CN103526218A - Aging method of titanium alloy anodic oxidation activation and film peeling two-in-one solution - Google Patents
Aging method of titanium alloy anodic oxidation activation and film peeling two-in-one solution Download PDFInfo
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- CN103526218A CN103526218A CN201310504207.8A CN201310504207A CN103526218A CN 103526218 A CN103526218 A CN 103526218A CN 201310504207 A CN201310504207 A CN 201310504207A CN 103526218 A CN103526218 A CN 103526218A
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Abstract
The invention discloses an aging method of a titanium alloy anodic oxidation activation and film peeling two-in-one solution. The aging method comprises the following steps: performing film peeling treatment on samples or rework samples subjected to titanium alloy anoxic oxidation in newly prepared basic solution consisting of sodium hydroxide, sodium gluconate, triethanolamine, dimethyl ketoxime and tap water under a heating condition; introducing oxide film products which are peeled or dissolved into impurity ions such as Ti, Al and V with catalytic effects to obtain the activation and film peeling two-in-one solution. The titanium alloy anodic oxidation activation and film peeling two-in-one solution obtained by the method is environment-friendly and stable in performance, can be sued for preventing hydrogen absorption of a titanium alloy, has high applicability to the titanium alloy, can be used for activation or film peeling treatment, and guarantees the quality and reproducibility of the oxide film obtained by titanium alloy anodic oxidation or reoxidation.
Description
Technical field
The present invention relates to titanium alloy surface processing technology field, specifically the ageing method of the two-in-one solution of film is moved back in a kind of titanium alloy anode oxidation activation.
Background technology
Due to the high-performance of titanium or titanium alloy itself, be widely used in the fields such as aviation, medical treatment, chemical industry and be rapidly developed.The chemical property of titanium is active, and equilibrium potential is more negative, and thermodynamic (al) corrosion tendency is large in theory, and in fact titanium is very stable in many media, because titanium very easily reacts and passivation with oxygen, the oxide film of generation improves its solidity to corrosion, has stoped titanium alloy to be further oxidized.In addition, the resistivity of this layer of oxide film is higher, makes titanium alloy have excellent electrochemistry resistance to corrosion.But when titanium alloy contacts with dissimilar metal, due to the existence of oxide film, the current potential of titanium alloy than other metals just, can cause other metals to come in contact corrosion as anode.And titanium alloy is as negative electrode, will cause inhaling hydrogen, make material generation hydrogen embrittlement.For preventing and alleviating the crevice corrosion tendency producing when titanium alloy contacts with other metallic substance, further improve resistance to corrosion and the surface property thereof of titanium alloy, titanium alloy adopts anodic oxidation treatment to obtain oxide film conventionally.Yet titanium alloy easily forms the natural oxide film of one deck in atmosphere, without activation treatment, the appearance of the problem such as this layer naturally oxide film can stop the further anodic oxidation of titanium alloy, causes anode oxide film inhomogeneous, and bonding force is poor.In addition, in actual production, the qualification rate due to anode oxidation process can not guarantee absolutely, to cause the appearance of substandard product; In aviation field, a large amount of lightweight metal materials such as titanium or titanium alloy that adopt, aircraft is after flight for some time, and fuselage part there will be the phenomenons such as wearing and tearing, corrosion, if these parts are directly scrapped, the waste of huge financial loss and resource, the energy, manpower and materials will be brought.Therefore reprocessing, how to carry out the reprocessing of part, material has also become an important process.
The oxide film of the more civilian titanium alloy of oxide film of aero titanium alloy is more difficult, because aviation purposes is high to the mechanical property requirements of titanium alloy, do not allow to cause because inhale hydrogen material mechanical performance to decline, meanwhile, even if experiment shows still to have suction hydrogen in pH value in higher than 5 organic acidity system.So general acid system is suitable for the activation of Titanium Alloys for Aviation oxide film, not moving back film processing, is the effective way of avoiding inhaling hydrogen and adopt alkalescence or neutral system to move back film.In actual production, the technology of the existing using basic hydrogen peroxide system stripping of Aviation Enterprise rete.This method is to rely on oxydol H
2o
2oxidation-reduction quality and the characteristic on activated metal surface, there is the advantages such as composition is simple, easy care, product is pollution-free.But find in actual applications, H in membrane process is moved back in activation
2o
2the shortcomings such as rate of decomposition is too fast, and the poor consumption of existence and stability is large.
The oxide film TiO of titanium alloy
2be intermediate oxide, can react with sodium hydroxide NaOH, so titanium alloy is in alkaline hydrogen peroxide system, NaOH can remove surface part oxide compound, and makes oxide film loosening, makes the short texture of oxide compound, has formed many passages.H
2o
2by passage, arrive between titanium alloy substrate and oxide compound, the compositions such as the Fe in titanium alloy alloying constituent, V, as catalyzer, accelerate H
2o
2decomposition, decomposite H
2o and [O], [O] forms O
2in inside, produce outside pressure, and outside H
2o
2decomposite O simultaneously
2, produced a kind of airflow fluctuation, effect when making oxide film be subject to two kinds of power; And H
2o
2have reduction concurrently and be oxidized two kinds of effects, playing a part reduction oxide on surface here.Multiple effect is carried out simultaneously, has played activation or has moved back film effect.
Due to H
2o
2at normal temperature, can there is slow decomposition reaction and generate H
2o and O
2, in heating or after adding catalyzer, can accelerate decomposition reaction.In addition, H
2o
2aobvious slightly acidic, in alkaline environment, more unstable, degradation production H
2a large amount of gatherings of O, volume of bath solution constantly increases, and strength of solution is diluted, for assurance result of use need to often be added H
2o
2, bath maintenance is frequent, and complex operation has brought inconvenience to daily production.
Along with China's Economic development and environmental demand is improved constantly, the modern times move back film liquid formula judging criterion and are: it is high to move back membrane efficiency, and Stability of Bath Solution is good, easy to use, can not reduce titanium alloy and again be oxidized rear film quality, not inhale not etched the matrix of hydrogen, to titanium alloy material strong adaptability.
In the basal liquid being comprised of sodium hydroxide, Sunmorl N 60S, trolamine, DMKO and tap water, sodium hydroxide provides alkaline condition to dissolve or is loosening by TiO
2the oxide film forming, TiO
2with reacting as shown in reaction equation (1) of NaOH.
TiO
2+ 2NaOH(is dense) → Na
2tiO
3+ H
2o ... (1)
The meta-titanium perborate that above-mentioned reaction generates is insoluble in basal liquid, thereby is adsorbed on the carrying out that specimen surface stops reaction.
Sunmorl N 60S in basal liquid is main complexing agent, can improve the dissolving power of meta-titanium perborate in water; But in Sunmorl N 60S structure, contain carboxyl and hydroxyl that polarity is very strong, be easy to, in the fresh titanium alloy surface occurrence features absorption of exposing through excessive erosion, reduce again on the contrary activation effect.
Trolamine in basal liquid, as a kind of auxiliary complex-former, plays synergy with Sunmorl N 60S, further improves the solubleness of meta-titanium perborate complex compound in solution, and reaction equation (1) is carried out to the right, improves activation efficiency.Trolamine can play dissemination simultaneously, increases the stability of solution.
DMKO in basal liquid, as a kind of reductive agent, has stronger reductibility, soluble in water in, can with water in oxygen react, reduce the content of water oxygen, when having avoided moving back film activation, titanium alloy consumes a certain amount of O in the aqueous solution
2there is passivation again.DMKO and O
2reaction equation suc as formula shown in (2), (3).
2C
3H
7NO + O
2 → 2C
3H
6CO + N
2O + H
2O …………（2）
4(CH
3)
2C=N-OH + O
2 → 4(CH
3)
2C=O + 2N
2 + H
2O …………（3）
But result of study discovery, only according to the effect of four kinds of compositions of basal liquid, the basal liquid of new preparation is unsatisfactory to activation effect and the adaptability of titanium alloy, the homogeneity of the anode oxide film obtaining and poor adhesive force.
Under heating condition, in the basal liquid forming at the new sodium hydroxide of preparing, Sunmorl N 60S, trolamine, DMKO and tap water, adopting the sample after titanium alloy anode oxidation or the sample of doing over again to move back film processes, oxide film product that dependence is peeled off or is dissolved down is introduced the foreign ions such as Ti, Al, V activation to katalysis, participate in chemical reaction, reduced reaction activity.This solution obtaining of preparing by ageing method, has activation and moves back the two-in-one effect of film, makes titanium alloy anode oxidation or is again oxidized coating mass and the circulation ratio of gained, is obviously better than the treatment effect of basal liquid.
Summary of the invention
The object of the invention is to the deficiency for acidity or peroxide systems, provide a kind of titanium alloy anode oxidation activation to move back the ageing method of the two-in-one solution of film.The two-in-one solution of film is moved back in the activation of preparing by ageing method, overcome existing activation or moved back the defect that film system function singleness, acid system are harmful to base material corrosion, alkaline peroxide system stability is poor, both the activation treatment that can be used for titanium alloy anode oxidation, the film that moves back that can be used for again defective of titanium alloy anode oxidation, strong adaptability to different titanium alloys, environmentally friendly, tank liquor stable performance, safeguards easy to use.After this solution activates or move back film processing, anodic oxidation can access sticking power and the good oxide film of wear resistance.
The present invention is achieved by the following technical programs:
An ageing method for the two-in-one solution of film is moved back in titanium alloy anode oxidation activation, comprises the steps:
Under heating condition, in the basal liquid forming at the new sodium hydroxide of preparing, Sunmorl N 60S, trolamine, DMKO and tap water, adopting the sample after titanium alloy anode oxidation or the sample of doing over again to move back film processes, product that dependence is peeled off or is dissolved down is introduced the foreign ions such as Ti, Al, V activation to katalysis, by means of the katalysis of these foreign ions, make this solution possess activation simultaneously and move back film effect.
Adopt the present invention to prepare the step that the two-in-one solution of film is moved back in activation, in the basal liquid being formed by sodium hydroxide 35 ~ 85g/L, Sunmorl N 60S 20 ~ 70g/L, trolamine 15 ~ 65ml/L, DMKO 5 ~ 45g/L and tap water at every 2L of new preparation, adopt the TC4 of 2 ~ 6 100 mm X 100 mm X 1.5 ~ 10 mm or the sample after TB6 titanium alloy anode oxidation or the sample of doing over again to move back film and process (processing condition are: 85 ~ 100 ℃ of temperature, time 20 ~ 40min); Again this solution is added to tap water and be diluted to 2L scale, and boil 15 ~ 20min, obtain activation and move back the two-in-one solution of film.
Adopt the titanium alloy anode oxidation activation of the present invention's preparation to move back the two-in-one solution of film, the impurity ion content such as the Ti in solution, Al, V are controlled at Ti ion 5 ~ 2800 mg/L, Al ion 5 ~ 500mg/L, V ion 5 ~ 500 mg/L, utilize the impurity ion content such as ICP-MS ion chromatography Ti, Al, V.
Cross cut test according to GB/T9286-1998(paint and varnish paint film) bioassay standard, evaluates the bonding force of titanium alloy anodic oxide film and epoxy zinc chromate primer by cross-hatching.Test-results is divided into 0 ~ 5 six grade, and 0 grade of adhesion property is best, and 5 grades the poorest.
The present invention is environmentally friendly, and not fluoride or acid can not cause base material to inhale hydrogen; Move back film system with alkaline hydrogen peroxide and compare, there is the compatibility of better stability and better titanium alloy material, significantly reduced the consumption of hydrogen peroxide; Resulting titanium alloy anodic oxide film is even, fine and close, and wear resistance improves, good with the bonding force of paint film.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
With sodium hydroxide 55g/L, Sunmorl N 60S 35g/L, trolamine 20ml/L, DMKO 10g/L and tap water, form basal liquid, the sample of doing over again after titanium alloy check sample and titanium alloy anode oxidation is research object, in identical activation or move back under membrane process condition, in comparison basis liquid and basal liquid, introduce the impact that the two-in-one solution antianode of film oxide film bonding force is moved back in activation prepared by the foreign ions such as Ti, Al, V.
Embodiment 1
Adopt the sample of doing over again after the TC4 titanium alloy anode oxidation of 3 100 mm X 100 mm X 10 mm, (processing condition are: 85 ℃ of temperature in the 2L of above-mentioned new preparation basal liquid, to move back film processing, time 30min), again this solution is added to tap water and be diluted to 2L scale, and boil 15min, obtain titanium alloy anode oxidation activation and move back the two-in-one solution of film.The impurity ion content such as sampling analysis Ti, Al, V are respectively 261.1 mg/L, 55.1 mg/L, 59.7 mg/L.
TC4, TB6, each of TA15 titanium alloy check sample carry out respectively anodic oxidation after adopting activation to move back the two-in-one solution activation of film, and the bonding force of oxide film is 0 grade; Each, the sample of doing over again after TC4, TB6, TA15 titanium alloy anode oxidation adopts activation to move back after the two-in-one solution of film moves back film and re-starts respectively anodic oxidation, and the bonding force of oxide film is at 0 ~ 1 grade; And identical three kinds of titanium alloy check samples or the sample of doing over again adopt the basal liquid activation of new preparation or move back film after carry out respectively anodic oxidation, 3 grades of the equal > of bonding force of oxide film.
Embodiment 2
Adopt each 1 of the TC4, the sample after TB6 titanium alloy anode oxidation of 100 mm X 100 mm X 10 mm, (processing condition are: temperature is 85 ℃ in the 2L of above-mentioned new preparation basal liquid, to move back film processing, time is 25min), again this solution is added to tap water and be diluted to 2L scale, and boil 20min, obtain activation and move back the two-in-one solution of film.The impurity ion content such as sampling analysis Ti, Al, V are respectively 321.1 mg/L, 70.3 mg/L, 89.1 mg/L.
TC4, TB6, each of TA15 titanium alloy check sample carry out respectively anodic oxidation after adopting activation to move back the two-in-one solution activation of film, and the bonding force of oxide film is 0 grade; Each, the sample of doing over again after TC4, TB6, TA15 titanium alloy anode oxidation adopts activation to move back after the two-in-one solution of film moves back film and re-starts respectively anodic oxidation, and the bonding force of oxide film is at 0 ~ 1 grade; And identical three kinds of titanium alloy check samples or the sample of doing over again adopt the basal liquid activation of new preparation or move back film after carry out respectively anodic oxidation, 3 grades of the equal > of bonding force of oxide film.
Embodiment 3
Adopt the sample after the TB6 titanium alloy anode oxidation of the sample of doing over again after the TC4 titanium alloy anode oxidation of 2 100 mm X 100 mm X 2.5 mm, 2 100 mm X 100 mm X 10 mm, (processing condition are: temperature is 85 ℃ in the 2L of above-mentioned new preparation basal liquid, to move back film processing, time is 25min), again this solution is added to tap water and be diluted to 2L scale, and boil 20min, obtain activation and move back the two-in-one solution of film.The impurity ion content such as sampling analysis Ti, Al, V are respectively 424.1 mg/L, 124.7 mg/L, 146.2 mg/L.
TC4, TB6, each of TA15 titanium alloy check sample carry out respectively anodic oxidation after adopting activation to move back the two-in-one solution activation of film, and the bonding force of oxide film is 0 grade; Each, the sample of doing over again after TC4, TB6, TA15 titanium alloy anode oxidation adopts activation to move back after the two-in-one solution of film moves back film and re-starts respectively anodic oxidation, and the bonding force of oxide film is at 0 ~ 1 grade; And identical three kinds of titanium alloy check samples or the sample of doing over again adopt the basal liquid activation of new preparation or move back film after carry out respectively anodic oxidation, 3 grades of the equal > of bonding force of oxide film.
Embodiment 4
Adopt the sample after the TB6 titanium alloy anode oxidation of the sample after the TC4 titanium alloy anode oxidation of 3 100 mm X 100 mm X 10 mm, 2 100 mm X 100 mm X 10 mm, (processing condition are: temperature is 100 ℃ in the 2L of above-mentioned new preparation basal liquid, to move back film processing, time is 30min), again this solution is added to tap water and be diluted to 2L scale, and boil 15min, obtain activation and move back the two-in-one solution of film.The impurity ion content such as sampling analysis Ti, Al, V are respectively 724.1 mg/L, 184.7 mg/L, 226.2 mg/L.
TC4, TB6, each of TA15 titanium alloy check sample carry out respectively anodic oxidation after adopting activation to move back the two-in-one solution activation of film, and the bonding force of oxide film is 0 grade; Each, the sample of doing over again after TC4, TB6, TA15 titanium alloy anode oxidation adopts activation to move back after the two-in-one solution of film moves back film and re-starts respectively anodic oxidation, and the bonding force of oxide film is at 0 ~ 1 grade; And identical three kinds of titanium alloy check samples or the sample of doing over again adopt the basal liquid activation of new preparation or move back film after carry out respectively anodic oxidation, 3 grades of the equal > of bonding force of oxide film.
Claims (3)
1. a titanium alloy anode oxidation activates the ageing method that moves back the two-in-one solution of film, it is characterized in that: under heating condition, in the basal liquid forming in the new sodium hydroxide of preparing, Sunmorl N 60S, trolamine, DMKO, adopting the sample after titanium alloy anode oxidation or the sample of doing over again to move back film processes, oxide film product that dependence is peeled off or is dissolved down is introduced the foreign ions such as Ti, Al, V activation to katalysis, by means of the katalysis of these foreign ions, make this solution possess the effect that film is moved back in titanium alloy anode oxidation activation simultaneously.
2. the ageing method of the two-in-one solution of film is moved back in titanium alloy anode oxidation activation according to claim 1, it is characterized in that: in the basal liquid being formed by sodium hydroxide 35 ~ 85g/L, Sunmorl N 60S 20 ~ 70g/L, trolamine 15 ~ 65ml/L, DMKO 5 ~ 45g/L and tap water at every 2L of new preparation, adopt the TC4 of 2 ~ 6 100 mm X 100 mm X 1.5 ~ 10 mm or the sample after TB6 titanium alloy anode oxidation or the sample of doing over again to move back film processing, moving back membrane treatment process condition is: 85 ~ 100 ℃ of temperature, time 20 ~ 40min; Add afterwards tap water to 2L scale, and boil 15 ~ 20min, obtain titanium alloy anode oxidation activation and move back the two-in-one solution of film.
3. the ageing method of the two-in-one solution of film is moved back in titanium alloy anode oxidation activation according to claim 1 and 2, it is characterized in that: utilize the titanium alloy anode oxidation activation of ageing method preparation to move back the two-in-one solution of film, Ti in solution, Al, V impurity ion content are controlled at Ti ion 5 ~ 2800 mg/L, Al ion 5 ~ 500mg/L, V ion 5 ~ 500 mg/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088313A (en) * | 2015-09-14 | 2015-11-25 | 江西洪都航空工业集团有限责任公司 | Titanium alloy activation technological method |
| CN106702460A (en) * | 2016-11-30 | 2017-05-24 | 江西洪都航空工业集团有限责任公司 | Titanium alloy anodized film withdrawing method |
| CN107091840A (en) * | 2017-06-15 | 2017-08-25 | 南昌航空大学 | The analysis method of sodium gluconate in a kind of titanium alloy activating solution |
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| CN101245467A (en) * | 2008-03-21 | 2008-08-20 | 北京航空航天大学 | Stripping liquid and stripping method for stripping titanium and titanium alloy anodized film |
| CN102586791A (en) * | 2012-02-13 | 2012-07-18 | 江西洪都航空工业集团有限责任公司 | Efficient environment-friendly conditioning fluid for titanium and titanium alloy anodized repair members |
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Patent Citations (2)
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| CN101245467A (en) * | 2008-03-21 | 2008-08-20 | 北京航空航天大学 | Stripping liquid and stripping method for stripping titanium and titanium alloy anodized film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105088313A (en) * | 2015-09-14 | 2015-11-25 | 江西洪都航空工业集团有限责任公司 | Titanium alloy activation technological method |
| CN106702460A (en) * | 2016-11-30 | 2017-05-24 | 江西洪都航空工业集团有限责任公司 | Titanium alloy anodized film withdrawing method |
| CN107091840A (en) * | 2017-06-15 | 2017-08-25 | 南昌航空大学 | The analysis method of sodium gluconate in a kind of titanium alloy activating solution |
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