CN106340398B - A kind of preparation method of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material - Google Patents
A kind of preparation method of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material Download PDFInfo
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Abstract
The present invention relates to the preparation methods of a kind of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material, it includes following preparation step: 1) carbon cloth or foam nickel base is successively used into deionized water, acetone, ethyl alcohol, deionized water supersound washing, it is dry；2) nickel nitrate, cobalt nitrate and sodium molybdate are dissolved in deionized water, add hexamethylenetetramine and urea stirring, is uniformly mixed, forms clear mixed solution；3) mixed solution obtained is moved into autoclave, and carbon cloth or foam nickel base that pretreatment obtains is added into mixed solution, carry out hydro-thermal reaction；After reaction, cooled to room temperature；4) resulting reaction product is washed with deionized, it is dry.It prepares nickel cobalt hydroxide and molybdenum oxide composite nano materials by hydro-thermal method, can be directly as the electrode material of supercapacitor, and process flow is simple, at low cost, is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to the preparation fields of capacitor electrode material, and in particular to a kind of electrode material for super capacitor nickel cobalt
The preparation method of hydroxide and molybdenum oxide composite material.
Background technique
Supercapacitor is a kind of advanced energy storage device, is received significant attention in recent years, it has power density
High, many advantages, such as charging time is short, good temp characteristic, long service life, in the high-power applications such as following electric car
There is good application prospect.The electrode material of supercapacitor mainly includes carbon material, transition metal oxide, transition metal hydrogen
Oxide and conducting polymer materials etc..According to energy storage mechnism, supercapacitor can be divided into double layer capacitor and faraday's electricity
Container, wherein faraday's capacitor has specific capacity more higher than double layer capacitor, has bigger development potentiality.Faraday
Electrode material for super capacitor study at present it is more for conduction high polymer and metal oxide and its hydroxide, relative to leading
For electric high polymer, metal oxide and its hydroxide have better electrochemical stability, so as to cause numerous researchs
The great interest of person.
The optimum electrode material of supercapacitor is metal oxide containing precious metals RuO at present2, it has very high specific capacity and good
Good conductivity, but its price is very expensive, limit its application industrially.Nickel/cobalt composite oxide/hydroxide because
Have many advantages, such as that at low cost, redox active is good, theoretical specific capacitance is high, and is paid special attention to, but cyclical stability difference is
Its current critical issue urgently to be solved.Therefore exploitation high capacity, high stability and cheap novel composite electrode material
It is of great significance.Molybdenum oxide has a variety of oxidation state structures, and redox reaction process is abundant, in addition it is with unique one
Layer structure is tieed up, is quickly embedded in and extracts out convenient for particle or ion, therefore be considered as the ideal electrode material of supercapacitor.
Nickel cobalt double-hydroxide and the mutually compound super capacitance electrode material that is used for of molybdenum oxide be yet there are no into relevant report.
Summary of the invention
The object of the present invention is to provide a kind of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite wood
The preparation method of material is prepared nickel cobalt hydroxide and molybdenum oxide composite nano materials by hydro-thermal method, can directly be made
For the electrode material of supercapacitor, process flow is simple, at low cost, is suitable for large-scale industrial production.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material comprising
Following preparation step:
1) carbon cloth or foam nickel base successively substrate pretreatment: are used into deionized water, acetone, ethyl alcohol, deionized water ultrasound
Washing, it is dry；
2) it prepares mixed liquor: nickel nitrate, cobalt nitrate and sodium molybdate is dissolved in deionized water, add six methines four
Amine and urea stirring, are uniformly mixed, form clear mixed solution；
3) it carries out hydro-thermal reaction: mixed solution made from step 2 being moved into autoclave, and into mixed solution
The carbon cloth or foam nickel base that step 1) pre-processes is added, carries out hydro-thermal reaction；After reaction, room is naturally cooled to
Temperature；
4) composite material is made: the resulting reaction product of step 3) is washed with deionized, it is dry, obtain nickel cobalt hydrogen-oxygen
Compound and molybdenum oxide composite material.
Further, the substrate in the step 1) after supersound washing is dried in vacuo, and guarantees that substrate cleans up no dirt
Dye.
Further, concentration of the nickel nitrate in mixed solution is 1-1.5mol/L in the step 2, and cobalt nitrate is mixing
Concentration in solution is 3-4.5mol/L, and concentration of the sodium molybdate in mixed solution is 2-3mol/L.
Further, concentration of the nickel nitrate in mixed solution is 1mol/L in the step 2, and cobalt nitrate is in mixed solution
In concentration be 3mol/L, concentration of the sodium molybdate in mixed solution be 2mol/L.
Further, concentration of the hexamethylenetetramine in mixed solution is 6-8g/L in the step 2, and urea is mixing
Concentration in solution is 6-8g/L
Further, concentration of the hexamethylenetetramine in mixed solution is 7g/L in the step 2, and urea is molten in mixing
Concentration in liquid is 6g/L.
Further, the temperature of hydro-thermal reaction is 100-200 DEG C in the step 3), and the reaction time is 3-9h.
Further, washing times are 2-4 times in the step 4), and drying temperature is 60-80 DEG C.
Further, nickel cobalt hydroxide obtained and molybdenum oxide composite material are flaky nanometer structure, with a thickness of 5-
15nm。
Compared with prior art, the beneficial effects of the present invention are:
Using hydro-thermal method carbon cloth or foam nickel base previous step synthesis nickel cobalt hydroxide with molybdenum oxide is compound receives
Rice material, can be directly as the electrode material of supercapacitor, obtained nickel cobalt hydroxide and molybdenum oxide composite wood
Expect specific capacity with higher and preferable cyclical stability, there is preferable application value in terms of energy stores；It is made
The technique of Preparation Method is very simple, at low cost, high production efficiency, is suitable for large-scale industrial production, can also promote and be used for
Synthesize other ternary hydroxide electrode material for super capacitor.
Detailed description of the invention
Fig. 1 is the SEM figure of nickel cobalt hydroxide prepared by the embodiment of the present invention 1 and molybdenum oxide composite material；
Fig. 2 is the XRD diagram of nickel cobalt hydroxide and molybdenum oxide composite material prepared by the embodiment of the present invention 1；
Fig. 3 is nickel cobalt hydroxide prepared by the embodiment of the present invention 1 and molybdenum oxide composite material in the case where difference sweeps speed
Cyclic voltammetry curve figure；
Fig. 4 is that nickel cobalt hydroxide prepared by the embodiment of the present invention 1 is close in different electric currents from molybdenum oxide composite material
Constant current charge-discharge curve graph under degree；
Fig. 5 is nickel cobalt hydroxide prepared by the embodiment of the present invention 1 and molybdenum oxide composite material in 1000 charge and discharges
Specific capacitance value when electric with charge and discharge number opposite variation diagram.
Specific embodiment
The present invention will be described in detail with reference to the accompanying drawings and examples.
Embodiment 1, a kind of preparation side of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material
Method, including following preparation step:
1) substrate pretreatment: carbon cloth substrate is torn open and is cut into a thickness of 0.36mm, surface area is 3 × 3cm2Size, then according to
It is secondary to use deionized water, acetone, ethyl alcohol, deionized water supersound washing, finally it is dried in vacuo；
2) it prepares mixed liquor: nickel nitrate, cobalt nitrate and sodium molybdate is dissolved in 30ml deionized water, nickel nitrate is mixing
Concentration in solution is 1mol/L, and concentration of the cobalt nitrate in mixed solution is 3mol/L, and sodium molybdate is dense in mixed solution
Degree is 2mol/L, adds 0.21g hexamethylenetetramine and the stirring of 0.18g urea, is uniformly mixed, and it is molten to form clear mixing
Liquid；
3) it carries out hydro-thermal reaction: mixed solution made from step 2 being moved into autoclave, and into mixed solution
The carbon cloth substrate that step 1) pre-processes, 120 DEG C of hydro-thermal reaction 3h are added；After reaction, cooled to room temperature；
4) composite material is made: the resulting reaction product of step 3) is washed with deionized 2 times, in the case where temperature is 60 DEG C
It is dried, obtains nickel cobalt hydroxide and molybdenum oxide composite material, be flaky nanometer structure, with a thickness of 5-15nm.
Embodiment 2, a kind of preparation side of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material
Method, including following preparation step:
1) substrate pretreatment: carbon cloth substrate is torn open and is cut into a thickness of 0.5mm, surface area is 3 × 3cm2Size, then successively
With deionized water, acetone, ethyl alcohol, deionized water supersound washing, finally it is dried in vacuo；
2) it prepares mixed liquor: nickel nitrate, cobalt nitrate and sodium molybdate is dissolved in 30ml deionized water, nickel nitrate is mixing
Concentration in solution is 1.5mol/L, and concentration of the cobalt nitrate in mixed solution is 4.5mol/L, and sodium molybdate is in mixed solution
Concentration be 3mol/L, add 0.24g hexamethylenetetramine and 0.24g urea stirring, be uniformly mixed, form clear mixing
Solution；
3) it carries out hydro-thermal reaction: mixed solution made from step 2 being moved into autoclave, and into mixed solution
The carbon cloth substrate that step 1) pre-processes, 120 DEG C of hydro-thermal reaction 6h are added；After reaction, cooled to room temperature；
4) composite material is made: the resulting reaction product of step 3) is washed with deionized 4 times, in the case where temperature is 80 DEG C
It is dry, nickel cobalt hydroxide and molybdenum oxide composite material are obtained, is flaky nanometer structure, with a thickness of 5-15nm.
Embodiment 3, a kind of preparation side of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material
Method, including following preparation step:
1) substrate pretreatment: carbon cloth substrate is torn open and is cut into a thickness of 0.5mm, surface area is 3 × 3cm2Size, then successively
With deionized water, acetone, ethyl alcohol, deionized water supersound washing, finally it is dried in vacuo；
2) it prepares mixed liquor: nickel nitrate, cobalt nitrate and sodium molybdate is dissolved in 30ml deionized water, nickel nitrate is mixing
Concentration in solution is 1.3mol/L, and concentration of the cobalt nitrate in mixed solution is 3.8mol/L, and sodium molybdate is in mixed solution
Concentration be 2.5mol/L, add 0.18g hexamethylenetetramine and the stirring of 0.21g urea, be uniformly mixed, formed clear mixed
Close solution；
3) it carries out hydro-thermal reaction: mixed solution made from step 2 being moved into autoclave, and into mixed solution
The carbon cloth substrate that step 1) pre-processes, 140 DEG C of hydro-thermal reaction 6h are added；After reaction, cooled to room temperature；
4) composite material is made: the resulting reaction product of step 3) is washed with deionized 4 times, in the case where temperature is 70 DEG C
It is dried, obtains nickel cobalt hydroxide and molybdenum oxide composite material, be flaky nanometer structure, with a thickness of 5-15nm.
Embodiment 4, a kind of preparation side of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material
Method, including following preparation step:
1) substrate pretreatment: foam nickel base is torn open and is cut into a thickness of 1mm, surface area is 3 × 3cm2Size, then successively
With deionized water, acetone, ethyl alcohol, deionized water supersound washing, finally it is dried in vacuo；
2) it prepares mixed liquor: nickel nitrate, cobalt nitrate and sodium molybdate is dissolved in 50ml deionized water, nickel nitrate is mixing
Concentration in solution is 1.4mol/L, and concentration of the cobalt nitrate in mixed solution is 4mol/L, and sodium molybdate is in mixed solution
Concentration is 2.8mol/L, adds 0.35g hexamethylenetetramine and the stirring of 0.3g urea, is uniformly mixed, forms clear mixing
Solution；
3) it carries out hydro-thermal reaction: mixed solution made from step 2 being moved into autoclave, and into mixed solution
The foam nickel base that step 1) pre-processes, 180 DEG C of hydro-thermal reaction 3h are added；After reaction, cooled to room temperature；
4) composite material is made: the resulting reaction product of step 3) is washed with deionized 2 times, in the case where temperature is 80 DEG C
It is dried, obtains nickel cobalt hydroxide and molybdenum oxide composite material, be flaky nanometer structure, with a thickness of 5-15nm.
Embodiment 5, a kind of preparation side of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material
Method, including following preparation step:
1) substrate pretreatment: carbon cloth substrate is torn open and is cut into a thickness of 1.0mm, surface area is 3 × 3cm2Size, then successively
With deionized water, acetone, ethyl alcohol, deionized water supersound washing, finally it is dried in vacuo；
2) it prepares mixed liquor: nickel nitrate, cobalt nitrate and sodium molybdate is dissolved in 50ml deionized water, nickel nitrate is mixing
Concentration in solution is 1mol/L, and concentration of the cobalt nitrate in mixed solution is 3.8mol/L, and sodium molybdate is in mixed solution
Concentration is 2.4mol/L, adds 0.3g hexamethylenetetramine and the stirring of 0.35g urea, is uniformly mixed, forms clear mixing
Solution；
3) it carries out hydro-thermal reaction: mixed solution made from step 2 being moved into autoclave, and into mixed solution
The carbon cloth substrate that step 1) pre-processes, 160 DEG C of hydro-thermal reaction 9h are added；After reaction, cooled to room temperature；
4) composite material is made: the resulting reaction product of step 3) is washed with deionized 4 times, in the case where temperature is 80 DEG C
It is dried, obtains nickel cobalt hydroxide and molybdenum oxide composite material, be flaky nanometer structure, with a thickness of 5-15nm.
Embodiment 6, nickel cobalt hydroxide prepared by embodiment 1 and molybdenum oxide composite material scanning electron microscopic observation,
Shown in Figure 1, a and b respectively indicate the SEM figure of the composite material under the conditions of different multiples, obtained nickel cobalt hydroxide with
Molybdenum oxide composite material is flaky nanometer structure, they are crossed-over, at the same uniformly, intensive be covered on the every of carbon cloth
On a piece fiber, the thickness of each small pieces is minimum, and statistics can obtain its thickness between 5-15nm, mutually support again between them, shape
At highly stable cellular structure, it can guarantee that nickel cobalt hydroxide and molybdenum oxide composite material have biggish specific surface in this way
Product, and electrolyte can be come into full contact with, help to improve its capacitive property.
Nickel cobalt hydroxide prepared by embodiment 1 is carried out object using XRD with molybdenum oxide composite wood and mutually tied by embodiment 7
Structure analysis, it is shown in Figure 2, it is located at 34.3 ° and 59.9 ° there are two stronger diffraction maximum, corresponds to nickel cobalt hydroxide
The diffraction maximum of object (100) and (110), furthermore there are two relatively weak peaks at 37.0 ° and 53.6 °, correspond to molybdenum and aoxidize
(020) and (220) peak of object illustrates that the material of synthesis is nickel cobalt hydroxide and molybdenum oxide composite material.
Embodiment 8, shown in Figure 3, using three-electrode system, working electrode is the ㎜ of 10 ㎜ × 10 cut out
The product for preparing of embodiment 1, be platinized platinum to electrode, reference electrode is silver/silver chloride electrode, and electrolyte is 2mol/L
KOH tests the cyclic voltammetry curve under different scanning rates with electrochemical workstation, can see from cyclic voltammetry curve
Apparent oxidation peak and reduction peak, with the increase of scanning speed, the peak value of corresponding oxidation peak and reduction peak is all increasing, this says
Bright to have occurred reversible redox reaction well on this electrode, prepared nickel cobalt hydroxide and molybdenum oxide are answered
Condensation material has pseudo capacitance characteristic.
Embodiment 9, shown in Figure 4, the composite material of nickel cobalt hydroxide and molybdenum oxide prepared by embodiment 1 exists
Constant current charge-discharge curve under different current densities, charge and discharge behavior also show apparent fake capacitance characteristic, computational chart
Bright, the specific capacitance in 1A/g is maximum, reaches 3207 F/g；When discharge current density is respectively 2A/g, 3A/g, 10A/g, phase
The specific capacitance value answered is respectively 3130 F/g, 3070 F/g, 2825F/g.Specific volume when current density increases to 10A/g by 1A/g
Amount is decayed with the increase of current density, but specific capacity has only decayed 12%, shows the nickel cobalt hydroxide and molybdenum oxygen of preparation
The composite material of compound has preferable high current rate capability performance under high current density.
Embodiment 10, shown in Figure 5, the composite material of nickel cobalt hydroxide and molybdenum oxide prepared by embodiment 1
The opposite variation diagram of specific capacitance value in 1000 charge and discharge, with the increase of charge and discharge number, specific capacitance value is declined slightly, but
Specific capacitance value has kept stable after 400 charge and discharge, does not continue to decline, until being still able to maintain initial ratio after 1000 charge and discharge
The 91% of capacitance, it is shown that the nickel cobalt hydroxide of preparation and the composite material of molybdenum oxide have preferable cyclical stability.
Embodiments of the present invention above described embodiment only expresses, the description thereof is more specific and detailed, but can not
Therefore limitations on the scope of the patent of the present invention are interpreted as, as long as skill obtained in the form of equivalent substitutions or equivalent transformations
Art scheme should all be fallen within the scope and spirit of the invention.
Claims (6)
1. a kind of preparation method of electrode material for super capacitor nickel cobalt hydroxide and molybdenum oxide composite material, feature exist
In including following preparation step:
1) substrate pretreatment: successively using deionized water, acetone, ethyl alcohol, deionized water supersound washing for carbon cloth or foam nickel base,
It is dry；
2) prepare mixed liquor: nickel nitrate, cobalt nitrate and sodium molybdate be dissolved in deionized water, add hexamethylenetetramine and
Urea stirring, is uniformly mixed, forms clear mixed solution；Concentration of the nickel nitrate in mixed solution is 1-1.5mol/L, nitre
Concentration of the sour cobalt in mixed solution is 3-4.5mol/L, and concentration of the sodium molybdate in mixed solution is 2-3mol/L, six first
Concentration of the urotropine in mixed solution is 6-8g/L, and concentration of the urea in mixed solution is 6-8g/L；
3) it carries out hydro-thermal reaction: mixed solution made from step 2) being moved into autoclave, and is added into mixed solution
The carbon cloth or foam nickel base that step 1) pretreatment obtains, carry out hydro-thermal reaction；After reaction, cooled to room temperature；
4) composite material is made: the resulting reaction product of step 3) is washed with deionized, it is dry, obtain nickel cobalt hydroxide
With molybdenum oxide composite material.
2. a kind of electrode material for super capacitor nickel cobalt hydroxide according to claim 1 and molybdenum oxide composite material
Preparation method, it is characterised in that: the substrate in the step 1) after supersound washing is dried in vacuo.
3. a kind of electrode material for super capacitor nickel cobalt hydroxide according to claim 1 and molybdenum oxide composite material
Preparation method, it is characterised in that: concentration of the nickel nitrate in mixed solution is 1mol/L in the step 2), and cobalt nitrate is mixed
Closing the concentration in solution is 3mol/L, and concentration of the sodium molybdate in mixed solution is 2mol/L.
4. a kind of electrode material for super capacitor nickel cobalt hydroxide according to claim 1 and molybdenum oxide composite material
Preparation method, it is characterised in that: concentration of the hexamethylenetetramine in mixed solution is 7g/L in the step 2), and urea exists
Concentration in mixed solution is 6g/L.
5. a kind of electrode material for super capacitor nickel cobalt hydroxide according to claim 1 and molybdenum oxide composite material
Preparation method, it is characterised in that: in the step 3) temperature of hydro-thermal reaction be 100-200 DEG C, reaction time 3-9h.
6. a kind of electrode material for super capacitor nickel cobalt hydroxide according to claim 1 and molybdenum oxide composite material
Preparation method, it is characterised in that: in the step 4) washing times be 2-4 time, drying temperature be 60-80 DEG C.
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| CN108118362B (en) * | 2018-01-09 | 2020-03-10 | 国家纳米科学中心 | Molybdenum disulfide electrocatalytic hydrogen production electrode and preparation method and application thereof |
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| CN108630444B (en) * | 2018-05-10 | 2019-12-06 | 长沙理工大学 | preparation method of porous Ni-Mo-Co ternary hydroxide nanosheet supercapacitor material |
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| CN113130214B (en) * | 2021-03-17 | 2022-10-14 | 上海应用技术大学 | NF @ molybdenum oxide @ nickel cobalt-LDH composite material and preparation method and application thereof |
| CN114335448B (en) * | 2022-01-04 | 2023-10-31 | 湖北大学 | Nickel-cobalt hydroxide with multilayer nano-sheet structure, and preparation method and application thereof |
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