CN104211055B - A kind of preparation method of Graphene metallic nanoparticle composite membrane - Google Patents
A kind of preparation method of Graphene metallic nanoparticle composite membrane Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of Graphene metallic nanoparticle composite membrane, the method adopts the method for solution wet spinning, Graphene or graphene oxide metal nanoparticle mixed dispersion liquid 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 metallic nanoparticle composite membrane, after dry reduction, obtain Graphene/metallic nanoparticle composite membrane.The present invention has simple, convenient, the efficient feature of technique, the Graphene that can prepare/metallic nanoparticle composite membrane kind is many, the Graphene obtained/metallic nanoparticle composite membrane size can regulate, and effectively can improve the electroconductibility of composite membrane and be applied to many different industrial circles.
Description
Technical field
The present invention relates to a kind of continuous production method of composite membrane, particularly relate to a kind of preparation method of Graphene metallic nanoparticle composite membrane.
Background technology
Graphene is with the two-dimentional monoatomic layer crystal of hexagon bonding by carbon atom, based on its chemical structure, Graphene has many physicochemical property exceeding the excellence of traditional material, as high in high-specific surface area, high conductivity, physical strength, be easy to modify and scale operation etc.From AndreGeim and KonstantinNovoselov of Univ Manchester UK in 2010 because successfully isolated since stable Graphene obtains Nobel Prize in physics first, the whole world has started the upsurge of research Graphene.Nanoparticle refer to nanostructure be at least one dimension size at the fine particle in 1 ~ 100nm region, because the surface atom of nanoparticle sharply increases with the minimizing of grain size with the ratio of body phase total atom number, it is made to demonstrate strong volume effect, quantum effect, surface effects and macro quanta tunnel effect.Metal nanoparticle, because its excellent performance and receiving with the special performance that other materials compound tense shows is paid close attention to widely, has broad application prospects in catalyzer, electromagnetic functional material, absorbing material, sensing element material, nano composite material.Graphene is nano level in the dimension of thickness, with nanoparticle in same size range.If by Graphene and metal nanoparticle compound, Graphene metal nanoparticle macrocomposite can be constructed, will make full use of and play the advantage of the two, realize high performance and the multifunction of material, and the material designability on higher level.By with different metal Nanocomposites, the composite membrane of difference in functionality can be obtained, metallic nanoparticle composite membrane based on Graphene has following advantage: (1) Graphene and metal nanoparticle excellent performance, and chemical stability is good, can prepare in enormous quantities; (2) by selecting kind and the proportion adjustment graphene composite film performance of metal nanoparticle; (3) membrane material characteristic Graphene and metal nanoparticle compound obtained is by far beyond traditional mould material.
The conventional method preparing graphene nano particle composite membrane is mechanical blending method, solution blended process, in-situ synthesized, layer assembly method etc.But the graphene nano particle composite material preparation method complex process of existing report, the composite structure poor controllability of acquisition, time consumption and energy consumption, be difficult to the large-scale continuous preparation of the regular Graphene metal nano particle composite material of implementation structure.The controlled Graphene metal nano particle composite material of continuous production compound with regular structure, size remains a challenge.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of Graphene metallic nanoparticle composite membrane is provided.
The object of the invention is to be achieved through the following technical solutions: a kind of preparation method of Graphene metallic nanoparticle composite membrane, is characterized in that its step is as follows:
(1) by the Graphene of 1 weight part, the metal nanoparticle of 0.01 ~ 2 weight part, the solvent of 5 ~ 150 weight parts, obtains the mixed dispersion liquid of Graphene/metal nanoparticle after ultrasonic disperse;
(2) mixed dispersion liquid of Graphene/metal nanoparticle step 1 obtained, extrude in the preparation facilities of in-line die orifice with the speed of 1 ~ 100mL/h, in the solidification liquid of 10 ~ 80 DEG C, stop 1 ~ 100s freezing film after extruding, obtain Graphene metallic nanoparticle composite membrane.
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.
Metal nanoparticle in described step (1) is selected from the nanoparticle of gold and silver, aluminium, copper, iron, zinc, chromium, nickel, cobalt, platinum, palladium, iridium, rhodium, ruthenium, titanium, vanadium, magnesium, indium, lanthanum, indium, antimony.
The solvent of described step (1) is by water, methyl alcohol, ethanol, 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 pressed arbitrarily than 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 calcium chloride water of 10-20%, massfraction is the sodium nitrate aqueous solution of 5-10%, massfraction is the calcium 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 arbitrarily than forming.
The method also can be realized by following steps:
(1) by the graphene oxide of 1 weight part, the metal nanoparticle of 0.01 ~ 2 weight part, the solvent of 5 ~ 150 weight parts, obtains the mixed dispersion liquid of graphene oxide/metal nanoparticle after ultrasonic disperse;
(2) mixed dispersion liquid of graphene oxide/metal nanoparticle step 1 obtained, extruding in the preparation facilities of in-line die orifice with 1 ~ 100mL/h, in the solidification liquid of 10 ~ 80 DEG C, stop 1 ~ 100s freezing film after extruding, obtain graphene oxide/metallic nanoparticle composite membrane;
(3) graphene oxide/metallic nanoparticle composite membrane that step (2) obtains is reduced in reductive agent, after washing is dry, obtain Graphene metallic nanoparticle composite membrane.
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.
Metal nanoparticle in described step (1) is selected from the nanoparticle of gold and silver, aluminium, copper, iron, zinc, chromium, nickel, cobalt, platinum, palladium, iridium, rhodium, ruthenium, titanium, vanadium, magnesium, indium, lanthanum, indium, antimony.
The solvent of described step (1) is by water, methyl alcohol, ethanol, 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 pressed arbitrarily than 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 calcium chloride water of 10-20%, massfraction is the sodium nitrate aqueous solution of 5-10%, massfraction is the calcium 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 arbitrarily than forming.
It is the hydrazine hydrate of 1%-40% that reductive agent described in step (3) is selected from by massfraction, 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: the Graphene metallic nanoparticle composite membrane prepared is made up of the Graphene arranged along in-plane and the equally distributed metal nanoparticle of graphene film interlayer, according to metal nano particle-doped difference, show different functions; When metal nanoparticle is Fe nanometer particles, composite membrane shows paramagnetism, can be used for magnetic response conductor and Magnetic Sensor; When metal nanoparticle is golden nanometer particle, the electroconductibility of film effectively can be improved; When metal nanoparticle is the nano grain of silver period of the day from 11 p.m. to 1 a.m, the heat conductance of film effectively can be improved.
This preparation method has the following advantages: 1) primary raw materials of Graphene or graphene oxide is graphite, a large amount of mature preparation process of metal nanoparticle, raw material sources extensively, be easy to get, with low cost; 2) method adopting solution to spin has prepared Graphene metallic nanoparticle composite membrane, operates fast and convenient, environmental protection, can prepare on a large scale; 3) ratio of Graphene and metal nanoparticle and the thickness of Graphene metallic nanoparticle composite membrane and width can be controlled.
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: the electron scanning micrograph of Graphene/Fe nanometer particles film section and plane;
Fig. 5: the current-voltage curve of Graphene/silver nanoparticle film.
Embodiment
As Figure 1-3, the preparation facilities of in-line die orifice 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 the graphene oxide of 1 weight part, the golden nanometer particle of 0.01 weight part, the ethanol of 2 weight parts, the ethylene glycol mixing of 3 weight parts, obtain the mixed dispersion liquid of graphene oxide/golden nanometer particle after ultrasonic disperse;
(2) mixed dispersion liquid step 1 obtained, extrude in the preparation facilities of in-line die orifice with the speed of 1mL/h, in the ethanolic soln (massfraction is 10%) of the sodium hydroxide of 80 DEG C, stop 1s freezing film after extruding, obtain graphene oxide/golden nanometer particle composite membrane;
(3) graphene oxide golden nanometer particle composite membrane step (2) obtained is reduce in 20% hydrazine hydrate solution at massfraction, obtains Graphene/golden nanometer particle composite membrane after washing drying.
Through above step, preparing width is 50 millimeters, thickness is the Graphene/golden nanometer particle composite membrane of 1 micron, and this composite membrane can as the stationary phase of golden nanometer particle, is used for the assembling of control molecule, molecular recognition template, catalysis biological chemical reaction or as application such as biosensors.
embodiment 2:
(1) by the Graphene of 1 weight part, the Fe nanometer particles of 2 weight parts, the water of 150 weight parts mixes, and obtains Graphene/Fe nanometer particles mixed dispersion liquid after ultrasonic disperse.
(2) by Graphene/Fe nanometer particles mixed dispersion liquid, extrude in the preparation facilities of in-line die orifice with the speed of 30mL/h, in the methanol solution (massfraction of sodium hydroxide and potassium hydroxide is 2.5%) of the sodium hydroxide of 10 DEG C and potassium hydroxide, stop 100s freezing film after extruding, after drying, obtain Graphene/Fe nanometer particles composite membrane.
Through above step, preparing width is 20 millimeters, and thickness is the graphene oxide/Fe nanometer particles composite membrane of 50 microns.As shown in Figure 4, Fe nanometer particles is evenly distributed on graphenic surface, and Fe nanometer particles and Graphene are piled up layer by layer.Prepared Graphene/Fe nanometer particles composite membrane has good paramagnetism, can be applied to the switch of magnetic control and wire and magnetic transducing field.
embodiment 3:
(1) by the graphene oxide of 1 weight part, the Nano silver grain of 2 weight parts, the methyl-sulphoxide mixing of 150 weight parts, obtains the mixed dispersion liquid of graphene oxide/Nano silver grain after ultrasonic disperse;
(2) mixed dispersion liquid step 1 obtained, extrude in the preparation facilities of in-line die orifice with the speed of 1mL/h, in the methanol solution (massfraction is 6%) of the potassium hydroxide of 50 DEG C, stop 100s freezing film after extruding, after drying, obtain graphene oxide/Nano silver grain composite membrane;
(3) graphene oxide composite membrane step (2) obtained is reduce in the tea-polyphenol aqueous solution of 40% at massfraction, obtains Graphene/Nano silver grain composite membrane after washing drying.
Through above step, preparing width is 50 millimeters, thickness is the Graphene/Nano silver grain composite membrane of 50 microns, as shown in Figure 5, this graphene composite film has very high electroconductibility, compared with there is no the specific conductivity of compound silver nanometer particle graphene film (8500S/m), Graphene/Nano silver grain nanoparticle composite membrane there is better electroconductibility, reach 25000S/m, alternative metals can be used as electro-conductive material.
embodiment 4:
(1) by the Graphene of 1 weight part, the nano platinum particle of 0.1 weight part, the N-Methyl pyrrolidone mixing of 20 weight parts, obtains graphene/platinum nano mix particles dispersion liquid after ultrasonic disperse.
(2) by graphene/platinum nano mix particles dispersion liquid, with 100mL/h speed extrude in the preparation facilities of in-line die orifice, in the ethanolic soln (massfraction is 8%) of the potassium hydroxide of 60 DEG C, stop 100s freezing film after extruding, after drying, obtain graphene/platinum nano particle composite membrane.
Through above step, preparing width is 200 millimeters, thickness is the graphene/platinum nano particle composite membrane of 200 microns, and this graphene composite film can be used as the effective catalyst of organic molecule and catalystic hydrogenation of coal tar, and temperature and the catalysis that effectively can reduce catalyzed reaction improve speed of reaction.
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 Graphene metallic nanoparticle composite membrane, is characterized in that, the method step is as follows:
(1) by the Graphene of 1 weight part, the metal nanoparticle of 0.01 ~ 2 weight part, the solvent of 5 ~ 150 weight parts, obtains the mixed dispersion liquid of Graphene/metal nanoparticle after ultrasonic disperse;
(2) mixed dispersion liquid of Graphene/metal nanoparticle step (1) obtained, extrude in the preparation facilities of in-line die orifice with the speed of 1 ~ 100mL/h, in the solidification liquid of 10 ~ 80 DEG C, stop 1 ~ 100s freezing film after extruding, obtain Graphene metallic nanoparticle composite membrane;
The preparation facilities of the in-line die orifice in described step (2) is rectangular structure, and centre has in-line die orifice, and described in-line die orifice is a runner narrowed gradually;
Metal nanoparticle in described step (1) is selected from the nanoparticle of gold and silver, aluminium, copper, iron, zinc, chromium, nickel, cobalt, platinum, palladium, iridium, rhodium, ruthenium, titanium, vanadium, magnesium, indium, lanthanum, indium, antimony;
The solvent of described step (1) is by water, methyl alcohol, ethanol, 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 pressed arbitrarily than 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 calcium chloride water of 10-20%, massfraction is the sodium nitrate aqueous solution of 5-10%, massfraction is the calcium 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 arbitrarily than forming.
2. a preparation method for Graphene metallic nanoparticle composite membrane, is characterized in that, its step is as follows:
(1) by the graphene oxide of 1 weight part, the metal nanoparticle of 0.01 ~ 2 weight part, the solvent of 5 ~ 150 weight parts, obtains the mixed dispersion liquid of graphene oxide/metal nanoparticle after ultrasonic disperse;
(2) mixed dispersion liquid of graphene oxide/metal nanoparticle step (1) obtained, extruding in the preparation facilities of in-line die orifice with 1 ~ 100mL/h, in the solidification liquid of 10 ~ 80 DEG C, stop 1 ~ 100s freezing film after extruding, obtain graphene oxide/metallic nanoparticle composite membrane;
(3) graphene oxide/metallic nanoparticle composite membrane that step (2) obtains is reduced in reductive agent, after washing is dry, obtain Graphene metallic nanoparticle composite membrane;
The preparation facilities of the in-line die orifice in described step (2) is rectangular structure, and centre has in-line die orifice, and described in-line die orifice is a runner narrowed gradually;
Metal nanoparticle in described step (1) is selected from the nanoparticle of gold and silver, aluminium, copper, iron, zinc, chromium, nickel, cobalt, platinum, palladium, iridium, rhodium, ruthenium, titanium, vanadium, magnesium, indium, lanthanum, indium, antimony;
The solvent of described step (1) is by water, methyl alcohol, ethanol, 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 pressed arbitrarily than 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 calcium chloride water of 10-20%, massfraction is the sodium nitrate aqueous solution of 5-10%, massfraction is the calcium 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 arbitrarily than forming.
3. the preparation method of a kind of Graphene metallic nanoparticle composite membrane 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 |
| CN104841427A (en) * | 2015-04-24 | 2015-08-19 | 中国石油大学(北京) | GO/CNT-Au composite catalyst, preparation and application thereof |
| CN105375061B (en) * | 2015-12-09 | 2018-09-18 | 宋宏婷 | A kind of Graphene electrodes |
| CN108031837B (en) * | 2017-11-23 | 2019-10-25 | 西安理工大学 | A method of preparing chromium plating graphene/copper composite powder |
| CN108862247B (en) * | 2018-07-10 | 2020-06-19 | 杭州高烯科技有限公司 | Gas molecule detection composite membrane |
| CN110842190B (en) * | 2019-10-11 | 2021-10-15 | 云南大学 | Preparation method of silver-coated copper powder |
| CN114249318A (en) * | 2021-12-29 | 2022-03-29 | 杭州嘉悦智能设备有限公司 | Nitrogen-doped graphene-precious metal composite membrane and preparation method thereof |
| CN114348997A (en) * | 2021-12-29 | 2022-04-15 | 杭州嘉悦智能设备有限公司 | Nitrogen-doped graphene-metal nanoparticle film and preparation method thereof |
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