CN108075126A - A kind of preparation method of alkaline secondary cell cobalt cladding alpha-nickel hydroxide composite material - Google Patents
A kind of preparation method of alkaline secondary cell cobalt cladding alpha-nickel hydroxide composite material Download PDFInfo
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- CN108075126A CN108075126A CN201711378900.XA CN201711378900A CN108075126A CN 108075126 A CN108075126 A CN 108075126A CN 201711378900 A CN201711378900 A CN 201711378900A CN 108075126 A CN108075126 A CN 108075126A
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- nickel hydroxide
- alpha
- cobalt
- nickel
- secondary cell
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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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
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of alkaline secondary cell preparation method of cobalt coating alpha nickel hydroxide composite material, including step：(1) nickel chloride, ferrous nitrate and yttrium nitrate are dissolved in ethylene glycol, add in deionized water, then weak aqua ammonia is added to agent in above-mentioned mixed solution and is reacted, washed, dry to get to iron, doped yttrium α nickel hydroxide precursors；(2) α nickel hydroxide precursors with cobalt sulfate solution are mixed, be uniformly dispersed, potassium hydroxide solution is added dropwise, washed, filtered, it is dry, obtain the cobalt coating alpha nickel hydroxide of iron, doped yttrium.Alkaline secondary cell prepared by the present invention α nickel hydroxide composite materials while material energy densities are increased, also improve the electric conductivity and cyclical stability of ball-shape nickel hydroxide；It is when for alkaline secondary cell so that battery has high specific capacity and longer service life.
Description
Technical field
The present invention relates to alkaline secondary cell manufacturing technology field more particularly to a kind of alkaline secondary cell with cobalt coating alpha-
The preparation method of nickel hydroxide composite material.
Background technology
With energy crisis and the aggravation of environmental pollution, the development of electric vehicle is increasingly valued by people.Metal
Hydride nickel-hydrogen secondary cell (Ni/MH) is good etc. excellent comprehensive with its high-energy-density, high-specific-power, long-life, security
Can, compared to the best power source power supply that other accumulators become electric vehicle (EV) and hybrid vehicle (HEV).Ni-H cell
In, the performance of positive active material is the key that battery whole synthesis performance improves, especially as electrical vehicular power accumulator,
The high rate during charging-discharging of nickel electrode also needs to further improve.
Ni(OH)2The alkaline electros such as Ni/Cd, Ni/Zn, Ni/Fe, Ni/MH are widely used in as a positive electrode active material
Chi Zhong.There are two kinds of crystal structures, α-Ni (OH) for it2With β-Ni (OH)2.Current battery industrially mainly applies β-Ni (OH)2Make
For positive electrode, but pure β-Ni (OH)2Chemical property comes with some shortcomings.
In recent years, research finds α-Ni (OH)2In some aspects compared with β-Ni (OH)2Have the advantages that it is more, such as α-Ni
(OH)2Electrode expansion will not occur for the charge and discharge cycles of/γ-NiOOH electricity pair, not have interphase generation in electric order reaction, reversible
Property is good；α-Ni(OH)2/ γ-NiOOH electricity is 1.67 to theoretical electron transfer number in reaction, and Theoretical Mass specific capacity is than β-Ni
(OH)2It is high.From the point of view of chemically reacting, the generation of nickel hydroxide is very simple, in alkaline conditions, nickel ion and hydroxide ion knot
Symphysis is into nickel hydroxide precipitate.However, the nickel hydroxide so generated either in electro-chemical activity still in appearance structure
It is all difficult to reach requirement of the alkaline storage battery to positive electrode.
Therefore, in order to meet the requirement of high-capacity battery, high activity is prepared, highdensity nickel hydroxide anode material becomes
Current main direction of studying.
The content of the invention
To solve the above problem of the prior art, the present invention provides a kind of alkaline secondary cell cobalt coating alpha-hydroxide
The preparation method of nickel composite material, using this method prepare nickel hydroxide composite material, have good electric conductivity and
Cyclical stability.
To achieve the above object, the present invention uses following technical scheme：
The first aspect of the invention is to provide a kind of alkaline secondary cell cobalt cladding alpha-nickel hydroxide composite material
Preparation method specifically comprises the following steps：
(1) iron, doped yttrium alpha-nickel hydroxide precursor are prepared
Nickel chloride, ferrous nitrate and yttrium nitrate are dissolved in ethylene glycol in the reactor with agitating device, room temperature
Lower stirring 30-40 minutes adds in deionized water according still further to deionized water and the volume ratio of ethylene glycol for 1-2: 1, continues to stir 20-
30 minutes, form mixed solution；Weak aqua ammonia is added to above-mentioned mixed solution with the rate of addition of 20-40mL/min simultaneously in stirring
In, until pH value of solution=8-10；At a temperature of 40-50 DEG C, when keeping 3-4 small；It treats to be cooled to room temperature after reaction, after filtering
Obtained precipitation is washed with deionized water to pH=7-8, when dry 8-10 is small at 90-100 DEG C to get to iron, doped yttrium α-
Nickel hydroxide precursor；
(2) cobalt coats
Above-mentioned alpha-nickel hydroxide precursor and cobalt ions mole are equivalent to the nickel ion mole 3- of alpha-nickel hydroxide
5% cobalt sulfate solution mixing, ultrasonic wave disperses 30-40 minute, stir under conditions of ul-trasonic irradiation, to scattered
Potassium hydroxide solution is added dropwise in cobalt salt solution containing alpha-nickel hydroxide, controls the addition speed of precipitating reagent so that reaction system
PH value is reacted between being maintained at 9-11, stops stirring after reaction, is filtered, and obtains being coated with α-hydrogen-oxygen of cobalt hydroxide
Change nickel precipitation, the cobalt clad nanometer alpha-nickel hydroxide precipitated, the 3-5 pH value to eluate is washed with water as neutrality,
The cobalt cladding alpha-nickel hydroxide for constant weight, obtaining iron, doped yttrium is dried in filtering under 70-90 DEG C of temperature conditionss.
Further, in the alkaline secondary cell coats the preparation method of alpha-nickel hydroxide composite material with cobalt,
Nickel ion molar concentration is 1-2mol/L in the mixed solution in step (1), ferrous ion molar concentration is 0.1-
0.3mol/L, ruthenium ion molar concentration are 0.03-0.05mol/L.
Further, in the alkaline secondary cell coats the preparation method of alpha-nickel hydroxide composite material with cobalt,
Weak aqua ammonia concentration described in step (1) is 10%.
Further, in the alkaline secondary cell coats the preparation method of alpha-nickel hydroxide composite material with cobalt,
The temperature reacted described in step (2) is 40-45 DEG C, and the reaction time is 30-40 minutes.
The second aspect of the invention be to provide alkaline secondary cell prepared by a kind of method described above with cobalt coating alpha-
Nickel hydroxide composite material.
The present invention compared with prior art, is had the following technical effect that using above-mentioned technical proposal：
Alkaline secondary cell prepared by present invention alpha-nickel hydroxide composite material employs rare earth element yttrium and metal member
Plain sheet carries out wet method doping vario-property to alpha-nickel hydroxide, and uniform cobalt oxide clad is formed on the surface of alpha-nickel hydroxide,
Therefore, while material energy densities are increased, the electric conductivity and cyclical stability of ball-shape nickel hydroxide are also improved, therefore should
Material is when for alkaline secondary cell so that battery has high specific capacity and longer service life.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
The preparation of 1 alkaline secondary cell of embodiment cobalt cladding alpha-nickel hydroxide composite material
(1) iron, doped yttrium alpha-nickel hydroxide precursor are prepared
Nickel chloride, ferrous nitrate and yttrium nitrate are dissolved in ethylene glycol in the reactor with agitating device, room temperature
Lower stirring 30 minutes adds in deionized water for 1: 1 according still further to deionized water and the volume ratio of ethylene glycol, continues stirring 20 minutes,
Formed mixed solution, wherein nickel ion molar concentration be 1mol/L, ferrous ion molar concentration be 0.1mol/L, ruthenium ion mole
Concentration is 0.03mol/L；Weak aqua ammonia is added to the rate of addition of 20mL/min in above-mentioned mixed solution simultaneously in stirring, until molten
Liquid pH=8；At a temperature of 40 DEG C, when holding 3 is small；It treats to be cooled to room temperature after reaction, uses obtained precipitation after filtering
Deionized water is washed till pH=7-8, at 90 DEG C it is dry 10 it is small when to get to iron, doped yttrium alpha-nickel hydroxide precursor.
(2) cobalt coats
Above-mentioned alpha-nickel hydroxide precursor and cobalt ions mole are equivalent to the nickel ion mole 3% of alpha-nickel hydroxide
Cobalt sulfate solution mixing, ultrasonic wave disperses 30 minutes, stir and ul-trasonic irradiation under conditions of, contain α-hydrogen to scattered
Potassium hydroxide solution is added dropwise in the cobalt salt solution of nickel oxide, controls the addition speed of precipitating reagent so that the pH value of reaction system is protected
It holds between 9-11, controlling reaction temperature is 40 DEG C, 40 minutes reaction time, stops stirring after reaction, and filtering is wrapped
The alpha-nickel hydroxide precipitation of cobalt hydroxide is covered with, the cobalt clad nanometer alpha-nickel hydroxide is precipitated, is washed with water 3 times to washing
Go out the pH value of liquid for neutrality, filtering is dried to constant weight under 70 DEG C of temperature conditionss, obtains cobalt coating alpha-hydrogen-oxygen of iron, doped yttrium
Change nickel.
The preparation of 2 alkaline secondary cell of embodiment cobalt cladding alpha-nickel hydroxide composite material
(1) iron, doped yttrium alpha-nickel hydroxide precursor are prepared
Nickel chloride, ferrous nitrate and yttrium nitrate are dissolved in ethylene glycol in the reactor with agitating device, room temperature
Lower stirring 40 minutes adds in deionized water for 2: 1 according still further to deionized water and the volume ratio of ethylene glycol, continues stirring 30 minutes,
Formed mixed solution, wherein nickel ion molar concentration be 2mol/L, ferrous ion molar concentration be 0.3mol/L, ruthenium ion mole
Concentration is 0.05mol/L；Weak aqua ammonia is added to the rate of addition of 40mL/min in above-mentioned mixed solution simultaneously in stirring, until molten
Liquid pH=8-10；At a temperature of 50 DEG C, when holding 3 is small；It treats to be cooled to room temperature after reaction, the precipitation that will be obtained after filtering
Be washed with deionized water to pH=7-8, at 100 DEG C it is dry 8 it is small when to get to iron, doped yttrium alpha-nickel hydroxide precursor.
(2) cobalt coats
Above-mentioned alpha-nickel hydroxide precursor and cobalt ions mole are equivalent to the nickel ion mole 5% of alpha-nickel hydroxide
Cobalt sulfate solution mixing, ultrasonic wave disperses 40 minutes, stir and ul-trasonic irradiation under conditions of, contain α-hydrogen to scattered
Potassium hydroxide solution is added dropwise in the cobalt salt solution of nickel oxide, controls the addition speed of precipitating reagent so that the pH value of reaction system is protected
It holds between 9-11, controlling reaction temperature is 45 DEG C, 30 minutes reaction time, stops stirring after reaction, and filtering is wrapped
The alpha-nickel hydroxide precipitation of cobalt hydroxide is covered with, the cobalt clad nanometer alpha-nickel hydroxide is precipitated, is washed with water 5 times to washing
Go out the pH value of liquid for neutrality, filtering is dried to constant weight under 90 DEG C of temperature conditionss, obtains cobalt coating alpha-hydrogen-oxygen of iron, doped yttrium
Change nickel.
Comparative example
The methenamine of the Nickel dichloride hexahydrate of 0.238g and 0.280g are added in 5mL deionized waters and stirred, is dissolved, so
The ethyl alcohol of 25mL is added in backward mixed liquor；It is 40mL by deionized water to volume is added in obtained solution, is transferred to 50mL
Inner liner polytetrafluoroethylene autoclave in, after reacting 2h at 160 DEG C, cool down, filtering then spends ionic hydration respectively
Absolute ethyl alcohol washing filters out product for several times, and is placed in 60 DEG C of vacuum drying chamber dry, obtained flower-shaped α-Ni (OH) 2.
Above-described embodiment one, two and comparative example products therefrom are separately added into same amount of sodium carboxymethylcellulose
(CMC) and polytetrafluoroethylene (PTFE) (PTFE) paste, is stirred to obtain, wherein, the quality of sodium carboxymethylcellulose is the 1% of mixture,
The quality of polytetrafluoroethylene (PTFE) is the 3% of mixture.Then by paste full-filling on the nickel foam substrate of 1cm × 1cm, and 60
When vacuum drying 3 is small at DEG C.Dried pole piece is tabletted under 5MPa, and anode is made.By anode obtained and mistake
For the Cd electrode assemblings of amount into cadmium nickel simulated battery, electrolyte is 7mol/L KOH+15g/L LiOH solution.It is 25 in test temperature
Electric performance test is carried out at DEG C, compared with the product of comparative example, specific capacity improves the material of the embodiment one and two after tested
47-56%, service life improve 2 times or more.
Specific embodiments of the present invention are described in detail above, but it is intended only as example, it is of the invention and unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
It substitutes also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, all should be contained within the scope of the invention.
Claims (5)
1. a kind of alkaline secondary cell preparation method of cobalt cladding alpha-nickel hydroxide composite material, which is characterized in that including such as
Lower step：
(1) iron, doped yttrium alpha-nickel hydroxide precursor are prepared
Nickel chloride, ferrous nitrate and yttrium nitrate are dissolved in ethylene glycol in the reactor with agitating device, stirred at room temperature
It mixes 30-40 minutes, deionized water is added in for 1-2: 1 according still further to deionized water and the volume ratio of ethylene glycol, continue to stir 20-30 points
Clock forms mixed solution；Weak aqua ammonia is added to the rate of addition of 20-40mL/min in above-mentioned mixed solution simultaneously in stirring,
To pH value of solution=8-10；At a temperature of 40-50 DEG C, when keeping 3-4 small；It treats to be cooled to room temperature after reaction, it will after filtering
Obtained precipitation is washed with deionized water to pH=7-8, to get to iron, doped yttrium α-hydrogen when dry 8-10 is small at 90-100 DEG C
Nickel oxide precursor；
(2) cobalt coats
Above-mentioned alpha-nickel hydroxide precursor and cobalt ions mole are equivalent to the nickel ion mole 3-5%'s of alpha-nickel hydroxide
Cobalt sulfate solution mixes, and ultrasonic wave disperses 30-40 minute, stir and ul-trasonic irradiation under conditions of, to it is scattered contain α-
Potassium hydroxide solution is added dropwise in the cobalt salt solution of nickel hydroxide, controls the addition speed of precipitating reagent so that the pH value of reaction system
It is maintained between 9-11 and is reacted, stop stirring after reaction, filtering obtains being coated with the alpha-nickel hydroxide of cobalt hydroxide
Precipitation precipitates the cobalt clad nanometer alpha-nickel hydroxide, and the 3-5 pH value to eluate is washed with water as neutrality, filtering,
The cobalt cladding alpha-nickel hydroxide for constant weight, obtaining iron, doped yttrium is dried under 70-90 DEG C of temperature conditionss.
2. the alkaline secondary cell according to claim 1 preparation method of cobalt cladding alpha-nickel hydroxide composite material,
It is characterized in that, nickel ion molar concentration is 1-2mol/L in the mixed solution in step (1), ferrous ion molar concentration is
0.1-0.3mol/L, ruthenium ion molar concentration are 0.03-0.05mol/L.
3. the alkaline secondary cell according to claim 1 preparation method of cobalt cladding alpha-nickel hydroxide composite material,
It is characterized in that, weak aqua ammonia concentration described in step (1) is 10%.
4. the alkaline secondary cell according to claim 1 preparation method of cobalt cladding alpha-nickel hydroxide composite material,
It is characterized in that, the temperature reacted described in step (2) is 40-45 DEG C, and the reaction time is 30-40 minutes.
It is 5. a kind of as compound with cobalt cladding alpha-nickel hydroxide such as alkaline secondary cell prepared by any one of claim 1-4 the method
Material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111041214A (en) * | 2019-12-23 | 2020-04-21 | 先进储能材料国家工程研究中心有限责任公司 | Method for recycling and preparing α spherical nickel by utilizing waste zinc-containing nickel-hydrogen battery |
| CN111092196A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | Silicon oxide and nickel hydroxide composite material and synthesis method thereof |
| CN114314682A (en) * | 2021-12-13 | 2022-04-12 | 上海应用技术大学 | Preparation method of metal cobalt-coated cobalt aluminum hydroxide supercapacitor material |
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| JPH04237951A (en) * | 1991-01-18 | 1992-08-26 | Matsushita Electric Ind Co Ltd | Manufacture of nickel electrode for alkaline storage battery |
| CN101774653A (en) * | 2010-02-05 | 2010-07-14 | 北京化工大学 | Alpha-nickel hydroxide nano/micro structure material and preparation method thereof |
| CN101982402A (en) * | 2010-09-10 | 2011-03-02 | 广东工业大学 | Multi-element doped nano alpha-Ni(OH)2 material and preparation method thereof |
| CN102544477A (en) * | 2012-01-04 | 2012-07-04 | 广州市云通磁电有限公司 | Preparation method of cobalt-clad nanometer alpha-nickel hydroxide |
-
2017
- 2017-12-19 CN CN201711378900.XA patent/CN108075126A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04237951A (en) * | 1991-01-18 | 1992-08-26 | Matsushita Electric Ind Co Ltd | Manufacture of nickel electrode for alkaline storage battery |
| CN101774653A (en) * | 2010-02-05 | 2010-07-14 | 北京化工大学 | Alpha-nickel hydroxide nano/micro structure material and preparation method thereof |
| CN101982402A (en) * | 2010-09-10 | 2011-03-02 | 广东工业大学 | Multi-element doped nano alpha-Ni(OH)2 material and preparation method thereof |
| CN102544477A (en) * | 2012-01-04 | 2012-07-04 | 广州市云通磁电有限公司 | Preparation method of cobalt-clad nanometer alpha-nickel hydroxide |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111092196A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | Silicon oxide and nickel hydroxide composite material and synthesis method thereof |
| CN111041214A (en) * | 2019-12-23 | 2020-04-21 | 先进储能材料国家工程研究中心有限责任公司 | Method for recycling and preparing α spherical nickel by utilizing waste zinc-containing nickel-hydrogen battery |
| CN111041214B (en) * | 2019-12-23 | 2021-08-31 | 先进储能材料国家工程研究中心有限责任公司 | Method for preparing alpha spherical nickel by recycling waste zinc-containing nickel-hydrogen batteries |
| CN114314682A (en) * | 2021-12-13 | 2022-04-12 | 上海应用技术大学 | Preparation method of metal cobalt-coated cobalt aluminum hydroxide supercapacitor material |
| CN114314682B (en) * | 2021-12-13 | 2023-06-27 | 上海应用技术大学 | Preparation method of metallic cobalt coated cobalt aluminum hydroxide supercapacitor material |
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