CN107068415A - The preparation and application of a kind of sour nickel composite material of core shell structure nickel molybdate@cobalts - Google Patents
The preparation and application of a kind of sour nickel composite material of core shell structure nickel molybdate@cobalts Download PDFInfo
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- CN107068415A CN107068415A CN201710265019.2A CN201710265019A CN107068415A CN 107068415 A CN107068415 A CN 107068415A CN 201710265019 A CN201710265019 A CN 201710265019A CN 107068415 A CN107068415 A CN 107068415A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- 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
Abstract
The invention discloses the preparation and application of a kind of sour nickel composite material of core shell structure nickel molybdate@cobalts, this method can be obtained using nickel molybdate nano wire as skeleton, the sour nickel composite material of core shell structure nickel molybdate@cobalts of the sour nickel material of flaky nanometer structure cobalt is coated outside it, structure vertical growth, marshalling, have well-regulated 3-D heterojunction structure.Using hydro-thermal aid coprecipitation method, compared with prior art, extensively, preparation process is simple and safe, green non-pollution for raw material sources of the present invention, and prepared product purity height, good dispersion and process control, production cost are low, favorable reproducibility.
Description
Technical field
The present invention relates to ultracapacitor field, particularly a kind of core shell structure nickel molybdate@suitable for ultracapacitor
The preparation and application of cobalt acid nickel composite material.
Background technology
With the fast development and the sharp increase of population of economic society, and the raising that people are required quality of life,
This all accelerates the consumption of the energy and resource.And traditional energy such as coal, oil, natural gas etc. are all non-renewable energy resources, by
In the huge consumption of today's society, its amount of storage is soon close to exhaustion.21 century, during energy stores problem is lot of challenges
It is a kind of.Therefore, need badly and work out a kind of high-performance, inexpensive and environmentally friendly energy storage device meets the demand of people.
Ultracapacitor, is called and does electrochemical capacitor, because with higher energy density, quick charge and discharge process, environment-friendly
The advantages of with long service life, get more and more people's extensive concerning.According to energy storage mechnism, ultracapacitor can be divided into two classes：It is double
Electric layer capacitor and Faraday pseudo-capacitance device.In double layer capacitor, electric charge is on the surface of electrode material and electrolyte solution
Accumulated（Such as carbon material）.And Faraday pseudo-capacitance device storage energy is by the way that quick and reversible oxidation occurs in electrode surface
Reduction reaction（Such as metal oxide/hydroxide and conducting polymer）.Metal oxide electrode makes it dive because of fake capacitance behavior
Specific capacitance it is higher than carbon material.In metal oxide, particularly binary metal oxide, because with many oxidation states,
Can occur there is cooperative effect between abundant redox reaction, single oxide, be expected to turn into high performance super electricity
Container electrode material.In recent years, metal molybdate（CoMoO4、NiMoO4、MnMoO4）With cheap, environment-friendly, resource
Abundant the features such as, is paid close attention to by researcher.NiMoO is made due to the high electrochemical activity of Ni ions4With higher ratio
Capacity.With NiMoO4It is keyword in science citation index（SCI）In the retrieval result of nearly 5 years, it can be found that：With NiMoO4Have
The document of pass increases year by year, has been increasingly becoming study hotspot.
Cobalt acid nickel（NiMoO4）As a kind of new electrode material for super capacitor, with specific capacity it is high, cheap,
The advantages of environment-friendly and aboundresources.Although NiMoO4More other metal oxides possess higher specific capacity, but still because
Its own electric conductivity is poor and hinders its development and application.Faraday pseudo-capacitance energy storage mode, only electrode material surface or
The active material on nearly top layer can participate in redox reaction, and the active material of material internal can not be fully utilized, so as to lead
Its specific capacity is caused to be less than theoretical value.The present invention, using in nickel foam superficial growth active material, it is ensured that active material and conduction
Abundant contact between matrix and electrolyte, improves its specific capacitance, high rate performance and cyclical stability.
Cobalt acid nickel（NiCo2O4）It is to utilize less expensive, more environmentally friendly Ni atoms substitution Co3O4In Co atoms obtained from
A kind of bimetal composite oxide, it has and main body Co3O4Identical spinel structure, up to the present, due to NiCo2O4
With than Co3O4The electrical conductivity of two orders of magnitude is higher by with NiO, thus is showed as the fake capacitance material of advanced ultracapacitor
Good chemical property is gone out.
The content of the invention
It is an object of the invention to provide a kind of sour nickel composite material of new core shell structure nickel molybdate@cobalts.
The technical scheme is that,（1）The pretreatment of nickel foam：Nickel foam is carried out surface clean to remove surface
Impurity and oxide；
（2）The preparation of nano bar-shape structure molybdic acid nickel material by matrix of nickel foam
（2-1）Step will be passed through（1）Nickel foam after processing is vertically put into reactor；
（2-2）By a certain proportion of sodium molybdate, nickel nitrate and sodium acetate, scattered in deionized water, magnetic agitation 3h, is obtained
Even mixed solution；
（2-3）Above-mentioned mixed liquor is transferred to reactor, temperature is to react 2-15h at 80-200 DEG C；
（2-4）Reaction is finished, and resulting product is cleaned for several times with deionized water, obtained after drying using nickel foam as matrix
Nanometer wire nickel molybdate material；
（3）The molybdic acid nickel material of preparation and cobalt nitrate, nickel nitrate, ammonium nitrate and ammonia spirit are subjected to coprecipitation reaction；
（4）Reaction is finished, and resulting product is cleaned for several times with deionized water, after drying, roasting, is cooled to room temperature, most
The sour nickel composite material of core shell structure nickel molybdate@cobalts is obtained eventually.
The mol ratio 1 of sodium molybdate and nickel nitrate:1, the mol ratio 1 of sodium molybdate and sodium acetate:1~10:1, nickel molybdate：Nitric acid
The mol ratio 10 of nickel:1~1:1.
The cleaning is cleaned three times, every time 3 minutes using ultrasonic wave cleaning.
The composite obtained after hydro-thermal aid coprecipitation is reacted is calcined, and the temperature of roasting is 250-450 DEG C, when
Between be 1-4h, heating rate be 0.1-10 DEG C/min between.
Prepared by the wire nanostructured NiMoO4 materials using nickel foam as matrix, its hydrothermal temperature is 100-
160 DEG C, the reaction time is 4-10h.
The core shell structure NiMoO4@NiCo2O4Preparation, its coprecipitation reaction temperature be 100-120 DEG C, the reaction time
For 5-10h, PH=10-12, ammoniacal liquor drop rate is 1 drop/sec, and calcining heat is 250-450 DEG C, and the time is 1-4h.
The electrode of the application predominantly ultracapacitor of the sour nickel composite material of core shell structure nickel molybdate@cobalts produced by the invention
Material.
The beneficial effects of the invention are as follows:
This method can obtain core shell structure NiMoO4@NiCo2O4Composite；Prepared NiMoO4@NiCo2O4Composite is used
When making electrode material for super capacitor, with preferable cycle life and high rate performance, especially in high current density discharge and recharge bar
Still there is more excellent chemical property under part；Have preparation technology simple simultaneously, advantages of environment protection can be advised greatly
Mould is produced..
Brief description of the drawings
Fig. 1 is that the nickel foam after being handled by example 1 observes obtained pattern under ESEM.
Fig. 2 is the NiMoO prepared by example 14Composite observes obtained pattern under ESEM
Fig. 3 is the NiMoO as prepared by example 14@NiCo2O4Composite observes obtained pattern under ESEM.
Fig. 4 is the NiMoO as synthesized by example 14And NiMoO4@NiCo2O4Discharge and recharge of the material under 1A/g current densities
Curve.
Fig. 5 is the NiMoO as synthesized by example 14And NiMoO4@NiCo2O4Material is under 4A/g current densities, circulation 500
The cycle performance curve in week.
Fig. 6 is the NiMoO as synthesized by example 14And NiMoO4@NiCo2O4Material is in 1A/g, 4A/g, 7A/g, 10A/g electricity
High rate performance curve under current density.
Embodiment
Embodiment is described in detail with reference to the figures above,
Embodiment 1：
Nickel foam is cleaned by ultrasonic three times in HCl, deionized water, acetone soln respectively, 3 minutes every time, the oxygen on surface is removed
Compound；Then, sodium molybdate, nickel nitrate, sodium acetate are chosen, the wherein mol ratio of sodium molybdate and nickel nitrate is 1：1, sodium molybdate and vinegar
The mol ratio 4 of sour sodium：1, they are dispersed in 15ml deionized waters, after magnetic agitation 3h, solution be transferred to
In 25ml autoclaves, the hydro-thermal reaction 6h at 150 DEG C.After reaction terminates, pole piece is taken out, is cleaned in ultrasonic cleaner
Three times, 3 minutes every time, finally pole piece is transferred in air dry oven and carries out drying and processing, molybdic acid nickel material is obtained.By quality
Compare cobalt nitrate：Nickel nitrate：Ammonium nitrate=2:1:1 precise, wherein nickel molybdate：The mol ratio 3 of nickel nitrate：1, ammonia is slowly added dropwise
Water, speed is 1 drop/sec, as PH=10.8, the solution being stirred is transferred in three-necked flask, and is hanged in three-necked flask
The glass tube of both ends open is hung, immerses, wherein the nanometer linear structure NiMoO prepared in built-in step 24Material；Mixed solution
Coprecipitation reaction is carried out through 110 DEG C of condensing reflux 6h.After coprecipitation reaction terminates, pole piece is transferred in ultrasonic cleaner
Row is cleaned by ultrasonic three times, 3 minutes every time, product is calcined 3 hours at 350 DEG C, 2 DEG C/min of heating rate is cooled to room
Temperature, obtains NiMoO4@NiCo2O4Composite.
With reference to accompanying drawing：
Fig. 3 is the NiMoO prepared by embodiment 14@NiCo2O4Composite observes obtained pattern under ESEM.By scheming
In visible, the NiMoO obtained in embodiment 14@NiCo2O4Composite is core shell structure, flaky nanometer structure NiCo2O4Material
Uniformly it is coated with linear structure NiMoO4Material.This structure both can make electrolyte effectively be diffused into the interior of electrode material
Portion, and bigger specific surface area can be provided, it so as to increase avtive spot, can be changed the specific capacitance and cycle performance of electrode
It is kind, improve the chemical property of electrode.
The assembling of ultracapacitor, NiMoO are carried out using three-electrode system4@NiCo2O4Composite is used as working electrode；
20×20（mm）, the platinized platinum that thickness is 0.1mm is auxiliary electrode；Hg/HgO is reference electrode；Electrolyte is that 3 mol/L KOH are molten
Liquid；Barrier film is PE；；Electric performance test is carried out using electrochemical workstation.
Fig. 4 is charging and discharging curve at room temperature under 1A/g current densities.As seen from the figure, through NiCo2O4Composite wood after cladding
Material has higher specific capacitance.
Fig. 5 is the cycle performance curve after circulating 500 weeks at room temperature under 4A/g current densities.As seen from the figure, it is of the invention
Obtained NiMoO4@NiCo2O4When composite is as electrode material for super capacitor, still have after 500 weeks circulate
1569.8 F/g specific capacitance, and stable cycle performance.
Fig. 6 is at room temperature in the range of 0 ~ 0.55V with the high rate performance song of different current density progress charge-discharge tests
Line.As can be seen that NiMoO produced by the present invention4@NiCo2O4Composite has excellent high rate performance.
Embodiment 2：
First, nickel foam is cleaned by ultrasonic three times in HCl, deionized water, acetone soln respectively, 3 minutes every time, removes surface
Oxide；Then, sodium molybdate, nickel nitrate, sodium acetate are chosen, the wherein mol ratio of sodium molybdate and nickel nitrate is 1：1, sodium molybdate
With the mol ratio 1 of sodium acetate：1, they are dispersed in 15ml deionized waters, after magnetic agitation 3h, solution shifted
Into 25ml autoclaves, the hydro-thermal reaction 4h at 130 DEG C.After reaction terminates, pole piece is taken out, it is clear in ultrasonic cleaner
Wash three times, 3 minutes every time, finally pole piece is transferred in air dry oven and carries out drying and processing, molybdic acid nickel material is obtained.By matter
Amount compares cobalt nitrate：Nickel nitrate：Ammonium nitrate=2:1:1 precise, wherein nickel molybdate：The mol ratio 3 of nickel nitrate：1, it is slowly added dropwise
Ammoniacal liquor, speed is 1 drop/sec, and as PH=12, the solution being stirred is transferred in three-necked flask, and is hanged in three-necked flask
The glass tube of both ends open is hung, immerses, wherein the nanometer linear structure NiMoO prepared in built-in step 24Material；Mixed solution
Coprecipitation reaction is carried out through 100 DEG C of condensing reflux 5h.After coprecipitation reaction terminates, pole piece is transferred in ultrasonic cleaner
Row is cleaned by ultrasonic three times, 3 minutes every time, product is calcined 4 hours at 250 DEG C, 2 DEG C/min of heating rate is cooled to room
Temperature, obtains NiMoO4@NiCo2O4Composite.
Embodiment 3：
First, nickel foam is cleaned by ultrasonic three times in HCl, deionized water, acetone soln respectively, 3 minutes every time, removes surface
Oxide；Then, then, sodium molybdate, nickel nitrate, sodium acetate are chosen, the wherein mol ratio of sodium molybdate and nickel nitrate is 1：1,
The mol ratio 3 of sodium molybdate and sodium acetate：1, they are dispersed in 15ml deionized waters, will be molten after magnetic agitation 3h
Liquid is transferred in 25ml autoclaves, the hydro-thermal reaction 4h at 160 DEG C.After reaction terminates, pole piece is taken out, in ultrasonic wave cleaning
Cleaned three times in device, 3 minutes every time, finally pole piece is transferred in air dry oven and carries out drying and processing, nickel molybdate material is obtained
Material.Cobalt nitrate in mass ratio：Nickel nitrate：Ammonium nitrate=2:1:1 precise, wherein nickel molybdate：The mol ratio 10 of nickel nitrate：1,
It is slowly added dropwise ammoniacal liquor, speed is 1 drop/sec, as PH=12, the solution being stirred is transferred in three-necked flask, and in three mouthfuls of burnings
Suspension, the glass tube of immersion both ends open in bottle, wherein the nanometer linear structure NiMoO prepared in built-in step 24Material；It is mixed
Close solution and carry out coprecipitation reaction through 100 DEG C of condensing reflux 4h.After coprecipitation reaction terminates, pole piece is transferred to ultrasonic wave cleaning
Carry out being cleaned by ultrasonic three times in device, 3 minutes every time, product is calcined 2 hours at 450 DEG C, 10 DEG C/min of heating rate is cold
But to room temperature, NiMoO is obtained4@NiCo2O4Composite.
Embodiment 4：
First, nickel foam is cleaned by ultrasonic three times in HCl, deionized water, acetone soln respectively, 3 minutes every time, removes surface
Oxide；Then, then, sodium molybdate, nickel nitrate, sodium acetate are chosen, the wherein mol ratio of sodium molybdate and nickel nitrate is 1：1,
The mol ratio 10 of sodium molybdate and sodium acetate：1, they are dispersed in 15ml deionized waters, will be molten after magnetic agitation 3h
Liquid is transferred in 25ml autoclaves, the hydro-thermal reaction 10h at 100 DEG C.After reaction terminates, pole piece is taken out, it is clear in ultrasonic wave
Wash in device and clean three times, 3 minutes every time, finally pole piece is transferred in air dry oven and carries out drying and processing, nickel molybdate is obtained
Material.Cobalt nitrate in mass ratio：Nickel nitrate：Ammonium nitrate=2:1:1 precise, wherein nickel molybdate：The mol ratio 1 of nickel nitrate：1,
It is slowly added dropwise ammoniacal liquor, speed is 1 drop/sec, as PH=10, the solution being stirred is transferred in three-necked flask, and in three mouthfuls of burnings
Suspension, the glass tube of immersion both ends open in bottle, wherein the nanometer linear structure NiMoO prepared in built-in step 24Material；It is mixed
Close solution and carry out coprecipitation reaction through 100 DEG C of condensing reflux 4h.After coprecipitation reaction terminates, pole piece is transferred to ultrasonic wave cleaning
Carry out being cleaned by ultrasonic three times in device, 3 minutes every time, product is calcined 3 hours at 450 DEG C, room temperature, heating rate 5 is cooled to
DEG C/min, obtain NiMoO4@NiCo2O4Composite.
Above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.For institute
For the those of ordinary skill in category field, other various forms of changes or change can also be made on the basis of the above description
It is dynamic.There is no necessity and possibility to exhaust all the enbodiments, and the obvious change or change thus extended out
Move within still in the protection domain of the invention.
Claims (7)
1. a kind of preparation method of the sour nickel composite material of core shell structure nickel molybdate@cobalts, it is characterised in that：By following steps prepare and
：
（1）The pretreatment of nickel foam：Nickel foam is carried out surface clean to remove the impurity and oxide on surface；
（2）The preparation of nano bar-shape structure molybdic acid nickel material by matrix of nickel foam
（2-1）Step will be passed through（1）Nickel foam after processing is vertically put into reactor；
（2-2）By a certain proportion of sodium molybdate, nickel nitrate and sodium acetate, scattered in deionized water, magnetic agitation 3h, is obtained
Even mixed solution；
（2-3）Above-mentioned mixed liquor is transferred to reactor, temperature is to react 2-15h at 80-200 DEG C；
（2-4）Reaction is finished, and resulting product is cleaned for several times with deionized water, obtained after drying using nickel foam as matrix
Nanometer wire nickel molybdate material；
（3）The molybdic acid nickel material of preparation and cobalt nitrate, nickel nitrate, ammonium nitrate and ammonia spirit are subjected to coprecipitation reaction；
（4）Reaction is finished, and resulting product is cleaned for several times with deionized water, after drying, roasting, is cooled to room temperature, most
The sour nickel composite material of core shell structure nickel molybdate@cobalts is obtained eventually.
2. a kind of preparation method of the sour nickel composite material of core shell structure nickel molybdate@cobalts according to claim 1, its feature exists
In：The mol ratio 1 of sodium molybdate and nickel nitrate:1, the mol ratio 1 of sodium molybdate and sodium acetate:1~10:1, nickel molybdate：Nickel nitrate rubs
You compare 10:1~1:1.
3. a kind of preparation method of the sour nickel composite material of core shell structure nickel molybdate@cobalts according to claim 1, its feature exists
In：The cleaning is cleaned three times, every time 3 minutes using ultrasonic wave cleaning.
4. a kind of preparation method of the sour nickel composite material of core shell structure nickel molybdate@cobalts according to claim 1, its feature exists
In：Obtained composite is calcined after hydro-thermal aid coprecipitation is reacted, and the temperature of roasting is 250-450 DEG C, and the time is
1-4h, heating rate is between 1-10 DEG C/min.
5. a kind of preparation method of the sour nickel composite material of core shell structure nickel molybdate@cobalts according to claim 1, its feature exists
In：The wire nanostructured NiMoO using nickel foam as matrix4Prepared by material, its hydrothermal temperature is 100-160 DEG C,
Reaction time is 4-10h.
6. a kind of preparation method of the sour nickel composite material of core shell structure nickel molybdate@cobalts according to claim 1, its feature exists
In：The core shell structure NiMoO4@NiCo2O4Preparation, its coprecipitation reaction temperature be 100-120 DEG C, the reaction time is 5-
10h, PH=10-12, ammoniacal liquor drop rate are 1 drop/sec, and calcining heat is 250-450 DEG C, and the time is 1-4h.
7. a kind of application of the sour nickel composite material of core shell structure nickel molybdate@cobalts described in claim 1, it is characterised in that：As
The electrode material of ultracapacitor.
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| CN109092326A (en) * | 2018-07-02 | 2018-12-28 | 曲阜师范大学 | A kind of nucleocapsid shape nickel tungstate micro-ball load palladium catalyst and its preparation method and application |
| CN109911947A (en) * | 2019-02-22 | 2019-06-21 | 中国科学院山西煤炭化学研究所 | A kind of NiCo2O4@NiMoO4Core-shell structure and preparation method thereof |
| CN111268745A (en) * | 2020-02-03 | 2020-06-12 | 上海第二工业大学 | NiMoO4@Co3O4Core-shell nano composite material, preparation method and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109092326A (en) * | 2018-07-02 | 2018-12-28 | 曲阜师范大学 | A kind of nucleocapsid shape nickel tungstate micro-ball load palladium catalyst and its preparation method and application |
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| CN109911947A (en) * | 2019-02-22 | 2019-06-21 | 中国科学院山西煤炭化学研究所 | A kind of NiCo2O4@NiMoO4Core-shell structure and preparation method thereof |
| CN109911947B (en) * | 2019-02-22 | 2020-09-08 | 中国科学院山西煤炭化学研究所 | NiCo2O4@NiMoO4Core-shell structure and preparation method thereof |
| CN111268745A (en) * | 2020-02-03 | 2020-06-12 | 上海第二工业大学 | NiMoO4@Co3O4Core-shell nano composite material, preparation method and application |
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Application publication date: 20170818 |