CN111755261A - Preparation method of silver nanowire doped nano carbon ball electrode material - Google Patents
Preparation method of silver nanowire doped nano carbon ball electrode material Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 47
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 34
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 21
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 18
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- 229910001961 silver nitrate Inorganic materials 0.000 claims description 9
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 8
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- 238000009210 therapy by ultrasound Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/152—Fullerenes
- C01B32/154—Preparation
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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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- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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Abstract
A preparation method of a silver-doped nanowire nano carbon sphere electrode material comprises the following steps: the method comprises the following steps: preparing to obtain a nano polymer ball; step two: preparing the silver-doped nano polymer ball; step three: and (3) placing the silver nanowire-doped nano polymer ball in a tubular furnace, heating to 300 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, heating to 600 ℃ at a heating rate of 15 ℃/min, preserving heat at 600 ℃ for 2h, and cooling to room temperature to obtain the silver nanowire-doped nano carbon ball electrode material. The invention discloses a silver nanowire-doped nano carbon sphere electrode material, which overcomes the defect of large resistance of the traditional electrode material, and wraps silver nanowires in nano carbon spheres to enable the silver nanowires to interact with silver ions loaded on the nano carbon spheres, so that the capacitance of the silver nanowire-doped nano carbon sphere electrode material can be increased.
Description
Technical Field
The invention belongs to the field of electrode material preparation, and particularly relates to a preparation method of a silver nanowire doped carbon nanosphere electrode material.
Background
Supercapacitors, also known as electrochemical capacitors, are new types of energy storage devices with properties intermediate between batteries and electrostatic capacitors. The research core of the supercapacitor is mainly focused on the research of electrode materials.
Carbon materials, as an important electrode material, can be used either directly as an electrode material or as a further composite substrate or doped "backbone". The compounded or doped electrode material has higher capacitance value and energy density compared with the original carbon electrode material. The doped carbon material can also keep good cycling stability, which is an important performance index of the electrode material.
The nanometer material attracts the attention of many researchers due to the unique quantum size effect, small size effect, macroscopic quantum tunneling effect and the like. Metal nanomaterials are used in a variety of fields due to their unique photoelectric and chemical properties. Li et al proposed a new structured catalyst in 2017 with platinum nanoparticles partially embedded in resorcinol-formaldehyde carbon spheres (Pt @ RFC) towards MORs. Pt @ RFC has good compatibility and MOR activity, wherein the negative migration of CO electrooxidation peak potential is about 150mv, and the electrocatalytic activity is 2 times that of commercial Pt/C. It is worth noting that the mass activity of Pt @ RFC is well maintained after 3000 times of cyclic voltammetry accelerated degradation, which is 5.8 times that of commercial Pt/C.
Among the materials for preparing the conventional super capacitor, the carbon material is the most widely studied electrode material due to its wide source, low cost and various forms, such as: carbon nanotubes, graphene, activated carbon, and the like. However, most carbon electrode materials are relatively poorly conductive, which can lead to poor rate performance of the device. Therefore, an electrode with good conductivity is a basis for preparing a high-performance supercapacitor. In order to improve the conductivity of the carbon film, the conductive carbon black is added conventionally, but the high proportion of the conductive carbon black reduces the quality and the specific surface area of the carbon film, and the sheet resistance of the carbon film is still relatively high. Patent application CN107452515A discloses a slurry prepared based on binder, silver nanowire conductive agent and active material, which is prepared into electrode sheets by using nickel foam as current collector through rolling or coating transfer process, and then cut into electrode sheets to form super capacitors. However, this method requires the addition of a large amount of silver nanowires to lower the equivalent resistance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a nano carbon sphere electrode material doped with silver nanowires.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of a silver-doped nanowire nano carbon sphere electrode material comprises the following steps:
the method comprises the following steps: adding a resorcinol aqueous solution, a low-polymerization-degree paraformaldehyde aqueous solution and a sodium hydroxide solution into a reactor, stirring and mixing, heating to a certain temperature to obtain a low-molecular-weight phenolic resin prepolymer, then adding ammonia water, heating to 100 ℃, polymerizing for 24 hours, washing the obtained resin microspheres with deionized water after the reaction is finished, and drying for 5 hours in a constant-temperature drying oven at 120 ℃ to obtain nano polymer spheres;
step two: adding the nano polymer spheres into ethanol to form a mixture of 20-50mg/L, then adding silver nanowires of which the mass is 2-5% of that of the nano polymer spheres, adding a silver nitrate solution, performing ultrasound for 15min at normal temperature, then placing the mixture at 70 ℃ for condensation reflux reaction for 12 hours, and performing water washing and ethanol leaching for 3-5 times, and then performing vacuum drying to obtain the silver nanowire-doped nano polymer spheres;
step three: the nano polymer ball doped with the silver nanowires is placed in a tubular furnace, is heated to 300 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, is heated to 600 ℃ at a heating rate of 15 ℃/min, and is subjected to heat preservation at 600 ℃ for 2 h. And cooling to room temperature to obtain the silver nanowire doped carbon nanosphere electrode material.
Preferably, the concentration of the resorcinol aqueous solution in the step one is 0.05-0.10mol/L, the concentration of the sodium hydroxide solution is 0.1mol/L, the concentration of the ammonia water is 0.05-0.1mol/L, and the mass concentration of the paraformaldehyde aqueous solution with low polymerization degree is 280-380 g/L.
Preferably, the heating temperature of the phenolic resin prepolymer with low molecular weight obtained by heating in the step one is 40 ℃.
Preferably, in the second step, the concentration of the silver nitrate solution is 0.01-0.05mol/L, and the ultrasonic power is 150-200W.
The invention has the following beneficial effects:
the invention discloses a nano carbon sphere electrode material doped with silver nanowires, which overcomes the defect of large resistance of the traditional electrode material, and the silver nanowires are compounded into nano carbon spheres, so that the silver nanowires interact with silver ions loaded on the nano carbon spheres, and the capacitance of the nano carbon sphere electrode material doped with the silver nanowires can be increased. The nano carbon ball electrode material doped with the silver nanowires has a large specific surface area, and is beneficial to the transmission of electron ions. The preparation method disclosed by the invention is simple, the prepared electrode material is low in resistivity, high specific capacitance is provided for the supercapacitor material, the operation is easy, the equipment requirement is low, and the preparation method has a good application prospect.
Drawings
FIG. 1 is a scanning electron microscope photograph of the silver nanowire-doped nanocarbon sphere electrode material obtained in example 1;
fig. 2 is a cyclic voltammogram of a symmetrical capacitor assembled by using the silver-doped nanowire carbon nanosphere electrode material obtained in example 1 under different voltage windows.
Detailed Description
In the invention, the silver nanowires can be prepared by adopting the method in the prior art.
Example 1
A preparation method of a silver-doped nanowire nano carbon sphere electrode material comprises the following steps:
the method comprises the following steps: adding 50mL of 0.05mol/L resorcinol aqueous solution and 20mL of 0.1mol/L sodium hydroxide solution into a reactor, stirring and mixing the resorcinol aqueous solution and the sodium hydroxide solution, heating the mixture to 40 ℃ to obtain a low-molecular-weight phenolic resin prepolymer, then adding 20mL of 0.05mol/L ammonia water, heating the mixture to 100 ℃ for polymerization for 24 hours, washing the obtained resin microspheres with deionized water after the reaction is finished, and drying the resin microspheres in a constant-temperature drying oven at 120 ℃ for 5 hours to obtain nano polymer spheres;
step two: adding the nano polymer ball into ethanol to form a mixture of 20mg/L, then adding silver nanowires of 2% of the mass of the nano polymer ball, adding 20mL of 0.01mol/L silver nitrate solution, performing ultrasonic treatment at normal temperature with ultrasonic power of 150W for 15min, then placing the mixture at 70 ℃ for condensation reflux reaction for 12 hours, washing with water for 3-5 times, rinsing with ethanol, and performing vacuum drying to obtain the silver nanowire-doped nano polymer ball;
step three: the nano polymer ball doped with the silver nanowires is placed in a tubular furnace, is heated to 300 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, is heated to 600 ℃ at a heating rate of 15 ℃/min, and is subjected to heat preservation at 600 ℃ for 2 h. And cooling to room temperature to obtain the silver nanowire doped carbon nanosphere electrode material.
Example 2
A preparation method of a silver-doped nanowire nano carbon sphere electrode material comprises the following steps:
the method comprises the following steps: adding 50mL of 0.06mol/L resorcinol aqueous solution and 20mL of 0.1mol/L sodium hydroxide solution into a reactor, adding 85g/L low-polymerization-degree paraformaldehyde aqueous solution, stirring, mixing, heating to 40 ℃ to obtain a low-molecular-weight phenolic resin prepolymer, then adding 20mL of 0.06mol/L ammonia water, heating to 100 ℃ for polymerization for 24 hours, washing the obtained resin microspheres with deionized water after the reaction is finished, and drying in a constant-temperature drying oven at 120 ℃ for 5 hours to obtain nano polymer spheres;
step two: adding the nano polymer ball into ethanol to form a mixture of 20mg/L, then adding silver nanowires of 2% of the mass of the nano polymer ball, adding 20mL of 0.02mol/L silver nitrate solution, performing ultrasonic treatment at normal temperature with ultrasonic power of 160W for 15min, then placing the mixture at 70 ℃ for condensation reflux reaction for 12 hours, washing with water for 3-5 times, rinsing with ethanol, and performing vacuum drying to obtain the silver nanowire-doped nano polymer ball;
step three: the nano polymer ball doped with the silver nanowires is placed in a tubular furnace, is heated to 300 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, is heated to 600 ℃ at a heating rate of 15 ℃/min, and is subjected to heat preservation at 600 ℃ for 2 h. And cooling to room temperature to obtain the silver nanowire doped carbon nanosphere electrode material.
Example 3
A preparation method of a silver-doped nanowire nano carbon sphere electrode material comprises the following steps:
the method comprises the following steps: adding 50mL of 0.07mol/L resorcinol aqueous solution and 20mL of 0.1mol/L sodium hydroxide solution into a reactor, adding 90g/L low-polymerization-degree paraformaldehyde aqueous solution, stirring, mixing, heating to 40 ℃ to obtain a low-molecular-weight phenolic resin prepolymer, adding 20mL of 0.06mol/L ammonia water, heating to 100 ℃ for polymerization for 24 hours, washing the obtained resin microspheres with deionized water after the reaction is finished, and drying in a constant-temperature drying oven at 120 ℃ for 5 hours to obtain nano polymer spheres;
step two: adding the nano polymer ball into ethanol to form a mixture of 20mg/L, then adding silver nanowires of 2% of the mass of the nano polymer ball, adding 20mL of 0.03mol/L silver nitrate solution, performing ultrasonic treatment at the ultrasonic power of 170W for 15min at normal temperature, then placing the mixture at 70 ℃ for condensation reflux reaction for 12 hours, washing with water for 3-5 times, rinsing with ethanol, and performing vacuum drying to obtain the silver nanowire-doped nano polymer ball;
step three: the nano polymer ball doped with the silver nanowires is placed in a tubular furnace, is heated to 300 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, is heated to 600 ℃ at a heating rate of 15 ℃/min, and is subjected to heat preservation at 600 ℃ for 2 h. And cooling to room temperature to obtain the silver nanowire doped carbon nanosphere electrode material.
Example 4
A preparation method of a silver-doped nanowire nano carbon sphere electrode material comprises the following steps:
the method comprises the following steps: adding 50mL of 0.08mol/L resorcinol aqueous solution and 20mL of 0.1mol/L sodium hydroxide solution into a reactor, adding 95g/L low-polymerization-degree paraformaldehyde, stirring, mixing, heating to 40 ℃ to obtain a low-molecular-weight phenolic resin prepolymer, then adding 20mL of 0.08mol/L ammonia water, heating to 100 ℃ for polymerization for 24 hours, washing the obtained resin microspheres with deionized water after the reaction is finished, and drying in a constant-temperature drying oven at 120 ℃ for 5 hours to obtain the nano polymer spheres;
step two: adding the nano polymer ball into ethanol to form a mixture of 20mg/L, then adding silver nanowires of 2% of the mass of the nano polymer ball, adding 2mL of 0.04mol/L silver nitrate solution, performing ultrasonic treatment at normal temperature with ultrasonic power of 180W for 15min, then placing the mixture at 70 ℃ for condensation reflux reaction for 12 hours, washing with water for 3-5 times, rinsing with ethanol, and performing vacuum drying to obtain the silver nanowire-doped nano polymer ball;
step three: the nano polymer ball doped with the silver nanowires is placed in a tubular furnace, is heated to 300 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, is heated to 600 ℃ at a heating rate of 15 ℃/min, and is subjected to heat preservation at 600 ℃ for 2 h. And cooling to room temperature to obtain the silver nanowire doped carbon nanosphere electrode material.
Example 5
A preparation method of a silver-doped nanowire nano carbon sphere electrode material comprises the following steps:
the method comprises the following steps: adding 50mL of 0.10mol/L resorcinol aqueous solution and 20mL of 0.1mol/L sodium hydroxide solution into a reactor, adding 100g/L low-polymerization-degree paraformaldehyde aqueous solution, stirring and mixing, heating to 40 ℃ to obtain a low-molecular-weight phenolic resin prepolymer, then adding 20mL of 0.10mol/L ammonia water, heating to 100 ℃ for polymerization for 24 hours, washing the obtained resin microspheres with deionized water after the reaction is finished, and drying in a constant-temperature drying oven at 120 ℃ for 5 hours to obtain nano polymer spheres;
step two: adding the nano polymer ball into ethanol to form a mixture of 20mg/L, then adding silver nanowires of 2% of the mass of the nano polymer ball, adding 20mL of 0.05mol/L silver nitrate solution, performing ultrasonic treatment at normal temperature with ultrasonic power of 200W for 15min, then placing the mixture at 70 ℃ for condensation reflux reaction for 12 hours, washing with water for 3-5 times, rinsing with ethanol, and performing vacuum drying to obtain the silver nanowire-doped nano polymer ball;
step three: the nano polymer ball doped with the silver nanowires is placed in a tubular furnace, is heated to 300 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, is heated to 600 ℃ at a heating rate of 15 ℃/min, and is subjected to heat preservation at 600 ℃ for 2 h. And cooling to room temperature to obtain the silver nanowire doped carbon nanosphere electrode material.
And (3) electrochemical performance testing:
weighing the silver nanowire-doped carbon nanosphere electrode material obtained in the example 1-5, acetylene black and Polytetrafluoroethylene (PTFE) according to the mass ratio of 8:1:1, placing the mixture in an agate mortar, dropwise adding ethanol in a proper amount, and uniformly grinding; coating the nickel-base alloy on foamed nickel, drying the nickel-base alloy for 2 hours at 50 ℃ in a drying oven, taking out a pole piece, rolling the pole piece on a roller press, continuously drying the pole piece for 1 hour at 50 ℃, and using a punching sheet of a button cell punching machine as a button super capacitor electrode; assembling a symmetrical super capacitor by using the obtained pole pieces, wherein a polypropylene microporous membrane is used as a diaphragm, and 6mol/L KOH solution is used as electrolyte; and standing for 24h, and testing the electrochemical performance. The results are shown in Table 1. And the cyclic voltammetry of the symmetrical capacitor assembled by the silver nanowire doped nanocarbon sphere electrode material obtained in example 1 under different voltage windows is tested, as shown in fig. 2.
Table 1: results of electrochemical Performance test
The embodiment shows that the nano carbon ball electrode material capacitor of the silver-doped nano wire prepared by the method has a larger voltage window, can keep large specific capacitance under high current density, has small specific capacity attenuation after long-term use, and has good application prospect.
Claims (6)
1. A preparation method of a silver nanowire-doped carbon nanosphere electrode material is characterized by comprising the following steps of:
the method comprises the following steps: adding a resorcinol aqueous solution, a low-polymerization-degree paraformaldehyde aqueous solution and a sodium hydroxide solution into a reactor, stirring and mixing, heating to a certain temperature to obtain a low-molecular-weight phenolic resin prepolymer, then adding ammonia water, heating to 100 ℃, polymerizing for 24 hours, washing the obtained resin microspheres with deionized water after the reaction is finished, and drying for 5 hours in a constant-temperature drying oven at 120 ℃ to obtain nano polymer spheres;
step two: adding the nano polymer spheres into ethanol to form a mixture of 20-50mg/L, then adding silver nanowires of which the mass is 2-5% of that of the nano polymer spheres, adding a silver nitrate solution, performing ultrasound for 15min at normal temperature, then placing the mixture at 70 ℃ for condensation reflux reaction for 12 hours, and performing water washing and ethanol leaching for 3-5 times, and then performing vacuum drying to obtain the silver nanowire-doped nano polymer spheres;
step three: and (3) placing the silver nanowire-doped nano polymer ball in a tubular furnace, heating to 300 ℃ at a heating rate of 1 ℃/min in a nitrogen atmosphere, heating to 600 ℃ at a heating rate of 15 ℃/min, preserving heat at 600 ℃ for 2h, and cooling to room temperature to obtain the silver nanowire-doped nano carbon ball electrode material.
2. The method for preparing the silver nanowire-doped nanocarbon sphere electrode material as claimed in claim 1, wherein the mass concentration of the aqueous paraformaldehyde solution with low polymerization degree in the step one is 80-100 g/L.
3. The method for preparing the silver nanowire-doped carbon nanosphere electrode material as claimed in claim 1, wherein the concentration of the resorcinol aqueous solution in the first step is 0.05-0.10mol/L, the concentration of the sodium hydroxide solution is 0.1mol/L, and the concentration of ammonia water is 0.05-0.1 mol/L.
4. The method for preparing the silver nanowire-doped nanocarbon sphere electrode material as claimed in claim 1, wherein the heating to a certain temperature in the first step is 40 ℃.
5. The method for preparing the silver nanowire-doped carbon nanosphere electrode material as claimed in claim 1, wherein in the second step, the concentration of the silver nitrate solution is 0.01-0.05 mol/L.
6. The preparation method of the silver nanowire-doped carbon nanosphere electrode material as claimed in claim 1, wherein the ultrasonic power in the second step is 150-200W.
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| CN202010654723.9A CN111755261A (en) | 2020-07-09 | 2020-07-09 | Preparation method of silver nanowire doped nano carbon ball electrode material |
| JP2020131445A JP6810841B1 (en) | 2020-07-09 | 2020-08-03 | Method for manufacturing carbon nanoball electrode material of silver nanowires |
| GB2100497.3A GB2588558A (en) | 2020-07-09 | 2021-01-15 | A preparation method for carbon nanosphere electrode materials containing silver nanowires |
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| GB2588558A (en) * | 2020-07-09 | 2021-04-28 | Zhejiang Yanji Tech Co Ltd | A preparation method for carbon nanosphere electrode materials containing silver nanowires |
| CN113845180A (en) * | 2021-06-02 | 2021-12-28 | 哈尔滨工业大学（深圳） | Silver-carbon electrode material and preparation method and application thereof |
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| CN101397652B (en) * | 2008-10-31 | 2012-05-09 | 华东师范大学 | Metal microfiber-nano carbon composite material and preparation method |
| WO2012157506A1 (en) * | 2011-05-13 | 2012-11-22 | 国立大学法人熊本大学 | Carbon nanotube composite electrode and method for manufacturing same |
| KR101739295B1 (en) * | 2012-11-26 | 2017-05-24 | 삼성에스디아이 주식회사 | Composite anode active material, anode and lithium battery containing the same, and preparation method thereof |
| JP5497220B1 (en) * | 2013-03-14 | 2014-05-21 | 昭和電工株式会社 | Composite carbon fiber |
| WO2015139660A1 (en) * | 2014-03-21 | 2015-09-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Porous carbon nanotube microsphere and preparation method therefor and application thereof, lithium metal-skeleton carbon composite material and preparation method therefor, negative electrode, and battery |
| JP5838245B2 (en) * | 2014-07-22 | 2016-01-06 | 日本ケミコン株式会社 | Method for producing carbon having metal compound nanoparticles dispersed and supported |
| CN109309203A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | Nano carbon particle-stephanoporate framework composite material, its lithium metal compound, their preparation method and application |
| CN108122690B (en) * | 2017-12-15 | 2020-02-11 | 内蒙古科技大学 | Preparation method of sulfur-nitrogen co-doped carbon nanosphere electrode material |
| CN108172416B (en) * | 2018-01-23 | 2019-04-12 | 哈尔滨工业大学 | The preparation method and applications of three-dimensional carbon aerogels with porous tube wall nanotube |
| CN111755261A (en) * | 2020-07-09 | 2020-10-09 | 浙江奚态生物科技有限公司 | Preparation method of silver nanowire doped nano carbon ball electrode material |
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| GB2588558A (en) * | 2020-07-09 | 2021-04-28 | Zhejiang Yanji Tech Co Ltd | A preparation method for carbon nanosphere electrode materials containing silver nanowires |
| CN113845180A (en) * | 2021-06-02 | 2021-12-28 | 哈尔滨工业大学（深圳） | Silver-carbon electrode material and preparation method and application thereof |
| CN113845180B (en) * | 2021-06-02 | 2023-12-29 | 哈尔滨工业大学（深圳） | Silver carbon electrode material and preparation method and application thereof |
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| GB2588558A (en) | 2021-04-28 |
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