CN112500609A - Light high-strength cellulose nanocrystalline/graphene composite film and preparation method thereof - Google Patents
Light high-strength cellulose nanocrystalline/graphene composite film and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of electromagnetic shielding, and discloses a light high-strength cellulose nanocrystalline/graphene composite electromagnetic shielding film and a preparation method thereof, wherein a Cellulose Nanocrystalline (CNC) solution and a Graphene Oxide (GO) solution are mixed, uniformly stirred and subjected to ultrasonic treatment to obtain a uniformly dispersed CNC/GO mixed solution; drying by a film forming method to obtain a CNC/GO film; and reducing by using a reducing agent, cleaning the residual reducing agent on the surface, mechanically compressing and drying to obtain the cellulose nanocrystal/graphene composite film. The electromagnetic shielding film provided by the invention has the characteristics of being ultrathin, hydrophobic, flexible, high in mechanical strength and the like, overcomes the defects of poor mechanical strength and large thickness of the existing carbon-based electromagnetic shielding material, and has great application potential in the field of rapidly-growing flexible electronics.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding, and particularly relates to a light high-strength cellulose nanocrystal/graphene composite film and a preparation method thereof.
Background
In the world, with the rapid development of modern electronic technology, problems such as electromagnetic interference and electromagnetic radiation cause great attention due to the harm to precise electronic equipment and human health. At present, the most widely used metal and metal oxide electromagnetic shielding materials are greatly limited in practical application due to the defects of high material density, high rigidity, easy corrosion, high production and processing difficulty, high price and the like, and are difficult to meet the requirements of light weight, small size, folding and the like on the electromagnetic shielding materials. Compared with the traditional metal electromagnetic shielding material, the graphene serving as a novel two-dimensional nano carbon material has extremely excellent electrical, mechanical and thermodynamic properties, and the excellent properties enable the graphene to have excellent potential as an electromagnetic shielding material after being formed into a composite material with a high polymer material, particularly in the fields of airplanes, aerospace, fast-growing flexible electronics and the like.
However, the strong van der waals force existing between the graphenes limits the application of the graphenes as electromagnetic interference shielding materials. Graphene Oxide (GO), the most readily available precursor for graphene, is an ideal choice for preparing such materials due to its potential electrical conductivity, high processability and good dispersibility in aqueous media. Research shows that the graphene oxide is reduced after being loaded by 5-33%, so that the composite material can meet the requirement (20dB) of a commercial electromagnetic shielding material in an X wave band, but the sample thickness of 2.5-60 mm makes the composite material incapable of being used for portable equipment (Yan et al, Advanced Functional Materials,2015,25(4): 559-. On the other hand, electromagnetic shielding materials with higher GO concentration are also reported at present. For example, Shen et al (Advanced Functional Materials,2014,24(28):4542-4548) and Kumar et al (Carbon,2015:494-500) prepared reduced graphene oxide films with thicknesses of 8.4 μm and 15 μm by thermochemical and chemical reduction methods respectively have electromagnetic shielding effectiveness of 20dB and 15dB, but the graphene films prepared by the method have poor mechanical strength, which greatly limits the practical application thereof. Therefore, it is still a challenge to prepare an electromagnetic shielding material with ultra-thin thickness and high mechanical strength.
The nano cellulose whisker (CNC) has the characteristics of degradability, reproducibility, good biocompatibility and the like, and gradually arouses the interest of scholars in the electronic and energy storage industry in recent years. The CNC has excellent mechanical strength, and can obviously improve the mechanical strength of the composite material; meanwhile, the CNC surface contains a large amount of hydroxyl groups, has a large specific surface area, and can be used as a dispersing agent in the composite material, so that the agglomeration problem of the material and the bonding performance of the composite material interface are improved.
Through the above analysis, the problems and defects of the prior art are as follows:
(1) the existing metal and metal oxide electromagnetic shielding materials are greatly limited in practical application due to the defects of large material density, large rigidity, easy corrosion, large production and processing difficulty, high price and the like, and are difficult to meet the requirements of light weight, small size and folding of the electromagnetic shielding materials in the fields of aerospace, portable electronic products, portable wearable electronic equipment and the like.
(2) Most of the existing graphene-based electromagnetic shielding materials have the problems of large thickness, poor mechanical strength and nonuniform dispersion of graphene inside.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a light high-strength cellulose nanocrystal/graphene composite film which has the characteristics of ultrathin thickness, flexibility and high mechanical strength and has great application potential in the field of rapidly-growing flexible electronics.
The invention also aims to provide a light high-strength cellulose nanocrystalline/graphene composite film and a preparation method thereof.
The invention also aims to provide application of the nano-cellulose/graphene composite flexible film as an electromagnetic shielding material in the fields of aerospace, portable electronic products, portable wearable electronic equipment and the like, and the preparation method of the light high-strength cellulose nanocrystalline/graphene composite film comprises the following steps:
the method comprises the following steps: mixing a Cellulose Nanocrystalline (CNC) solution with a Graphene Oxide (GO) solution, uniformly stirring, and performing ultrasonic treatment to obtain a uniformly dispersed CNC/GO mixed solution;
step two: drying by a film forming method to obtain a CNC/GO film;
step three: and reducing by using a reducing agent, cleaning the residual reducing agent on the surface, mechanically compressing and drying to obtain the cellulose nanocrystal/graphene composite film.
Preferably, the cellulose nanocrystal is obtained by an acid hydrolysis method or an enzyme hydrolysis method, and the used raw materials comprise various biomass materials such as wood, bamboo, cotton, paper pulp and the like.
Preferably, the graphene oxide has a two-dimensional sheet structure.
Preferably, the concentration of the cellulose nanocrystal solution is 0.02-10 mg/mL.
Preferably, the concentration of the graphene oxide solution is 0.02-10 mg/mL.
Preferably, in the first step, the mass ratio of the cellulose nanocrystal solution to the graphene oxide solution is 1: 9-7: 3.
Preferably, in the first step, the stirring speed is 300-1000 rpm, the time is 4-12 hours, the temperature is 20-50 ℃, the ultrasonic time is 10-40 min, and the ultrasonic power is 600-1000W.
Preferably, in the second step, the film forming method includes a vacuum filtration method, a solvent evaporation method, a blade coating method, a spin coating method, and the like; the drying method comprises room temperature drying, vacuum drying, oven drying and the like.
Preferably, in the second step and the third step, the drying method comprises room temperature drying, vacuum drying, oven drying and the like.
Preferably, in step three, the reducing agent includes hydroiodic acid, ascorbic acid, hydrazine hydrate, amines and the like.
Preferably, in the third step, the mechanical compression pressure is 10-350 MPa, and the compression time is 10-60 min.
An electromagnetic shielding isolation film in the aerospace field, which is prepared from any one of the light high-strength cellulose nanocrystal/graphene composite films.
The light high-strength cellulose nanocrystalline/graphene composite film is applied as an electromagnetic shielding film in the fields of various portable electronic products, portable wearable electronic equipment and the like.
By combining all the technical schemes, the invention has the advantages and positive effects that:
the raw materials of the invention have rich sources, easy obtaining and low cost, and the preparation method has simple operation process and is beneficial to large-scale production; meanwhile, hydrophilic CNC is used as a raw material, so that the reduction time of the CNC/GO composite film can be remarkably reduced.
The CNC used for the light high-strength cellulose nanocrystalline/graphene composite film provided by the invention can effectively improve the dispersity of GO. The CNC and GO form an orderly arranged layered structure through layer-by-layer self-assembly, wherein one-dimensional CNC is orderly deposited between two-dimensional GO sheet structures to form a three-dimensional 'brick-mud' layered composite structure similar to a pearl layer.
The CNC used for the light high-strength cellulose nanocrystalline/graphene composite film provided by the invention can obviously improve the mechanical strength of the graphene film (the highest tensile strength of the film reaches 227MPa and is far better than the currently reported carbon-based electromagnetic shielding composite material); meanwhile, the brick-mud laminated composite structure formed by the CNC and the graphene can also effectively improve the electromagnetic shielding efficiency of the graphene film.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
FIG. 1 is a schematic diagram of the morphology of a cellulose nanocrystal/graphene composite film and raw materials. (a, b), composite film optical photographs; (c) the profile of the film; (d) CNC atomic force microscope height maps; (e) atomic force microscope height map of GO; (f) single layer GO height map
FIG. 2 is SEM images of the cross section of the thin film provided by the embodiment of the invention at different magnifications (b-d) before (a) and after (b-d) mechanical compression.
Fig. 3 is a schematic diagram of a "brick-clay" layered composite structure formed by self-assembly of cellulose nanocrystals and graphene according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a preparation method and application of a light high-strength cellulose nanocrystal/graphene composite film, and the invention is described in detail with reference to the accompanying drawings.
In the specific embodiment of the invention, the Cellulose Nanocrystals (CNC) are prepared from moso bamboo fiber cells and parenchyma cells serving as raw materials respectively by an acid hydrolysis method according to the following method:
dissolving alpha-cellulose sample of fibroblast and parenchyma cell in 60 wt% of H2SO4Reacting in the solution for 2 hours at the reaction temperature of 50 ℃ and the solid-to-liquid ratio of 1:20 (g/mL); after the reaction is finished, the mixture is used immediatelyThe reaction was terminated by 10-fold dilution with deionized water. And then repeatedly centrifuging to remove the surplus acid until the pH value reaches 3-4, filling the solution into a dialysis bag (with the molecular weight of 7000), and dialyzing with deionized water for 5-7 days until the pH value is 7. And putting the neutral solution after dialysis in an ice-water bath, and carrying out ultrasonic treatment for 0.5h by using an ultrasonic cell pulverizer (JY98-IIID, Ningbo) under the condition of output power of 800W to obtain uniformly dispersed fiber cell nanocrystalline (F-CNC) and thin-wall cell nanocrystalline (P-CNC) solutions. The prepared CNC morphologies were all rod-shaped, as shown in FIG. 1 d.
The graphene oxide is prepared by the following method:
under the conditions of ice bath and stirring, 3g of natural graphite powder and 1.5g of sodium nitrate are respectively and slowly added into a container filled with 69mL of 98 wt% H2SO4In a beaker. After stirring for 15min, 9g of potassium permanganate is slowly added, and the liquid in the beaker gradually changes from black to dark green. After 1.5h, the reaction system is transferred to a water bath with the temperature of 35 ℃ to continue the reaction for 2h, and the medium temperature reaction is completed. Then, the reaction system is transferred to a water bath with the temperature of 90 ℃ for reaction for 20min, 500mL of warm deionized water is slowly added to dilute the solution, 15mL of hydrogen peroxide (30 wt%) is added, and the solution is stirred for 10min to fully react the unreduced potassium permanganate, so that the solution is changed from dark green to bright yellow. Filtering while hot, washing the brown yellow precipitate with 5% hydrochloric acid and a large amount of deionized water until the precipitate is neutral to obtain graphite oxide, and air drying. After that, the mixture was dispersed in 750mL of deionized water and dialyzed for one week (molecular weight: 500). Centrifuging the dialyzed sample at 10000rpm for 20min, collecting lower-layer solid, dispersing the lower-layer solid with 500mL of deionized water, continuously centrifuging the sample at 4000rpm for 30min to remove solid residues, wherein the upper-layer liquid is GO dispersion, and ultrasonically treating the GO dispersion for 0.5h by using an ultrasonic cell disruptor (JY98-IIID, Ningbo) under the condition of output power of 800W to obtain the uniformly dispersed GO dispersion. GO is in a two-dimensional sheet structure, and the thickness of GO is about 2nm (1-2 layers) through an atomic force microscope, which indicates that GO prepared in the experiment is in an ideal single-layer or double-layer structure (shown in figures 1 e-f).
Example 1:
the preparation method of the nanocrystalline/graphene composite film specifically comprises the following steps:
compounding GO and CNC: mixing 100mL of 0.05mg/mL F-CNC aqueous solution and 100mL of 0.45mg/mL GO water dispersion (the mass ratio of the CNC uniform dispersion to the GO uniform dispersion is 1:9), stirring for 12h at 25 ℃, performing ultrasonic treatment for 30min, and performing ultrasonic treatment at the power of 800W to obtain a uniformly mixed CNC/GO solution;
preparing a CNC/GO film: carrying out suction filtration on the CNC/GO mixed solution obtained in the step (1) by adopting a vacuum filtration method to form a membrane, wherein the vacuum filtration membrane is a hydrophilic mixed cellulose filtration membrane, the aperture is 0.2 mu m, and the diameter is 50mm, then drying at room temperature, and tearing off the filtration membrane after drying to obtain a CNC/GO membrane;
nanocrystalline/graphene film: immersing the CNC/GO film obtained in the step (2) in a hydriodic acid solution, reducing GO by hydriodic acid steam at 85 ℃, taking out the film after 10min, repeatedly washing the film for 5 times by using ethanol and deionized water, then pressing the film for 0.5h under the pressure of 20MPa by using an infrared tablet press, and drying the film at room temperature to obtain the nanocrystalline/graphene composite film.
Through the steps, the prepared nanocrystalline/graphene composite electromagnetic shielding film has the thickness of 12 microns, the electric conductivity of 14388S/m, the tensile strength of 173.9MPa, the Young modulus of 4.16GPa and the electromagnetic shielding performance of 39 dB.
The prepared nanocrystalline/graphene composite film is shown in fig. 1, and the film can not be damaged under the conditions of 360-degree bending and folding, which shows that the film has better flexibility. The film is internally layered, but before mechanical compression, certain gaps are formed between the inner layers (as shown in figure 2 a); after mechanical compression, the layers become more compact from layer to layer (see fig. 2 b). Further enlarging the layered structure, it can be found that the CNC and graphene are highly orderly arranged between the layered structure (fig. 2c-d), wherein the one-dimensional CNC is orderly deposited between the two-dimensional graphene lamellar structures to form a three-dimensional nacreous "brick-mud" composite structure, the structure diagram of which is shown in fig. 3.
Example 2:
the preparation method of the nanocrystalline/graphene composite film specifically comprises the following steps:
compounding GO and CNC: mixing 100mL of 0.25mg/mL P-CNC aqueous solution and 50mL of 0.5mg/mL GO water dispersion (the mass ratio of the CNC uniform dispersion to the GO uniform dispersion is 5:5), stirring for 6h at 25 ℃, performing ultrasonic treatment for 30min, and performing ultrasonic treatment at the power of 800W to obtain a uniformly mixed CNC/GO solution;
preparing a CNC/GO film: carrying out suction filtration on the CNC/GO mixed solution obtained in the step (1) by adopting a vacuum filtration method to form a membrane, wherein the vacuum filtration membrane is a hydrophilic mixed cellulose filtration membrane, the aperture is 0.2 mu m, and the diameter is 50mm, then drying at room temperature, and tearing off the filtration membrane after drying to obtain a CNC/GO membrane;
nanocrystalline/graphene film: immersing the CNC/GO film obtained in the step (2) in a hydriodic acid solution, reducing GO by hydriodic acid steam at 85 ℃, taking out the film after 5min, repeatedly washing the film for 5 times by using ethanol and deionized water, pressing the film for 0.5h under the pressure of 25MPa by using an infrared tablet press, and drying the film at room temperature to obtain the nanocrystalline/graphene composite film.
Through the steps, the prepared nanocrystalline/graphene composite electromagnetic shielding film has the thickness of 18 microns, the electric conductivity of 4612S/m, the tensile strength of 227MPa, the Young modulus of 6.52GPa and the electromagnetic shielding performance of 30 dB.
According to the invention, CNC is used as a dispersing agent and a reinforcement and compounded with GO to prepare the flexible conductive film, and the comprehensive performance of the CNC/GO composite film applied to the field of electromagnetic shielding is further explored. In addition, according to the knowledge of the inventor, the CNC is also used as the substrate for the first time to be applied to the electromagnetic shielding material, and further the application range of the CNC in the electronic field can be widened.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The preparation method of the light high-strength cellulose nanocrystal/graphene composite conductive film is characterized by comprising the following steps of:
the method comprises the following steps: mixing a Cellulose Nanocrystalline (CNC) solution with a Graphene Oxide (GO) solution, uniformly stirring, and performing ultrasonic treatment to obtain a uniformly dispersed CNC/GO mixed solution;
step two: drying by a film forming method to obtain a CNC/GO film;
step three: and reducing by using a reducing agent, cleaning the residual reducing agent on the surface, mechanically compressing and drying to obtain the cellulose nanocrystal/graphene composite film.
2. The method according to claim 1, wherein the cellulose nanocrystals are obtained by acid hydrolysis or enzymatic hydrolysis, and the raw materials include various wood, bamboo, cotton, and pulp biomass materials.
3. The method according to claim 1, wherein the graphene oxide has a two-dimensional sheet structure.
4. The method of claim 1, wherein the concentration of the cellulose nanocrystal solution is 0.02 to 10 mg/mL; the concentration of the graphene oxide solution is 0.02-10 mg/mL.
5. The preparation method of claim 1, wherein in the first step, the mass ratio of the cellulose nanocrystal solution to the graphene oxide solution is 1: 9-7: 3.
6. The preparation method of claim 1, wherein in the first step, the stirring speed is 300-1000 rpm, the time is 4-12 h, the temperature is 20-50 ℃, the ultrasonic time is 10-40 min, and the ultrasonic power is 600-1000W.
7. The production method according to claim 1, wherein in the second step, the film forming method includes a vacuum filtration method, a solvent evaporation method, a blade coating method, a spin coating method, or the like; the drying method comprises room temperature drying, vacuum drying and oven drying.
8. The method according to claim 1, wherein in the second step and the third step, the drying method comprises room temperature drying, vacuum drying, oven drying;
in the third step, the reducing agent comprises hydriodic acid, ascorbic acid, hydrazine hydrate and amines.
9. The method of claim 1, wherein in step three, the mechanical compression pressure is 10 to 350MPa, and the compression time is 10 to 60 min.
10. An electromagnetic shielding isolation film in the aerospace field, various portable electronic products, portable wearable electronic equipment and other fields, which is prepared by applying the light high-strength cellulose nanocrystal/graphene composite film in any one of claims 1 to 9.
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| CN114149619A (en) * | 2021-12-17 | 2022-03-08 | 北京化工大学 | Preparation method of graphene/cellulose composite material |
| CN114163694A (en) * | 2021-12-23 | 2022-03-11 | 清远高新华园科技协同创新研究院有限公司 | Light transparent wave-absorbing heat-conducting composite material and preparation method and application thereof |
| WO2023221279A1 (en) * | 2022-05-19 | 2023-11-23 | 浙江理工大学 | Preparation method for rgo/cnc/cnf composite thin film |
| CN114957805A (en) * | 2022-05-24 | 2022-08-30 | 南京林业大学 | Two-dimensional cellulose nano fluid channel membrane and preparation method and application thereof |
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