CN107779921A - The preparation method of the compound heat absorbing coating of AAO photonic crystal based high-temp-resistant ternary nanos - Google Patents

The preparation method of the compound heat absorbing coating of AAO photonic crystal based high-temp-resistant ternary nanos Download PDF

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CN107779921A
CN107779921A CN201710914803.1A CN201710914803A CN107779921A CN 107779921 A CN107779921 A CN 107779921A CN 201710914803 A CN201710914803 A CN 201710914803A CN 107779921 A CN107779921 A CN 107779921A
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aao
temp
heat absorbing
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陈东初
魏红阳
常萌蕾
户华文
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Foshan University
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Foshan University
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/18After-treatment, e.g. pore-sealing
    • C25D11/20Electrolytic after-treatment
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys
    • C25D3/562Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt

Abstract

The preparation method of the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano of the present invention, using the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano made from the method, technological operation is relatively simple, coating absorptivity is 0.84~0.94, emissivity has preferable absorption of solar energy 0.12~0.21.Sample coatings are after 100~600 DEG C of heat treatment, coating absorptivity, emissivity are more stable, the compound heat absorbing coating of AAO photonic crystal based high-temp-resistant ternary nanos prepared by the present invention is higher to solar spectrum absorptivity, emissivity is relatively low, and material source is relatively broad, coating binding force is firm, resistance to elevated temperatures is good.The coating material can be with fields such as applied solar energy water heater, solar cooker thermal-arrest, high-temperature power generation, desalinizations.

Description

The preparation method of the compound heat absorbing coating of AAO photonic crystal based high-temp-resistant ternary nanos
Technical field
The present invention relates to the preparation method of the compound heat absorbing coating of AAO photonic crystal based high-temp-resistant ternary nanos, it uses anode Oxidation technology is combined the method for preparing the compound heat absorbing coating of high-temperature resistant nano with AC electrodeposition technology, more particularly to sun Based on the prepared AAO photonic crystals of pole oxidation, the sun is prepared with appropriate electro-deposition parameter and appropriate deposition formula of liquid High-temperature resistant nano composite absorption coating can be absorbed, belongs to solar energy heat absorbing field of material technology.
Background technology
The mode that solar energy directly utilizes is mainly photothermal conversion technology.Photothermal deformation technology is widely used in the sun On energy heat collector, solar energy absorbing coating is the key components of heat collector.At present, the method for solar energy absorbing coating has perhaps It is a variety of, but coating is poor with basal body binding force, easily comes off, and weatherability is poor, easy to aging, and collecting efficiency is low, high temperature heat-resistant stability It is poor.Aluminum alloy materials cost is relatively low, and material source is relatively abundanter, and for solar energy absorbing coating, its surface passes through anode The nano metal ion for aoxidizing high-absorbility in the porous oxide film device to hole of generation has good protective effect, it is therefore prevented that extraneous ring The bad erosion and interference in border.But its solar absorptance is not ideal enough, absorber coatings heat endurance is poor, in hot environment Using ripe not enough.
According to 2010《Solar energy materials and solar cell》94th phase, the reports of page 1578 to 1581, researcher are sharp first Electrochemically being sunk in alumina pore situ and obtain composite nanorod array, the array has good light absorption, but More than 300 DEG C, the coating quality factor is begun to decline its coating temperature later.
According to 2014《Energy Procedia》57th phase, the reports of page 2733 to 2742, researcher is in different alternating currents Pressure and a-c cycle under the conditions of metallic nickel simple substance is deposited into anodic alumina films hole, although its near-infrared 1500nm~ 2500nm nearby but shows higher reflectivity.
At present using anodizing prepare solar energy heat absorbing coating method can not meet simultaneously under higher temperature There is higher absorptivity in the range of solar spectrum, there is relatively low emissivity, and oxide-film in broader infrared range of spectrum Deposited metal particle is more single in hole, and metallic is oxidizable more than 300 DEG C, the high high-temp stability of coating system compared with Difference.
The content of the invention
The purpose of the present invention is the shortcomings that preparing solar energy absorbing coating method for existing anodizing, there is provided AAO The preparation method of the compound heat absorbing coating of photonic crystal based high-temp-resistant ternary nano, material source is relatively broad, coating binding force is firm Gu, solar spectrum absorptivity is higher, infrared emittance low and high temperature better heat stability.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions:
The preparation method of the compound heat absorbing coating of AAO photonic crystal based high-temp-resistant ternary nanos, comprises the following steps:
1) aluminum alloy base material after pre-treatment is put into H2SO4Electrolyte in do the oxidation of periodicity time variant voltage, and negative electrode Plate uses high-purity stereotype;
2) dried up after obtained anodic oxidation template is washed with distilled water, be put into 105g/L H3PO4Exchange and expand in solution Hole is handled;
3) after the anodized aluminum alloy after reaming is washed with distilled water, it is placed in using nickel sulfate, copper sulphate as main salt Deposition liquid in carry out AC electrodeposition.
Further, in step 1), the electrolyte that aluminium alloy carries out anodic oxidation is that mass fraction is 85~110g/L H2SO4 Solution.
Further, in step 1), mainly point 5 stages, its corresponding time parameter are for each periodic voltage change:t1=12 ~60s, t2=12~60s, t3=10~40s, t4=36~90s, t5=128s;t0When=300~2400s is initial oxidation Compensating action is played in section, drift of the initial time period voltage to forbidden photon band in the periodic oxidation stage afterwards.
Further, periodic voltage parameter:U0=U1=U5=1.8~4.2V;U2=6.0~8.5V;U3=3.8~6.2V; U4=2.8~5V;2~25/ DEG C of temperature;Oxidation cycle N=70~120.
Further, in step 2), ac pore-enlarging:It will be provided with the aluminum alloy specimen pure water rinsing of AAO photon crystal structures Totally, after drying, 105g/L H are put into3PO4Ac pore-enlarging, alternating voltage 4V (crest voltage), preimpregnation are carried out in phosphoric acid solution 10s, pore-enlargement are 300~600s, 25 DEG C or so of temperature.
Further, in step 3), the sedimentary condition for carrying out AC electrodeposition is:Voltage 14V (virtual value threshold voltage), deposition 10 DEG C~40 DEG C of time 100s~700s, depositing temperature, a-c cycle 50Hz.
Further, in step 3), electrodeposit liquid composition is:40g~60g/L NiSO4·6H2O, 3~4.5g/L CuSO4·5H2O, 25~30g/L H3BO4(pH=4.0), 10~20g/L MgSO4·7H2O, 1.5~3.5g/LC6H5O7 (NH4)3
Further, in step 1), aluminum alloy specimen pre-treatment:Aluminum alloy specimen is placed on the 45g/L that temperature is 70 DEG C NaOH、1g/L C12H25SO4Alkaline etching 3min in Na mixed solution, the sample after alkaline etching is rinsed well with water and is put into 10% H2SO4, 4%HNO3Pickling 4min in mixed solution, by the test piece after acid with the system that AAO photonic crystals are carried out after ultrapure water It is standby.
Compared with prior art, the beneficial effects of the invention are as follows:
The preparation method of the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano of the present invention, using the method The compound heat absorbing coating of obtained AAO photonic crystals based high-temp-resistant ternary nano, technological operation is relatively simple, and coating absorptivity exists 0.84~0.94, emissivity has preferable absorption of solar energy 0.12~0.21.Sample coatings through 100~600 DEG C heat at After reason, coating absorptivity, emissivity are more stable, the compound suction of AAO photonic crystal based high-temp-resistant ternary nanos prepared by the present invention Hot coating is higher to solar spectrum absorptivity, emissivity is relatively low, and material source is relatively broad, coating binding force is firm, high temperature resistant It is functional.The coating material can be with fields such as applied solar energy water heater, solar cooker thermal-arrest, high-temperature power generation, desalinizations.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, is used to explain the present invention together with embodiments of the present invention, It is not construed as limiting the invention, in the accompanying drawings:
Fig. 1 periodicity time variant voltage aoxidizes legend;
Fig. 2A AO photonic crystal hierarchies SEM schemes;
The schematic diagram of Fig. 3 coating spectral absorption.
Embodiment
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that described herein preferred real Apply example to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Embodiment 1:
(1) aluminum alloy specimen pre-treatment:Aluminum alloy specimen is placed on 45g/L NaOH, the 1g/L that temperature is 70 DEG C C12H25SO4Alkaline etching 3min in Na mixed solution.Sample after alkaline etching is rinsed well with water and is put into 10%H2SO4, 4%HNO3 Pickling 4min in mixed solution, by the test piece after acid with the preparation that AAO photonic crystals are carried out after ultrapure water.
(2) preparation of AAO photonic crystals:Aluminum alloy specimen is put into containing 85g/L H2SO4, electrolyte in do the cycle Property time variant voltage oxidation, and minus plate uses high-purity stereotype.Each periodic voltage change mainly divides 5 stages, its corresponding time ginseng Number is:t1=32s, t2=32s, t3=20s, t4=56s, t5=128s;t0=300s is the initial oxidation period, and the starting stage is electric The drift to forbidden photon band in the periodic oxidation stage afterwards is pressed to play certain compensating action.Periodic voltage parameter:U1= 3.2V;U2=7.0V;U3=5.2V;U4=3.8V;2 DEG C of temperature;Oxidation cycle N=80, Fig. 1 are periodicity time variant voltage oxidation figures Example.
(3) ac pore-enlarging:It is clean to will be provided with the aluminum alloy specimen pure water rinsing of AAO photon crystal structures, after drying, puts Enter 105g/L H3PO4Ac pore-enlarging is carried out in phosphoric acid solution, alternating voltage 4V (crest voltage) presoaks 10s, and pore-enlargement is 300s, 25 DEG C or so of temperature.
(4) AC electrodeposition:AAO photonic crystals aluminum alloy specimen after reaming totally, after drying is put with pure water rinsing Enter to deposit and electro-deposition is carried out in liquid, AC electrodeposition is carried out in using nickel sulfate, copper sulphate as the deposition liquid of main salt, deposit liquid group Turn into:40gg/L NiSO4·6H2O、4g/L CuSO4·5H2O、25/L H3BO4(pH=4.0), 15g/L MgSO4·7H2O、 2g/LC6H5O7(NH4)3.Sedimentary condition:Voltage 14V (virtual value threshold voltage), sedimentation time 100s, 10 DEG C of depositing temperature, exchange Frequency 50Hz.
Fig. 2 is AAO photonic crystal hierarchies SEM figures, obtains the compound heat absorption of AAO photonic crystal based high-temp-resistant ternary nanos Coating absorptivity 0.84, Fig. 3 are the schematic diagrames of coating spectral absorption, emissivity 0.14, quality factor 6.Through 600 DEG C of high temperature of highest 24h is handled, its absorptivity, emissivity fluctuation are smaller.
AAO English full name are:Anodic aluminum oxide, anodised aluminium.
Embodiment 2:
(1) aluminum alloy specimen pre-treatment:Aluminum alloy specimen is placed on 45g/L NaOH, the 1g/L that temperature is 70 DEG C C12H25SO4Alkaline etching 3min in Na mixed solution.Sample after alkaline etching is rinsed well with water and is put into 10%H2SO4, 4%HNO3 Pickling 4min in mixed solution, by the test piece after acid with the preparation that AAO photonic crystals are carried out after ultrapure water.
(2) preparation of AAO photonic crystals:Aluminum alloy specimen is put into containing 100g/L H2SO4, electrolyte in do the cycle Property time variant voltage oxidation, and minus plate uses high-purity stereotype.Each periodic voltage change mainly divides 5 stages, its corresponding time ginseng Number is:t1=36s, t2=32s, t3=25s, t4=70s;t0=800s is initial oxidation stage voltage, starting stage voltage pair Certain compensating action is played in the drift of forbidden photon band in the periodic oxidation stage afterwards.Periodic voltage parameter:U1=2.8V;U2 =7.0V;U3=4.8V;U4=3.8V;5 DEG C of temperature;Oxidation cycle N=70.
(3) ac pore-enlarging:It is clean to will be provided with the aluminum alloy specimen pure water rinsing of AAO photon crystal structures, after drying, puts Enter 105g/L H3PO4Ac pore-enlarging is carried out in phosphoric acid solution, alternating voltage 4V (crest voltage) presoaks 10s, and pore-enlargement is 300s, 25 DEG C or so of temperature.
(4) AC electrodeposition:AAO photonic crystals aluminum alloy specimen after reaming totally, after drying is put with pure water rinsing Enter to deposit and electro-deposition is carried out in liquid, AC electrodeposition is carried out in using nickel sulfate, copper sulphate as the deposition liquid of main salt, deposit liquid group Turn into:50g/L NiSO4·6H2O、3g/L CuSO4·5H2O、30g/L H3BO4(pH=4.0), 10g/L MgSO4·7H2O、 1.5g/LC6H5O7(NH4)3.Sedimentary condition:Voltage 14V (virtual value threshold voltage), sedimentation time 300s, 25 DEG C of depositing temperature, hand over Flow frequency 50Hz.
Obtain the compound heat absorbing coating absorptivity 0.87 of AAO photonic crystal based high-temp-resistant ternary nanos, emissivity 0.16, quality The factor 5.4.Through 600 DEG C of high-temperature process 24h of highest, its absorptivity, emissivity fluctuation are smaller.
Embodiment 3:
(1) aluminum alloy specimen pre-treatment:Aluminum alloy specimen is placed on 45g/L NaOH, the 1g/L that temperature is 70 DEG C C12H25SO4Alkaline etching 3min in Na mixed solution.Sample after alkaline etching is rinsed well with water and is put into 10%H2SO4, 4%HNO3 Pickling 4min in mixed solution, by the test piece after acid with the preparation that AAO photonic crystals are carried out after ultrapure water.
(2) preparation of AAO photonic crystals:Aluminum alloy specimen is put into containing 110g/L H2SO4, electrolyte in do the cycle Property time variant voltage oxidation, and minus plate uses high-purity stereotype.Each periodic voltage change mainly divides 5 stages, its corresponding time ginseng Number is:t1=40s, t2=36s, t3=25s, t4=70s, t5=128s;t0=2400s is the initial oxidation period, initial time period Certain compensating action is played in drift of the voltage to forbidden photon band in the periodic oxidation stage afterwards.Periodic voltage parameter:U1= 3.2V;U2=7.5V;U3=5.2V;U4=4V;8 DEG C of temperature;Oxidation cycle N=90.
(3) ac pore-enlarging:It is clean to will be provided with the aluminum alloy specimen pure water rinsing of AAO photon crystal structures, after drying, puts Enter 105g/L H3PO4Ac pore-enlarging is carried out in phosphoric acid solution, alternating voltage 4V (crest voltage) presoaks 10s, and pore-enlargement is 300s, 25 DEG C or so of temperature.
(4) AC electrodeposition:AAO photonic crystals aluminum alloy specimen after reaming totally, after drying is put with pure water rinsing Enter to deposit and electro-deposition is carried out in liquid, AC electrodeposition is carried out in using nickel sulfate, copper sulphate as the deposition liquid of main salt, deposit liquid group Turn into:60g/L NiSO4·6H2O、4.5g/L CuSO4·5H2O、30g/L H3BO4(pH=4.0), 20g/L MgSO4· 7H2O、3.5g/LC6H5O7(NH4)3.Sedimentary condition:Voltage 14V (virtual value threshold voltage), sedimentation time 700s, depositing temperature 40 DEG C, a-c cycle 50Hz.
Obtain the compound heat absorbing coating absorptivity 0.92 of AAO photonic crystal based high-temp-resistant ternary nanos, emissivity 0.18, quality The factor 5.1.Through 500 DEG C of high-temperature process 24h of highest, its absorptivity, emissivity fluctuation are smaller.
Wherein, modulation of the AAO photonic crystals to infrared spectrum, Cu-Ni nano particles, the CuAl that sedimentary obtains2O4With electricity Medium A l2O3Constitute three-component compound system, CuAl2O4Presence limit under hot environment metallic particles Ni, Cu in interface Diffusion, reduce its oxidized probability.
Embodiment 4:
(1) aluminum alloy specimen pre-treatment:Aluminum alloy specimen is placed on 45g/L NaOH, the 1g/L that temperature is 70 DEG C C12H25SO4Alkaline etching 3min in Na mixed solution.Sample after alkaline etching is rinsed well with water and is put into 10%H2SO4, 4%HNO3 Pickling 4min in mixed solution, by the test piece after acid with the preparation that AAO photonic crystals are carried out after ultrapure water.
(2) preparation of AAO photonic crystals:Aluminum alloy specimen is put into containing 100g/L H2SO4, electrolyte in do the cycle Property time variant voltage oxidation, and minus plate uses high-purity stereotype.Each periodic voltage change mainly divides 5 stages, its corresponding time ginseng Number is:t1=32s, t2=36s, t3=25s, t4=70s, t5=128s;t0=1800s is the initial oxidation period, initial time period Certain compensating action is played in drift of the voltage to forbidden photon band in the periodic oxidation stage afterwards.Periodic voltage parameter:U1= 3.2V;U2=7.0V;U3=4.8V;U4=3.8V;10 DEG C of temperature;Oxidation cycle N=100.
(3) ac pore-enlarging:It is clean to will be provided with the aluminum alloy specimen pure water rinsing of AAO photon crystal structures, after drying, puts Enter 105g/L H3PO4Ac pore-enlarging is carried out in phosphoric acid solution, alternating voltage 4V (crest voltage) presoaks 10s, and pore-enlargement is 300s, 25 DEG C or so of temperature.
(4) AC electrodeposition:AAO photonic crystals aluminum alloy specimen after reaming totally, after drying is put with pure water rinsing Enter to deposit and electro-deposition is carried out in liquid, AC electrodeposition is carried out in using nickel sulfate, copper sulphate as the deposition liquid of main salt, deposit liquid group Turn into:50g/L NiSO4·6H2O、4g/L CuSO4·5H2O、25g/L H3BO4(pH=4.0), 15g/L MgSO4·7H2O、 3g/LC6H5O7(NH4)3.Sedimentary condition:Voltage 14V (virtual value threshold voltage), sedimentation time 300s, 25 DEG C of depositing temperature, exchange Frequency 50Hz.
Obtain the compound heat absorbing coating absorptivity 0.94 of AAO photonic crystal based high-temp-resistant ternary nanos, emissivity 0.17, quality The factor 5.5.Through 500 DEG C of high-temperature process 24h of highest, its absorptivity, emissivity fluctuation are smaller.
Embodiment 5:
(1) aluminum alloy specimen pre-treatment:Aluminum alloy specimen is placed on 45g/L NaOH, the 1g/L that temperature is 70 DEG C C12H25SO4Alkaline etching 3min in Na mixed solution.Sample after alkaline etching is rinsed well with water and is put into 10%H2SO4, 4%HNO3 Pickling 4min in mixed solution, by the test piece after acid with the preparation that AAO photonic crystals are carried out after ultrapure water.
(2) preparation of AAO photonic crystals:Aluminum alloy specimen is put into containing 85~110g/L H2SO4, electrolyte in do Periodicity time variant voltage aoxidizes, and minus plate uses high-purity stereotype.Each periodic voltage change main point 5 stages, its to it is corresponding when Between parameter be:t1=40s, t2=40s, t3=25s, t4=63s, t5=128s;t0=2000s is the initial oxidation period, initially Certain compensating action is played in drift of the period voltage to forbidden photon band in the periodic oxidation stage afterwards.Periodic voltage parameter: U1=2.8V;U2=7.5V;U3=4.8V;U4=4V;15 DEG C of temperature;Oxidation cycle N=110.
(3) ac pore-enlarging:It is clean to will be provided with the aluminum alloy specimen pure water rinsing of AAO photon crystal structures, after drying, puts Enter 105g/L H3PO4Ac pore-enlarging is carried out in phosphoric acid solution, alternating voltage 4V (crest voltage) presoaks 10s, and pore-enlargement is 300s, 25 DEG C or so of temperature.
(4) AC electrodeposition:AAO photonic crystals aluminum alloy specimen after reaming totally, after drying is put with pure water rinsing Enter to deposit and electro-deposition is carried out in liquid, AC electrodeposition is carried out in using nickel sulfate, copper sulphate as the deposition liquid of main salt, deposit liquid group Turn into:60g/L NiSO4·6H2O、3.5g/L CuSO4·5H2O、25/L H3BO4(pH=4.0), 20g/L MgSO4·7H2O、 3.5g/LC6H5O7(NH4)3.Sedimentary condition:Voltage 14V (virtual value threshold voltage), sedimentation time 100s, 40 DEG C of depositing temperature, hand over Flow frequency 50Hz.
Obtain the compound heat absorbing coating absorptivity 0.86 of AAO photonic crystal based high-temp-resistant ternary nanos, emissivity 0.21, quality The factor 4.1.Through 600 DEG C of high-temperature process 24h of highest, its absorptivity, emissivity fluctuation are smaller.
Embodiment 6:
(1) aluminum alloy specimen pre-treatment:Aluminum alloy specimen is placed on 45g/L NaOH, the 1g/L that temperature is 70 DEG C C12H25SO4Alkaline etching 3min in Na mixed solution.Sample after alkaline etching is rinsed well with water and is put into 10%H2SO4, 4%HNO3 Pickling 4min in mixed solution, by the test piece after acid with the preparation that AAO photonic crystals are carried out after ultrapure water.
(2) preparation of AAO photonic crystals:Aluminum alloy specimen is put into containing 100g/L H2SO4, electrolyte in do the cycle Property time variant voltage oxidation, and minus plate uses high-purity stereotype.Each periodic voltage change mainly divides 5 stages, its corresponding time ginseng Number is:t1=36s, t2=40s, t3=25s, t4=70s, t5=128s;t0=2400s is the initial oxidation period, initial time period Certain compensating action is played in drift of the voltage to forbidden photon band in the periodic oxidation stage afterwards.Periodic voltage parameter:U1= 3.2V;U2=7.5V;U3=5.2V;U4=4V;4 DEG C of temperature;Oxidation cycle N=120.
(3) ac pore-enlarging:It is clean to will be provided with the aluminum alloy specimen pure water rinsing of AAO photon crystal structures, after drying, puts Enter 105g/L H3PO4Ac pore-enlarging is carried out in phosphoric acid solution, alternating voltage 4V (crest voltage) presoaks 10s, and pore-enlargement is 300s, 25 DEG C or so of temperature.
(4) AC electrodeposition:AAO photonic crystals aluminum alloy specimen after reaming totally, after drying is put with pure water rinsing Enter to deposit and electro-deposition is carried out in liquid, AC electrodeposition is carried out in using nickel sulfate, copper sulphate as the deposition liquid of main salt, deposit liquid group Turn into:50g/L NiSO4·6H2O、3g/L CuSO4·5H2O、27g/L H3BO4(pH=4.0), 15g/L MgSO4·7H2O、 1.5g/LC6H5O7(NH4)3.Sedimentary condition:Voltage 14V (virtual value threshold voltage), sedimentation time 700s, 10 DEG C of depositing temperature, hand over Flow frequency 50Hz.
Obtain the compound heat absorbing coating absorptivity 0.92 of AAO photonic crystal based high-temp-resistant ternary nanos, emissivity 0.12, quality The factor 7.6.Through 500 DEG C of high-temperature process 24h of highest, its absorptivity, emissivity fluctuation are smaller.
Finally it should be noted that:The preferred embodiments of the present invention are these are only, are not intended to limit the invention, although The present invention is described in detail with reference to embodiment, for those skilled in the art, it still can be to foregoing Technical scheme described in each embodiment is modified, or to which part technical characteristic carry out equivalent substitution, but it is all Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements made etc., the protection of the present invention should be included in Within the scope of.

Claims (8)

  1. The preparation method of the compound heat absorbing coating of 1.AAO photonic crystal based high-temp-resistant ternary nanos, it is characterised in that including following step Suddenly:
    1) aluminum alloy base material after pre-treatment is put into H2SO4Electrolyte in do the oxidation of periodicity time variant voltage, and minus plate is adopted With high-purity stereotype;
    2) dried up after obtained anodic oxidation template is washed with distilled water, be put into 105g/L H3PO4In solution at ac pore-enlarging Reason;
    3) after the anodized aluminum alloy after reaming is washed with distilled water, it is placed in using nickel sulfate, copper sulphate as the heavy of main salt AC electrodeposition is carried out in hydrops.
  2. 2. the preparation method of the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano according to claim 1, it is special Sign is, in step 1), the electrolyte that aluminium alloy carries out anodic oxidation is that mass fraction is 85~110g/L H2SO4Solution.
  3. 3. the preparation method of the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano according to claim 1, it is special Sign is, in step 1), mainly point 5 stages, its corresponding time parameter are for each periodic voltage change:t1=12~60s, t2 =12~60s, t3=10~40s, t4=36~90s, t5=128s;t0=300~2400s is the initial oxidation period.
  4. 4. the preparation method of the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano according to claim 1, it is special Sign is, periodic voltage parameter:U0=U1=U5=1.8~4.2V;U2=6.0~8.5V;U3=3.8~6.2V;U4=2.8~ 5V;2~25/ DEG C of temperature;Oxidation cycle N=70~120.
  5. 5. the preparation method of the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano according to claim 1, it is special Sign is, in step 2), ac pore-enlarging:It is clean to will be provided with the aluminum alloy specimen pure water rinsing of AAO photon crystal structures, dries up Afterwards, 105g/L H are put into3PO4Carrying out ac pore-enlarging in phosphoric acid solution, alternating voltage 4V presoaks 10s, and pore-enlargement is 300~ 600s, 25 DEG C of temperature.
  6. 6. the preparation method of the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano according to claim 1, it is special Sign is, in step 3), the sedimentary condition for carrying out AC electrodeposition is:Voltage 14V, sedimentation time 100s~700s, deposition temperature 10 DEG C~40 DEG C of degree, a-c cycle 50Hz.
  7. 7. the preparation method of the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano according to claim 1, it is special Sign is, in step 3), electrodeposit liquid composition is:40g~60g/L NiSO4·6H2O, 3~4.5g/L CuSO4·5H2O、25 ~30g/L H3BO4(pH=4.0), 10~20g/L MgSO4·7H2O, 1.5~3.5g/LC6H5O7(NH4)3
  8. 8. the preparation method of the compound heat absorbing coating of AAO photonic crystals based high-temp-resistant ternary nano according to claim 1, it is special Sign is, in step 1), aluminum alloy specimen pre-treatment:Aluminum alloy specimen is placed on 45g/L NaOH, the 1g/L that temperature is 70 DEG C C12H25SO4Alkaline etching 3min in Na mixed solution, the sample after alkaline etching is rinsed well with water and is put into 10%H2SO4, 4%HNO3 Pickling 4min in mixed solution, by the test piece after acid with the preparation that AAO photonic crystals are carried out after ultrapure water.
CN201710914803.1A 2017-09-30 2017-09-30 The preparation method of the compound heat absorbing coating of AAO photonic crystal based high-temp-resistant ternary nanos Pending CN107779921A (en)

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