CN106207115B - A kind of preparation method of nickel hydroxide electrode material - Google Patents
A kind of preparation method of nickel hydroxide electrode material Download PDFInfo
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- CN106207115B CN106207115B CN201610573238.2A CN201610573238A CN106207115B CN 106207115 B CN106207115 B CN 106207115B CN 201610573238 A CN201610573238 A CN 201610573238A CN 106207115 B CN106207115 B CN 106207115B
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/24—Alkaline accumulators
- H01M10/30—Nickel accumulators
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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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
- H01M4/521—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of iron for aqueous cells
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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
Abstract
The invention discloses a kind of preparation method of stable nickel hydroxide electrode material；Comprise the steps：S11：By solvable nickel salt, solvable manganese salt, soluble organic and glucose in molar ratio 6:2:5:(0~2) ratio is mixed in water, and the nickel manganese double-hydroxide presoma for obtaining Intercalation reaction glucose molecule is dried after water-filling thermal response of going forward side by side；S12：Nickel manganese double-hydroxide presoma is placed in the tube furnace of argon gas circulation and made annealing treatment, and nickel manganese double-hydroxide is obtained after drying；S13：Nickel manganese double-hydroxide and conductive agent, binding agent are pressed 8:1:Nickel hydroxide electrode material is formed after the mixing of 1 mass ratio.The present invention prepares the nickel manganese layered double-hydroxide of wide interlamellar spacing using one step hydro thermal method, strengthen the active force between glucose molecule and levels pole plate on the premise of keeping layer structure not to be destroyed by process annealing again, so that stability is greatly improved, the electrode obtained material obtains higher high current power characteristic and the chemical property such as good cycle life.
Description
Technical field
The invention belongs to new energy materialses and electrochemical energy storing device field, more particularly, to a kind of stable hydroxide
The preparation method of nickel electrode material.
Background technology
Aqueous electrolyte energy storage device, for the traditional storage batteries such as lithium ion battery, lead-acid battery, with price
Cheaply, the features such as charging is rapid, power density is high, stability is high, environment friendly and pollution-free, safety coefficient is high.This aqueous electrolyte
Energy storage device have broad application prospects in fields such as communications market, computer market, new-energy automobile and military equipments.
The energy storage mechnism of aqueous electrolyte energy storage device：The redox reaction mainly occurred with interface (is also known as method
Draw process) based on carry out the transmission of electric charge, ion.Carbon-based material of this energy storage device with depending on specific surface area
Ultracapacitor is compared, and feature is similar but distinguishes, and this energy storage device specific capacity based on redox reaction is remote
Higher than the electric double layer capacitance of carbon-based material, but multiplying power property and cyclical stability in heavy-current discharge is performed poor.
The content of the invention
For the defect of prior art, it is an object of the invention to provide a kind of preparation side of nickel hydroxide electrode material
Method, it is intended to solve that specific capacity of the existing nickel hydroxide electrode material in heavy-current discharge be small and the electrochemistry such as cyclical stability is special
The problem of property is undesirable.
The invention provides a kind of preparation method of nickel hydroxide electrode material, comprise the steps：
S11：By solvable nickel salt, solvable manganese salt, soluble organic and glucose in molar ratio 6:2:5:(0~2) ratio exists
Mixed in water, the nickel manganese double-hydroxide presoma for obtaining Intercalation reaction glucose molecule is dried after water-filling thermal response of going forward side by side；
S12：The nickel manganese double-hydroxide presoma is placed in the tube furnace of argon gas circulation and made annealing treatment, and after drying
Obtain nickel manganese double-hydroxide；
S13：The nickel manganese double-hydroxide and conductive agent, binding agent are pressed 8:1:Hydroxide is formed after the mixing of 1 mass ratio
Nickel electrode material.
Further, the temperature of the hydro-thermal reaction is 80 DEG C~160 DEG C, and the time is 2h~16h.Due to less than 80 DEG C
Resulting powder sample quality is too small, and this may be not exclusively relevant with reaction, in addition the too high resulting powder sample of temperature
Crystallinity is higher, and this is unfavorable for the progress of electrochemical reaction.
Further, the hydro-thermal reaction can be carried out in hydrothermal reaction kettle.
Further, the temperature of the annealing is 200 DEG C~500 DEG C, and the time is 1.5h~3h.Temperature is higher than
Quality reduces obvious quickening at 300 DEG C, illustrates the positive oxide transformation of hydroxide, and specific capacity is reduced rapidly, and temperature is less than 200
DEG C when, hydroxide can not combine closely with interlayer glucose, glucose prevent hydroxide phase transformation it is not obvious enough；Heating speed
Rate is less than 5 DEG C, and heating rate is too fast, and the pattern and structure for being easily caused the nanometer sheet of powder sample are destroyed, heating rate
Too low spent time is oversize, and we have selected more suitable 5 DEG C/min heating rate here.
Further, the solvable nickel salt includes the chlorion in nickel nitrate, nickel chloride or nickel sulfate, the nickel chloride
Without oxygen-containing functional group, size is smaller, more conducively the insertion of glucose macromolecular.
Further, the solvable manganese salt includes manganese nitrate, manganese chloride, manganese sulfate, the wherein chlorion in manganese chloride
Without oxygen-containing functional group, size is smaller, more conducively the insertion of glucose macromolecular.
The present invention prepares the nickel manganese layered double-hydroxide of intercalation glucose molecule using one step hydro thermal method, then passes through
Cross process annealing strengthens the effect between glucose molecule and levels pole plate on the premise of keeping layer structure not to be destroyed
Power so that stability is greatly improved, the electrode obtained material obtains higher high current power characteristic and good circulation
The chemical properties such as life-span.
Brief description of the drawings
Fig. 1 is the preparation method implementation process figure of electrode material provided in an embodiment of the present invention；
Fig. 2 is the SEM figures of the nickel manganese hydroxide after embedded glucose provided in an embodiment of the present invention and process annealing；
Fig. 3 is the nickel manganese hydrogen-oxygen after nickel manganese hydroxide provided in an embodiment of the present invention and embedded glucose and process annealing
The cyclic voltammetry curve schematic diagram of compound；
Fig. 4 is the nickel manganese hydroxide after the nickel manganese hydroxide that present example is provided and embedded glucose and process annealing
The curve synoptic diagram of thing constant current charge-discharge；
Fig. 5 is the nickel manganese hydroxide after the nickel manganese hydroxide that present example is provided and embedded glucose and process annealing
The curve synoptic diagram of thing cycle life.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
For short slab of the existing nickel hydroxide as electrode material, it is an object of the invention to provide a kind of stable hydroxide
The preparation method of nickel electrode material, it is intended to solve specific capacity of the existing nickel hydroxide electrode material in heavy-current discharge small and follow
The problem of electrochemical properties such as ring stability are undesirable.After incorporation manganese element, the heavy-current discharge characteristic of nickel hydroxide is obtained
It is obviously improved, secondly, it is exactly it in cyclic process that restriction nickel hydroxide, which is used to produce one of most important obstacle of energy storage device,
In, irreversible phase transformation can be produced, i.e., from high α phases (interlamellar spacing~8.0 of activity) decay for the β phase (interlamellar spacings of low activity
~4.6), we have been invented by passing through again in Intercalation reaction glucose macromolecular from the layer structure of nickel hydroxide
The method that annealing further lifts the active force of interlayer glucose and hydroxide undergoes phase transition to prevent or postpone it, according to
Measured chemical property, illustrates our this new approaches, and new method is very useful.
The invention provides a kind of preparation method of the nickel hydroxide electrode material of stabilization, comprise the following steps：
S11：By solvable nickel salt, solvable manganese salt, soluble organic and glucose in molar ratio 6 in water:2:5:(0~2)
Mixing, is placed in 80 DEG C~160 DEG C reaction 2h~16h in hydrothermal reaction kettle and completes, clean and Intercalation reaction grape is obtained after drying
The nickel manganese double-hydroxide presoma of glycan molecule；
S12：In the tube furnace that nickel manganese layered double-hydroxide presoma described in step S11 is placed in argon gas circulation
(more than annealing time 1.5h can obtain preferable chemical property to 200 DEG C~500 DEG C annealing 1.5h~3h, therefore we select
2h is used as annealing time the most conventional), the nickel manganese double-hydroxide after cleaning and being annealed after drying；Again by obtained powder
Body sample and conductive agent, binding agent in mass ratio 8:1:1 mixing, grinding are evenly applied to obtain electricity in nickel foam metal substrate
Pole.
Further, in step s 11, the solvable nickel salt includes nickel nitrate, nickel chloride, nickel sulfate, wherein chlorination
Chlorion in nickel is without functional group is contained, and size is smaller, more conducively the insertion of glucose macromolecular.
Further, in step s 11, the solvable manganese salt includes manganese nitrate, manganese chloride, manganese sulfate, wherein chlorination
Chlorion in manganese is without functional group is contained, and size is smaller, more conducively the insertion of glucose macromolecular.
Further, in step s 11,80~160 DEG C of the hydrothermal temperature, in experiment we have found that 80 DEG C with
Lower resulting powder sample quality is too small, and this may be not exclusively relevant with reaction, in addition the too high resulting powder-like of temperature
Product crystallinity is higher, and this is unfavorable for the progress of electrochemical reaction.
Further, in step s 12,200 DEG C~500 DEG C of the annealing temperature, passes through thermogravimetric interpretation of result, temperature
Quality reduces obvious quickening during higher than 300 DEG C, illustrates the positive oxide transformation of hydroxide, and specific capacity is reduced rapidly, and temperature is low
When 200 DEG C, hydroxide can not combine closely with interlayer glucose, and glucose prevents the phase transformation of hydroxide not obvious enough；
Heating rate is less than 5 DEG C, and heating rate is too fast, and the pattern and structure for being easily caused the nanometer sheet of powder sample are destroyed, and rises
The too low spent time of warm speed is oversize, and we have selected more suitable 5 DEG C/min heating rate here.
The present invention prepares the nickel manganese layered double-hydroxide of intercalation glucose molecule using one step hydro thermal method, then passes through
Cross process annealing strengthens the effect between glucose molecule and levels pole plate on the premise of keeping layer structure not to be destroyed
Power so that stability is greatly improved, the electrode obtained material obtains higher high current power characteristic and good circulation
The chemical properties such as life-span.
The present invention prepares transition metal hydroxide electrode material using one step hydro thermal method, react 2 at 80~160 DEG C~
Due to the random motion in aqueous of glucose molecule in 16h crystal growing process, there is part to be embedded into hydrogen-oxygen
Compound interlayer, obtains the hydroxide of interlamellar spacing expansion, then using heating rate as 5 DEG C/min in 200~500 DEG C of argon atmospheres
Annealing so that the active force enhancing of interlayer glucose and hydroxide, the cyclical stability of the electrode obtained material is significantly lifted,
The α phases of high activity are difficult to fail into low chemically active beta phase nickel hydroxide manganese, and obtained electrode material is due to manganese element
Doping also has the electrochemical properties such as higher high current power density.
Fig. 1 shows the preparation principle for the electrode material that present example is provided, and for convenience of description, illustrate only and this hair
The related part of bright embodiment, details are as follows：
The preparation method of electrode material includes：By nickel chloride, manganese chloride, glucose, hexa and hydromassage that
Than 6:2:(0~2):5 mixing, hydro-thermal reaction is to completion, and suction filtration cleans and dried the nickel manganese hydroxide for obtaining glucose insertion；
Again by the nickel manganese hydroxide of obtained powder 200~500 DEG C of glucose insertions more stablized of annealing in argon atmosphere
Thing.
The preparation method of the nickel hydroxide manganese electrode material for the stabilization that the present invention is provided, hence it is evident that improve class alpha-phase nickel hydroxide
The problem of failing to the beta phase nickel hydroxide of low activity, overcomes nickel hydroxide as being stranded that electrode material is applied to a certain extent
It is difficult；The power characteristic of the nickel hydroxide high current of the manganese element of vast scale incorporation simultaneously substantially gets a promotion, and has a wide range of applications
Prospect.
Fig. 2 shows the preparation method implementation process for the stable nickel hydroxide electrode material that present example is provided；It is stable
The preparation method of nickel hydroxide electrode material is specifically included：
S11：Solvable nickel salt, solvable manganese salt, soluble organic and glucose are mixed in water, are placed in hydrothermal reaction kettle
Reaction is cleaned and obtained after drying before the nickel manganese double-hydroxide (mixing manganese nickel hydroxide) of Intercalation reaction glucose molecule to completing
Drive body；Chemical equation：3Ni2++Mn2++7Cl-+2OH-+→Ni3Mn(OH)2Cl7+e-, wherein Mn2+Easily by the oxygen in air
It is oxidized to manganic.
S12：Nickel manganese layered double-hydroxide presoma described in step S11 is placed in the tube furnace of argon gas circulation and moved back
Fiery 2h, obtains the nickel manganese double-hydroxide after process annealing after cleaning and drying.
Wherein, in step s 11, the solvable nickel salt includes nickel nitrate or nickel chloride.In step s 11, it is described solvable
Manganese salt includes manganese nitrate or manganese chloride.In step s 11,80 DEG C~160 DEG C of the hydrothermal temperature.In step s 12, institute
State annealing temperature most appropriate at 280~320 DEG C, according to thermal gravimetric analysis results understand in this temperature range, hydroxide with
The active force of interlayer glucose molecule can increase and hydroxide remains to keep its prototype structure and be unlikely to be transformed into metal
Oxide.
In order to which the preparation method of electrode material provided in an embodiment of the present invention is further illustrated, in conjunction with instantiation
Details are as follows：
Embodiment 1：
(1) prepared by presoma：6mmol nickel chlorides, 2mmol manganese chlorides, 5mmol hexas, 1mmol grape glycogens
Material is dissolved in 60mL deionized waters, 100 DEG C of hydro-thermal reactions 10 hours.It is cleaned and dried to obtain presoma.
(2) stable nickel hydroxide manganese：Take 100mg presomas to be placed in tube furnace, vacuumize, be slowly introducing argon gas, repeat
Three times, heating rate is adjusted to 5 DEG C/minute, rises to 300 DEG C and is incubated 2 hours, reaction is finished, and room temperature is down to naturally.Clean and dry
To powder sample.
(4) preparation of electrode：Electrode material, acetylene black and ptfe emulsion are pressed 8:1:1 ratio mixing, and
Then mixture is added drop-wise in nickel foam, is pressed in 15MPa pressure in nickel foam, finally to well mixed by ultrasound for 1 hour
Dried 12 hours at 60 DEG C, obtain electrode.The chemical property of electrode material is carried out in three electrode test ponds, Hg/HgO conducts
Reference electrode, platinum electrode be to electrode, electrolyte be 6M KOH, its cyclic voltammetry curve as shown in figure 3, in figure closed curve
Area contrast understand that nickel hydroxide manganese redox reaction after modification is substantially enriched than the sample before untreated,
Hydroxide after proof processing is also obviously improved in specific capacity, and this is just corresponding with Fig. 4.In 5Ag-1Current density
Under, charging and discharging curve is as shown in figure 4, its discharge and recharge specific capacitance passes through Cs=IdM Δ t/ Δs V is calculated, and is 505.4Cg-1,
5A·g-1Under current density circulate 1000 times after capacity still keep 90.0%, such as Fig. 5, represent modification after hydroxide with
Untreated hydroxide is compared, and not only specific capacity, which has, is obviously improved, and stability has even more significantly been lifted, is that it can
Realize to commercially produce as electrode material and provide possible.
By checking, the electrode material that insertion different content (0,0.5,1,2mmol) glucose is obtained in the present embodiment is obtained
The chemical property obtained is as shown in following table one：
Table one
By checking, control in the case of the reaction volume and reaction time identical in hydro-thermal reaction, investigate in this example
Influence of the hydrothermal temperature to presoma chemical property, as shown in following table two：
Table two
By checking, control in the case of the reaction volume and reaction temperature identical in hydro-thermal reaction, investigate in this example
Influence of the hydro-thermal reaction time to presoma chemical property, as shown in following table three：
Table three
By verifying, in this example in the case of glucose amount identical is kept, different annealing temperature (200~500 DEG C)
The chemical property that obtained electrode material is obtained is as shown in Table 4：
Table four
By verifying, in this example in the case of other conditions identical is ensured, different annealing times (1.5~3h) are studied
Influence to electrode material performance, the chemical property that obtained electrode material is obtained is as shown in Table 5：
Table five
In summary, the present invention prepares transition double-metal hydroxide electrode material using one step hydro thermal method, is reacting
Glucose is inserted into hydroxide interlayer in journey, expands interlamellar spacing so as to accelerate the transmission of electrolyte ion, to lifting electrochemistry
Performance has obvious effect.In summary, this path the electrode obtained material have higher cyclical stability simultaneously its specific capacitance it is high, compared with
The chemical properties such as good high current power characteristic.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of nickel hydroxide electrode material, it is characterised in that comprise the steps：
S11：By solvable nickel salt, solvable manganese salt, hexa and glucose in molar ratio 6:2:5:(0.5~2) ratio exists
Mixed in water, the nickel manganese double-hydroxide presoma for obtaining Intercalation reaction glucose molecule is dried after water-filling thermal response of going forward side by side；
S12：The nickel manganese double-hydroxide presoma is placed in the tube furnace of argon gas circulation and made annealing treatment, and is obtained after drying
Nickel manganese double-hydroxide；
S13：The nickel manganese double-hydroxide and conductive agent, binding agent are pressed 8:1:Nickel hydroxide electricity is formed after the mixing of 1 mass ratio
Pole material.
2. preparation method as claimed in claim 1, it is characterised in that the temperature of the hydro-thermal reaction is 80 DEG C~160 DEG C, when
Between be 2h~16h.
3. preparation method as claimed in claim 1, it is characterised in that the hydro-thermal reaction is carried out in hydrothermal reaction kettle.
4. the preparation method as described in claim any one of 1-3, it is characterised in that the temperature of the annealing is 200 DEG C
~500 DEG C, the time is 1.5h~3h.
5. preparation method as claimed in claim 4, it is characterised in that heating rate is 5 DEG C/min.
6. the preparation method as described in claim any one of 1-3, it is characterised in that the solvable nickel salt includes nickel nitrate, chlorine
Change nickel or nickel sulfate.
7. the preparation method as described in claim any one of 1-3, it is characterised in that the solvable manganese salt includes manganese nitrate, chlorine
Change manganese or manganese sulfate.
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| CN107527752A (en) * | 2017-06-29 | 2017-12-29 | 江苏大学 | A kind of preparation method of composite electrode material for super capacitor |
| CN108264099B (en) * | 2018-01-03 | 2019-11-26 | 桂林理工大学 | A kind of preparation method of lithium ion battery high-performance two-dimensional sheet nickel oxide negative electrode material |
| CN112279313A (en) * | 2020-10-22 | 2021-01-29 | 哈尔滨工业大学 | Preparation method and application of manganese-doped nickel hydroxide composite material |
| CN114050057B (en) * | 2021-10-29 | 2023-05-30 | 上海应用技术大学 | copper-cobalt-sulfur@NiMn-G-LDH composite electrode material and preparation method and application thereof |
| CN114335448B (en) * | 2022-01-04 | 2023-10-31 | 湖北大学 | Nickel-cobalt hydroxide with multilayer nano-sheet structure, and preparation method and application thereof |
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| CN101882680B (en) * | 2010-06-23 | 2012-06-27 | 郑州轻工业学院 | Nickel-manganese composite hydroxide material for alkaline secondary battery and preparation method thereof |
| CN105655152A (en) * | 2015-12-31 | 2016-06-08 | 上海应用技术学院 | Ni-Mn layered double hydroxide@nickel foam@carbon three-dimensional hierarchically-structured electrode material and preparation method thereof |
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