CN110911176B - Preparation method of Te-C nano composite material applied to super capacitor - Google Patents
Preparation method of Te-C nano composite material applied to super capacitor Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 80
- 239000003990 capacitor Substances 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 48
- 238000001354 calcination Methods 0.000 claims abstract description 44
- 239000002131 composite material Substances 0.000 claims abstract description 25
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002105 nanoparticle Substances 0.000 claims abstract description 21
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 21
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 239000002135 nanosheet Substances 0.000 claims abstract description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 79
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 26
- 239000002244 precipitate Substances 0.000 claims description 21
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 16
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 16
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 16
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 14
- 229920006395 saturated elastomer Polymers 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000006479 redox reaction Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000007774 positive electrode material Substances 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 239000007772 electrode material Substances 0.000 abstract description 60
- 230000000717 retained effect Effects 0.000 abstract description 6
- QEZIKGQWAWNWIR-UHFFFAOYSA-N antimony(3+) antimony(5+) oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[Sb+3].[Sb+5] QEZIKGQWAWNWIR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000004146 energy storage Methods 0.000 description 16
- 238000012360 testing method Methods 0.000 description 12
- 238000004458 analytical method Methods 0.000 description 10
- 238000000840 electrochemical analysis Methods 0.000 description 10
- 239000003792 electrolyte Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 8
- 238000010276 construction Methods 0.000 description 5
- 230000001351 cycling effect Effects 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 150000004770 chalcogenides Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- 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
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- 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
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Abstract
The invention discloses Te-doped capacitor applied to a super capacitorThe preparation method of the C nano composite material prepares the nano composite electrode material applied to the super capacitor by a calcination method, and belongs to the technical field of new energy. According to the invention, the tellurium nanoparticle composite material Te-C coated by the ultrathin carbon nanosheets is obtained by calcining the powder mixture of the carbon quantum dots and the antimony dioxide. Te-C has excellent electrochemical properties, such as high specific capacity and specific energy, ultra-long cycle life and good rate capability. In addition, the preparation process of Te-C is simple, the cost is low, and the method has wide marketization application prospect. Te-C was used to assemble a supercapacitor, resulting in a capacitor of 33.7Wh Kg‑1The power density is 12kW Kg‑1After 10000 charge-discharge cycles, the initial capacity can be retained by 94.8%.
Description
Technical Field
The invention relates to a preparation method of a nano composite electrode material, in particular to a preparation method of a tellurium nano particle composite electrode material, which is applied to the technical field of electrode material preparation.
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 super capacitor has the advantages of high charging rate, long cycle life and wide working temperature range, and is promoted to be widely applied in multiple fields. Chalcogenide is a widely used electrode material with high specific capacitance and good rate capability. However, chalcogenide electrode materials have short cycle lives and less than ideal cycle stability.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a preparation method of a Te-C nano composite material applied to a super capacitor, wherein a Te-C nano composite electrode material is prepared by tightly bounding tellurium nano particles in an ultrathin carbon nanosheet shell under an ion confinement mechanism through a calcination method, and is applied to super capacitor construction.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of Te-C nano composite material applied to a super capacitor comprises the following steps:
a. under a normal condition, preparing a saturated aqueous solution of potassium hydroxide, slowly adding the saturated aqueous solution of potassium hydroxide into an acetaldehyde solution with the concentration of 40% (V/V), stirring for at least 30 minutes to prepare a mixed solution, standing at room temperature for one week, collecting a precipitate in the mixed solution, washing the precipitate with distilled water, and drying the precipitate to obtain carbon quantum dot powder;
b. b, mixing the carbon quantum dot powder prepared in the step a, ammonium dihydrogen phosphate and tellurium dioxide powder in an agate mortar, and uniformly grinding to obtain uniformly mixed powder;
c. b, placing the uniformly mixed powder obtained in the step b into a tubular furnace, heating to a calcination target temperature under the protection of nitrogen, and calcining the powder to obtain a calcined product;
d. and C, taking out the calcined product calcined in the step C, cooling to room temperature, washing with distilled water, and drying to obtain the Te-C nano composite material.
In a preferable embodiment of the present invention, in the step a, the volume ratio of the potassium hydroxide solution to the acetaldehyde solution is (1-5): 1.
In the step b, the mass ratio of the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder is 1 (5-10): (1-5). Further preferably, the mass ratio of the carbon quantum dot powder to the ammonium dihydrogen phosphate to the tellurium dioxide powder is 1:10: (1-3).
As a preferable technical scheme of the invention, in the step c, the calcination temperature is controlled to be 600-900 ℃; the calcination time is maintained at 1-3 h, and the temperature rising speed is controlled to be kept at 2-5 ℃/min. Further preferably controlling the calcining temperature to be 700-800 ℃; the calcination time is more preferably maintained at 2 to 3 hours.
As a preferred technical solution of the present invention, in the step d, the prepared Te-C nanocomposite is a tellurium nanoparticle composite material coated by ultrathin carbon nanosheets, wherein tellurium nanoparticles are bound in the shells of the ultrathin carbon nanosheets.
As a further preferable technical scheme of the invention, the prepared Te-C nano composite material is used for assembling a super capacitor: when the Te-C nano composite material is used as a positive electrode material, tellurium nano particles in the Te-C nano composite material generate oxidation-reduction reaction and form a pseudo capacitor; when the Te-C nano composite material is used as a negative electrode, the ultrathin carbon nano sheet forms an electric double layer capacitor.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the Te-C nano composite electrode material prepared by the method is simple to operate and low in cost, and can be used for obtaining the Te-C nano composite electrode material with excellent performance without complex equipment; the Te-C nano composite electrode material prepared by the method has higher specific capacitance, good rate capability and ultra-long cycle life;
2. the Te-C nano composite electrode material prepared by the method is used for constructing the super capacitor, and the obtained super capacitor has high energy density and power density and extraordinary cycling stability.
Drawings
Fig. 1 is an XRD pattern of the Te-C nanocomposite electrode material prepared by a method in an embodiment of the present invention.
Fig. 2 is an SEM image of the Te — C nanocomposite electrode material prepared by a method in an embodiment of the present invention.
Fig. 3 is a GCD diagram of the Te-C nanocomposite electrode material prepared by the method of the embodiment of the invention when used as the positive electrode of a supercapacitor.
Fig. 4 is a GCD diagram of the Te-C nanocomposite electrode material prepared by the method of the embodiment of the invention when used as a supercapacitor negative electrode.
Fig. 5 is a CV diagram of the Te-C nanocomposite electrode material prepared by the method of the embodiment of the invention in an electrochemical supercapacitor energy storage device.
Fig. 6 is a GCD diagram of the Te-C nanocomposite electrode material prepared by the method of the embodiment of the invention in an electrochemical supercapacitor energy storage device.
Fig. 7 is a cycle test chart of the Te-C nanocomposite electrode material prepared by the method of the embodiment of the invention in an electrochemical supercapacitor energy storage device.
Detailed Description
The foregoing aspects and many of the attendant advantages of this invention will become more readily appreciated as the same become better understood by reference to the following detailed description, when taken in conjunction with the accompanying drawings, wherein:
example one
In this embodiment, a method for preparing a Te-C nanocomposite for a supercapacitor includes the following steps:
a. under a normal condition, preparing a saturated aqueous solution of potassium hydroxide, slowly adding the saturated aqueous solution of potassium hydroxide into an acetaldehyde solution with the concentration of 40% (V/V), controlling the volume ratio of the potassium hydroxide solution to the acetaldehyde solution to be 5:1, stirring for 30min to prepare a mixed solution, standing for one week at room temperature, collecting a precipitate in the mixed solution, washing the precipitate with distilled water, and drying the precipitate to obtain carbon quantum dot powder;
b. mixing the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder in an agate mortar according to the mass ratio of the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder prepared in the step a being 1:10:1, and uniformly grinding to obtain uniformly mixed powder;
c. b, placing the uniformly mixed powder obtained in the step b into a tube furnace, heating to a calcination target temperature under the protection of nitrogen, calcining the powder, and controlling the calcination temperature to be 700 ℃; the calcination time is maintained at 2h, and the temperature rise speed is controlled to be kept at 5 ℃/min, so that a calcination product is obtained;
d. and C, taking out the calcined product calcined in the step C, cooling to room temperature, washing with distilled water, and drying to obtain the Te-C nano composite material.
Experimental test analysis:
the Te-C nanocomposite material prepared in this example was used as an electrode material for experimental test analysis, and a three-electrode system electrochemical test method was used: the electrochemical performance of Te-C was tested using Hg/HgO as a reference electrode, a platinum wire as a counter electrode, the Te-C nanocomposite prepared in this example as a working electrode, and 2M KOH solution as an electrolyte.
In addition, the two-electrode system electrochemical test method: the Te-C electrode prepared in the embodiment is respectively used as a positive electrode and a negative electrode, 2M KOH solution is used as electrolyte, an electrochemical super capacitor energy storage device is constructed, and electrochemical performance test is carried out.
In the present example, referring to fig. 1-7, fig. 1 is an XRD pattern of the Te-C nanocomposite electrode material prepared by the method of the present example, and a series of sharp diffraction peaks in fig. 1 prove that the Te nanoparticles have a higher crystallinity, indicating the successful preparation of the Te-C composite material. Fig. 2 is an SEM image of the Te — C nanocomposite electrode material prepared by the method of this example, and it can be seen from fig. 2 that the composite material is a two-dimensional sheet material with a porous structure. Fig. 3 is a GCD diagram of the Te-C nanocomposite electrode material prepared by the method of this embodiment when used as the positive electrode of a supercapacitor, and it can be known from fig. 3 that the composite material is a pseudocapacitance reaction mechanism when used as the positive electrode. Fig. 4 is a GCD diagram of the Te-C nanocomposite electrode material prepared by the method of this example when used as a supercapacitor negative electrode, and fig. 4 shows that the composite material is an electric double layer reaction mechanism when used as a negative electrode. Fig. 5 is a CV diagram of the Te-C nanocomposite electrode material prepared by the method of the present embodiment in an electrochemical supercapacitor energy storage device, and it can be known from fig. 5 that the composite material has higher electrochemical activity in the energy storage device. Fig. 6 is a GCD diagram of the Te-C nanocomposite electrode material prepared by the method of this embodiment in an electrochemical supercapacitor energy storage device, and it can be seen from fig. 6 that the energy storage device has a higher specific capacity. Fig. 7 is a cycle test chart of the Te-C nanocomposite electrode material prepared by the method of the present embodiment in an electrochemical supercapacitor energy storage device, and it can be seen from fig. 7 that the energy storage device has higher cycle stability.
In the method of the embodiment, the Te-C nano composite electrode material is prepared by pyrolyzing a powder mixture of carbon quantum dots and antimony dioxide and is used for assembling a super capacitor. When the Te-C nano composite electrode material is used as the anode, tellurium nano particles in the Te-C nano composite electrode material generate oxidation-reduction reaction and provide pseudo capacitance; when the Te-C nano composite electrode material is used as a negative electrode, the ultrathin carbon nano sheet provides electric double layer capacitance. Tellurium is the most metallic non-metallic material, and its excellent electrical conductivity helps to improve the structural stability of the material. After high-temperature calcination, tellurium nanoparticles are tightly bound in the shell of the ultrathin carbon nanosheet under an ion confinement mechanism, the circulation capacity of the tellurium nanoparticles is greatly improved, and the defect of short cycle life of the traditional chalcogenide is overcome. The preparation method of the embodiment is simple, low in cost and high in yield. The Te-C nano composite electrode material prepared by the method has higher specific capacitance and good cycling stability. The material is applied to the electrode of a super capacitor, and the energy density of the obtained super capacitor is 33.7Wh Kg-1The power density is 12kW Kg-1After 10000 charge-discharge cycles, the initial capacity can be retained by 94.8%. The Te-C nano composite electrode material prepared by the preparation method has higher specific capacitance, good rate capability and ultra-long cycle life. The material is used for constructing a super capacitor, and the obtained super capacitor has high energy density and power density and extraordinary cycle stability.
Example two
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a method for preparing a Te-C nanocomposite for a supercapacitor includes the following steps:
a. under a normal condition, preparing a saturated aqueous solution of potassium hydroxide, slowly adding the saturated aqueous solution of potassium hydroxide into an acetaldehyde solution with the concentration of 40% (V/V), controlling the volume ratio of the potassium hydroxide solution to the acetaldehyde solution to be 5:1, stirring for 30min to prepare a mixed solution, standing for one week at room temperature, collecting a precipitate in the mixed solution, washing the precipitate with distilled water, and drying the precipitate to obtain carbon quantum dot powder;
b. mixing the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder in an agate mortar according to the mass ratio of the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder prepared in the step a being 1:10:2, and uniformly grinding to obtain uniformly mixed powder;
c. b, placing the uniformly mixed powder obtained in the step b into a tube furnace, heating to a calcination target temperature under the protection of nitrogen, calcining the powder, and controlling the calcination temperature to be 700 ℃; the calcination time is maintained at 2h, and the temperature rise speed is controlled to be kept at 5 ℃/min, so that a calcination product is obtained;
d. and C, taking out the calcined product calcined in the step C, cooling to room temperature, washing with distilled water, and drying to obtain the Te-C nano composite material.
Experimental test analysis:
the Te-C nanocomposite material prepared in this example was used as an electrode material for experimental test analysis, and a three-electrode system electrochemical test method was used: the electrochemical performance of Te-C was tested using Hg/HgO as a reference electrode, a platinum wire as a counter electrode, the Te-C nanocomposite prepared in this example as a working electrode, and 2M KOH solution as an electrolyte.
In addition, the two-electrode system electrochemical test method: the Te-C electrode prepared in the embodiment is respectively used as a positive electrode and a negative electrode, 2M KOH solution is used as electrolyte, an electrochemical super capacitor energy storage device is constructed, and electrochemical performance test is carried out.
The Te-C nano composite electrode material prepared by the method has higher specific capacitance and good performanceThe cycle stability of (c). The material is applied to the electrode of a super capacitor, and the energy density of the obtained super capacitor is 30.5Wh Kg-1The power density is 10.8kW Kg-1After 10000 charge-discharge cycles, the initial capacity can be retained 91.7%. The Te-C composite electrode material of the tellurium nanoparticles coated by the ultrathin carbon nanosheets prepared by the method is used for assembling the supercapacitor, and when the Te-C composite electrode material is used as the anode, the tellurium nanoparticles in the Te-C composite electrode material are subjected to redox reaction and provide pseudo capacitance; when the Te-C composite electrode material is used as a negative electrode, the ultrathin carbon nanosheets provide electric double layer capacitance. The method of the embodiment prepares the Te-C nano composite electrode material by a calcination technology, is applied to the construction of the super capacitor, and has the advantages of high energy density, high power density, long cycle life and great application prospect.
EXAMPLE III
This embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a method for preparing a Te-C nanocomposite for a supercapacitor includes the following steps:
a. under a normal condition, preparing a saturated aqueous solution of potassium hydroxide, slowly adding the saturated aqueous solution of potassium hydroxide into an acetaldehyde solution with the concentration of 40% (V/V), controlling the volume ratio of the potassium hydroxide solution to the acetaldehyde solution to be 5:1, stirring for 30min to prepare a mixed solution, standing for one week at room temperature, collecting a precipitate in the mixed solution, washing the precipitate with distilled water, and drying the precipitate to obtain carbon quantum dot powder;
b. mixing the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder in an agate mortar according to the mass ratio of the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder prepared in the step a being 1:10:3, and uniformly grinding to obtain uniformly mixed powder;
c. b, placing the uniformly mixed powder obtained in the step b into a tube furnace, heating to a calcination target temperature under the protection of nitrogen, calcining the powder, and controlling the calcination temperature to be 700 ℃; the calcination time is maintained at 2h, and the temperature rise speed is controlled to be kept at 5 ℃/min, so that a calcination product is obtained;
d. and C, taking out the calcined product calcined in the step C, cooling to room temperature, washing with distilled water, and drying to obtain the Te-C nano composite material.
Experimental test analysis:
the Te-C nanocomposite material prepared in this example was used as an electrode material for experimental test analysis, and a three-electrode system electrochemical test method was used: the electrochemical performance of Te-C was tested using Hg/HgO as a reference electrode, a platinum wire as a counter electrode, the Te-C nanocomposite prepared in this example as a working electrode, and 2M KOH solution as an electrolyte.
In addition, the two-electrode system electrochemical test method: the Te-C electrode prepared in the embodiment is respectively used as a positive electrode and a negative electrode, 2M KOH solution is used as electrolyte, an electrochemical super capacitor energy storage device is constructed, and electrochemical performance test is carried out.
The Te-C nano composite electrode material prepared by the method has higher specific capacitance and good cycling stability. The material is applied to the electrode of a super capacitor, and the energy density of the obtained super capacitor is 29.8Wh Kg-1The power density is 10.2kW Kg-1After 10000 charge-discharge cycles, the initial capacity can be retained by 90.3%. The Te-C composite electrode material of the tellurium nanoparticles coated by the ultrathin carbon nanosheets prepared by the method is used for assembling the supercapacitor, and when the Te-C composite electrode material is used as the anode, the tellurium nanoparticles in the Te-C composite electrode material are subjected to redox reaction and provide pseudo capacitance; when the Te-C composite electrode material is used as a negative electrode, the ultrathin carbon nanosheets provide electric double layer capacitance. The method of the embodiment prepares the Te-C nano composite electrode material by a calcination technology, is applied to the construction of the super capacitor, and has the advantages of high energy density, high power density, long cycle life and great application prospect.
Example four
This embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a method for preparing a Te-C nanocomposite for a supercapacitor includes the following steps:
a. under a normal condition, preparing a saturated aqueous solution of potassium hydroxide, slowly adding the saturated aqueous solution of potassium hydroxide into an acetaldehyde solution with the concentration of 40% (V/V), controlling the volume ratio of the potassium hydroxide solution to the acetaldehyde solution to be 5:1, stirring for 30min to prepare a mixed solution, standing for one week at room temperature, collecting a precipitate in the mixed solution, washing the precipitate with distilled water, and drying the precipitate to obtain carbon quantum dot powder;
b. mixing the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder in an agate mortar according to the mass ratio of the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder prepared in the step a being 1:10:1, and uniformly grinding to obtain uniformly mixed powder;
c. b, placing the uniformly mixed powder obtained in the step b into a tube furnace, heating to a calcination target temperature under the protection of nitrogen, calcining the powder, and controlling the calcination temperature to be 800 ℃; the calcination time is maintained at 2h, and the temperature rise speed is controlled to be kept at 5 ℃/min, so that a calcination product is obtained;
d. and C, taking out the calcined product calcined in the step C, cooling to room temperature, washing with distilled water, and drying to obtain the Te-C nano composite material.
Experimental test analysis:
the Te-C nanocomposite material prepared in this example was used as an electrode material for experimental test analysis, and a three-electrode system electrochemical test method was used: the electrochemical performance of Te-C was tested using Hg/HgO as a reference electrode, a platinum wire as a counter electrode, the Te-C nanocomposite prepared in this example as a working electrode, and 2M KOH solution as an electrolyte.
In addition, the two-electrode system electrochemical test method: the Te-C electrode prepared in the embodiment is respectively used as a positive electrode and a negative electrode, 2M KOH solution is used as electrolyte, an electrochemical super capacitor energy storage device is constructed, and electrochemical performance test is carried out.
The Te-C nano composite electrode material prepared by the method has higher specific capacitance and good cycling stability. The material is applied to the electrode of a super capacitor, and the energy density of the obtained super capacitor is 31.9Wh Kg-1The power density is 11.1kW Kg-1After 10000 charge-discharge cycles, the initial capacity can be retained by 88.5%. The Te-C composite electrode material of the tellurium nanoparticles coated by the ultrathin carbon nanosheets prepared by the method is used for assembling the supercapacitor, and when the Te-C composite electrode material is used as the anode, the tellurium nanoparticles in the Te-C composite electrode material are subjected to redox reaction and provide pseudo capacitance; when the Te-C composite electrode material is used as a negative electrode, the ultrathin carbon nanosheets provide electric double layer capacitance. The method of the embodiment prepares the Te-C nano composite electrode material by a calcination technology, is applied to the construction of the super capacitor, and has the advantages of high energy density, high power density, long cycle life and great application prospect.
EXAMPLE five
This embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a method for preparing a Te-C nanocomposite for a supercapacitor includes the following steps:
a. under a normal condition, preparing a saturated aqueous solution of potassium hydroxide, slowly adding the saturated aqueous solution of potassium hydroxide into an acetaldehyde solution with the concentration of 40% (V/V), controlling the volume ratio of the potassium hydroxide solution to the acetaldehyde solution to be 5:1, stirring for 30min to prepare a mixed solution, standing for one week at room temperature, collecting a precipitate in the mixed solution, washing the precipitate with distilled water, and drying the precipitate to obtain carbon quantum dot powder;
b. mixing the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder in an agate mortar according to the mass ratio of the carbon quantum dot powder, the ammonium dihydrogen phosphate and the tellurium dioxide powder prepared in the step a being 1:10:2, and uniformly grinding to obtain uniformly mixed powder;
c. b, placing the uniformly mixed powder obtained in the step b into a tube furnace, heating to a calcination target temperature under the protection of nitrogen, calcining the powder, and controlling the calcination temperature to be 800 ℃; the calcination time is maintained at 2h, and the temperature rise speed is controlled to be kept at 5 ℃/min, so that a calcination product is obtained;
d. and C, taking out the calcined product calcined in the step C, cooling to room temperature, washing with distilled water, and drying to obtain the Te-C nano composite material.
Experimental test analysis:
the Te-C nanocomposite material prepared in this example was used as an electrode material for experimental test analysis, and a three-electrode system electrochemical test method was used: the electrochemical performance of Te-C was tested using Hg/HgO as a reference electrode, a platinum wire as a counter electrode, the Te-C nanocomposite prepared in this example as a working electrode, and 2M KOH solution as an electrolyte.
In addition, the two-electrode system electrochemical test method: the Te-C electrode prepared in the embodiment is respectively used as a positive electrode and a negative electrode, 2M KOH solution is used as electrolyte, an electrochemical super capacitor energy storage device is constructed, and electrochemical performance test is carried out.
The Te-C nano composite electrode material prepared by the method has higher specific capacitance and good cycling stability. The material is applied to the electrode of a super capacitor, and the energy density of the obtained super capacitor is 26.9Wh Kg-1The power density is 8.3kW Kg-1After 10000 charge-discharge cycles, the initial capacity can be retained by 85.2%. The Te-C composite electrode material of the tellurium nanoparticles coated by the ultrathin carbon nanosheets prepared by the method is used for assembling the supercapacitor, and when the Te-C composite electrode material is used as the anode, the tellurium nanoparticles in the Te-C composite electrode material are subjected to redox reaction and provide pseudo capacitance; when the Te-C composite electrode material is used as a negative electrode, the ultrathin carbon nanosheets provide electric double layer capacitance. The method prepares the Te-C nano-composite electrode material by a calcination technology, is applied to the construction of the super capacitor, and constructs the super capacitorThe stage capacitor has high energy density, large power density and long cycle life, and has great application prospect.
While the embodiments of the present invention have been described with reference to the accompanying drawings, the present invention is not limited to the above embodiments, and various changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention should be replaced by equivalents thereof, so long as the objects of the present invention are met, and the present invention is within the protection scope of the present invention without departing from the technical principle and inventive concept of the method for preparing Te — C nanocomposite for a supercapacitor according to the present invention.
Claims (7)
1. A preparation method of Te-C nano composite material applied to a super capacitor is characterized by comprising the following steps:
a. under a normal condition, preparing a saturated aqueous solution of potassium hydroxide, slowly adding the saturated aqueous solution of potassium hydroxide into an acetaldehyde solution with the concentration of 40% (V/V), stirring for at least 30 minutes to prepare a mixed solution, standing at room temperature for one week, collecting a precipitate in the mixed solution, washing the precipitate with distilled water, and drying the precipitate to obtain carbon quantum dot powder;
b. b, mixing the carbon quantum dot powder prepared in the step a, ammonium dihydrogen phosphate and tellurium dioxide powder in an agate mortar, and uniformly grinding to obtain uniformly mixed powder;
c. b, placing the uniformly mixed powder obtained in the step b into a tubular furnace, heating to a calcination target temperature under the protection of nitrogen, and calcining the powder to obtain a calcined product;
d. c, taking out the calcined product calcined in the step C, cooling to room temperature, washing with distilled water, and drying to obtain the Te-C nano composite material; the prepared Te-C nano composite material is a tellurium nano particle composite material coated by ultrathin carbon nano sheets, wherein tellurium nano particles are bound in the shells of the ultrathin carbon nano sheets.
2. The method for preparing Te-C nanocomposite for application in supercapacitors as claimed in claim 1, wherein: in the step a, the volume ratio of the potassium hydroxide solution to the acetaldehyde solution is (1-5): 1.
3. The method for preparing Te-C nanocomposite for application in supercapacitors as claimed in claim 1, wherein: in the step b, the mass ratio of the carbon quantum dot powder to the ammonium dihydrogen phosphate to the tellurium dioxide powder is 1 (5-10): (1-5).
4. The method for preparing Te-C nanocomposite for application in supercapacitors as claimed in claim 3, wherein: in the step b, the mass ratio of the carbon quantum dot powder to the ammonium dihydrogen phosphate to the tellurium dioxide powder is 1:10: (1-3).
5. The method for preparing Te-C nanocomposite for application in supercapacitors as claimed in claim 1, wherein: in the step c, the calcining temperature is controlled to be 600-900 ℃; the calcination time is maintained at 1-3 h, and the temperature rising speed is controlled to be kept at 2-5 ℃/min.
6. The method for preparing Te-C nanocomposite for application in supercapacitors according to claim 5, wherein: in the step c, the calcining temperature is controlled to be 700-800 ℃; the calcination time is maintained at 2-3 h.
7. The method for preparing a Te-C nanocomposite for application to a supercapacitor according to claim 1, wherein the Te-C nanocomposite prepared is used for the assembly of a supercapacitor:
when the Te-C nano composite material is used as a positive electrode material, tellurium nano particles in the Te-C nano composite material generate oxidation-reduction reaction and form a pseudo capacitor;
when the Te-C nano composite material is used as a negative electrode, the ultrathin carbon nano sheet forms an electric double layer capacitor.
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