CN107611379A - A kind of three-dimensional nickel hydroxide graphene composite material, its preparation method and application - Google Patents
A kind of three-dimensional nickel hydroxide graphene composite material, its preparation method and application Download PDFInfo
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- CN107611379A CN107611379A CN201710731129.3A CN201710731129A CN107611379A CN 107611379 A CN107611379 A CN 107611379A CN 201710731129 A CN201710731129 A CN 201710731129A CN 107611379 A CN107611379 A CN 107611379A
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- 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
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Abstract
The present invention provides a kind of three-dimensional nickel hydroxide graphene composite material, is made up of the conductive network with three-dimensional structure and the nickel hydroxide loaded above it；The three-dimensional conductive network of composite is made up of stannic oxide/graphene nano piece, has macropore, micropore and mesoporous pore structure；The size for the nickel hydroxide being supported on three-dimensional conductive network is 50 nanometers~500 microns, and the quality accounting of nickel hydroxide is the preparation method that 50~95% present invention also propose the composite in composite.Three-dimensional nickel hydroxide graphene composite material proposed by the present invention has high electric conductivity, excellent resistance to poison and good circulation stability with super, it is ideal zinc-nickel cell positive electrode, can be widely applied to the fields such as various portable electric appts, electric automobile and Aero-Space；In addition, the compound can be prepared, suitable for industrialized production from low-cost raw material by repeated high, simple, the time-consuming few technique of process.
Description
Technical field
The invention belongs to battery material field, and in particular to a kind of positive electrode of nickel radical battery, and preparation method thereof and
Using.
Background technology
With the continuous enhancing of environmental protection consciousness, the research and development of novel high-performance green secondary power battery at present oneself
Through as key subjects in the urgent need to address.Zinc-nickel cell is made up of zinc electrode and nickel electrode, is had zinc in zinc-silver oxide cell concurrently and is born
The superior function of nickel positive pole long-life in high capacity and ickel-cadmium cell, it is a kind of High-performance green secondary power battery.Zinc-nickel
Secondary cell performance characteristics include:Operating voltage is high (higher than Ni-MH battery and nickel-cadmium cell), high (the generally plumbic acid of energy density
2 times of battery, 1,5 times of nickel-cadmium cell), power density height (being only second to lithium ion battery), operating temperature is wide (- 20-50 DEG C),
Memory-less effect, the production of battery and does not produce pollution to environment using process, is described as real green battery, the storage of zinc
Amount is abundant, cheap.Oneself turns into after lead-acid battery, ickel-cadmium cell, Ni-H cell and lithium ion battery zinc-nickel cell, more
For cheap and practical novel high-performance green power battery.
So far, compared relative to zinc-nickel battery anode material and electrolyte system, zinc-nickel cell with positive electrode
It is more ripe, but easily poisoned there are still positive pole, and the notable of the specific capacity poor efficiency of positive pole low (~200mAh/g) lacks
Point.Therefore, the research in this current field concentrate on Non-toxic, high usage, low cost new positive electrode research, develop and
In technology of preparing.
In recent years, three-dimensional net structure has been studied for zinc-nickel cell positive electrode, and in zinc-nickel cell cyclic process
Caused zinc oxide easily poisons positive pole, poison when causing the positive pole degradation failure, especially high power charging-discharging in charge and discharge process
Change problem is more prominent, and it is low to ultimately result in positive pole utilization rate.In three-dimensional net structure, conducting three-dimensional network structure has orderly
Porous structure, very stablize in charge and discharge process and homogeneous current distribution can be made, prevent the generation poisoned.But at present
The characteristics of zinc-nickel cell and limited preparation method still limit its practical application.
The content of the invention
The technical problems to be solved by the invention are easily poisoned and utilization rate for the nickel hydroxide positive plate of prior art
Deficiency the deficiencies of, there is provided it is a kind of it is resistance to poison, utilization rate height, excellent cycling performance, can be as the three of zinc-nickel cell positive electrode
Tie up nickel hydroxide-graphene composite material.
Second object of the present invention is to propose the preparation method of the composite.
Third object of the present invention is to propose the application of the composite.
The technical scheme for realizing the object of the invention is：
A kind of three-dimensional nickel hydroxide-graphene composite material, by the conductive network with three-dimensional structure and load above it
Nickel hydroxide composition；The three-dimensional conductive network of composite is made up of stannic oxide/graphene nano piece, has macropore, micropore and Jie
The pore structure in hole；The size for the nickel hydroxide being supported on three-dimensional conductive network is 50 nanometers~500 microns, composite
The quality accounting of middle nickel hydroxide is 50~95%.
The preparation method of three-dimensional nickel hydroxide-graphene composite material of the present invention, including step：
(1) nickel based compound is dispersed in water and/or organic solvent with graphene oxide, is then carried out in water heating kettle
Hydro-thermal reaction and/or solvent thermal reaction, temperature are 100 DEG C~300 DEG C, the wherein matter that feeds intake of nickel based compound and graphene oxide
Amount is than being 0.5~30:1；
(2) use selected from vacuum drying, be freeze-dried and (use freeze drier, dry according to a conventional method) and surpass and face
The product of preceding step is dried any of boundary's seasoning seasoning, obtains solid product, and as described three-dimensional nickel hydroxide-
Graphene composite material.
Wherein, the nickel based compound is nickel hydroxide, nickel chloride, nickel nitrate, nickel sulfate, one kind in nickel acetate or more
Kind；Described nickel based compound and the mass ratio that feeds intake of graphene oxide are 1~10:1.
One of optimal technical scheme of the present invention is that described organic solvent is ethanol, propyl alcohol, ethylene glycol, isopropanol, methyl
One or more combinations in pyrrolidones.
Another optimal technical scheme of the present invention is that nickel based compound is dispersed in water with graphene oxide in step (1)
In, the mass ratio of nickel based compound and water is 5：10~30.
It is highly preferred that step (1) uses hydro-thermal reaction, reaction temperature is 170~190 DEG C, and the reaction time is 10~15h.
According to the present invention, step (2) is preferably using freeze-drying or supercritical drying.Freeze-dried Medium and overcritical
Medium may each be water, ethanol, propyl alcohol, isopropanol etc..
Three-dimensional nickel hydroxide-graphene composite material of the present invention, or described preparation method is in nickel radical battery
Application.
A kind of nickel radical battery, the nickel radical battery just extremely following methods are made：By the three-dimensional hydrogen described in claim 1
Nickel oxide-graphene composite material, binder 60%PTFE, acetylene black, by 80：10：10 mass ratio is well mixed, and uses water
Uniformly it is applied to after being modulated into paste in nickel foam；
Dried 10~15 hours at 80 DEG C in vacuum drying oven.
The present invention has the following advantages that compared with prior art：
(1) present invention uses low-cost nickel based compound and graphene oxide (graphene) as raw material；(2) using simple
Hydro-thermal method or solvent-thermal method prepare three-dimensional nickel hydroxide-graphene composite material with three-dimensional network, their three-dimensional
Conductive network is highly stable in charge and discharge process；(3) the three-dimensional nickel hydroxide-graphene composite material of gained is used as zinc-nickel cell
Specific capacity during positive electrode is more than 200mAh/g；(4) the three-dimensional nickel hydroxide-graphene composite material of gained is used as zinc-nickel cell
With with good cycle performance (being higher than 160mAh/g after 500 repeated charges) during positive electrode.
To sum up, three-dimensional nickel hydroxide-graphene composite material of the invention has high electric conductivity, has super excellent resistance to
Poison and good circulation stability, be ideal zinc-nickel cell positive electrode, can be widely applied to various portable electrics
The fields such as sub- equipment, electric automobile and Aero-Space；In addition, the compound can pass through repetition from low-cost raw material
Property it is high, process is simple, takes few technique prepares, suitable for industrialized production.
Brief description of the drawings
Fig. 1 is the photo in kind of three-dimensional nickel hydroxide-graphene composite material of embodiment 1, it was demonstrated that it has three-dimensional
Gel structure；
Fig. 2 be embodiment 1 three-dimensional nickel hydroxide-graphene composite material morphology characterization result, scanning electron microscope (SEM) photograph
(SEM) confirm that nickel hydroxide is supported on graphenic surface；
Fig. 3 is the structural characterization result of three-dimensional nickel hydroxide-graphene composite material of embodiment 1,
Fig. 4 is the chemical property result of the three-dimensional nickel hydroxide-graphene composite material of the present invention：Embodiment 1 it is compound
100th constant-current discharge curve of the electrode made of thing under 1C multiplying powers；
Fig. 5 is the chemical property result of the three-dimensional nickel hydroxide-graphene composite material of the present invention：Embodiment 1 it is compound
Constant current cycle performance curve of the electrode made of thing under 1C multiplying powers.
Embodiment
Detailed description below is used to illustrate the present invention, but should not be construed as limiting the invention.
In embodiment, unless otherwise instructed, technological means used is this area conventional technology.
Embodiment 1：
A kind of three-dimensional nickel hydroxide-graphene composite material, it is made by the steps to obtain：
(1) by nickel hydroxide 500g and graphene oxide (graphene) 100g, (the two mass ratio is 5:1) mix, disperse
In 2100g water, then it is sealed in water heating kettle, at 180 ± 5 DEG C, reacts 12 hours or so；The gel photograph being prepared is shown in
Fig. 1.
(2) solid product is freeze-dried to obtain, as three-dimensional nickel hydroxide-graphene composite material.Product is spongy more
The three-dimensional composite material in hole, it is formed with micropore, mesoporous, macropore conductive network.
Pattern to gained three-dimensional nickel hydroxide-graphene composite material etc. characterizes.Fig. 2 shows the microcosmic shape of material
Looks, it is seen that three-dimensional nickel hydroxide-graphene composite material is by graphene of the average length between 1~100 μm and spherical hydrogen-oxygen
Change nickel composition.According to the addition of reactant, it is known that the mass ratio that ball-shape nickel hydroxide accounts for composite is 80% or so.Fig. 3
For the XRD spectrum of material, X-ray diffraction confirms that the nickel hydroxide crystal formation in gained nickel hydroxide-Graphene gel belongs to β-Ni
(OH)2；And there is the characteristic peak of graphene in collection of illustrative plates.
Battery performance test：
(1) by three-dimensional nickel hydroxide-graphene composite material, binder 60%PTFE, acetylene black, by 80：10：10 ratio
Example is well mixed, is uniformly applied to after being modulated into paste with water in nickel foam；
(2) dried 12 hours at 80 DEG C in vacuum drying oven；
(3) nickel foam for scribbling three-dimensional nickel hydroxide-graphene composite material is cut into disk and working electrode is made.
Test to the chemical property of electrode material is：Simulated battery using button CR2032 type systems, wherein
It is oxidation zinc load to electrode.Reversible capacity performance and the cycle performance experiment of electrode material are tested using constant current charge-discharge
Analysis.Discharge and recharge system is：Voltage range：1.2-2.0V；Cycle-index is generally 1-500 times.The present embodiment circulates 500 times.
Three-dimensional nickel hydroxide-graphene composite material is made into working electrode according to above-mentioned method and carries out corresponding electricity
Performance test, it is as a result as follows：In 1C discharge and recharges, stable specific capacity is 250mAh/g；Under above-mentioned multiplying power during discharge and recharge, 500
Capacity can keep more than the 80% of initial capacity after secondary repeated charge.As a result referring to table 1 and Fig. 4, Fig. 5.
Embodiment 2
Embodiment 2 provides a kind of three-dimensional nickel hydroxide-graphene composite material, and its preparation method is substantially with embodiment 1, no
With the mass ratio that feeds intake of its raw material nickel hydroxide and graphene oxide (graphene) is 10:1.(nickel hydroxide and graphene
It is 1000 mass parts and 100 mass parts respectively, the mass parts of water 4200)
Three-dimensional nickel hydroxide-graphene composite material is made into working electrode according to method same as Example 1 to go forward side by side
The corresponding electric performance test of row, it is as a result as follows：In 1C discharge and recharges, stable specific capacity is 200mAh/g；Filled under above-mentioned multiplying power
During electric discharge, capacity can keep more than the 70% of initial capacity after 500 repeated charges.
Embodiment 3
This example provides a kind of three-dimensional nickel hydroxide-graphene composite material, and its preparation method is different substantially with embodiment 1
, the mass ratio that feeds intake of its raw material nickel hydroxide and graphene oxide (graphene) is 0.5:1 (nickel hydroxide and graphene point
It is not 50 mass parts and 100 mass parts, the mass parts of water 210).
Three-dimensional nickel hydroxide-graphene composite material is made into working electrode according to method same as Example 1 to go forward side by side
The corresponding electric performance test of row, it is as a result as follows：In 1C discharge and recharges, stable specific capacity is 180mAh/g；Filled under above-mentioned multiplying power
During electric discharge, capacity can keep more than the 60% of initial capacity after 500 repeated charges.
Embodiment 4
This example provides a kind of three-dimensional nickel hydroxide-graphene composite material, and its preparation method is different substantially with embodiment 1
, its raw material nickel hydroxide replaces with nickel nitrate.
Three-dimensional nickel hydroxide-graphene composite material is made into working electrode according to method same as Example 1 to go forward side by side
The corresponding electric performance test of row, it is as a result as follows：In 1C discharge and recharges, stable specific capacity is 220mAh/g；Filled under above-mentioned multiplying power
During electric discharge, capacity can keep more than the 80% of initial capacity after 500 repeated charges.
The cycle performance of battery of table 1
The present invention is easily poisoned existing deficiency low with utilization rate for nickel hydroxide positive plate, passes through preparation method and system
The control of standby condition, it is final obtain with it is resistance to poison, the zinc-nickel cell positive electrode of high usage and good circulation performance.This
Had very important significance to promoting the development of high power zinc-nickel cell and solving energy shortage etc..
Example above is only that the embodiment of the present invention is described, and not the scope of the present invention is carried out
Limit, those skilled in the art can also do numerous modifications and variations, not depart from design of the present invention on the basis of existing technology
On the premise of spirit, all variations and modifications that this area ordinary skill technical staff makes to technical scheme,
It should fall into the protection domain of claims of the present invention determination.
Claims (8)
1. a kind of three-dimensional nickel hydroxide-graphene composite material, it is characterised in that by the conductive network with three-dimensional structure and bear
Carry the nickel hydroxide composition above it；The three-dimensional conductive network of composite is made up of stannic oxide/graphene nano piece, has macropore,
Micropore and mesoporous pore structure；The size for the nickel hydroxide being supported on three-dimensional conductive network is 50 nanometers~500 microns,
The quality accounting of nickel hydroxide is 50~95% in composite.
2. the preparation method of three-dimensional nickel hydroxide-graphene composite material described in claim 1, it is characterised in that including step：
(1) nickel based compound is dispersed in water and/or organic solvent with graphene oxide, and hydro-thermal is then carried out in water heating kettle
Reaction and/or solvent thermal reaction, temperature are 100 DEG C~300 DEG C, the wherein mass ratio that feeds intake of nickel based compound and graphene oxide
For 0.5~30:1；
(2) using the product selected from any of vacuum drying, freeze-drying and supercritical drying seasoning to preceding step
It is dried, obtains solid product, as described three-dimensional nickel hydroxide-graphene composite material.
3. preparation method according to claim 2, it is characterised in that the nickel based compound be nickel hydroxide, nickel chloride,
One or more in nickel nitrate, nickel sulfate, nickel acetate；Described nickel based compound and the mass ratio that feeds intake of graphene oxide are
1~10:1.
4. preparation method according to claim 2, it is characterised in that described organic solvent is ethanol, propyl alcohol, second two
One or more combinations in alcohol, isopropanol, methyl pyrrolidone.
5. preparation method according to claim 2, it is characterised in that nickel based compound and graphene oxide in step (1)
It is dispersed in water, the mass ratio of nickel based compound and water is 5：10~30.
6. preparation method according to claim 2, it is characterised in that step (1) uses hydro-thermal reaction, and reaction temperature is
170~190 DEG C, the reaction time is 10~15h.
7. three-dimensional nickel hydroxide-graphene composite material described in claim 1, or any described preparation of claim 2~6
Application of the method in nickel radical battery.
A kind of 8. nickel radical battery, it is characterised in that the nickel radical battery just extremely following methods are made：By claim 1 institute
Three-dimensional nickel hydroxide-graphene composite material for stating, binder 60%PTFE, acetylene black, by 80：10：10 mass ratio mixes
Close uniformly, be uniformly applied to after being modulated into paste with water in nickel foam；
Dried 10~15 hours at 80 DEG C in vacuum drying oven.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109686580A (en) * | 2019-01-07 | 2019-04-26 | 湖北文理学院 | A kind of ultra-thin Ni of 3D structure (OH)2Nanometer sheet/Ni nanoparticle@rGO combination electrode material preparation method and application |
| CN109950500A (en) * | 2019-03-29 | 2019-06-28 | 北京航空航天大学 | A kind of manganese dioxide positive pole material for Zinc ion battery can be filled and preparation method thereof and battery |
| CN110212168A (en) * | 2019-04-12 | 2019-09-06 | 泉州劲鑫电子有限公司 | A kind of preparation method of the nanocomposite of simple hydrothermal synthesis beta phase nickel hydroxide/graphene |
| CN111790387A (en) * | 2020-08-07 | 2020-10-20 | 福州大学 | Transition metal hydroxide-graphene composite material for efficient photocatalytic reduction of carbon dioxide and preparation method and application thereof |
| CN114823158A (en) * | 2022-05-19 | 2022-07-29 | 一汽解放汽车有限公司 | Zinc ion capacitor, preparation method thereof and storage battery |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109686580A (en) * | 2019-01-07 | 2019-04-26 | 湖北文理学院 | A kind of ultra-thin Ni of 3D structure (OH)2Nanometer sheet/Ni nanoparticle@rGO combination electrode material preparation method and application |
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| CN110212168A (en) * | 2019-04-12 | 2019-09-06 | 泉州劲鑫电子有限公司 | A kind of preparation method of the nanocomposite of simple hydrothermal synthesis beta phase nickel hydroxide/graphene |
| CN111790387A (en) * | 2020-08-07 | 2020-10-20 | 福州大学 | Transition metal hydroxide-graphene composite material for efficient photocatalytic reduction of carbon dioxide and preparation method and application thereof |
| CN111790387B (en) * | 2020-08-07 | 2021-11-26 | 福州大学 | Transition metal hydroxide-graphene composite material for efficient photocatalytic reduction of carbon dioxide and preparation method and application thereof |
| CN114823158A (en) * | 2022-05-19 | 2022-07-29 | 一汽解放汽车有限公司 | Zinc ion capacitor, preparation method thereof and storage battery |
| CN114823158B (en) * | 2022-05-19 | 2023-07-25 | 一汽解放汽车有限公司 | Zinc ion capacitor and preparation method thereof and storage battery |
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