CN102392284A - One-step treatment method for coloring and sealing aluminium anodic oxide film - Google Patents
One-step treatment method for coloring and sealing aluminium anodic oxide film Download PDFInfo
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- CN102392284A CN102392284A CN2011103436517A CN201110343651A CN102392284A CN 102392284 A CN102392284 A CN 102392284A CN 2011103436517 A CN2011103436517 A CN 2011103436517A CN 201110343651 A CN201110343651 A CN 201110343651A CN 102392284 A CN102392284 A CN 102392284A
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Abstract
The invention belongs to the field of metal finishing and provides a one-step treatment method for coloring and sealing an aluminium anodic oxide film. Firstly, preparing a coloring and sealing treatment fluid: adding nickel salt, fluoride, fluotitanic acid, hexamethylene tetramine, a complexing agent and a pruina restrainer into deionized water, enabling every component to reach a certain concentration, then adjusting the pH value within 5 to 6, and finally adding an organic addition agent. Secondly, implementing the one-step treatment method for coloring and sealing the aluminium anodic oxide film: washing an anodized aluminium alloy sample, then placing the sample in the treatment fluid of 20 to 40 DEG C to be treated for 5 to 25 minutes; and after the treatment, placing the sample in water of 55 to 60 DEG C for heat preservation for 5 to 15 minutes, and then washing and blow-drying the sample. Through the adoption of the method, the treatment technology is simple, chromium is avoided, the sealing treatment temperature is low, the aluminium anodic oxide film colored and sealed by the method has favorable corrosion resistance and good stain resistance and appears evenly and densely chartreuse, and coloring and sealing are finished at one step. Therefore, the method can replace the conventional chromate sealing technology.
Description
Technical field
The invention belongs to field of metal surface treatment, is a kind of painted sealing single stage method treatment process of aluminum anodized film, can be used as the alternative techniques of aluminum anodized film chromic salt sealing.
Background technology
Anodic oxidation is the main mode of aluminium surface-treated, yet the vesicular structure of anode oxide film seriously influences its corrosion resistance nature, therefore must carry out suitable sealing treatment.It is that the chromic salt sealing perhaps is main enclosure method with the nickelous fluoride that enclosure method commonly used is gone up in present industry; Adopt the former to handle and to obtain the oyster closing membrane; Have good anti-corrosion, yet chromic salt is a highly toxic substance, the chromate treating method is demanded urgently replacing; The latter is normal low temperature Chrome-free sealing treatment, commercial application at present, but this enclosure method simultaneously the antianode sull carry out paintedly, if need paintedly, chemical staining or electrolytic colouring technology step need be set separately.
Disclose the enclosure method that a kind of nickelous fluoride is a staple like patent 200810120737, compared the chromic salt system, this method has advantages such as technology is simple, treatment temp is low, pollution is little.200810048493 of patents disclose water-soluble closed dose that a kind of salt by basic metal or earth alkali metal, complexing agent, pH buffer reagent are formed, have effectively replaced deleterious chromium ion.Patent 200610065870 discloses a kind of enclosure method based on Ce-Mo salt.Although above method has reached the requirement of Chrome-free sealing treatment; But the anode oxide film than the chromic salt sealing all also has a certain distance on erosion resistance; And can't obtain coloured closing membrane; If must carry out the process step of electrolytic coloring or chemical staining before the painted then anodic oxidation membrane closure of needs, increase the production cycle, reduced production efficiency.
Summary of the invention
The technical problem that the present invention will solve is; Weak point to prior art; Propose the method for the painted sealing one step processing of a kind of aluminum anodized film, this method does not contain chromic salt, and treatment temp is low; Sealing back anode oxidation membrane corrosion resistance and good and near the yellow-green colour color of chromic salt closing membrane can be used as the substitution technique of chromic salt sealing.
For realizing above-mentioned purpose, technical scheme of the present invention is:
The treatment solution that painted one step of sealing of a kind of aluminum anodized film handles, contain in its every premium on currency solution:
Said nickel salt is one or more in single nickel salt, nickelous fluoride, nickel acetate and the nickelous carbonate;
Said fluorochemical is one or more in Sodium Fluoride, Neutral ammonium fluoride, Potassium monofluoride, fluoroboric acid and the nickelous fluoride;
Said organic additive prepares according to following method: multi-hydroxy carboxy acid, alkyl polyols, catalyzer and organic solvent were reacted 1 hour～3 hours at 100 ℃～130 ℃; Be cooled to room temperature then, treat that removing upper strata liquid after its layering promptly obtains the water-soluble organic additive of reddish-brown; Wherein the consumption of each component is: alkyl polyols and multi-hydroxy carboxy acid's mol ratio is 6～2: 1, and catalyst consumption is the 0.2wt%～0.5wt% of pure and mild sour total amount, and consumption of organic solvent is the 10wt%～50wt% of pure and mild sour total amount;
Said complexing agent is one or more in trolamine, amine triacetic acid, YD 30 and the sulfamate;
Said pollen suppressor factor is one or more in thiocarbamide, N.F,USP MANNITOL, polyoxyethylene glycol, acetate, PARA AMINOPHENOL and the glycerine.
In above-mentioned organic additive, said multi-hydroxy carboxy acid is one or more in tanpic acid, gallic acid and the xitix;
Said alkyl polyols is one or more in the following polyvalent alcohol: terepthaloyl moietie, 1,2-Ucar 35,1, ammediol, 1,4-butyleneglycol, 1,2-butyleneglycol, 1; 3-butyleneglycol, 2-methyl isophthalic acid, ammediol, 2,1,5-pentanediol, 1; 6-pinakon, 3-methyl isophthalic acid, 5-pentanediol, 2-ethyl-2-butyl 1, ammediol, 2,2,4-trimethylammonium-1; 3-pentanediol, 2,4-diethylammonium-1,5-pentanediol, 1-methyl isophthalic acid, 8-ethohexadiol, 3-methyl isophthalic acid; 6-pinakon, 4-methyl 1,7-heptanediol, 4-propyl group 1,8-ethohexadiol, 1,9-nonanediol, sorbyl alcohol, tetramethylolmethane and Tetraglycol 99;
Said organic solvent is one or more of toluene, YLENE, chlorobenzene, N-BUTYL ACETATE, EGME, Ucar 35 butyl ether;
Said catalyzer be following acid catalyst in any one: p-methyl benzenesulfonic acid, Mono-n-butyltin, Dibutyltin oxide, dibutyl tin dilaurate, dibutyl tin acetate or monobutyl-tin-trichloride.
Wherein, alkyl polyols described in the organic additive and multi-hydroxy carboxy acid's mol ratio is preferably 4: 1; Said catalyst consumption is preferably the 0.3wt% of pure and mild sour total amount; The consumption of said organic solvent is preferably the 38wt% of pure and mild sour total amount.The temperature of reaction of said organic additive preparation is preferably 130 ℃, and the reaction times is preferably 2 hours.
The compound method of the treatment solution that painted one step of sealing of above-mentioned aluminum anodized film handles is: in deionized water, add nickel salt, fluorochemical, hydrofluotitanic acid, hexamethylenetetramine, complexing agent and pollen suppressor factor; The concentration that makes each composition as stated; Using nitric acid or ammoniacal liquor that treatment solution is transferred to the pH value then is 5～6, and adds an amount of pH buffer reagent boric acid; Treat that its stable back adds above-mentioned organic additive, gets final product.
The method that one step of the painted sealing of a kind of aluminum anodized film handles: anodised aluminum alloy specimen is after washing or de-ionized washing from the beginning, and placing temperature is the treatment solution processing 5 minutes～25 minutes of 20 ℃～40 ℃ one of claim 1～5; After the processing test piece is placed 55 ℃～60 ℃ water insulations 5 minutes～15 minutes, then with washed with de-ionized water, cold wind dries up and gets final product.
The preferably treatment process is: anodised aluminum alloy specimen is after washing or de-ionized washing from the beginning, and placing temperature is that the treatment solution of 25 ℃ one of claim 1～5 was handled 10 minutes; After the processing test piece is placed 55 ℃ of water insulations 15 minutes, then with washed with de-ionized water, cold wind dries up and gets final product.
Do further explanation and explanation in the face of the present invention down:
The related detecting method of antianode oxidation sealing rete of the present invention comprises:
1. the alumilite process test piece outward appearance and the color that adopt digital camera to observe the painted sealing treatment of process of the present invention.
2. adopt the Japanese PHILIPS XL-30 of company type ESEM (SEM) observe sealing, with the anode oxide film surface microstructure of chromic salt sealing and the present invention's sealing.
3. adopt the sealing effect of phosphorus-chromium test determination anode oxide film: with reference to ISO 3210-1983 standard (being equal to GB/T8753-2005) method, preparation H
3PO
4(85%) 35ml/L, CrO
3The chromium of 20g/L-phosphoric acid corrosion liquid.The alumilite process test piece that 2.5cm * 7cm is big or small is after deionized water is cleaned, and cold wind dries up, and will pass through anodised test piece and adopt painted sealing one step process according to the invention to carry out placing aging 24 hours after the sealing treatment; Above-mentioned chromium-phosphoric acid corrosion liquid of putting into temperature then and being 38 ℃ soaked 15 minutes; Test piece weight before and after the weighing corrosion obtains test piece weight loss Δ W, and weight loss is more little; Then sealing effect is good more, and weight loss Δ W is less than 30mg/dm
2It is qualified to be regarded as, if less than 20mg/dm
2Then sealing effect is good.
Compare with chromic salt closed system and nickelous fluoride closed system, main advantage of the present invention is:
(1) the painted sealing one trip technique of alumilite process of the present invention has and similar corrosion resistance nature of chromic salt sealing treatment and yellow-green colour color, but the present invention does not contain the chromium that environment is had severe contamination, helps environment protection;
(2) anode oxide film of common nickelous fluoride sealing is colourless, and through obtaining the yellow-green colour closing membrane after the painted encapsulant processing of the present invention, one step of realization enclosed coloring accomplishes, and has certain decoration and excellent protection performance;
(3) because the present invention has realized the painted sealing one step processing behind the alumilite process, so technical process is simple, and cost is low, and this treatment process can be handled at normal temperature, helps industrial applications, alternative chromic salt closing process.
Description of drawings:
Fig. 1 is that from left to right, nickel ion concentration increases successively, color burn through the inventive method sealing gained aluminium alloy anode oxide film digital photograph;
Fig. 2 is the scanning electron microscope sem figure (2000 times) without the aluminum anodized film of sealing;
Fig. 3 is the scanning electron microscope sem figure (2000 times) of the aluminum anodized film after the present invention handles in painted one step of sealing;
Fig. 4 is the scanning electron microscope sem figure (2000 times) of the aluminum anodized film after the sealing of traditional chromic acid salt.
Embodiment
Below in conjunction with embodiment, the present invention is done further explanation and explanation, but the invention is not restricted to the scope of embodiment.
Embodiment 1:
The preparation of organic additive 1: with 25g xitix, 50g terepthaloyl moietie, 0.2g tosic acid; And 10g YLENE joins in the four-hole round-bottomed flask that has agitator arm, condensing works and division box, while stirring temperature risen to 130 ℃, after insulation half a hour; Add 18g YLENE; Insulation, when the amount of water in the water trap no longer changes, stopped reaction.Material is reduced to room temperature, treat to remove after its layering supernatant liquid and be that to obtain the water miscible organic additive of reddish-brown behind the solvent for use.
Embodiment 2:
Take by weighing single nickel salt 9g, Sodium Fluoride 3g, hydrofluotitanic acid 0.5g; Hexamethylenetetramine 0.6g, trolamine 1.6g, N.F,USP MANNITOL 0.8g; Boric acid 1.2g, with its respectively water dissolve in the large beaker that the back adds 1 liter, add the organic additive of 0.75g embodiment 1 preparation then; Add deionized water and regulate pH value to 5, add water at last and be painted sealing treatment liquid up to one liter of solution.
Prepare 2024 duraluminum test pieces, preparation 180g/L H
2After SO4 anodizing solution, aluminium test piece were handled 5 minutes through commercially available acid degreasing agent, washing was then with 1A/dm
2Sulphuric acid anodizing 40min is clean with deionized water rinsing under the current density, immerses the above-mentioned temperature for preparing and be in 25 ℃ the painted confining liquid 15 minutes.After the test piece washing test piece is placed 55 ℃ of warm water insulations 15 minutes, the sull after the sealing is yellow-green colour, and chromium-phosphoric acid test test piece weightlessness is less than 20mg/dm
2
Experimental result detects and analyzes:
(1) as shown in Figure 1 to the alumilite process test piece outward appearance behind embodiment 2 sealing treatment; Handle through treatment solution of painted one step of sealing of aluminum anodized film of the present invention; Can obtain the painted closing membrane of yellow-green colour alumilite process of even compact; The anode oxide film outward appearance of color and chromic salt sealing is similar, has ornamentally preferably, and phosphorus-chromium test shows that closing membrane has excellent corrosion-resistant and anti-fouling performance.Each components in proportions of the shade of anode oxidation coloration closing membrane of the present invention and encapsulant has certain relation, particularly organic additive and nickel ion content, therefore can regulate color as required.This anode oxidation coloration sealing one step process not only quality but also the reason that plays sealing process is inferred and is: the present invention since in the hydrofluotitanic acid that adds titanium ion with have containing of certain molecular weight polyhydric organic additive and aluminium substrate combine the organic fast eolor base of formation group; In closed process, follow nickel ion and fluorion to get in the hole of sull; Carrying out along with sealing; Form depositions such as ALUMNIUM FLUORIDE, nickel hydroxide in the hole; The organic colour developing group that combines to form with aluminium also is fixed in the micropore thereupon, thereby forms the yellow-green colour color of even compact.
(2) ESEM (2000 times) SEM without the anode oxide film that seals schemes like Fig. 2, has shown the vesicular structure behind the alumilite process; Seal ESEM (2000 times) SEM such as Fig. 3 and shown in Figure 4 of gained aluminum anodized film through the anode oxide film of peroxychromate sealing and through the inventive method; Two kinds of sealing methods all have sealing effect preferably; It is evenly smooth that the visible the inventive method of Fig. 4 is handled the painted closing membrane surface tissue of back gained, and the hole in the sull all is closed.More smooth evenly than chromic salt sealing method.
(3) handle the weightless result of the chromium of the anode oxide film after 10 minutes, 20 minutes and 35 minutes-phosphoric acid corrosion respectively through treatment solution of the present invention and be 18.76mg/dm
2, 16.84mg/dm
2And 15.31mg/dm
2, according to ISO 3210 standard codes, weight loss Δ W＜30mg/dm
2It is qualified to be regarded as, Δ W＜20mg/dm
2It is good then to be regarded as sealing effect.Therefore the anode oxide film of handling painted one step of sealing through the present invention reaches the erosion resistance requirement fully, and the result shows that increase limited to erosion resistance long off-period.
(4) immersion test result such as the table 1 of anode oxide film test piece in 3.5%NaCl solution that adopts chromic salt sealing and the painted encapsulant of the present invention to obtain respectively.The result shows that sealing treatment agent of the present invention is equivalent to chromic salt sealing level, and the salt water resistance performance is more excellent.
Table 1 is tested in the 3.5%NaCl solution soaking through the anode oxide film of sealing treatment
Embodiment 3:
Take by weighing single nickel salt 8.5g, fluoroboric acid 5.5, hydrofluotitanic acid 0.5g; Hexamethylenetetramine 0.6g, sodium ethylene diamine tetracetate 0.5g, thiocarbamide 0.8g; Boric acid 1.5g dissolves its water in the large beaker of 1 liter of back adding, adds the organic additive 0.8g of embodiment 1 then; Stir and regulate pH to 6, add water to 1 and liter be painted sealing treatment liquid.
Prepare 2024 duraluminum test pieces, the anodizing solution of preparation sulfuric acid (98%) 180g/L, after the aluminium test piece was handled 5 minutes through alkaline defatting agent, washing was then through after the nitric acid polishing washing in 1: 1, with 1A/dm
2Sulphuric acid anodizing is 20 minutes under the current density, and is clean with deionized water rinsing, immerses the above-mentioned temperature for preparing and be in 25 ℃ the painted confining liquid 15 minutes.After the test piece washing test piece is placed 55 ℃ of warm water insulations 15 minutes, it is yellow that the sull after the sealing is, and chromium-phosphoric acid weightlessness is less than 20mg/dm
2
Embodiment 4:
The preparation of organic additive: with 26g gallic acid, 48g 1,4-butyleneglycol, 0.2g dibutyl tin dilaurate, and the 12g N-BUTYL ACETATE joins in the four-hole round-bottomed flask that has agitator arm, condensation and division box; While stirring temperature is risen to 120 ℃; After being incubated half a hour, add the 16g N-BUTYL ACETATE, insulation; When the amount of water in the water trap no longer changes, stopped reaction.Material is reduced to room temperature, and treating to remove after its layering supernatant liquid, to obtain brown organic additive for use.
Embodiment 5:
Take by weighing nickel acetate 10.5g, Potassium monofluoride 7.5, hydrofluotitanic acid 0.8g; Hexamethylenetetramine 0.9g, thionamic acid sodium 1.5g, polyoxyethylene glycol 0.6g; Boric acid 0.8g; Its water is dissolved in the large beaker that the back adds 1 liter, add the organic additive 1.0g of embodiment 4 then, test and regulate the pH value and add water to one 5 and liter be painted sealing treatment liquid stirs.
The test piece of preparation pure aluminum foil, preparation 160g/LH
2SO
4And 80g/LH
3PO
4After mixed acid anodic oxidation liquid, aluminium test piece were handled 5 minutes through commercially available acid degreasing agent, washing was then with 1A/dm
2Sulphuric acid anodizing is 20 minutes under the current density, and is clean with deionized water rinsing, immerses the above-mentioned temperature for preparing and be in 25 ℃ the painted confining liquid 15 minutes.After the test piece washing test piece is placed 55 ℃ of warm water insulations 15 minutes, it is yellow that the sull after the sealing is, and chromium-phosphoric acid weightlessness is less than 20mg/dm
2
Embodiment 6:
Take by weighing single nickel salt 12.5g, fluoride amine 6.5, hydrofluotitanic acid 0.7g; Hexamethylenetetramine 0.6g, sodium ethylene diamine tetracetate 2.5g, PARA AMINOPHENOL 0.6g; Boric acid 1.3g dissolves its water in the large beaker of 1 liter of back adding, adds the organic additive of 0.9g embodiment 4 then; Stir and regulate pH value to 5.5, add water to one and liter be painted sealing treatment liquid.
Prepare 6061 duraluminum test plate (panel)s, preparation 180g/L sulphuric acid anodizing liquid, after the aluminium test piece was handled 5 minutes through commercially available acid degreasing agent, washing was then with 1A/dm
2Sulphuric acid anodizing is 20 minutes under the current density, and is clean with deionized water rinsing, immerses the above-mentioned temperature for preparing and be in 25 ℃ the painted confining liquid 10 minutes.After the test piece washing test piece is placed 55 ℃ of warm water insulations 15 minutes, the sull after the sealing is oyster, and chromium-phosphoric acid test test piece weightlessness is less than 20mg/dm
2
Claims (7)
1. the treatment solution of the painted sealing one step processing of aluminum anodized film is characterized in that, contains in its every premium on currency solution:
Said nickel salt is one or more in single nickel salt, nickelous fluoride, nickel acetate and the nickelous carbonate;
Said fluorochemical is one or more in Sodium Fluoride, Neutral ammonium fluoride, Potassium monofluoride, fluoroboric acid and the nickelous fluoride;
Said organic additive prepares according to following method: multi-hydroxy carboxy acid, alkyl polyols, catalyzer and organic solvent were reacted 1 hour～3 hours at 110 ℃～140 ℃; After treating that branch water finishes; Product is cooled to room temperature, treats that removing upper strata liquid after its layering promptly obtains the reddish-brown organic additive; Wherein the consumption of each component is: alkyl polyols and multi-hydroxy carboxy acid's mol ratio is 6～2: 1, and catalyst consumption is the 0.2wt%～0.5wt% of pure and mild sour total amount, and consumption of organic solvent is the 10wt%～50wt% of pure and mild sour total amount;
Said complexing agent is one or more in trolamine, amine triacetic acid, YD 30 and the sulfamate;
Said pollen suppressor factor is one or more in thiocarbamide, N.F,USP MANNITOL, polyoxyethylene glycol, acetate, PARA AMINOPHENOL and the glycerine.
2. the treatment solution of handling according to painted one step of sealing of the said a kind of aluminum anodized film of claim 1 is characterized in that multi-hydroxy carboxy acid described in the organic additive is one or more in tanpic acid, gallic acid and the xitix;
Said alkyl polyols is one or more in the following polyvalent alcohol: terepthaloyl moietie, 1,2-Ucar 35,1, ammediol, 1,4-butyleneglycol, 1,2-butyleneglycol, 1; 3-butyleneglycol, 2-methyl isophthalic acid, ammediol, 2,1,5-pentanediol, 1; 6-pinakon, 3-methyl isophthalic acid, 5-pentanediol, 2-ethyl-2-butyl 1, ammediol, 2,2,4-trimethylammonium-1; 3-pentanediol, 2,4-diethylammonium-1,5-pentanediol, 1-methyl isophthalic acid, 8-ethohexadiol, 3-methyl isophthalic acid; 6-pinakon, 4-methyl 1,7-heptanediol, 4-propyl group 1,8-ethohexadiol, 1,9-nonanediol, sorbyl alcohol, tetramethylolmethane and Tetraglycol 99;
Said organic solvent is one or more of toluene, YLENE, chlorobenzene, N-BUTYL ACETATE, EGME, Ucar 35 butyl ether;
Said catalyzer be following acid catalyst in any one: p-methyl benzenesulfonic acid, Mono-n-butyltin, Dibutyltin oxide, dibutyl tin dilaurate, dibutyl tin acetate or monobutyl-tin-trichloride.
3. the treatment solution of handling according to painted one step of sealing of the said a kind of aluminum anodized film of claim 1 is characterized in that alkyl polyols described in the organic additive and multi-hydroxy carboxy acid's mol ratio is 4: 1; Said catalyst consumption is the 0.3wt% of pure and mild sour total amount; The consumption of said organic solvent is the 38wt% of pure and mild sour total amount.
4. the treatment solution of handling according to painted one step of sealing of the said a kind of aluminum anodized film of claim 1 is characterized in that the temperature of reaction of said organic additive preparation is 130 ℃, and the reaction times is 2 hours.
5. the treatment solution of handling according to painted one step of sealing of the said a kind of aluminum anodized film of claim 1; It is characterized in that; Compound method is: in deionized water, add nickel salt, fluorochemical, hydrofluotitanic acid, hexamethylenetetramine, complexing agent and pollen suppressor factor; The concentration that makes each composition is the concentration described in the claim 1, and using nitric acid or ammoniacal liquor that treatment solution is transferred to the pH value then is 5～6, and adds an amount of pH buffer reagent boric acid; Treat that its stable back adds above-mentioned organic additive, gets final product.
6. the painted sealing one of aluminum anodized film goes on foot the method for handling; It is characterized in that; Anodised aluminum alloy specimen is after washing or de-ionized washing from the beginning, and placing temperature is that the treatment solution of 20 ℃～40 ℃ one of claim 1-5 was handled 5 minutes～25 minutes; After the processing test piece is placed 55 ℃～60 ℃ water insulations 5 minutes～15 minutes, then with washed with de-ionized water, cold wind dries up and gets final product.
7. the method for handling according to painted one step of sealing of the said a kind of aluminum anodized film of claim 6; It is characterized in that; Anodised aluminum alloy specimen is after washing or de-ionized washing from the beginning, and placing temperature is that the treatment solution of 25 ℃ one of claim 1～5 was handled 10 minutes; After the processing test piece is placed 55 ℃ of water insulations 15 minutes, then with washed with de-ionized water, cold wind dries up and gets final product.
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| CN105200495A (en) * | 2015-09-24 | 2015-12-30 | 马鞍山杰创塑胶科技有限公司 | Nickel-free hole sealing agent for improving compactness of aluminum alloy anode oxide film and preparation method of nickel-free hole sealing agent |
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