CN109935799A - A kind of preparation method of alkaline secondary cell multi-layer alpha-nickel hydroxide composite material - Google Patents
A kind of preparation method of alkaline secondary cell multi-layer alpha-nickel hydroxide composite material Download PDFInfo
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- CN109935799A CN109935799A CN201711378883.XA CN201711378883A CN109935799A CN 109935799 A CN109935799 A CN 109935799A CN 201711378883 A CN201711378883 A CN 201711378883A CN 109935799 A CN109935799 A CN 109935799A
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Abstract
The invention discloses a kind of alkaline secondary cell preparation methods of multi-layer alpha-nickel hydroxide composite material, comprising steps of (1) is using nickel sulfate, manganese chloride and ytterbium nitrate as raw material, urea is precipitating reagent, using the mixed liquor of distilled water and ethyl alcohol as solvent, mixed solution is subjected to microwave heating treatment, separation, it is dry, obtain manganese, ytterbium doped multi-layer grade alpha-nickel hydroxide precursor；(2) alpha-nickel hydroxide precursor is mixed with cobalt sulfate solution, potassium hydroxide solution is added dropwise, obtain cobalt hydroxide cladding alpha-nickel hydroxide；(3) it is electrolysed covering hydroxyl cobalt oxide layer.Alkaline secondary cell prepared by the present invention multi-layer alpha-nickel hydroxide composite material also improves the electric conductivity and cyclical stability of ball-shape nickel hydroxide while increasing material energy densities；It is when being used 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 multi-layer α-
The preparation method of nickel hydroxide composite material.
Background technique
With the aggravation of energy crisis and environmental pollution, the development of electric car is increasingly valued by people.Alkalinity
Secondary cell compares other batteries with the excellent comprehensive performance such as its high-energy-density, high-specific-power, long-life, safety be good
Best power source power supply as electric car (EV) and hybrid vehicle (HEV).
Ni(OH)2It is a kind of important alkaline storage battery (Ni/Cd, Ni/H2, Ni/Zn, Ni/MH, Ni/Fe) positive-active
Material plays a crucial role to the capacity of battery, service life and chemical property.There are two types of crystal structures for nickel hydroxide: α-Ni (OH)2
With β-Ni (OH)2, corresponding Charging state is respectively γ-NiOOH and β-NiOOH.Currently, the anode of nickel-metal hydride battery all uses β-Ni
(OH)2/ β-NiOOH electricity is to circulation, and nickle atom electron transfer number theoretical in electrochemical reaction process is 1, theoretical specific capacity
For 289mAhg-1.Due to β-Ni (OH)2Theoretical specific capacity it is low, and the β-NiOOH generated in overcharge will cause electricity
Pole volume expansion has seriously affected the performance of electrode.α-Ni(OH)2Since its average oxidation valence state with higher is (close
3.67) it can be well solved, thus theoretical specific capacity with higher (482mAhg-1), and again β-Ni (OH)2It is overcharging
The electrode volume expansion issues that are generated when electric and receive significant attention.
Although many researchers recent years attempt to overcome above-mentioned disadvantage by preparing alpha-nickel hydroxide, also
There are following deficiencies: first, prepared class alpha-phase nickel hydroxide density is smaller, thus influence battery volume discharge specific energy and
Electric discharge specific power, it is difficult to the requirement for reaching high specific energy required by power battery, measuring high-specific-power；Second, incorporation it is nonactive
Impurity not only reduces the actual capacity of active material, and can directly reduce electrode discharge specific capacity, to influence battery
Charge-discharge performance.
Summary of the invention
To overcome above-mentioned deficiency, the present invention provides a kind of alkaline secondary cell multi-layer alpha-nickel hydroxide composite material
Preparation method, the nickel hydroxide composite material prepared using this method, specific capacity with higher and good stable circulation
Property.
To achieve the above object, the invention adopts the following technical scheme:
The first aspect of the invention is to provide a kind of alkaline secondary cell multi-layer alpha-nickel hydroxide composite material
Preparation method specifically comprises the following steps:
(1) manganese, ytterbium doped multi-layer grade alpha-nickel hydroxide precursor are prepared
Using nickel sulfate, manganese chloride and ytterbium nitrate as raw material, urea is precipitating reagent, is molten with the mixed liquor of distilled water and ethyl alcohol
Agent, magnetic agitation obtains mixed solution at room temperature, and wherein the concentration of nickel ion is 2-3mol/L, the concentration of manganese ion is
0.15-0.25mol/L, ytterbium ion concentration be 0.02-0.03mol/L, mixed solution is transferred in microwave reaction bottle
Carry out microwave heating treatment at 150-200 DEG C, the microwave combustion method time is 30-50 minutes, to the liquid-phase system after heat treatment into
The centrifuge separation of row product, is washed and is dried to the product separated, obtain manganese, ytterbium doped multi-layer grade α-hydroxide
Nickel precursor；
(2) cobalt hydroxide is coated
Above-mentioned alpha-nickel hydroxide precursor and cobalt ions mole are equivalent to the nickel ion mole 2- of alpha-nickel hydroxide
3% cobalt sulfate solution mixing, ultrasonic wave disperse 30-40 minute, under conditions of stirring and ultrasonic wave act on, 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, which is maintained between 9-11, is reacted, and stops stirring after reaction, and filtering obtains the α-hydrogen-oxygen for being coated with cobalt hydroxide
Change nickel precipitating, the 3-5 pH value to eluate is washed with water as neutrality, filtering is dried under the conditions of 70-90 DEG C of temperature to perseverance
Weight obtains cobalt hydroxide cladding alpha-nickel hydroxide；
(3) it is electrolysed covering hydroxyl cobalt oxide layer
Electrolytic cell is separated into anode chamber and cathode chamber with the diaphragm of alkaline battery, by ti-supported lead dioxide electric anode and
Cathode made of stainless steel is respectively put into the anode chamber and cathode chamber equipped with sodium chloride alkaline electrolyte, and cobalt hydroxide is coated
Alpha-nickel hydroxide is added in anode chamber, and being adjusted to pH value with KOH is 10-12, is electrolysed life in the case where 5-10 lies prostrate constant pressure, room temperature and stirring
At the alpha-nickel hydroxide of hydroxyl cobalt oxide layer, it is filtered, washed, dries, finished product.
Further, in the preparation method in the alkaline secondary cell with multi-layer alpha-nickel hydroxide composite material,
The volume ratio of distilled water described in step (1) and ethyl alcohol is 1-2:1.
Further, in the preparation method in the alkaline secondary cell with multi-layer alpha-nickel hydroxide composite material,
Drying temperature described in step (1) is 90-100 DEG C.
Further, in the preparation method in the alkaline secondary cell with multi-layer alpha-nickel hydroxide composite material,
The temperature of reaction described in step (2) is 40-45 DEG C, and the reaction time is 30-40 minutes.
The second aspect of the invention is to provide a kind of alkaline secondary cell multi-layer of method preparation as described above
Alpha-nickel hydroxide composite material.
The present invention by adopting the above technical scheme, compared with prior art, has the following technical effect that
Alkaline secondary cell prepared by the present invention multi-layer alpha-nickel hydroxide composite material, use Rare earth element ytterbium and
Metallic element manganese carries out wet process doping vario-property to alpha-nickel hydroxide, and is formed in being coated and being electrolysed by wet process for alpha-nickel hydroxide
Therefore uniform hydroxy cobalt oxide clad while increasing material energy densities, also improves leading for ball-shape nickel hydroxide
Electrical property and cyclical stability, therefore the material is when being used for alkaline secondary cell so that battery have high specific capacity and compared with
Long 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 embodiment 1 alkaline secondary cell multi-layer alpha-nickel hydroxide composite material
(1) manganese, ytterbium doped multi-layer grade alpha-nickel hydroxide precursor are prepared
Using nickel sulfate, manganese chloride and ytterbium nitrate as raw material, urea is precipitating reagent, with the distilled water and ethyl alcohol of volume ratio 1:1
Mixed liquor be solvent, magnetic agitation obtains mixed solution at room temperature, and wherein the concentration of nickel ion is 2mol/L, manganese ion
Concentration be 0.15mol/L, the concentration of ytterbium ion is 0.02mol/L, and mixed solution is transferred in microwave reaction bottle at 150 DEG C
Lower carry out microwave heating treatment, microwave combustion method time are 50 minutes, carry out product centrifugation point to the liquid-phase system after heat treatment
From, the product separated is washed and is dried, drying temperature be 90 DEG C, obtain manganese, ytterbium doped multi-layer grade α-hydrogen
Nickel oxide precursor.
(2) cobalt hydroxide is coated
Above-mentioned alpha-nickel hydroxide precursor and cobalt ions mole are equivalent to the nickel ion mole 2% of alpha-nickel hydroxide
Cobalt sulfate solution mixing, ultrasonic wave disperse 30 minutes, stirring and ultrasonic wave effect under conditions of, to it is scattered contain α-hydrogen
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, control reaction temperature is 40 DEG C, the reaction time 40 minutes, stops stirring after reaction, filtering is wrapped
It is covered with the alpha-nickel hydroxide precipitating of cobalt hydroxide, 3 pH value to eluate are washed with water as neutrality, filter, in 70 DEG C of temperature
Under the conditions of dry to constant weight, obtain cobalt hydroxide cladding alpha-nickel hydroxide.
(3) it is electrolysed covering hydroxyl cobalt oxide layer
Electrolytic cell is separated into anode chamber and cathode chamber with the diaphragm of alkaline battery, by ti-supported lead dioxide electric anode and
Cathode made of stainless steel is respectively put into the anode chamber and cathode chamber equipped with sodium chloride alkaline electrolyte, and cobalt hydroxide is coated
Alpha-nickel hydroxide is added in anode chamber, and being adjusted to pH value with KOH is 10-12, electrolytically generated under 5 volts of constant pressures, room temperature and stirring
The alpha-nickel hydroxide of hydroxyl cobalt oxide layer is filtered, washed, dries, finished product.
The preparation of embodiment 2 alkaline secondary cell multi-layer alpha-nickel hydroxide composite material
(1) manganese, ytterbium doped multi-layer grade alpha-nickel hydroxide precursor are prepared
Using nickel sulfate, manganese chloride and ytterbium nitrate as raw material, urea is precipitating reagent, with the distilled water and ethyl alcohol of volume ratio 2:1
Mixed liquor be solvent, magnetic agitation obtains mixed solution at room temperature, and wherein the concentration of nickel ion is 3mol/L, manganese ion
Concentration be 0.25mol/L, the concentration of ytterbium ion is 0.03mol/L, and mixed solution is transferred in microwave reaction bottle at 200 DEG C
Lower carry out microwave heating treatment, microwave combustion method time are 30 minutes, carry out product centrifugation point to the liquid-phase system after heat treatment
From, the product separated is washed and is dried, drying temperature be 100 DEG C, obtain manganese, ytterbium doped multi-layer grade α-hydrogen
Nickel oxide precursor.
(2) cobalt hydroxide is coated
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 disperse 40 minutes, stirring and ultrasonic wave effect under conditions of, to it is scattered contain α-hydrogen
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, control reaction temperature is 45 DEG C, the reaction time 30 minutes, stops stirring after reaction, filtering is wrapped
It is covered with the alpha-nickel hydroxide precipitating of cobalt hydroxide, 5 pH value to eluate are washed with water as neutrality, filter, in 90 DEG C of temperature
Under the conditions of dry to constant weight, obtain cobalt hydroxide cladding alpha-nickel hydroxide.
(3) it is electrolysed covering hydroxyl cobalt oxide layer
Electrolytic cell is separated into anode chamber and cathode chamber with the diaphragm of alkaline battery, by ti-supported lead dioxide electric anode and
Cathode made of stainless steel is respectively put into the anode chamber and cathode chamber equipped with sodium chloride alkaline electrolyte, and cobalt hydroxide is coated
Alpha-nickel hydroxide is added in anode chamber, and being adjusted to pH value with KOH is 10-12, electrolytically generated under 10 volts of constant pressures, room temperature and stirring
The alpha-nickel hydroxide of hydroxyl cobalt oxide layer is filtered, washed, dries, finished product.
Comparative example
It prepares six water nickel chloride of 0.001mol and 0.12mol ethylene glycol is packed into the polytetrafluoroethyllining lining of volume 40mL not
It becomes rusty in steel reaction kettle, 0.45g sodium acetate is added, stirred with glass bar to being completely dissolved, form light green transparent mixed solution.It will
Reaction kettle closing is tightened, and is put into baking oven, and temperature is set in 190 DEG C, reaction kettle is taken out after reacting 3h, makes its natural cooling.
Then reaction precipitate is poured out, first three times, then with dehydrated alcohol is washed three times with distillation washing.Finally 60 DEG C in vacuum drying oven
Lower dry 8h collects sample and is stored in drier.
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
It is dried in vacuo 3 hours at DEG C.Pole piece after drying is tabletted at 5MPa, and anode is made.By anode obtained and mistake
The hydrogen-bearing alloy electrode of amount is assembled into ni-mh simulated battery, and electrolyte is 7mol/LKOH+15g/LLiOH solution.In test temperature
It is to carry out electric performance test at 25 DEG C, the material of the embodiment one and two is compared with the product of comparative example after tested, specific capacity
25-35% is improved, service life improves 1.5 times or more.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (5)
1. a kind of alkaline secondary cell preparation method of multi-layer alpha-nickel hydroxide composite material, which is characterized in that including such as
Lower step:
(1) manganese, ytterbium doped multi-layer grade alpha-nickel hydroxide precursor are prepared
Using nickel sulfate, manganese chloride and ytterbium nitrate as raw material, urea is precipitating reagent, using the mixed liquor of distilled water and ethyl alcohol as solvent,
Magnetic agitation obtains mixed solution at room temperature, and wherein the concentration of nickel ion is 2-3mol/L, the concentration of manganese ion is 0.15-
0.25mol/L, ytterbium ion concentration be 0.02-0.03mol/L, mixed solution is transferred in microwave reaction bottle in 150-200
Carry out microwave heating treatment at DEG C, the microwave combustion method time is 30-50 minute, to the liquid-phase system progress product after heat treatment from
Heart separation, is washed and is dried to the product separated, obtain body before manganese, ytterbium doped multi-layer grade alpha-nickel hydroxide
Body；
(2) cobalt hydroxide is coated
Above-mentioned alpha-nickel hydroxide precursor and cobalt ions mole are equivalent to the nickel ion mole 2-3%'s of alpha-nickel hydroxide
Cobalt sulfate solution mixing, ultrasonic wave disperse 30-40 minutes, under conditions of stirring and ultrasonic wave effect, contain α-to scattered
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 the alpha-nickel hydroxide for being coated with cobalt hydroxide
The 3-5 pH value to eluate is washed with water as neutrality in precipitating, and filtering is dried to constant weight under the conditions of 70-90 DEG C of temperature, obtained
Alpha-nickel hydroxide is coated to cobalt hydroxide；
(3) it is electrolysed covering hydroxyl cobalt oxide layer
Electrolytic cell is separated into anode chamber and cathode chamber with the diaphragm of alkaline battery, by the anode of ti-supported lead dioxide electric and stainless
Cathode made of steel is respectively put into the anode chamber and cathode chamber equipped with sodium chloride alkaline electrolyte, by cobalt hydroxide coating alpha-hydrogen
Nickel oxide is added in anode chamber, and being adjusted to pH value with KOH is 10-12, the electrolytically generated hydroxyl in the case where 5-10 lies prostrate constant pressure, room temperature and stirs
The alpha-nickel hydroxide of base cobalt oxide layer is filtered, washed, dries, finished product.
2. the alkaline secondary cell according to claim 1 preparation method of multi-layer alpha-nickel hydroxide composite material,
It is characterized in that, the volume ratio of distilled water described in step (1) and ethyl alcohol is 1-2:1.
3. the alkaline secondary cell according to claim 1 preparation method of multi-layer alpha-nickel hydroxide composite material,
It is characterized in that, drying temperature described in step (1) is 90-100 DEG C.
4. the alkaline secondary cell according to claim 1 preparation method of multi-layer alpha-nickel hydroxide composite material,
It is characterized in that, the temperature of reaction described in step (2) is 40-45 DEG C, and the reaction time is 30-40 minutes.
5. a kind of alkaline secondary cell such as any one of claim 1-4 the method preparation is compound with multi-layer alpha-nickel hydroxide
Material.
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Citations (7)
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|---|---|---|---|---|
| JP2000133259A (en) * | 1998-10-29 | 2000-05-12 | Sanyo Electric Co Ltd | Sealed alkaline storage battery |
| US6066416A (en) * | 1995-11-22 | 2000-05-23 | Matsushita Electric Industrial Co., Ltd. | Nickel hydroxide positive electrode active material having a surface layer containing a solid solution nickel hydroxide with manganese incorporated therein |
| US6190801B1 (en) * | 1998-03-24 | 2001-02-20 | Sanyo Electric Co., Ltd. | Sealed alkaline-zinc storage battery |
| US6479189B1 (en) * | 1999-08-02 | 2002-11-12 | Sanyo Electric Co., Ltd. | Sealed alkaline storage battery with a manganese containing NiOH electrode |
| CN101117725A (en) * | 2007-06-28 | 2008-02-06 | 河南师范大学 | Method for electrolyzing nickel hydroxide covering hydroxyl cobalt oxide layer |
| CN101618895A (en) * | 2008-07-04 | 2010-01-06 | 中国科学院福建物质结构研究所 | Multi-level structure alpha type nickel hydroxide prepared by microwave auxiliary and 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 CN201711378883.XA patent/CN109935799A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6066416A (en) * | 1995-11-22 | 2000-05-23 | Matsushita Electric Industrial Co., Ltd. | Nickel hydroxide positive electrode active material having a surface layer containing a solid solution nickel hydroxide with manganese incorporated therein |
| US6190801B1 (en) * | 1998-03-24 | 2001-02-20 | Sanyo Electric Co., Ltd. | Sealed alkaline-zinc storage battery |
| JP2000133259A (en) * | 1998-10-29 | 2000-05-12 | Sanyo Electric Co Ltd | Sealed alkaline storage battery |
| US6479189B1 (en) * | 1999-08-02 | 2002-11-12 | Sanyo Electric Co., Ltd. | Sealed alkaline storage battery with a manganese containing NiOH electrode |
| CN101117725A (en) * | 2007-06-28 | 2008-02-06 | 河南师范大学 | Method for electrolyzing nickel hydroxide covering hydroxyl cobalt oxide layer |
| CN101618895A (en) * | 2008-07-04 | 2010-01-06 | 中国科学院福建物质结构研究所 | Multi-level structure alpha type nickel hydroxide prepared by microwave auxiliary and 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 |
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