CN103103512B - The rare earth modified titanium zirconium system's chemical passivation liquid processed for aluminium shape surface and using method - Google Patents
The rare earth modified titanium zirconium system's chemical passivation liquid processed for aluminium shape surface and using method Download PDFInfo
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Abstract
The invention discloses a kind of rare earth modified titanium zirconium system's chemical passivation liquid processed for aluminium shape surface and using method thereof, it is characterized in that, described passivating solution is to utilize rare earth compound as the main salt of auxiliary film forming of Ti Zr inactivating treatment liquid, give the light yellow outward appearance of passivating film, there is the quality of forming film scene property of can determine whether.Specifically every liter solution of its formula contains: potassium fluotitanate (fluotitanic acid) 0.5g L‑1～10 g L‑1, potassium fluorozirconate (fluorine zirconic acid) 0.5g L‑1～10 g L‑1, cerous nitrate (ceric sulfate, ammonium ceric nitrate) 0.5g L‑1～5g L‑1, potassium nitrate 2g L‑1～10g L‑1, sodium fluoride (potassium fluoride) 0.5g L‑1～3g L‑1, dodecylbenzene sodium sulfonate or OP 10 0.5 g L‑1～1 g L‑1, nitric acid 0.2mL～5mL L‑1, boric acid 1 g L‑1～5g L‑1.Its using method includes, the dirts such as attachment dust removed by aluminium alloy by (1)；(2) again aluminum alloy surface is made pretreatment；(3) treatment fluid is used to be passivated processing；(4) rinse with water, dry.Treatment fluid of the present invention has the advantages such as outward appearance is pale yellow, film forming speed is fast, technique is simple, even film layer, corrosion resistance are strong, environmental pollution is few.
Description
Technical field
The present invention relates to aluminium alloy surface treatment method, be specifically related to use a kind of non-chromium inactivating treatment liquid, at aluminium alloy
Surface preparation has the rare earth modified Ti-Zr system composite passivation film of good corrosion resistance.
Background technology
Aluminium alloy is that consumption is only second to iron and steel and occupies the structural metallic materials of second, be widely used in automobile, Aero-Space,
The numerous areas such as building decoration, household electrical appliances, instrument and meter, computer, mobile phone, haberdashery and hardware.Al-alloy products the most all must be through
Crossing surface to process, wherein chemical passivation processes and has little to base material Influence of Fatigue Properties, easy to operate, low cost, production efficiency
The advantage such as high, applied widely, is one of process for treating surface of being most widely used.Carry out again after the passivated process of aluminium alloy
Application, is greatly improved the adhesion of matrix and coating, is obviously enhanced the corrosion protection of aluminium alloy.Aluminum current section bar is being adopted
Generally using passivation technology to process before carrying out application with organic coating, particularly decay resistance is superior, coloury
High-grade aluminium section bar all uses passivated surface to process technique before being coated with organic coating, uses the electrostatic powder coating section bar of this technique
It it is with fastest developing speed with electrostatic F-C paint Spray-painted aluminum profile and the maximum high-grade section bar of market demand.Aluminum current alloy is passivated
The commonly used chromate process of technique, at Aeronautics and Astronautics, automobile, household electrical appliances, build and obtain universal on the industry aluminium such as decoration
Application, but the hexavalent chromium compound contained in its technical recipe is a kind of toxic chemical, and dealing with improperly not only can be to environment
Cause and greatly pollute and meeting serious harm human health.Just because of this, chromate is by the environmental protection relevant departments of many countries
Being classified as extremely toxic product, within 2000, European Parliament is used for the Cr VI of component surface protective treatment by each automobile of ELVs law regulation
Consumption must not exceed 2g, and the ROHS of European Union clearly limits and includes Cr6+Six kinds of compositions, can be pre-in the use of electric/electronic device
Seeing, chromate application in the industry will be limited by more and more stricter.Although the most both at home and abroad to for chromium passivation film work
Skill has carried out a lot of research, and titanium zirconium system is the chromium-free treatment system developed the earliest, and current industrialized production major part is to use
The process solution of this titaniferous (zirconium) fluoro complex, but its passivating film is colourless, brings certain difficulty to industrial operation, combines
Close performance also to have much room for improvement, therefore these technology can't substitute chromate system completely.
Summary of the invention
It is an object of the invention to overcome above-mentioned deficiency, it is provided that a kind of aluminum alloy surface excellent corrosion resistance that gives is passivated
Film, and have low temperature fast filming, appearance color can naked eyes judge, the metal surface treating liquid of environmental friendliness feature.
Another object of the present invention is to provide a kind of method utilizing above-mentioned treatment fluid that aluminum alloy surface is processed.
The present invention is to realize above-mentioned purpose by following technical solution.
The present invention proposes to prepare the treatment fluid of corrosion resistance rare earth modified Ti-Zr system composite passivation film in aluminum alloy surface,
Its formula includes: the main salt of titanium, zirconium compounds, rare-earth salts auxiliary film for additive, oxidant, fluoride film forming accelerating, pH adjust
Joint agent, wetting agent, it is characterised in that described passivating solution is to utilize rare earth compound to become as the auxiliary of Ti-Zr inactivating treatment liquid
The main salt of film, gives the light yellow outward appearance of passivating film, has the quality of forming film scene property of can determine whether.In specifically every liter solution of its formula
Contain:
Potassium fluotitanate (fluotitanic acid) 0.5g L-1～10 g L-1
Potassium fluorozirconate (fluorine zirconic acid) 0.5g L-1～10 g L-1
Cerous nitrate (ceric sulfate, ammonium ceric nitrate) 0.5g L-1～5g L-1
Potassium nitrate 2g L-1～10g L-1
Sodium fluoride (potassium fluoride) 0.5g L-1～3g L-1
Dodecylbenzene sodium sulfonate or OP-10 0.5 g L-1～1 g L-1
Nitric acid 0.2mL L-1～5mL L-1
Boric acid 1 g L-1～5g L-1。
Present invention also offers the using method of above-mentioned passivating solution, it is characterised in that it comprises the steps.
(1) aluminium alloy is removed dust attachment.
(2) again aluminum alloy surface being made pretreatment, its technological process is, acid-soluble oil-water rinsing-alkali neutralization-water drift
Wash-naturally dry.
(3) using treatment fluid to be passivated processing, temperature is at 0～50 DEG C, and pH value is 1.5～5.0, and the immersion of aluminium alloy is anti-
It is 0.5～10min between Ying Shi；After having reacted, i.e. formed by answering that aluminum, titanium, zirconium, rare earth oxide form in aluminum alloy surface
Close passivating film.
(4) rinse Al alloy parts with water, dry,.
In above-mentioned steps (2), in described acid deoiling flow process, deoiling method is: 60～80 DEG C, 1～5min；Oil removal treatment
The main component of liquid: 5～15% sulphuric acid, 2～10% Fluohydric acid., 1～4mL L-1OP emulsifying agent, 0.1～2g L-1Thiourea.
In described alkali neutralization step, neutralization method is: 50～100 DEG C, 0.5～1min；The main one-tenth of alkali neutralisation treatment liquid
It is divided into 5% sodium hydroxide.
Described water rinse method is, in above-mentioned oil removing, neutralization flow process, each flow process is required at room temperature with pure after completing
Water purification is rinsed well in order to avoid producing excessive erosion and polluting next tank liquor.
The present invention selects fluotitanic acid (potassium), fluorine zirconic acid (potassium) to add as auxiliary film forming as main film forming component, rare-earth salts
Add agent and improve the compactness of passivating film and combination property by complex effect, and give the light yellow outward appearance of passivating film improve scene can
Judgement property, introduce potassium nitrate, Nitric Acid Oxidation agent improve film forming efficiency, can under room temperature or low temperature fast filming, introduce boric acid,
Nitric acid/potassium nitrate pH adjusting agent and wetting agent improve quality of forming film and stability of solution.By above film forming additive, preparation
Go out the Chrome-free yellow multiple elements design passivating film of good corrosion resistance, overcome the drawback that Ti-Zr system passivating film is colourless, it is achieved that low temperature
Efficiently fast filming, not only saves the energy, also improves production efficiency；Passivating film excellent corrosion prepared by this treatment fluid
The tack of good and coating is good, even film layer, light yellow in color, and preparation process need not heating, production efficiency high,
Little, the energy efficient to aluminium Influence of Fatigue Properties, the advantages such as environmental pollution is few, it is possible to replace the chromate gradually prohibitted the use of
Processing technique, the surface that can be widely used for aluminium alloy extrusions, aluminium alloy castings and Al-alloy products processes.
Detailed description of the invention
Solution of the present invention needs agitated after being configured to, so that solution is sufficiently mixed dissolving, and the main salt of film forming and oxidant
In the presence of, the reaction that passivating film generates can be expressed as.
The micro cathode of aluminum alloy surface, micro anode generation electrochemical reaction (are divided into micro anode and micro cathode aluminium alloy, sun
Pole: the aluminum solid solution phase relatively born for current potential；Negative electrode: may be the second phase or the intermetallic compound of crystal boundary precipitation of current potential calibration).
Anode: Al → Al3+ + 3e
Negative electrode: H+ + e→1/2 H2
NO3 - + 2H+ + e → NO2 +H2O
NO3 – + 3H+ + 2e → HNO2 + H2O。
The Al being dissolved down3+With the F in solution-There is following reaction, to keep solution-stabilized, promote the dissolving of aluminum.
Al3++6F-→AlF6 3-。
The Al being dissolved down3+There is following reaction with the fluotitanic acid root in solution, fluorine zirconate ion, generate Ti4+With Zr4 +Ion.
Al3++TiF6 2-→AlF6 3- + Ti4+
Al3++ZrF6 2-→AlF6 3- + Zr4+。
Due to negative electrode H+Consumption, result causes solution local ph to raise, and makes metal ion in solution occur as follows
Deposition reaction.
Ce3+ + 3OH- → Ce(OH)3↓→1/2Ce2O3+ 3/2H2O
2Al3+ + 6OH- → 2 Al (OH)3→Al2O3+ 3H2O
Ti4+ + 4OH- → Ti(OH)4↓→TiO2+ 2H2O
Zr4+ + 4OH- → Zr(OH)4↓→ZrO2+ 2H2O
2Al3+ + 6 F-→ Al2F6。
Contained passivating film defines by Al in aluminum alloy surface after being dried dehydration2O3、Ce2O3、TiO2、ZrO2And AlF6Composition
Composite oxides passivating film.
Main component in treatment fluid can be divided into six parts: main salt, oxidant, auxiliary film for additive rare-earth salts, rush
Enter agent, wetting agent, pH adjusting agent.The present embodiment selects fluotitanic acid (salt) and fluorine zirconic acid (salt) as main salt, nitric acid and potassium nitrate
For oxidant, fluoride is accelerator, and auxiliary film for additive rare-earth salts is Ce (NO3) 3Or Ce (SO4)2、(NH4)2Ce
(NO3)6 , dodecylbenzene sodium sulfonate or OP-10 are wetting agent.
Generally, fluotitanic acid (salt) and fluorine zirconic acid (salt) are as the main salt of film forming, certain limit inner membrance weight and thickness
Can increase along with the increase of its concentration, but fluotitanic acid (salt) is excessive as main salt consumption with fluorine zirconic acid (salt), film forming speed
Instead result in soon passivating film skewness or cause passivating film to ftracture, the problem such as come off, thus causes passivation corrosion resistance
Weaken.
Nitric acid and potassium nitrate play film forming oxidant effect, can accelerate the cathodic process of film forming in film forming electrochemical process,
When its content is relatively low, forming passivating film in aluminum alloy surface imperfect, concentration causes the most greatly passivating film to loosen.
Fluoride is relatively big on the impact of passivating film as film forming accelerating, when without fluoride or its content relatively low time,
The passivating film that aluminum alloy surface is formed is imperfect, is even difficult to film forming.When adding content of fluoride and being too high, easily cause aluminum and close
, there is brown point on passivating film surface in the excessive erosion of gold.
Auxiliary film for additive rare-earth salts can generate rare earth oxide when pH raises, and on the one hand can promote other oxide
Nucleation and growth, it is also possible to participate in film forming and generate containing the composite passivation film of rare earth oxide, improved by complex effect blunt
Change the decay resistance of film；On the other hand, it is light yellow that rare earth oxide makes passivating film present, and overcomes colourless the lacking of passivating film
Fall into, improve on-the-spot Chromating Film On Zn Deposits and can determine whether ability, but the passivating film generated when rare-earth salts concentration is the highest loosens on the contrary.
In film forming solution, add wetting agent dodecylbenzene sodium sulfonate (or OP-10) in a small amount, solution can be reduced
Surface tension, improves passivating film growth motive force and enters process, affect the dynamic growth of passivating film in micromechanism so that it is becoming
Film reaction is easier to be adsorbed onto the surface of aluminium alloy, improves passivating film at the deposition capability of aluminum alloy surface and adhesive force, also
The thickness increase of surfacing and passivating film can be increased.
Boric acid, nitric acid/potassium nitrate are as the pH adjusting agent of solution so that passivating solution pH stable is between 1.5～5.0.
Film forming situation is generally had a major impact by pH value of solution, in an acidic solution, in film forming accelerating F-Under the effect of ion, be conducive to
Oxidant reduction and being smoothed out of film forming procedure and form passivating film.
2. this passivating solution using method includes that step is as follows,, first by aluminium alloy remove attachment dirt；, again by aluminum
Alloy surface makees pretreatment, concrete grammar: dry up with water rinsing cold wind in acid deoiling-water rinsing-alkali.
Wherein.
(1) acid deoiling method and degreaser composition.
A. deoiling method is: 60～80 DEG C, 1～5min.
B. the main component of oil removal treatment liquid: 5～15% sulphuric acid, 2～10% Fluohydric acid., 1～4mL L-1OP emulsifying agent,
0.1～2g L-1Thiourea.
(2) alkali neutralization method and alkali nertralizer composition.
A. neutralization method is: 50～100 DEG C, 0.5～1min.
B. the main component of alkali neutralizer: 5% sodium hydroxide.
(3) water rinse method, each step is required for after completing at room temperature rinsing well with pure water in order to avoid producing corruption
Erosion.
3, using inactivating treatment liquid to carry out aluminum alloy surface Passivation Treatment, temperature controls at 0～50 DEG C, and pH value controls
1.5～5.0, be 0.5～10min with the aluminium alloy response time.
4, after having reacted, rinse Al alloy parts with water, dry,.
Embodiment 1.
A, by 6063 aluminum alloy surface remove attachment dirts, then rinse with pure water.
B, the aluminium alloy after a step process is immersed 15% sulphuric acid, 5% Fluohydric acid., 3mL L-1OP emulsifying agent, 0. 2g
L-1In 70 DEG C of acid deoiling liquid of thiourea, 2min carries out oil removing and the process removing oxide film dissolving, is disposed and rushes with pure water
Wash.
C, by after b step processes aluminium alloy immerse 5g L-1In the alkali neutralizer of sodium hydroxide, 0.5min is carried out in alkali
And process, react and rinsed with pure water.
D, the aluminium alloy after step c processes is placed in inactivating treatment liquid processes.Inactivating treatment liquid composition is fluorine titanium
Acid potassium 3g L-1, potassium fluorozirconate 2g L-1, cerous nitrate 1g L-1, potassium nitrate 5g L-1, sodium fluoride 0.8g L-1, dodecane
Base benzene sulfonic acid sodium salt 0.5g L-1, nitric acid 1.5mL L-1, boric acid 2 g L-1, regulation pH is 3.0, and temperature is 25 DEG C, the response time
For 3min.
E, by after Step d processes aluminium alloy pure water rinse, at a temperature of 80 DEG C be dried 8min, through above-mentioned process
6063 aluminum alloy surface formed one layer of preferable passivating film of light yellow corrosion resistance.
F, by the passivating film after Step d processes again carry out spray polyester powder coating process, through 210 DEG C of baking-curings
After, coating layer thickness controls at 60～120 m.The coating performance of aluminium section bar reaches the requirement of GB 5237.4-2008, passes through
After the acetic acid salt spray test of 1000h, corrosion-free, without obscission.
Embodiment 2.
By above-mentioned 2024 aluminium alloys after pretreatment as embodiment 1, it is placed in inactivating treatment liquid and processes.Passivation
Liquid composition is potassium fluotitanate 2.5g L-1, potassium fluorozirconate 2.5g L-1, ceric sulfate 2g L-1, potassium nitrate 3g L-1, potassium fluoride
0.5g·L-1、OP-10 0.5 g·L-1, nitric acid 0.8mL L-1, boric acid 3g L-1, regulation pH is 3.5, and temperature is 40 DEG C, instead
It is 2min between Ying Shi.Rinse with pure water after having reacted, naturally dry, kept dry.2024 treated aluminum alloy surface
Form the passivating film of one layer of light yellow excellent corrosion resistance, show themselves in that after being tested by the acetic acid salt spray of 1000h, corrosion-free, nothing
Obscission.
Only presently preferred embodiments of the present invention shown above, it is impossible to limit the right model of the present invention with this
Enclose, the equivalent variations therefore made according to scope of the present invention patent, still belong to the scope that the present invention is contained.
Claims (3)
1. the rare earth modified titanium zirconium system chemical passivation liquid processed for aluminium shape surface, its formula includes: titanium compound master
The main salt of salt, zirconium compounds, rare-earth salts auxiliary film for additive, oxidant, fluoride film forming accelerating, pH adjusting agent, wetting agent,
Wherein, the main salt of titanium compound is potassium fluotitanate, and the main salt of zirconium compounds is potassium fluorozirconate, and rare-earth salts auxiliary film for additive is nitric acid
Cerium or ceric sulfate or ammonium ceric nitrate, oxidant is potassium nitrate and nitric acid, and fluoride film forming accelerating is sodium fluoride or potassium fluoride,
PH adjusting agent is boric acid, potassium nitrate and nitric acid, and wetting agent is dodecylbenzene sodium sulfonate or OP-10, it is characterised in that described blunt
Changing liquid is to utilize rare earth compound as the main salt of auxiliary film forming of Ti-Zr inactivating treatment liquid, gives the light yellow outward appearance of passivating film, tool
Have the quality of forming film scene property of can determine whether, its formula specifically:
2. the using method of one kind processes for aluminium shape surface rare earth modified titanium zirconium system chemical passivation liquid, it is characterised in that
The method comprises the steps,
(1) aluminium alloy is removed dust attachment；
(2) again aluminum alloy surface being made pretreatment, its technological process is, acid deoiling-water rinsing-alkali neutralization-water rinsing-
Naturally dry；
(3) using treatment fluid to be passivated processing, temperature is at 0～50 DEG C, and pH value is 1.5～5.0, when the immersion of aluminium alloy is reacted
Between be 0.5～10min；After having reacted, i.e. aluminum alloy surface formed by aluminum, titanium, zirconium, rare earth oxide form compound blunt
Change film；
Here its formula of passivating solution liquid is specifically:
(4) rinse Al alloy parts with water, dry,.
The user of the rare earth modified titanium zirconium system chemical passivation liquid processed for aluminium shape surface the most according to claim 2
Method, it is characterised in that in above-mentioned steps (2), in described acid deoiling flow process, deoiling method is: 60～80 DEG C, 1～5min；Acid
The main component of property oil removal treatment liquid: 5～15% sulphuric acid, 2～10% Fluohydric acid., 1～4mL L-1OP emulsifying agent, 0.1～2g
L-1Thiourea；
In described alkali neutralization step, neutralization method is: 50～100 DEG C, 0.5～1min；Being mainly composed of of alkali neutralisation treatment liquid
5% sodium hydroxide；
Described water rinse method is, each flow process is required for after completing at room temperature using in above-mentioned acid deoiling, alkali and in flow process
Pure water is rinsed well in order to avoid producing excessive erosion and polluting next tank liquor.
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