CN109545573B - Preparation method of metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material - Google Patents
Preparation method of metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material Download PDFInfo
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- USBWXQYIYZPMMN-UHFFFAOYSA-N rhenium;heptasulfide Chemical compound [S-2].[S-2].[S-2].[S-2].[S-2].[S-2].[S-2].[Re].[Re] USBWXQYIYZPMMN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 53
- 239000002184 metal Substances 0.000 title claims abstract description 53
- 239000007772 electrode material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims description 10
- 239000002077 nanosphere Substances 0.000 title description 43
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 5
- 235000013878 L-cysteine Nutrition 0.000 claims description 5
- 239000004201 L-cysteine Substances 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 239000003990 capacitor Substances 0.000 abstract description 8
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000008151 electrolyte solution Substances 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 9
- 238000011056 performance test Methods 0.000 description 8
- 238000002484 cyclic voltammetry Methods 0.000 description 6
- 238000004146 energy storage Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 230000001351 cycling effect Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- -1 transition metal chalcogenide Chemical class 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
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Abstract
The invention discloses a method for synthesizing a rhenium sulfide supercapacitor electrode material with a hollow metal 1T-phase structure by a hydrothermal synthesis method, and belongs to the technical field of new energy. The electrode material of the super capacitor has the advantages of large specific capacitance, high electrochemical stability, long cycle life and good electrochemical performance; the working electrode is simple to prepare, energy-saving and environment-friendly, and has wide industrial application prospect.
Description
Technical Field
The invention belongs to the field of preparation of capacitor electrode materials, and particularly relates to a preparation method of a metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material.
Background
The rapid consumption of energy promotes the rapid development of economy, and simultaneously, the problems of more serious environmental pollution, global warming and the like are brought. It is therefore of paramount importance to find new energy storage and conversion systems that are inexpensive, efficient and environmentally friendly. The super capacitor is also called as an electrochemical capacitor, is a novel energy storage device between a traditional capacitor and a secondary battery, which develops rapidly in recent years, and has the advantages of the traditional capacitor and the secondary battery, namely higher energy density than the traditional capacitor and higher power density than various secondary batteries. In addition, the typical advantages of supercapacitors, including fast charge rate, long cycle life, wide operating temperature range, maintenance-free, economical and environmentally friendly, have also prompted their use in many areas.
The transition metal chalcogenide has the advantages of high theoretical capacity, low price and simple preparation, and is widely applied to the field of energy storage. However, due to its poor conductivity, the practical capacity and cycling performance of transition metal chalcogenides is yet to be further improved. Research shows that the transition metal sulfide has three phase structures of 1T, 2H and 3R. Compared with other two phase structures, the metal 1T phase has very strong conductivity and can enhance the specific capacitance and the cycling stability of the material.
Disclosure of Invention
The invention aims to provide a preparation method of a metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material with high specific capacitance and good stability.
In order to achieve the purpose, the invention adopts the technical scheme that the preparation method of the metal 1T-phase rhenium sulfide nanometer hollow sphere super capacitor electrode material comprises the following steps:
(1) mixing and stirring 30-40 mL of absolute ethyl alcohol, 100-150 mL of water and 1-2 mL of ammonia water with the mass concentration of 25-28% for 30-60 minutes, then adding 1-2.5 mL of tetraethoxysilane, continuously stirring for 10-20 minutes, then adding 0.4-0.8 g of dopamine hydrochloride, stirring for 24-48 hours, and then centrifugally drying; calcining for 2-5 hours at the temperature of 750-850 ℃, and etching by using hydrofluoric acid to obtain hollow carbon spheres;
(2) dispersing 30-70 mg of hollow carbon spheres in 40-60 mL of ethanol, adding 0.1-0.3 g of ammonium perrhenate, 0.1-0.3 g L-cysteine and 0.02-0.08 g of CTAB (cetyl trimethyl ammonium bromide), carrying out hydrothermal reaction at 160-200 ℃ for 12-36 hours, and carrying out centrifugal drying to obtain the metal 1T-phase rhenium sulfide nano hollow sphere supercapacitor electrode material.
Preferably, the etching with hydrofluoric acid comprises the following specific steps: and dispersing the solid obtained by calcination in a hydrofluoric acid solution with the mass concentration of 10-20%, soaking in a water bath at 50-70 ℃ for more than 24h, filtering, washing with deionized water, and drying to obtain the hollow carbon spheres.
The invention has the following beneficial effects: the preparation method provided by the invention is simple to operate, the 1T-phase rhenium sulfide nano hollow sphere nano material with a complete structure and excellent performance can be prepared in a short time, no complex equipment is needed, the cost is low, the synthesized 1T-phase rhenium sulfide has a good internal porous structure, a high specific capacitance, stable electrochemical performance and a long cycle life, and the method provides possibility for industrial production, is an excellent supercapacitor electrode material, and has a good development prospect.
Drawings
FIG. 1a is an XRD (X-ray diffraction) diagram of a metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 1 of the invention; b is a Raman diagram;
FIG. 2 is an SEM image of a metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 1 of the invention;
FIG. 3 is a cyclic voltammogram of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 1 of the invention at different sweep rates;
FIG. 4 is a charging and discharging curve diagram of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 1 of the invention under different current densities;
FIG. 5 shows that the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 1 of the invention is 1A g-1A plot of cycling stability at current density;
FIG. 6 is an electrochemical impedance diagram of the electrode material of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor prepared in example 1 of the invention;
FIG. 7 is an SEM image of a metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 2 of the invention;
FIG. 8 is a cyclic voltammetry curve diagram of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 2 of the invention at different sweep rates;
FIG. 9 is a charging and discharging curve diagram of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 2 of the invention under different current densities;
FIG. 10 shows that the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 2 of the invention is 1A g-1A plot of cycling stability at current density;
FIG. 11 is an electrochemical impedance diagram of the electrode material of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor prepared in example 2 of the invention;
FIG. 12 is an SEM image of a metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 3 of the invention;
FIG. 13 is a cyclic voltammogram of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 3 of the invention at different sweep rates;
FIG. 14 is a charging and discharging curve diagram of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 3 of the invention under different current densities;
FIG. 15 shows that the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 3 of the invention is 1A g-1A plot of cycling stability at current density;
fig. 16 is an electrochemical impedance diagram of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material prepared in example 3 of the invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. In addition, after reading the teaching of the present invention, those skilled in the art can make various changes or modifications to the invention, and these equivalents also fall within the scope of the claims appended to the present application. The manufacturing process of the electrode plate when the electrochemical performance test is carried out in the following embodiment is as follows: the manufacturing process of the electrode plate when the electrochemical performance test is carried out in the following embodiment is as follows: preparing slurry by using the obtained rhenium sulfide hollow nanosphere powder particles, carbon black and polytetrafluoroethylene according to the mass ratio of 80:10:10, then uniformly coating the slurry on foamed nickel, tabletting and drying, wherein the loading capacity of rhenium sulfide is about 2-3 mg.
Example 1
(1) Mixing 36 mL of absolute ethyl alcohol, 120 mL of water and 1.5 mL of ammonia water (the mass concentration is 25% -28%), stirring for 45 minutes, then adding 1.5 mL of ethyl orthosilicate, continuing stirring for 15 minutes, then adding 0.6 g of dopamine hydrochloride, stirring for 32 hours, then centrifugally drying, calcining at 800 ℃ for 3 hours, dispersing the calcined solid in a hydrofluoric acid solution with the mass concentration of 10%, soaking in a water bath at 60 ℃ for 24 hours, filtering, washing with deionized water, and drying to obtain the hollow carbon spheres;
(2) dispersing 50 mg hollow carbon spheres in 50 mL absolute ethyl alcohol, adding 0.2 g ammonium perrhenate, 0.2 g L-cysteine and 0.05g CTAB, carrying out hydrothermal reaction at 180 ℃ for 24 hours, and carrying out centrifugal drying to obtain the hollow rhenium sulfide nanospheres in the metal 1T phase.
The performance test of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material in the embodiment 1 of the invention is carried out, and the results are shown in the figures 1-6.
As shown in fig. 1, XRD and Raman tests prove that the prepared rhenium sulfide is of a metal 1T phase structure;
as shown in fig. 2, the metal 1T-phase rhenium sulfide is uniformly and densely attached to the surface of the hollow carbon sphere, and it can be seen by a high power microscope that rhenium sulfide is in a lamellar structure, which is beneficial to providing a larger specific surface area and cycle stability;
FIG. 3 shows a cyclic voltammetry curve of a metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material at a scanning speed of 10-50 mV/s and with 2M KOH as an electrolyte solution, wherein redox peaks in the cyclic curve are symmetrically distributed and are represented as a typical Faraday pseudo-capacitance model;
fig. 4 shows a charge-discharge performance test curve of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material with 2M KOH as an electrolyte solution at a current density of 1-10A/g, the curve deviating from a symmetrical triangular curve model, and with reference to fig. 3, it is illustrated that the energy storage mechanism of the metal 1T-phase rhenium sulfide hollow nanosphere is a faraday pseudocapacitance model; with the increase of the current density, the specific capacitance of the material is reduced, but the descending trend is gentle, and meanwhile, the curve is symmetrical about an axis, so that the material has good capacitive behavior to a certain extent;
fig. 5 shows a cycle stability test curve of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material under a current density of 1A/g and with 2M KOH as an electrolyte solution, and through a 1000-cycle charge-discharge test, 83.4% of the initial capacity is preserved, which indicates that the material has good electrochemical stability;
fig. 6 shows an electrochemical impedance test of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material with 2M KOH as an electrolyte solution, and it is seen from the figure that the resistance of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material is relatively small, which is beneficial to electron transmission and exhibits good electrochemical performance.
Example 2
(1) Mixing 36 mL of absolute ethyl alcohol, 120 mL of water and 1.5 mL of ammonia water (the mass concentration is 25% -28%), stirring for 45 minutes, then adding 1.5 mL of ethyl orthosilicate, continuing stirring for 15 minutes, then adding 0.6 g of dopamine hydrochloride, stirring for 32 hours, then centrifugally drying, calcining at 800 ℃ for 3 hours, dispersing the calcined solid in a hydrofluoric acid solution with the mass concentration of 10%, soaking in a water bath at 60 ℃ for 24 hours, filtering, washing with deionized water, and drying to obtain the hollow carbon spheres;
(2) dispersing 30 mg hollow carbon spheres in 50 mL absolute ethyl alcohol, adding 0.2 g ammonium perrhenate, 0.2 g L-cysteine and 0.05g CTAB, carrying out hydrothermal reaction at 180 ℃ for 24 hours, and carrying out centrifugal drying to obtain the hollow rhenium sulfide nanospheres in the metal 1T phase.
The performance test of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material in the embodiment 2 of the invention is carried out, and the results are shown in FIGS. 7-11.
As shown in fig. 7, the metallic 1T-phase rhenium sulfide is piled up in a large amount, and the globular structure becomes less noticeable;
FIG. 8 shows a cyclic voltammetry curve of a metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material at a scanning speed of 10-50 mV/s and with 2M KOH as an electrolyte solution, wherein redox peaks in the cyclic curve are symmetrically distributed and are represented as a typical Faraday pseudo-capacitance model;
fig. 9 shows a charge-discharge performance test curve of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material with 2M KOH as an electrolyte solution at a current density of 1-20A/g, the curve deviates from a symmetrical triangular curve model, and the energy storage mechanism of the metal 1T-phase rhenium sulfide hollow nanosphere is a faraday pseudo-capacitance model; with the increase of the current density, the specific capacitance of the material is reduced, but the descending trend is gentle, and meanwhile, the curve is symmetrical about an axis, so that the material has good capacitive behavior to a certain extent;
fig. 10 shows a cycle stability test curve of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material under a current density of 1A/g and with 2M KOH as an electrolyte solution, and after a 1000-cycle test, 79.7% of the initial capacity is retained, which indicates better cycle stability;
fig. 11 shows that in the electrochemical impedance test of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material with 2M KOH as an electrolyte solution, a smaller resistance is beneficial to improving the electrochemical performance of the material.
Example 3
(1) Mixing and stirring 36 mL of absolute ethyl alcohol, 120 mL of water and 1.5 mL of ammonia water (the mass concentration is 25% -28%) for 45 minutes, then adding 1.5 mL of ethyl orthosilicate, continuously stirring for 15 minutes, then adding 0.6 g of dopamine hydrochloride, stirring for 32 hours, then centrifugally drying, calcining at 800 ℃ for 3 hours, dispersing the calcined solid in a hydrofluoric acid solution with the mass concentration of 10%, soaking in a water bath at 60 ℃ for 24 hours, filtering, washing with deionized water, and drying to obtain the hollow carbon sphere.
(2) Dispersing 70 mg hollow carbon spheres in 50 mL absolute ethyl alcohol, adding 0.2 g ammonium perrhenate, 0.2 g L-cysteine and 0.05g CTAB, carrying out hydrothermal reaction at 180 ℃ for 24 hours, and carrying out centrifugal drying to obtain the hollow rhenium sulfide nanospheres in the metal 1T phase.
The performance test of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material in the embodiment 3 of the invention is carried out, and the results are shown in the figures 12-16:
as shown in fig. 12, the metal 1T-phase rhenium sulfide is uniformly attached to the surface of the carbon sphere, and presents a spherical structure;
FIG. 13 shows a cyclic voltammetry curve of a metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material at a scanning speed of 10-50 mV/s and with 2M KOH as an electrolyte solution, wherein redox peaks in the cyclic curve are symmetrically distributed and represent a typical Faraday pseudo-capacitance model;
fig. 14 shows a charge-discharge performance test curve of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material with 2M KOH as an electrolyte solution at a current density of 1-10A/g, the curve deviates from a symmetrical triangular curve model, and the energy storage mechanism of the metal 1T-phase rhenium sulfide hollow nanosphere is a faraday pseudo-capacitance model; with the increase of the current density, the specific capacitance of the material is reduced, but the descending trend is gentle, and meanwhile, the curve is symmetrical about an axis, so that the material has good capacitive behavior to a certain extent;
fig. 15 shows a cycle stability test curve of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material under a current density of 1A/g and with 2M KOH as an electrolyte solution, after 1000 cycles, 84.6% of the initial capacity is preserved, which indicates the excellent cycle stability;
as shown in fig. 16, the electrochemical impedance test of the metal 1T-phase rhenium sulfide hollow nanosphere supercapacitor electrode material with 2M KOH as an electrolyte solution is performed, and the smaller resistance is beneficial to improving the electrochemical performance of the material.
Claims (3)
1. A preparation method of a metal 1T-phase rhenium sulfide nanometer hollow sphere supercapacitor electrode material is characterized by comprising the following steps:
(1) mixing and stirring 30-40 mL of absolute ethyl alcohol, 100-150 mL of water and 1-2 mL of ammonia water with the mass concentration of 25-28% for 30-60 minutes, then adding 1-2.5 mL of tetraethoxysilane, continuously stirring for 10-20 minutes, then adding 0.4-0.8 g of dopamine hydrochloride, stirring for 24-48 hours, and then centrifugally drying; calcining for 2-5 hours at the temperature of 750-850 ℃, and etching by using hydrofluoric acid to obtain hollow carbon spheres;
(2) dispersing 30-70 mg of hollow carbon spheres in 40-60 mL of ethanol, adding 0.1-0.3 g of ammonium perrhenate, 0.1-0.3 g of L-cysteine and 0.02-0.08 g of CTAB, carrying out hydrothermal reaction at 160-200 ℃ for 12-36 hours, and carrying out centrifugal drying to obtain the metal 1T-phase rhenium sulfide nano hollow sphere supercapacitor electrode material.
2. The preparation method of the metal 1T-phase rhenium sulfide nanometer hollow sphere supercapacitor electrode material according to claim 1, characterized in that the specific steps of etching with hydrofluoric acid are as follows: and dispersing the solid obtained by calcination in a hydrofluoric acid solution with the mass concentration of 10-20%, soaking in a water bath at 50-70 ℃ for more than 24h, filtering, washing with deionized water, and drying to obtain the hollow carbon spheres.
3. The metal 1T-phase rhenium sulfide nanometer hollow sphere supercapacitor electrode material prepared by the method of claim 1 or 2.
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| CN105858646A (en) * | 2016-04-19 | 2016-08-17 | 北京航空航天大学 | Preparation method of transparent thin film |
| CN106277064A (en) * | 2016-07-22 | 2017-01-04 | 电子科技大学 | A kind of method preparing rhenium disulfide nanometer sheet |
| CN107362812A (en) * | 2017-07-25 | 2017-11-21 | 苏州大学 | A kind of compound two-dimensional material of selenium sulfuration rhenium, preparation method and applications |
| CN107611388A (en) * | 2017-08-31 | 2018-01-19 | 扬州大学 | A kind of shell has the preparation method of the carbon coating tungsten sulfide hollow nano-sphere of sandwich structure |
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Patent Citations (4)
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| CN105858646A (en) * | 2016-04-19 | 2016-08-17 | 北京航空航天大学 | Preparation method of transparent thin film |
| CN106277064A (en) * | 2016-07-22 | 2017-01-04 | 电子科技大学 | A kind of method preparing rhenium disulfide nanometer sheet |
| CN107362812A (en) * | 2017-07-25 | 2017-11-21 | 苏州大学 | A kind of compound two-dimensional material of selenium sulfuration rhenium, preparation method and applications |
| CN107611388A (en) * | 2017-08-31 | 2018-01-19 | 扬州大学 | A kind of shell has the preparation method of the carbon coating tungsten sulfide hollow nano-sphere of sandwich structure |
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| "二硫族二维半导体材料的制备及性能研究";戚飞;《中国博士学位论文全文数据库 息科技辑》;20180115;论文第1页第1段-第9页倒数第1段、第88页第1段-94页第1段 * |
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