CN114606601B - Hybrid fiber, preparation method and application thereof in electrode material - Google Patents
Hybrid fiber, preparation method and application thereof in electrode material Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 48
- 239000007772 electrode material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 54
- 229910017709 Ni Co Inorganic materials 0.000 claims abstract description 23
- 229910003267 Ni-Co Inorganic materials 0.000 claims abstract description 23
- 229910003262 Ni‐Co Inorganic materials 0.000 claims abstract description 23
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 230000001112 coagulating effect Effects 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000009987 spinning Methods 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 7
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 7
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000007493 shaping process Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 8
- 238000006722 reduction reaction Methods 0.000 claims description 6
- 238000002166 wet spinning Methods 0.000 claims description 6
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 5
- 229940071870 hydroiodic acid Drugs 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 5
- 239000002657 fibrous material Substances 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 description 6
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 5
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002135 nanosheet Substances 0.000 description 3
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- UUCGKVQSSPTLOY-UHFFFAOYSA-J cobalt(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Co+2].[Ni+2] UUCGKVQSSPTLOY-UHFFFAOYSA-J 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/40—Fibres
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the field of functional fiber materials, and discloses a hybrid fiber, a preparation method and application thereof in an electrode material. The preparation method of the invention comprises the following steps: dissolving nickel nitrate, cobalt nitrate and hexadecyl trimethyl ammonium bromide in graphene oxide solution, transferring into a reaction kettle for reaction for 12 hours at 180 ℃ after ultrasonic treatment, and taking a precipitate; dispersing the precipitate in deionized water for ultrasonic treatment after cleaning, adding graphene oxide for ultrasonic treatment, and stirring until gel is formed to obtain spinning solution; taking acetic acid as a coagulating bath, extruding spinning solution into the coagulating bath by using a needle cylinder, and collecting fibers after drafting, drying and shaping; and (3) drying the fiber, soaking the fiber in HI for reduction, washing with water, and drying to obtain the Ni-Co LDHs/graphene hybrid fiber. The hybrid fiber is used as an electrode material, has good flexibility, small volume and excellent electrochemical performance, and can be applied to super capacitors.
Description
Technical Field
The invention belongs to the field of functional fiber materials, relates to a hybrid fiber, a preparation method and application thereof in electrode materials, in particular to a Ni-Co LDHs/graphene hybrid fiber, a preparation method and application thereof in electrode materials, and particularly relates to a Ni-Co LDHs/graphene hybrid fiber, a preparation method and application thereof in electrode materials for super capacitors.
Background
In the following, flexible and wearable electronics have become a focus of attention in the heavy industry, and flexible/wearable energy sources are needed to power the next generation portable intelligent electronics. Because the traditional energy storage device has a rigid, heavy or plane structure, the future application possibility is very small, so the development of the portable, small and predictable-performance energy storage device is particularly important, and the realization of portable and flexible wearable electronic energy sources is realized. Fibrous Supercapacitors (SCs), which are a promising energy storage device, show considerable application potential in flexible electronics due to their small size and ability to be woven into textiles or other portable devices. Graphene is an alternative material for the Jing Rouxing electrode with larger application due to light weight, high mechanical strength, large specific surface area and excellent conductivity.
However, in the preparation process of graphene, irreversible agglomeration caused by strong pi-pi interaction between flakes makes it difficult to achieve a theoretical large specific surface area, so that the maximization of the performance of graphene as an electrode is difficult to achieve. Therefore, structural design for preparing graphene fibers with porous structures and large-sized specific surface areas have become important tasks for expanding the application of the graphene fibers in flexible SCs.
The nickel cobalt-based oxide/hydroxide is used for super capacitors, and can be traced back to the work of Liu et al (K C Liu, M A Anderson. Journal of the Electrochemical Society,1996,143 (1): 124) in 1996 at the earliest, and the specific capacitance of the electrode materials prepared by the nickel cobalt-based oxide/hydroxide is only 50-64F g-1. Transition metal oxides and hydroxides have been widely studied for use in pseudocapacitive electrode materials over the past few years. According to the report of the literature, the transition metal-based oxide material has high theoretical specific capacitance, and RuO2 is the metal oxide electrode material which is applied to super capacitors at the earliest, and the specific capacitance can reach 1300F g-1, but the practical application is limited due to the high price of the RuO 2. Nickel-cobalt-based oxide/hydroxide is regarded as an electrode material of a supercapacitor, and has high theoretical specific capacitance, but most of nickel-cobalt compounds have poor conductivity, and phase change causes obvious volume change in the charge and discharge process, so that the specific capacitance, the rate capability and the cycle performance of the material are poor. In order to overcome these defects, an important strategy is to combine transition metal oxide/hydroxide with a conductive material with high specific surface area such as graphene, and the like, so as to increase ion transmission and conductivity, thereby constructing an efficient nickel-cobalt-based compound array.
Disclosure of Invention
The invention aims at providing a Ni-Co LDHs/graphene hybrid fiber, a preparation method and application thereof in an electrode material.
The invention provides a preparation method of Ni-Co LDHs/graphene hybrid fibers, which comprises the following steps:
step 1, dispersing graphene oxide in deionized water for ultrasonic treatment to obtain a uniformly dispersed graphene oxide solution; wherein, the graphene oxide is preferably prepared by a modified Hummers method;
step 2, dissolving nickel nitrate, cobalt nitrate and hexadecyl trimethyl ammonium bromide in a graphene oxide solution, performing ultrasonic treatment to obtain a reaction solution, transferring the reaction solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, and taking a precipitate after reacting for 12 hours at 180 ℃; in the reaction solution, the concentration of nickel nitrate is 1-5 g/L, the concentration of cobalt nitrate is 1-5 g/L, and the concentration of hexadecyl trimethyl ammonium bromide is 1-10 g/L;
step 3, dispersing the precipitate in deionized water for ultrasonic treatment for 1h after cleaning, adding graphene oxide, continuing ultrasonic treatment for 2h, and stirring until gel is formed to obtain spinning solution; the ultrasonic power of the ultrasonic treatment is preferably 40%;
step 4, using a wet spinning instrument, taking acetic acid as a coagulating bath, extruding spinning solution into the coagulating bath by using a needle cylinder, and collecting after drafting, drying and shaping;
and 5, drying the fiber collected in the step 4 for 24 hours at 60 ℃, soaking in a hydroiodic acid (HI) solution for reduction reaction, and then fully washing with ethanol for 5 times, and drying at 60 ℃ for 12 hours to obtain the Ni-Co LDHs/graphene hybrid fiber.
Further, in the step 1, the dosage ratio of the graphene oxide to the deionized water is 0.5g:100mL.
Further, in step 1, the ultrasonic treatment specifically includes: the cells were sonicated for 2h at room temperature using a cell disruptor.
Further, in step 3, the cleaning is: sequentially and respectively centrifugally cleaning with deionized water and ethanol for 5 times, wherein the centrifugal speed is 3000r/min, and the centrifugal cleaning time is 10min.
Further, in the step 3, the usage ratio of the precipitate, deionized water and graphene oxide is (0.1-0.5) g:100mL:0.5g.
Further, in step 3, the stirring is: stirring was performed at 60℃with a magnetic stirrer.
Further, in step 4, the extrusion rate was 50. Mu.l/min.
Further, in step 4, the temperature of the reduction reaction is 95 ℃ and the time is 10 hours.
The invention also provides the Ni-Co LDHs/graphene hybrid fiber prepared by the preparation method.
The invention also provides application of the Ni-Co LDHs/graphene hybrid fiber in an electrode material.
Further, the electrode material is an electrode material for a super capacitor.
Compared with the prior art, the invention provides a method for preparing Ni-Co LDHs/graphene hybrid fiber by wet spinning, and in the technical scheme provided by the invention, ni 2+ And Co 2+ First with OH - The reaction produces nickel hydroxide and cobalt hydroxide monomers which precipitate in the form of atomic nuclei and rapidly grow into main particles, nickel and cobalt hydroxide primary particles continue to grow to form nano sheets and are cross-linked with each other, and the obtained Ni-Co LDHs/graphene hybrid fibers have spherical structures formed by nano sheets with interlayer spacing, have the advantages of high conductivity, high redox performance and nano sheet array morphology, provide more stable structures, larger specific surface area and more exposed active sites, are favorable for contact of Ni-Co LDHs with electrolytes, and further enhance electrochemical performance. In addition, the hybrid fiber prepared by wet spinning has large flexibility, small volume and excellent electrochemical performance.
Drawings
FIG. 1 is an optical photograph of Ni-Co LDHs/graphene hybrid fibers in example 2 of the present invention;
fig. 2 is a diagram of embodiment 2 of the present invention: (a) XRD pattern of Ni-Co LDHs; (b) XRD pattern of Ni-Co LDHs/graphene hybrid fibers;
FIG. 3 is a CV curve measured at a scan rate of 10mV/s for different hybrid fibers and pure graphene fibers over a potential range of 0-0.6V.
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present invention, and equivalent changes and modifications are also within the scope of the present application as defined in the claims.
Example 1
Step 1, weighing 0.5g of graphene oxide, dispersing in 100ml of deionized water, and carrying out ultrasonic treatment on the graphene oxide for 2 hours by using a cell pulverizer under the condition of room temperature to obtain a uniformly dispersed graphene oxide solution;
and 2, weighing 0.1g of nickel nitrate, 0.1g of cobalt nitrate and 0.1g of hexadecyl trimethyl ammonium bromide, dissolving in 100ml of graphene oxide solution prepared in the step 1, carrying out ultrasonic treatment for 30min, transferring the solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, and reacting for 12h at 180 ℃. And then the product is centrifugally washed for 5 times by deionized water and ethanol respectively.
And 3, weighing 0.1g of the precipitate prepared in the step 2, dispersing in 100ml of deionized water, performing ultrasonic treatment for 1h by using a cell pulverizer, and adding 0.5g of graphene oxide for continuous ultrasonic treatment for 2h. And then stirring and concentrating the treated solution at 60 ℃ by using a magnetic stirrer to form gel so as to obtain spinning solution.
And 4, using a wet spinning instrument, taking acetic acid as a coagulating bath, extruding the spinning solution into the coagulating bath at a speed of 50 mu l/min by using a needle cylinder, and collecting after drafting, drying and shaping.
And 5, drying the collected fibers at 60 ℃ for 24 hours. And soaking the dried fiber in HI for reduction, then fully washing with ethanol for 5 times, and drying at 60 ℃ for 12 hours to obtain the Ni-Co LDHs/RGO hybrid fiber.
Example 2
Step 1, weighing 0.5g of graphene oxide, dispersing in 100ml of deionized water, and carrying out ultrasonic treatment on the graphene oxide for 2 hours by using a cell pulverizer under the condition of room temperature to obtain a uniformly dispersed graphene oxide solution;
and 2, weighing 0.5g of nickel nitrate, 0.5g of cobalt nitrate and 1g of hexadecyl trimethyl ammonium bromide, dissolving in 100ml of graphene oxide solution prepared in the step 1, carrying out ultrasonic treatment for 30min, transferring the solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, and reacting for 12h at 180 ℃. And then the product is centrifugally washed for 5 times by deionized water and ethanol respectively.
And 3, weighing 0.5g of the precipitate prepared in the step 2, dispersing in 100ml of deionized water, performing ultrasonic treatment for 1h by using a cell pulverizer, and adding 0.5g of graphene oxide to continue ultrasonic treatment for 2h. And then stirring and concentrating the treated solution at 60 ℃ by using a magnetic stirrer to form gel so as to obtain spinning solution.
And 4, using a wet spinning instrument, taking acetic acid as a coagulating bath, extruding the spinning solution into the coagulating bath at a speed of 50 mu l/min by using a needle cylinder, and collecting after drafting, drying and shaping.
And 5, drying the collected fibers at 60 ℃ for 24 hours. And soaking the dried fiber in HI for reduction, then fully washing with ethanol for 5 times, and drying at 60 ℃ for 12 hours to obtain the Ni-Co LDHs/RGO hybrid fiber. An optical photograph of the Ni-Co LDHs/graphene hybrid fiber is shown in FIG. 1.
Analysis of the Ni-Co LDHs and Ni-Co LDHs/graphene hybrid fiber crystal structures of example 2 by XRD showed that fig. 2 (a) corresponds to diffraction peaks of (003) (006) (012) and (015) planes when 2θ angle is equal to 10.8 °,22.1 °,33.2 ° and 38.4 °, respectively, and that fig. 2 (b) shows one more diffraction peak at 2θ=26.6° compared to fig. 2 (a), which peak belongs to the characteristic diffraction peak of RGO, corresponds to (002) plane, indicating that example 2 successfully produced hybrid fiber.
Test case
The Cyclic Voltammetry (CV) test was performed on the hybrid fibers prepared in examples 1-2 and the comparative example, respectively, using pure graphene fibers as a comparative example, and the results are shown in the cyclic voltammetry curves of the pure graphene fibers and the hybrid fibers in fig. 3. As can be seen from fig. 3, the hybrid fiber material has a redox peak which contributes to the redox reaction of the nickel cobalt hydroxide. At a scanning rate of 10mV s-1, the CV curve of the pure graphene fiber of the comparative example is very narrow, while the CV curve areas of the hybrid fibers in examples 1 and 2 are far larger than those of the comparative example, and the corresponding specific capacitance value is higher, so that the pure graphene fiber has better electrochemical performance.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. The preparation method of the Ni-Co LDHs/graphene hybrid fiber is characterized by comprising the following steps of:
step 1, dispersing graphene oxide in deionized water for ultrasonic treatment to obtain a uniformly dispersed graphene oxide solution;
step 2, dissolving nickel nitrate, cobalt nitrate and hexadecyl trimethyl ammonium bromide in a graphene oxide solution, performing ultrasonic treatment to obtain a reaction solution, transferring the reaction solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, and taking a precipitate after reacting for 12 hours at 180 ℃; in the reaction solution, the concentration of nickel nitrate is 1-5 g/L, the concentration of cobalt nitrate is 1-5 g/L, and the concentration of cetyl trimethyl ammonium bromide is 1-10 g/L;
step 3, dispersing the precipitate in deionized water for ultrasonic treatment for 1h after cleaning, adding graphene oxide, continuing ultrasonic treatment for 2h, and stirring until gel is formed to obtain spinning solution; the dosage ratio of the sediment to the deionized water to the graphene oxide is (0.1-0.5) g:100mL:0.5 g;
step 4, using a wet spinning instrument, taking acetic acid as a coagulating bath, extruding spinning solution into the coagulating bath by using a needle cylinder, and collecting fibers after drafting, drying and shaping, wherein the extrusion rate is 50 mu l/min;
and 5, drying the fiber collected in the step 4 for 24 hours at 60 ℃, soaking in a hydroiodic acid solution for reduction reaction, then fully cleaning with ethanol for 5 times, and drying at 60 ℃ for 12 hours to obtain the Ni-Co LDHs/graphene hybrid fiber.
2. The method according to claim 1, wherein in step 1, the dosage ratio of graphene oxide to deionized water is 0.5g:100 And (3) mL.
3. The method according to claim 1, wherein in step 1, the ultrasonic treatment is specifically: the cells were sonicated for 2h at room temperature using a cell disruptor.
4. The method according to claim 1, wherein in step 3, the washing is: sequentially and respectively centrifugally cleaning with deionized water and ethanol for 5 times, wherein the centrifugal speed is 3000r/min, and the centrifugal cleaning time is 10min.
5. The method according to claim 1, wherein in step 3, the stirring is: stirring was performed at 60℃with a magnetic stirrer.
6. The method according to claim 1, wherein in step 5, the reduction reaction is carried out at a temperature of 95℃for a period of 10 hours.
7. The Ni-Co LDHs/graphene hybrid fiber prepared by the preparation method of any one of claims 1 to 6.
8. The use of the Ni-Co LDHs/graphene hybrid fiber of claim 7 in an electrode material.
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| 三维石墨烯基Co-Ni双氢氧化物复合材料的制备及其电化学性能;祁永东;;应用化工(第12期);第2210-2213、2216页 * |
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