CN107331538B - 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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- CN107331538B CN107331538B CN201710667018.0A CN201710667018A CN107331538B CN 107331538 B CN107331538 B CN 107331538B CN 201710667018 A CN201710667018 A CN 201710667018A CN 107331538 B CN107331538 B CN 107331538B
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- electrode material
- carbon electrode
- composite carbon
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- nano nickel
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- 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 fields, disclose a kind of preparation method of nano nickel bicarbonate composite carbon electrode material,(1)Honey is dissolved in the water, after stirring evenly, centrifugal treating takes supernatant liquor;(2)In step(1)Urea, six water nickel chlorides are added in the supernatant liquor, is configured to solution, after being sufficiently stirred, obtains precursor solution;(3)By step(2)The precursor solution is transferred in autoclave, after reaction, is cooled to room temperature, is obtained pre-product;(4)By step(3)The pre-product carries out centrifugal treating, lower sediment after centrifugation is dried, crude product is obtained;(5)By step(4)The crude product is then cooled to room temperature, obtains nano nickel bicarbonate composite carbon electrode material using being kept the temperature after the heating of 0.5-15 DEG C/min heating rates.The present invention solves the problems, such as that bicarbonate nickel composite carbon electrode material component is non-uniform, and is prepared with excellent properties composite material.
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 quickly universal of portable electronic device, wearable device continue to bring out and the electronic vapour of clean environment firendly
Vehicle flourishes, and power storage already becomes 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, higher power density, energy stores
It is density, the advantages that charging time is short, service life is long, many in mobile communication, national defence, aerospace, consumption electronic product etc.
Field is widely used there is huge application value and market potential and is expected to change traditional energy-consuming pattern, solves
The environmental problem of getting worse.
Electrode material is the core component of performance of the supercapacitor, and commercialization degree higher carbon material has higher at present
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 has apparent 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, environmental-friendly in electrode material for super capacitor
It is widely studied.Research shows that 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 above-mentioned electrode material there are resistivity it is higher, cyclical stability is poor the shortcomings of;And pass through compound tool
Have excellent conductive capability, mechanical property carbon material, utilize the excellent electric conductivity of carbon material to improve charge in electrochemical process
Transporting in combination electrode material, excellent mechanical property reduce Ni (HCO in electrochemical process3)2Relaxation variation generates
Influence of the stress to electrode material cycle life, to be expected further to promote the electrochemistry storing up electricity performance of 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 obtains
Excellent chemical property.
Invention content
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 unevenly distributed
Problem, the present invention provide a kind of preparation method of nano nickel bicarbonate composite carbon electrode material.
The present invention adopts the following technical scheme that:A kind of preparation method of nano nickel bicarbonate composite carbon electrode material, it is described
Preparation method includes the following steps:
(1)The honey of 1-10 parts by weight is dissolved in the water, after stirring evenly, the first centrifugal treating is carried out, takes upper layer clear
Liquid;
(2)In step(1)Six water chlorinations of 1-10 parts by weight of urea, 0.5-15 parts by weight are added in the supernatant liquor
Nickel, 40-80 parts by weight water, after being sufficiently stirred, obtains precursor solution;
(3)By step(2)The solution is transferred in autoclave, and setting reaction condition is 100-200 DEG C, the time
It is cooled to room temperature after reaction for 12-24h, obtains pre-product;
(4)By step(3)The pre-product carries out the second centrifugal treating, lower sediment after centrifugation is dried, is obtained
Crude product;
(5)By step(4)The crude product is kept the temperature after being warming up to 250-350 DEG C using 0.5-15 DEG C/min heating rates
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, is with deionized water, ethyl alcohol
Solvent displacement centrifuges pre-product 3-5 times.
The step(4)In the condition of drying process be temperature be 40-70 DEG C, drying time 15-28h.
The step(5)Middle heating rate is 1-10 DEG C/min.
It is 3000-5000 rpms that the condition of first centrifugal treating, which is rotating speed, and the time is 5-20 minutes.
Preparation method of the present invention is simple and easy to operate, industrial easy to implement;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.
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
Specific implementation mode
The invention will be further described With reference to embodiment.
A kind of preparation method of nano nickel bicarbonate composite carbon electrode material, the preparation method include the following steps:
(1)The honey of 1-10 parts by weight is dissolved in the water, after stirring evenly, the first centrifugal treating is carried out, takes upper layer clear
Liquid;
(2)In step(1)Six water chlorinations of 1-10 parts by weight of urea, 0.5-15 parts by weight are added in the supernatant liquor
Nickel, 40-80 parts by weight water, after being sufficiently stirred, obtains precursor solution;
(3)By step(2)The solution is transferred in autoclave, and setting reaction temperature is 100-200 DEG C, the time
It is cooled to room temperature after reaction for 12-24h, obtains pre-product;
(4)By step(3)The pre-product carries out the second centrifugal treating, lower sediment after centrifugation is dried, is obtained
Crude product;
(5)By step(4)The crude product is kept the temperature after being warming up to 250-350 DEG C using 0.5-15 DEG C/min heating rates
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, ethyl alcohol.
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, it is 3000-5000 revolutions per minute that the condition of first centrifugal treating, which is rotating speed,
Clock, time are 5-20 minutes.In the mainly effective removal natural honey of heretofore described first centrifugal treating honey solution
Impurity not soluble in water.
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 so that nickel ion be anchored on oxygen-containing official
Can group nearby, with the progress of hydro-thermal reaction, honey is spherical shape carbon by high temperature cabonization, at the same the carbonate that is decomposed to form of urea with
And hydroxyl generates bicarbonate nickel with nickel ion precipitation, obtains each component and is distributed relatively uniform combination electrode material.
The present invention overcomes in the prior art due to carbon material and Ni (HCO3)2It is deposited between crystal structure and surface texture
In larger difference, lead to carbon material and Ni (HCO3)2Between interface bond intensity is weaker, nanocomposite constituents are unevenly distributed, 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
At process, Ni (HCO are synthetically prepared while synthesizing carbon material using simple hydro-thermal reaction3)2, synchronized compound preparation
Obtain the Ni nanoparticle (HCO being evenly distributed3)2/ C-material improves and is bonded binding force 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
Conductivity it is relatively low, be unfavorable for transporting for charge in electrochemical process, and the excellent carbon ball of electric conductivity can be made in composite material
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 the destruction that electrode electro Chemical reaction process stress stablizes electrode mechanics row,
To obtain the combination electrode material that electrochemical energy storage is had excellent performance.
On the other hand, the raw material that the present invention uses has honey, urea etc., belongs to derive from a wealth of sources and cheap original
Material, is greatly saved cost, is suitable for industrialized production.Preparation method of the present invention is simple and easy to operate, industrial easy to implement;It prepares
Nanocomposite constituents distribution it is relatively uniform, the conductive network provided using carbon material improves the conductance property of system;Carbon materials
Expect that excellent mechanical property 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, includes the following steps:
(1)It weighs edible 1 gram of honey and is dissolved in water, after 2 hours, 4000 revs/min centrifuge 10 minutes magnetic agitation, take
Layer clear liquid is 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, it is small that reaction solution passes through 1
When be sufficiently stirred, obtain precursor solution;
(3)It will be by step(2)The precursor solution is transferred in autoclave, and it is anti-to be placed in 180 DEG C of environment hydro-thermals
It answers 20 hours;
(4)After reaction, it waits for autoclave cooled to room temperature, obtains pre-product;
(5)Above-mentioned pre-product is subjected to the second centrifugal treating, using 8000 rpms of rotating speed, deionized water and second
Alcohol alternating centrifugal 5 times;The precipitation obtained after above-mentioned centrifugation is placed in 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 keeping the temperature 2 hours, i.e.,
?.
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, includes the following steps:
(1)It weighs edible 2 grams of honey and is dissolved in water, after 5 hours, 3000 revs/min centrifuge 10 minutes magnetic agitation, take
Layer clear liquid is 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, it is small that reaction solution passes through 1
When be sufficiently stirred, obtain precursor solution;
(3)It will be by step(2)The precursor solution is transferred in autoclave, and it is anti-to be placed in 100 DEG C of environment hydro-thermals
It answers 24 hours;
(4)After reaction, it waits for autoclave cooled to room temperature, obtains pre-product;
(5)Above-mentioned pre-product is subjected to the second centrifugal treating, using 6000 rpms of rotating speed, deionized water and second
Alcohol alternating centrifugal 3 times;The precipitation obtained after above-mentioned centrifugation is placed in 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, after heat preservation 2 hours furnace cooling to get.
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, includes the following steps:
(1)It weighs edible 5 grams of honey and is dissolved in water, after 5 hours, 4000 revs/min centrifuge 20 minutes magnetic agitation, take
Layer clear liquid is 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 was by 1 hour
Be sufficiently stirred, obtain precursor solution;
(3)It will be by step(2)The precursor solution is transferred in autoclave, and it is anti-to be placed in 150 DEG C of environment hydro-thermals
When answering 20;
(4)After reaction, it waits for autoclave cooled to room temperature, obtains pre-product;
(5)Above-mentioned pre-product is subjected to the second centrifugal treating, using 7000 rpms of rotating speed, deionized water and second
Alcohol alternating centrifugal 5 times;The precipitation obtained after above-mentioned centrifugation is placed in 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 keeping the temperature 5 hours, i.e.,
?.
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, includes the following steps:
(1)It weighs edible 10 grams of honey and is dissolved in water, after 5 hours, 5000 revs/min centrifuge 5 minutes magnetic agitation, take
Layer clear liquid is as reaction solution;
(2)10 grams of urea are added into above-mentioned reaction solution, 15 gram of six water nickel chloride, 80g water, it is small that reaction solution passes through 1
When be sufficiently stirred, obtain precursor solution;
(3)It will be by step(2)The precursor solution is transferred in autoclave, and it is anti-to be placed in 200 DEG C of environment hydro-thermals
When answering 12;
(4)After reaction, it waits for autoclave cooled to room temperature, obtains pre-product;
(5)Above-mentioned pre-product is subjected to the second centrifugal treating, using 8000 rpms of rotating speed, deionized water and second
Alcohol alternating centrifugal 4 times;The precipitation obtained after above-mentioned centrifugation is placed in 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 keeping the temperature 3 hours, i.e.,
?.
A kind of nano nickel bicarbonate composite carbon electrode material, is prepared using above-mentioned preparation method.
In conjunction with attached drawing 1-4, the nano nickel bicarbonate composite carbon electrode material X-ray diffraction of the invention being prepared in Fig. 1
Figure coincide with standard card 15-0782, illustrates that bicarbonate nickel is prepared;The nano-calcium carbonate hydrogen that the present invention is prepared in Fig. 2
The composite material 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 being prepared illustrates that the electrode material prepared is typical
Fake capacitance electrode material, electrode material have 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 the charging and discharging currents density of 1 A/g,
The specific capacitance value of electrode material can reach 505 F/g, have higher specific capacitance value, illustrate the unit mass of electrode material
Store charge can be higher, it can thus be appreciated that the energy density of electrode material is larger, the storage of large capacity charge may be implemented.
The present invention is anti-using simple hydro-thermal using raw material cheap and easy to get using simple, one-step synthesis process
It should be synthetically prepared Ni (HCO while synthesizing carbon material3)2, synchronized compound prepares the Ni nanoparticle (HCO being evenly distributed3)2/
C-material improves and is bonded binding force at composite material interface, obtains the electrode material of electrochemical performance.The present invention overcomes
In the prior art due to carbon material and Ni (HCO3)2There are larger differences between crystal structure and surface texture, lead to carbon material
With Ni (HCO3)2Between interface bond intensity is weaker, nanocomposite constituents are unevenly distributed and the electrification of combination electrode material
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, which is characterized in that the preparation method includes such as
Lower step:
(1)The honey of 1-10 parts by weight is dissolved in the water, after stirring evenly, the first centrifugal treating is carried out, takes supernatant liquor;
(2)In step(1)Be added in the supernatant liquor 1-10 parts by weight of urea, 0.5-15 parts by weight six water nickel chlorides,
40-80 parts by weight water, after being sufficiently stirred, obtains precursor solution;
(3)By step(2)The precursor solution is transferred in autoclave, and setting reaction temperature is 100-200 DEG C, when
Between be cooled to room temperature after reaction for 12-24h, obtain pre-product;
(4)By step(3)The pre-product carries out the second centrifugal treating, lower sediment after centrifugation is dried, obtains and slightly produces
Object;
(5)By step(4)The crude product keeps the temperature 0.5- after being warming up to 250-350 DEG C using 0.5-15 DEG C/min heating rates
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, which is characterized 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, ethyl alcohol
Product centrifuges 3-5 times.
3. the preparation method of nano nickel bicarbonate composite carbon electrode material according to claim 1, which is characterized in that described
Step(4)In drying process temperature be 40-70 DEG C, time 15-28h.
4. the preparation method of nano nickel bicarbonate composite carbon electrode material according to claim 1, which is characterized 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, which is characterized 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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CN108364798B (en) * | 2018-01-04 | 2019-07-05 | 同济大学 | Spongy C/Ni (HCO3) the 2-Ni composite material and preparation method in sea |
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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