CN108735518A - A kind of hexagonal flake manganese oxide@nickel oxide composite materials and preparation method thereof - Google Patents
A kind of hexagonal flake manganese oxide@nickel oxide composite materials and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention provides the preparation methods that a kind of hexagonal flake manganese oxide aoxidizes ni compound oxide：First manganese-nickel-aluminum alloy mother's ingot melt spinning method processing will be prepared into alloy thin band；Alloy thin band is subjected to de- alloying corrosion with ammonium salt solution again and obtains de- alloyed product；Alloyed product difference deionized water and washes of absolute alcohol are finally taken off, is then dried, hexagonal flake manganese oxide is obtained and aoxidizes ni compound oxide；Its structure is that hexagonal flake manganese oxide wraps up one layer of graininess nano-nickel oxide；The size of the manganese oxide is 0.65-3.15 μm, and nickel oxide size is 100-200nm.The hexagonal flake manganese oxide of the present invention aoxidizes nickel compound, is in positive hexagonal flake structure, and manganese oxide piece wrapped up by rule particle shape nickel oxide, pattern rule, better crystallinity degree, size uniform, controllable, has higher specific surface area.In addition, the alloy thin band that the present invention is prepared using melt spinning method ensure that structural homogeneity as presoma, it can effective Improving The Quality of Products.
Description
Technical field
The invention belongs to new material technology fields, and in particular to compound transition metal oxide synthetic technology, especially one
Kind hexagonal flake manganese oxide oxidation ni compound oxide and preparation method thereof.
Background technology
Compound transition metal oxide is the polynary complexity being compounded to form by two or more transition metal oxide
Oxide.Compared with single oxide, which has more preferably property in terms of optics, magnetics, electricity, therefore
It is widely used in energy related field（Electro-catalysis, lithium ion battery, ultracapacitor etc.）.At the same time, such is multiple
It closes oxide and is also equipped with the features such as good stability, corrosion resistance, high temperature resistant.
Used as catalyst, such material is generally non-stoichiometric compound, in system there is anion, just from
A large amount of vacancy of son closely form specific activated centre, promote reactant to activate by the electronics transfer between metal-oxygen.?
During metal oxide oxidation catalyst, the Transient oxygen of activation can be formed, by means of adsorbing oxygen effect, Lattice Oxygen acts on and to form catalysis
Cycle.
As one kind of transition metal oxide, it is formed by binary compound that there are multiple stoichiometries in Mn-O
Than, such as MnO2、Mn2O3、MnO、Mn3O4、Mn2O7、Mn5O8Etc..MnO2Complicated, molecular formula should be expressed as MnOx, x tables
Show that oxygen content, numerical value are less than 2.Low price Mn ions and OH are typically contained in chemical composition-, can additionally contain other gold of part
Belong to ion.Presently, it is recognized that MnO2Crystal structure is：Mn4+It is coordinated to form octahedron [MnO with O6] and be built into a cube Mi Dui
Product, oxygen atom is on octahedra angle top at this time, Mn4+Positioned at octahedra center.[MnO6] it is octahedra between altogether rib connect into it is single-stranded
Or double-strand, these chains push up altogether with other octahedra chains to be connected, and ultimately forms gap or tunnel structure.The above structure is its conduct
Strong oxidizer in electrochemical capacitor material, catalysts and acid solution, organic synthesis provides foundation.
Synthesize MnO2Conventional method include hydro-thermal method, sol-gel method, pyrolysismethod and coprecipitation etc..Above-mentioned side
In method, hydro-thermal reaction, liquid-phase precipitation and molten-salt growth method are all to prepare MnO using redox reaction mostly2, i.e., using reduction
Agent restores the compound containing high price manganese ion, and then obtains MnO2Product.It is more using the obtained product of liquid-phase precipitation method
For α-MnO2, and using molten-salt growth method prepare such material when, tend to obtain α-MnO when reaction temperature is at 400 DEG C -500 DEG C2
With γ-MnO2Mixture then causes to obtain amorphous state MnO at 300 DEG C when reaction temperature is controlled2, crystallinity is poor.Sol-gel
Method prepares MnO2When, then it needs to prepare precursors, then calcining removal of impurities at high temperature.
Application No. is 201310069196.5 Chinese patents to report a kind of preparation side of overlength manganese dioxide nanowire
Method.For this method using manganese sulfate as reducing agent, potassium chlorate is oxidant, using potassium acetate and acetic acid as additive, in polytetrafluoroethylene (PTFE)
In the autoclave of liner, the hydro-thermal reaction 6-24h at 140-200 DEG C, after natural cooling, product washs, filters, it is super to be dried to obtain
Long manganese dioxide nanowire.Application No. is 201110063644.1 Chinese patents to disclose a kind of bigger serface stratiform oxidation
The preparation method of manganese bouquet.It is 1 in molar ratio by potassium permanganate and ammonium sulfate, deionized water:0.25-1:123-222 is added to
It in hydrothermal reaction kettle, is uniformly mixed, places it in homogeneous reactor, reacted 18-36 hours in 90-110 DEG C of incubation water heating, from
So cooling, it is neutrality that deionized water, which is washed to filtrate, and products therefrom is 12 hours dry at 50 DEG C of baking oven.Currently, document and phase
Close the MnO that patent is reported2Compound is mostly nano wire, nanometer rods, flower ball-shaped.
It how to be further simplified synthesis path, shortens the reaction time, and then promotes product the effective output rate, is to need to solve
Main problem.
Invention content
For the problems such as oxidation manganese composite oxide reaction time is long, output capacity is low is prepared in the prior art, the present invention carries
For a kind of preparation method of manganese oxide@nickel oxide composite materials, this method simple process is easily-controllable, does not need the instrument such as autoclave
Device, and required time is short, output capacity is high, no coupling product pollution.
It is a further object of the present invention to provide a hexagonal flake manganese oxide@nickel oxide using above method preparation is compound
Material, better crystallinity degree is size uniform, controllable, has higher specific surface area.
To achieve the above object, the present invention adopts the following technical scheme that.
A kind of preparation method of hexagonal flake manganese oxide oxidation ni compound oxide, includes the following steps：
（1）Manganese-nickel-aluminum alloy mother's ingot melt spinning method processing is prepared into alloy thin band；
（2）Alloy thin band is subjected to de- alloying corrosion with ammonium salt solution and obtains de- alloyed product；
（3）De- alloyed product cleaning, it is dry, it obtains hexagonal flake manganese oxide and aoxidizes ni compound oxide.
Step（1）In, the alloy thin band thickness is 25-60 μm, width 2.0-4.0mm.
Each element atomic percent is manganese 55-75%, nickel 17-30%, aluminium 5-25% in the manganese-nickel-aluminum alloy mother's ingot.
The manganese-nickel-aluminum alloy mother's ingot is made using pure manganese piece or manganese-aluminium alloy as manganese source with pure nickel or nickel-aluminum alloy
For nickel source, using fine aluminium as silicon source.Preferably, the mass percentage of aluminium is 0.5-20.0% in manganese-aluminium alloy, remaining is manganese
And trace impurity；The mass percentage of nickel-aluminum Aluminum in Alloy is 2.0-32.5%, remaining is nickel and trace impurity.Above-mentioned raw materials
It can also be prepared by commercially available.
The manganese-nickel-aluminum alloy mother's ingot is that induction melting forms in the argon atmosphere that pressure is 0.5MPa.Melting
In the process, prevent alloying component from aoxidizing using induction melting, inert gas shielding.Preferred melting number is 3-5 times.
Preferably, manganese-nickel-aluminum alloy mother's ingot revolves the obtained alloy thin band of method of quenching using single roller；Roll shaft rotating speed is preferably
1000-2000r/min。
Step（2）In, the ammonium salt is preferably ammonium sulfate, ammonium chloride or ammonium nitrate；A concentration of 0.9- of ammonium salt solution
1.2mol/L, preferably 1.0mol/L.The de- alloy time is 60min or more, preferably 90min.The temperature of de- alloy is 20-50
DEG C, preferably 25 DEG C.Add 600mL ammonium salt solutions according to every gram of alloy thin band.
Preferably, step（2）In, further include the steps that supersonic oscillations：It is primary with ultrasonic oscillation per hour, every time
Time 10min.
The step（3）Middle cleaning step is to be respectively washed using deionized water and absolute ethyl alcohol.
A kind of manganese oxide oxidation nickel compound that the above method obtains；Its structure is that hexagonal flake manganese oxide wraps up one layer
Graininess nano-nickel oxide；The size of the manganese oxide is 0.65-3.15 μm, and nickel oxide size is 25-270nm.
The present invention has the following advantages：
The hexagonal flake manganese oxide of the present invention aoxidizes nickel compound, is in positive hexagonal flake structure, manganese oxide piece is by rule particle shape
Nickel oxide is wrapped up, pattern rule, better crystallinity degree, size uniform, controllable, has higher specific surface area.In addition, the present invention adopts
Alloy thin band prepared by melt spinning method is used to ensure that structural homogeneity as presoma, it can effective Improving The Quality of Products.In system
Aluminium is added, the Relative distribution situation of manganese, nickel in controllable master alloy, and then in corrosion process, coordinate etchant solution, corrosion temperature
The synergistic effect of degree realizes the entrance of oxygen atom, to realize that different-grain diameter manganese oxide aoxidizes the generation of nickel product.Using de-
Alloying prepares metal oxide composite, for perfect and Development of Novel oxide characterization, understands in depth and designs
Developing electrochemical capacitor, catalyst material etc. has important theory value and directive significance.
Description of the drawings
Fig. 1 is manganese-nickel-aluminum alloy thin band prepared by embodiment 1；
Fig. 2 is the scanning electron microscopic picture that hexagonal flake manganese oxide prepared by embodiment 2 aoxidizes nickel compound；
Fig. 3 is the scanning electron microscopic picture that hexagonal flake manganese oxide prepared by embodiment 3 aoxidizes nickel compound.
Specific implementation mode
With reference to embodiment and attached drawing, the present invention will be further described, but the present invention is not limited by following embodiments
System.
Embodiment 1
（1）Manganese-nickel-aluminum alloy mother's ingot melt spinning method processing is prepared into alloy thin band：Pure manganese, pure nickel, fine aluminium are pressed into atomic ratio
75:20:5 ratios mix, using argon gas（Pressure is 0.5MPa）Atmosphere protection, electric arc melting 3 times, are made after ingredient is uniform
Standby manganese-nickel-aluminum alloy mother's ingot；Above-mentioned alloy mother ingot revolves the system of quenching with single roller and handles, and copper roller rotating speed is set in 1700-
Within the scope of 2000r/min, thickness is obtained between 25 μm -60 μm, strip of the width between 3.0-4.0mm, as shown in Figure 1：
Alloy thin band has metallic luster, smooth surface, bright and clean；
（2）Weigh step（1）The alloy thin band 0.2g of gained intercepts into segment, is placed in 25 DEG C, a concentration of 0.9mol/L of 120mL
Ammonium nitrate solution in, it is primary with ultrasonic oscillation per hour, vibrate 10min every time, persistently corrode 180min obtain take off alloy
Change product；
（3）De- alloyed product uses deionized water and washes of absolute alcohol respectively, is then placed in drying in 50 DEG C of thermostatic drying chambers,
It obtains hexagonal flake manganese oxide and aoxidizes ni compound oxide；Hexagonal flake manganese oxide size range is at 1.95-3.05 μm in product
Between, it is uniformly wrapped up by one layer of particulate oxidation nickel, the nickel oxide size is between 97.7-192.5nm.
Embodiment 2
（1）Manganese-nickel-aluminum alloy mother's ingot melt spinning method processing is prepared into alloy thin band：By pure manganese, nickel-aluminum alloy（Wherein aluminum
Amount percentage is 10.0wt.%）, fine aluminium press manganese-nickel-aluminum atomic ratio 63:25:12 ratios mix, using argon gas（Pressure is
0.5MP）Atmosphere protection, electric arc melting 4 times obtain preparing manganese-nickel-aluminum alloy mother's ingot after ingredient is uniform；Above-mentioned alloy mother ingot
It is handled with single roller rotation system of quenching, copper roller rotating speed is set within the scope of 1200-1500r/min, obtains thickness at 25 μm -50 μm
Between, strip of the width between 3.0-4.0mm；
（2）Weigh step（1）The alloy thin band 0.2g of gained intercepts into segment, is placed in 50 DEG C, a concentration of 1.0mol/L of 120mL
Ammonium sulfate in, persistently corrode 90min obtain take off alloyed product；
（3）De- alloyed product uses deionized water and washes of absolute alcohol respectively, is then placed in drying in 50 DEG C of thermostatic drying chambers,
It obtains hexagonal flake manganese oxide and aoxidizes ni compound oxide；Its scanning electron microscopic picture is as shown in Figure 2, wherein（a）For gained six
Square piece shape manganese oxide aoxidizes the microscopic appearance picture of nickel product, figure（b）For figure（a）Shown in region enlarged drawing.Figure（c-e）
Respectively scheme（b）The element Surface scan analysis chart of Mn, Ni and O element in region, different elements are indicated with different colours：Mn is red
Color, Ni are green, and O is purple, and each element is distributed on composite oxides.Hexagonal flake manganese oxide size range exists in product
Between 1.77-2.97 μm, uniformly wrapped up by one layer of particulate oxidation nickel, the nickel oxide size 115.2-162.9nm it
Between.
Embodiment 3
（1）Manganese-nickel-aluminum alloy mother's ingot melt spinning method processing is prepared into alloy thin band：By manganese-aluminium（Wherein aluminium mass percent
For 10.5wt.%）, nickel-aluminum（Wherein aluminium mass percent is 19.0wt.%）By manganese-nickel-aluminum atomic ratio 60:17:23 ratios are mixed
It closes, using argon gas（Pressure is 0.5MP）Atmosphere protection, electric arc melting 5 times obtain preparing manganese-nickel-aluminum alloy after ingredient is uniform
Female ingot；Above-mentioned alloy mother ingot revolves the system of quenching with single roller and handles, and copper roller rotating speed is set within the scope of 1000-1200r/min, is obtained
Thickness is obtained between 20 μm -50 μm, strip of the width between 2.7-3.8mm；
（2）Weigh step（1）The alloy thin band 0.2g of gained intercepts into segment, is placed in 20 DEG C, a concentration of 1.1mol/L of 120mL
Ammonium chloride solution in, persistently corrode 120min obtain take off alloyed product；
（3）De- alloyed product uses deionized water and washes of absolute alcohol respectively, is then placed in drying in 50 DEG C of thermostatic drying chambers,
It obtains hexagonal flake manganese oxide and aoxidizes ni compound oxide；Its scanning electron microscopic picture is as shown in Figure 3：In product, hexagon sheet
The size range of manganese oxide is between 0.85-1.79 μm, regular shape, any surface finish, and manganese oxide edge is by micro-oxidation nickel
Grain is wrapped up, and nickel oxide size is between 26.8-60.0nm.
Claims (10)
1. a kind of preparation method of hexagonal flake manganese oxide oxidation ni compound oxide, which is characterized in that include the following steps：
（1）Manganese-nickel-aluminum alloy mother's ingot melt spinning method processing is prepared into alloy thin band；
（2）Alloy thin band is subjected to de- alloying corrosion with ammonium salt solution and obtains de- alloyed product；
（3）De- alloyed product cleaning, it is dry, it obtains hexagonal flake manganese oxide and aoxidizes ni compound oxide.
2. preparation method according to claim 1, which is characterized in that step（1）In, in the manganese-nickel-aluminum alloy mother's ingot
Each element atomic percent is manganese 55-75%, nickel 17-30%, aluminium 5-25%.
3. preparation method according to claim 1, which is characterized in that step（1）In, the manganese-nickel-aluminum alloy mother's ingot,
Using pure manganese piece or manganese-aluminium alloy as manganese source, using pure nickel or nickel-aluminum alloy as nickel source, using fine aluminium as silicon source.
4. preparation method according to claim 3, which is characterized in that the mass percentage of aluminium is in manganese-aluminium alloy
0.5-20.0%, remaining is manganese and trace impurity；The mass percentage of nickel-aluminum Aluminum in Alloy is 2.0-32.5%, remaining is nickel
And trace impurity.
5. preparation method according to claim 1, which is characterized in that step（1）In, the manganese-nickel-aluminum alloy mother's ingot is
Induction melting forms in the argon atmosphere that pressure is 0.5MPa；Melting number is 3-5 times.
6. preparation method according to claim 1, which is characterized in that step（1）In, manganese-nickel-aluminum alloy mother's ingot is using single
Roller revolves method of quenching and alloy thin band is made；Roll shaft rotating speed is 1000-2000r/min；The alloy thin band thickness is 25-60 μm, wide
Degree is 2.0-4.0mm.
7. preparation method according to claim 1, which is characterized in that step（2）In, the ammonium salt be preferably ammonium sulfate,
Ammonium chloride or ammonium nitrate；A concentration of 0.9-1.2mol/L of ammonium salt solution.
8. preparation method according to claim 1, which is characterized in that step（2）In, it is 60min or more to take off the alloy time；
The temperature of de- alloy is 20-50 DEG C；The mass volume ratio of the alloy thin band and ammonium salt solution is preferably 1:500-600.
9. preparation method according to claim 1, which is characterized in that step（2）In, further include the step of supersonic oscillations
Suddenly：It is primary with ultrasonic oscillation per hour, each time 10min.
10. a kind of manganese oxide obtained using any preparation methods of claim 1-9 aoxidizes nickel compound, which is characterized in that its
Structure is that hexagonal flake manganese oxide wraps up one layer of graininess nano-nickel oxide；The size of the manganese oxide is 0.65-3.15 μm, oxygen
Change nickel size is 25-270nm.
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