CN104773762A - NiCo2O4 mesoporous nanotube material grown on carbon fiber cloth and preparation method thereof - Google Patents
NiCo2O4 mesoporous nanotube material grown on carbon fiber cloth and preparation method thereof Download PDFInfo
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- CN104773762A CN104773762A CN201510114920.0A CN201510114920A CN104773762A CN 104773762 A CN104773762 A CN 104773762A CN 201510114920 A CN201510114920 A CN 201510114920A CN 104773762 A CN104773762 A CN 104773762A
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Abstract
The invention discloses a NiCo2O4 mesoporous nanotube material grown on carbon fiber cloth. The NiCo2O4 mesoporous nanotube material grows on a carbon fiber cloth substrate and is composed of NiCo2O4 nano crystals with a particle size of 5 to 10 nm; the internal diameter of the NiCo2O4 mesoporous nanotube material is 20 to 50 nm, the wall thickness is 10 to 20 nm, the tube length is 0.5 to 2.0 [mu]m, and the length/diameter ratio is 250 to 1000; the mesopores are gaps between the NiCo2O4 nano crystals and the size of the mesopores is in a range of 2 to 5 nm. The invention further provides a preparation method of the NiCo2O4 mesoporous nanotube material. By precisely controlling the hydrothermal reaction conditions, the NiCo2O4 mesoporous nanotube material with a special structure can grow on carbon fiber cloth. The NiCo2O4 mesoporous nanotube material can be used to produce the electrode of a super capacitor, and has the advantages of high specific capacitance, rate capability under a large current density, and long-term cycle performance.
Description
Technical field
The present invention relates to the preparation field of nano material, particularly relate to the NiCo of a kind of growth on carbon cloth
2o
4meso-porous nano tube material and preparation method thereof.
Background technology
Transition metal oxide is as NiO, Co
3o
4, MnO
2, NiCo
2o
4deng aboundresources, cheap, theoretical ratio capacitance is high, and electrochemical reversibility is good, is considered to a kind of electrode material for super capacitor had a extensive future.Wherein, the transiton metal binary oxides NiCo of spinel structure
2o
4because of advantages such as its theoretical specific capacity is high, Stability Analysis of Structures, good cycle, receive extensive concern.Because fake capacitance reaction mainly occurs in material surface, the material with high specific surface area will have higher actual specific electric capacity, and high rate during charging-discharging also can be better, therefore by NiCo
2o
4make nano material, utilize the bigger serface characteristic of nano material to be an effective strategy to improve its chemical property, NiCo
2o
4the multiple nanostructures such as nano wire, nanometer rod and nanometer sheet have report in recent years, all show higher electrochemical capacitance performance.
NiCo
2o
4primary synthetic methods have: high temperature solid-state method, mechanochemical synthesis, sol-gel method, liquid phase chemical coprecipitation method, co-precipitation thermolysis and hydrothermal method etc., high temperature solid-state method is traditional synthetic method, although technique is simple, due to NiCo
2o
4the character of poor heat stability, decomposed between 400-600 DEG C, some is active in catalytic activity reduction to make it.Mechanical activation synthesis method, introduces a large amount of strain and defect, products therefrom bad dispersibility in preparation process.Sol-gel method is less and be evenly distributed by the product grain particle diameter that adds tensio-active agent and obtain, but easily introduces impurity.And the product structure of liquid chemical precipitation method synthesis is imperfect, can generating portion metastable phase.
At present, co-precipitation thermolysis and the hydrothermal method of adopting prepares NiCo more
2o
4.As the publication number Chinese patent literature that is CN103318978A discloses a kind of preparation method of mesoporous cobalt acid nickel, with soluble nickel salt, cobalt salt for raw material, oxalate is precipitation agent, at Ni
2+-Co
2+-NH
3-NH
4 +-SG
n--Co
2o
4 2-H
2o-C
2h
5prepare fibrous presoma in OH system, be then placed in 250-400 DEG C of temperature, air atmosphere thermolysis obtains mesoporous NiCo
2o
4fiber.And for example publication number is method and the application thereof that the Chinese patent literature of CN102745752A discloses a kind of water heat transfer mesoporous cobalt acid nickel nano wire, by CoCl
2.6H
2o, NiCl
2.6H
2o and CO (NH
2) be dissolved in appropriate amount of deionized water, wherein CoCl
2.6H
2o and NiCl
2.6H
2the mol ratio of O is 1:2, utilizes magnetic stirring apparatus stirred by mixing solutions and be transferred in autoclave, is heated to 100 DEG C, constant temperature 10h.To be cooled to room temperature, by reactant filter, washing, after drying in air atmosphere 250 DEG C annealing 2h.But the product that aforesaid method prepares respectively is fibrous texture.
At present, for NiCo
2o
4nano-tube material also have research, but mainly adopt method of electrostatic spinning preparation, thick with the standby nanotube caliber of this legal system, residual organic matter can reduce NiCo
2o
4specific conductivity, it makes the slurry-scraping method that electrode of super capacitor generally adopts mixed chemical glue and conductive agent, and the electrode interior material dense packing made, internal resistance are comparatively large, and these factors reduce Ni nanoparticle Co
2o
4nanometer size effect, be unfavorable for the further improvement of electrochemical capacitance performance.In addition, although NiCo
2o
4specific conductivity is higher, but with carbon material and metal oxide containing precious metals phase specific conductivity or not high enough, under high current density, ratio capacitance decay is very fast, high rate performance is poor, existing research or with high conductive material compound, as with the compound such as carbon nanotube, Graphene, or by NiCo
2o
4be grown directly upon in the metal base such as nickel foam, but be limited to NiCo
2o
4the restriction of material structure and base material, electrochemical capacitance improvement in performance is limited.
Summary of the invention
The invention provides the NiCo of a kind of growth on carbon cloth
2o
4the preparation method of meso-porous nano tube material, by the accurate control to hydrothermal reaction condition, carbon cloth grown the NiCo with special construction
2o
4meso-porous nano tube material, when using as electrode material for super capacitor, possesses high ratio capacitance, the high rate performance under high current density and long-term cycle performance.
The NiCo of a kind of growth on carbon cloth
2o
4meso-porous nano tube material, NiCo
2o
4meso-porous nano tube material grows in carbon cloth substrate, described NiCo
2o
4meso-porous nano tube material is the NiCo of 5 ~ 10nm by particle diameter
2o
4nanocrystallinely assemble, internal diameter is 20 ~ 50nm, and wall thickness is 10 ~ 20nm, and pipe range is 0.5 ~ 2.0 μm, and length-to-diameter ratio is 250 ~ 1000; Described mesoporous be NiCo
2o
4hole between nanocrystalline, mesopore size is 2 ~ 5nm.
A kind of described NiCo of growth on carbon cloth
2o
4the preparation method of meso-porous nano tube material, concrete steps are as follows:
Be stoichiometrically that 42 ~ 48:1:2:6 ~ 8 mix with deionized water by urea, nickelous nitrate, cobalt chloride and vulkacit H, dissolve completely and obtain precursor solution, carbon cloth is placed in precursor solution, through hydro-thermal reaction 6 ~ 8h at 90 ~ 110 DEG C, then obtain the NiCo of described growth on carbon cloth through washing, drying and thermal treatment
2o
4meso-porous nano tube material.
After adding substrate, at substrate surface fabricated in situ by NiCo
2o
4the nanocrystalline NiCo assembled
2o
4meso-porous nano tube material.
As preferably, Ni in described precursor solution
2+concentration is 2.6 ~ 3.2g/L.
Described nickelous nitrate also can be Nickelous nitrate hexahydrate, and cobalt chloride is cobalt chloride hexahydrate.
As preferably, described hydro-thermal reaction is carried out in tetrafluoroethylene reactor, and the compactedness of described reactor is 60 ~ 80%.Further preferably, described hydrothermal temperature is 95 ~ 105 DEG C.
As preferably, described carbon cloth is of a size of 2 × 2cm
2.
As preferably, described drying temperature is 70 DEG C.
As preferably, described thermal treatment is carried out under protection of inert gas, and thermal treatment temp is 300 ~ 400 DEG C, and soaking time is 2 ~ 6h.
Growth prepared by the present invention NiCo on carbon cloth
2o
4meso-porous nano tube material is a kind of excellent electrode material for super capacitor, is that the nanocrystalline of 5 ~ 10nm assembles by particle diameter, and small particle size material significantly can reduce electronics, ion in the transmission range of material internal, improves large current density power; Material specific surface area is large, and skin-material accounting is high, can significantly improve NiCo
2o
4discharge and recharge utilising efficiency; NiCo
2o
4have the hole being of a size of 2 ~ 5nm between nanocrystalline, make tube wall present meso-hole structure, simultaneously material center also has a larger hollow pipeline, and these structural characteristics make to construct NiCo
2o
4the inside and outside crystal grain of meso-porous nano pipe all facilitates and fully touches electrolytic solution, and the bigger serface of material by efficiently and effectively utilize, thus significantly improves NiCo
2o
4ratio capacitance, the high rate performance under high current density and long-term cycle performance.The carbon cloth of Choice of substrate materials high connductivity.The carbon cloth be made up of neat carbon fiber, can ensure that growth is at suprabasil NiCo
2o
4nano-tube material fully contacts with electrolytic solution, increases effective contact area, is conducive to electronics, the ion fast transport in electrode simultaneously, can strengthens NiCo
2o
4electroconductibility.The NiCo of growth
2o
4electrode materials maintains suitable space each other, reduces the resistance that electrolyte ion interts between electrode materials, also can promote NiCo
2o
4utilization ratio, improve NiCo under high current charge-discharge condition
2o
4multiplying power property.
Compared with prior art, tool of the present invention has the following advantages:
The present invention, by the accurate control to hydrothermal reaction condition, has prepared the NiCo of a kind of growth on carbon cloth
2o
4meso-porous nano tube material, this NiCo
2o
4meso-porous nano tube material possesses special pattern, when using as electrode material for super capacitor, possesses high ratio capacitance, the high rate performance under high current density and long-term cycle performance.
Accompanying drawing explanation
Fig. 1 and Fig. 2 is respectively the NiCo of growth on carbon cloth prepared by embodiment 1
2o
4the SEM figure of meso-porous nano tube material under different amplification, the illustration of Fig. 1 is NiCo
2o
4the partial enlargement SEM of meso-porous nano pipe schemes.
Fig. 3 is NiCo prepared by embodiment 1
2o
4the XRD spectra of meso-porous nano tube material.
Embodiment
Embodiment 1
Get 0.32g Ni (NO
3)
26H
2o, 0.53g CoCl
26H
2o, 2.97g CO (NH
2)
2and 1.1gN
4(CH
2)
6be dissolved in 100mL deionized water, to dissolving the pink colour solution forming clarification completely; Then 60mL solution is transferred in the autoclave of 100mL, then by 2 × 2cm that one piece cleans up
2carbon cloth be positioned over solution, put into baking oven after reactor is airtight, be heated to 95 DEG C; soaking time 8h; carbon cloth after hydro-thermal reaction is taken out rear washed with de-ionized water, 70 DEG C of oven dry, then be placed in the quartz tube furnace anneal under protection of inert gas; Heating temperature is 350 DEG C; soaking time is 3h, to be cooled to room temperature taking-up sample, finds its SEM atlas analysis; as illustrated in fig. 1 and 2, the NiCo on carbon cloth is grown
2o
4present nanotube morphologies, bore is about 40nm, and thickness of pipe is about 20nm, pipe range about 1.2 μm, length-to-diameter ratio about 300.To nanometer mouth of pipe amplifying observation, as shown in Fig. 1 illustration, NiCo
2o
4nanotube is assembled by nanocrystalline, nanocrystalline particle diameter about 5 ~ 10nm, there is the mesoporous of size about 2 ~ 5nm between nanocrystalline.The aqueous solution is placed in sample and uses vibration of ultrasonic wave, shake off powder and regather and carry out XRD material phase analysis, shown in Fig. 3, the diffraction peak of sample and NiCo
2o
4(JCPDS 20-0781) fits like a glove, and there is no other impurity peaks and exists, show that product is high-purity NiCo
2o
4material.
Embodiment 2
Get 0.29g Ni (NO
3)
26H
2o, 0.48g CoCl
26H
2o, 2.50g CO (NH
2)
2and 1gN
4(CH
2)
6be dissolved in 100mL deionized water, to dissolving the pink colour solution forming clarification completely; Then 80mL solution is transferred in the autoclave of 100mL, then by 2 × 2cm that one piece cleans up
2carbon cloth be positioned over solution; put into baking oven after reactor is airtight, be heated to 100 DEG C, insulation reaction 8h; carbon cloth after hydro-thermal reaction is taken out rear washed with de-ionized water; 70 DEG C of oven dry, then be placed in the quartz tube furnace anneal under protection of inert gas, Heating temperature is 380 DEG C; soaking time is 2h; to be cooled to room temperature taking-up sample, the discovery of SEM atlas analysis is carried out to it, grows the NiCo on carbon cloth
2o
4the nanocrystalline particle diameter about 5 ~ 10nm of meso-porous nano tube material, mesopore size is 2 ~ 5nm about, and bore is about 30nm, and thickness of pipe is about 16nm, pipe range about 0.9 μm, length-to-diameter ratio about 300.
Embodiment 3
Get 0.26g Ni (NO
3)
26H
2o, 0.43g CoCl
26H
2o, 2.43g CO (NH
2)
2and 0.9gN
4(CH
2)
6be dissolved in 100mL deionized water, to dissolving the pink colour solution forming clarification completely; Then 80mL solution is transferred in the autoclave of 100mL, then by 2 × 2cm that one piece cleans up
2carbon cloth be positioned over solution, put into baking oven after reactor is airtight, be heated to 105 DEG C, soaking time 6h, 70 DEG C of oven dry; Be placed in the quartz tube furnace anneal under protection of inert gas again, Heating temperature is 300 DEG C, and soaking time is 6h, to be cooled to room temperature taking-up sample, finds, grow the NiCo on carbon cloth to its SEM atlas analysis
2o
4the nanocrystalline particle diameter about 5 ~ 10nm of meso-porous nano tube material, mesopore size is 2 ~ 5nm about, and bore is about 20nm, and thickness of pipe is about 12nm, pipe range 0.6 μm, length-to-diameter ratio about 300.
Claims (8)
1. the NiCo of growth on carbon cloth
2o
4meso-porous nano tube material, is characterized in that, NiCo
2o
4meso-porous nano tube material grows in carbon cloth substrate, described NiCo
2o
4meso-porous nano tube material is the NiCo of 5 ~ 10nm by particle diameter
2o
4nano-crystalline granule assembles, and internal diameter is 20 ~ 50nm, and wall thickness is 10 ~ 20nm, and pipe range is 0.5 ~ 2.0 μm, and length-to-diameter ratio is 250 ~ 1000; Described mesoporous be NiCo
2o
4hole between nanocrystalline, mesopore size is 2 ~ 5nm.
2. the NiCo of growth according to claim 1 on carbon cloth
2o
4the preparation method of meso-porous nano tube material, is characterized in that, step is as follows:
Be stoichiometrically that 42 ~ 48:1:2:6 ~ 8 mix with deionized water by urea, nickelous nitrate, cobalt chloride and vulkacit H, dissolve completely and obtain precursor solution, carbon cloth is placed in precursor solution, through hydro-thermal reaction 6 ~ 8h at 90 ~ 110 DEG C, then obtain the NiCo of described growth on carbon cloth through washing, drying and thermal treatment
2o
4meso-porous nano tube material.
3. the NiCo of growth according to claim 2 on carbon cloth
2o
4the preparation method of meso-porous nano tube material, is characterized in that, Ni in described precursor solution
2+concentration is 2.6 ~ 3.2g/L.
4. the NiCo of growth according to claim 2 on carbon cloth
2o
4the preparation method of meso-porous nano tube material, is characterized in that, described hydro-thermal reaction is carried out in tetrafluoroethylene reactor, and the compactedness of described reactor is 60 ~ 80%.
5. the NiCo of growth according to claim 4 on carbon cloth
2o
4the preparation method of meso-porous nano tube material, is characterized in that, described hydrothermal temperature is 95 ~ 105 DEG C.
6. the NiCo of growth according to claim 2 on carbon cloth
2o
4the preparation method of meso-porous nano tube material, is characterized in that, described carbon cloth is of a size of 2 × 2cm
2.
7. the NiCo of growth according to claim 2 on carbon cloth
2o
4the preparation method of meso-porous nano tube material, is characterized in that, described drying temperature is 70 DEG C.
8. the NiCo of growth according to claim 2 on carbon cloth
2o
4the preparation method of meso-porous nano tube material, is characterized in that, described thermal treatment is carried out under protection of inert gas, and thermal treatment temp is 300 ~ 400 DEG C, and soaking time is 2 ~ 6h.
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|---|---|---|---|
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Cited By (12)
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|---|---|---|---|---|
| CN105070515A (en) * | 2015-08-19 | 2015-11-18 | 华东理工大学 | Foamed nickel composite material, and preparation method and application thereof |
| CN105225844A (en) * | 2015-09-09 | 2016-01-06 | 南京航空航天大学 | The preparation method of nitrogen-doped graphene/nitrogen-doped carbon nanometer pipe/cobalt acid zinc composite material and application |
| CN105417590A (en) * | 2015-11-24 | 2016-03-23 | 青岛能迅新能源科技有限公司 | Method for synthesizing nickel cobaltate spinel |
| CN106299271A (en) * | 2016-08-23 | 2017-01-04 | 南京理工大学 | Nano nickel cobaltate/graphene composite material and preparation method thereof |
| CN107195470A (en) * | 2017-05-27 | 2017-09-22 | 中国海洋大学 | Nanotube-shaped composite of nickel cobalt iron ternary metal oxide and preparation method thereof |
| CN107740136A (en) * | 2017-10-16 | 2018-02-27 | 太原理工大学 | A kind of preparation method of the order mesoporous cathode composite of MEC |
| CN107774264A (en) * | 2017-09-19 | 2018-03-09 | 浙江工商大学 | Load composite oxides magnetic nanometer and the electrode of CNT and its preparation and application |
| CN107993849A (en) * | 2017-11-27 | 2018-05-04 | 陕西科技大学 | A kind of flexible electrode material of carbon fiber loaded cobalt acid nickel nano-array and preparation method thereof |
| CN108010733A (en) * | 2017-12-25 | 2018-05-08 | 电子科技大学 | A kind of flower-shaped Cu2SnS3The preparation method of flexible super capacitor electrode material |
| CN109148163A (en) * | 2017-06-16 | 2019-01-04 | 南京理工大学 | Carbon cloth/cobalt acid nickel nickel flexible electrode material and preparation method thereof |
| CN109216663A (en) * | 2017-06-30 | 2019-01-15 | 南京理工大学 | A kind of nano particle/carbon cloth combination electrode material and preparation method thereof |
| CN114632536A (en) * | 2022-04-01 | 2022-06-17 | 吉林化工学院 | NiCo with photocatalytic properties2O4/NiO/g-C3N4Nanotube preparation method and application |
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| CN105070515A (en) * | 2015-08-19 | 2015-11-18 | 华东理工大学 | Foamed nickel composite material, and preparation method and application thereof |
| CN105225844A (en) * | 2015-09-09 | 2016-01-06 | 南京航空航天大学 | The preparation method of nitrogen-doped graphene/nitrogen-doped carbon nanometer pipe/cobalt acid zinc composite material and application |
| CN105417590A (en) * | 2015-11-24 | 2016-03-23 | 青岛能迅新能源科技有限公司 | Method for synthesizing nickel cobaltate spinel |
| CN105417590B (en) * | 2015-11-24 | 2016-10-05 | 青岛能迅新能源科技有限公司 | A kind of method synthesizing cobalt acid nickel spinelle |
| CN106299271A (en) * | 2016-08-23 | 2017-01-04 | 南京理工大学 | Nano nickel cobaltate/graphene composite material and preparation method thereof |
| CN107195470B (en) * | 2017-05-27 | 2019-05-10 | 中国海洋大学 | The nanotube-shaped composite material and preparation method of nickel cobalt iron ternary metal oxide |
| CN107195470A (en) * | 2017-05-27 | 2017-09-22 | 中国海洋大学 | Nanotube-shaped composite of nickel cobalt iron ternary metal oxide and preparation method thereof |
| CN109148163A (en) * | 2017-06-16 | 2019-01-04 | 南京理工大学 | Carbon cloth/cobalt acid nickel nickel flexible electrode material and preparation method thereof |
| CN109148163B (en) * | 2017-06-16 | 2020-10-30 | 南京理工大学 | Carbon cloth/nickel cobaltate/nickel oxide flexible electrode material and preparation method thereof |
| CN109216663A (en) * | 2017-06-30 | 2019-01-15 | 南京理工大学 | A kind of nano particle/carbon cloth combination electrode material and preparation method thereof |
| CN107774264A (en) * | 2017-09-19 | 2018-03-09 | 浙江工商大学 | Load composite oxides magnetic nanometer and the electrode of CNT and its preparation and application |
| CN107740136A (en) * | 2017-10-16 | 2018-02-27 | 太原理工大学 | A kind of preparation method of the order mesoporous cathode composite of MEC |
| CN107993849A (en) * | 2017-11-27 | 2018-05-04 | 陕西科技大学 | A kind of flexible electrode material of carbon fiber loaded cobalt acid nickel nano-array and preparation method thereof |
| CN108010733A (en) * | 2017-12-25 | 2018-05-08 | 电子科技大学 | A kind of flower-shaped Cu2SnS3The preparation method of flexible super capacitor electrode material |
| CN114632536A (en) * | 2022-04-01 | 2022-06-17 | 吉林化工学院 | NiCo with photocatalytic properties2O4/NiO/g-C3N4Nanotube preparation method and application |
| CN114632536B (en) * | 2022-04-01 | 2023-10-20 | 吉林化工学院 | NiCo with photocatalytic properties 2 O 4 /NiO/g-C 3 N 4 Nanotube preparation method and application |
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