CN115440509B - Preparation method of array type nickel cobalt nitrogen nanosheet/carbon felt for super capacitor - Google Patents
Preparation method of array type nickel cobalt nitrogen nanosheet/carbon felt for super capacitor Download PDFInfo
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- CN115440509B CN115440509B CN202211086532.2A CN202211086532A CN115440509B CN 115440509 B CN115440509 B CN 115440509B CN 202211086532 A CN202211086532 A CN 202211086532A CN 115440509 B CN115440509 B CN 115440509B
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- carbon felt
- array type
- cobalt
- nitrogen
- electrode
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 46
- RMKJDGIKQWEFFT-UHFFFAOYSA-N [N].[Co].[Ni] Chemical compound [N].[Co].[Ni] RMKJDGIKQWEFFT-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000002135 nanosheet Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000003990 capacitor Substances 0.000 title abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 16
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims abstract description 10
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims description 15
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000007772 electrode material Substances 0.000 abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 3
- 229910017052 cobalt Inorganic materials 0.000 abstract description 2
- 239000010941 cobalt Substances 0.000 abstract description 2
- 238000004070 electrodeposition Methods 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 229910052757 nitrogen Inorganic materials 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 150000004767 nitrides Chemical class 0.000 description 4
- -1 transition metal nitrides Chemical class 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003623 transition metal compounds Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
Abstract
The preparation process of array type nanometer nickel-cobalt-nitrogen sheet/carbon felt for super capacitor belongs to the field of super capacitor electrode material, and the nanometer material has sheet array structure growing on the surface of the carbon felt. The array type nickel cobalt nitrogen nano material adopts a synthesis method of electrodeposition and ammonia nitridation, takes a pretreated carbon felt as a substrate, nickel chloride hexahydrate as a nickel source, cobalt chloride hexahydrate as a cobalt source and ammonia as a nitrogen source, and the prepared nickel cobalt nitrogen nano sheet uniformly and vertically grows on the surface of the carbon felt. When the electrode is directly used as an electrode of a super capacitor, the three-electrode test shows that the specific capacity is 21710F/m 2 when the current density is 3A/m 2. The array type nickel-cobalt-nitrogen nanosheet/carbon felt prepared by the invention has the characteristics of high specific capacity, simple preparation method, low cost and the like.
Description
Technical Field
A preparation method of an array type nickel cobalt nitrogen nanosheet/carbon felt for a supercapacitor belongs to the field of supercapacitor electrode materials.
Technical Field
With the rise of the consumption and price of the traditional energy sources (such as petroleum, coal, natural gas and the like), the cost of daily production and life is increased and the environmental problem is increasingly highlighted, so that people are urgently required to develop green new energy sources (such as solar energy, wind energy and the like) and novel energy storage devices. The super capacitor is used as one of novel energy storage devices, has the characteristics of high power density, short charge and discharge time, long service life, wide applicable temperature range, safety and the like, and is widely applied to intelligent power grid systems, industrial energy-saving systems, power supply systems and numerous electronic equipment. Therefore, the super capacitor becomes one of hot research directions of the novel energy storage device. Wherein the electrode material is one of the main factors affecting the performance of the supercapacitor.
The transition metal compound has higher theoretical specific capacity, so that the transition metal compound is one of hot spot directions of the pseudo-capacitance electrode materials in research at present. Compared with the transition metal oxide, the metal nitride has higher conductivity, is more beneficial to realizing the improvement of the energy density of the super capacitor and ensures higher power density, but the conductivity of the existing metal nitride still cannot meet the requirement. In order to improve the conductivity of transition metal nitrides, most of the prior art is based on single metal nitride/carbon composites, whereas bimetallic nitride/carbon composites have been reported to a lesser extent and the composites produced are based on powders. In addition, although both the carbon nanotubes and the graphene can improve the conductivity, the cost is high, and the commercialized application is not facilitated. In contrast, commercial graphite carbon felts not only have higher conductivity, but also have larger specific surface area, and are also relatively low-priced, especially the self-supporting array type nickel cobalt nitride/carbon felt composite materials are less reported.
Disclosure of Invention
The invention provides a method with low cost, simple preparation process, short period and simple operation, which successfully prepares the self-supported array type nickel cobalt nitrogen nano-sheet/carbon felt composite by using a synthesis method of electrodeposition and ammonia nitriding, and the self-supported array type nickel cobalt nitrogen nano-sheet/carbon felt composite shows good electrochemical performance when being directly used as an electrode of a supercapacitor.
The invention provides a preparation method of a self-supporting array type nickel cobalt nitrogen nanosheet/carbon felt for a supercapacitor, which comprises the following steps:
a) Placing a carbon felt with the thickness of 3mm into a plasma cleaning machine, setting the power to 80W under the air atmosphere condition, and shearing the carbon felt into a shape with the length and the width of 2 x 1cm for later use after 5min of treatment;
b) Adding deionized water, nickel chloride hexahydrate, cobalt chloride hexahydrate and thiourea into a 100mL beaker, and stirring for 10min for later use;
c) Placing the beaker with the precursor liquid in the b into a water bath kettle with a certain temperature, simultaneously connecting the sheared carbon felt in the a into a working electrode, respectively taking a foil and a saturated calomel electrode as a counter electrode and a reference electrode to form three electrodes together, then placing the three electrodes into the precursor liquid, and then taking out the carbon felt after depositing for a period of time under a specific voltage, and washing and drying the carbon felt;
d) And c, placing the carbon felt after drying in the step c in a porcelain boat, transferring the porcelain boat into a tube furnace, heating to a preset temperature, carrying out heat preservation treatment for a period of time in an ammonia atmosphere, and cooling to room temperature along with the furnace to obtain the self-supporting array type nickel cobalt nitrogen nano sheet/carbon felt composite material.
E) The self-supporting array type nickel cobalt nitrogen nano sheet/carbon felt composite material is directly used as an electrode to be applied to a super capacitor.
The addition amounts of deionized water, nickel chloride hexahydrate, cobalt chloride hexahydrate and thiourea in the step b) are respectively 80ml, 0.08mmol, 0.16mmol and 1.6mmol;
the step c) is carried out for 9min when the deposition voltage is-0.8V at the water bath temperature of 40 ℃;
In the step d), under the ammonia atmosphere, the temperature is increased from room temperature to 420 ℃ at a speed of 8 ℃/min, and the heat is preserved for 3 hours;
in the three-electrode performance test of the super capacitor, the electrolyte is 1mol/L sodium hydroxide solution, and the specific capacity of the electrode is 21710F/m 2 when the current density is 3A/m 2.
Compared with other methods for preparing nickel cobalt nitrogen/carbon composite materials, the method has the advantages that firstly, the array type nickel cobalt nitrogen nanosheets are prepared on the surface of the commercial carbon felt, in addition, the preparation process is simple, the raw materials are cheap and easy to obtain, the method is suitable for large-scale production, the production cost is reduced, and the production period is shortened; and can be directly used as an electrode of a super capacitor, and has better specific capacity.
A Bruker Advance D8X-ray powder diffractometer (Cu ka radiation,2 Θ=10 to 80°) the structure of the prepared material was determined. The surface morphology of the prepared material was observed using a Hitachi S-4800 scanning electron microscope. The test for superelectrical performance was performed using an electrochemical workstation (CHI 660E).
As can be seen from curve 1 of FIG. 1, when the addition amount of nickel chloride hexahydrate is 0.24mmol and the addition amount of cobalt chloride hexahydrate is 0, the prepared material is a nickel nitride/carbon felt composite material (JCPLDS card No. 10-0280); as can be seen from curve 3 of FIG. 1, when the addition amount of nickel chloride hexahydrate is 0 and the addition amount of cobalt chloride hexahydrate is 0.24mmol, the prepared material is a cobalt nitride/carbon felt composite material (JCPLDS card No. 06-0647); as can be seen from the graph 2 of FIG. 1 and the graph 2, when the addition amount of the nickel chloride hexahydrate is 0.08mmol and the addition amount of the cobalt chloride hexahydrate is 0.16mmol, the prepared material is a nickel cobalt nitrogen/carbon felt composite material. As can be seen from fig. 3, the obtained product nickel cobalt nitrogen is mainly in a plate structure, and grows on the surface of the carbon felt in an array state, but the sizes of the nano plates are different. As can be seen from FIG. 4, when the self-supporting array type nickel cobalt nitrogen nano-sheet/carbon felt composite material is used as an electrode of a super capacitor for cyclic voltammetry test, the area of a CV curve is increased along with the increase of the sweeping speed from 2mV/s to 20mV/s, and the peak position is also shifted. As is clear from FIG. 5, the specific capacity of the electrode was 21710F/m 2 at a current density of 3A/m 2.
Drawings
FIG. 1 is an X-ray diffraction pattern of the resulting product at a molar ratio of nickel chloride hexahydrate to cobalt chloride hexahydrate of 0.24/0 (1), 0.08/0.16 (2) and 0/0.24 (3), respectively.
FIG. 2 is an X-ray diffraction pattern of the three products of FIG. 1
FIG. 3 is a scanning electron microscope image of the product.
FIG. 4 is a CV plot of a self-supporting array type nickel cobalt nitrogen nanoplatelet/carbon felt composite material made in accordance with an embodiment.
Fig. 5 is a charge-discharge graph of a self-supporting array type nickel cobalt nitrogen nanoplatelet/carbon felt composite material prepared according to an embodiment.
Detailed Description
1. Placing a carbon felt with the length of 10cm and the width of 5cm and the thickness of 3mm into a plasma cleaning machine, setting the power to 80W, treating for 5min under the air atmosphere condition, taking out, and shearing the carbon felt into a shape with the length of 2 x 1cm for later use;
2. 80mL of deionized water, 0.08mmol of nickel chloride hexahydrate, 0.16mmol of cobalt chloride hexahydrate and 1.6mmol of thiourea are added into a 100mL beaker in sequence, and the mixture is stirred for 10 minutes for later use;
3. Placing a beaker filled with 80ml of precursor liquid in a water bath kettle at 40 ℃, simultaneously connecting a sheared carbon felt into a working electrode, connecting a foil and a saturated calomel electrode into a counter electrode and a reference electrode circuit respectively to form three electrodes together, placing the three electrodes into the precursor liquid, then depositing for 8min at a voltage of-0.8V, taking out the carbon felt, and washing and drying the carbon felt;
4. and then placing the dried carbon felt in a porcelain boat, transferring the porcelain boat into a tube furnace, and carrying out heat preservation treatment for 3 hours at a heating rate of 8 ℃/min from room temperature to 420 ℃ in an ammonia atmosphere, and cooling the porcelain boat to room temperature along with the furnace to obtain the self-supporting array type nickel-cobalt-nitrogen nanosheet/carbon felt composite material (see figures 1,2 and 3).
Claims (2)
1. The preparation method of the array type nickel cobalt nitrogen nanosheet/carbon felt for the supercapacitor comprises the following steps:
a) Placing a carbon felt with the thickness of 3mm into a plasma cleaning machine, setting the power to 80W under the air atmosphere condition, and shearing the carbon felt into a shape with the length and the width of 2 x 1cm for later use after 5min of treatment;
b) Adding deionized water, nickel chloride hexahydrate, cobalt chloride hexahydrate and thiourea into a 100mL beaker, and stirring for 10min for later use;
c) Placing the beaker with the precursor liquid in the b into a water bath kettle with a certain temperature, simultaneously connecting the sheared carbon felt in the a into a working electrode, respectively taking a foil and a saturated calomel electrode as a counter electrode and a reference electrode to form three electrodes together, then placing the three electrodes into the precursor liquid, and then taking out the carbon felt after depositing for a period of time under a specific voltage, and washing and drying the carbon felt;
d) Transferring the carbon felt after drying in the step c into a porcelain boat, placing the porcelain boat into a tube furnace, heating to a preset temperature, carrying out heat preservation treatment for a period of time in an ammonia atmosphere, and cooling to room temperature along with the furnace to obtain a self-supporting array type nickel cobalt nitrogen nanosheet/carbon felt composite material;
the step c) is carried out for 9min when the deposition voltage is-0.8V at the water bath temperature of 40 ℃;
in the step d), the temperature is increased from room temperature to 420 ℃ at a speed of 8 ℃/min under the ammonia atmosphere, and the heat is preserved for 3 hours.
2. The method for preparing the array type nickel cobalt nitrogen nanosheet/carbon felt for the supercapacitor according to claim 1, wherein the addition amounts of deionized water, nickel chloride hexahydrate, cobalt chloride hexahydrate and thiourea in the step b) are 80ml, 0.08mmol, 0.16mmol and 1.6mmol respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211086532.2A CN115440509B (en) | 2022-08-26 | 2022-08-26 | Preparation method of array type nickel cobalt nitrogen nanosheet/carbon felt for super capacitor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211086532.2A CN115440509B (en) | 2022-08-26 | 2022-08-26 | Preparation method of array type nickel cobalt nitrogen nanosheet/carbon felt for super capacitor |
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| Publication Number | Publication Date |
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| CN115440509A CN115440509A (en) | 2022-12-06 |
| CN115440509B true CN115440509B (en) | 2024-04-30 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642304A (en) * | 2019-10-09 | 2020-01-03 | 上海师范大学 | Trimetal nitride material for super capacitor and preparation method thereof |
| CN113270274A (en) * | 2021-04-23 | 2021-08-17 | 中国科学院合肥物质科学研究院 | Flexible honeycomb-shaped bimetal nitride supercapacitor electrode and preparation method thereof |
| CN113410062A (en) * | 2021-06-17 | 2021-09-17 | 大连理工大学 | Carbon nanocoil stack/nickel-cobalt compound supercapacitor composite electrode material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7147966B2 (en) * | 2001-11-30 | 2006-12-12 | The Trustees Of Boston College | Coated carbon nanotube array electrodes |
| US10680300B2 (en) * | 2016-09-19 | 2020-06-09 | Sparkle Power Llc | Supercapattery employing carbon nanosheets in the electrodes |
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- 2022-08-26 CN CN202211086532.2A patent/CN115440509B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642304A (en) * | 2019-10-09 | 2020-01-03 | 上海师范大学 | Trimetal nitride material for super capacitor and preparation method thereof |
| CN113270274A (en) * | 2021-04-23 | 2021-08-17 | 中国科学院合肥物质科学研究院 | Flexible honeycomb-shaped bimetal nitride supercapacitor electrode and preparation method thereof |
| CN113410062A (en) * | 2021-06-17 | 2021-09-17 | 大连理工大学 | Carbon nanocoil stack/nickel-cobalt compound supercapacitor composite electrode material and preparation method thereof |
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