CN107248453B - A kind of preparation method of hydroxyl nickel nitrate/carbon composite electrode material - Google Patents
A kind of preparation method of hydroxyl nickel nitrate/carbon composite electrode material Download PDFInfo
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- CN107248453B CN107248453B CN201710325117.0A CN201710325117A CN107248453B CN 107248453 B CN107248453 B CN 107248453B CN 201710325117 A CN201710325117 A CN 201710325117A CN 107248453 B CN107248453 B CN 107248453B
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- nickel nitrate
- electrode material
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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 invention discloses a kind of preparation methods of hydroxyl nickel nitrate/carbon composite electrode material, belong to field of material technology.Water-soluble organic-fuel is dissolved in water and is stirred evenly；Nickel nitrate is added in above-mentioned aqueous solution and is uniformly mixing to obtain predecessor aqueous solution；Adjust the pH of predecessor aqueous solution；Predecessor aqueous solution is placed in heating equipment, is passed through air, increases temperature, reacts certain time, obtains composite material washing, a kind of hydroxyl nickel nitrate/carbon composite electrode material of drying to obtain.The present invention prepares hydroxyl nickel nitrate/carbon composite electrode material by single step reaction, and preparation process is simple, quick, low energy consumption and is suitable for large-scale production.Hydroxyl nickel nitrate/carbon composite electrode material of preparation has nano-grade size, and hydroxyl nickel nitrate crystallinity is low, has excellent chemical property, can make the electrode material of supercapacitor.
Description
Technical field
The invention belongs to field of material technology, in particular to a kind of preparation side of hydroxyl nickel nitrate/carbon composite electrode material
Method.
Background technique
As the fast development of global economy, the continuous consumption of fossil energy, environmental pollution are got worse, one kind is studied
Efficiently, inexpensive, environmental-friendly, high performance energy conversion and stocking system are extremely urgent.Supercapacitor is due to it
Power density is high, and charge-discharge velocity is fast, has extended cycle life, and advantages of environment protection becomes a kind of energy storage of great potential
Device.Supercapacitor can be divided into double layer capacitor and fake capacitance capacitor according to the difference of Storage mechanism.Carbon material tool
Have the advantages that high-specific surface area, it is at low cost, have extended cycle life and be applied in electrochemical capacitor in double electrode layer, but it is than electricity
Hold and low seriously limits the business development of carbon-based electrode material；Transition metal based materials are since it is with high specific capacitance and excellent
Cyclic reversibility, therefore be considered as optimal Faraday pseudo-capacitance device electrode material, but the conduction of metal_based material
Property, stability it is poor, make actual capacity lower than theoretical capacity.Therefore at present more research trends in by double layer capacitor material
It is mutually compound with fake capacitance capacitor material, composite material is prepared, the coordinative role of the two is played, improves its electrification to a greater extent
Learn performance.And in terms of the preparation of combination electrode material, complicated cumbersome chemical synthesis path, high-cost synthesis material takes
When preparation process, the uncontrollable duplicate preparation condition of hardly possible, become limit its development and industrialization powerful resistance and bottleneck.
Summary of the invention
It is an object of the invention to disclose a kind of hydroxyl nickel nitrate/carbon composite as electrode material for super capacitor
And preparation method thereof.This method preparation process is simple, and reactant is cheap, is suitble to large-scale production；It consumes energy in production process
It is few, it is pollution-free；Obtained novel hydroxyl nickel nitrate/carbon composite is as electrode material specific capacity with higher.
Technical solution of the present invention:
A kind of preparation method of hydroxyl nickel nitrate/carbon composite electrode material, steps are as follows:
(1) precursor water solution is prepared
Precursor water solution includes water, fuel and nickel nitrate, is mixed according to mass ratio 100:5~40:20~50；
The pH of the precursor water solution is 1-6, preferably 3-4.
(2) solution combustion reacts to obtain crude product
Precursor water solution that step (1) obtains carries out combustion reaction, and combustion reaction condition is normal pressure, in air environment,
Reaction temperature is 200~230 DEG C, and the reaction time is 40min~1h, obtains the thick production of hydroxyl nickel nitrate/carbon composite electrode material
Object；
(3) it washes, dry hydroxyl nickel nitrate/carbon composite electrode material crude product, obtain hydroxyl nitric acid nickel carbon compound electric
Pole material；Wherein, hydroxyl nickel nitrate chemical formula is Ni3(NO3)2(OH)4, crystalline state is amorphous or crystal, crystal grain
Having a size of 5-50nm；In hydroxyl nickel nitrate/carbon composite electrode material of every 100 parts of quality, the quality of carbon is 3~8.
The fuel be water soluble organic substance, water soluble starch, glucose, hydroxyl glucose, chitosan, citric acid,
The mixing of one or more of sucrose, water-soluble cellulose.
Sodium hydrate aqueous solution, potassium hydroxide aqueous solution or ammonium hydroxide is selected to adjust the pH of precursor water solution, preferably ammonia
Water.
Reaction temperature is increased to 215 DEG C from room temperature in step (2), and heating rate is 30-50 DEG C/min, preferred heating speed
Rate is 40 DEG C/min.
Reaction temperature is 215 DEG C in step (2).
Beneficial effects of the present invention: hydroxyl nickel nitrate/carbon composite is prepared using solution combustion method, not only preparation process
Simply, the consumption of energy is reduced, and higher specific capacity can be shown with the material of large scale preparation and preparation, in 1A/g
Current density under, capacity has huge potentiality and practical application value up to 1086F/g, in supercapacitor field.
Detailed description of the invention
Fig. 1 is the hydroxyl nickel nitrate/carbon composite electrode material XRD diagram prepared in the present invention.
Fig. 2 is the hydroxyl nickel nitrate/carbon composite electrode material electrode material TEM figure prepared in the present invention.
Fig. 3 is the hydroxyl nickel nitrate/carbon composite electrode material electrode material constant current charge-discharge figure prepared in the present invention.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Embodiment 1
The nickel nitrate and glucose that mass ratio is 8:1 are weighed, first glucose is dissolved in 9ml deionized water, it is completely molten
Nickel nitrate is added after solution thereto, progress ultrasonic mixing is uniform, ultrasonic time 20min, and ammonium hydroxide adjusting pH value of solution is then added and is
4, ultrasound 20min again.Then it is gradually warmed up from room temperature to 215 DEG C, in 215 DEG C of reaction time 40min, will react in an oven
Material afterwards is washed, and in 60 DEG C of vacuum dry 12h, obtains hydroxyl nickel nitrate/carbon composite electrode material to the end.
Electrode material for super capacitor hydroxyl nickel nitrate/carbon composite electrode material XRD diagram made from the present embodiment is as schemed
1, it can be seen that the hydroxyl nickel nitrate generated, crystallization degree be not high.Hydroxyl nickel nitrate/carbon composite electrode material electrode of preparation
The TEM figure of material such as Fig. 2, it can be observed that the random cake mass that surface is smooth；Apparent striated is not observed, says
It is bright to be amorphous material, it is more advantageous to the transmitting of charge；Nickel nitrate/carbon composite electrode material constant current charge-discharge curve can
To find out under the current density of 1A/g, capacity is up to 1086F/g.Therefore the method for the present invention is used, experiment can be greatly simplified
Process, and the abundant raw material used, cost is relatively low, while can also obtain higher electrochemistry capacitance.
Embodiment 2
The nickel nitrate and glucose that mass ratio is 10:1 are weighed, first glucose is dissolved in 9ml deionized water, it is completely molten
Nickel nitrate is added after solution thereto, progress ultrasonic mixing is uniform, ultrasonic time 20min, and ammonium hydroxide adjusting pH value of solution is then added and is
4, ultrasound 20min again.Then it is gradually warmed up from room temperature to 215 DEG C, in 215 DEG C of reaction time 40min, will react in an oven
Material afterwards is washed, and in 60 DEG C of vacuum dry 12h, obtains hydroxyl nickel nitrate/carbon composite electrode material to the end.
The embodiment hydroxyl nickel nitrate/the preparation method is the same as that of Example 1 for carbon composite electrode material, difference is only that forerunner
The mass ratio of nickel nitrate and glucose is 10:1 in object.Hydroxyl nickel nitrate/carbon composite electrode material appearance of embodiment preparation
Amount is 1054F/g.
Embodiment 3
The nickel nitrate and glucose that mass ratio is 8:1 are weighed, first glucose is dissolved in 9ml deionized water, it is completely molten
Nickel nitrate is added after solution thereto, progress ultrasonic mixing is uniform, ultrasonic time 20min, and ammonium hydroxide adjusting pH value of solution is then added and is
3, ultrasound 20min again.Then it is gradually warmed up from room temperature to 215 DEG C, in 215 DEG C of reaction time 40min, will react in an oven
Material afterwards is washed, and in 60 DEG C of vacuum dry 12h, obtains hydroxyl nickel nitrate/carbon composite electrode material to the end.
The embodiment hydroxyl nickel nitrate/the preparation method is the same as that of Example 1 for carbon composite electrode material, difference is only that forerunner
Object pH is adjusted to 3.Hydroxyl nickel nitrate/carbon composite electrode material capacity of embodiment preparation is 1023F/g.
Embodiment 4
The nickel nitrate and water soluble starch that mass ratio is 8:1 are weighed, water soluble starch is first dissolved in 9ml deionized water
In, nickel nitrate is added after being completely dissolved thereto, progress ultrasonic mixing is uniform, ultrasonic time 20min, and ammonium hydroxide is then added and adjusts
PH value of solution is 4, again ultrasound 20min.Then it is gradually warmed up in an oven from room temperature to 215 DEG C, 215 DEG C of reaction time
40min washes the material after reaction, and in 60 DEG C of vacuum dry 12h, the hydroxyl nitric acid nickel carbon obtained to the end is compound
Electrode material.
The embodiment hydroxyl nickel nitrate/the preparation method is the same as that of Example 1 for carbon composite electrode material, difference is only that forerunner
Fuel is selected as water soluble starch in object.The embodiment preparation hydroxyl nickel nitrate/carbon composite electrode material capacity be
1066F/g。
Claims (4)
1. a kind of preparation method of hydroxyl nickel nitrate/carbon composite electrode material, which is characterized in that steps are as follows:
(1) precursor water solution is prepared
Precursor water solution includes water, water soluble organic substance and nickel nitrate, is mixed according to mass ratio 100:5 ~ 40:20 ~ 50；
The pH of the precursor water solution is 1-6；
(2) solution combustion reacts to obtain crude product
Precursor water solution that step (1) obtains carries out combustion reaction, and combustion reaction condition is normal pressure, in air environment, reaction
Temperature is 200 ~ 230 DEG C, and the reaction time is 40min ~ 1h, obtains hydroxyl nickel nitrate/carbon composite electrode material crude product；
(3) it washes, dry hydroxyl nickel nitrate/carbon composite electrode material crude product, obtain hydroxyl nickel nitrate/carbon composite electrode material
Material；Wherein, hydroxyl nickel nitrate chemical formula is Ni3(NO3)2(OH)4, crystalline state is amorphous or crystal, crystal grain size
For 5-50nm；In hydroxyl nickel nitrate/carbon composite electrode material of every 100 parts of quality, the quality of carbon is 3 ~ 8.
2. preparation method according to claim 1, which is characterized in that the water soluble organic substance be water soluble starch,
The mixing of one or more of glucose, chitosan, citric acid, sucrose, water-soluble cellulose.
3. preparation method according to claim 1 or 2, which is characterized in that selection sodium hydrate aqueous solution, potassium hydroxide water
Solution or ammonium hydroxide adjust the pH of precursor water solution.
4. preparation method according to claim 1 or 2, which is characterized in that reaction temperature is increased to from room temperature in step (2)
215 DEG C, heating rate is 30-50 DEG C/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1564345A (en) * | 2004-03-31 | 2005-01-12 | 北京科技大学 | Method of synthetizing lithium ion cell positive electrode material through solution burning |
| CN102509785A (en) * | 2011-10-31 | 2012-06-20 | 长沙宝锋能源科技有限公司 | Process for synthesizing three-dimensional nanometer porous composite strips by combusting controllable solution |
| CN104815983A (en) * | 2015-04-20 | 2015-08-05 | 齐鲁工业大学 | Carbon-coated nickel oxide/metallic nickel and simple synthesis method thereof |
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- 2017-05-11 CN CN201710325117.0A patent/CN107248453B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1564345A (en) * | 2004-03-31 | 2005-01-12 | 北京科技大学 | Method of synthetizing lithium ion cell positive electrode material through solution burning |
| CN102509785A (en) * | 2011-10-31 | 2012-06-20 | 长沙宝锋能源科技有限公司 | Process for synthesizing three-dimensional nanometer porous composite strips by combusting controllable solution |
| CN104815983A (en) * | 2015-04-20 | 2015-08-05 | 齐鲁工业大学 | Carbon-coated nickel oxide/metallic nickel and simple synthesis method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Shape tailored Ni3(NO3)2(OH)4 nano-flakes simulating 3-D bouquet-like structures for supercapacitors: exploring the effect of electrolytes on stability and performance;Jickson Joseph et al.;《RSC Advances》;20140812;第4卷;第39378–39385页 |
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