GB2588558A - A preparation method for carbon nanosphere electrode materials containing silver nanowires - Google Patents
A preparation method for carbon nanosphere electrode materials containing silver nanowires Download PDFInfo
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- 239000002077 nanosphere Substances 0.000 title claims abstract description 75
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 61
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000007772 electrode material Substances 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000011347 resin Substances 0.000 claims abstract description 25
- 229920005989 resin Polymers 0.000 claims abstract description 25
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004005 microsphere Substances 0.000 claims abstract description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 abstract 2
- 229910001961 silver nitrate Inorganic materials 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000002484 cyclic voltammetry Methods 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 108020001612 μ-opioid receptors Proteins 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
- 241000577218 Phenes Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- BXGJXQJWUCUHJQ-UHFFFAOYSA-N [C].C1(O)=C(C(O)=CC=C1)C=O Chemical compound [C].C1(O)=C(C(O)=CC=C1)C=O BXGJXQJWUCUHJQ-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/152—Fullerenes
- C01B32/154—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
-
- 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
- H01G11/24—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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- 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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- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
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Abstract
A preparation method for carbon nanosphere electrode materials containing silver nanowires is disclosed which comprises stirring aqueous resorcinol, aqueous polyformaldehyde and sodium hydroxide in a reactor, Low Molecular Weight Phenolaldehyde resin prepolymer is obtained, ammonium hydroxide added and the mixture heated to 100 ℃ and polymerised for 24 hours. Resin microspheres are obtained, washed with water, and dried in a drying oven at 120 ℃ for 5 hours, and Macromolecular Nanospheres obtained. The Macromolecular Nanospheres are formed into a 20-50mg/L mixture in ethanol, and silver nanowires with a 2-5% of mass of the Macromolecular Nanospheres and silver nitrate added, the mixture ultrasonicated for 15 min at room temperature, and then refluxed at 70℃ for 12 hours. The mixture is vacuum-dried after being water washed and washed with ethanol, and Macromolecular Nanospheres containing silver nanowires obtained. These are placed into a furnace, and the temperature raised from room temperature to 300 ℃ at heating rate 1 ℃/min, and then to 600 ℃ at heating rate 15 ℃/min in nitrogen atmosphere and then heated at 600 ℃ for 2 hours, forming carbon nanosphere electrode materials containing silver nanowires.
Description
A PREPARATION METHOD FOR CARBON NANOSPHERE ELECTRODE MATERIALS CONTAINING SILVER NANOWIRES
TECHNICAL FIELD
[0001] The present invention relates to the field of electrode material preparation, in particular to a preparation method for carbon nanosphere electrode materials containing silve nanovvires.
BACKGROUND OF THE INVENTION
[0002] Supercapacitor (electrochemical capacitor) is a new energy storage device whose performance falls between battery and static condenser; at present, the research core of the supercapacitor is mainly focus on studying electrode materials.
[0003] Carbon materials, as an important electrode material, is not only directly used as electrode materials, but also further used as compound basement or doped 'framework"; compared with original carbon electrode materials, the electrode materials being compounded or doped has a higher capacitance and energy density; however, the doped carbon materials is able to maintain a good cycling stability, which is also an important performance index of the electrode materials.
[0004] As special quantum size efiect, small size effect and quantum tunnel effect, liailOtTleter materials attracts a large number of researcher's attention, as special photoelectric effect and chemical property, metal nanometer materials is applied in various of fields; in 2017, Li et al. proposed a new type of Ai-actual catalyst that resorcinol-formaldehyde carbon sphere (Pt(ise...RFC) facing MORs are embedded in part of platinum nanoparticles, and PtiORFC has a good compatibility and MOR activity, wherein CO oxidation peak potential shifts negatively at about 15Omy and an electrocatalytic activity is two times as high as that of commercially available Pt/C; what is noteworthy is that a mass revivification of PtaRFC is maintained greatly after accelerated degradation with 3000 times cyclic voltammetry experiments, which is 5.8 times as that of commercial available Pt/C.
[0005] Among existing materials to be prepared supercapacitors, as a wide source, low cost and various forms, the carbon materials has became the most widely electrode materials being studied, like carbon nano tube(CNT), gra.phene, activated carbon and etc.; howe er, most of the carbon electrode materials has a not so good electrical conductivity, which will leads to a poor rate capability of the equipment; therefore, electrode with a good electrical conductivity is a basis to prepare supercapacitors with high performance; to improve a electrical conductivity of carbon film, conductive black is added in traditional method, but a very high conductive black will reduce quality and specific surface area of the carbon film, and at the same time, square impedance of the carbon films is relative high; the patent application CN107452515A discloses a sizing agent prepared with binder, silver nanowire conductive agent and active substance, which prepares into electrode pole piece by taking nickel foam as current collector through a roiling or coating transfer process to compose the supercapacitor; however, the method is required to add a large amount of silver nanowires to reduce equivalent resistance.
BRIEF SUMMARY OF THE INVENTION
[00061 This invention discloses a preparation method for carbon nanosphere electrode materials containing silver nanowires so as to overcome the problems existing in the prior art [0007] For achieving above mentioned invention target, the invention provides following technical schemes [0008] A preparation method for carbon nanosphere electrode materials containing silver nanowires, comprising the following steps: [0009] Step 1: Resorcinol aqueous solution, lower polyfommIdehyde aqueous solution and sodium hydroxide solution were added into a rector to be stirred to mix together to heat to a definite temperature, and then Low Molecular Weight Phenolaldehyde resin prepolymer (PFRFPS) were obtained, and then ammonium hydroxide were added into to be heated to 100 °C arid polymerized for 24 hours, after reaction was finished, resin microspheres were obtained after being washing with deionized water, and then the resin microspheres were dried in a constant temperature drying oven at 120 °C for 5 hours, and then Macromolecular Nanospheres were obtained.
[0010] Step 2: put the Macromolecular Nanospheres into 20-50mg/L mixture formed in ethyl alcohol, and then the silver nanowires with a 2-5% of mass of the Macromolecular Nanospheres were added, and then liquor argenti nitratis ophthalmicus were added, the above mixture was dealt with supersonic for 15 min in room temperature, and then the mixture was placed in 70°C to be condensed and refluxed for 12 hours, and then the mixture was dried in vacuum after being water washed for 3-5 times and drip washed with the ethyl alcohol, and then Macromolecular Nanospheres containing silver nanowires were obtained [0011] Step 3: put the Macromolecular Nanospheres containing silver nanowires into a tube furnace, and then the temperature was over the range from room temperature to 300 °C at the heating rate of 1 °C/min to 600 °C at the heating rate of 15 °C/min in nitrogen atmosphere and then heated at 600 °C for 2 hours, after cooling to the room temperature, carbon nanosphere electrode materials containing silver nanowires were obtained.
[0012] Preferably, the concentration of the Resorcinol aqueous solution stated in Step 1 is 0.05-0.10mol/L, the concentration of the sodium hydroxide solution is 0.1mol/L, the concentration of the ammonium hydroxide is 0.05-0.1mol/L, the mass concentration of the lower polyfonnaldehyde aqueous solution is 280-380g1.
[0013] Preferably, the heating temperature when obtaining Low Molecular Weight Phenolaldehyde resin prepolymer in Step 1 is 40°C.
[0014] Preferably, the concentration of the liquor argenti n tratis ophthalmicus is 0.01-0.05mol/L, and an ultrasonic power is 150-200W.
[0015] The benefits of the invention are as follows: the carbon nanosphere electrode materials containing silver nanowires disclosed in the present invention is able to overcome the disadvantage like large resistance of the traditional electrode materials to compound the silver nanowires into the carbon nanospheres, thereby the silver nanowires interacts with silver ion loaded on the carbon nanospheres, thereby the capacitance of the carbon nanosphere electrode materials containing silver nanowires enlarges;with a relative large specific area, the carbon nanosphere electrode materials containing silver nanowires is conductive to transport electron ions; the preparation method disclosed in this invention is simple and the electrode material to be prepared has a low specific resistance, which provides a high specific capacitance for supercapacitor materials and easy to be operated, moreover, the apparatus is low in requirements, which has a good application prospect.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 is a scanning electron microscopic image of the carbon nanosphere electrode materials containing silver nanowires obtained in embodiment 1; [0017] FIG. 2 is a chart showing the cyclic voltammetry of symmetric capacitor assembled by the carbon nanosphere electrode materials containing silver nanowires obtained in embodiment 1 at different voltage windows.
DETAILED DESCRIPTION OF THE INVENTION
[0018] A preparation method for carbon nanosphere electrode materials containing silver nanowires [0019] In present invention, silver nanowires are prepared by existing technologies [0020] Embodiment 1 [0021] A preparation method for carbon nanosphere electrode materials containing silver nanowires, comprising the following steps: [0022] Step 1: 50 ml of 0.05mol/L Resorcinol aqueous solution and 20 ml of 0.1mol/L sodium hydroxide solution were added into a rector, and then lower polyformaldehyde aqueous solution with a mass concentration of 80g/L were also added into the reactor, and then the above mixture were stirred to mix together to heat to 40°C, and then a Low Molecular Weight Phenolaldehyde Resin Prepolymer (PFREPS) were obtained, and then 20 mL of 0.05mol/L ammonium hydroxide were added into for being heated to 100°C and polymerized for 24 hours, after reaction was finished, resin microspheres were obtained after being washing with deionized water, and then the resin microspheres were dried in a constant temperature drying oven at 120°C for 5 hours, and then Macromolecular Nanospheres were obtained.
[0023] Step 2: put the Macromolecular Nanospheres into 20mg/L mixture formed in ethyl alcohol, and then the silver nanowires with 2% of mass of the Macromolecular Nanospheres were added, and then 20 mL of 0.01mol/L liquor argenti nitratis ophthalmicus were added, the above mixture was dealt with supersonic for 15 min with an ultrasonic power of 150W in room temperature, and then the mixture was placed in 70°C to be condensed and refluxed for 12 hours, arid then the mixture was dried in vacuum after being water washed for 3-5 times and drip washed with the ethyl alcohol, and then Macromolecular Nanospheres containing silver nanowires were obtained.
[0024] Step 3: put the Macromolecular Nanospheres containing silver nanowires into a tube furnace, and then the temperature was over the range from room temperature to 300°C at a heating rate of 1°C/min to 600°C at the heating rate of 15°C/min in nitrogen atmosphere and then heated at 600 °C for 2 hours, after cooling to room temperature, carbon nanosphere electrode materials containing silver nanowires were obtained.
[0025] Embodiment 2 [0026] A preparation method for carbon nanosphere electrode materials containing silver nanowires, comprising the following steps: [0027] Step 1: 50 ml of 0.06mol/L Resorcinol aqueous solution and 20 ml of 0.1mol/L sodium hydroxide solution were added into a rector, and then lower polyfonnaldehyde aqueous solution with a mass concentration of 85g/L were also added into the reactor, and then the above mixture were stirred to mix together to heat to 40°C, and then a Low Molecular Weight Phenolaldehyde Resin Prepolymer (PFRFPS) were obtained, and then 20 mL of 0.06mol/L ammonium hydroxide were added into for being heated to 100°C and polymerized for 24 hours, after reaction was finished, resin microspheres were obtained after being washing with deionized water, and then the resin microspheres were dried in a constant temperature drying oven at 120°C for 5 hours, and then Macromolecular Nanospheres were obtained.
[0028] Step 2: put the Macromolecular Nanospheres into 20mg/L mixture formed in ethyl alcohol, and then the silver nanowires with 2% of mass of the Macromolecular Nanospheres were added, and then 20 mL of 0.02mol/L liquor argenti nitratis ophthalmicus were added, the above mixture was dealt with supersonic for 15 min with an ultrasonic power of 160W in room temperature, and then the mixture was placed in 70°C to be condensed and refluxed for 12 hours, and then the mixture was dried in vacuum after being water washed for 3-5 times and drip washed with the ethyl alcohol, and then Macromolecular Nanospheres containing silver nanowires were obtained [0029] Step 3: put the Macromolecular Nanospheres containing silver nanowires into a tube furnace, and then the temperature was over the range from room temperature to 3 00°C at a heating rate of 1°C/min to 600°C at the heating rate of 15°C/min in nitrogen atmosphere and then heated at 600 °C for 2 hours, after cooling to room temperature, carbon nanosphere electrode materials containing silver nanowires were obtained.
[0030] Embodiment 3 [0031] A preparation method for carbon nanosphere electrode materials containing silver nanowires, comprising the following steps: [0032] Step 1: 50 ml of 0.07mol/L Resorcinol aqueous solution and 20 ml of 0.1mol/L sodium hydroxide solution were added into a rector, and then lower polyformaldehyde aqueous solution with a mass concentration of 90g/L were also added into the reactor, and then the above mixture were stirred to mix together to heat to 40°C, and then a Low Molecular Weight Phenolaldehyde Resin Prepolymer (PFRFPS) were obtained, and then 20 mL of 0.06mol/L ammonium hydroxide were added into for being heated to 100°C and polymerized for 24 hours, after reaction was finished, resin microspheres were obtained after being washing with deionized water, and then the resin microspheres were dried in a constant temperature drying oven at 120°C for 5 hours, and then Macromolecular Nanospheres were obtained.
[0033] Step 2: put the Macromolecular Nanospheres into 20mg/L mixture formed in ethyl alcohol, and then the silver nanowires with 2% of mass of the Macromolecular Nanospheres were added, and then 20 mL of 0.03mol/L liquor argenti nitratis ophthalmicus were added, the above mixture was dealt with supersonic for 15 min with an ultrasonic power of 170W in room temperature, and then the mixture was placed in 70°C to be condensed and refluxed for 12 hours, and then the mixture was dried in vacuum after being water washed for 3-5 times and drip washed with the ethyl alcohol, and then Macromolecular Nanospheres containing silver nanowires were obtained.
[0034] Step 3: put the Macromolecular Nanospheres containing silver nanowires into a tube furnace, and then the temperature was over the range from room temperature to 300°C at a heating rate of 1°C/min to 600°C at the heating rate of 15°C/min in nitrogen atmosphere and then heated at 600 °C for 2 hours, after cooling to room temperature, carbon nanosphere electrode materials containing silver nanowires were obtained [0035] Embodiment 4 [0036] A preparation method for carbon nanosphere electrode materials containing silver nanowires, comprising the following steps: [0037] Step 1: 50 ml of 0.08mol/L Resorcinol aqueous solution and 20 ml of 0.1mol/L sodium hydroxide solution were added into a rector, and then lower polyformaldehyde aqueous solution with a mass concentration of 95g/L were also added into the reactor, and then the above mixture were stirred to mix together to heat to 40°C, and then a Low Molecular Weight Phenolaldehyde Resin Prepolymer (PFRFPS) were obtained, and then 20 mL of 0.08mol/L ammonium hydroxide were added into for being heated to 100°C and polymerized for 24 hours, after reaction was finished, resin microspheres were obtained after being washing with deionized water, and then the resin microspheres were dried in a constant temperature drying oven at 120°C for 5 hours, and then Macromolecular Nanospheres were obtained.
[0038] Step 2: put the Macromolecular Nanospheres into 20mg/L mixture formed in ethyl alcohol, and then the silver nanowires with 2% of mass of the Macromolecular Nanospheres were added, and then 20 mL of 0.04mol/L liquor argenti nitratis ophthalmicus were added, the above mixture was dealt with supersonic for 15 min with an ultrasonic power of 180W in room temperature, and then the mixture was placed in 70°C to be condensed and refluxed for 12 hours, and then the mixture was dried in vacuum after being water washed for 3-5 times and drip washed with the ethyl alcohol, and then Macromolecular Nanospheres containing silver nanowires were obtained.
[0039] Step 3: put the Macromolecular Nanospheres containing silver nanowires into a tube furnace, and then the temperature was over the range from room temperature to 300°C at a heating rate of 1°C/min to 600°C at the heating rate of 15°C/min in nitrogen atmosphere and then heated at 600 °C for 2 hours, after cooling to room temperature, carbon nanosphere electrode materials containing silver nanowires were obtained.
[0040] Embodiment 5 [0041] A preparation method for carbon nanosphere electrode materials containing silver nanowires, comprising the following steps: [0042] Step 1 50 ml of 0.10mol/L Resorcinol aqueous solution and 20 ml of 0.1mol/L sodium hydroxide solution were added into a rector, and then lower polyformaldehyde aqueous solution with a mass concentration of 100g/L were also added into the reactor, and then the above mixture were stirred to mix together to heat to 40°C, and then a Low Molecular Weight Phenolaldehyde Resin Prepolymer (PFRFPS) were obtained, and then 20 mL of 0.10mol/L ammonium hydroxide were added into for being heated to 100°C and polymerized for 24 hours, after reaction was finished, resin microspheres were obtained after being washing with deionized water, and then the resin microspheres were dried in a constant temperature drying oven at 120°C for 5 hours, and then Macromolecular Nanospheres were obtained [0043] Step 2: put the Macromolecular Nanospheres into 20mg/L mixture formed in ethyl alcohol, and then the silver nanowires with 2% of mass of the Macromolecular Nanospheres were added, and then 20 mL of 0 05mol/L liquor argenti nitratis ophthalmicus were added, the above mixture was dealt with supersonic for 15 min with an ultrasonic power of 200W in room temperature, and then the mixture was placed in 70°C to be condensed and refluxed for 12 hours, and then the mixture was dried in vacuum after being water washed for 3-5 times and drip washed with the ethyl alcohol, and then Macromolecular Nanospheres containing silver nanowires were obtained.
[0044] Step 3: put the Macromolecular Nanospheres containing silver nanowires into a tube furnace, and then the temperature was over the range from room temperature to 300°C at a heating rate of 1°C/min to 600°C at the heating rate of 15°C/min in nitrogen atmosphere and then heated at 600 °C for 2 hours, after cooling to room temperature, carbon nanosphere electrode materials containing silver nanowires were obtained.
[0045] Electrochemical performance test: [0046] Put the carbon nanosphere electrode materials containing silver nanowires obtained in embodiments 1-5, acetylene black and polytetrafluoroethylene(PTFE) with the mass ratio of 8:1:1 into an agate mortar, and then proper amount of ethyl alcohol was added dropwise, and then the above mixture was ground evenly to coat on the nickel foam, and then the nickel foam coated with the above mixture was placed in the drying oven in 50°C for 2 hours, and then the electrodes were taken out to be rolled-in on rolling machine and the drying was continued in 50°C for 1 hour, and took button cell press as electrodes of button supercapacitor, the obtained electrodes were assembled into symmetric supercapacitors; after 24 hours standing, the electrochemical performance is tested, and results are shown in table 1, and then cyclic voltammetry of the symmetric supercapacitor assembled by carbon nanosphere electrode materials containing silver nanowires at different voltage windows was tested, the results are shown in figure 2.
[0047] Table 1 Testing Results of Electrochemical Performance Testing items Embodiment Embodiment Embodiment Embodiment Embodiment 1 2 3 4 5 Configuration Smooth regular and Smooth regular and Smooth regular and Smooth regular and Smooth regular and Voltage window 0-1.5V 0-1.5V 0-1.5V 0-1.6V 0-1.7V Specific capacitance at a current density of I A/g 175F/g 176Fig 178F/g 179F7g 180F/g Specific capacitance at a current density of 20A/g 256Fig 262F/g 265F/g 268E/g 275F/g An attenuation of specific 5.1% 4.8% 4.5% 4.3% 4.1% capacitance after 3000 [0048] As can be seen from the embodiments, the capacitor voltage window of the carbon nanosphere electrode materials containing silver nanowires prepared in this method is relative large and is able to maintain a large specific capacitance at a large current density, moreover, the attenuation of the specific capacitance is small after a long time using, which has a good application prospect.
Claims (6)
- CLAIMS1. A preparation method for carbon nanosphere electrode materials containing silver nanowires, comprising the following steps: Step 1: Resorcinol aqueous solution, lower polyformaldehyde aqueous solution and sodium hydroxide solution were added into a rector to be stirred to mix together to heat to a definite temperature, and then Low Molecular Weight Phenolaldehyde resin prepolymer (PFRFPS) were obtained, and then ammonium hydroxide were added into to be heated to 100 °C and polymerized for 24 hours, after reaction was finished, resin microspheres were obtained after being washing with deionized water, and then the resin microspheres were dried in a constant temperature drying oven at 120 °C for 5 hours, and then Macromolecular Nanospheres were obtained.Step 2. put the Macromolecular Nanospheres into 20-50mg/L mixture formed in ethyl alcohol, and then the silver nanowires with a 2-5% of mass of the Macromolecular Nanospheres were added, and then liquor argenti nitratis ophthalmicus were added, the above mixture was dealt with supersonic for 15 min in room temperature, and then the mixture was placed in 70°C to be condensed and refluxed for 12 hours, and then the mixture was dried in vacuum after being water washed for 3-5 times and drip washed with the ethyl alcohol, and then Macromolecular Nanospheres containing silver nanowires were obtained Step 3: put the Macromolecular Nanospheres containing silver nanowires into a tube furnace, and then the temperature was over the range from room temperature to 300 °C at the heating rate of 1 °C/min to 600 °C at the heating rate of 15 °C/min in nitrogen atmosphere and then heated at 600 °C for 2 hours, after cooling to the room temperature, carbon nanosphere electrode materials containing silver nanowires were obtained.
- 2. The preparation method for carbon nanosphere electrode materials containing silver nanowires defined in claim 1, wherein the mass concentration of the lower polyfonnaldehyde aqueous solution in Step 1 is 80-100g/L.
- 3. The preparation method for carbon nanosphere electrode materials containing silver nanowires defined in claim 1, wherein the concentration of the Resorcinol aqueous solution stated in Step 1 is 0.05-0.10mol/L, the concentration of the sodium hydroxide solution is 0.1mol/L, the concentration of the ammonium hydroxide is 0.05-0.1mol/L.
- 4. The preparation method for carbon nanosphere electrode materials containing silver nanowires defined in claim 1, wherein the heating temperature when obtaining Low Molecular Weight Phenolaldehyde resin prepolymer in Step 1 is 40°C.
- 5. The preparation method for carbon nanosphere electrode materials containing silver nanowires defined in claim 1, wherein the concentration of the liquor argenti nitratis ophthalmicus is 0.01-0.05mol/L.
- 6. The preparation method for carbon nanosphere electrode materials containing silver nanowires defined in claim 1, wherein an ultrasonic power in Step 2 is 150-200W
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| US20140147741A1 (en) * | 2012-11-26 | 2014-05-29 | Samsung Sdi Co., Ltd. | Composite anode active material, anode and lithium battery containing the same, and method of preparing the composite anode active material |
| CN108172416A (en) * | 2018-01-23 | 2018-06-15 | 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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| CN108172416A (en) * | 2018-01-23 | 2018-06-15 | 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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