CN101928973A - Aluminum or aluminium alloy oxide precursor anodic oxidation method - Google Patents
Aluminum or aluminium alloy oxide precursor anodic oxidation method Download PDFInfo
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- CN101928973A CN101928973A CN2009100877864A CN200910087786A CN101928973A CN 101928973 A CN101928973 A CN 101928973A CN 2009100877864 A CN2009100877864 A CN 2009100877864A CN 200910087786 A CN200910087786 A CN 200910087786A CN 101928973 A CN101928973 A CN 101928973A
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Abstract
The invention relates to an aluminum or aluminium alloy oxide precursor anodic oxidation method which adopts Ni (NO3)2 solution of rare earth salt for chemical pretreatment to form Ni-Al double-hydroxy metal oxide on the surface of aluminum, and leads a rare earth composite anodic oxidation film to be formed on the surface of aluminum or aluminium alloy through electrochemical anodic oxidation treatment. As the composite anodic oxidation film with rare-earth elements is introduced, the invention has more compact structure, and remarkably improves the surface hardness and the corrosion resistance of the material.
Description
Technical field:
The present invention relates to a kind of aluminum or aluminum alloy oxide precursor anodic oxidation method.
Background technology:
Anodic oxidation is the most frequently used surface treatment means of aluminum or aluminum alloy, can greatly improve the solidity to corrosion of aluminium and aluminium alloy.Aluminium and alloy thereof generate the porous anodized film that thickness can be controlled in acid solution (in sulfuric acid) anodic oxidation.The purpose of anodic oxidation treatment is to improve solidity to corrosion, surperficial contamination resistance, fast light weathering resistance, is crucial sport technique segment.
The introducing of alloying element during anodic oxidation makes aluminum anodized film have the performance of alloy part element, thereby improves the performance of oxide film.In oxide film, introduce titanium, can significantly improve the solidity to corrosion of oxide film, and oxide film is more smooth and fine and close; In oxide film, introduce nickel, can improve the hardness of oxide film; In oxide film, introduce chromium, can improve the solidity to corrosion of oxide film in various corrosive mediums.At present, Many researchers adopts composition metal (to see A.C.Crossland, G.E.Thompson, P.Skeldon, G.C.Wood, C.J.E.Smith, H.Habazaki, K.shimizu, Anodic oxidation of Al-Ce alloys and inhibitive behaviour of cerium species, Corros.Sci., 1998,40 (6): 871-885), sputter (is seen Liu Zhenyu, Gao Wei, Li Meishuan, Cyclic Oxidation of sputter-deposited Nanocrystalline Fe-Cr-Ni-Al Alloy Coatings, Oxidation of Metals, 1999,51 (5/6): 403-419), ion implantationly (see G.K.Wolf, An historical perspective of ion bombardment research for corrosion studies, Surf.Coat.Technol., 1996,83:1-9), sol-gel method (is seen Tammy L.Metroke, Robert L.Parkhill, Edward T.Knobbe, Passivation of metal alloys using sol-gel-derived materials-a review, Prog.in Org.Coat., 2001,41:233-238) etc. method is introduced Ce, Ti, Cr, alloying elements such as Ni, the complex oxide film of formation aluminium and alloy thereof.The introducing of these elements all can improve the solidity to corrosion of oxide film, but above-mentioned anodised pre-treating process is all relatively complicated, and cost is higher, is difficult in and realizes in the industry using.
Development along with industrial technology, common sulphuric acid anodizing technology can not satisfy under the various harsh corrosive environments requirement to oxidation film corrosion resistance, prepare new clad aluminum anode oxide film in conjunction with alloying element, improve its performance and become one of present research focus.Aluminium element itself can and Ni
2+Form the two hydroxy metal oxide compounds (Layered Double Hydroxide is abbreviated as LDH) of Ni-Al of similar water magnesite structure, chemical constitution formula is: [Ni
2+1-xAl
3+X (OH)
2] x+ (An
-) x/nmH
2O, wherein An
-Be interlayer anion; X is Ni
2+/ (Ni
2++ Al
3+) molar ratio; M is the molar weight of middle water molecule.Behind aluminium and alloy surface formation Ni-Al layered di-hydroxyl composite metal oxidate thereof, in anodizing solution, carry out anodic oxidation, can form the Al-Ni composite anode oxide film.But the current report of in the Al-Ni anode oxide film, introducing other the third alloying elements that yet there are no.
Summary of the invention:
The purpose of this invention is to provide a kind of environmental protection, aluminum or aluminum alloy oxide precursor anodic oxidation method cheaply, adopt the Ni (NO that contains rare-earth salts
3)
2Solution carries out chemical pre-treatment, forms the two hydroxy metal oxide compounds of Ni-Al on the aluminium surface, handles making the aluminum or aluminum alloy surface form the rare earth composite anode oxide film again through electrochemical anodic oxidation.
A kind of aluminum or aluminum alloy oxide precursor anodic oxidation method of the present invention is immersed in Ni (NO with aluminum or aluminum alloy
3)
2/ Ce (NO
3)
3Or Ni (NO
3)
2/ Nd (NO
3)
3In the mixing solutions, form the two hydroxy metal oxide precursors of the Ni-Al that contains rare earth element on the aluminium surface, carry out anodic oxidation subsequently again, make the aluminum or aluminum alloy surface form the composite anode oxide film that contains rare earth element ce or Nd, concrete steps are as follows:
A. prepare 65-85g/L Ce (NO
3)
3With 144-198g/L Ni (NO
3)
2Or 75-95g/L Nd (NO
3)
3With 144-198g/LNi (NO
3)
2Mixing solutions, regulating the pH value with yellow soda ash is 8, and the aluminum or aluminum alloy sample of surface through cleaning, oil removing immersed in the solution, solution temperature is heated to 80-95 ℃, and constant temperature is behind the maintenance 1-3h, take out sample and clean and dry up, put into baking oven, 70-80 ℃ keeps 0.5-1h.
B. with sample at 150-200g/LH
2SO
4In the solution, current density 1.5-2A/dm
2, under the condition that temperature is 20 ± 2 ℃, carry out the 30-40min anodic oxidation.
C. for making the anodic oxidation better effects if, also sample can be put into boiling water and seal 30-40min, sealing treatment can stop up the oxide film surface micropore, improves the solidity to corrosion of oxide film.
Above-mentioned anode oxidation method of the present invention is applicable to various aluminum or aluminum alloy, is more suitable for the technical pure anodizing of aluminium.
Characteristics of the present invention are since aluminium element itself can and Ni
2+Form the two hydroxy metal oxide compounds (Layered Double Hydroxide is abbreviated as LDH) of Ni-Al of similar water magnesite structure, chemical constitution formula is: [Ni
2+1-xAl
3+X (OH)
2] x+ (An
-) x/nmH2
O, An wherein
-Be interlayer anion; X is Ni
2+/ (Ni
2++ Al
3+) molar ratio; M is the molar weight of middle water molecule.Behind aluminium or its alloy surface formation Ni-Al layered di-hydroxyl composite metal oxidate, rare earth element ce or Nd enter oxide compound in Al and Ni reaction formation composite oxides; In anodizing solution, carry out anodic oxidation again, can form the Al-Ni composite anode oxide film that contains rare earth.The present invention utilizes These characteristics, at Ni (NO
3)
2Add Ce (NO in the solution
3)
3Or Nd (NO
3)
3Aluminum or aluminum alloy is immersed this solution, make the aluminium surface generate the Al-Ni composite oxides, and rare earth element ce or Nd enter oxide compound in Al and Ni reaction formation composite oxides, form the oxide precursor that contains rare earth element on the aluminium surface, carry out anodic oxidation with proper technical conditions more subsequently, thereby obtain containing the composite anode oxide film of rare earth element ce or Nd.Introduce the composite anode oxide film of rare earth element, its structure is fine and close more, and hardness and erosion resistance all obviously improve.
The various properties of oxide-film parameter comparison of table 1 table
Table 1 is various properties of oxide-film parameter comparison tables, embodiment 1, embodiment 2, embodiment 3 and embodiment 4 usefulness KEVEX Sigma can spectrum testing systems (EDXA) be measured the content of various elements in the metal oxide that the aluminium surface after the pre-treatment forms, and the result proves in the aluminum anodized film of formation and contains Ni, Ce or Ni, Nd.Antianode oxide film microhardness (HV) test result illustrates that the oxide film hardness after the inventive method is handled obviously improves, and wherein the modified oxidized film hardness of Ce is the highest, the 81Kg/mm when unmodified
2, bring up to 146Kg/mm
2, the hardness of oxide film is higher after the sealing.Therefore, the rare earth modified anode oxide film of the present invention has higher microhardness and better wearability than sulphuric acid oxidation coating.
Advantage of the present invention:
(1) processing method is simple, and process stabilizing does not need complex apparatus, and processing ease is identical with the common anode oxidation unit.
(2) composite anode oxide film of rare-earth element cerium or neodymium modification, the aperture significantly diminishes, and pore space structure is fine and close more, sees Fig. 2.
(3) corrosion resistance excellent significantly improves with respect to the sulphuric acid oxidation coating solidity to corrosion, sees Fig. 4, Fig. 5, Fig. 6, Fig. 7.
(4) hardness improves.
Description of drawings:
Fig. 1 anodic oxidation device synoptic diagram of the present invention
Fig. 2 anode oxide film surface topography scanning electronic microscope (SEM) figure
A is the microvoid structure (Comparative Examples 1) on the original oxide film surface of non-modified among Fig. 2, b only soaks the oxide film pore space structure (Comparative Examples 2) that anodic oxidation again obtains through nickel nitrate solution, c soaks the oxide film pore space structure (embodiment 1) that the back obtains in anodic oxidation through nickelous nitrate+cerous nitrate solution, and d is the oxide film pore space structure (embodiment 2) that obtains in anodic oxidation after nickelous nitrate+neodymium nitrate solution soaking.
Fig. 3 is the polarization curve of oxide film in neutral 3.5%NaCl solution
A is the polarization curve of original oxide film (Comparative Examples 1) among Fig. 3, and b is through Ni (NO
3)
2The polarization curve of pre-treatment (Comparative Examples 2), c is through Nd (NO
3)
3+ Ni (NO
3)
2The polarization curve of pre-treatment (embodiment 1), d is through Ce (NO
3)
3+ Ni (NO
3)
2The polarization curve of pre-treatment (embodiment 2).
Fig. 4 seals the polarization curve of oxide film in neutral 3.5%NaCl solution,
A is the polarization curve that compound rare-earth salt seals original oxide film (Comparative Examples 3) among Fig. 4, and b is boiling water sealing Ni (NO
3)
2The polarization curve of pre-treatment (Comparative Examples 4), c are boiling water sealing Nd (NO
3)
3+ Ni (NO
3)
2The polarization curve of pre-treatment (embodiment 3), d are boiling water sealing Ce (NO
3)
3+ Ni (NO
3)
2The polarization curve of pre-treatment (embodiment 4).
The polarization curve of Fig. 5 oxide film in acid 3.5%NaCl solution (pH2)
A is the polarization curve of original oxide film (Comparative Examples 1) among Fig. 5, and b is through Ni (NO
3)
2The polarization curve of pre-treatment (Comparative Examples 2), c is through Nd (NO
3)
3+ Ni (NO
3)
2The polarization curve of pre-treatment (embodiment 1), d is through Ce (NO
3)
3+ Ni (NO
3)
2The polarization curve of pre-treatment (embodiment 2).
The polarization curve of Fig. 6 oxide film in alkaline 3.5%NaCl solution (pH12)
A is the polarization curve of original oxide film (Comparative Examples 1) among Fig. 6, and b is through Ni (NO
3)
2The polarization curve of pre-treatment (Comparative Examples 2), c is through Nd (NO
3)
3+ Ni (NO
3)
2The polarization curve of pre-treatment (embodiment 1), d is through Ce (NO
3)
3+ Ni (NO
3)
2The polarization curve of pre-treatment (embodiment 2).
From Fig. 3, Fig. 5, Fig. 6 as can be seen, no matter in neutral, acidity or alkaline sodium chloride solution, the anodic polarization electric current of rare earth modified oxide film is all obviously lower, and particularly the modified oxidized membrane current of Ce is minimum, hangs down one more than the order of magnitude than unmodified oxide film.
Fig. 4 is that the original oxide film and the boiling water of compound rare-earth sealing seals the polarization curve of three kinds of rare earth modified anode oxide films in 3.5%NaCl solution later on, can find among the figure, anodic current density through oxide film after the sealing reduces, the original oxide film of anodizing current density ratio of two kinds of rare earth modified oxide films and not add the oxide film of rare earth pre-treatment little, the anodic current density minimum of cerium modified oxide film wherein, the solidity to corrosion that it is described is best, secondly is the modified oxidized film of neodymium.
The alternating-current impedance figure of Fig. 7 oxide film in neutral 3.5%NaCl solution
■ represents the alternating-current impedance figure of original oxide film (Comparative Examples 1) among Fig. 7, and zero expression is through Ni (NO
3)
2The alternating-current impedance figure of pre-treatment (Comparative Examples 2), ▲ expression is through Nd (NO
3)
3+ Ni (NO
3)
2The alternating-current impedance figure of pre-treatment (embodiment 1), represents the (NO through Ce
3)
3+ Ni (NO
3)
2The alternating-current impedance figure of pre-treatment (embodiment 2).
Fig. 8 seals the alternating-current impedance figure of oxide film in neutral 3.5%NaCl solution
■ represents that compound rare-earth salt seals the alternating-current impedance figure of original oxide film (Comparative Examples 3) among Fig. 8, and O represents boiling water sealing Ni (NO
3)
2The alternating-current impedance figure of pre-treatment (Comparative Examples 4), ▲ expression boiling water sealing Nd (NO
3)
3+ Ni (NO
3)
2The alternating-current impedance figure of pre-treatment (embodiment 3), represent the (NO through boiling water sealing Ce
3)
3+ Ni (NO
3)
2Pre-treatment (embodiment 4).
No matter whether oxide film passes through sealing treatment as can be seen from Fig. 7 and Fig. 8, the resistance value that method of the present invention is handled back gained anode oxide film is significantly improved than untreated, illustrates that rare earth modified oxide film has better solidity to corrosion.
Generally speaking, from above-mentioned accompanying drawing, pass through as can be seen rare earth modified after, contain Rare-Earth Ce and Nd in the oxide film for preparing; The porosity of rare earth modified oxide film reduces, and microhardness increases; Do not seal and seal oxide film at neutral (pH7), in acid (pH2) and alkalescence (pH12) 3.5%NaCl solution, the modified oxidized film of Ce has best solidity to corrosion, next is the modified oxidized film of Nd, the enclosure method of contrast compound rare-earth salt, the oxidation film corrosion resistance that the inventive method obtains obviously is better than compound rare-earth salt sealing oxide film; Through after rare earth modified, the impedance that has improved aluminum anodized film blocking layer and porous layer.
Embodiment:
Comparative Examples 1
1.1 commercial-purity aluminium L2 specimen surface arrives the 800# liquid honing with 300# successively, acetone degreasing degreasing, sodium hydroxide alkalescence electrochemical deoiling, salpeter solution bright dipping.
1.2 anodic oxidation, condition is: 200g/L H
2SO
4Solution, current density 1.5A/dm
2, 20 ± 2 ℃ of temperature, oxidization time 30min; The washing of taking-up sample, cold wind dries up.
Comparative Examples 2
2.1 commercial-purity aluminium L2 specimen surface arrives the 800# liquid honing with 300# successively, acetone degreasing degreasing, sodium hydroxide alkalescence electrochemical deoiling, salpeter solution bright dipping.
2.2 preparation 180g/L Ni (NO
3)
2Solution, regulating the pH value with yellow soda ash is 8.Reagent is all used chemical purity.
2.3 open the constant temperature oil bath switch, solution temperature be heated to 90 ℃, constant temperature.
2.4 solution is put into, reaction times 1h through the aluminium sample of cleaning, oil removing in the surface.
2.5 finishing the back, reaction takes out sample, washing, and cold wind dries up, and is placed in the baking oven, and 80 ℃ keep 1h.
2.6 anodic oxidation, condition is: 200g/L H
2SO
4Solution, current density 1.5A/dm
2, 20 ± 2 ℃ of temperature, oxidization time 30min; The washing of taking-up sample, cold wind dries up.
Comparative Examples 3
3.1 commercial-purity aluminium L2 specimen surface arrives the 800# liquid honing with 300# successively, acetone degreasing degreasing, sodium hydroxide alkalescence electrochemical deoiling, salpeter solution bright dipping.
3.2 anodic oxidation, condition is: 200g/L H
2SO
4Solution, current density 1.5A/dm
2, 20 ± 2 ℃ of temperature, oxidization time 30min; The washing of taking-up sample, cold wind dries up.
3.3 the sample that anodic oxidation is good is put into 90 ℃ of saturated Nd
2(CO
3)
3+ La
2(CO
3)
330 minutes (seeing ZL200410074541.5) of sealing takes out sample in the aqueous solution, and cold wind dries up to be deposited.
Comparative Examples 4
4.1 commercial-purity aluminium L2 specimen surface arrives the 800# liquid honing with 300# successively, acetone degreasing degreasing, sodium hydroxide alkalescence electrochemical deoiling, salpeter solution bright dipping.
4.2 preparation 180g/L Ni (NO
3)
2Solution, regulating the pH value with yellow soda ash is 8.Reagent is all used chemical purity.
4.3 open the constant temperature oil bath switch, solution temperature be heated to 90 ℃, constant temperature.
4.4 solution is put into, reaction times 1h through the aluminium sample of cleaning, oil removing in the surface.
4.5 finishing the back, reaction takes out sample, washing, and cold wind dries up, and is placed in the baking oven, and 80 ℃ keep 1h.
4.6 anodic oxidation, condition is: 200g/L H
2SO
4Solution, current density 1.5A/dm
2, 20 ± 2 ℃ of temperature, oxidization time 30min; The washing of taking-up sample, cold wind dries up.
4.7 the sample that anodic oxidation is good is put into boiling water sealing 30 minutes, takes out sample, cold wind dries up to be deposited.
1 commercial-purity aluminium L2 specimen surface arrives the 800# liquid honing with 300# successively, acetone degreasing degreasing, sodium hydroxide alkalescence electrochemical deoiling, salpeter solution bright dipping.
2 preparation 85g/L Nd (NO
3)
3+ 180g/L Ni (NO
3)
2Solution, regulating the pH value with yellow soda ash is 8.Reagent is all used chemical purity.
3 open the constant temperature oil bath switch, solution temperature are heated to 90 ℃, constant temperature.
4 with the surface through the cleaning, oil removing the aluminium sample put into solution, reaction times 1h.
5 reactions finish the back and take out sample, washing, and cold wind dries up, and is placed in the baking oven, and 80 ℃ keep 1h.
6 anodic oxidations, condition is: 200g/L H
2SO
4Solution, current density 1.5A/dm
2, 20 ± 2 ℃ of temperature, oxidization time 30min; The washing of taking-up sample, cold wind dries up.
1 commercial-purity aluminium L2 specimen surface arrives the 800# liquid honing with 300# successively, acetone degreasing degreasing, sodium hydroxide alkalescence electrochemical deoiling, salpeter solution bright dipping.
2 preparation 75g/L Ce (NO
3)
3+ 180g/L Ni (NO
3)
2Solution, regulating the pH value with yellow soda ash is 8.Reagent is all used chemical purity.
3 open the constant temperature oil bath switch, solution temperature are heated to 90 ℃, constant temperature.
4 with the surface through the cleaning, oil removing the aluminium sample put into solution, reaction times 1h.
5 reactions finish the back and take out sample, washing, and cold wind dries up, and is placed in the baking oven, and 80 ℃ keep 1h.
6 anodic oxidations, condition is: 200g/L H
2SO
4Solution, current density 1.5A/dm
2, 20 ± 2 ℃ of temperature, oxidization time 30min; The washing of taking-up sample, cold wind dries up.
1 commercial-purity aluminium L2 specimen surface arrives the 800# liquid honing with 300# successively, acetone degreasing degreasing, sodium hydroxide alkalescence electrochemical deoiling, salpeter solution bright dipping.
2 preparation 95g/L Nd (NO
3)
3+ 180g/L Ni (NO
3)
2Solution, regulating the pH value with yellow soda ash is 8.Reagent is all used chemical purity.
3 open the constant temperature oil bath switch, solution temperature are heated to 80 ℃, constant temperature.
4 with the surface through the cleaning, oil removing the aluminium sample put into solution, reaction times 3h.
5 reactions finish the back and take out sample, washing, and cold wind dries up, and is placed in the baking oven, and 70 ℃ keep 0.5h.
6 anodic oxidations, condition is: 150g/LH
2SO
4Solution, current density 2A/dm
2, 20 ± 2 ℃ of temperature, oxidization time 30min; The washing of taking-up sample, cold wind dries up.
7 samples that anodic oxidation is good are put into boiling water sealing 30 minutes, take out sample, and cold wind dries up to be deposited.
1 commercial-purity aluminium L2 specimen surface arrives the 800# liquid honing with 300# successively, acetone degreasing degreasing, sodium hydroxide alkalescence electrochemical deoiling, salpeter solution bright dipping.
2 preparation 85g/L Ce (NO
3)
3+ 180g/LNi (NO
3)
2Solution, regulating the pH value with yellow soda ash is 8.Reagent is all used chemical purity.
3 open the constant temperature oil bath switch, solution temperature are heated to 95 ℃, constant temperature.
4 with the surface through the cleaning, oil removing the aluminium sample put into solution, reaction times 3h.
5 reactions finish the back and take out sample, washing, and cold wind dries up, and is placed in the baking oven, and 80 ℃ keep 0.5h.
6 anodic oxidations, condition is: 150g/L H
2SO
4Solution, current density 2A/dm
2, 20 ± 2 ℃ of temperature, oxidization time 30min; The washing of taking-up sample, cold wind dries up.
7 samples that anodic oxidation is good are put into boiling water sealing 30 minutes, take out sample, and cold wind dries up to be deposited.
Claims (4)
1. aluminum or aluminum alloy oxide precursor anodic oxidation method: aluminum or aluminum alloy is immersed in Ni (NO
3)
2/ Ce (NO
3)
3Or Ni (NO
3)
2/ Nd (NO
3)
3In the mixing solutions, form the two hydroxy metal oxide precursors of the Ni-Al that contains rare earth element, carry out anodic oxidation subsequently again, make the aluminum or aluminum alloy surface form the composite anode oxide film that contains rare earth element ce or Nd on the aluminium surface.
2. according to the anode oxidation method of claim 1, it is characterized in that: concrete steps are as follows:
A. prepare 65-85g/L Ce (NO
3)
3With 144-198g/L Ni (NO
3)
2Or 75-95g/L Nd (NO
3)
3With 144-198g/L Ni (NO
3)
2Mixing solutions, regulating the pH value is 8; The aluminum or aluminum alloy sample of surface through cleaning, oil removing immersed in the mixing solutions, solution temperature is heated to 80-95 ℃, constant temperature keeps 1-3h, takes out sample and cleans and dry up, and puts into baking oven, and 70-80 ℃ keeps 0.5-1h;
B. with sample at 150-200g/LH
2SO4 solution, current density 1.5-2A/dm
2, under the condition that temperature is 20 ± 2 ℃, carry out the 30-40min anodic oxidation.
3. according to the anode oxidation method of claim 2, it is characterized in that: after the anodic oxidation of step B, sample is put into boiling water seal 30-40min.
4. according to the anode oxidation method of claim 1 or 2 or 3, it is characterized in that: said aluminium is commercial-purity aluminium.
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|---|---|---|---|
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|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107904646A (en) * | 2017-11-15 | 2018-04-13 | 北京半导体专用设备研究所（中国电子科技集团公司第四十五研究所） | A kind of processing method of CMP tool carrier-table surface |
-
2009
- 2009-06-26 CN CN2009100877864A patent/CN101928973A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107904646A (en) * | 2017-11-15 | 2018-04-13 | 北京半导体专用设备研究所（中国电子科技集团公司第四十五研究所） | A kind of processing method of CMP tool carrier-table surface |
| CN107904646B (en) * | 2017-11-15 | 2019-04-12 | 北京半导体专用设备研究所（中国电子科技集团公司第四十五研究所） | A kind of processing method of CMP tool carrier-table surface |
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Open date: 20101229 |