian University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian University of Technology filed Critical Xian University of Technology
Priority to CN202011189822.0A priority Critical patent/CN112390986B/en
Publication of CN112390986A publication Critical patent/CN112390986A/en
Application granted granted Critical
Publication of CN112390986B publication Critical patent/CN112390986B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073Shielding materials
    • H05K9/0081Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02Cellulose; Modified cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2375/00Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04Polyurethanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/02Cellulose; Modified cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2475/00Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2475/04Polyurethanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/10Metal compounds
    • C08K3/14Carbides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/28Nitrogen-containing compounds

Abstract

The invention discloses a preparation method of a sandwich structure reinforced and toughened electromagnetic shielding composite film, which comprises the following steps: preparing a few layers of MXene by using an etching stripping method, acidifying waste corrugated paper to obtain nano cellulose fibers, and then preparing a flexible film with a certain gradient and a sandwich structure by adding a water polyurethane solution by adopting an alternative suction filtration method. The invention obviously improves the mechanical property of the composite film on the basis of keeping the electromagnetic shielding property of the MXene material, and solves the problems of large brittleness, poor environmental tolerance and difficulty in bearing certain processing deformation of the MXene material. Meanwhile, the composite film prepared by the invention has the advantages of simple process, low cost and high repeatability. Is not easily affected by environmental factors such as temperature and humidity, and can be preserved for a long time.

Description

Preparation method of sandwich structure reinforced and toughened electromagnetic shielding composite film
Technical Field
The invention belongs to the technical field of material preparation, and relates to a preparation method of a sandwich structure reinforced and toughened electromagnetic shielding composite film.
Background
With the rapid development of electronic technology, functional electromagnetic materials and devices are widely used, so that the generated electromagnetic pollution is increasingly serious, the normal operation of electronic elements is interfered, and the long-term high-intensity electromagnetic radiation pollution can also cause potential harm to human health. The traditional electromagnetic shielding material mostly uses metal materials such as copper, aluminum and the like, has large specific gravity and large volume, and has poor acid and alkali resistance, so that the application of the traditional electromagnetic shielding material in the fields of movable equipment, wearable electronics, human body protection and the like is limited. Therefore, how to prepare the ultrathin, flexible, high-strength and high-toughness electromagnetic shielding material has important research significance and practical application value.
MXenes is a new class of two-dimensional layered structure transition metal carbides/carbonitrides. In recent years, MXene materials have been widely reported as electromagnetic shielding materials because of their characteristics such as large specific surface area and high conductivity. However, MXene also has the corresponding defects of poor mechanical property, high brittleness and difficulty in bearing certain degree of processing deformation, and the expansion of the application field of MXene is limited. The nano cellulose fiber is a natural polymer material, has the advantages of high mechanical strength, strong hydrophilicity, environmental protection and the like, and is often used as a mechanical reinforcing phase of a composite material. Its unique nanofiber structure will result in reduced insulating contact of the conducting nanosheet layer. In recent years, it has been reported that the compound can be used in the field of electromagnetic shielding by being compounded with graphene, graphene oxide, carbon nanotubes, and the like. However, it is difficult to improve both toughness and machinability of the material while maintaining its shielding properties. Therefore, a preparation method of the reinforced and toughened electromagnetic shielding composite film is needed to be found, so that the machinability of the electromagnetic shielding composite film is improved, and the application of the electromagnetic shielding composite film in the fields of flexible electronics, wearable equipment and the like is further widened.
The waterborne polyurethane is a well-known elastomer, the slippage between MXenes nanosheets is promoted through the interaction of a soft-segment polymer phase and MXenes, and the addition of the waterborne polyurethane greatly improves the toughness of the MXenes/polymer material. In addition, the aqueous polyurethane structure has a microphase separation structure, and urea groups on the main chain of the polyurethane polymer can be reacted with Ti3C2TxA large number of hydroxyl groups contained on the MXene surface form compact hydrogen bonds, so that the mechanical strength of the composite material is further improved.
Disclosure of Invention
The invention aims to provide a preparation method of a sandwich structure reinforced and toughened electromagnetic shielding composite film, which solves the problems that MXene serving as an electromagnetic shielding material in the prior art is poor in mechanical property, large in brittleness and difficult to bear certain processing deformation.
The technical scheme adopted by the invention is that the preparation method of the sandwich structure reinforced and toughened electromagnetic shielding composite film is implemented according to the following steps:
step 1, preparing MXene solution:
mixing LiF and HCl solution in a certain mass ratio to obtain mixed solution 1, and adding Ti into the mixed solution 13AlC2Obtaining a mixed solution 2, placing the mixed solution 2 in an oil bath at 35-45 ℃ for magnetic stirring for 24-36h, then centrifuging and washing to weak acidity, taking the precipitate for ultrasonic treatment, then centrifuging and separating, and taking the supernatant as MXene solution;
step 2, preparing a nano cellulose solution:
adding 50-70% of H by mass into a certain mass of waste corrugated paper powder2SO4Obtaining a mixed solution 3 from the solution, placing the mixed solution 3 in an oil bath at 40-50 ℃ for magnetic stirring, cleaning the mixed solution 3 to weak acidity by adopting a vacuum filtration mode, carrying out centrifugal separation, and taking supernatant fluid, namely the nano cellulose solution;
step 3, preparing a composite film:
mixing the MXene solution obtained in the step 1 and the nano-cellulose solution obtained in the step 2 according to a certain volume ratio to obtain a mixed solution 4, preparing 5-10mL of an aqueous polyurethane solution with the mass fraction of 4-8%, preparing the mixed solution 4 and the aqueous polyurethane solution into a sandwich structure film by adopting an alternative suction filtration method, and naturally airing at room temperature to obtain the electromagnetic shielding composite film.
The invention is also characterized in that:
LiF and Ti in step 13AlC2The mass ratio is 1: 1, mass ratio of LiF to HCl 1: 10-15, and the concentration of HCl is 8-12M.
The ultrasonic treatment time in the step 1 is 10-30 min.
In the step 1, the rotating speed of centrifugal separation in the step 1 is 3000-4000 r/min, and the centrifugal separation time is 30-60 min.
In the step 2, the mass ratio of the waste corrugated paper to the sulfuric acid is 1: 20 to 30.
And 2, magnetically stirring for 4-6 h.
The rotating speed of centrifugal separation in the step 2 is 5000-6000 r/min, and the centrifugal separation time is 5-15 min.
In the step 3, the volume ratio of the MXene solution to the cellulose solution is 4-6: 1.
the alternative suction filtration method in the step 3 specifically comprises the steps of firstly carrying out suction filtration on the mixed solution 4 to obtain a lower layer, then carrying out suction filtration on the aqueous polyurethane solution to obtain an intermediate layer, and then carrying out suction filtration on the mixed solution 4 to obtain an upper layer.
The invention has the beneficial effects that: the preparation method of the sandwich structure reinforced and toughened electromagnetic shielding composite film comprises the steps of preparing hydrophilic nano cellulose fibers by using waste corrugated paper, and preparing a flexible film with a certain gradient and a sandwich structure by adding a water polyurethane solution by adopting a simple alternative suction filtration method; on the basis of maintaining the MXene electromagnetic shielding performance, the mechanical property of the composite film is obviously improved, and the problems of high brittleness, poor environmental tolerance and difficulty in bearing certain processing deformation of the MXene material are solved; meanwhile, the composite film prepared by the invention has the advantages of simple process, low cost, high repeatability, insusceptibility to environmental factors such as temperature and humidity and long-term storage.
Drawings
FIG. 1 is a graph of the tensile mechanical properties of composite films prepared in examples 1-5 of the present invention;
FIG. 2 is a graph showing fracture toughness and electromagnetic shielding effectiveness of the composite films prepared in examples 1 to 5 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a sandwich structure reinforced and toughened electromagnetic shielding composite film, which is implemented according to the following steps:
step 1, preparing MXene solution:
mixing the components in a mass ratio of 1: mixing 10-15 LiF and HCl solution to obtain mixed solution 1, and adding Ti into the mixed solution 13AlC2Obtaining a mixed solution 2, LiF and Ti3AlC2The mass ratio is 1: 1, putting the mixed solution 2 in an oil bath at 35-45 ℃ for magnetic stirring for 24-36h, then centrifugally washing to weak acidity, taking the precipitate for ultrasonic treatment, wherein the ultrasonic treatment time is 10-30 min, then centrifugally separating, the rotational speed of centrifugal separation is 3000-4000 r/min, the time is 30-60 min, and taking the supernatant, namely the MXene solution;
step 2, preparing a nano cellulose solution:
adding 50-70% of H by mass into a certain mass of waste corrugated paper powder2SO4Obtaining a mixed solution 3 in the solution, wherein the mass ratio of the waste corrugated paper to the sulfuric acid is 1: 20-30, placing the mixed solution 3 in an oil bath at 40-50 ℃ for magnetic stirring for 4-6 hours, cleaning the mixed solution 3 to weak acidity by adopting a vacuum filtration mode, carrying out centrifugal separation at the rotating speed of 5000-6000 r/min for 5-15 min, and taking the supernatant as the nano cellulose solution;
step 3, preparing a composite film:
mixing the MXene solution obtained in the step 1 and the nano-cellulose solution obtained in the step 2 according to a volume ratio of 4-6: 1, mixing to obtain a mixed solution 4, preparing 5-10mL of an aqueous polyurethane solution with the mass fraction of 4-8%, and performing an alternative suction filtration method on the mixed solution 4 and the aqueous polyurethane solution, specifically, firstly performing suction filtration on the mixed solution 4 to obtain a lower layer, then performing suction filtration on the aqueous polyurethane solution to obtain a middle layer, then performing suction filtration on the mixed solution 4 to obtain an upper layer, preparing a sandwich structure film, and naturally drying at room temperature to obtain the electromagnetic shielding composite film.
Example 1
0.75g of LiF and 10mL of HCl solution (12M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added to the mixed solution 13AlC2Obtaining a mixed solution 2, placing the mixed solution 2 in an oil bath with the temperature of 35 ℃ for magnetic stirring for 24 hours, then centrifuging and washing to weak acidity, taking the precipitate for ultrasonic treatment for 10min, then centrifuging and separating, wherein the centrifugal speed is 3000r/min, the centrifugal time is 30min, and taking supernatant fluid, namely the supernatant fluidAs MXene solution.
Adding 20g of H with the mass fraction of 50% into 1g of waste corrugated paper powder2SO4Obtaining a mixed solution 3 from the solution, placing the mixed solution 3 in an oil bath at 40 ℃ for magnetic stirring for 4 hours, cleaning the mixed solution 3 to weak acidity by adopting a vacuum filtration mode, carrying out centrifugal separation, wherein the centrifugal rotation speed is 5000r/min, the centrifugal time is 5min, and taking supernatant fluid, namely the nano cellulose solution.
Weighing 40mL of MXene solution obtained in the step 1 and 10mL of nano-cellulose solution obtained in the step 2, mixing according to a certain volume ratio to obtain a mixed solution 4, preparing 6mL of aqueous polyurethane solution with the mass fraction of 4%, preparing the mixed solution 4 and the aqueous polyurethane solution into a sandwich structure film by adopting an alternative suction filtration method, and naturally airing at room temperature to obtain the electromagnetic shielding composite film.
Example 2
0.75g of LiF and 12mL of HCl solution (10M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added to the mixed solution 13AlC2And (3) obtaining a mixed solution 2, placing the mixed solution 2 in an oil bath at 37 ℃ for magnetic stirring for 30h, then centrifuging and washing to weak acidity, taking the precipitate for ultrasonic treatment for 20min, then centrifuging and separating, wherein the centrifugal rotating speed is 3250r/min, the centrifugal time is 38min, and taking the supernatant, namely the MXene solution.
Adding 22g of 60 mass percent H into 1g of waste corrugated paper powder2SO4Obtaining a mixed solution 3 from the solution, placing the mixed solution 3 in an oil bath at 42 ℃ for magnetic stirring for 4.5h, cleaning the mixed solution 3 to weak acidity by adopting a vacuum filtration mode, carrying out centrifugal separation, wherein the centrifugal rotation speed is 5500r/min, the centrifugal time is 10min, and taking the supernatant fluid, namely the nano cellulose solution.
Weighing 45mL of MXene solution obtained in the step 1 and 10mL of nano-cellulose solution obtained in the step 2, mixing according to a certain volume ratio to obtain a mixed solution 4, preparing 7mL of aqueous polyurethane solution with the mass fraction of 5%, preparing a sandwich structure film from the mixed solution 4 and the aqueous polyurethane solution by adopting an alternative suction filtration method, and naturally airing at room temperature to obtain the electromagnetic shielding composite film.
Example 3
0.75g of LiF and 12mL of HCl solution (10M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added to the mixed solution 13AlC2And (3) obtaining a mixed solution 2, placing the mixed solution 2 in an oil bath at 40 ℃ for magnetic stirring for 30h, then centrifuging and washing to weak acidity, taking the precipitate for ultrasonic treatment for 20min, then centrifuging and separating, wherein the centrifugal rotation speed is 3500r/min, the centrifugal time is 45min, and taking the supernatant, namely the MXene solution.
Adding 25g of 60 mass percent H into 1g of waste corrugated paper powder2SO4Obtaining a mixed solution 3 from the solution, placing the mixed solution 3 in an oil bath at 45 ℃ for magnetic stirring for 5 hours, cleaning the mixed solution 3 to weak acidity by adopting a vacuum filtration mode, carrying out centrifugal separation, wherein the centrifugal rotation speed is 5500r/min, the centrifugal time is 10min, and taking supernatant fluid, namely the nano cellulose solution.
Weighing 50mL of MXene solution obtained in the step 1 and 10mL of nano-cellulose solution obtained in the step 2, mixing according to a certain volume ratio to obtain a mixed solution 4, preparing 8mL of aqueous polyurethane solution with the mass fraction of 6%, preparing a sandwich structure film from the mixed solution 4 and the aqueous polyurethane solution by adopting an alternative suction filtration method, and naturally airing at room temperature to obtain the electromagnetic shielding composite film.
Example 4
0.75g of LiF and 14mL of HCl solution (11M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added to the mixed solution 13AlC2And (3) obtaining a mixed solution 2, placing the mixed solution 2 in a 42 ℃ oil bath, magnetically stirring for 32h, centrifuging and washing to be weakly acidic, taking the precipitate, performing ultrasonic treatment for 25min, then performing centrifugal separation, wherein the centrifugal rotation speed is 3750r/min, the centrifugal time is 52min, and taking the supernatant, namely the MXene solution.
Adding 27g of 65 mass percent H into 1g of waste corrugated paper powder2SO4Obtaining a mixed solution 3 from the solution, placing the mixed solution 3 in an oil bath at 48 ℃ for magnetic stirring for 5.5h, cleaning the mixed solution 3 to weak acidity by adopting a vacuum filtration mode, carrying out centrifugal separation, wherein the centrifugal rotation speed is 5750r/min, the centrifugal time is 12min, and taking the supernatant, namely the nano cellulose solution.
Weighing 55mL of MXene solution obtained in the step 1 and 10mL of nano-cellulose solution obtained in the step 2, mixing according to a certain volume ratio to obtain a mixed solution 4, preparing 9mL of aqueous polyurethane solution with the mass fraction of 7%, preparing the mixed solution 4 and the aqueous polyurethane solution into a sandwich structure film by adopting an alternative suction filtration method, and naturally airing at room temperature to obtain the electromagnetic shielding composite film.
Example 5
0.75g of LiF and 15mL of HCl solution (8M) were mixed to obtain a mixed solution 1, and 0.75g of Ti was added to the mixed solution 13AlC2And (3) obtaining a mixed solution 2, placing the mixed solution 2 in an oil bath at 45 ℃ for magnetic stirring for 36h, then centrifuging and washing to weak acidity, taking the precipitate for ultrasonic treatment for 30min, then centrifuging and separating, wherein the centrifugal speed is 4000r/min, the centrifugal time is 60min, and taking the supernatant, namely the MXene solution.
Adding 30g of H with the mass fraction of 50% into 1g of waste corrugated paper powder2SO4Obtaining a mixed solution 3 from the solution, placing the mixed solution 3 in an oil bath at 40 ℃ for magnetic stirring for 6 hours, cleaning the mixed solution 3 to weak acidity by adopting a vacuum filtration mode, carrying out centrifugal separation, wherein the centrifugal rotation speed is 6000r/min, the centrifugal time is 15min, and taking supernatant fluid, namely the nano-cellulose solution.
Measuring 60mL of MXene solution obtained in the step 1 and 10mL of nano-cellulose solution obtained in the step 2, mixing according to a certain volume ratio to obtain a mixed solution 4, preparing 10mL of aqueous polyurethane solution with the mass fraction of 8%, preparing the mixed solution 4 and the aqueous polyurethane solution into a sandwich structure film by adopting an alternative suction filtration method, and naturally airing at room temperature to obtain the electromagnetic shielding composite film.
FIG. 1 is a graph of tensile mechanical properties of the composite films prepared in examples 1-5, sample 0 representing a pure MXene sample, without added cellulose and aqueous polyurethane. Samples 1-5 are the samples in examples 1-5; the addition of the cellulose and the waterborne polyurethane can obviously improve the tensile strength and the breaking strain of the composite film; wherein, when the volume ratio of the added cellulose to MXene is 1: and 5, when 8mL of aqueous polyurethane solution with the mass fraction of 6% is added, the tensile mechanical property of the composite film is best.
Fig. 2 is a graph of fracture toughness and electromagnetic shielding effectiveness of the composite films prepared in examples 1-5, wherein sample 0 represents pure MXene sample without added cellulose and aqueous polyurethane. Samples 1-5 are the samples in examples 1-5; the addition of the cellulose and the waterborne polyurethane can obviously improve the toughness of the composite film; wherein when the volume ratio of the added cellulose to MXene is 1: 5, when 8mL of aqueous polyurethane solution with the mass fraction of 6% is added, the toughness of the composite film is strongest; meanwhile, the conductivity of the polymer is reduced along with the increase of the content of the waterborne polyurethane, so that the electromagnetic shielding performance of the composite film is slightly reduced; the mechanical property and the electromagnetic shielding property of the composite film are integrated, and the comprehensive property of the sample 3 is excellent, so that the composite film is reinforced and toughened and has high-efficiency electromagnetic shielding property.

Claims (7)

1. A preparation method of a sandwich structure reinforced and toughened electromagnetic shielding composite film is characterized by comprising the following steps:
step 1, preparing MXene solution:
mixing LiF and HCl solution in a certain mass ratio to obtain mixed solution 1, and adding Ti into the mixed solution 13AlC2Obtaining a mixed solution 2, placing the mixed solution 2 in an oil bath at 35-45 ℃ for magnetic stirring for 24-36h, then centrifuging and washing to weak acidity, taking the precipitate for ultrasonic treatment, then centrifuging and separating, and taking the supernatant as MXene solution;
step 2, preparing a nano cellulose solution:
adding 50-70% of H by mass into a certain mass of waste corrugated paper powder2SO4Obtaining a mixed solution 3 from the solution, placing the mixed solution 3 in an oil bath at 40-50 ℃ for magnetic stirring, cleaning the mixed solution 3 to weak acidity by adopting a vacuum filtration mode, carrying out centrifugal separation, and taking supernatant fluid, namely the nano cellulose solution;
step 3, preparing a composite film:
mixing the MXene solution obtained in the step 1 and the nano-cellulose solution obtained in the step 2 according to a volume ratio of 4-6: 1 to obtain a mixed solution 4, preparing 5-10mL of aqueous polyurethane solution with the mass fraction of 4-8%, carrying out suction filtration on the mixed solution 4 and the aqueous polyurethane solution alternately to obtain a lower layer by suction filtration of the mixed solution 4, then carrying out suction filtration of the aqueous polyurethane solution to obtain a middle layer, then carrying out suction filtration of the mixed solution 4 to obtain an upper layer, preparing a sandwich structure film, and naturally airing at room temperature to obtain the electromagnetic shielding composite film.
2. The method for preparing the sandwich structure reinforced and toughened electromagnetic shielding composite film according to claim 1, wherein LiF and Ti are used in the step 13AlC2The mass ratio is 1: 1, mass ratio of LiF to HCl 1: 10-15, and the concentration of HCl is 8-12M.
3. The preparation method of the sandwich structure reinforced and toughened electromagnetic shielding composite film according to claim 1, wherein the ultrasonic treatment time in the step 1 is 10-30 min.
4. The method for preparing the sandwich structure reinforced and toughened electromagnetic shielding composite film according to claim 1, wherein the rotational speed of the centrifugal separation in step 1 is 3000-4000 r/min, and the centrifugal separation time is 30-60 min.
5. The method for preparing the sandwich structure reinforced and toughened electromagnetic shielding composite film according to claim 1, wherein the mass ratio of the waste corrugated paper to the sulfuric acid in the step 2 is 1: 20 to 30.
6. The preparation method of the sandwich structure reinforced and toughened electromagnetic shielding composite film according to claim 1, wherein the magnetic stirring time in the step 2 is 4-6 hours.
7. The method for preparing the sandwich structure reinforced and toughened electromagnetic shielding composite film according to claim 1, wherein the rotational speed of the centrifugal separation in the step 2 is 5000-6000 r/min, and the centrifugal separation time is 5-15 min.
CN202011189822.0A 2020-10-30 2020-10-30 Preparation method of sandwich structure reinforced and toughened electromagnetic shielding composite film Active CN112390986B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011189822.0A CN112390986B (en) 2020-10-30 2020-10-30 Preparation method of sandwich structure reinforced and toughened electromagnetic shielding composite film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011189822.0A CN112390986B (en) 2020-10-30 2020-10-30 Preparation method of sandwich structure reinforced and toughened electromagnetic shielding composite film

Publications (2)

Publication Number Publication Date
CN112390986A CN112390986A (en) 2021-02-23
CN112390986B true CN112390986B (en) 2022-07-01

Family

ID=74598485

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011189822.0A Active CN112390986B (en) 2020-10-30 2020-10-30 Preparation method of sandwich structure reinforced and toughened electromagnetic shielding composite film

Country Status (1)

Country Link
CN (1) CN112390986B (en)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113047059B (en) * 2021-03-15 2022-11-11 合肥学院 Hydrophobic folding-resistant titanium carbide/polymer composite fabric and preparation method and application thereof
CN113087972A (en) * 2021-03-25 2021-07-09 北京林业大学 MXene/silver nanowire/nanocellulose composite film and preparation method thereof
CN113072725A (en) * 2021-03-31 2021-07-06 北京林业大学 Nano-cellulose/MXene/silver nanowire sandwich-structure composite film and preparation method thereof
CN113293655B (en) * 2021-05-27 2022-08-02 电子科技大学 Preparation method of MXene composite film with controllable thickness and novel structure
CN113645821B (en) * 2021-07-20 2024-01-16 西安理工大学 Preparation method of sandwich-structure FA/MXene/CNF composite material
CN113692211B (en) * 2021-08-09 2024-02-20 中国人民解放军陆军工程大学 Preparation method of composite film electromagnetic protection material based on MXene-rGO
CN114620706B (en) * 2022-02-10 2023-08-08 深圳市丽德宝纸品有限公司 Wood-based carbon sponge with high-efficiency electromagnetic shielding performance and preparation method and application thereof
CN115466408A (en) * 2022-08-12 2022-12-13 齐鲁工业大学 Preparation method of multifunctional conductive composite hydrogel based on nanocellulose

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101534298B1 (en) * 2014-06-17 2015-07-06 (주)다산 a composition for electro-magnetic interference shielding film, a method of fabricating a electro-magnetic interference shielding film therewith and an electro-magnetic interference shielding film fabricated thereby
CN107973920A (en) * 2017-11-15 2018-05-01 深圳大学 A kind of cellulose/two-dimensional layer Material cladding hydrogel and preparation method thereof
CN108264885A (en) * 2018-01-18 2018-07-10 北京林业大学 A kind of electromagnetic shielding film of mechanics enhancing and preparation method thereof
CN110436923A (en) * 2019-07-01 2019-11-12 深圳先进技术研究院 Electromagnetic shielding material and preparation method thereof
CN110698847A (en) * 2019-10-21 2020-01-17 西北工业大学 Waterborne polyurethane-MXene electromagnetic shielding bionic nano composite material film and preparation method thereof
WO2020097514A1 (en) * 2018-11-08 2020-05-14 Drexel University Mxene-based sensor devices
CN111303449A (en) * 2020-01-17 2020-06-19 华中科技大学 Degradable electroactive bacterial cellulose/MXene composite hydrogel and preparation and application thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019135533A1 (en) * 2018-01-05 2019-07-11 한국과학기술연구원 Method for manufacturing electromagnetic interference shielding film

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101534298B1 (en) * 2014-06-17 2015-07-06 (주)다산 a composition for electro-magnetic interference shielding film, a method of fabricating a electro-magnetic interference shielding film therewith and an electro-magnetic interference shielding film fabricated thereby
CN107973920A (en) * 2017-11-15 2018-05-01 深圳大学 A kind of cellulose/two-dimensional layer Material cladding hydrogel and preparation method thereof
CN108264885A (en) * 2018-01-18 2018-07-10 北京林业大学 A kind of electromagnetic shielding film of mechanics enhancing and preparation method thereof
WO2020097514A1 (en) * 2018-11-08 2020-05-14 Drexel University Mxene-based sensor devices
CN110436923A (en) * 2019-07-01 2019-11-12 深圳先进技术研究院 Electromagnetic shielding material and preparation method thereof
CN110698847A (en) * 2019-10-21 2020-01-17 西北工业大学 Waterborne polyurethane-MXene electromagnetic shielding bionic nano composite material film and preparation method thereof
CN111303449A (en) * 2020-01-17 2020-06-19 华中科技大学 Degradable electroactive bacterial cellulose/MXene composite hydrogel and preparation and application thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Bioinspired ultra-thin polyurethane/MXene nacre-like nanocomposite films with synergistic mechanical properties for electromagnetic interference shielding;Liu, Zongxu等;《JOURNAL OF MATERIALS CHEMISTRY C》;20200421;第8卷(第21期);第7170-7180页 *
Flexible, Robust, and Multifunctional Electromagnetic Interference Shielding Film with Alternating Cellulose Nanofiber and MXene Layers;Zhou, Bing等;《ACS APPLIED MATERIALS & INTERFACES》;20200103;第12卷(第4期);第4895-4905页 *

Also Published As

Publication number Publication date
CN112390986A (en) 2021-02-23

Similar Documents

Publication Publication Date Title
CN112390986B (en) Preparation method of sandwich structure reinforced and toughened electromagnetic shielding composite film
Chen et al. Porous aerogel and sponge composites: Assisted by novel nanomaterials for electromagnetic interference shielding
CN111809439B (en) Flexible high-strength MXene-based electromagnetic shielding composite film and preparation method thereof
CN109897343B (en) MXene aerogel/epoxy resin electromagnetic shielding nanocomposite and preparation method thereof
Liu et al. Aqueous solution-processed MXene (Ti3C2Tx) for non-hydrophilic epoxy resin-based composites with enhanced mechanical and physical properties
CN108530676B (en) Template-based three-dimensional reticular carbon material/high-molecular functional composite material and preparation method thereof
CN113817230A (en) CNF-MXene-PEI high-strength high-conductivity material and preparation method and application thereof
CN111132533A (en) MXene/silver nanowire composite electromagnetic shielding film
CN110606998B (en) MXene/natural rubber flexible composite film and preparation method thereof
CN109880178B (en) Nano-cellulose-reinforced graphene oxide/polydopamine layered bionic material and preparation method thereof
CN113005780B (en) Multi-layer MXenes electromagnetic shielding fabric and preparation method thereof
CN108439457B (en) Method for preparing zinc oxide nanorod/carbon cloth friction material by hydrothermal electrophoresis method
CN104403275A (en) Modified grapheme/thermosetting resin composite material and preparation method thereof
CN104893197B (en) A kind of preparation method of the oxycellulose composite membrane of water-resistant polyvinyl alcohol/load silver
CN106930100A (en) A kind of preparation method of polyimides/graphene oxide complex fiber material
CN109777044B (en) Electromagnetic shielding composite material based on graphene honeycomb structure and preparation method and application thereof
CN114164647B (en) Carbon fiber with multicomponent bionic hierarchical structure, preparation method and composite material
CN102924274A (en) Preparation method of conducting shell-like layered graphene composite material
CN113373728A (en) High-strength electromagnetic shielding and heat conducting ultrathin composite paper and preparation method and application thereof
CN113831686A (en) Preparation method of porous network composite material with shielding and sound absorption functions
CN115260551A (en) Preparation method of light graphene film for aerospace cable
Zou et al. Efficient electromagnetic interference shielding of flexible Ag microfiber sponge/polydimethylsiloxane composite constructed by blow spinning
Da et al. A high-performance, oxidation resistance and flexible Zn@ MXene/cellulose nanofibers electromagnetic shielding film
CN110438845B (en) Hydrophilic graphene, cellulose-based graphene flexible conductive nano-paper and preparation method thereof
CN108428565B (en) Tungsten disulfide/graphene oxide composite material, preparation method and application

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant