CN108735518B - Hexagonal flaky manganese oxide @ nickel oxide composite material and preparation method thereof - Google Patents
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Abstract
The invention provides a preparation method of a hexagonal flaky manganese oxide @ nickel oxide composite oxide, which comprises the following steps: firstly, carrying out rotary quenching treatment on a manganese-nickel-aluminum alloy mother ingot melt to prepare an alloy thin strip; then, carrying out dealloying corrosion on the alloy thin strip by using an ammonium salt solution to obtain a dealloyed product; finally, respectively washing the dealloying product with deionized water and absolute ethyl alcohol, and then drying to obtain hexagonal flaky manganese oxide @ nickel oxide composite oxide; the structure is that hexagonal flaky manganese oxide is wrapped with a layer of granular nano nickel oxide; the size of the manganese oxide is 0.65-3.15 μm, and the size of the nickel oxide is 100-200 nm. The hexagonal flaky manganese oxide @ nickel oxide compound is in a regular hexagonal flaky structure, and manganese oxide sheets are wrapped by regular granular nickel oxide, so that the compound is regular in appearance, good in crystallinity, uniform and controllable in size and higher in specific surface area. In addition, the alloy thin strip prepared by melt spinning is used as a precursor, so that the structural uniformity is ensured, and the product quality can be effectively improved.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a synthesis technology of a transition metal composite oxide, in particular to a hexagonal flaky manganese oxide @ nickel oxide composite oxide and a preparation method thereof.
Background
The transition metal composite oxide is a multi-component complex oxide formed by compounding two or more transition metal oxides. Compared with single oxides, the composite oxides have better properties in the aspects of optics, magnetics and electricity, so the composite oxides are widely applied to energy related fields (electrocatalysis, lithium ion batteries, super capacitors and the like). Meanwhile, the composite oxide also has the characteristics of good stability, corrosion resistance, high temperature resistance and the like.
When the material is used as a catalyst, the material is generally a non-stoichiometric compound, a large number of vacancies of negative ions and positive ions exist in a system, a specific active center is formed, and the activation of reactants is promoted through the electron transfer between metal and oxygen. In the process of metal oxide catalysis, activated transition state oxygen is formed, and a catalytic cycle is formed by virtue of the action of adsorbed oxygen and the action of lattice oxygen.
As one of the transition metal oxides, there are multiple stoichiometric ratios in the binary compound formed from Mn-O, such as MnO2、Mn2O3、MnO、Mn3O4、Mn2O7、Mn5O8And so on. MnO2The structure is complex, and the molecular formula of the complex is expressed as MnOxAnd x represents the oxygen content, the value being less than 2. Generally contains low-valent Mn ions and OH in chemical composition-And in addition, the metal ions can also contain part of other metal ions. At present, MnO is generally accepted2The crystal structure is as follows: mn4+Coordinated to O to form octahedra [ MnO ]6]And is built into cubic close packing, where the oxygen atoms are located on the vertices of octahedron, Mn4+Located in the center of the octahedron. [ MnO ] of6]The octahedrons are connected into a single chain or a double chain in a common arris mode, and the chains are connected with other octahedron chains in a common vertex mode to finally form a gap or a tunnel structure. The structure provides a basis for the electrochemical capacitor material, the reaction catalyst, the acidic solution and the strong oxidant in organic synthesis.
Synthesis of MnO2Conventional methods include hydrothermal method, sol-gel method, thermal decomposition and coprecipitation method, etc. Among the above methods, hydrothermal reaction, liquid-phase precipitation and molten-salt growth are mostly used for producing MnO by redox reaction2By reducing compounds containing high-valent manganese ions with reducing agents, MnO is obtained2The product obtained by the liquid phase precipitation method is α -MnO mostly2When the material is prepared by a molten salt methodα -MnO tends to be obtained at reaction temperatures of 400 ℃ to 500 ℃2And gamma-MnO2Mixture, when the reaction temperature is controlled at 300 ℃ results in obtaining amorphous MnO2The crystallinity is poor. Preparation of MnO by sol-gel method2In the case of the method, a reaction precursor is prepared, and then the reaction precursor is calcined at a high temperature to remove impurities.
Chinese patent application No. 201310069196.5 reports a method for preparing ultra-long manganese dioxide nanowires. The method comprises the steps of taking manganese sulfate as a reducing agent, potassium chlorate as an oxidizing agent, potassium acetate and acetic acid as additives, carrying out hydrothermal reaction for 6-24 hours in a polytetrafluoroethylene-lined high-pressure kettle at 140-200 ℃, naturally cooling, washing, filtering and drying a product to obtain the ultralong manganese dioxide nanowire. The Chinese patent with the application number of 201110063644.1 discloses a preparation method of a layered manganese oxide flower ball with a large specific surface area. Adding potassium permanganate, ammonium sulfate and deionized water into a hydrothermal reaction kettle according to the mol ratio of 1:0.25-1:123-222, uniformly mixing, placing the mixture into a homogeneous reactor, carrying out hydrothermal reaction for 18-36 hours at the constant temperature of 90-110 ℃, naturally cooling, washing with deionized water until the filtrate is neutral, and drying the obtained product for 12 hours at the temperature of 50 ℃ in an oven. MnO reported in the literature and related patents at present2The compounds are mostly in the shapes of nanowires, nanorods and flower spheres.
How to further simplify the synthesis path, shorten the reaction time and further improve the effective yield of the product is a main problem to be solved.
Disclosure of Invention
Aiming at the problems of long reaction time, low yield and the like of the manganese oxide composite oxide prepared in the prior art, the invention provides the preparation method of the manganese oxide @ nickel oxide composite material, which has the advantages of simple and easily-controlled process, no need of high-pressure reaction kettles and other instruments, short required time, high yield and no byproduct pollution.
The invention also aims to provide the hexagonal flaky manganese oxide @ nickel oxide composite material prepared by the method, which has the advantages of good crystallinity, uniform and controllable size and higher specific surface area.
In order to achieve the purpose, the invention adopts the following technical scheme.
A preparation method of a hexagonal flaky manganese oxide @ nickel oxide composite oxide comprises the following steps:
(1) carrying out rotary quenching treatment on the manganese-nickel-aluminum alloy mother ingot melt to prepare an alloy thin strip;
(2) dealloying the alloy thin strip by using an ammonium salt solution to obtain a dealloyed product;
(3) and cleaning and drying the dealloyed product to obtain the hexagonal flaky manganese oxide @ nickel oxide composite oxide.
In the step (1), the thickness of the alloy thin strip is 25-60 μm, and the width is 2.0-4.0 mm.
The manganese-nickel-aluminum alloy mother ingot comprises 55-75% of manganese, 17-30% of nickel and 5-25% of aluminum in atomic percentage.
The manganese-nickel-aluminum alloy mother ingot takes a pure manganese sheet or a manganese-aluminum alloy as a manganese source, takes pure nickel or a nickel-aluminum alloy as a nickel source and takes pure aluminum as an aluminum source. Preferably, the mass percentage of aluminum in the manganese-aluminum alloy is 0.5-20.0%, and the balance is manganese and trace impurities; the mass percentage of aluminum in the nickel-aluminum alloy is 2.0-32.5%, and the balance is nickel and trace impurities. The above raw materials can be purchased commercially or can be prepared.
The manganese-nickel-aluminum alloy mother ingot is formed by induction melting in an argon protective atmosphere with the pressure of 0.5 MPa. In the smelting process, the oxidation of alloy components is prevented by adopting induction smelting and inert gas protection. The preferred number of heats is 3-5.
Preferably, the manganese-nickel-aluminum alloy master ingot is made into an alloy thin strip by a single-roller rotary quenching method; the rotating speed of the roller shaft is preferably 1000-.
In the step (2), the ammonium salt is preferably ammonium sulfate, ammonium chloride or ammonium nitrate; the concentration of the ammonium salt solution is 0.9-1.2mol/L, and 1.0mol/L is preferred. The dealloying time is more than 60min, preferably 90 min. The dealloying temperature is 20-50 deg.C, preferably 25 deg.C. Adding 600mL of ammonium salt solution per gram of alloy thin strip.
Preferably, the step (2) further includes a step of ultrasonic oscillation: shaking with ultrasonic wave once per hour for 10min each time.
And the cleaning step in the step (3) is to respectively clean the glass substrate by using deionized water and absolute ethyl alcohol.
A manganese oxide @ nickel oxide compound obtained by the above process; the structure is that hexagonal flaky manganese oxide is wrapped with a layer of granular nano nickel oxide; the size of the manganese oxide is 0.65-3.15 mu m, and the size of the nickel oxide is 25-270 nm.
The invention has the following advantages:
the hexagonal flaky manganese oxide @ nickel oxide compound is in a regular hexagonal flaky structure, and manganese oxide sheets are wrapped by regular granular nickel oxide, so that the compound is regular in appearance, good in crystallinity, uniform and controllable in size and higher in specific surface area. In addition, the alloy thin strip prepared by melt spinning is used as a precursor, so that the structural uniformity is ensured, and the product quality can be effectively improved. Aluminum is added into the system, the relative distribution condition of manganese and nickel in the master alloy can be regulated and controlled, and further, the synergistic effect of a corrosion solution and corrosion temperature is coordinated in the corrosion process, so that oxygen atoms are introduced, and the generation of manganese oxide @ nickel oxide products with different particle sizes is realized. The dealloying method is adopted to prepare the metal oxide composite material, and has important theoretical value and guiding significance for perfecting and developing the characterization of novel oxides, deeply knowing, designing and developing electrochemical capacitors, catalyst materials and the like.
Drawings
FIG. 1 is a thin strip of manganese-nickel-aluminum alloy made according to example 1;
FIG. 2 is a scanning electron micrograph of hexagonal plate-like manganese oxide @ nickel oxide compound prepared in example 2;
fig. 3 is a scanning electron micrograph of the hexagonal plate-shaped manganese oxide @ nickel oxide compound prepared in example 3.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the present invention is not limited to the following examples.
Example 1
(1) Carrying out melt spinning quenching treatment on a manganese-nickel-aluminum alloy mother ingot to prepare an alloy thin strip: mixing pure manganese, pure nickel and pure aluminum according to an atomic ratio of 75:20:5, carrying out arc melting for 3 times under the protection of an argon atmosphere (the pressure is 0.5 MPa), and obtaining a manganese-nickel-aluminum alloy mother ingot after the components are uniform; the alloy mother ingot is treated by a single-roller rotary quenching system, the rotating speed of a copper roller is set within the range of 1700-2000r/min, and a thin strip with the thickness of 25-60 mu m and the width of 3.0-4.0mm is obtained, as shown in figure 1: the alloy thin strip has metallic luster and smooth and bright surface;
(2) weighing 0.2g of the alloy thin strip obtained in the step (1), cutting the alloy thin strip into small sections, placing the small sections in 120mL ammonium nitrate solution with the concentration of 0.9mol/L at the temperature of 25 ℃, oscillating the alloy thin strip once per hour by using ultrasonic waves for 10min each time, and continuously corroding the alloy thin strip for 180min to obtain a dealloyed product;
(3) respectively cleaning the dealloying product by using deionized water and absolute ethyl alcohol, and then drying in a constant-temperature drying oven at 50 ℃ to obtain hexagonal flaky manganese oxide @ nickel oxide composite oxide; the size of hexagonal flaky manganese oxide in the product ranges from 1.95 to 3.05 mu m, and the hexagonal flaky manganese oxide is uniformly wrapped by a layer of granular nickel oxide, wherein the size of the nickel oxide ranges from 97.7 to 192.5 nm.
Example 2
(1) Carrying out melt spinning quenching treatment on a manganese-nickel-aluminum alloy mother ingot to prepare an alloy thin strip: mixing pure manganese, nickel-aluminum alloy (wherein the aluminum content is 10.0 wt.%), pure aluminum according to manganese-nickel-aluminum atomic ratio 63:25:12, adopting argon (pressure is 0.5 MP) atmosphere protection, arc melting 4 times, obtaining manganese-nickel-aluminum alloy mother ingot after the components are uniform; the alloy mother ingot is treated by a single-roller rotary quenching system, the rotating speed of a copper roller is set within the range of 1200-1500r/min, and a thin strip with the thickness of 25-50 mu m and the width of 3.0-4.0mm is obtained;
(2) weighing 0.2g of the alloy thin strip obtained in the step (1), cutting the alloy thin strip into small sections, placing the small sections in an ammonium sulfate solution with the concentration of 1.0mol/L and the temperature of 50 ℃, and continuously corroding for 90min to obtain a dealloyed product;
(3) respectively cleaning the dealloying product by using deionized water and absolute ethyl alcohol, and then drying in a constant-temperature drying oven at 50 ℃ to obtain hexagonal flaky manganese oxide @ nickel oxide composite oxide; the scanning electron microscope picture is shown in figure 2, wherein, (a) is the micro-morphology picture of the obtained hexagonal flaky manganese oxide @ nickel oxide product, and (b) is the enlarged view of the area shown in the picture (a). Graphs (c-e) are elemental surface scan analysis graphs of the Mn, Ni and O elements, respectively, in the region of graph (b), with different colors representing the different elements: mn is red, Ni is green, O is purple, and each element is distributed on the composite oxide. The size of hexagonal flaky manganese oxide in the product ranges from 1.77 to 2.97 mu m, and the hexagonal flaky manganese oxide is uniformly wrapped by a layer of granular nickel oxide, wherein the size of the nickel oxide is 115.2 to 162.9 nm.
Example 3
(1) Carrying out melt spinning quenching treatment on a manganese-nickel-aluminum alloy mother ingot to prepare an alloy thin strip: mixing manganese-aluminum (wherein the aluminum content is 10.5 wt.%), nickel-aluminum (wherein the aluminum content is 19.0 wt.%) according to the manganese-nickel-aluminum atomic ratio of 60:17:23, performing arc melting for 5 times under the protection of argon (pressure of 0.5 MP), and obtaining a manganese-nickel-aluminum alloy mother ingot after the components are uniform; the alloy mother ingot is treated by a single-roller rotary quenching system, the rotating speed of a copper roller is set within the range of 1000-1200r/min, and a thin strip with the thickness of 20-50 mu m and the width of 2.7-3.8mm is obtained;
(2) weighing 0.2g of the alloy thin strip obtained in the step (1), cutting the alloy thin strip into small sections, placing the small sections in 120mL of ammonium chloride solution with the concentration of 1.1mol/L at the temperature of 20 ℃, and continuously corroding for 120min to obtain a dealloyed product;
(3) respectively cleaning the dealloying product by using deionized water and absolute ethyl alcohol, and then drying in a constant-temperature drying oven at 50 ℃ to obtain hexagonal flaky manganese oxide @ nickel oxide composite oxide; the scanning electron microscope picture is shown in FIG. 3: in the product, the size range of the hexagonal flaky manganese oxide is between 0.85 and 1.79 mu m, the shape is regular, the surface is smooth, the edges of the manganese oxide are wrapped by trace nickel oxide particles, and the size of the nickel oxide is between 26.8 and 60.0 nm.
Claims (8)
1. A preparation method of a hexagonal flaky manganese oxide @ nickel oxide composite oxide is characterized by comprising the following steps of:
(1) carrying out rotary quenching treatment on the manganese-nickel-aluminum alloy mother ingot melt to prepare an alloy thin strip;
(2) dealloying the alloy thin strip by using an ammonium salt solution to obtain a dealloyed product;
(3) cleaning and drying the dealloyed product to obtain hexagonal flaky manganese oxide @ nickel oxide composite oxide;
in the step (1), the manganese-nickel-aluminum alloy mother ingot comprises 55-75% of manganese, 17-30% of nickel and 5-25% of aluminum in atomic percentage;
in the step (2), the ammonium salt is selected from ammonium sulfate, ammonium chloride or ammonium nitrate; the concentration of the ammonium salt solution is 0.9-1.2 mol/L;
in the step (2), the mass-to-volume ratio of the alloy thin strip to the ammonium salt solution is 1: 500-600.
2. The method according to claim 1, wherein in the step (1), the manganese-nickel-aluminum alloy mother ingot is prepared by using a pure manganese sheet or a manganese-aluminum alloy as a manganese source, pure nickel or a nickel-aluminum alloy as a nickel source, and pure aluminum as an aluminum source.
3. The preparation method according to claim 2, wherein the mass percentage of aluminum in the manganese-aluminum alloy is 0.5-20.0%, and the balance is manganese and trace impurities; the mass percentage of aluminum in the nickel-aluminum alloy is 2.0-32.5%, and the balance is nickel and trace impurities.
4. The preparation method according to claim 1, wherein in the step (1), the manganese-nickel-aluminum alloy mother ingot is induction-smelted in an argon protective atmosphere with the pressure of 0.5 MPa; the smelting times are 3-5 times.
5. The method according to claim 1, wherein in the step (1), the manganese-nickel-aluminum alloy master ingot is subjected to single-roll rotary quenching to obtain an alloy thin strip; the rotating speed of the roller shaft is 1000-; the thickness of the alloy thin strip is 25-60 mu m, and the width of the alloy thin strip is 2.0-4.0 mm.
6. The production method according to claim 1, wherein in the step (2), the dealloying time is 60min or more; the dealloying temperature is 20-50 ℃.
7. The method according to claim 1, wherein the step (2) further comprises the step of ultrasonically oscillating: shaking with ultrasonic wave once per hour for 10min each time.
8. The manganese oxide @ nickel oxide compound obtained by the preparation method of any one of claims 1 to 7 is characterized in that the structure is that hexagonal flaky manganese oxide is wrapped with a layer of granular nano nickel oxide; the size of the manganese oxide is 0.65-3.15 mu m, and the size of the nickel oxide is 25-270 nm.
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