CN104916451A - Method for preparing super capacitor electrode material made of nickel oxide nanosheet grown on micro carbon tube - Google Patents
Method for preparing super capacitor electrode material made of nickel oxide nanosheet grown on micro carbon tube Download PDFInfo
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- CN104916451A CN104916451A CN201510232508.9A CN201510232508A CN104916451A CN 104916451 A CN104916451 A CN 104916451A CN 201510232508 A CN201510232508 A CN 201510232508A CN 104916451 A CN104916451 A CN 104916451A
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 48
- 229910000480 nickel oxide Inorganic materials 0.000 title claims abstract description 26
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000007772 electrode material Substances 0.000 title claims abstract description 15
- 239000002135 nanosheet Substances 0.000 title claims abstract description 11
- 239000003990 capacitor Substances 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 44
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003763 carbonization Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000002131 composite material Substances 0.000 claims description 16
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 8
- 239000002120 nanofilm Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 abstract description 8
- 239000000047 product Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 241000124033 Salix Species 0.000 abstract 3
- 238000010000 carbonizing Methods 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 5
- 230000033116 oxidation-reduction process Effects 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000003487 electrochemical reaction Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000011274 Benincasa cerifera Nutrition 0.000 description 1
- 244000036905 Benincasa cerifera Species 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- H01G11/46—Metal oxides
-
- 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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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A method for preparing a super capacitor electrode material made of a nickel oxide nanosheet grown on a micro carbon tube. The method comprises the following steps: cleaning collected willow catkins, putting the willow catkins in a carbonization furnace, and carbonizing the willow catkins under protective atmosphere to obtain a micro carbon tube; adding the micro carbon tube to N,N-dimethyl formamide, and carrying out ultrasonic processing to obtain a solution A; dissolving Ni(NO3)2.6H2O powder in deionized water to form a solution B, slowly adding the solution A to the solution B drop by drop for hydrothermal reaction, and cooling the mixed solution to room temperature; washing a product obtained in the previous step with deionized water, drying the product, and calcining the product under protective atmosphere to obtain a final product. The method of the invention has the advantages of simple process, mild preparation conditions, simple operation, low energy consumption, good rate performance, and good cycle performance.
Description
Affiliated field
The invention belongs to a kind of preparation method of capacitor electrode material, relate in particular to the preparation method of the electrode material for super capacitor of growth oxidation nickel nano film on a kind of micro-carbon pipe.
Technical background
Along with day by day consuming of conventional energy resource and warming of global climate, cheap, clean energy resource becomes the object that scientific worker extensively chases.Wherein, the advantages such as charge-discharge velocity is fast, power density is high because having for ultracapacitor, cycle performance good (discharge and recharge up to 5-50 ten thousand times), it is at electric automobile, hybrid vehicle, exceptional load automobile, have important application in various fields such as solar energy and wind power generation, military field and consumption electronic products, be considered to a kind of the most promising can the green energy storage device of iterative cycles.In order to meet the requirement of high-specific-power and specific energy density, till now, a series of oxidation-reduction quality material (such as metal oxide/hydroxide, conducting polymer) is applied to electrode material for super capacitor (Adv.Funct.Mater., 2012,22 (12): 2632-2641; Advanced function material, 22 volume 12 phases in 2012: 2632-2641 page).Wherein, nickel oxide has high theoretical ratio capacitance (2583F g because of it
-1), high chemistry/thermal stability, good invertibity, environmental friendliness and low cost and gain great popularity (Nanoscale, 2013,5 (17): 7984-7990; Nanometer, 2013,5 volume 17 phases: 7984-7990 page; ) (J.PowerSources, 2010,195:3950-3955; Power supply, 2010,195 volumes: 3950-3955 page).But pure nickel in use often because its intrinsic conductivity is low, and causes high rate performance not good.In addition, in repeated charge process, also can there is powder reuniting and volume acute variation in nickel oxide itself, and therefore its inducing capacity fading is very fast, and cyclical stability is not fully up to expectations.So, adopt nickel oxide to be still subject to certain restrictions as electrode material for super capacitor at present.
In order to overcome the problems referred to above, people have developed the methods and strategies of a series of raising oxidation-reduction quality material electrochemical performance.Wherein comparatively effective strategy be prepare nano-scale oxidation-reduction quality material granule to shorten a migration distance for electronics and lithium ion, improve material reacting dynamics characteristic.Second method constructs a kind of composite material of special construction, is dispersed in carbon base body by active material.This carbon base body not only can serve as flexible bumper, as conductive network, can also increase the electrical conductance of oxidation-reduction quality material.3rd class methods are electrode materials of preparation porous micro/nano structure.The cavity of porous micro/nano structure or hole not only can alleviate material volume change, improve cycle performance; The specific area of electrode material can also be improved, increase the electrochemical reaction area of material.Based on this, if while the nickel oxide of nano-scale being dispersed in conductive carbon matrix, composite material itself can be built into porous micro/nano structure again, so this special composite material will in conjunction with multiple advantage as above, and expection farthest improves nickel oxide electrode material electrochemical performance.
Nowadays, template becomes advanced method and the available strategy of controlledly synthesis novel nano/micrometer structure composite material already.(H.W.Shim, Y.H.Jin, S.D.Seo, ACS Nano, 2011,115 (1): 443-449; H.W.Shim, Y.H.Jin, S.D.Seo, American Chemical Society's nanometer, 115 volume 1 phase: 443-449 in 2011).In this respect, the Nature is we provide outstanding biological template of all kinds, as wax gourd (Y.Q.Li, Y.A.Samad, K.Liao, ACS Sustainable Chem.Eng., 2014,2:1492-1497; Y.Q.Li, Y.A.Samad, K.Liao, American Chemical Society's sustainable chemistry and engineering, 2014,2 volumes: 1492-1497 page), pig bone (S.C.Wei, H.Zhang, Y.Q.Huang, Energy & Environmental Science, 2011,4 (3): 736-740; S.C.Wei, H.Zhang, Y.Q.Huang, energy and environment science, 4 volume 3 phase: 736-740 in 2011), crab shell (H.B.Yao, G.Y.Zheng, Nano Lett., 2013,13:3385-3390; H.B.Yao, G.Y.Zheng, nanometer bulletin, 13 volumes: 3385-3390 page in 2013) etc.These native template all have highly regular, homogeneous geometry, and researchers can utilize these biological templates to prepare the multilevel hierarchy composite material of different scale, different-shape easily.
Micro-carbon pipe that the carbonization of employing catkin obtains, as template and carbon source, in conjunction with the method for hydro-thermal, is prepared nickel oxide-micro-carbon pipe nano/micron structure combination electrode material, is found no prior art through retrieval.
Summary of the invention
For overcoming the above-mentioned defect existing for prior art, the object of the present invention is to provide a kind of technique simple, preparation condition is gentle, simple to operate, energy consumption is low, the preparation method of the electrode material for super capacitor of growth oxidation nickel nano film on micro-carbon pipe of good rate capability and good cycle.
From analyzing above, both the electrical conductance of nickel oxide can have been increased at the Nano/micron composite construction of micro-carbon tube-surface growth oxidation nickel nano film, thus increase the electrochemical reaction area of material, the cavity of porous micro/nano structure or hole can alleviate again material volume change, finally improve its high rate performance and cycle performance.
The present invention is achieved by following technical proposals:
(1) first the catkin collected be impregnated in ethanol solution, and ultrasonic disperse 10-60min, obtain the catkin sample cleaned up, then the catkin sample cleaned up is loaded carbide furnace, under protective atmosphere, at 500-1000 DEG C, carry out carbonization, obtain micro-carbon pipe;
(2) by micro-carbon pipe: DMF=0.1-0.5g:50-100ml, micro-carbon pipe is joined in DMF, through ultrasonic, obtains solution A;
(3) by Ni (NO
3)
26H
2o: deionized water=1g:10-100ml, by Ni (NO
3)
26H
2o powder dissolves in deionized water, forms solution B, then solution A is dropwise slowly added in solution B, fully stir;
(4) the mixed solution hydro-thermal reaction 12-36h between 100-250 DEG C step (3) obtained, is cooled to room temperature;
(5) product suction filtration step (4) obtained also uses deionized water cyclic washing, and dry, finally, under protective atmosphere, 150-500 DEG C of calcining obtains nickel oxide nano sheet/micro-carbon pipe composite material for 4 hours.
The present invention obtains growth oxidation nickel nano film composite material on micro-carbon pipe can be used as electrode material for super capacitor.This nano-chip arrays electrode has excellent high rate performance, higher ratio capacitance and good cycle life.
Beneficial effect of the present invention:
Micro-carbon pipe that the present invention adopts catkin carbonization to obtain first is as template and carbon source, and in conjunction with the method for hydro-thermal, vertical-growth is on the surface of micro-carbon pipe in large area to make nickel oxide nano sheet, and sheet and sheet are intertwined to form three-dimensional porous network structure.The hierarchy deposited mutually by micro-carbon pipe and nickel oxide substantially increases the conductivity of nickel oxide, increases its capacitive property, and nickel oxide is grown directly upon on micro-carbon pipe, without any need for binding agent, thus decreases " dead volume " of active material.Meanwhile, the cavity of porous micro/nano structure or hole not only can alleviate material volume change, are beneficial to the infiltration of electrolyte ion, improve cycle performance; The specific area of electrode material can also be improved, increase the electrochemical reaction area of material, finally affect its chemical property.In addition, preparation method's technique of the present invention is simple, and preparation condition is gentle, and simple to operate, energy consumption is low, therefore, is easy to promote.
Accompanying drawing explanation
The all embodiment products of Fig. 1 are at current density 1A g
-1under charging and discharging curve (a) and embodiment 4 at current density 10A g
-1under cycle performance (b).
The scanning electron microscope (SEM) photograph of Fig. 2 embodiment 4 product.
Embodiment
Further illustrate the present invention by embodiment below, but protection scope of the present invention is not limited in embodiment.To those skilled in the art not deviating from the other changes and modifications made in spirit of the present invention and protection range situation, be still included within scope.
Embodiment 1
First the catkin collected be impregnated in ethanol solution, and ultrasonic disperse 10min obtains the catkin sample cleaned up, then the catkin sample cleaned up is loaded carbide furnace, micro-carbon pipe is obtained through 500 DEG C of carbonizations under argon gas atmosphere, then micro-for 0.1g carbon pipe is joined the N of 50ml, in dinethylformamide, through ultrasonic, obtain solution A; Again by 1g Ni (NO
3)
26H
2o powder is dissolved in the deionized water of 10ml, forms solution B.Then, under magnetic stirring, solution A is dropwise slowly added in solution B.Be transferred in reactor by the mixed liquor obtained, at 100 DEG C, heat 36h, after reaction terminates, by products therefrom suction filtration, washing, dries.Finally, under an argon atmosphere, 150 DEG C of calcinings, 4 hours obtained specific areas are 189m
2g
-1, the load factor of nickel oxide is nickel oxide nano sheet/micro-carbon pipe composite material of 85.5%.
Add growth oxidation nickel nano film composite material, acetylene black, polytetrafluoroethylene on obtained micro-carbon pipe according to the ratio of mass ratio 85:10:5, striking out diameter after mixing is rolled into film is 1cm
2electrode slice, with the KOH of 6M for electrolyte, be 1A g in current density
-1time, its specific capacity is 404F g
-1.
Embodiment 2
First the catkin collected be impregnated in ethanol solution, and ultrasonic disperse 10min obtains the catkin sample cleaned up, then the catkin sample cleaned up is loaded carbide furnace, micro-carbon pipe is obtained through 1000 DEG C of carbonizations under nitrogen atmosphere, then the micro-carbon pipe getting 0.5g joins the N of 100ml, in dinethylformamide, through ultrasonic, obtain solution A; Again by 1g Ni (NO
3)
26H
2o powder is dissolved in the deionized water of 100ml, forms solution B.Under emulsifying agent strong stirring, solution A is dropwise slowly added in solution B.The mixed liquor obtained is transferred in reactor, at 180 DEG C, heats 18h, after reaction terminates, by products therefrom suction filtration, washing, 60 DEG C of oven dry.Finally, in a nitrogen atmosphere, 500 DEG C of calcinings, 4 hours obtained specific areas are 180m
2g
-1, the load factor of nickel oxide is nickel oxide nano sheet/micro-carbon pipe composite material of 65.2%.
Identical with the method that embodiment 1 prepares electrode, after tested, be 1A g in current density
-1time, its specific capacity is 431F g
-1.
Embodiment 3
First the catkin collected be impregnated in ethanol solution, and ultrasonic disperse 10min obtains the catkin sample cleaned up, then the catkin sample cleaned up is loaded carbide furnace, micro-carbon pipe is obtained through 600 DEG C of carbonizations under nitrogen atmosphere, then the micro-carbon pipe getting 0.3g joins the N of 100ml, in dinethylformamide, through ultrasonic, obtain solution A; Again by 1g Ni (NO
3)
26H
2o powder is dissolved in the deionized water of 80ml, forms solution B.Under cell disruptor strong stirring condition, solution A is dropwise slowly added in solution B.The mixed liquor obtained is transferred in reactor, at 250 DEG C, heats 12h, after reaction terminates, by products therefrom suction filtration, washing, 60 DEG C of oven dry.Finally, in a nitrogen atmosphere, 500 DEG C of calcinings, 4 hours obtained specific areas are 186m
2g
-1, the load factor of nickel oxide is nickel oxide nano sheet/micro-carbon pipe composite material of 73.5%.
Identical with the method that embodiment 1 prepares electrode, after tested, be 1A g in current density
-1time, its specific capacity is 460F g
-1.
Embodiment 4
First the catkin collected be impregnated in ethanol solution, and ultrasonic disperse 10min obtains the catkin sample cleaned up, then the catkin sample cleaned up is loaded carbide furnace, micro-carbon pipe is obtained through 700 DEG C of carbonizations under argon gas atmosphere, then the micro-carbon pipe getting 0.1g joins the N of 50ml, in dinethylformamide, through ultrasonic, obtain solution A; Again by 1g Ni (NO
3)
26H
2o powder is dissolved in the deionized water of 50ml, forms solution B.Under magnetic agitation condition, solution A is dropwise slowly added in solution B.Be transferred in reactor by the mixed liquor obtained, at 180 DEG C, heat 12h, after reaction terminates, by products therefrom suction filtration, washing, dries.Finally, under an argon atmosphere, 250 DEG C of calcinings, 4 hours obtained specific areas are 216m
2g
-1, the load factor of nickel oxide is nickel oxide nano sheet/micro-carbon pipe composite material of 83.5%.
Identical with the method that embodiment 1 prepares electrode, after tested, be 1A g in current density
-1under, its specific capacity is 628F g
-1.
Embodiment 5
First the catkin collected be impregnated in ethanol solution, and ultrasonic disperse 10min obtains the catkin sample cleaned up, then the catkin sample cleaned up is loaded carbide furnace, micro-carbon pipe is obtained through 800 DEG C of carbonizations under argon gas atmosphere, then the micro-carbon pipe getting 0.1g joins the N of 80ml, in dinethylformamide, through ultrasonic, obtain solution A; Again by 1g Ni (NO
3)
26H
2o powder is dissolved in the deionized water of 50ml, forms solution B.Under magnetic agitation condition, solution A is dropwise slowly added in solution B.Be transferred in reactor by the mixed liquor obtained, at 200 DEG C, heat 12h, after reaction terminates, by products therefrom suction filtration, washing, dries.Finally, under an argon atmosphere, 250 DEG C of calcinings, 4 hours obtained specific areas are 198m
2g
-1, the load factor of nickel oxide is nickel oxide nano sheet/micro-carbon pipe composite material of 80.3%.
Identical with the method that embodiment 1 prepares electrode, after tested, be 1A g in current density
-1under, its specific capacity is 553F g
-1.
Embodiment 6
First the catkin collected be impregnated in ethanol solution, and ultrasonic disperse 10min obtains the catkin sample cleaned up, then the catkin sample cleaned up is loaded carbide furnace, micro-carbon pipe is obtained through 1000 DEG C of carbonizations under nitrogen atmosphere, then the micro-carbon pipe getting 0.1g joins the N of 80ml, in dinethylformamide, through ultrasonic, obtain solution A; Again by 1g Ni (NO
3)
26H
2o powder is dissolved in the deionized water of 100ml, forms solution B.Under cell disruptor strong stirring condition, solution A is dropwise slowly added in solution B.Be transferred in reactor by the mixed liquor obtained, at 200 DEG C, heat 12h, after reaction terminates, by products therefrom suction filtration, washing, dries.Finally, in a nitrogen atmosphere, 250 DEG C of calcinings, 4 hours obtained specific areas are 198m
2g
-1, the load factor of nickel oxide is nickel oxide nano sheet/micro-carbon pipe composite material of 89.2%.
Identical with the method that embodiment 1 prepares electrode, after tested, be 1A g in current density
-1under, its specific capacity is 486F g
-1.
Claims (1)
1. on micro-carbon pipe, growth is oxidized a preparation method for the electrode material for super capacitor of nickel nano film, it is characterized in that comprising following steps:
(1) first the catkin collected be impregnated in ethanol solution, and ultrasonic disperse 10-60 min, obtain the catkin sample cleaned up, then the catkin sample cleaned up is loaded carbide furnace, at 500-1000 under protective atmosphere
oCunder carry out carbonization, obtain micro-carbon pipe;
(2) by micro-carbon pipe: N, N dimethyl formamide=0.1-0.5 g:50-100 ml, joins N by micro-carbon pipe, in N dimethyl formamide, through ultrasonic, obtains solution A;
(3) by Ni (NO
3)
26H
2o: deionized water=1 g: 10-100 ml, by Ni (NO
3)
26H
2o powder dissolves in deionized water, forms solution B, then solution A is dropwise slowly added in solution B, fully stir;
(4) mixed solution step (3) obtained is at 100-250
obetween C, hydro-thermal reaction 12-36 h, is cooled to room temperature;
(5) product suction filtration step (4) obtained also uses deionized water cyclic washing, dries, finally, under protective atmosphere, and 150-500
oc calcines and within 4 hours, obtains nickel oxide nano sheet/micro-carbon pipe composite material.
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| CN201510232508.9A CN104916451A (en) | 2015-05-08 | 2015-05-08 | Method for preparing super capacitor electrode material made of nickel oxide nanosheet grown on micro carbon tube |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110002429A (en) * | 2019-05-09 | 2019-07-12 | 中国科学院山西煤炭化学研究所 | Carbon micron tube/transition metal hydroxide combination electrode material and preparation method thereof |
| CN110660968A (en) * | 2019-09-17 | 2020-01-07 | 天津大学 | Composite lithium metal negative electrode and preparation method thereof |
| CN111341567A (en) * | 2020-03-02 | 2020-06-26 | 齐鲁工业大学 | 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and preparation method thereof |
| CN113036166A (en) * | 2021-03-04 | 2021-06-25 | 哈尔滨工程大学 | Porous CoNi-coated carbon microtubule H2O2 electro-oxidation electrode prepared from endive flower template |
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|---|---|---|---|---|
| CN101549865A (en) * | 2009-05-12 | 2009-10-07 | 复旦大学 | Method for modifying carbon nano-tube by nickel nanometer particles |
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| CN113036166A (en) * | 2021-03-04 | 2021-06-25 | 哈尔滨工程大学 | Porous CoNi-coated carbon microtubule H2O2 electro-oxidation electrode prepared from endive flower template |
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