CN103614716B - A kind of preparation method of environment-friendly type aluminum alloy surface rare earth inorganic compounding conversion film - Google Patents
A kind of preparation method of environment-friendly type aluminum alloy surface rare earth inorganic compounding conversion film Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of environment-friendly type aluminum alloy surface rare earth inorganic compounding conversion film, the aluminium test specimen good through surface preparation is placed in treatment solution and carries out Passivation Treatment, stir speed (S.S.) is 50-150r/min, and temperature is 20-35 DEG C, and the time is 3-10min; Then use washed with de-ionized water, cold wind dries up and get final product.Advantage of the present invention: treatment solution of the present invention is not containing chromium or other toxic substance, environment friendly and pollution-free, treatment process is simple, cost is low, and gained conversion film is golden yellow and uniformly continous is fine and close, grows in laminated form, film forming oxide diameter sizes is about 50nm and part is non-crystalline state, conversion film excellent anti-corrosion performance, alternative traditional chromic acid salt technique, has vast potential for future development.
Description
Technical field
The present invention relates to the corrosion and protection technical field of aluminium alloy, be specially a kind of preparation method of environment-friendly type aluminum alloy surface rare earth inorganic compounding conversion film.
Background technology
Aluminum alloy materials is that in industry, usage quantity is only second to ferrous materials, it is the metallic substance that in non-ferrous metal, usage quantity is maximum, application surface is the widest, because there is the advantage that density is little, specific tenacity is high, widespread use in communications and transportation, communication, electronics, packing business, aerospace and building trade field.But the active chemical property of aluminium alloy makes it corrosion of various ways easily occur in application process as spot corrosion, crevice corrosion, intergranular corrosion, stress corrosion etc., cause the wasting of resources, property damage even directly threatens life security, constrain the application of aluminium alloy.Although Aluminum-aluminum alloy forms the oxide film of one deck thin (thickness is 1-3nm) on its surface; but its protective capability extreme difference; and the bonding strength of the organic coating such as natural oxide film and paint is low, easily there is corrosion in use procedure and make its performance degradation or reduction in Al and Alalloy under arms.In the surface protection technique of aluminium, the chemical conversion coating of aluminium alloy for preparing transitional interlayer before the protective coating on its surface or spraying, to improve the sticking power of coating, improves solidity to corrosion and the protection efficiency of coating in a large number.The surface chemistry transformation technology of aluminium becomes aluminium alloy broadened application scope and the indispensable gordian technique that increases the service life.
Traditional chromic salt chemical conversion processing method can be good at the etching problem solving aluminium alloy, but owing to containing sexavalent chrome human body to carcinogenesis in treatment solution, also can cause environmental pollution if deal with improperly.Many countries such as the countries such as the U.S., Japan, European Union or tissue prohibites use sexavalent chrome in the world." about prohibitting the use some Hazardous Substances Directive in electronic electric equipment " (ROHS) of European Union announced on January 23rd, 2003, was the use that first plaintext forbids poisonous chromium ion, and implemented on July 1st, 2006.China also prohibits the use poisonous sexavalent chrome on January 19th, 2010.The chromiumfree conversion treatment technology of therefore researching and developing environment-friendly type becomes the development inexorable trend of conversion processing technology, and it is very necessary for widening effective utilization of aluminium alloy and purposes.
The process of current environment-friendly type Al and Alalloy surface chemical conversion film is as rare earth metal salt, molybdate process, cobalt salt process, tungstate, manganate, titanium salt or zirconates, and the method for the conversion film process such as titanium zirconates is more, as patent (ZL200510010441.0) discloses a kind of rare-earth transfer film method improving light metal and composite material surface erosion resistance thereof, do not affect the mechanical property of body material, there is good preservative property and environment friendly and pollution-free performance.Number of patent application (200710027057.0) disclose a kind of aluminum alloy surface containing cobaltic main salt, permanganate and nitrate be the conversion treating solution of composite oxidant; Japanese Patent JP2004018992-A discloses and adopts titanium salt, zirconates prepares conversion film in aluminum alloy surface; Patent 200610046292.8 and 200410051673.6 etc. has been invented and has been prepared conversion film at aluminum alloy surface zirconates, titanium salt and phosphoric acid salt or organic acid etc. as conversion treating solution.Number of patent application 201110198490.7 discloses a kind of process preparing golden yellow sodium aluminum fluoride conversion film in aluminum alloy surface also i.e. treatment process, overcomes the shortcoming that the colourless and treatment temp of titanium zirconium conversion film prepared by prior art is high.Other number of patent application is the conversion film treatment process that the Chinese invention patent such as 200710034656,200710158469,200910085265,201110399391,201210076122,201110024810.7,201310187909.8 and patent 101525746A all relate to environment-friendly chromium-free.Existing aluminum alloy surface chromium-free treatment method and traditional chromic salt process still have a certain distance on corrosion resistance nature and self-reparing capability, develop new environment-friendly chromium-free treatment agent and treatment process thereof and remain Hot spots for development from now on and trend.
Summary of the invention
The present invention is the defect that the part solving prior art exists, and provides a kind of preparation method of environment-friendly type aluminum alloy surface rare earth inorganic compounding conversion film.This preparation method's technical process is simple, cost is low, treatment temp is normal temperature, the treatment time is short, and the conversion film that the present invention obtains is in golden yellow and uniformly continous is fine and close, corrosion resistance and good, close to the antiseptic power of chromate film.
The lower technical scheme that the present invention solves the problems of the technologies described above is as follows:
1. a preparation method for environment-friendly type rare earth inorganic compounding conversion film, operates according to the following steps:
The first step: the surface preparation of aluminum alloy specimen:
(1) mechanical pretreatment
Washed with deionized water after 600#, 800# and 1000# sand paper step by step mechanical polishing respectively on aluminum alloy specimen surface, per pass washing time is 2-5min; Use acetone or alcohol ultrasonic cleaning 5-10min again;
(2) Chemical Pretreatment
1) degreasing
By pretreated aluminum alloy specimen degreasing fluid: 30g/LNaOH, 8g/LNa
2cO
3, 12g/LNa
3pO
412H
2o, under temperature is 50-65 DEG C of condition, the soak degreasing time is 2-5min, obtains the aluminum alloy specimen after degreasing;
2) alkali, acid etch
1. by the aluminum alloy specimen Alkaline etchant after degreasing: 20g/LNaOH, 4g/LNa
2cO
3, alkali leaching under temperature is 45-60 DEG C of condition, the time is 2-5min;
The salpeter solution acidleach at ambient temperature of the aluminum alloy specimen 30wt% after 2. alkali being corroded, the time is 2-5min;
Second step: the preparation of conversion coating treating fluid:
First add a certain amount of deionized water in a reservoir, be added into described rare-earth salts 5.0-20.0g/L, titanate 3.0-15.0g/L, manganese salt 1.0-4.0g/L, fluorochemical 0.1-0.5g/L and tensio-active agent 0.3-1.5g/L again, stirring after fully dissolving adopts a kind of pH value of conversion treating solution that regulates in conditioning agent sodium hydroxide, potassium hydroxide or ammoniacal liquor to be 1.5-4.0, namely prepares to obtain treatment solution;
Described treatment solution is for preparation of raw material forms with rare-earth salts, titanate, manganese salt, fluorochemical and tensio-active agent;
Described rare-earth salts is one or more the arbitrary proportion mixture in Cerium II Chloride, Lanthanum trichloride, cerous nitrate, lanthanum nitrate;
Described titanate is one or more the arbitrary proportion mixture in potassium fluotitanate, hydrofluotitanic acid;
Described manganese salt is one or more the arbitrary proportion mixture in potassium permanganate and ammonium permanganate;
Described fluorochemical is one or more the arbitrary proportion mixture in sodium hydrogen fluoride, Sodium Fluoride, Potassium monofluoride;
Described tensio-active agent is one or more the arbitrary proportion mixture in Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, Witco 1298 Soft Acid ammonium;
3rd step: conversion film conversion processing
Aluminum alloy specimen after soda acid is corroded process is placed in treatment solution, mechanical stirring, speed are 50-150r/min, stir 3-10min under temperature is 20-35 DEG C of condition after, densification is continuously formed and uniform golden yellow rare earth inorganic compounding conversion film in aluminum alloy surface, take out sample, clean by washed with de-ionized water, and dry up with cold wind and get final product;
Gained conversion film is golden yellow and uniformly continous is fine and close, the growth in laminated form, the oxide compound of the chemical constitution of the conversion film mainly oxyhydroxide of rare earth RE and oxide compound, Ti and Mn.Film forming oxide diameter sizes is about 50nm and part is non-crystalline state, and conversion film thickness is 0.8-2.0 μm.
Compared with prior art, the beneficial effect that can reach is as follows for the preparation method of environment-friendly type rare earth inorganic compounding conversion film of the present invention:
1. to prepare the conversion treating solution composition and engineering of rare earth inorganic compounding conversion film simple in the present invention, and cost is low, and treatment temp is room temperature, does not need heating, at room temperature can fast filming, and film formation time is 3-10min;
2. environment-friendly type rare earth inorganic compounding conversion film of the present invention is in golden yellow and uniformly continous is fine and close;
3. the oxide compound of environment-friendly type rare earth inorganic compounding conversion film the chemical constitution of the present invention mainly oxyhydroxide of rare earth RE and oxide compound, Ti and Mn, film forming oxide particle diameter is about 50nm; Partial oxide is non-crystalline state;
4. environment-friendly type rare earth inorganic compounding conversion film of the present invention has excellent corrosion resistance nature;
5. rare earth inorganic compounding conversion film preparation process non-pollutant discharge of the present invention, belong to environmentally friendly technology, be expected to alternative traditional chromic acid salt treatment process and phosphorization treatment process, application prospect is good.
Accompanying drawing illustrates:
Fig. 1 is the SEM picture of conversion film prepared by the embodiment of the present invention 1.
Fig. 2 is the SEM picture of conversion film prepared by the embodiment of the present invention 2.
Fig. 3 is the SEM picture of conversion film prepared by the embodiment of the present invention 3.
Fig. 4 is the TEM picture of conversion film prepared by the embodiment of the present invention 3.
Fig. 5 is the TEM-SADP picture of conversion film prepared by the embodiment of the present invention 3.
Fig. 6 is the TEM-EDS picture of conversion film prepared by the embodiment of the present invention 3.
Fig. 7 is the XRD figure spectrum of conversion film prepared by the embodiment of the present invention 3.
Fig. 8 is the AFM collection of illustrative plates of conversion film prepared by the embodiment of the present invention 4.
Embodiment:
Below in conjunction with embodiment, the invention will be further described, but implementation method of the present invention is not limited thereto.
Embodiment 1
The preparation of environment-friendly type rare earth inorganic compounding conversion film
1. aluminum alloy specimen surface preparation:
1) be 3mm rolling 6061 aluminium alloy plate linear cutter by thickness be the test piece of 30 × 30mm, sample is successively through 600#, 800# and 1000# sand paper mechanical polishing step by step, and by washed with de-ionized water, under then adopting acetone or alcohol ultrasonic wave room temperature, clean 5min;
2) by step 1) process after aluminum alloy specimen be placed in degreasing fluid (30g/LNaOH, 8g/LNa
2cO
3, 12g/LNa
3pO
412H
2o, temperature is 55 DEG C, and the time is 3min, Hou Yong bis-road deionized water room temperature cleaning 3min.3) through step 2) process after sample be placed in Alkaline etchant (20g/LNaOH, 4g/LNa
2cO
3, temperature is 50 DEG C) and 3min, Hou Yong bis-road deionized water room temperature cleaning 3min.
4) by step 3) sample that processes immerses after room temperature 30wt% salpeter solution carries out optical processing 3min, adopts two road washed with de-ionized water.
The aluminum alloy surface pretreatment technology of following example and example 1 are together.
2. the preparation of rare earth inorganic compounding conversion coating treating fluid: cerous nitrate 5.0g/L, potassium fluotitanate 3.0g/L, potassium permanganate 1.0g/L, Sodium Fluoride 0.1g/L and Sodium dodecylbenzene sulfonate 0.3g/L.By each component: cerous nitrate 1.0g, potassium fluotitanate 0.6g, potassium permanganate 0.2g, Sodium Fluoride 0.02g and Sodium dodecylbenzene sulfonate 0.06g are soluble in water, and add water and make treatment solution be 200ml, adjust ph is 1.5.Adopt magnetic agitation in solution preparation process, speed is 100r/min.
3. aluminum alloy surface rare earth inorganic compounding conversion film conversion processing: aluminum alloy specimen step 1 pre-treatment obtained immerses in the treatment solution of step 2, treatment temp is 35 DEG C, dipping 10min, keep magnetic machinery to stir in treating processes, stirring velocity is 50r/min always.Complete film forming, take out sample, clean by washed with de-ionized water, and dry up with cold wind.
Adopt the corrosion resistance nature of topical application test conversion film.The etchant solution that described dropping corrosion test adopts is 3g potassium bichromate (K
2cr
2o
7)+25mL concentrated hydrochloric acid (HCl)+75mL distilled water (H
2o), it is the anti-corrosion time that surperficial drop solution of materialsing becomes green mean time by yellow.
Following embodiment gained conversion film corrosion resistance nature testing method and example 1 are together.
Adopt scanning electron microscope to carry out morphology analysis, the SEM figure of gained conversion film as shown in Figure 1.The surface of conversion film is continuous, fine and close, even, does not have obvious crackle.
Embodiment 2
The preparation of environment-friendly type rare earth inorganic compounding conversion film
Difference from Example 1 is:
1. the preparation of rare earth inorganic compounding conversion coating treating fluid: cerous nitrate 20.0g/L, hydrofluotitanic acid 15.0g/L, potassium permanganate 4.0g/L, Sodium Fluoride 0.5g/L and Sodium dodecylbenzene sulfonate 1.5g/L.By each component: cerous nitrate 4.0g, hydrofluotitanic acid 3.0g, potassium permanganate 0.8g, Sodium Fluoride 0.1g and Sodium dodecylbenzene sulfonate 0.3g are soluble in water, and add water and make treatment solution be 200ml, adjust ph is 4.Adopt magnetic agitation in solution preparation process, speed is 100r/min.
2 aluminum alloy surface rare earth inorganic compounding conversion film conversion processing: aluminum alloy specimen pre-treatment obtained immerses in the treatment solution of step 1, and treatment temp is 20 DEG C, dipping 3min, keep magnetic machinery to stir in treating processes, stirring velocity is 150r/min always.Complete film forming, take out sample, clean by washed with de-ionized water, and dry up with cold wind.
Adopt scanning electron microscope to carry out morphology analysis, the SEM figure of gained conversion film as shown in Figure 2.The surface of conversion film is continuous, fine and close, even, does not have remarkable crackle.
Embodiment 3
The preparation of environment-friendly type rare earth inorganic compounding conversion film
Difference from Example 1 is:
1. the preparation of rare earth inorganic compounding conversion coating treating fluid: cerous nitrate 15.0g/L, potassium fluotitanate 7.5g/L, potassium permanganate 2.5g/L, Sodium Fluoride 0.3g/L and sodium laurylsulfonate 0.5g/L.By each component: cerous nitrate 3.0g, potassium fluotitanate 1.5g, potassium permanganate 0.5g, Sodium Fluoride 0.06g and sodium laurylsulfonate 0.1g are soluble in water, and add water and make treatment solution be 200ml, adjust ph is 2.Adopt magnetic agitation in solution preparation process, speed is 100r/min.
2. aluminum alloy surface rare earth inorganic compounding conversion film conversion processing: aluminum alloy specimen pre-treatment obtained immerses in the treatment solution of step 1, and treatment temp is 30 DEG C, dipping 5min, keep magnetic machinery to stir in treating processes, stirring velocity is 100r/min always.Complete film forming, take out sample, clean by washed with de-ionized water, and dry up with cold wind.
Adopt Electronic Speculum, energy spectrometer (EDS) and X-ray diffractometer (XRD) to carry out conversion film surface microscopic topographic, chemical composition and material phase analysis, the SEM of gained conversion film figure, TEM figure and TEM-EDS scheme and XRD figure as Fig. 3,4,5, shown in 6 and 7.The surface of conversion film is continuous, fine and close, even, does not have obvious crackle, becomes the particle diameter of membrane granule to be about 50nm.The thing phase composite mainly oxyhydroxide of rare earth RE and the oxide compound of oxide compound, titanium and manganese of conversion film, its content is about 10%, 60 and 25% respectively, and partial oxide is non-crystalline state.Form the oxide stability of conversion film, self-healing property and corrosion resistance and good.
Embodiment 4
The preparation of environment-friendly type rare earth inorganic compounding conversion film
Difference from Example 1 is:
(1) preparation of rare earth inorganic compounding conversion coating treating fluid: lanthanum nitrate 20.0g/L, potassium fluotitanate 10.0g/L, ammonium permanganate 3.0g/L, Potassium monofluoride 0.2g/L and Witco 1298 Soft Acid ammonium 1.0g/L.By each component: lanthanum nitrate 4.0g, potassium fluotitanate 2.0g, ammonium permanganate 0.6g, Potassium monofluoride 0.04g and Witco 1298 Soft Acid ammonium 0.2g are soluble in water, and add water and make treatment solution be 200ml, adjust ph is 3.0.Adopt magnetic agitation in solution preparation process, speed is 100r/min.
(2) aluminum alloy surface rare earth inorganic compounding conversion film conversion processing: aluminum alloy specimen pre-treatment obtained immerses in the treatment solution of step (1), treatment temp is 25 DEG C, dipping 6min, keep magnetic machinery to stir in treating processes, stirring velocity is 120r/min always.Complete film forming, take out sample, clean by washed with de-ionized water, and dry up with cold wind.
Adopt atomic force microscope to carry out Morphology analysis, the AFM figure of gained conversion film as shown in Figure 8.Conversion film is laminated form growth, and the ladder of film growth is maximum is about 0.3 μm.
Embodiment 5
The preparation of environment-friendly type rare earth inorganic compounding conversion film
Difference from Example 1 is:
1. the preparation of rare earth inorganic compounding conversion coating treating fluid: Lanthanum trichloride 10.0g/L, hydrofluotitanic acid 15.0g/L, ammonium permanganate 2.0g/L, sodium hydrogen fluoride 0.4g/L and sodium laurylsulfonate 1.2g/L.By each component: Lanthanum trichloride 2.0g, hydrofluotitanic acid 3.0g, ammonium permanganate 0.4g, sodium hydrogen fluoride 0.08g and sodium laurylsulfonate 0.24g are soluble in water, and add water and make treatment solution be 200ml, adjust ph is 2.5.Adopt magnetic agitation in solution preparation process, speed is 100r/min.
2. aluminum alloy surface rare earth inorganic compounding conversion film conversion processing: aluminum alloy specimen pre-treatment obtained immerses in the treatment solution of step 1, and treatment temp is 30 DEG C, dipping 8min, keep magnetic machinery to stir in treating processes, stirring velocity is 100r/min always.Complete film forming, take out sample, clean by washed with de-ionized water, and dry up with cold wind.
Embodiment 6
The preparation of environment-friendly type rare earth inorganic compounding conversion film
Difference from Example 1 is:
1. the preparation of rare earth inorganic compounding conversion coating treating fluid: Cerium II Chloride 15.0g/L, hydrofluotitanic acid 12.0g/L, ammonium permanganate 3.5g/L, Sodium Fluoride 0.3g/L and Sodium dodecylbenzene sulfonate 1.0g/L.By each component: Cerium II Chloride 3.0g, hydrofluotitanic acid 2.4g, ammonium permanganate 0.7g, Sodium Fluoride 0.06g and Sodium dodecylbenzene sulfonate 0.2g are soluble in water, and add water and make treatment solution be 200ml, adjust ph is 3.5.Adopt magnetic agitation in solution preparation process, speed is 100r/min.
2. aluminum alloy surface rare earth inorganic compounding conversion film conversion processing: aluminum alloy specimen pre-treatment obtained immerses in the treatment solution of step 1, and treatment temp is 25 DEG C, dipping 4min, keep magnetic machinery to stir in treating processes, stirring velocity is 150r/min always.Complete film forming, take out sample, clean by washed with de-ionized water, and dry up with cold wind.
Prepared by each embodiment, the corrosion resistance nature of conversion film is as shown in table 1.
Table 1
Claims (1)
1. a preparation method for environment-friendly type rare earth inorganic compounding conversion film, is characterized in that, operates according to the following steps:
The first step: the surface preparation of aluminum alloy specimen:
(1) mechanical pretreatment
Washed with deionized water after 600#, 800# and 1000# sand paper step by step mechanical polishing respectively on aluminum alloy specimen surface, per pass washing time is 2-5min; Use acetone or alcohol ultrasonic cleaning 5-10min again;
(2) Chemical Pretreatment
1) degreasing
By pretreated aluminum alloy specimen degreasing fluid: 30g/LNaOH, 8g/LNa
2cO
3, 12g/LNa
3pO
412H
2o, under temperature is 50-65 DEG C of condition, the soak degreasing time is 2-5min, obtains the aluminum alloy specimen after degreasing;
2) alkali, acid etch
1. by the aluminum alloy specimen Alkaline etchant after degreasing: 20g/LNaOH, 4g/LNa
2cO
3, alkali leaching under temperature is 45-60 DEG C of condition, the time is 2-5min;
The salpeter solution acidleach at ambient temperature of the aluminum alloy specimen 30wt% after 2. alkali being corroded, the time is 2-5min;
Second step: the preparation of conversion coating treating fluid:
Described conversion coating treating fluid is for preparation of raw material forms with rare-earth salts, titanate, manganese salt, fluorochemical and tensio-active agent;
Described rare-earth salts is more than one the arbitrary proportion mixture in Cerium II Chloride, Lanthanum trichloride, cerous nitrate, lanthanum nitrate;
Described titanate is more than one the arbitrary proportion mixture in potassium fluotitanate, hydrofluotitanic acid;
Described manganese salt is more than one the arbitrary proportion mixture in potassium permanganate and ammonium permanganate;
Described fluorochemical is more than one the arbitrary proportion mixture in sodium hydrogen fluoride, Sodium Fluoride, Potassium monofluoride;
Described tensio-active agent is more than one the arbitrary proportion mixture in Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, Witco 1298 Soft Acid ammonium;
First add a certain amount of deionized water in a reservoir, be added into described rare-earth salts 5.0-20.0g/L, titanate 3.0-15.0g/L, manganese salt 1.0-4.0g/L, fluorochemical 0.1-0.5g/L and tensio-active agent 0.3-1.5g/L again, stirring after fully dissolving adopts a kind of pH value of conversion treating solution that regulates in conditioning agent sodium hydroxide, potassium hydroxide or ammoniacal liquor to be 1.5-4.0, namely prepares to obtain conversion coating treating fluid;
3rd step: conversion film conversion processing
Aluminum alloy specimen after soda acid is corroded process is placed in conversion coating treating fluid, mechanical stirring, speed are 50-150r/min, stir 3-10min under temperature is 20-35 DEG C of condition after, densification is continuously formed and uniform golden yellow rare earth inorganic compounding conversion film in aluminum alloy surface, take out sample, clean by washed with de-ionized water, and dry up with cold wind and get final product;
Gained conversion film is golden yellow and uniformly continous is fine and close, grow in laminated form, the oxide compound of the chemical constitution of the conversion film mainly oxyhydroxide of rare earth and oxide compound, Ti and Mn, film forming oxide diameter sizes 50nm and part are in non-crystalline state, and conversion film thickness is 0.8-2.0 μm.
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