CN107195470B - The nanotube-shaped composite material and preparation method of nickel cobalt iron ternary metal oxide - Google Patents
The nanotube-shaped composite material and preparation method of nickel cobalt iron ternary metal oxide Download PDFInfo
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- CN107195470B CN107195470B CN201710393193.5A CN201710393193A CN107195470B CN 107195470 B CN107195470 B CN 107195470B CN 201710393193 A CN201710393193 A CN 201710393193A CN 107195470 B CN107195470 B CN 107195470B
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- 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
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of nanotube-shaped composite material and preparation methods of nickel cobalt iron ternary metal oxide.Carbon cloth is pre-processed first, it is dry；Using distilled water as solvent, the mixed solution of cobalt chloride hexahydrate, Nickel dichloride hexahydrate, cetyl trimethylammonium bromide and urea is prepared, it is put into reaction kettle with carbon cloth and carries out hydro-thermal reaction, NiCo is made2O4Presoma.Ferric chloride hexahydrate is added in the presoma prepared and carries out water-bath, NiCo is finally made2‑xFexO4Nanotube-shaped composite material.Prepared composite material is due to tubular structure in the present invention, and is nano-scale particle, and the specific surface area of material has been significantly greatly increased, has accelerated electrode reaction dynamics, has improved its electrochemical capacitance performance.The composite material has excellent invertibity and cyclical stability.Preparation method of the invention is easy to operate, low in cost, has broad application prospects in fields such as energy stores, catalyst.
Description
Technical field
The present invention relates to a kind of preparation field of super capacitor material, follow more particularly to a kind of good reversibility and for a long time
The stable nanotube-shaped supercapacitor composite material and preparation method of nickel cobalt iron ternary metal oxide of ring.
Background technique
With the burning of fossil fuel, the consumption of non-renewable resources and increasingly increased problem of environmental pollution, need
People develop and use renewable and clean energy resource.Based on economize on resources, the reason of the energy and environmental protection, novel green energy-storage travelling wave tube by
Gradually grow up.Due to energy density high, charge and discharge rapidly, it is invertibity and good cycling stability, environmental-friendly, at low cost
The advantages such as honest and clean, supercapacitor are a kind of novel, practical, efficient energy storage devices.
Electrode material plays very important effect in the component part of supercapacitor.Instantly to the spy of electrode material
Rope and to study intensively dense convergence all very high in preparation specific capacity, energy density, power density, and large current density can be carried out
Electricity, while having the active material of high performance-price ratio as electrode again.In recent years, since its fake capacitance performance is prominent, abundance,
It is at low cost, the advantages such as environmental-friendly, transition metal oxide NiCo2O4It is widely used in super capacitor material.Wei etc.
NiCo is synthesized using sol-gel method2O4Nano particle, capacitive property are greatly improved (1400 Fg−1) and have very
Good invertibity and cyclical stability (Wei T Y, Chen C H, Chien H C, et al. (2010) Advanced
Materials, 22 (3): 347-351.).Shen etc. has synthesized NiCo using hydro-thermal method2O4Nanowire composite is presented
Excellent capacitance characteristic and cyclical stability (Shen L, Che Q, Li H, et al. (2014) Advanced are gone out
Functional Materials, 24 (18): 2630-2637.).But NiCo2O4With relatively poor electric conductivity and compared with
Small specific surface area, so that its actual capacitance is much smaller than theoretical capacity.
Summary of the invention
In view of the above-mentioned problems, large specific surface area, capacitive character is high, reversible the object of the present invention is to provide a kind of good conductivity
Good, the lasting nanotube-shaped composite material of nickel cobalt iron ternary metal oxide of cyclical stability of property.
It is a further object to provide a kind of preparation process is simple, reaction condition is mild, and preparation cost is cheap
The nanotube-shaped composite material and preparation method thereof of nickel cobalt iron ternary metal oxide.
The nanotube-shaped composite material of nickel cobalt iron ternary metal oxide of the invention is on carbon cloth using hydro-thermal method
Synthesize NiCo2O4Presoma makes NiCo2O4It can be uniformly coated on carbon cloth, enhance its attachment on carbon cloth；
Then NiCo is synthesized using immersion method2-xFexO4The specific surface of material has been significantly greatly increased in nanotube-shaped composite material, tubular structure
Product, accelerates electrode reaction dynamics, improves its electrochemical capacitance performance.The composite material has better invertibity and circulation steady
It is qualitative.
The nanotube-shaped composite material of nickel cobalt iron ternary metal oxide of the present invention, including carbon cloth, it is coated on carbon fiber
Nickel cobalt iron ternary metal oxide nanotube on cloth, the molecular composition of the nickel cobalt iron ternary metal oxide are NiCo2- xFexO4, x=0.2 ~ 1.2；Its tubular structure is Co element oxide nucleation, introduces Fe3+Afterwards by part Co3+Atomic substitutions, Ni, Co,
Fe, O element collectively constitute tube wall, Fe3+Replace part Co3+Form hollow structure.
The nickel cobalt iron ternary metal oxide nanometer pipe outside diameter is 100 ~ 300 nm, and thickness of pipe wall is 30 ~ 100 nm.
The preparation method of the nanotube-shaped composite material of nickel cobalt iron ternary metal oxide of the present invention includes the following steps:
(1) pretreatment of basis material:
First carbon fiber cloth material ultrasound is pre-processed, is then cleaned up, drying is stand-by；
(2) hydro-thermal method prepares NiCo2O4Presoma:
Using distilled water as solvent, cobalt chloride hexahydrate, Nickel dichloride hexahydrate, cetyl trimethylammonium bromide are prepared
(CTAB) and the mixed solution of urea, by the pretreated carbon fiber cloth material of step (1) and mixed liquor be put into reaction kettle into
Row hydro-thermal reaction, it is then that resulting product distilled water and washes of absolute alcohol is clean, NiCo is made2O4Presoma；
(3) immersion method prepares NiCo2-xFexO4(x value range is 0.2 ~ 1.2) nanotube-shaped composite material:
Using distilled water as solvent, by presoma and ferric chloride hexahydrate prepared in step (2) be added in beaker into
Row heating in water bath for reaction, obtained product distilled water and washes of absolute alcohol is clean, calcines after drying, finally obtains NiCo2- xFexO4Nanotube-shaped composite material.
The preprocess method of carbon fiber cloth material described in step (1) is, respectively at dehydrated alcohol and distilled water ultrasound
It manages, is dried at 60 DEG C.
Cobalt chloride hexahydrate described in step (2), Nickel dichloride hexahydrate, CTAB and urea molal weight ratio be 10:5:
4:18。
The temperature of step (2) described hydro-thermal reaction is 80 ~ 150 DEG C, and the time is 12 ~ 24 h.
The molar concentration that iron is added in step (3) is 0.1 ~ 2 mol/L.
The temperature of heating in water bath for reaction described in step (3) is 60 ~ 120 DEG C, and the time is 0.5 ~ 3 h；The temperature of calcining is
300 DEG C, the time is 3 h.
Application of the above-mentioned prepared nanotube-shaped composite material of nickel cobalt iron ternary metal oxide in supercapacitor.
Compared with existing super capacitor material, the present invention has the advantage that
(1) carbon cloth does matrix, and carbon cloth is conductive good, the advantages such as mechanical strength is good, and flexibility is good.
(2) NiCo being grown directly upon on carbon cloth matrix2O4Presoma improves the electric conductivity of electronics and forthright again
Energy.
(3) NiCo prepared by the present invention2-xFexO4Composite material is nano tubular structure, greatly improves material
Specific surface area can provide more electroactive materials.As super capacitor material, there is preferable cyclic reversibility and stabilization
Property.
(4) preparation method of the invention is easy to operate, low in cost, has a extensive future.
Detailed description of the invention
Fig. 1 is the stereoscan photograph (a) of blank carbon cloth；Partial enlargement pattern (b).
Fig. 2 is NiCo prepared by embodiment 12O4Presoma stereoscan photograph (a)；The pattern (b) of partial enlargement.
Fig. 3 is NiCo prepared by embodiment 12-xFexO4Nanotube-shaped composite material stereoscan photograph (a)；It puts part
Big pattern (b).
Fig. 4 is NiCo prepared by embodiment 12-xFexO4Nanotube-shaped composite material EDS figure.
Fig. 5 is NiCo prepared by embodiment 12-xFexO4Nanotube-shaped composite material charge-discharge test curve.
Specific embodiment
The present invention will be described in detail with reference to the accompanying drawing and by specific embodiment, so that advantages of the present invention and spy
Sign can be easier to be understood by the person skilled in the art, to make apparent specific boundary to protection scope of the present invention
It is fixed.
Embodiment 1:
(1) carbon cloth pre-processes: by the carbon cloth of 30 × 30 × 0.1 mm respectively in dehydrated alcohol and distilled water
15 min of ultrasound are cleaned and are dried and weigh.
(2) Hydrothermal Growth NiCo2O4Presoma: taking 50 ml distilled water, 1.1897 g cobalt chloride hexahydrates, and 0.5942
G Nickel dichloride hexahydrate, 0.7289 g CTAB, 0.5405 g urea, be added 200 ml beakers in, be sufficiently mixed uniformly after with
Handled carbon cloth, which is added together in the water heating kettle of polytetrafluoroethyllining lining, in step (1) carries out hydro-thermal reaction, at 100 DEG C
React 12 h.To after reaction, take out sample, cleaned up with deionized water, drying weighing.
(3) immersion method prepares NiCo2-xFexO4Nanotube-shaped composite material: it takes made in 50 ml distilled water and step (2)
Standby material is added in 200 ml beakers, heating water bath.Taking ferric chloride hexahydrate, (molar concentration in terms of iron is 0.1mol/
L it) is dissolved in distilled water, is added when water-bath is to 100 DEG C and contains Fe3+Solution, the reaction was continued 2 h.To after reaction, with steaming
Distilled water cleans up drying.
(4) material prepared by step (3) is calcined into 3 h at 300 DEG C.
Embodiment 2:
(1) carbon cloth pre-processes: by the carbon cloth of 30 × 30 × 0.1 mm respectively in dehydrated alcohol and distilled water
15 min of ultrasound are cleaned and are dried and weigh.
(2) Hydrothermal Growth NiCo2O4Presoma: taking 50 ml distilled water, 1.1897 g cobalt chloride hexahydrates, and 0.5942
G Nickel dichloride hexahydrate, 0.7289 g CTAB, 0.5405 g urea, be added 200 ml beakers in, be sufficiently mixed uniformly after with
Handled carbon cloth, which is added together in the water heating kettle of polytetrafluoroethyllining lining, in step (1) carries out hydro-thermal reaction, at 100 DEG C
React 24 h.To after reaction, take out sample, cleaned up with deionized water, drying weighing.
(3) immersion method prepares NiCo2-xFexO4Nanotube-shaped composite material: it takes made in 50 ml distilled water and step (2)
Standby material is added in 200 ml beakers, heating water bath.Taking ferric chloride hexahydrate, (molar concentration in terms of iron is 0.2
Mol/L it) is dissolved in distilled water, is added when water-bath is to 90 DEG C and contains Fe3+Solution, the reaction was continued 1.5 h.To the end of reacting
Afterwards, clean drying wash with distilled water.
(4) material prepared by step (3) is calcined into 3 h at 300 DEG C.
Embodiment 3:
(1) carbon cloth pre-processes: by the carbon cloth of 30 × 30 × 0.1 mm respectively in dehydrated alcohol and distilled water
15 min of ultrasound are cleaned and are dried and weigh.
(2) Hydrothermal Growth NiCo2O4Presoma: taking 50 ml distilled water, 1.1897 g cobalt chloride hexahydrates, and 0.5942
G Nickel dichloride hexahydrate, 0.7289 g CTAB, 0.5405 g urea, be added 200 ml beakers in, be sufficiently mixed uniformly after with
Handled carbon cloth, which is added together in the water heating kettle of polytetrafluoroethyllining lining, in step (1) carries out hydro-thermal reaction, at 120 DEG C
React 24 h.To after reaction, take out sample, cleaned up with deionized water, drying weighing.
(3) immersion method prepares NiCo2-xFexO4Nanotube-shaped composite material: it takes made in 50 ml distilled water and step (2)
Standby material is added in 200 ml beakers, heating water bath.Taking ferric chloride hexahydrate, (molar concentration in terms of iron is 1 mol/
L it) is dissolved in distilled water, is added when water-bath is to 120 DEG C and contains Fe3+Solution, the reaction was continued 2 h.To after reaction, with steaming
Distilled water cleans up drying.
(4) material prepared by step (3) is calcined into 3 h at 300 DEG C.
Sample is characterized:
To understand growing state of the prepared nanocomposite on carbon cloth, scanning electron microscopic observation sample is utilized
Surface topography, the result is shown in Figure 1, Fig. 2, Fig. 3；EDS characterization is carried out to prepared nanocomposite constituents, as a result sees Fig. 4,
In can be calculated by EDS data, NiCo in embodiment 12-xFexO4The value of x be 0.2, x value is 0.3 in embodiment 2,
X value is 0.5 in embodiment 3.Fig. 1 is blank carbon cloth scanned photograph.Fig. 2 is the NiCo of Hydrothermal Growth2O4Presoma,
As seen from the figure, NiCo2O4Presoma is uniformly coated on carbon cloth.As seen from Figure 3, NiCo2O4Forerunner
Body has had changed into tubulose (65 nm of tube wall, 300 nm of outer diameter), and coats more uniform.
Embodiment 4:
By the NiCo of preparation2-xFexO4The working electrode of 1 × 1 cm, saturated calomel electrode is made in nanotube-shaped composite material
For reference electrode, platinum electrode is that charge-discharge test is carried out in the KOH solution of 6 mol/L to electrode, as a result such as Fig. 5.Charge and discharge
Current density is respectively 1,2,4,8,10,20 A/g, and capacitance size is respectively 2057,1912,1650,1400,1045,950
F/g.It can be seen that NiCo prepared in the present invention2-xFexO4Nanotube-shaped composite material has good capacitance characteristic.
Claims (9)
1. a kind of nanotube-shaped composite material of nickel cobalt iron ternary metal oxide, it is characterised in that it includes carbon cloth, cladding
Nickel cobalt iron ternary metal oxide nanotube on carbon cloth, the nickel cobalt iron ternary metal oxide nanometer pipe outside diameter
For 100~300 nm, thickness of pipe wall is 30~100 nm；The molecular composition of the nickel cobalt iron ternary metal oxide is NiCo2- xFexO4, x=0.2~1.2；Its tubular structure is Co element oxide nucleation, introduces Fe3+Afterwards by part Co3+Atomic substitutions, Ni,
Co, O, Fe element collectively constitute tube wall, Fe3+Replace part Co3+Form hollow structure.
2. a kind of preparation method of the nanotube-shaped composite material of ternary metal oxide, feature the following steps are included:
(1) basis material pre-processes: carbon cloth basis material is first subjected to ultrasonic pretreatment, is then cleaned up, drying to
With；
(2) hydro-thermal method prepares NiCo2O4Presoma: using distilled water as solvent, cobalt chloride hexahydrate, Nickel dichloride hexahydrate, ten are prepared
The mixed solution of six alkyl trimethyl ammonium bromides and urea, by the pretreated carbon fiber cloth material of step (1) and mixed solution
It is put into reaction kettle and carries out hydro-thermal reaction, it is then that resulting product distilled water and washes of absolute alcohol is clean, it is made
NiCo2O4Forerunner's composite material；
(3) immersion method prepares NiCo2-xFexO4Nanotube-shaped composite material:, will be prepared in step (2) using distilled water as solvent
Presoma and ferric chloride hexahydrate be added in beaker and carry out heating in water bath for reaction, obtained product distilled water and anhydrous second
Alcohol cleans up, and calcines after drying, finally obtains the nanotube-shaped composite material of nickel cobalt iron ternary metal oxide.
3. preparation method according to claim 2, it is characterised in that the pretreatment of ultrasound described in step (1) is respectively in nothing
It is ultrasonically treated in water-ethanol and distilled water, drying condition are as follows: dried under the conditions of 60 DEG C.
4. preparation method according to claim 2, it is characterised in that step (2) cobalt chloride hexahydrate, six hydration chlorine
The molar ratio for changing nickel, cetyl trimethylammonium bromide and urea is 10:5:4:18.
5. preparation method according to claim 2, it is characterised in that the temperature of step (2) described hydro-thermal reaction be 80~
150 DEG C, the time is 12~24 h.
6. preparation method according to claim 2, it is characterised in that the molar concentration of addition iron ion is in step (3)
0.1~2 mol/L.
7. preparation method according to claim 2, it is characterised in that the temperature of heating in water bath for reaction described in step (3) is
60~120 DEG C, the time is 0.5~3 h.
8. preparation method according to claim 2, it is characterised in that calcination temperature described in step (3) is 300 DEG C, the time
For 3 h.
9. the nanotube-shaped composite material of nickel cobalt iron ternary metal oxide answering in supercapacitor described in claim 1
With.
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| CN108380224B (en) * | 2018-02-01 | 2021-01-05 | 安徽师范大学 | Nickel-cobalt sulfide @ bimetal nickel-iron hydroxide core-shell heterostructure nanotube array material and preparation method and application thereof |
| CN108470631A (en) * | 2018-05-23 | 2018-08-31 | 中国海洋大学 | Nickel cobalt iron sulphur multi-element metal oxygen（Sulphur）Compound nano core-shell shape composite material and preparation method |
| CN109174147A (en) * | 2018-08-08 | 2019-01-11 | 东华大学 | The nitrogen-doped carbon nanocomposite of hollow Fe2O3 doping cobalt oxide nickel coated and preparation |
| CN109755037B (en) * | 2018-12-28 | 2021-04-02 | 南昌大学 | Preparation method of nickel cobalt oxide-tin dioxide composite supercapacitor electrode material |
| CN109786136B (en) * | 2019-02-25 | 2021-10-08 | 天津艾克凯胜石墨烯科技有限公司 | Method for growing Ni-Co-Mn nanoneedle on 3D graphene |
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