CN102817111A - Preparation method and product of one-dimensional macroscopic graphene fibers - Google Patents
Preparation method and product of one-dimensional macroscopic graphene fibers Download PDFInfo
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Abstract
The invention discloses a preparation method of one-dimensional macroscopic graphene fibers. The preparation method comprises the following steps of: firstly, providing oxidized graphene dispersion liquid; then, adding the oxidized graphene dispersion liquid in a cetyltrimethylammonium bromide aqueous solution as coagulating bath to obtain oxidized graphene fibers; and finally, reducing and drying the oxidized graphene fibers to obtain the graphene fibers. The continuous, super-long and soft graphene fibers, which are prepared by the simple technology, have the good properties of high mechanical strength, excellent electrical conductivity and ease of processing, thus having a good application prospect.
Description
Technical field
The present invention relates to field of nanometer technology, specifically, the present invention relates to Graphene fiber preparation method and products thereof.
Background technology
Graphene is as the most basic construction unit of all material with carbon elements; Have real monatomic thickness and strict two-dimensional structure; This just structural specificity makes it have excellent physicochemical properties, like quantum hall effect, high-specific surface area, high conductivity, high mechanical properties, high carrier mobility and high light transmittance matter etc.Since Britain scientist An Delie Jim in 2004 and Ke Siteyanuowosailuo find Graphene, increasing discovering, there is great application prospect in it in fields such as energy storage device, photovoltaic device, sensor and catalysis.
In order further to develop the excellent properties of two-dimentional graphene film, consider from the practical application angle, graphene film is transferred to a beyond doubt individual interesting and valuable research direction in the macroscopic material.A large amount of research has been arranged to macroscopical graphene-based material, comprised three-dimensional complex and the Graphene aquogel bulk of graphene film, Graphene and polymer etc.But because graphene film dispersed limited in most usual vehicles, this has just limited Graphene is assembled the bulk direction to one dimension from nanometer sheet development.And graphene oxide is from structure, and at its two dimensional surface and a large amount of oxy radical of marginal existence, like hydroxyl, carboxyl and epoxy radicals etc., this forms sol dispersion with regard to making it in water and other polar solvent, can be peeled off fully.Thereby this graphene oxide has just become to prepare the attractive raw material candidate of macroscopical Graphene fiber.For the current situation of macroscopical carbon-based material fiber production, both at home and abroad scientist has utilized wet spinning and dry state spining technology that single wall and multi-walled carbon nano-tubes are assembled into macroscopic fibres (Britain's " nature " (Nature, 801 pages of 2002 419 phases; 703 pages of 2003 423 phases); U.S.'s " science " (Science, 276 pages of 2004 304 phases; 1447 pages of 2004 305 phases).Yet, in the process of preparation carbon nano-tube macroscopic fiber, have some drawbacks that can not be ignored, such as the price of the costliness of the carbon pipe of highly arranging and when preparing these fibers, used like superhigh temperature or highly corrosive solvent etc.Therefore, the shortcoming when when obtaining excellent properties, not having the assembling of carbon pipe is badly in need of that exploitation is a kind of effectively, easy operating and prepare the technical method of macroscopical Graphene fiber fast, for the application of macroscopical grapheme material lays the foundation.
Summary of the invention
The present invention provides a kind of one dimension macroscopic view Graphene fiber preparation method to present technical deficiency.
For this reason, the present invention provides a kind of one dimension macroscopic view Graphene fiber preparation method, it is characterized in that, may further comprise the steps:
A., the graphene oxide dispersion liquid is provided;
B. with said graphene oxide dispersion liquid join as in the softex kw aqueous solution of coagulating bath to obtain the graphene oxide fiber; And
C. said graphene oxide fiber through reduction with, obtain said one dimension macroscopic view Graphene fiber.
In a preferred implementation, said graphene oxide dispersion liquid provides through following steps:
A1. the mixture with Graphene scale and nitrate such as sodium nitrate joins in the strong acid such as the concentrated sulfuric acid, carries out pre-oxidation, stirs to obtain dispersion liquid;
A2. in the said dispersion liquid of a1, add strong oxidizer such as potassium permanganate, stir, placed 1-10 days, obtain the taupe pastel;
A3. in the said taupe pastel of a2, add deionized water and hydrogen peroxide solution successively, obtain glassy yellow suspension;
A4. the said glassy yellow suspension of a3 is centrifugal, the washing and the dialysis, obtain said graphene oxide dispersion liquid.
In a preferred implementation, the concentration of the graphene oxide solution that uses among the said step b is 5～20mg/mL.
In a preferred implementation, the concentration of the softex kw aqueous solution that uses among the said step b is 0.1-5mg/mL.
In a preferred implementation, in said step c, use hydroiodic acid or the said graphene oxide fiber of hydrazine hydrate reduction.
In a preferred implementation, in said step c, use hydroiodic acid as reductant and reaction 2-12 hour.
In a preferred implementation, in said step c, using hydroiodic acid is 50～80 ℃ as reductant and reaction temperature.
In a preferred implementation, after said step c, after said one dimension macroscopic view Graphene fiber taken out and clean with deionized water, drying at room temperature and obtain said one dimension macroscopic view Graphene fiber.
In a preferred implementation, in said step b, said graphene oxide dispersion liquid is injected in the said softex kw aqueous solution through syringe.
In a preferred implementation, the syringe needle diameter of said syringe is 0.10～1.0mm.
In addition, the present invention provides a kind of one dimension macroscopic view Graphene fiber that obtains through above-mentioned preparation method.
One dimension provided by the invention macroscopic view Graphene fiber preparation method step is simple, operate simple and easyly, has economy, characteristics fast, and the Graphene fiber for preparing has the advantage that overlength, softness, mechanical performance are high, conduct electricity very well and be prone to process.
Description of drawings
Fig. 1 is the optical photograph according to the one dimension macroscopic view Graphene fiber of embodiments of the invention 1 acquisition;
Fig. 2 is the electron scanning micrograph according to the one dimension macroscopic view Graphene fiber of the embodiment of the invention 1 acquisition;
Fig. 3 is the electron scanning micrograph according to the cross section structure of the one dimension macroscopic view Graphene fiber of the embodiment of the invention 1 acquisition;
Fig. 4 is the electron scanning micrograph according to the surface texture of the one dimension macroscopic view Graphene fiber of the embodiment of the invention 1 acquisition;
Fig. 5 is the electron scanning micrograph according to the one dimension macroscopic view Graphene fiber of the embodiment of the invention 2 acquisitions;
Fig. 6 is the electron scanning micrograph according to the one dimension macroscopic view Graphene fiber of the embodiment of the invention 5 acquisitions;
Fig. 7 is the electron scanning micrograph according to the one dimension macroscopic view Graphene fiber of the embodiment of the invention 7 acquisitions;
Fig. 8 is the stretching-strain curve according to the single one dimension macroscopic view Graphene fiber of the embodiment of the invention 1 acquisition; With
Fig. 9 is current-voltage (I-V) curve according to the single one dimension macroscopic view Graphene fiber of the embodiment of the invention 1 acquisition.
The specific embodiment
The present invention provides a kind of macroscopical Graphene fiber preparation method; A kind of graphene oxide dispersion liquid at first is provided; Then this graphene oxide dispersion liquid is joined in the softex kw aqueous solution as coagulating bath, obtains the graphene oxide fiber, at last with the graphene oxide fiber through reductant for example after hydroiodic acid or the hydrazine hydrate electronation; Washing, drying obtain one dimension macroscopic view Graphene fiber.
More preferably, one dimension macroscopic view Graphene fiber preparation method of the present invention may further comprise the steps:
A. prepare a kind of graphene oxide dispersion liquid;
B. the dispersion liquid of graphene oxide is for example packed in the syringe, be injected into then as in the softex kw aqueous solution of coagulating bath and obtain the graphene oxide fiber;
C. the graphene oxide fiber for example obtains the Graphene fiber behind hydroiodic acid or the hydrazine hydrate reduction through reductant.
In a preferred implementation, above-mentioned steps a can may further comprise the steps:
A1. the mixture with Graphene scale and nitrate such as sodium nitrate joins in strong acid such as the concentrated sulfuric acid or the red fuming nitric acid (RFNA), carries out pre-oxidation, stirs to obtain dispersion liquid;
A2. in the said dispersion liquid of a1, add strong oxidizer such as potassium permanganate, stir, placed 1-10 days, be preferably 5 days, obtain the taupe pastel;
A3. in the said taupe pastel of a2, add deionized water and hydrogen peroxide solution successively, obtain glassy yellow suspension;
A4. the said glassy yellow suspension of a3 is for example repeatedly centrifugal, the washing and the dialysis after, obtain said graphene oxide dispersion liquid.
Preferably, the concentration of stating the graphene oxide dispersion liquid that uses among the step b is 5～20mg/mL.
The concentration of the softex kw aqueous solution that preferably, uses among the above-mentioned steps b is 0.1-5mg/mL.
Preferably, among the above-mentioned steps c, the graphene oxide fiber reacted 2-12 hour in reductant such as hydroiodic acid, was preferably 8 hours.
Preferably, the reaction temperature of graphene oxide fiber in reductant such as hydroiodic acid is 50～90 ℃ among the above-mentioned steps c, is preferably 80 ℃.
Preferably, the graphene oxide fiber takes out through the reduction back among the above-mentioned steps c, cleans with deionized water, makes the Graphene fiber after the drying at room temperature.
The invention has the advantages that and utilize simple operations that prepare the Graphene fiber of overlength, softness continuously, in large quantities, it has high mechanical properties, high conduction performance and is easy to machining characteristics, has a good application prospect.
Below in conjunction with embodiment, specific embodiments of the invention is done and is described in further detail.Following examples are in order to further specify the present invention, but are not used for limiting scope of the present invention.
Embodiment 1
(1) preparation of graphene oxide dispersion liquid: under continuous condition of stirring, with 5g graphite scale and 3.75g NaNO
3Join in the 150ml concentrated sulfuric acid (98%), reactant mixes the back and in ice bath, cools off; After stirring half an hour, with 20g KMnO
4In half an hour, join in the above-mentioned dispersion; Remove ice bath then, the temperature of suspension will be gone up to about 35 ℃, continue to stir after 20 hours to become the taupe pastel; Afterwards, stop to stir, place after 5 days, slowly add 500ml deionized water and 30ml H successively while stirring
2O
2, generate glassy yellow suspension; This suspension is centrifugal, remove supernatant, keep lower sediment, then deposition is added aqueous dispersion, this process triplicate, flush away kish ion; Then, the deposition that obtains is added aqueous dispersion, centrifugal, collect upper strata centrifugate, it is centrifugal that lower sediment is continued to add aqueous dispersion, collects upper strata centrifugate, and so repeatedly, centrifugate is limpid until the upper strata, discarded lower sediment.The upper strata centrifugate of collecting is merged, use molecular weight to dialyse as the bag filter of 8000-14000 then, the product of gained has been carried out the Raman spectrum sign, it is positioned at 1350cm
-1The intensity of D band characteristic peak be positioned at 1590cm less than it
-1The G band characteristic peak at place, the result shows and has obtained the even dispersion liquid of graphene oxide.
(2) the graphene oxide dispersion liquid with 5mg/ml is encased in the syringe that the syringe needle diameter is 0.26mm; Speed injection with 25ml/min obtains macroscopical graphene oxide fiber in the solution of 0.5mg/ml softex kw; Then; Fiber is taken out, place polytetrafluoroethylsubstrate substrate, drying at room temperature ten minutes.
(3) the graphene oxide fiber is placed the beaker of the hydroiodic acid that 20ml is housed, wrap up beaker with masking foil, put into 80 ℃ of baking ovens reactions after 8 hours, spend deionised water, drying at room temperature obtains the one dimension macroscopic fibres.With Raman spectrum resulting fiber is characterized, it is positioned at 1353cm
-1The intensity of D band characteristic peak be positioned at 1589cm greater than it
-1The G band characteristic peak at place, this explanation graphene oxide fiber successfully is reduced into the Graphene fiber, and is of Fig. 1, and Fig. 1 shows the optical photograph that one dimension macroscopic view Graphene fiber that embodiment 1 obtains is curled into the spring-like fiber.Fig. 2 is the electron scanning micrograph according to the one dimension macroscopic view Graphene fiber of the embodiment of the invention 1 acquisition; The diameter that from electron scanning micrograph shown in Figure 2, can obtain fiber is about 45 microns; And electron scanning micrograph shown in Figure 3 has shown that the cross section of the fiber that embodiment 1 is prepared has the design feature that stratiform is piled up; Electron scanning micrograph shown in Figure 4 has shown that the Graphene fiber of embodiment 1 acquisition is regularly arranged along long axis direction by graphene film, has consistent orientation.
Repeat embodiment 1, following difference is arranged: the graphene oxide dispersion liquid of 5mg/ml is encased in the syringe that the syringe needle diameter is 0.11mm.Fig. 5 is that the diameter that from electron scanning micrograph shown in Figure 5, can obtain fiber is about 27 microns according to the electron scanning micrograph of the one dimension macroscopic view Graphene fiber of present embodiment 2 acquisitions.In addition, can find out that the diameter of fiber reduces and reduces with the syringe needle diameter in conjunction with the result of above embodiment 1.
Embodiment 3
Repeat embodiment 1, following difference is arranged: the graphene oxide dispersion liquid of 5mg/ml is encased in the syringe that the syringe needle diameter is 0.41mm, and result and embodiment 2 are similar.
Repeat embodiment 1, following difference is arranged: the graphene oxide dispersion liquid of 5mg/ml is encased in the syringe that the syringe needle diameter is 0.60mm, and result and embodiment 2 are similar.
Repeat embodiment 1, following difference is arranged: the graphene oxide dispersion liquid of 8mg/ml is encased in the syringe that the syringe needle diameter is 0.26mm.Fig. 6 is that the diameter that from electron scanning micrograph shown in Figure 6, can obtain fiber is about 53 microns according to the electron scanning micrograph of the one dimension macroscopic view Graphene fiber of present embodiment 5 acquisitions.
Repeat embodiment 1, following difference is arranged: the graphene oxide dispersion liquid of 10mg/ml is encased in the syringe that the syringe needle diameter is 0.26mm, and the result of acquisition and embodiment 5 are similar.
Embodiment 7
Repeat embodiment 1, following difference is arranged: the graphene oxide dispersion liquid of 20mg/ml is encased in the syringe that the syringe needle diameter is 0.26mm.Fig. 7 is that the diameter that from electron scanning micrograph shown in Figure 7, can obtain fiber is about 120 microns according to the electron scanning micrograph of the one dimension macroscopic view Graphene fiber of present embodiment 7 acquisitions.Result in conjunction with previous embodiment can find out that the diameter of the Graphene fiber of acquisition increases with the concentration of the graphene oxide dispersion liquid that uses.
Embodiment 8
Repeat embodiment 1; Following difference is arranged: the graphene oxide fiber is placed the beaker of the hydrazine hydrate that 20ml is housed, wrap up beaker, put into 80 ℃ of baking ovens reactions after 8 hours with masking foil; Spend deionised water; Drying at room temperature obtains one dimension macroscopic view Graphene fiber, and its result and embodiment 1 are similar.
Above embodiment explanation; Adopt the preparation method who provides among the present invention; The diameter of the macroscopical Graphene fiber that obtains is adjustable; Wherein increase syringe needle diameter that uses syringe or the concentration that improves the graphene oxide dispersion liquid, the diameter of resulting macroscopical Graphene fiber also correspondingly increases.
In addition, the present invention also embodiment 1 prepared single Graphene fiber has been carried out TENSILE STRENGTH-deformation curve measurement and electric conductivity is measured, and the result is referring to Fig. 8 and Fig. 9.As can beappreciated from fig. 8, its largest deformation amount is 3.2%, and corresponding TENSILE STRENGTH is 182MPa, and Young's modulus reaches 8.7GPa; And as can be seen from Figure 9, the electric current (I) of the Graphene fiber that is obtained and voltage (V) have good linear relationship, and the conductance that calculates is 35S/cm.The one dimension macroscopic view Graphene fiber that this shows among the present invention to be obtained has the advantage that mechanical strength is high and conduct electricity very well.
Should be understood that; The above only is a preferred implementation of the present invention, to those skilled in the art, and under the prerequisite that does not break away from know-why of the present invention and scope; Can realize multiple change or conversion, and these modifications should be regarded as in protection scope of the present invention also to these embodiment.
Claims (11)
1. an one dimension macroscopic view Graphene fiber preparation method is characterized in that, may further comprise the steps:
A., the graphene oxide dispersion liquid is provided;
B. with said graphene oxide dispersion liquid join as in the softex kw aqueous solution of coagulating bath to obtain the graphene oxide fiber; With
C. said graphene oxide fiber obtains said one dimension macroscopic view Graphene fiber through reduction and dry.
2. one dimension macroscopic view Graphene fiber preparation method according to claim 1 is characterized in that said graphene oxide dispersion liquid provides through following steps:
A1. the mixture of Graphene scale and nitrate is joined and carry out pre-oxidation in the strong acid, stir and obtain dispersion liquid;
A2. in the said dispersion liquid of a1, add strong oxidizer, stir, placed 1-10 days, obtain the taupe pastel;
A3. in the said taupe pastel of a2, add deionized water and hydrogen peroxide solution successively, obtain glassy yellow suspension;
A4. the said glassy yellow suspension of a3 is centrifugal, the washing and the dialysis, obtain said graphene oxide dispersion liquid.
3. one dimension macroscopic view Graphene fiber preparation method according to claim 1 is characterized in that the concentration of the graphene oxide dispersion liquid that uses among the said step b is 5～20mg/mL.
4. one dimension macroscopic view Graphene fiber preparation method according to claim 1 is characterized in that the concentration of the softex kw aqueous solution that uses among the said step b is 0.1-5mg/mL.
5. one dimension according to claim 1 macroscopic view Graphene fiber preparation method is characterized in that, in said step c, uses hydroiodic acid or hydrazine hydrate to reduce said graphene oxide fiber.
6. one dimension according to claim 5 macroscopic view Graphene fiber preparation method is characterized in that, in said step c, uses hydroiodic acid as reductant and reaction 2-12 hour.
7. one dimension macroscopic view Graphene fiber preparation method according to claim 5 is characterized in that in said step c, using hydroiodic acid is 50～80 ℃ as reductant and reaction temperature.
8. one dimension macroscopic view Graphene fiber preparation method according to claim 1; It is characterized in that; After said step c, after said one dimension macroscopic view Graphene fiber taken out and clean with deionized water, drying at room temperature and obtain said one dimension macroscopic view Graphene fiber.
9. one dimension macroscopic view Graphene fiber preparation method according to claim 1 is characterized in that in said step b, said graphene oxide dispersion liquid is injected in the said softex kw aqueous solution through syringe.
10. one dimension macroscopic view Graphene fiber preparation method according to claim 9 is characterized in that the syringe needle diameter of said syringe is 0.10～1.0mm.
11. one dimension macroscopic view Graphene fiber that obtains through each described preparation method among the claim 1-10.
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Application publication date: 20121212 |