CN107331538A - A kind of preparation method of nano nickel bicarbonate composite carbon electrode material - Google Patents
A kind of preparation method of nano nickel bicarbonate composite carbon electrode material Download PDFInfo
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- CN107331538A CN107331538A CN201710667018.0A CN201710667018A CN107331538A CN 107331538 A CN107331538 A CN 107331538A CN 201710667018 A CN201710667018 A CN 201710667018A CN 107331538 A CN107331538 A CN 107331538A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
- 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 present invention relates to electrode material field, a kind of preparation method of nano nickel bicarbonate composite carbon electrode material is disclosed,（1）Honey is dissolved in the water, after stirring, centrifugal treating takes supernatant liquor；（2）In step（1）Urea, six water nickel chlorides are added in described supernatant liquor, solution is configured to, after being sufficiently stirred for, obtains precursor solution；（3）By step（2）Described precursor solution is transferred in autoclave, after reaction terminates, is cooled to room temperature, is obtained pre-product；（4）By step（3）Described pre-product, carries out centrifugal treating, by lower sediment drying process after centrifugation, obtains crude product；（5）By step（4）Described crude product is then cooled to room temperature, obtains nano nickel bicarbonate composite carbon electrode material using being incubated after the heating of 0.5 15 DEG C/min heating rates.The present invention solves the problem of bicarbonate nickel composite carbon electrode material component is uneven, and prepares with excellent properties composite.
Description
Technical field
The present invention specifically relates to electrode material field, relates more specifically to a kind of nano nickel bicarbonate composite carbon electrode material
Preparation method.
Background technology
With the quick popularizations of portable electric appts, wearable device continue to bring out and clean environment firendly electronic vapour
Car flourishes, and power storage already turns into the hot issue of government of state of the world and scientists study with conversion.It is super
Capacitor is a kind of new type of energy storage device between electrostatic condenser and battery, its higher power density, energy stores
Density, the advantages of the charging interval is short, service life is long, it is many in mobile communication, national defence, Aero-Space, consumption electronic product etc.
Field has huge application value and market potential, and it, which is widely used, is expected to change traditional energy-consuming general layout, solves
Increasingly serious environmental problem.
Electrode material is the core component of performance of the supercapacitor, and current commercialization degree higher carbon material has higher
Power density, but relatively low (the 5-20 μ F/cm of charge storage density2)；And the theoretical specific capacitance value of fake capacitance electrode material is carbon
10-100 times of material, with obvious memory capacity advantage.The compound of common nickel（Nickel oxide, nickel hydroxide, nickel sulfide
Deng）Because of the changeable chemical valence of nickel, higher theoretical specific capacitance value, cheap, environment-friendly in electrode material for super capacitor
It is widely studied.Research shows bicarbonate nickel（Ni(HCO3)2）Be a kind of specific capacitance value it is higher, with the counterfeit of potential using value
Capacitance electrode material.But, there is the shortcomings of resistivity is higher, cyclical stability is poor in above-mentioned electrode material；And pass through compound tool
There are excellent conductive capability, the carbon material of mechanical property, electric charge in electrochemical process is improved using the excellent electric conductivity of carbon material
Transporting in combination electrode material, its excellent mechanical property reduces Ni (HCO in electrochemical process3)2Relaxation change is produced
Influence of the stress to electrode material cycle life, so as to be expected the electrochemistry storing up electricity performance of further lifting electrode.Therefore, this hair
It is bright to be prepared using a kind of simple one-step synthesis, prepare nano nickel bicarbonate composite carbon（Ni(HCO3)2/C）Electrode material, is obtained
Excellent chemical property.
The content of the invention
To solve first to prepare the composite wood obtained by composite means after carbon material using multistep processes in the prior art
Material normally results in carbon material and Ni (HCO3)2Between interface bond intensity it is weaker and nanocomposite constituents are pockety
Problem, the present invention provides a kind of preparation method of nano nickel bicarbonate composite carbon electrode material.
The present invention is adopted the following technical scheme that：A kind of preparation method of nano nickel bicarbonate composite carbon electrode material, it is described
Preparation method comprises the following steps：
（1）The honey of 1-10 parts by weight is dissolved in the water, after stirring, the first centrifugal treating is carried out, takes supernatant liquor；
（2）In step（1）1-10 parts by weight of urea, six water nickel chlorides of 0.5-15 parts by weight are added in described supernatant liquor,
40-80 parts by weight water, after being sufficiently stirred for, obtains precursor solution；
（3）By step（2）Described solution is transferred in autoclave, and it is 100-200 DEG C to set reaction condition, and the time is
12-24h, after reaction terminates, is cooled to room temperature, obtains pre-product；
（4）By step（3）Described pre-product, carries out the second centrifugal treating, by lower sediment drying process after centrifugation, obtains and slightly produce
Thing；
（5）By step（4）Described crude product is warming up to after 250-350 DEG C using 0.5-15 DEG C/min heating rates and is incubated 0.5-
5h, is then cooled to room temperature, obtains nano nickel bicarbonate composite carbon electrode material.
The step（4）In, the rotating speed of the second centrifugal treating is 6000-8000 rpms, using deionized water, ethanol as
Solvent displacement is centrifuged 3-5 times to pre-product.
The step（4）In the condition of drying process be that temperature is 40-70 DEG C, drying time is 15-28h.
The step（5）Middle heating rate is 1-10 DEG C/min.
The condition of first centrifugal treating is that rotating speed is 3000-5000 rpms, and the time is 5-20 minutes.
Preparation method of the present invention is simple and easy to operate, industrial easily to realize；The nanocomposite constituents of preparation are evenly distributed, profit
The conductive network provided with carbon material improves the conductance property of system；The excellent mechanical property of carbon material improves electrode material
Cyclical stability and service life.
Brief description of the drawings
The nano nickel bicarbonate composite carbon electrode material X-ray diffractogram that Fig. 1 present invention is prepared;
The nano nickel bicarbonate composite carbon electrode material SEM shape appearance figures that Fig. 2 present invention is prepared（10μm）;
The nano nickel bicarbonate composite carbon electrode material SEM shape appearance figures that Fig. 3 present invention is prepared（0.4μm）;
The nano nickel bicarbonate composite carbon electrode material circulation volt-ampere curve figure that Fig. 4 present invention is prepared;
The nano nickel bicarbonate composite carbon electrode material constant current charge-discharge diagram that Fig. 5 present invention is prepared.
Symbol description：
a：5mv/s；b:10 mv/s；c: 20 mv/s；d：50 mv/s；e：1A/g；f：2A/g；g：5 A/g；h：10A/g.
Embodiment
With reference to embodiment, the invention will be further described.
A kind of preparation method of nano nickel bicarbonate composite carbon electrode material, the preparation method comprises the following steps：
（1）The honey of 1-10 parts by weight is dissolved in the water, after stirring, the first centrifugal treating is carried out, takes supernatant liquor；
（2）In step（1）1-10 parts by weight of urea, six water nickel chlorides of 0.5-15 parts by weight are added in described supernatant liquor,
40-80 parts by weight water, after being sufficiently stirred for, obtains precursor solution；
（3）By step（2）Described solution is transferred in autoclave, and it is 100-200 DEG C to set reaction temperature, and the time is
12-24h, after reaction terminates, is cooled to room temperature, obtains pre-product；
（4）By step（3）Described pre-product, carries out the second centrifugal treating, by lower sediment drying process after centrifugation, obtains and slightly produce
Thing；
（5）By step（4）Described crude product is warming up to after 250-350 DEG C using 0.5-15 DEG C/min heating rates and is incubated 0.5-
5h, is then cooled to room temperature, obtains nano nickel bicarbonate composite carbon electrode material.
As a kind of perferred technical scheme, the step（4）In, the rotating speed of the second centrifugal treating turns for 6000-8000
It is per minute, pre-product is centrifuged 3-5 times as solvent displacement using deionized water, ethanol.
As a kind of perferred technical scheme, the step（4）In the temperature of drying process be 40-70 DEG C, the time is
15-28h。
As a kind of perferred technical scheme, the step（5）Middle heating rate is 1-10 DEG C/min.
As a kind of perferred technical scheme, the condition of first centrifugal treating is that rotating speed is 3000-5000 revolutions per minute
Clock, the time is 5-20 minutes.Heretofore described first centrifugal treating honey solution is mainly effective remove in natural honey
Water insoluble impurity.
Due to different in natural honey in the preparation method of nano nickel bicarbonate composite carbon electrode material of the present invention
The carbohydrate of chain length（Such as：Fructose, glucose etc.）, urea, six water nickel chlorides be sufficiently mixed in whipping process, wherein in nickel chloride
Nickel ion and above-mentioned carbohydrate surface oxygen-containing functional group between electrostatic attraction act on cause nickel ion be anchored on oxygen-containing official
Can group nearby, with the progress of hydro-thermal reaction, honey is spherical carbon by high temperature cabonization, at the same the carbonate that is decomposed to form of urea with
And hydroxyl and nickel ion precipitation generation bicarbonate nickel, obtain each component and be distributed relatively uniform combination electrode material.
Instant invention overcomes in the prior art due to carbon material and Ni (HCO3)2Deposited between crystal structure and surface texture
In larger difference, cause carbon material and Ni (HCO3)2Between interface bond intensity is weaker, nanocomposite constituents skewness, with
And the technology resistance that the electrochemical energy storage performance of combination electrode material is greatly reduced.The present invention is closed by an a kind of simple, step
Into process, using simple hydro-thermal reaction while carbon material is synthesized synthetically prepared Ni (HCO3)2, synchronized compound preparation
Obtain the Ni nanoparticle (HCO being evenly distributed3)2/ C-material, improves and adhesion is bonded at composite material interface, obtains chemical property
Excellent electrode material.
A kind of nano nickel bicarbonate composite carbon electrode material, is prepared using above-mentioned preparation method.Due to bicarbonate nickel
Electrical conductivity it is relatively low, be unfavorable for transporting for electric charge in electrochemical process, and the excellent carbon ball of electric conductivity can be made in composite
For conductive network, effectively improve the electrons transport property of electrode, so as to improve the efficiency of electrode electro Chemical reaction, simultaneously
The carbon material of above-mentioned excellent in mechanical performance can alleviate destruction of the electrode electro Chemical course of reaction stress to the stable row of electrode mechanics,
So as to obtain the combination electrode material of electrochemical energy storage excellent performance.
On the other hand, the raw material that the present invention is used has honey, urea etc., belongs to wide material sources and cheap original
Material, greatlys save cost, suitable for industrialized production.Preparation method of the present invention is simple and easy to operate, industrial easily to realize；Small system
Standby nanocomposite constituents distribution is relatively uniform, and the conductive network provided using carbon material improves the conductance property of system；Carbon
The excellent mechanical property of material improves the cyclical stability and service life of electrode material.
Embodiment 1
A kind of preparation method of nano nickel bicarbonate composite carbon electrode material, comprises the following steps：
（1）Weigh edible 1 gram of honey and be dissolved in water, magnetic agitation is after 2 hours, and 4000 revs/min centrifuge 10 minutes, take upper strata clear
Liquid is used as reaction solution；
（2）1 gram of urea is added into above-mentioned reaction solution, 0.5 gram of six water nickel chloride, 50g water, reaction solution passes through 1 hour
It is sufficiently stirred for, obtains precursor solution；
（3）Will be by step（2）Described precursor solution is transferred in autoclave, is placed in 180 DEG C of environment hydro-thermal reactions 20
Hour；
（4）After reaction terminates, treat that autoclave naturally cools to room temperature, obtain pre-product；
（5）Above-mentioned pre-product is subjected to the second centrifugal treating, handed over using 8000 rpms of rotating speed, deionized water and ethanol
For centrifugation 5 times；The precipitation obtained after above-mentioned centrifugation is placed in into 60 DEG C of drying boxes to dry 24 hours；
（6）Above-mentioned product is warming up to 300 DEG C using 0.5 DEG C/min heating rates, furnace cooling after being incubated 2 hours is produced.
A kind of nano nickel bicarbonate composite carbon electrode material, is prepared using above-mentioned preparation method.
Embodiment 2
A kind of preparation method of nano nickel bicarbonate composite carbon electrode material, comprises the following steps：
（1）Weigh edible 2 grams of honey and be dissolved in water, magnetic agitation is after 5 hours, and 3000 revs/min centrifuge 10 minutes, take upper strata clear
Liquid is used as reaction solution；
（2）3 grams of urea are added into above-mentioned reaction solution, 0.5 gram of six water nickel chloride, 40g water, reaction solution passes through 1 hour
It is sufficiently stirred for, obtains precursor solution；
（3）Will be by step（2）Described precursor solution is transferred in autoclave, is placed in 100 DEG C of environment hydro-thermal reactions 24
Hour；
（4）After reaction terminates, treat that autoclave naturally cools to room temperature, obtain pre-product；
（5）Above-mentioned pre-product is subjected to the second centrifugal treating, handed over using 6000 rpms of rotating speed, deionized water and ethanol
For centrifugation 3 times；The precipitation obtained after above-mentioned centrifugation is placed in into 60 DEG C of drying boxes to dry 24 hours；
（6）Above-mentioned product is warming up to 300 DEG C using 1 DEG C/min heating rates, furnace cooling after being incubated 2 hours is produced.
A kind of nano nickel bicarbonate composite carbon electrode material, is prepared using above-mentioned preparation method.
Embodiment 3
A kind of preparation method of nano nickel bicarbonate composite carbon electrode material, comprises the following steps：
（1）Weigh edible 5 grams of honey and be dissolved in water, magnetic agitation is after 5 hours, and 4000 revs/min centrifuge 20 minutes, take upper strata clear
Liquid is used as reaction solution；
（2）5 grams of urea are added into above-mentioned reaction solution, 10 gram of six water nickel chloride, 60g water, reaction solution filled by 1 hour
Divide stirring, obtain precursor solution；
（3）Will be by step（2）Described precursor solution is transferred in autoclave, is placed in 150 DEG C of environment hydro-thermal reactions 20
When；
（4）After reaction terminates, treat that autoclave naturally cools to room temperature, obtain pre-product；
（5）Above-mentioned pre-product is subjected to the second centrifugal treating, handed over using 7000 rpms of rotating speed, deionized water and ethanol
For centrifugation 5 times；The precipitation obtained after above-mentioned centrifugation is placed in into 70 DEG C of drying boxes to dry 20 hours；
（6）Above-mentioned product is warming up to 250 DEG C using 10 DEG C/min heating rates, furnace cooling after being incubated 5 hours is produced.
A kind of nano nickel bicarbonate composite carbon electrode material, is prepared using above-mentioned preparation method.
Embodiment 4
A kind of preparation method of nano nickel bicarbonate composite carbon electrode material, comprises the following steps：
（1）Weigh edible 10 grams of honey and be dissolved in water, magnetic agitation is after 5 hours, and 5000 revs/min centrifuge 5 minutes, take upper strata clear
Liquid is used as reaction solution；
（2）10 grams of urea are added into above-mentioned reaction solution, 15 gram of six water nickel chloride, 80g water, reaction solution passes through 1 hour
It is sufficiently stirred for, obtains precursor solution；
（3）Will be by step（2）Described precursor solution is transferred in autoclave, is placed in 200 DEG C of environment hydro-thermal reactions 12
When；
（4）After reaction terminates, treat that autoclave naturally cools to room temperature, obtain pre-product；
（5）Above-mentioned pre-product is subjected to the second centrifugal treating, handed over using 8000 rpms of rotating speed, deionized water and ethanol
For centrifugation 4 times；The precipitation obtained after above-mentioned centrifugation is placed in into 70 DEG C of drying boxes to dry 20 hours；
（6）Above-mentioned product is warming up to 350 DEG C using 15 DEG C/min heating rates, furnace cooling after being incubated 3 hours is produced.
A kind of nano nickel bicarbonate composite carbon electrode material, is prepared using above-mentioned preparation method.
With reference to accompanying drawing 1-4, the nano nickel bicarbonate composite carbon electrode material X-ray diffraction that the present invention is prepared in Fig. 1
Figure coincide with standard card 15-0782, illustrates to prepare bicarbonate nickel；The nano-calcium carbonate hydrogen that the present invention is prepared in Fig. 2
The composite regular appearance that the nickel composite carbon electrode material SEM display present invention is prepared, is evenly distributed；It is of the invention in Fig. 3
The nano nickel bicarbonate composite carbon electrode material circulation volt-ampere curve figure prepared, illustrates that the electrode material prepared is typical
Fake capacitance electrode material, electrode material has excellent electrochemical reversibility；The nano-calcium carbonate hydrogen that the present invention is prepared in Fig. 4
The specific capacitance value of nickel composite carbon electrode material constant current charge-discharge diagram electrode as seen from the figure under 1 A/g charging and discharging currents density,
The specific capacitance value of electrode material can reach 505 F/g, with higher specific capacitance value, illustrate the unit mass of electrode material
Store electric charge can be higher, it can thus be appreciated that the energy density of electrode material is larger, it is possible to achieve the storage of Large Copacity electric charge.
The present invention is anti-using simple hydro-thermal using raw material cheap and easy to get using simple, one-step synthesis process
Should synthesize carbon material while synthetically prepared Ni (HCO3)2, synchronized compound prepares the Ni nanoparticle (HCO being evenly distributed3)2/
C-material, improves and adhesion is bonded at composite material interface, obtains the electrode material of electrochemical performance.Instant invention overcomes
In the prior art due to carbon material and Ni (HCO3)2There is larger difference between crystal structure and surface texture, cause carbon material
With Ni (HCO3)2Between interface bond intensity is weaker, nanocomposite constituents skewness, and combination electrode material electrification
Learn the technology resistance that energy-storage property is greatly reduced.
Claims (5)
1. a kind of preparation method of nano nickel bicarbonate composite carbon electrode material, it is characterised in that the preparation method is included such as
Lower step：
（1）The honey of 1-10 parts by weight is dissolved in the water, after stirring, the first centrifugal treating is carried out, takes supernatant liquor；
（2）In step（1）1-10 parts by weight of urea, six water nickel chlorides of 0.5-15 parts by weight are added in described supernatant liquor,
40-80 parts by weight water, after being sufficiently stirred for, obtains precursor solution；
（3）By step（2）Described precursor solution is transferred in autoclave, and it is 100-200 DEG C to set reaction temperature, when
Between be 12-24h, reaction terminate after, be cooled to room temperature, obtain pre-product；
（4）By step（3）Described pre-product, carries out the second centrifugal treating, by lower sediment drying process after centrifugation, obtains and slightly produce
Thing；
（5）By step（4）Described crude product is warming up to after 250-350 DEG C using 0.5-15 DEG C/min heating rates and is incubated 0.5-
5h, is then cooled to room temperature, obtains nano nickel bicarbonate composite carbon electrode material.
2. the preparation method of nano nickel bicarbonate composite carbon electrode material according to claim 1, it is characterised in that described
Step（4）In, the rotating speed of the second centrifugal treating is 6000-8000 rpms, is solvent displacement to pre- using deionized water, ethanol
Product is centrifuged 3-5 times.
3. the preparation method of nano nickel bicarbonate composite carbon electrode material according to claim 1, it is characterised in that described
Step（4）In drying process temperature be 40-70 DEG C, the time is 15-28h.
4. the preparation method of nano nickel bicarbonate composite carbon electrode material according to claim 1, it is characterised in that described
Step（5）Middle heating rate is 1-10 DEG C/min.
5. the preparation method of nano nickel bicarbonate composite carbon electrode material according to claim 1, it is characterised in that described
The condition of first centrifugal treating is that rotating speed is 3000-5000 rpms, and the time is 5-20 minutes.
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Cited By (2)
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| CN108364798A (en) * | 2018-01-04 | 2018-08-03 | 同济大学 | Spongy C/Ni (the HCO in sea3)2- Ni composite material and preparation methods |
| CN112551523A (en) * | 2021-01-05 | 2021-03-26 | 齐鲁工业大学 | Microwave-assisted method for preparing honey-based derived carbon electrode material |
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| CN101962211A (en) * | 2010-10-26 | 2011-02-02 | 南京工业大学 | Method for preparing nano nickel bicarbonate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108364798A (en) * | 2018-01-04 | 2018-08-03 | 同济大学 | Spongy C/Ni (the HCO in sea3)2- Ni composite material and preparation methods |
| CN112551523A (en) * | 2021-01-05 | 2021-03-26 | 齐鲁工业大学 | Microwave-assisted method for preparing honey-based derived carbon electrode material |
| CN112551523B (en) * | 2021-01-05 | 2022-07-19 | 齐鲁工业大学 | Microwave-assisted method for preparing honey-based derived carbon electrode material |
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