CN1844483A - Process for anode oxidation coloration of titanium and titanium alloy surface - Google Patents
Process for anode oxidation coloration of titanium and titanium alloy surface Download PDFInfo
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Abstract
This invention relates to titanium and titanium alloy surface anode oxidation bepainting method. This invention has following steps: dealing with titanium and titanium alloy in alkali solution for 10-15min under 60-75deg C and ultrasonic condition, then rinsing, and then putting it in acid solution for 0.5-1min, and then rinsing, and then under the condition that the temperature is 15-35deg C, the current density is 5-10Am-2, the voltage is 20-90V, putting it in anode oxidation bepainting solution to bepaint for 15-30min,then rinsing, and then dealing with it closely for 15-30min in non-ionic water, and then drying for 30-60min under 110-130deg C. The advantage in this invention is that the steps are few, the operation is simple, and it is easy to maintain.
Description
Technical field
The present invention relates to a kind of titanium or titanium alloy, especially relate to a kind of titanium or titanium alloy surface anode oxidation coloration technology.
Background technology
Titanium or titanium alloy has good thermostability and high specific tenacity, is and magnesium alloy, the same active metal that can generate oxide film rapidly of aluminium alloy, and can remedies aluminium alloy and magnesium alloy can't be higher than the deficiency of using under 425 ℃ of conditions.In recent years, titanium or titanium alloy all is being used widely aspect national defence hard-core technology field and the civilian industry.For example, aspect aerospace,, and be applied to Aircraft Production of new generation because titanium or titanium alloy proportion is little, in light weight, intensity is high; Medically, titanium or titanium alloy and human body repellency are low, are widely used in aspects such as tooth, bone and stent, become a kind of noticeable biomedical metal material; Architectural, because the titanium or titanium alloy uniqueness, its consumption increases year by year, and some developed countries have also built up titanium material construction structural thing in succession.
But titanium or titanium alloy also has the some shortcomings part, and is low as wear resistance, specific conductivity and thermal conductivity, is difficult for bearing soldering, relatively more responsive to hydrogen and fused salt stress corrosion, easily comes in contact corrosion etc. with other metallic contact, limited its range of application.Therefore, for further enlarging the Application Areas of titanium alloy, must carry out modification to its surface and handle.Just attach great importance to the research of titanium anode oxidation process in 60～seventies of 20th century abroad, obtained bigger progress, and be applied to every profession and trade.And domestic about titanium alloy surface processing aspect research also seldom, do not set up corresponding national standards so far yet.In the process for treating surface of titanium or titanium alloy, from present research and applicable cases, laser melts and covers surface treatment, surface deposition coating (CVD and PVD method), thermodiffusion, Surface Nanocrystalline all also do not reach industrial production requirement on cost and technology maturation degree, and the anodic oxidation treatment technology is simple with technology, oxide film wear resisting property, anti-crevice corrosion and anti-hydrogen embrittlement performance are good, (the sufacing of in industrial production, being used widely, 2001,30 (2): 33～34).The titanium or titanium alloy anode oxide film is along with the variation of thicknesses of layers, and its surface can present shades of colour, is ideal ornament layer and protective layer.Though the anodised recipe ratio of titanium or titanium alloy is more, (the accurate manufacturing technology of aviation such as dc anodizing, pulse anodic oxidation, thick film anodic oxidation is arranged, 2004,4 (40): 17～22), but the anode oxidation process of these types scarcely possesses anodised and carries out painted ability simultaneously, and there is the following problem in the technology that minority can obtain coloring effect:
1) titanium or titanium alloy is along with the variation of various oxidizing conditions, and the oxide film color and luster is difficult to be consistent.(aerospace processing, 1993,4:17～19).
2) anode oxidation process contains environmentally harmful material (as chromium cpd).(aerospace processing technology, 1994,6:20～21).
3) anodic oxidation of adopting phosphoric acid and sulfuric acid to form can obtain certain coloring effect by control voltage, and still, but because acidity causes operating restraint low too by force, temperature is too high will to be caused rete to melt causing that color and luster is inhomogeneous.(electroplate and environmental protection 2003,23 (4): 37～38).
4) disclosed anode oxidation coloration patent can only form single coloring effect (Chinese patent: 200310103374.8).
There is following difficult point in the titanium or titanium alloy anode oxidation coloration:
1) the titanium or titanium alloy chemical property is active, and self just can form the oxide membranous layer with certain protective value, and this rete has chemical instability and is easy to occur defective obstruction anode oxide film and combines with substrate, causes the oxide film color and luster inhomogeneous simultaneously.
2) traditional anode oxidation coloration can only obtain single coloring effect, when the oxide film stack of different thickness can cause color and luster inhomogeneous.
3) change of processing condition is bigger to the coloring effect influence, obtain the necessary strict control condition of uniform coloring effect, comprises temperature, current density, voltage and bath composition etc.
Summary of the invention
Purpose of the present invention aims to provide a kind of cheapness, simple, can have the processing method of the anode oxidation membrane of different color effect in the acquisition of titanium or titanium alloy surface.
Its step of the present invention is as follows:
1) at 60～75 ℃ and add under the ultrasonic wave condition, titanium or titanium alloy are put into soda-wash solution handle 10～15min, take out the back water rinse;
2) titanium that will be after step 1) is handled or titanium alloy are put into Acidwash solution and are handled 0.5～1min, take out the back water rinse;
3) at 15～35 ℃, current density 5～10Adm
-2, under voltage 20～90V, will put into anode oxidation coloration solution anode oxidation coloration 15～30min through titanium after alkali cleaning and the cleanup acid treatment or titanium alloy, take out the back water rinse, obtain to have the anode oxidation membrane of color and luster;
4) titanium or the titanium alloy of anode oxidation coloration are put into the ebullient deionized water, sealing treatment 15～30min;
5) with the titanium behind the sealing treatment or titanium alloy under 110～130 ℃, 30～60min is handled in oven dry.
Described soda-wash solution is by 20～25gL
-1Yellow soda ash, 20～25gL
-1Sodium phosphate and 10～15gL
-1Water glass is formed.Described Acidwash solution is 50～80mLL of 40% by concentration
-1Hydrofluoric acid and 180～200mLL
-1Nitric acid is formed.Described anode oxidation coloration solution is by 50～80mLL
-1Phosphoric acid, 5～15gL
-1Oxalic acid, 2～5gL
-1Manganous sulfate and composite additive are formed, and described composite additive comprises 2～5gL
-1P-TOLUENE SULFO ACID 99's sodium and 1～4gL
-1Sulphosalicylic acid.
Processing step of the present invention is few, and each step is simple to operate, is easy to safeguard.By setting the anode oxide film that different magnitudes of voltage can obtain different color and lusters; Painted anode oxide film bright in color, even non-variegation have good decoration effect.Anode oxide film has high surface hardness, good bonding force and corrosion resisting property.By adding the plating continuously of each main component, good actual application prospect is arranged.
Description of drawings
Fig. 1 is the titanium alloy XRD structural analysis figure after cleanup acid treatment among the embodiment 2.In Fig. 1, X-coordinate be 2theta (°), ordinate zou is Counts.
Fig. 2 is the titanium alloy XRD structural analysis figure after anode oxidation coloration is handled among the embodiment 2.In Fig. 2, X-coordinate be 2theta (°), ordinate zou is Counts.
Embodiment
Embodiment 1
1) alkali cleaning, under the room temperature, (1L) adds yellow soda ash (20g), sodium phosphate (20g), water glass (10g) successively in deionized water solution, wait to dissolve complete post-heating to 70 ℃, the industrially pure titanium sample that will be processed into 10mm * 10mm * 2mm size is put into the lasting ultrasonic stirring of soda-wash solution, takes out behind the processing 15min.Under the room temperature, the titanium after the alkali cleaning put into take out after the mobile deionized water cleans 2min.
2) pickling, under the room temperature, in deionized water solution (750mL) to add concentration successively be 40% hydrofluoric acid (50mL), nitric acid (200mL), the titanium after will handling through alkali cleaning be put into and take out after this Acidwash solution is handled 60s.Under the room temperature, the titanium after the pickling put into take out after the mobile deionized water cleans 2min.
3) anode oxidation coloration, under 15 ℃, (700mL) adds phosphoric acid (80mL), oxalic acid (5g), manganous sulfate (5g) under stirring successively in deionized water solution, treats under agitation to add composite additive after the dissolving fully, is followed successively by: P-TOLUENE SULFO ACID 99's sodium (5g), sulphosalicylic acid (1g).Add deionized water at last to 1L.To put into this solution through the titanium after the above-mentioned processing, as negative electrode, sample applies 5Adm as anode with stainless steel
-2Constant current boosts to constant voltage behind the 22V, takes out after handling 25min.Under the room temperature, the titanium after the anodic oxidation put into take out after the mobile deionized water cleans 2min.
4) sealing is put into the ebullient deionized water with the titanium of anode oxidation coloration, sealing treatment 15min.
5) oven dry will be taken out after the titanium of above-mentioned processing is put into 130 ℃ of baking oven oven dry 30min at last.
Below provide the performance of embodiment 1 gained anode oxide film.
1, anode oxide film bonding properties:
A, qualified by the bonding force of mensuration coating of the scratch method among the standard GB 5270-85 and matrix.
B, qualified by the bonding force of mensuration coating of the thermal shock method among standard GB/T 13913-92 and matrix.
2, other performance of anode oxide film:
Other performance of anode oxide film sees Table 1.
Table 1
| Color and luster | Dark blue |
| Thickness (μ m) | 6 |
| Hardness (HV) | 301.5 |
Embodiment 2
1) alkali cleaning, under the room temperature, (1L) adds yellow soda ash (20g), sodium phosphate (20g), water glass (15g) successively in deionized water solution, waits to dissolve complete post-heating to 70 ℃, TC4 titanium alloy sample is put into soda-wash solution continue ultrasonic stirring, take out behind the processing 15min.Under the room temperature, the titanium alloy after the alkali cleaning put into take out after the mobile deionized water cleans 2min.
2) pickling, under the room temperature, in deionized water solution (750mL) to add concentration successively be 40% hydrofluoric acid (50mL), nitric acid (200mL), the titanium alloy after will handling through alkali cleaning be put into and take out after this Acidwash solution is handled 60s.Under the room temperature, the titanium alloy after the pickling put into take out after the mobile deionized water cleans 2min.Fig. 1 is seen in titanium alloy surface structural analysis after the processing, shows among the figure that what obtain after overpickling is the surface structure that is made of mutually single titanium, provides the surface of an electrochemical properties unanimity for subsequent disposal.
3) anode oxidation coloration, under 20 ℃, (700mL) adds phosphoric acid (80mL), oxalic acid (5g), manganous sulfate (5g) under stirring successively in deionized water solution, treats under agitation to add composite additive after the dissolving fully, is followed successively by: P-TOLUENE SULFO ACID 99's sodium (4g), sulphosalicylic acid (2g).Add deionized water at last to 1L.To put into this solution through the titanium alloy after the above-mentioned processing, as negative electrode, the titanium alloy sample applies 6Adm as anode with stainless steel
-2Constant current boosts to constant voltage behind the 30V, takes out after handling 20min.Under the room temperature, the titanium alloy after the anodic oxidation put into take out after the mobile deionized water cleans 2min.
4) sealing is put into the ebullient deionized water with the titanium alloy of anode oxidation coloration, sealing treatment 20min.
5) oven dry will be taken out after the titanium alloy of above-mentioned processing is put into 130 ℃ of baking oven oven dry 30min at last.The oxide film color and luster that obtains is even, attractive in appearance.Fig. 2 is seen in titanium alloy surface structural analysis after the processing, shows among the figure that the oxide film through obtaining behind the anode oxidation coloration mainly is made of titanium oxide and titanium dioxide.
Below provide the performance of embodiment 2 gained anode oxide films.
1, anode oxide film bonding properties:
Testing method and experimental result are with embodiment 1.
2, other performance of anode oxide film:
Other performance of anode oxide film sees Table 2.
Embodiment 3
1) alkali cleaning is with embodiment 2.
2) pickling is with embodiment 2.
3) anode oxidation coloration, under 25 ℃, (700mL) adds phosphoric acid (80mL), oxalic acid (12g), manganous sulfate (3g) under stirring successively in deionized water solution, treats under agitation to add composite additive after the dissolving fully, is followed successively by: P-TOLUENE SULFO ACID 99's sodium (3g), sulphosalicylic acid (3g).Add deionized water at last to 1L.To put into this solution through the titanium alloy after the above-mentioned processing, as negative electrode, titanium alloy applies 7Adm as anode with stainless steel
-2Constant current boosts to constant voltage behind the 45V, takes out after handling 25min.Under the room temperature, the titanium alloy after the anodic oxidation put into take out after the mobile deionized water cleans 2min.
4) sealing is put into the ebullient deionized water with the titanium alloy of anode oxidation coloration, sealing treatment 30min.
5) oven dry is with embodiment 2.Even, attractive in appearance through the oxide film color and luster that obtains behind the anode oxidation coloration.
Below provide the performance of embodiment 3 gained anode oxide films.
1, anode oxide film bonding properties:
Testing method and experimental result are with embodiment 1.
2, other performance of anode oxide film:
Other performance of anode oxide film sees Table 2.
Embodiment 4
1) alkali cleaning, under the room temperature, (1L) adds yellow soda ash (25g), sodium phosphate (25g), water glass (15g) successively in deionized water solution, waits to dissolve complete post-heating to 65 ℃, TC1 titanium alloy sample is put into soda-wash solution continue ultrasonic stirring, take out behind the processing 10min.Under the room temperature, the titanium alloy after the alkali cleaning put into take out after the mobile deionized water cleans 2min.
2) pickling, under the room temperature, in deionized water solution (750mL) to add concentration successively be 40% hydrofluoric acid (80mL), nitric acid (180mL), the titanium alloy after will handling through step 1～2 be put into and take out after Acidwash solution is handled 30s.Under the room temperature, the titanium alloy after the pickling put into take out after the mobile deionized water cleans 2min.
3) anode oxidation coloration, under 30 ℃, (700mL) adds phosphoric acid (80mL), oxalic acid (5g), manganous sulfate (5g) under stirring successively in deionized water solution, treats under agitation to add composite additive after the dissolving fully, is followed successively by: P-TOLUENE SULFO ACID 99's sodium (3g), sulphosalicylic acid (2g).Add deionized water at last to 1L.To put into this solution through the titanium alloy after the above-mentioned processing, as negative electrode, sample applies 8Adm as anode with stainless steel
-2Constant current boosts to constant voltage behind the 60V, takes out after handling 20min.Under the room temperature, the titanium alloy after the anodic oxidation put into take out after the mobile deionized water cleans 2min.
4) sealing is put into the ebullient deionized water with the titanium alloy of anode oxidation coloration, sealing treatment 25min.
5) oven dry will be taken out after the titanium alloy of above-mentioned processing is put into 110 ℃ of baking oven oven dry 60min at last.The oxide film color and luster that obtains is even, attractive in appearance.
Below provide the performance of embodiment 4 gained anode oxide films.
1, anode oxide film bonding properties:
Testing method and experimental result are with embodiment 1.
2, other performance of anode oxide film:
Other performance of anode oxide film sees Table 2.
Embodiment 5
1) alkali cleaning is with embodiment 4.
2) pickling is with embodiment 4.
3) anode oxidation coloration, under 25 ℃, (700mL) adds phosphoric acid (80mL), oxalic acid (10g), manganous sulfate (4g) under stirring successively in deionized water solution, treats under agitation to add composite additive after the dissolving fully, is followed successively by: P-TOLUENE SULFO ACID 99's sodium (2g), sulphosalicylic acid (3g).Add deionized water at last to 1L.To put into this solution through the titanium alloy after the above-mentioned processing, as negative electrode, titanium alloy applies 9Adm as anode with stainless steel
-2Constant current boosts to constant voltage behind the 70V, takes out after handling 30min.Under the room temperature, the titanium alloy after the anodic oxidation put into take out after the mobile deionized water cleans 2min.
4) sealing is put into the ebullient deionized water with the titanium alloy of anode oxidation coloration, sealing treatment 30min.
5) oven dry is with embodiment 4.
Below provide the performance of embodiment 5 gained anode oxide films.
1, anode oxide film bonding properties:
Testing method and experimental result are with embodiment 1.
2, other performance of anode oxide film:
Other performance of anode oxide film sees Table 2.
Embodiment 6
1) alkali cleaning is with embodiment 4.
2) pickling is with embodiment 4.
3) anode oxidation coloration, under 35 ℃, (700mL) adds phosphoric acid (80mL), oxalic acid (8g), manganous sulfate (3g) under stirring successively in deionized water solution, treats under agitation to add composite additive after the dissolving fully, is followed successively by: P-TOLUENE SULFO ACID 99's sodium (4g), sulphosalicylic acid (2g).Add deionized water at last to 1L.To put into this solution through the titanium alloy after the above-mentioned processing, as negative electrode, titanium alloy applies 10Adm as anode with stainless steel
-2Constant current boosts to constant voltage behind the 82V, takes out after handling 30min.Under the room temperature, the titanium alloy after the anodic oxidation put into take out after the mobile deionized water cleans 2min.
4) sealing is with embodiment 4.
5) oven dry is with embodiment 4.
Below provide the performance of embodiment 6 gained anode oxide films.
1, anode oxide film bonding properties:
Testing method and experimental result are with embodiment 1.
2, other performance of anode oxide film:
Other performance of anode oxide film sees Table 2.
Table 2
| Embodiment | Color and luster | Thickness (μ m) | Hardness (HV) |
| 2 | Sky blue | 9 | 402.6 |
| 3 | Golden yellow | 14 | 572.6 |
| 4 | Purplish red | 18 | 638.2 |
| 5 | Purple | 22 | 746.1 |
| 6 | Green | 23 | 802.8 |
Claims (4)
1, the method for titanium or titanium alloy surface anode oxidation coloration is characterized in that its step is as follows:
1) at 60～75 ℃ and add under the ultrasonic wave condition, titanium or titanium alloy are put into soda-wash solution handle 10～15min, take out the back water rinse;
2) titanium that will be after step 1) is handled or titanium alloy are put into Acidwash solution and are handled 0.5～1min, take out the back water rinse;
3) at 15～35 ℃, current density 5～10Adm
-2, under voltage 20～90V, will put into anode oxidation coloration solution anode oxidation coloration 15～30min through titanium after alkali cleaning and the cleanup acid treatment or titanium alloy, take out the back water rinse, obtain to have the anode oxidation membrane of color and luster;
4) titanium or the titanium alloy of anode oxidation coloration are put into the ebullient deionized water, sealing treatment 15～30min;
5) with the titanium behind the sealing treatment or titanium alloy under 110～130 ℃, 30～60min is handled in oven dry.
2, the method for titanium or titanium alloy anode oxidation coloration as claimed in claim 1 is characterized in that described soda-wash solution is by 20～25gL
-1Yellow soda ash, 20～25gL
-1Sodium phosphate and 10～15gL
-1Water glass is formed.
3, the method for titanium or titanium alloy anode oxidation coloration as claimed in claim 1 is characterized in that described Acidwash solution is 50～80mLL of 40% by concentration
-1Hydrofluoric acid and 180～200mLL
-1Nitric acid is formed.
4, the method for titanium or titanium alloy anode oxidation coloration as claimed in claim 1 is characterized in that described anode oxidation coloration solution is by 50～80mLL
-1Phosphoric acid, 5～15gL
-1Oxalic acid, 2～5gL
-1Manganous sulfate and composite additive are formed, and described composite additive comprises 2～5gL
-1P-TOLUENE SULFO ACID 99's sodium and 1～4gL
-1Sulphosalicylic acid.
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