CN101629314B - Aluminate-metal-aluminum oxide composite material coating and preparation method thereof - Google Patents
Aluminate-metal-aluminum oxide composite material coating and preparation method thereof Download PDFInfo
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- CN101629314B CN101629314B CN2009100556079A CN200910055607A CN101629314B CN 101629314 B CN101629314 B CN 101629314B CN 2009100556079 A CN2009100556079 A CN 2009100556079A CN 200910055607 A CN200910055607 A CN 200910055607A CN 101629314 B CN101629314 B CN 101629314B
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Abstract
The invention relates an aluminate-metal-aluminum oxide composite material coating and a preparation method thereof; the preparation method comprises the following steps: placing aluminum sheet in 480-520 DEG C of air environment to perform annealing treatment so as to eliminate internal stress, then performing defatting treatment and electrochemical surface surfacing treatment in turn; then placing the treated aluminum sheet in dilute phosphoric acid to perform anodic oxidation treatment to form a layer of dense order porous aluminum oxide layer on the surface of the aluminum sheet; adopting the porous aluminum oxide layer as work electrode and graphite plate as cathode to perform electroplating treatment in electroplate liquid and forming aluminate-metal-aluminum oxide composite material on the surface of the porous aluminum oxide layer. The preparation method to the invention can prepare the composite material which is stable at high temperature and has wideband light responsivity through simple processes.
Description
Technical field
What the present invention relates to is coating of a kind of technical field of composite materials and preparation method thereof, specifically is a kind of aluminate-metal-aluminum oxide composite material coating and preparation method thereof.
Background technology
Composition with inorganic materials of wideband photoresponse often is not single, but form by the dielectric medium of undersized metal particle and these metal particles of load.The optical Response of matrix material is mainly by the size of metal particle, and decision distributes.In addition, also be subjected to Temperature Influence.Because at high temperature, the metal particle of these nanometer sizes is easy to be oxidized to oxide compound, thereby has reduced its response characteristics to light.That the spinel aluminate of nanostructure has is high temperature resistant, mechanical resistance is high and characteristics such as hydrophobic nature, has been widely used in fields such as beramic color, coating and catalyzer.Studies show that aluminate is at high temperature protected the not oxidized effect of metal in addition.This mainly is can not form its oxidation state because be in the metal of aluminate among surrounding.The ternary complex that is made of metal, aluminate, the dielectric medium of nano-scale size has unique optical property.The good ionogen of chemical stability provides ideal appendix environment, be in the metal particle of aluminate among surrounding incident light is had very strong absorption, and having good thermostability, the optical Response that whole mixture shows changes not obvious under extreme temperature.
At present, the method of the spinel aluminate crystal of synthetic one-component has: sol-gel method, the solid phase pyroreaction, chemical codeposition etc., a common feature of these methods is the aluminate crystals that at high temperature just can obtain spinel structure, and be difficult to control aluminate/metal ratio, on the angle of energy consumption this process also uneconomical.
Through retrieval, do not find extensive this mixture of synthesizing aluminate-metal-aluminum oxide under the room temperature as yet with special optical character to prior art.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of aluminate-metal-aluminum oxide composite material coating and preparation method thereof is provided, prepare wideband optical Response and at high temperature stable matrix material at normal temperatures by easy steps.
The present invention is achieved by the following technical solutions:
The present invention relates to aluminate-metal-aluminum oxide composite material coating, its component and mass percentage content thereof are: aluminate 33.42%～41.05%, metallic element 10.58%～18.75% and aluminum oxide 42.95%～56%.
Described aluminate layer is a spinel structure, and this aluminate is: a kind of in Leyden blue, cupric aluminate or the Zinc aluminate.
Described metallic element is a kind of in cobalt element, copper or the zinc element.
The present invention relates to the preparation method of above-mentioned aluminate-metal-aluminum oxide composite material coating, may further comprise the steps:
The first step, with aluminium flake with anneal under 480～520 ℃ the air ambient to eliminate internal stress, the processing of carrying out successively subsequently that degrease is handled and electrochemical surface is scraped.
Described degrease is handled and is meant: the aluminium flake after will annealing immerses in the acetone and with ultrasonic 10min under the 60Hz.
Described electrochemical surface polished finish is meant: the one side of aluminium flake is sealed with paraffin, and another side is over against negative electrode, is polished to the surfacing light in volume ratio is ethanol-perchloric acid electrolytic solution of 9: 1, and polishing voltage is 18～20V, and polish temperature is less than 20 ℃.
Second step, the aluminium flake after the surface scraped place dilute phosphoric acid to carry out anodic oxidation treatment, form the fine and close orderly porous alumina layer of one deck on the aluminium flake surface.
Described anodic oxidation treatment is meant: as negative electrode, as anode, control reaction temperature is controlled at 18～20 ℃ with aluminium flake with graphite cake, and anodizing time is 15～20min.
The 3rd step, with porous alumina layer as working electrode, graphite cake carries out electroplating processes as negative electrode in electroplate liquid, form aluminate-metal-aluminum oxide composite material on the surface of porous alumina layer.
The component of described electroplate liquid and volumetric molar concentration thereof are: heavy metallic salt 0.15～0.20mol/L, anhydrous slufuric acid aluminium 0.2～0.25mol/L and anhydrous magnesium sulfate 0.15～0.20mol/L, the pH value of this electroplate liquid is 3～5.
Described heavy metallic salt is meant: copper sulfate, Xiao Suangu or zinc nitrate.
Described electroplating processes is meant: setting voltage 10～13V, and frequency 60～220Hz, temperature is to electroplate under 20～25 ℃ the environment.
The present invention synthesizes the ternary complex film of being made up of metal, aluminate, alumina dielectric medium with significant optical characteristics at normal temperatures.This film not only has very strong wideband optical Response, and it is at high temperature stable, can not only be used for non-focusing formula low temperature luminous energy absorber coatings, also can be used for the focusing absorber coatings of extensive high temperature, luminous energy is converted into heat energy, and then is converted into electric energy, such power generation process is a cleanliness without any pollution, and it is efficient, sustainable.
Description of drawings
Fig. 1 is the luminous reflectance curve comparison diagram of embodiment 1.
Fig. 2 is the XRD comparison diagram of embodiment 1.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
In prepared cupric aluminate/copper/aluminum oxide ternary complex film, cupric aluminate is the spinel phase, and copper is the nano level crystal.The content of cupric aluminate accounts for 36.25%, and the content of copper accounts for 18.75%, and the content of aluminum oxide accounts for 45.00%.
Aluminium flake is annealed in 500 ℃ of following air to eliminate internal stress, and the aluminium flake after will annealing subsequently immerses in the acetone and with ultrasonic 10min under the 60Hz; Carry out the electrochemical surface processing of scraping then: the aluminium flake of being scraped in the surface places the dilute phosphoric acid anodic oxidation, aluminium flake is as anode, graphite cake is as negative electrode, electrolyte temperature is controlled at 19 ± 1 ℃, anodic oxidation voltage is controlled at 15 ± 1V, anodizing time is 15 minutes, promptly forms the porous alumina formwork of one deck densification on the aluminium flake surface.With alumina formwork as working electrode, graphite cake is made counter electrode, at Salzburg vitriol (0.15mol/L), anhydrous slufuric acid aluminium (0.2mol/L), adopt alternating-current to electroplate in anhydrous magnesium sulfate (0.17mol/L) electroplate liquid 40 seconds, electroplating voltage is controlled at 11V, and frequency is at 60Hz, and electroplate liquid pH value is controlled at 3.5.
Embodiment 2
In prepared Leyden blue/cobalt/aluminum oxide ternary complex film, Leyden blue is the spinel phase, and cobalt is the nano level crystal.The content of Leyden blue accounts for 41.05%, and the content of cobalt accounts for 16.00%, and the content of aluminum oxide accounts for 42.95%.
Aluminium flake is annealed in 500 ℃ of following air to eliminate internal stress, and the aluminium flake after will annealing subsequently immerses in the acetone and with ultrasonic 10min under the 60Hz; Carry out the electrochemical surface processing of scraping then: the aluminium flake of being scraped in the surface places the dilute phosphoric acid anodic oxidation, aluminium flake is as anode, graphite cake is as negative electrode, electrolyte temperature is controlled at 19 ± 1 ℃, anodic oxidation voltage is controlled at 15 ± 1V, anodizing time is 15 minutes, promptly forms the porous alumina formwork of one deck densification on the aluminium flake surface.With alumina formwork as working electrode, graphite cake is made counter electrode, at Xiao Suangu (0.2mol/L), anhydrous slufuric acid aluminium (0.25mol/L), adopt alternating-current to electroplate in anhydrous magnesium sulfate (0.15mol/L) electroplate liquid 40 seconds, electroplating voltage is controlled at 13V, frequency is at 200Hz, and electroplate liquid pH value is controlled at 4.
Embodiment 3:
In prepared Zinc aluminate/zinc/aluminum oxide ternary complex film, Zinc aluminate is the spinel phase, and zinc is the nano level crystal.The content of Zinc aluminate accounts for 33.42%, and the content of zinc accounts for 10.58%, and the content of aluminum oxide accounts for 56.00%.
Aluminium flake is annealed in 500 ℃ of following air to eliminate internal stress, and the aluminium flake after will annealing subsequently immerses in the acetone and with ultrasonic 10min under the 60Hz; Carry out the electrochemical surface processing of scraping then: the aluminium flake of being scraped in the surface places the dilute phosphoric acid anodic oxidation, aluminium flake is as anode, graphite cake is as negative electrode, electrolyte temperature is controlled at 19 ± 1 ℃, anodic oxidation voltage is controlled at 15 ± 1V, anodizing time is 20 minutes, promptly forms the porous alumina formwork of one deck densification on the aluminium flake surface.With alumina formwork as working electrode, graphite cake is made counter electrode, at zinc nitrate (0.18mol/L), anhydrous slufuric acid aluminium (0.22mol/L), adopt alternating-current to electroplate in anhydrous magnesium sulfate (0.15mol/L) electroplate liquid 40 seconds, electroplating voltage is controlled at 13V, frequency is at 200Hz, and electroplate liquid pH value is controlled at 4.5.
Claims (5)
1. an aluminate-metal-aluminum oxide composite material coating is characterized in that, component and mass percentage content thereof are: aluminate 33.42%～41.05%, metallic element 10.58%～18.75% and aluminum oxide 42.95%～56%;
Described aluminate layer is a spinel structure, and this aluminate is: a kind of in Leyden blue, cupric aluminate or the Zinc aluminate; Described metallic element is cobalt element, copper or the zinc element of corresponding aluminate.
2. the preparation method of an aluminate-metal-aluminum oxide composite material coating according to claim 1 is characterized in that, may further comprise the steps:
The first step, with aluminium flake with anneal under 480～520 ℃ the air ambient to eliminate internal stress, carry out degrease subsequently successively and handle and the electrochemical surface polished finish;
Second step, place dilute phosphoric acid to carry out anodic oxidation treatment the aluminium flake after the surface finish, form the fine and close orderly porous alumina layer of one deck on aluminium flake surface;
The 3rd step, with porous alumina layer as working electrode, graphite cake carries out electroplating processes as negative electrode in electroplate liquid, form aluminate-metal-aluminum oxide composite material on the surface of porous alumina layer;
The component of described electroplate liquid and volumetric molar concentration thereof are: heavy metallic salt 0.15～0.20mol/L, anhydrous slufuric acid aluminium 0.2～0.25mol/L and anhydrous magnesium sulfate 0.15～0.20mol/L, and the pH value of this electroplate liquid is 3～5;
Described heavy metallic salt is meant: copper sulfate, Xiao Suangu or zinc nitrate;
Described electroplating processes is meant: setting voltage 10～13V, and frequency 60～220Hz, temperature is to electroplate under 20～25 ℃ the environment.
3. the preparation method of aluminate-metal-aluminum oxide composite material coating according to claim 2 is characterized in that, described degrease is handled and is meant: the aluminium flake after will annealing immerses in the acetone and with ultrasonic 10min under the 60Hz.
4. the preparation method of aluminate-metal-aluminum oxide composite material coating according to claim 2, it is characterized in that, described electrochemical surface polished finish is meant: the one side of aluminium flake is sealed with paraffin, another side is over against negative electrode, in being ethanol-perchloric acid electrolytic solution of 9: 1, volume ratio is polished to the surfacing light, polishing voltage is 18～20V, and polish temperature is less than 20 ℃.
5. the preparation method of aluminate-metal-aluminum oxide composite material coating according to claim 2, it is characterized in that described anodic oxidation treatment is meant: with graphite cake as negative electrode, with aluminium flake as anode, control reaction temperature is controlled at 18～20 ℃, and anodizing time is 15～20min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002327292A (en) * | 2001-04-27 | 2002-11-15 | Soken:Kk | Antimold goods and surface treatment method therefor |
| WO2008034471A1 (en) * | 2006-09-22 | 2008-03-27 | Istanbul Teknik Universitesi | Method for the preparation of nanostructures and nanowires |
| CN101319388A (en) * | 2008-05-16 | 2008-12-10 | 昆明理工大学 | Preparation method of multicenter zinc aluminate nanometer pipe |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002327292A (en) * | 2001-04-27 | 2002-11-15 | Soken:Kk | Antimold goods and surface treatment method therefor |
| WO2008034471A1 (en) * | 2006-09-22 | 2008-03-27 | Istanbul Teknik Universitesi | Method for the preparation of nanostructures and nanowires |
| CN101319388A (en) * | 2008-05-16 | 2008-12-10 | 昆明理工大学 | Preparation method of multicenter zinc aluminate nanometer pipe |
Non-Patent Citations (1)
| Title |
|---|
| 李 燕等.Ni、Co /AAO 纳米有序阵列复合结构光吸收特性的比较研究.《光学学报》.2005,第25卷(第1期),77-82. * |
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