CN1560328A - Preparation process for anode oxidation thick film of aluminium copper alloy - Google Patents
Preparation process for anode oxidation thick film of aluminium copper alloy Download PDFInfo
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- CN1560328A CN1560328A CNA2004100168600A CN200410016860A CN1560328A CN 1560328 A CN1560328 A CN 1560328A CN A2004100168600 A CNA2004100168600 A CN A2004100168600A CN 200410016860 A CN200410016860 A CN 200410016860A CN 1560328 A CN1560328 A CN 1560328A
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- anodic oxidation
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Abstract
The invention is a high Cu-Al alloy anodic oxidized thick membrane preparing process, adopting low-concentration compound electrolyte, stage by stage raising the pressure to make the electrolyte maintain larger current density, rapidly forming a thicker membrane layer on the surface of Cu-Al alloy in a short time, then reducing the current density to slow down the membrane layer growth, finally reaching a certain thickness, and generating an anodic oxidized thick membrane with silvery glaze gloss. The concentration of anodic oxidizing solution phosphatic acid is 0.5%-1%; the added organic acid is oxalic or citric acid and the corresponding concentration is 0.1%-0.5%; and the added rare-earth salt is cerium or lanthanum sulphate, and the corresponding concentration is 0.05%-0.2%; washing the sample in a 60g/L, 70 deg.C NaOH basic solution for 3 min to eliminate the grease; the surface area ratio of cathode to anode in anodic oxidation is controlled at 2 : 1-1 : 2, and the cathode is Pb plate; placing the sample in a drying box for drying at 120 deg.C for 30 min. It breaks through the limitation of making only at low temperature and in high-concentration electrolyte, and shortens oxidizing time and the membrane has good ornamentality.
Description
Technical field
The present invention relates to a kind of aluminum-copper alloy anodic oxidation thick film new preparation process, grading voltage prepares high-copper aluminium alloy anode oxide thick-film technique fast under particularly a kind of lower concentration composite electrolytic solution, the high temperature, is used for aluminum alloy surface decorative and protective Application Areas.
Background technology
The anodic oxidation that contains X alloy is a surface-treated difficult problem, especially cupric＞4% (massfraction) always, CuAl in oxidising process
2Phased soln is very fast, usually becomes electric current accumulative center, and the rete that makes this position easily is overheated and dissolve, and punctures and burns part.This alloy anode oxidation at present mainly improves from two aspects, and the one, improve electrolyte prescription and operating procedure, the 2nd, the electric current output form of change power supply.Aforesaid way has improved the oxidation susceptibility of X alloy really to a certain extent, yet, the oxidation liquid of aluminum current copper alloy mainly is based on sulfuric acid, add the additive that some improve film quality, as oxalic acid, glycerine etc., concentration of electrolyte higher (sulfuric acid concentration general 15%～20%), the liquid waste disposal difficulty is big, to serious environment pollution.
In addition, in order to obtain thicker rete, electrolyte temperature is lower, generally is no more than 20 ℃, needs to lower the temperature with refrigerating apparatus in oxidising process; The change of supply current form can be alleviated aluminum-copper alloy excessive dissolution and heat release problem to a certain extent, the thick film that obtained performance is good, but required power unit complexity, and cost is higher.
Find " electroplating and environmental protection " 2001:21 (4) by literature search: published the article " electrochemical deposition of the nonmetal rete of neutral medium aluminium surface inorganic " that people such as spacious Asia and Africa introduce inorganic non-metallic rete preparation technology on 20～24.People such as spacious Asia and Africa adopt high voltage and than high current density in phosphoric acid and sodium wolframate electrolytic solution, made the grey based ceramic film that thick 30 μ m, hardness reach 500HV on the common aluminum alloy surface; Hou Chaohui etc. also make 10～30 μ m in neutral mixed system, hardness reaches the ornamental grey based ceramic film of being rich in of 500～600HV layer.But above-mentioned research system (＞4%) when copper content reaches certain value in the aluminum-copper alloy adopts anode oxidation process aluminum bronze surface to cause that very easily efflorescence burns phenomenon.And the rete color that above-mentioned technology makes is grey or black, has limited the decorative applications of aluminum-copper alloy to a certain extent.
Summary of the invention
The present invention is directed to the deficiency that exists in the above-mentioned technology, a kind of lower concentration composite electrolytic solution high temperature aluminum-copper alloy anodic oxidation fast thick film preparation is provided, make it adopt novel lower concentration composite electrolytic solution, grading voltage under comparatively high temps, prepare the anodic oxidation thick film of silvery white glaze colours in the big high-copper aluminum alloy surface of oxidisability difficulty, the high X alloy thick-film technique that has broken through preparation can only be at low temperature, the restriction of carrying out under the high density electrolytic solution, improve and broadening the anodic oxidation temperature, shortened oxidization time, reduced the hazard rating of electrolytic solution to environment, widened the ornamental range of application of high X alloy, suitable industry is applied.
The present invention is achieved by the following technical solutions.The present invention is in anode oxidation process, adopt the lower concentration composite electrolytic solution, grading voltage makes it to keep than high current density under comparatively high temps, aluminum-copper alloy forms thicker rete rapidly in the short period of time of surface, current density descends gradually subsequently, coating growth speed is slowed down, and finally reaches a constant thickness, generates to have silvery white glaze colours glossy anodic oxidation thick film.Processing step is as follows:
(1) preparation anodic oxidation solution.
The anodizing solution that the present invention adopts is the combined oxidation liquid of phosphoric acid, organic acid and rare-earth salts.Phosphoric acid anodizing liquid can generate complete, translucent pellumina in aluminum alloy surface.The interpolation organic acid can relax the acidity of phosphoric acid, reduces the dissolution rate of aluminum anodized film, helps generating thicker rete, does not add organic acid, and then the rete of Sheng Chenging is thinner.The adding of an amount of rare-earth salts can be played even rete, accelerate the effect of anodically deposit speed.
The anodizing solution concentration of phosphoric acid scope that the present invention adopts is 0.5%～1%, and the organic acid of interpolation is oxalic acid or citric acid, and its concentration range is 0.1%～0.5%, and the rare-earth salts of interpolation is cerous sulfate or lanthanum sulfat, and concentration range is 0.05%～0.2%.
(2) Chemical Pretreatment
At 60g/L, clean the grease that 3min removes sample in 70 ℃ of NaOH alkali solution.
(3) anode oxidation process
Anodic oxidation cathode and anode surface area ratio is controlled between 2: 1～1: 2, and what negative electrode adopted is stereotype.Oxidation voltage is one of anodised significant parameter, and the present invention adopts the grading voltage method, and boosting fast the fs, (30s～2min, magnitude of voltage 80～120V) make current density reach 7～15A/dm rapidly
2, keeping constant voltage 1min～3min, this moment, current density descended rapidly.And then (140～180V), the lowering speed of reduction current density makes it rete and keeps the fast speed growth to improve oxidation voltage.In anodised process, the formation and the performance impact of the temperature antianode oxide film of electrolytic solution are little, and the electrolyte temperature in the anode oxidation process can be controlled in 20 ℃～50 ℃.Owing to adopted the high-voltage great-current oxidation style, the required oxidization time of this technology is shorter, only needs 10～30min.Overlong time is nonsensical to the thickness of further increase oxide film.
(4) drying
Sample is placed in the loft drier at 120 ℃ of following dry 30min.
Adopt the high-copper aluminium alloy anode oxide aluminium film thickness of the present invention's preparation can reach 15～40 microns, hardness 300～400HV, rete color silvery white glaze colours has satisfied the requirement of aluminum alloy surface protected decoration aspect.Compared with prior art, the present invention has broken through the restriction that the high X alloy thick-film technique of preparation can only be carried out under low temperature, high density electrolytic solution, overcome high voltage electric chemical ceramics film technique rete ornamental poor, be difficult to film forming shortcoming at high X alloy.Anode oxidation process of the present invention can at high temperature carry out, and needn't use cooled compressed equipment; The growth of aluminum oxide rete is insensitive to variation of temperature in the oxidising process, needn't carry out temperature control in the oxidising process.Concentration of electrolyte is lower, can reduce the pollution to environment greatly, and to alloying constituent require lowly, can on various aluminas, use, the rete color is silvery white glaze colours, has strengthened the decorate properties of rete greatly.
Embodiment
The present invention adopts the lower concentration composite electrolytic solution, and at high temperature grading voltage prepares high-copper aluminium alloy anode oxide thick film.The electrolytic solution total concn is (0.65～1.7%), and required oxidation voltage is fs: 80～120V, keeps constant voltage 1min～3min, rate of rise 30s～2min; Subordinate phase: 140～180V keeps constant voltage to anode oxidation to finish.Oxidizing temperature can reach 50 ℃.Anodizing time is 10min～30min.The thickness of gained anode oxide film can reach 15～40 microns.
Embodiment 1: the composite electrolytic solution parameter of preparation is: phosphatase 11 %, oxalic acid 0.5%, lanthanum sulfat 0.05%.At 60g/L, carry out anodic oxidation behind the cleaning 3min in 70 ℃ of NaOH alkali solution.Fs oxidation voltage 80V, rate of rise 2min.After keeping constant voltage 3min, boost to 140V again, keep constant.Oxidization time 30min.Be placed on 120 ℃ of following dry 30min in the loft drier then.In the process of test, the temperature of solution is 20 ℃～30 ℃ variations.After the anodic oxidation, thickness is 15 μ m, the rete silvery white.
Embodiment 2: the composite electrolytic solution parameter of preparation is: phosphoric acid 0.5%, citric acid 0.5%, cerous sulfate 0.1%.At 60g/L, anodic oxidation behind the cleaning 3min in 70 ℃ of NaOH alkali solution.Fs oxidation voltage 110V, rate of rise 1min keeps boosting to 170V again behind the constant voltage 2min, keeps constant.Oxidization time 10min.Be placed on 120 ℃ of following dry 30min in the loft drier then.In the process of the test, the temperature of solution is 30 ℃～40 ℃ variations.After the anodic oxidation, the thickness of oxide film is 40 μ m, and rete is silvery white glaze colours.
Embodiment 3: the composite electrolytic solution parameter of preparation is: phosphoric acid 0.5%, citric acid 0.3%, cerous sulfate 0.2%.At 60g/L, anodic oxidation behind the cleaning 3min in 70 ℃ of NaOH alkali solution.Fs oxidation voltage 120V, rate of rise 30s keeps boosting to 180V again behind the constant voltage 1min, keeps constant.Oxidization time 15min.Be placed on 120 ℃ of following dry 30min in the loft drier then.In the process of the test, 40 ℃～50 ℃ of the temperature of solution.After the anodic oxidation, the thickness of oxide film is 25 μ m, and rete is silvery white glaze colours.
Claims (6)
1, a kind of aluminum-copper alloy anodic oxidation thick film preparation, it is characterized in that, in anode oxidation process, adopt the lower concentration composite electrolytic solution, grading voltage makes it to keep than high current density, and aluminum-copper alloy forms thicker rete rapidly in the short period of time of surface, current density descends gradually subsequently, coating growth speed is slowed down, and finally reaches a constant thickness, generates to have silvery white glaze colours glossy anodic oxidation thick film.
2, aluminum-copper alloy anodic oxidation thick film preparation according to claim 1 is characterized in that, below the present invention is further limited, and concrete steps are:
(1) preparation anodic oxidation solution
Anodizing solution concentration of phosphoric acid scope is 0.5%～1%, and the organic acid of interpolation is oxalic acid or citric acid, and its concentration range is 0.1%～0.5%, and the rare-earth salts of interpolation is cerous sulfate or lanthanum sulfat, and concentration range is 0.05%～0.2%;
(2) Chemical Pretreatment
At 60g/L, clean the grease that 3min removes sample in 70 ℃ of NaOH alkali solution;
(3) anode oxidation process
Anodic oxidation cathode and anode surface area ratio is controlled between 2: 1～1: 2, and what negative electrode adopted is stereotype;
(4) drying
Sample is placed in the loft drier at 120 ℃ of following dry 30min.
3, aluminum-copper alloy anodic oxidation thick film preparation according to claim 2 is characterized in that, in the step (1), the organic acid of interpolation is oxalic acid or citric acid, and the rare-earth salts of interpolation is cerous sulfate or lanthanum sulfat.
4, aluminum-copper alloy anodic oxidation thick film preparation according to claim 2 is characterized in that, when step (3), adopt the grading voltage method, fs boosts fast: 30s～2min, magnitude of voltage 80～120V makes current density reach 7～15A/dm rapidly
2After, keeping constant voltage 1min～3min, this moment, current density descended rapidly, and then improved oxidation voltage: 140～180V, reduced the lowering speed of current density, made it rete and kept the fast speed growth.
5, aluminum-copper alloy anodic oxidation thick film preparation according to claim 2 is characterized in that, when step (3), in anodised process, electrolyte temperature is controlled at 20 ℃～50 ℃.
6, aluminum-copper alloy anodic oxidation thick film preparation according to claim 2 is characterized in that, when step (3), owing to adopted the high-voltage great-current oxidation style, the required oxidization time of this technology is: 10～30min.
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| CN102256441A (en) * | 2011-05-23 | 2011-11-23 | 中山大学 | Metal substrate of heat conducting aluminium-based core and preparation method thereof |
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