CN104211056B - A kind of preparation method of high strength graphite alkene film - Google Patents
A kind of preparation method of high strength graphite alkene film Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of high strength graphite alkene film, the method adopts the method for solution wet spinning, Graphene or graphene oxide dispersion are extruded in the preparation facilities of in-line die orifice, with Graphene or graphene oxide liquid crystal for template, be frozen into based on Graphene or graphene oxide gel film, after drying, obtain Graphene or graphene oxide membrane.The inventive method is easy, technique is simple, energy consumption is low, environmental protection, and the graphene film thickness obtained, size all can regulate, microstructure is regular, can be applied to many different fields.
Description
Technical field
The present invention relates to the preparation method of graphene film, particularly relate to a kind of preparation method of high strength graphite alkene film.
Background technology
2010, two professor AndreGeim and KonstantinNovoselov of Univ Manchester UK obtained Nobel Prize in physics because successfully isolate stable Graphene first, have started the upsurge that the whole world is studied Graphene.Graphene (Graphene) is a kind of unimolecular layer two dimensional crystal, have the highest intensity of known materials (Science, 2008,
321, 385-388) and the electroconductibility of excellence and thermal conductivity, be current optimal two-dimension nano materials.The graphene film of macroscopic view is one of main application form of nanoscale graphite alkene.But, the large-scale continuous preparation of the graphene film still not having implementation structure regular so far.
Graphene can be considered to the handkerchief polymer molecule of rigidity, the preparation method of reference polymer film can obtain graphene film.The preparation method of traditional polymer film mainly based on melt-processed blowing, extrude, roll, suppress, plastic uptake (vacuum forming), casting film-forming and rotation molding etc.Graphene has the fusing point of degree more than high molecular weight and 3,000, is not suitable for using melt-processed.Another kind of polymer film forming method be based on polymers soln casting film and coating film forming, be applicable to the prepolymer that some have very dystectic polymkeric substance or have crosslinking structure.These polymkeric substance of solution processing can only generally have the conjugate ring structure of very high molecular weight, crosslinking structure or rigidity, and graphene molecules also has quite similar character.Based on above similarity, by graphene solution prepare graphene film suction method, scrape the techniques such as embrane method, spin-coating method, spraying method and dip coating and achieve.But these methods are difficult to realize on a large scale, the preparation of the graphene film of compound with regular structure.Continuous production compound with regular structure, high performance graphene film remain a challenge.
For rigid macromolecule, high performance polymer filamentary material can be prepared continuously, such as: aramid fiber, cellulose acetate, triacetate, acrylic acid modified polyacrylonitrile, polybenzimidazole fibre, acrylic fibers, viscose fiber, spandex and vinyon fibre by the wet-spinning of macromolecular solution.There is bibliographical information by wet-spinning continuous production High-performance graphene fiber (Xu, Z.; Gao, C.,
nat.Commun. 2011, 2,571.).Concentration due to wet-spinning stoste is all generally that prepared fiber product has great contraction in diametric(al), and the contraction of fiber is conducive to the maintenance of fibrous texture and performance lower than 20%.Generally believe, the method of wet-spinning can not be used for producing polymeric film, because the structure of film is at in-plane and thickness direction very different, the polymeric film of wet-layer preparation causes the uncontrollable of final product structure and performance in the different meeting of different directions shrinking percentage, even cannot form membrane structure.Be subject to the restriction of lower concentration spinning solution, the final product of wet-spinning has very large contraction, only has and keeps the stable of product pattern in all directions, could obtain the film that structure properties is stable.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of wet preparation method of the film based on Graphene is provided.
The object of the invention is to be achieved through the following technical solutions: a kind of preparation method of high strength graphite alkene film, step is as follows:
(1) by the Graphene of 1 weight part, the solvent of 5 ~ 150 weight parts, obtains graphene dispersing solution after ultrasonic disperse;
(2) graphene dispersing solution step 1 obtained, extrudes in the preparation facilities of in-line die orifice with the extruded velocity of 10 ~ 1000mL/h, stops 1 ~ 100 second freezing film, obtain high strength graphite alkene film after drying in the solidification liquid of 10 ~ 80 DEG C.
The preparation facilities of the in-line die orifice in described step (1) is rectangular structure, and centre has an in-line die orifice narrowed gradually.
The solvent of described step (1) is primarily of water, N-Methyl pyrrolidone, acetone, methyl-sulphoxide, pyridine, dioxane, N, one or more in dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran (THF), butanone, ethylene glycol, glycol ether are according to any proportioning mixing composition.
The solidification liquid of described step (2) is the methanol solution of the sodium hydroxide of 5-10% primarily of massfraction, massfraction is the ethanolic soln of the sodium hydroxide of 5-10%, massfraction is the methanol solution of the potassium hydroxide of 5-8%, massfraction is the ethanolic soln of the potassium hydroxide of 5-8%, massfraction is the aqueous sodium hydroxide solution of 5-10%, massfraction is the aqueous sodium persulfate solution of 10-20%, massfraction is the sodium chloride aqueous solution of 10-20%, massfraction is the sodium nitrate aqueous solution of 5-10%, massfraction is the sodium phosphate aqueous solution of 5-10%, massfraction is the potassium chloride solution of 5-8%, massfraction is the aqueous ammonium chloride solution of 5-10%, massfraction is that one or more in the ammoniacal liquor of 5-15% are according to any proportioning mixing composition.
The method also can be made up of following steps:
(1) by the graphene oxide of 1 weight part, the solvent of 5 ~ 150 weight parts, obtains graphene oxide dispersion after ultrasonic disperse;
(2) by graphene oxide dispersion, extrude in the preparation facilities of in-line die orifice with the extruded velocity of 10 ~ 1000mL/h, in the solidification liquid of 10 ~ 80 DEG C, stop 1 ~ 100 second freezing film, after drying, obtain graphene oxide membrane;
(3) graphene oxide membrane that step (2) obtains reduced in reductive agent, washing drying obtains high strength graphite alkene film.
The preparation facilities of the in-line die orifice in described step (1) is rectangular structure, and centre has an in-line die orifice narrowed gradually.
The solvent of described step (1) is primarily of water, N-Methyl pyrrolidone, acetone, methyl-sulphoxide, pyridine, dioxane, N, one or more in dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran (THF), butanone, ethylene glycol, glycol ether are according to any proportioning mixing composition.
The solidification liquid of described step (2) is the methanol solution of the sodium hydroxide of 5-10% primarily of massfraction, massfraction is the ethanolic soln of the sodium hydroxide of 5-10%, massfraction is the methanol solution of the potassium hydroxide of 5-8%, massfraction is the ethanolic soln of the potassium hydroxide of 5-8%, massfraction is the aqueous sodium hydroxide solution of 5-10%, massfraction is the aqueous sodium persulfate solution of 10-20%, massfraction is the sodium chloride aqueous solution of 10-20%, massfraction is the sodium nitrate aqueous solution of 5-10%, massfraction is the sodium phosphate aqueous solution of 5-10%, massfraction is the potassium chloride solution of 5-8%, massfraction is the aqueous ammonium chloride solution of 5-10%, massfraction is that one or more in the ammoniacal liquor of 5-15% are according to any proportioning mixing composition.
Further, described reductive agent is selected from the hydrazine hydrate that massfraction is 1%-40%, massfraction is the sodium borohydride aqueous solution of 1%-40%, massfraction is the phenylhydrazine aqueous solution of 1%-40%, massfraction is the hydrobromic acid aqueous solution of 1%-40%, massfraction is the tea-polyphenol aqueous solution of 1%-40%, massfraction is the aqueous solution of urea of 1%-40%, massfraction is the sodium thiosulfate solution of 1%-20%, massfraction is the aqueous sodium hydroxide solution of 1%-5%, massfraction is the potassium hydroxide aqueous solution of 1%-40%, massfraction is the vitamins C aqueous solution of 5%-50%, massfraction is the D/W of 1%-40%, massfraction is the hydriodic acid aqueous solution of 1%-40%, massfraction is the aqueous acetic acid of 1%-40%, massfraction is the phenol solution of 1%-40%.
The beneficial effect that the present invention compared with prior art has is: apply high strength graphite alkene film that method of the present invention prepares and arrange accumulation by Graphene along in-plane and form, tensile strength is 20 ~ 300MPa, elongation at break is 0.3-20%, electric conductivity is greater than 10000S/m, and thermal conductivity is 10-2000W/mK.The method has following characteristics: the primary raw materials of (1) Graphene or graphene oxide is graphite, raw material sources extensively, be easy to get, with low cost; (2) method adopting solution to spin has prepared graphene film, operates fast and convenient, environmental protection, can large-scale continuously prepare; (3) thickness and the width of graphene film can be controlled; (4) obtained graphene film has good intensity and toughness, has excellent heat conductance and electroconductibility simultaneously.
Accompanying drawing explanation
Fig. 1 is the sectional view of the preparation facilities of in-line die orifice;
Fig. 2 is the front view of the preparation facilities of in-line die orifice;
Fig. 3 is the rear view of the preparation facilities of in-line die orifice;
Fig. 4 is the electron scanning micrograph of graphene film Tensile fracture.
Embodiment
As Figure 1-3, the preparation facilities of in-line die orifice of the present invention is rectangular structure, and centre has in-line die orifice, and described in-line die orifice is a runner narrowed gradually.The runner narrowed gradually effectively can increase the reactive force of flow field to graphene film, is conducive to the formation of the regular oriented structure of graphene dispersion system.
Below in conjunction with embodiment, the present invention is described specifically; the present embodiment is only for the present invention is described further; limiting the scope of the invention can not be interpreted as; those skilled in the art makes some nonessential change and adjustment according to the content of foregoing invention, all belongs to protection scope of the present invention.
embodiment 1:
(1) by 1g graphene oxide and the mixing of 5g deionized water, in 20 DEG C with the supersound process 10 hours of 50KHz, graphene oxide dispersion is obtained.
(2) by graphene oxide dispersion, extrude in the preparation facilities of in-line die orifice with the extruded velocity of 200mL/h, in the methanol solution (massfraction is 10%) of the sodium hydroxide of 80 DEG C, stop 1 second freezing film, after drying, obtain graphene oxide membrane.
(3) graphene oxide membrane step (2) obtained is fully reduce in 20% D/W at massfraction, and washing drying obtains high strength graphite alkene film.
As shown in Figure 4, through above step, the graphene film thickness of preparation is 1 micron and has good stratiform orientation arrangement structure; Tensile strength is 260MPa, and elongation at break is 0.68%.Electric conductivity is greater than 10000S/m, and thermal conductivity is 700W/mK, has good toughness simultaneously.
embodiment 2:
(1) by 1g graphene oxide, 50g tetrahydrofuran (THF), the mixing of 100g methyl-sulphoxide, in 20 DEG C with the supersound process 1 hour of 50KHz, graphene oxide dispersion is obtained.
(2) by graphene oxide dispersion, extrude in the preparation facilities of in-line die orifice with the extruded velocity of 100mL/h, in the ethanolic soln (massfraction of sodium hydroxide and potassium hydroxide is 2.5%) of the sodium hydroxide of 10 DEG C and potassium hydroxide, stop 100 seconds freezing films, after drying, obtain graphene oxide membrane.
(3) graphene oxide membrane step (2) obtained is fully reduce in the hydroiodic acid HI of 20% at massfraction, and washing drying obtains high strength graphite alkene film.
Through above step, the graphene film thickness of preparation is 1 millimeter, and tensile strength is 210MPa, and elongation at break is 1.1%, and electric conductivity is greater than 10000S/m, and thermal conductivity is 680W/mK, has good toughness simultaneously.
embodiment 3:
(1) acetone of the DMF of 1g graphene oxide, 25g, 25g is mixed, the butanone of 50g, in 20 DEG C with the supersound process 1 hour of 50KHz, obtain graphene oxide dispersion.
(2) by graphene oxide dispersion, extrude in the preparation facilities of in-line die orifice with the extruded velocity of 10mL/h, in the Alkitrates of 40 DEG C (massfraction is 10%), stop 60 seconds freezing films, after drying, obtain graphene oxide membrane.
(3) graphene oxide membrane step (2) obtained is fully reduce in the hydroiodic acid HI of 20% at massfraction, and washing drying obtains high strength graphite alkene film.
Through above step, the graphene film thickness of preparation is 30 microns, and tensile strength is 230MPa, and elongation at break is 1.6%, and electric conductivity is greater than 10000S/m, and thermal conductivity is 600W/mK, has good toughness simultaneously.
embodiment 4:
(1) by the N-Methyl pyrrolidone of 2g Graphene and 100g, in 20 DEG C with the supersound process 2 hours of 50KHz, graphene dispersing solution is obtained.
(2) by graphene dispersing solution, extrude in the preparation facilities of in-line die orifice with the extruded velocity of 500mL/h, in the aqueous solution (massfraction of sodium sulfate and Repone K is 10%) of the sodium sulfate of 20 DEG C and Repone K, stop 20 seconds freezing films, after drying, obtain graphene film.
Through above step, the graphene film thickness of preparation is 8 microns, and tensile strength is 280MPa, and elongation at break is 1.5%, and electric conductivity is greater than 10000S/m, and thermal conductivity is 1200W/mK, has good toughness simultaneously.
embodiment 5:
(1) N-Methyl pyrrolidone of 2g Graphene and 40g, in 20 DEG C with the supersound process 2 hours of 50KHz, obtains graphene dispersing solution.
(2) by graphene dispersing solution, extrude in the preparation facilities of in-line die orifice with the extruded velocity of 1000mL/h, in the methanol solution (massfraction of sodium hydroxide and potassium hydroxide is 5%) of the sodium hydroxide of 60 DEG C and potassium hydroxide, stop 20 seconds freezing films, after drying, obtain graphene film.
Through above step, the graphene film thickness of preparation is 8 microns, and tensile strength is 280MPa, and elongation at break is 1.5%, and electric conductivity is greater than 10000S/m, and thermal conductivity is 1200W/mK, has good toughness simultaneously.
embodiment 6:
(1) glycol ether of 2g Graphene, 20g, the N,N-dimethylacetamide of 40g, in 20 DEG C with the supersound process 2 hours of 50KHz, obtains graphene dispersing solution.
(2) by graphene dispersing solution, extrude in the preparation facilities of in-line die orifice with the extruded velocity of 800mL/h, in the ammoniacal liquor of 80 DEG C (massfraction is 5%), stop 20 seconds freezing films, after drying, obtain graphene film.
Through above step, the graphene film thickness of preparation is 20 microns, and tensile strength is 320MPa, and elongation at break is 1.1%, and electric conductivity is greater than 10000S/m, and thermal conductivity is 1500W/mK, has good toughness simultaneously.
Above-described embodiment is used for explaining and the present invention is described, instead of limits the invention, and in the protection domain of spirit of the present invention and claim, any amendment make the present invention and change, all fall into protection scope of the present invention.
Claims (3)
1. a preparation method for high strength graphite alkene film, is characterized in that, comprises the steps:
(1) by the Graphene of 1 weight part, the solvent of 5 ~ 150 weight parts, obtains graphene dispersing solution after ultrasonic disperse;
(2) by the graphene dispersing solution that step (1) obtains, extrude in the preparation facilities of in-line die orifice with the extruded velocity of 10 ~ 1000mL/h, stop 1 ~ 100 second in the solidification liquid of 10 ~ 80 DEG C, freezing film, obtains high strength graphite alkene film after drying;
The preparation facilities of the in-line die orifice in described step (2) is rectangular structure, and centre has an in-line die orifice narrowed gradually;
The solvent of described step (1) is primarily of water, N-Methyl pyrrolidone, acetone, methyl-sulphoxide, pyridine, dioxane, N, one or more in dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran (THF), butanone, ethylene glycol, glycol ether are according to any proportioning mixing composition;
The solidification liquid of described step (2) is the methanol solution of the sodium hydroxide of 5-10% primarily of massfraction, massfraction is the ethanolic soln of the sodium hydroxide of 5-10%, massfraction is the methanol solution of the potassium hydroxide of 5-8%, massfraction is the ethanolic soln of the potassium hydroxide of 5-8%, massfraction is the aqueous sodium hydroxide solution of 5-10%, massfraction is the aqueous sodium persulfate solution of 10-20%, massfraction is the sodium chloride aqueous solution of 10-20%, massfraction is the sodium nitrate aqueous solution of 5-10%, massfraction is the sodium phosphate aqueous solution of 5-10%, massfraction is the potassium chloride solution of 5-8%, massfraction is the aqueous ammonium chloride solution of 5-10%, massfraction is that one or more in the ammoniacal liquor of 5-15% are according to any proportioning mixing composition.
2. a preparation method for high strength graphite alkene film, is characterized in that, step is as follows:
(1) by the graphene oxide of 1 weight part, the solvent of 5 ~ 150 weight parts, obtains graphene oxide dispersion after ultrasonic disperse;
(2) by graphene oxide dispersion prepared by step (1), extrude in the preparation facilities of in-line die orifice with the extruded velocity of 10 ~ 1000mL/h, in the solidification liquid of 10 ~ 80 DEG C, stop 1 ~ 100 second freezing film, after drying, obtain graphene oxide membrane;
(3) graphene oxide membrane that step (2) obtains is reduced in reductive agent, after washing drying, obtain high strength graphite alkene film;
The preparation facilities of the in-line die orifice in described step (2) is rectangular structure, and centre has an in-line die orifice narrowed gradually;
The solvent of described step (1) is primarily of water, N-Methyl pyrrolidone, acetone, methyl-sulphoxide, pyridine, dioxane, N, one or more in dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran (THF), butanone, ethylene glycol, glycol ether are according to any proportioning mixing composition;
The solidification liquid of described step (2) is the methanol solution of the sodium hydroxide of 5-10% primarily of massfraction, massfraction is the ethanolic soln of the sodium hydroxide of 5-10%, massfraction is the methanol solution of the potassium hydroxide of 5-8%, massfraction is the ethanolic soln of the potassium hydroxide of 5-8%, massfraction is the aqueous sodium hydroxide solution of 5-10%, massfraction is the aqueous sodium persulfate solution of 10-20%, massfraction is the sodium chloride aqueous solution of 10-20%, massfraction is the sodium nitrate aqueous solution of 5-10%, massfraction is the sodium phosphate aqueous solution of 5-10%, massfraction is the potassium chloride solution of 5-8%, massfraction is the aqueous ammonium chloride solution of 5-10%, massfraction is that one or more in the ammoniacal liquor of 5-15% are according to any proportioning mixing composition.
3. the preparation method of a kind of high strength graphite alkene film according to claim 2, it is characterized in that, described reductive agent is selected from the hydrazine hydrate that massfraction is 1%-40%, massfraction is the sodium borohydride aqueous solution of 1%-40%, massfraction is the phenylhydrazine aqueous solution of 1%-40%, massfraction is the hydrobromic acid aqueous solution of 1%-40%, massfraction is the tea-polyphenol aqueous solution of 1%-40%, massfraction is the aqueous solution of urea of 1%-40%, massfraction is the sodium thiosulfate solution of 1%-20%, massfraction is the aqueous sodium hydroxide solution of 1%-5%, massfraction is the potassium hydroxide aqueous solution of 1%-40%, massfraction is the vitamins C aqueous solution of 5%-50%, massfraction is the D/W of 1%-40%, massfraction is the hydriodic acid aqueous solution of 1%-40%, massfraction is the aqueous acetic acid of 1%-40%, massfraction is the phenol solution of 1%-40%.
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| PCT/CN2015/070510 WO2016037456A1 (en) | 2014-09-10 | 2015-01-12 | Method for preparing graphene and composite film thereof based on i-shaped die |
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| WO2016037456A1 (en) * | 2014-09-10 | 2016-03-17 | 浙江碳谷上希材料科技有限公司 | Method for preparing graphene and composite film thereof based on i-shaped die |
| CN105271209A (en) * | 2015-11-05 | 2016-01-27 | 北京旭碳新材料科技有限公司 | Graphene film and method and device for continuously producing graphene film |
| CN105732038A (en) * | 2016-01-15 | 2016-07-06 | 东南大学 | Highly conductive flexible self-supported graphene film and preparation method thereof |
| CN105741980B (en) * | 2016-04-01 | 2018-01-16 | 东南大学 | A kind of surface has flexible self-supporting graphene conductive film of micro structured pattern and preparation method thereof |
| CN106384769B (en) * | 2016-11-23 | 2019-12-10 | Tcl集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
| CN108249432A (en) * | 2016-12-28 | 2018-07-06 | 海门市源美美术图案设计有限公司 | A kind of dextran modification graphene oxide composite material and its application |
| CN112125297A (en) * | 2020-09-22 | 2020-12-25 | 杭州高烯科技有限公司 | Preparation method of graphene film |
| CN112938957A (en) * | 2021-04-14 | 2021-06-11 | 新乡医学院 | Graphene oxide paper and preparation method thereof |
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| CN102534865A (en) * | 2012-01-05 | 2012-07-04 | 浙江大学 | Ion-enhanced graphene fiber and preparation method thereof |
| CN203510676U (en) * | 2013-08-20 | 2014-04-02 | 上海工程技术大学 | Mold for extruding film |
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