CN103646792A - Preparation method for metal / metallic oxide nano-composite materials - Google Patents
Preparation method for metal / metallic oxide nano-composite materials Download PDFInfo
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- CN103646792A CN103646792A CN201310705152.7A CN201310705152A CN103646792A CN 103646792 A CN103646792 A CN 103646792A CN 201310705152 A CN201310705152 A CN 201310705152A CN 103646792 A CN103646792 A CN 103646792A
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Abstract
The invention belongs to the technical field of preparation of nano materials and relates to a preparation method for metal / metallic oxide nano-composite materials. The preparation method for the metal / metallic oxide nano-composite materials is characterized by preparing an oxalic acid solution according to the concentration between 0.01 to 1.5 mole every liter to obtain an electrolyte solution; placing panel metal or foam metal into the prepared electrolyte solution and performing anodic oxidation through a constant pressure method or a current constant method; controlling reaction degrees by controlling reaction conditions such as reaction voltage or current, reaction time, reaction temperature and the like and effectively preparing the metal / metallic oxide nano-composite materials having different shapes, thickness and components in a controllable mode. According to the preparation method for the metal / metallic oxide nano-composite materials, the obtained metal / metallic oxide nano-composite materials comprise the panel or foam state metal substrate and a metallic oxide layer with the thickness between 50 nanometers to 100 micrometers and the metallic oxide which is petal-shaped or grain-shaped with the size between 50 to 500 nanometers is directly formed on the surface of the metal. The preparation method for the metal / metallic oxide nano-composite materials has the advantages of being simple and easy to operate, short in period, strong in adaptability, low in cost and benefited to commercial application.
Description
Technical field
The invention belongs to nano material preparing technical field, relate to a kind of preparation method of metal/metal oxide nano composite material.
Background technology
Metal oxide is as the common electrode material of ultracapacitor, and it has advantages of than the high electric capacity of carbon electrode material and the electrochemical stability higher than macromolecular material.The preparation method of metal oxide is a lot, mainly contains at present electrochemical deposition method, sol-gal process, template and hydro thermal method etc., and operation is comparatively complicated, and experimental implementation is had relatively high expectations and wasted time and energy.In addition,, as a kind of electrode material, metal oxide often need load on metal to support and enhancing conductivity.Common method, a kind of is that the mealy metallic oxide of preparation is coated on foam metal; A kind of is that original position generates on metal.These two kinds of methods, the first lack of homogeneity, loose contact easily cause poor stability, and the second operation is comparatively loaded down with trivial details, wayward.
Hu Junqing, Xu Kaibing etc. have reported that in 2013 a kind of hydro-thermal legal system of using is for the method for electrode material for super capacitor nickel oxide, the method length consuming time, complex steps (Hu Junqing, Xu Kaibing " a kind of preparation method of electrode material for super capacitor nickel oxide " CN201210438935, on January 16th, 2013).The preparation method that Song dynasty's literary composition, pipeline peace etc. were reported a kind of nano nickel oxide composite electrode in 2011, to make by the nano oxidized nickel material of calcined powder shape and a certain amount of metallic element the composite material that slurry obtains, the method needs substep operation, can not go out metal/nickel oxide composite material by one time to produce, and the material made of also will take is afterwards made electrode (Song dynasty's literary composition, pipeline peace " for nano nickel oxide composite electrode of ultracapacitor and preparation method thereof " CN201010265362.5, on January 19th, 2011) by conventional method as active material.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the preparation method of the metal/metal oxide nano composite material of a kind of easy row easy and simple to handle, controlled, wide adaptability is provided.The method has the metal oxide of even structure in dull and stereotyped and the upper directly preparation of foam metal (iron, cobalt, copper, nickel, manganese etc.), can improve the contact of metallic substrates and metal oxide, stability, the conductivity of electrode material have been strengthened, greatly improve the utilance of metal oxide, and the step that simplifies the operation.
The present invention is achieved in the following ways:
A preparation method for metal/metal oxide nano composite material, is characterized in that comprising the following steps:
(1) according to the concentration preparation oxalic acid solution of 0.01～1.5mol/L, make electrolyte;
(2) by flat metal or foam metal, be placed in the prepared electrolyte of step (1), metal used is a kind of in iron, cobalt, copper, nickel, manganese; With constant-voltage method or constant flow method, carry out anodized; The reaction condition of constant-voltage method is: 1～100 volt of reaction potential, 10 seconds～1 hour reaction time, reaction temperature-10～90 degree Celsius; The reaction condition of constant flow method is: kinetic current 10 milliamperes～30 peaces, 10 seconds～1 hour reaction time, reaction temperature-10～90 degree Celsius; Make corresponding metal/metal oxide nano composite material.
The preparation method of above-mentioned a kind of metal/metal oxide nano composite material, it is characterized in that when flat metal or foam metal are nickel, the composite material making in step (2) need to be carried out to annealing in process at 325～400 degrees Celsius, obtain nickel/nickel oxide nano composite material.
The preparation method of above-mentioned a kind of metal/metal oxide nano composite material, is characterized in that the metal/metal oxide nano composite material of preparation comprises that base metal and thickness are the metal oxide layer of 50 nanometer～100 micron; Metal oxide is petal-shaped or graininess, is of a size of 50～500 nanometers; Metal oxide layer is that the oxide of base metal also directly generates in base metal surfaces, and uniform fold is in base metal surfaces.
Embodiment of the present invention are preparation oxalic acid solutions, oxide by anodised method at metal (iron, cobalt, copper, nickel, manganese etc.) Surface Creation metal, by changing the parameters such as the concentration of solution and volume, proportioning and reaction temperature, voltage (electric current), time, electrode spacing, regulate the structure that generates oxide.The thickness of the metal/metal oxide nano composite material that the present invention is prepared is adjustable, structure is controlled, and the conductivity of material, uniformity, stability etc. are all effectively improved.The metal/metal oxide nano composite material of preparation can be applicable to aspects such as preparing transducer, chemical catalysis, lithium ion battery and ultracapacitor.
The present invention has the following advantages:
(1) the metal/metal oxide nano composite material of preparing different-shape, thickness, composition that preparation method of the present invention can be effectively controlled, low, the controlled easy row of the method cost, applied widely, is beneficial to business application;
(2) metal/metal oxide nano composite material of the present invention, do not need binding agent, metal oxide directly generates in metal surface, the feature that has simultaneously possessed metal oxide high-specific surface area and metal high conductivity, the metal oxide obtaining has application at aspects such as transducer, chemical catalysis, lithium ion battery and ultracapacitors.
Embodiment
Provide 21 specific embodiments of the present invention below, but institute of the present invention protection range is not limited to this.
Embodiment 1
A kind of preparation method of nickel foam/nickel oxide nano composite material is as follows:
(1) oxalic acid solution of preparation 0.01mol/L is standby;
(2) by 2 centimetres of 2 cm x, the nickel foam of 2 millimeters thick is placed in (1) described electrolyte, connects wire, and nickel foam is done positive pole, and dull and stereotyped nickel sheet is done negative pole;
(3) under 70 volts of voltages of subzero 5 degrees Celsius of constant potentials, nickel foam is carried out to anodized, react 40 minutes, make nickel foam/bis-oxalic acid hydrate nickel nano composite material.
In resulting materials, two oxalic acid hydrate nickel are block and reunite, on the ligament that is deposited in nickel foam straggly, block diamondwise, the length of side is in 500 nanometers left and right, between block, there is space, on it, have micropore, pore size, in several nanometers, has further increased specific area, these gaps and micropore are that electrolytical diffusion leaves large quantity space, are conducive to the mass transfer in charge and discharge process.
Above-mentioned material is annealed and is obtained nickel foam/nickel oxide nano composite material under 400 degrees Celsius, and nickel oxide shape approaches cauliflower, the bottom surface length of side 200 nanometer left and right, top gathering is connected in nickel foam, on it, have many nanochannels, it is large that space becomes, and is more conducive to the diffusion transport of electrolyte.
Embodiment 2
A kind of preparation method of nickel foam/bis-oxalic acid hydrate nickel nano composite material is as follows:
(1) oxalic acid solution of preparation 0.5mol/L is standby;
(2) by 2 centimetres of 2 cm x, the nickel foam of 2 millimeters thick is placed in (1) described electrolyte, connects wire, and nickel foam is done positive pole, and dull and stereotyped nickel sheet is done negative pole;
(3) under 50 volts of voltages of subzero 10 degrees Celsius of constant potentials, nickel foam is carried out to anodized, react 5 minutes, make nickel foam/bis-oxalic acid hydrate nickel nano composite material.
Embodiment 3
A kind of preparation method of nickel foam/bis-oxalic acid hydrate nickel nano composite material is as follows:
(1) oxalic acid solution of preparation 1.5mol/L is standby;
(2) by 2 centimetres of 2 cm x, the nickel foam of 2 millimeters thick is placed in (1) described electrolyte, connects wire, and nickel foam is done positive pole, and dull and stereotyped nickel sheet is done negative pole;
Under 20 volts of voltages of (3) 30 degrees Celsius of constant potentials, nickel foam is carried out to anodized, react 10 minutes, make nickel foam/bis-oxalic acid hydrate nickel nano composite material.
Embodiment 4
A kind of preparation method of nickel foam/bis-oxalic acid hydrate nickel nano composite material is as follows:
(1) oxalic acid solution of preparation 0.5mol/L is standby;
(2) by 2 centimetres of 2 cm x, the nickel foam of 2 millimeters thick is placed in (1) described electrolyte, connects wire, and nickel foam is done positive pole, and dull and stereotyped nickel sheet is done negative pole;
(3) under subzero 5 degrees Celsius of constant currents, 3 peaces, nickel foam is carried out to anodized, react 10 minutes, make nickel foam/bis-oxalic acid hydrate nickel nano composite material.
Embodiment 5
A kind of preparation method of nickel foam two oxalic acid hydrate nickel nano composite materials is as follows:
(1) oxalic acid solution of preparation 0.1mol/L is standby;
(2) by 2 centimetres of 2 cm x, the nickel foam of 2 millimeters thick is placed in (1) described electrolyte, connects wire, and nickel foam is done positive pole, and dull and stereotyped nickel sheet is done negative pole;
Under 40 volts of voltages of (3) 25 degrees Celsius of constant potentials, nickel foam is carried out to anodized, react 10 minutes, make nickel foam/bis-oxalic acid hydrate nickel nano composite material.
Embodiment 6
A kind of preparation method of dull and stereotyped nickel/bis-oxalic acid hydrate nickel nano composite material is as follows:
(1) oxalic acid solution of preparation 0.05mol/L is standby;
(2) by 2 centimetres of 2 cm x, the dull and stereotyped nickel of 100 micron thickness is placed in (1) described electrolyte, connects wire, and positive and negative pole material is all dull and stereotyped nickel;
(3) under 60 volts of voltages of subzero 5 degrees Celsius of constant potentials, dull and stereotyped nickel is carried out to anodized, react 45 minutes, make dull and stereotyped nickel/bis-oxalic acid hydrate nickel nano composite material.
Embodiment 7
A kind of preparation method of dull and stereotyped nickel/bis-oxalic acid hydrate nickel nano composite material is as follows:
(1) oxalic acid solution of configuration 0.3mol/L is standby;
(2) by 2 centimetres of 2 cm x, the dull and stereotyped nickel of 100 micron thickness is placed in (1) described electrolyte, connects wire, and positive and negative pole material is all dull and stereotyped nickel;
(3) under 40 volts of voltages of subzero 5 degrees Celsius of constant potentials, dull and stereotyped nickel is carried out to anodized, react 20 minutes, make dull and stereotyped nickel/bis-oxalic acid hydrate nickel nano composite material.
Embodiment 8
A kind of preparation method of dull and stereotyped nickel/bis-oxalic acid hydrate nickel nano composite material is as follows:
(1) oxalic acid solution of preparation 1mol/L is standby;
(2) by 2 centimetres of 2 cm x, the dull and stereotyped nickel of 100 micron thickness is placed in (1) described electrolyte, connects wire, and positive and negative pole material is all dull and stereotyped nickel;
(3) under 30 volts of voltages of subzero 5 degrees Celsius of constant potentials, dull and stereotyped nickel is carried out to anodized, react 10 minutes, make dull and stereotyped nickel/bis-oxalic acid hydrate nickel nano composite material.
Embodiment 9
A kind of preparation method of dull and stereotyped nickel/bis-oxalic acid hydrate nickel nano composite material is as follows:
(1) oxalic acid solution of configuration 0.1mol/L is standby;
(2) by 2 centimetres of 2 cm x, the dull and stereotyped nickel of 100 micron thickness is placed in (1) described electrolyte, connects wire, and positive and negative pole material is all dull and stereotyped nickel;
(3) subzero 5 degrees Celsius of constant currents, 5 peaces are carried out anodized to dull and stereotyped nickel, react 10 minutes, make dull and stereotyped nickel/bis-oxalic acid hydrate nickel nano composite material.
Embodiment 10
A kind of preparation method of dull and stereotyped cobalt/cobalt oxide nano composite material is as follows:
(1) oxalic acid solution of configuration 0.3mol/L is standby;
(2) by 2 centimetres of 2 cm x, the dull and stereotyped cobalt of 100 micron thickness is placed in (1) described electrolyte, connects wire, and positive and negative pole material is all dull and stereotyped cobalt;
(3) under 50 volts of voltages of subzero 5 degrees Celsius of constant potentials, dull and stereotyped cobalt is carried out to anodized, react 15 minutes, make dull and stereotyped cobalt/cobalt oxide nano composite material.
Embodiment 11
A kind of preparation method of dull and stereotyped cobalt/cobalt oxide nano composite material is as follows:
(1) oxalic acid solution of configuration 1mol/L is standby;
(2) by 2 centimetres of 2 cm x, the dull and stereotyped cobalt of 100 micron thickness is placed in (1) described electrolyte, connects wire, and positive and negative pole material is all dull and stereotyped cobalt;
Under 40 volts of voltages of (3) 10 degrees Celsius of constant potentials, dull and stereotyped cobalt is carried out to anodized, react 15 minutes, make dull and stereotyped cobalt/cobalt oxide nano composite material.
Embodiment 12
A kind of preparation method of dull and stereotyped cobalt/cobalt oxide nano composite material is as follows:
(1) oxalic acid solution of configuration 1.2mol/L is standby;
(2) by 2 centimetres of 2 cm x, the dull and stereotyped cobalt of 100 micron thickness is placed in (1) described electrolyte, connects wire, and positive and negative pole material is all dull and stereotyped cobalt;
Under (3) 20 degrees Celsius of constant current 2 peaces, dull and stereotyped cobalt is carried out to anodized, react 15 minutes, make dull and stereotyped cobalt/cobalt oxide nano composite material.
Embodiment 13
A preparation method for iron/ferric oxide nano composite material, metal used is iron, all the other are with embodiment 2.
Embodiment 14
A preparation method for iron/ferric oxide nano composite material, metal used is iron, all the other are with embodiment 3.
Embodiment 15
A preparation method for iron/ferric oxide nano composite material, metal used is iron, all the other are with embodiment 4.
Embodiment 16
A preparation method for copper/cupric oxide nano composite material, metal used is copper, all the other are with embodiment 2.
Embodiment 17
A preparation method for copper/cupric oxide nano composite material, metal used is copper, all the other are with embodiment 3.
Embodiment 18
A preparation method for copper/cupric oxide nano composite material, metal used is copper, all the other are with embodiment 4.
Embodiment 19
A preparation method for manganese/manganese oxide nano composite material, metal used is manganese, all the other are with embodiment 2.
Embodiment 20
A preparation method for manganese/manganese oxide nano composite material, metal used is manganese, all the other are with embodiment 3.
Embodiment 21
A preparation method for manganese/manganese oxide nano composite material, metal used is manganese, all the other are with embodiment 4.
Claims (3)
1. a preparation method for metal/metal oxide nano composite material, is characterized in that comprising the following steps:
(1) according to the concentration preparation oxalic acid solution of 0.01～1.5mol/L, make electrolyte;
(2) by flat metal or foam metal, be placed in the prepared electrolyte of step (1), flat metal used or foam metal are a kind of in iron, cobalt, copper, nickel, manganese; With constant-voltage method or constant flow method, carry out anodized; The reaction condition of constant-voltage method is: 1～100 volt of reaction potential, 10 seconds～1 hour reaction time, reaction temperature-10～90 degree Celsius; The reaction condition of constant flow method is: kinetic current 10 milliamperes～30 peaces, 10 seconds～1 hour reaction time, reaction temperature-10～90 degree Celsius; Make corresponding metal/metal oxide nano composite material.
2. the preparation method of a kind of metal/metal oxide nano composite material according to claim 1, it is characterized in that when step (2) middle plateform metal or foam metal are nickel, need again the composite material making in step (2) to be carried out to annealing in process at 325～400 degrees Celsius, obtain nickel/nickel oxide nano composite material.
3. the preparation method of a kind of metal/metal oxide nano composite material according to claim 1 and 2, the metal/metal oxide nano composite material that it is characterized in that preparation comprises that base metal and thickness are the metal oxide layer of 50 nanometer～100 micron; Metal oxide is petal-shaped or graininess, is of a size of 50～500 nanometers; Metal oxide layer is that the oxide of base metal also directly generates in base metal surfaces, and uniform fold is on metal surface.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104120480A (en) * | 2014-08-13 | 2014-10-29 | 南京大学（苏州）高新技术研究院 | Method for preparing nickel oxide buffer layer for high temperature superconducting coated conductors |
| CN105097297A (en) * | 2014-05-08 | 2015-11-25 | 同济大学 | Method for preparing high-activity nano-copper oxide serving as super-capacitor electrode material |
| CN105118691A (en) * | 2015-09-14 | 2015-12-02 | 南京大学 | Foamed nickel-supported cobalt acid ferrous submicron tube electrode material and preparation method thereof |
| CN106531464A (en) * | 2016-11-28 | 2017-03-22 | 东莞市联洲知识产权运营管理有限公司 | Method for manufacturing high-performance symmetric super-capacitor |
| CN113394030A (en) * | 2021-06-26 | 2021-09-14 | 南昌师范学院 | Nickel-based electrode material and preparation method and application thereof |
| US11559791B2 (en) * | 2020-01-22 | 2023-01-24 | The Regents Of The University Of California | Carbon-doped nickel oxide catalyst and methods for making and using thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105097297A (en) * | 2014-05-08 | 2015-11-25 | 同济大学 | Method for preparing high-activity nano-copper oxide serving as super-capacitor electrode material |
| CN105097297B (en) * | 2014-05-08 | 2018-04-03 | 同济大学 | The method for preparing high activity electrode material for super capacitor nano cupric oxide |
| CN104120480A (en) * | 2014-08-13 | 2014-10-29 | 南京大学（苏州）高新技术研究院 | Method for preparing nickel oxide buffer layer for high temperature superconducting coated conductors |
| CN105118691A (en) * | 2015-09-14 | 2015-12-02 | 南京大学 | Foamed nickel-supported cobalt acid ferrous submicron tube electrode material and preparation method thereof |
| CN105118691B (en) * | 2015-09-14 | 2018-01-23 | 南京大学 | Nickel foam supports ferrous sub-micron tube electrode material of cobalt acid and preparation method thereof |
| CN106531464A (en) * | 2016-11-28 | 2017-03-22 | 东莞市联洲知识产权运营管理有限公司 | Method for manufacturing high-performance symmetric super-capacitor |
| CN106531464B (en) * | 2016-11-28 | 2018-10-16 | 东佳电子（郴州）有限公司 | A kind of preparation method of high-performance symmetric form ultracapacitor |
| US11559791B2 (en) * | 2020-01-22 | 2023-01-24 | The Regents Of The University Of California | Carbon-doped nickel oxide catalyst and methods for making and using thereof |
| CN113394030A (en) * | 2021-06-26 | 2021-09-14 | 南昌师范学院 | Nickel-based electrode material and preparation method and application thereof |
| CN113394030B (en) * | 2021-06-26 | 2022-09-09 | 南昌师范学院 | Nickel-based electrode material and preparation method and application thereof |
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