CN111304643A - Passivating agent for surface treatment of aluminum alloy material and preparation method thereof - Google Patents
Passivating agent for surface treatment of aluminum alloy material and preparation method thereof Download PDFInfo
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- CN111304643A CN111304643A CN202010224085.7A CN202010224085A CN111304643A CN 111304643 A CN111304643 A CN 111304643A CN 202010224085 A CN202010224085 A CN 202010224085A CN 111304643 A CN111304643 A CN 111304643A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
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Abstract
The invention relates to the technical field of metal surface treatment, in particular to a passivator for aluminum alloy material surface treatment and a preparation method thereof. The preparation raw materials of the passivator for the surface treatment of the aluminum alloy material at least comprise the following components in parts by weight: 3-12 parts of film-forming agent, 5-15 parts of complexing agent, 1-6 parts of oxidant, 1-3 parts of additive and 60-90 parts of water. The passivating agent prepared by the invention can form a compact passivating film on the surface of metal, and has excellent salt mist resistance stability and sulfur dioxide corrosion resistance.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a passivator for aluminum alloy material surface treatment and a preparation method thereof.
Background
The aluminum alloy is obtained by adding elements such as magnesium, zinc, copper and the like into pure aluminum, and has a series of advantages of small specific gravity, high mechanical strength, excellent electrical conductivity, thermal conductivity, corrosion resistance and the like, so that the aluminum alloy has wide application prospects and irreplaceable positions in the aviation, aerospace, ship, nuclear industry and weapon industry, and the aluminum alloy technology is listed as a key technology and a basic technology for key development of national defense science and technology.
Pure aluminum has high corrosion resistance because it can form a thin and dense oxide film with oxygen in the air, but after other metal elements are added into the aluminum alloy, the aluminum alloy is easy to generate galvanic effect due to different electrode potentials of the metals and the generation of a second phase, thereby causing the corrosion of the aluminum alloy. The aluminum alloy needs to be subjected to corresponding surface treatment before use so as to meet the adaptability and safety of the aluminum alloy to the environment, the corrosion resistance of the aluminum and the aluminum alloy surface is remarkably improved after chromate passivation treatment, and the aluminum and aluminum alloy surface has excellent adhesion to a coating. At present, a large amount of hexavalent chromium-containing wastewater is generated in the chromate treatment process and is discharged, so that pollution is caused. In view of the pressure of environmental protection, the use of chromium-free environment-friendly treatment solutions is increasing, and researchers in various countries strive to develop more effective and environment-friendly metal surface treatment solutions to reduce hexavalent chromium emission and alleviate the influence of environmental pollution. The chromium-free passivation film system applied in industry is mostly in the direction of titanium system, zirconium system, silane system or rare earth system, but the current research in all directions has no satisfactory research result, and the corrosion protection performance of the product in all directions to metal and the adhesive force performance of the product in all directions can not be comparable with the chromium-free passivation film.
Trivalent chromium, which is only 1% toxic to hexavalent chromium and has properties similar to hexavalent chromium in many respects, is considered to be the most accepted alternative process for passivation of hexavalent chromium, and for this reason, the development of a passivator containing trivalent chromium and having excellent corrosion resistance has been the focus of the development of those skilled in the art.
Disclosure of Invention
In order to solve the technical problems, the invention provides a passivating agent for surface treatment of an aluminum alloy material, which comprises the following raw materials in parts by weight: 3-12 parts of film-forming agent, 5-15 parts of complexing agent, 1-6 parts of oxidant, 1-3 parts of additive and 60-90 parts of water.
As a preferred technical solution of the present invention, the film forming agent is selected from one or more of chromium nitrate, basic chromium sulfate, and chromium chloride.
As a preferable technical scheme, the film forming agent is basic chromium sulfate.
As a preferred technical solution of the present invention, the complexing agent is a fluorine compound.
In a preferred embodiment of the present invention, the fluorine-based compound is one or more selected from the group consisting of sodium fluoride, ammonium bifluoride, potassium fluorozirconate, potassium fluoride and fluorozirconate.
In a preferred embodiment of the present invention, the oxidizing agent is one or more selected from sodium nitrate, potassium nitrate, cobalt nitrate, lanthanum nitrate, and cerium nitrate.
As a preferable technical solution of the present invention, the oxidant is a combination of cobalt nitrate and cerium nitrate, wherein the mass ratio of cobalt nitrate to cerium nitrate is 1: (1-3).
As a preferable technical scheme of the invention, the additive is nano silica sol.
As a preferable technical scheme of the invention, the particle size of the nano silica sol is 10-50 nm.
The invention provides a preparation method of a passivator for surface treatment of an aluminum alloy material, which comprises the following steps: dissolving film-forming agent, complexing agent, oxidant and additive in water, stirring, and adjusting pH to 3.6-4.5 with sodium hydroxide and dilute sulfuric acid.
Has the advantages that: the invention provides a passivator for surface treatment of an aluminum alloy material and a preparation method thereof. The passivating agent prepared by the invention can form a compact passivating film on the metal surface, can improve the salt spray resistance stability and the sulfur dioxide corrosion resistance of a metal material compared with the traditional passivating agent, is more environment-friendly in the manufacturing process, saves the cost, and is particularly suitable for aluminum alloy materials. When the passivating agent provided by the invention is used in combination with a sealing agent to carry out surface treatment on an aluminum alloy material, the salt mist resistance and the corrosion resistance of the aluminum alloy material are better; in addition, the passivator provided by the invention belongs to a trivalent chromium passivator, the corrosion resistance of the passivator is equivalent to that of a hexavalent chromium conversion film, the problems of environment, potential safety hazards and the like in the process of the traditional hexavalent chromium conversion film process can be solved, the use process is safe and environment-friendly, and the development prospect is considerable.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
In order to solve the technical problems, the invention provides a passivating agent for surface treatment of an aluminum alloy material, which comprises the following raw materials in parts by weight: 3-12 parts of film-forming agent, 5-15 parts of complexing agent, 1-6 parts of oxidant, 1-3 parts of additive and 60-90 parts of water.
In a preferred embodiment, the passivating agent for surface treatment of an aluminum alloy material according to the present invention is prepared from at least: 5-10 parts of film-forming agent, 6-11 parts of complexing agent, 2-5 parts of oxidant, 1.5-2.5 parts of additive and 75-85 parts of water.
In a most preferred embodiment, the passivating agent for surface treatment of an aluminum alloy material according to the present invention is prepared from at least the following raw materials in parts by weight: 6 parts of film-forming agent, 7.5 parts of complexing agent, 3 parts of oxidizing agent, 2 parts of additive and 81.5 parts of water.
Film forming agent
The film forming agent is a main film forming substance in the passivator, wherein the film forming substance mainly refers to trivalent chromium ions, and the trivalent chromium ions can be obtained by dissolving trivalent chromium salt.
In a preferred embodiment, the film forming agent is selected from one or more of chromium nitrate, basic chromium sulfate and chromium chloride.
In a most preferred embodiment, the film former of the present invention is basic chromium sulfate.
The basic chromium sulfate is mainly used for tanning leather. Is a raw material for producing the chromium hydroxide. The dye industry is used to produce reactive black dyes. The printing and dyeing industry is used as a mordant. It should be stored in a cool, ventilated and dry storehouse. The packaging container is to be sealed and moisture-proof. The basic chromium sulfate can not be stored and transported together with edible articles, organic matters, inflammable matters and acids. The transportation needs to be protected from rain and burning sun. The package should be carefully handled to prevent damage to the package.
Complexing agents
The complexing agent in the invention refers to a compound capable of forming complex ions with metal ions. At room temperature, trivalent chromium ions in the passivating agent exist in the form of stable hexahydrate in water, and the existence of the trivalent chromium ions is relatively stable, so that the passivation film forming process of the trivalent chromium ions is not facilitated. For this reason, it is necessary to replace a part of the water molecules in the hydrated ions with other ligands in order to form a ligand complex which facilitates the progress of the passivation reaction.
In a preferred embodiment, the complexing agent of the present invention is a fluorine-based compound.
In a more preferred embodiment, the fluorine-based compound according to the present invention is selected from one or more of sodium fluoride, ammonium bifluoride, potassium fluorozirconate, potassium fluoride, and fluorozirconate.
In a more preferred embodiment, the fluorine-based compound of the present invention is a combination of potassium fluorozirconate, potassium fluoride and fluorozirconic acid, wherein the mass ratio of potassium fluorozirconate to fluorozirconic acid is (2.5 to 11): 1: (1-3).
In a more preferred embodiment, the fluorine compound of the present invention is a combination of potassium fluorozirconate, potassium fluoride and fluorozirconic acid, wherein the mass ratio of potassium fluorozirconate to fluorozirconic acid is (4-8): 1: (1-2).
In a most preferred embodiment, the fluorine compound of the present invention is a combination of potassium fluorozirconate, potassium fluoride and fluorozirconic acid, wherein the mass ratio of potassium fluorozirconate to fluorozirconic acid is 5: 1: 1.5.
oxidizing agent
The oxidizing agent in the present invention means a substance that can obtain electrons in an oxidation reaction, and may also mean a substance that can obtain oxygen from another substance. According to the electron capacity of the substance, the substance can be divided into a strong oxidant, a medium-strength oxidant and a weak oxidant to describe the performance of the substance in the oxidation-reduction process.
In the present invention, the oxidizing agent serves as an essential component of the passivating agent, and serves to ionize the metal.
In a preferred embodiment, the oxidant according to the present invention is selected from one or more of sodium nitrate, potassium nitrate, cobalt nitrate, lanthanum nitrate, and cerium nitrate.
In a more preferred embodiment, the oxidant of the present invention is a combination of cobalt nitrate and cerium nitrate, wherein the mass ratio of cobalt nitrate to cerium nitrate is 1: (1-3).
In a most preferred embodiment, the oxidant of the present invention is a combination of cobalt nitrate and cerium nitrate, wherein the mass ratio of cobalt nitrate to cerium nitrate is 1: 1.
additive agent
In a preferred embodiment, the additive of the present invention is a nanosilica sol.
The nano silica sol is a dispersion liquid of nano silica particles in water or a solvent. Due to SiO in the silica sol2Contains a large amount of water and hydroxyl groups, so that the silica sol can also be expressed as mSiO2.nH2And O. There are different approaches to the preparation of silica sols. The most commonly used methods are ion exchange, one-step hydrolysis of silicon powder, silane hydrolysis, etc.
In a more preferred embodiment, the nano silica sol of the present invention has a particle size of 10 to 50 nm.
In a more preferred embodiment, the nano silica sol of the present invention has a particle size of 10 to 20 nm.
In a most preferred embodiment, the nanosilica sol according to the invention has a particle size of 15 nm.
The nano silica sol can be obtained from commercial sources including but not limited to
The inventor finds in experiments that the passivator provided by the invention has excellent salt spray resistance stability and sulfur dioxide corrosion resistance after being applied to aluminum materials, wherein basic chromium sulfate is used as a film forming agent, so that complex compounds can be formed with metal ions and hydroxide ions, and a compact passivation film can be formed on the surface of a metal material; in addition, the invention also finds that the addition of the complexing agent is beneficial to the passivation reaction of trivalent chromium ions, but if the action of the complexing agent is too strong, the complexing agent is not beneficial to the formation of a passivation film by the trivalent chromium ions, and if the complexing action is too weak, the stability of the passivating agent is poor, and the glossiness of the film layer is poor; through the research of the invention for many years, on the basis that basic chromium sulfate is selected as a film forming agent and cobalt nitrate and cerium nitrate are selected as oxidizing agents, the invention further selects the combination of potassium fluozirconate, potassium fluoride and fluozirconate as a complexing agent, can effectively improve the film forming quality of the passivating agent, and particularly the mass ratio of the potassium fluozirconate to the fluozirconate is (2.5-11): 1: (1-3), the effect is best, finally, the invention also adopts nano silica sol as an additive, regulates and controls the particle size of the nano silica sol, uniformly fills the nano silica sol in the pores of the passivation film layer, enhances the compactness of the passivation film and greatly improves the corrosion resistance of the passivation film.
The invention provides a preparation method of a passivator for surface treatment of an aluminum alloy material, which comprises the following steps: dissolving film-forming agent, complexing agent, oxidant and additive in water, stirring, and adjusting pH to 3.6-4.5 with sodium hydroxide and dilute sulfuric acid.
It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the raw materials used are commercially available from national chemical reagents, unless otherwise specified.
Examples
In order to better understand the above technical solutions, the following detailed descriptions will be provided with reference to specific embodiments. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention. In addition, the raw materials are commercially available and the extraction methods of the extract are all conventional extraction methods, if not otherwise specified.
Example 1
The passivator for the surface treatment of the aluminum alloy material is characterized by comprising the following preparation raw materials in parts by weight: 6 parts of film-forming agent, 7.5 parts of complexing agent, 3 parts of oxidizing agent, 2 parts of additive and 81.5 parts of water.
The film forming agent is basic chromium sulfate.
The complexing agent is a fluorine compound.
The fluorine compound is a combination of potassium fluozirconate, potassium fluoride and fluozirconic acid, wherein the mass ratio of the potassium fluozirconate to the fluozirconic acid is 5: 1: 1.5.
the oxidant is a combination of cobalt nitrate and cerium nitrate, wherein the mass ratio of the cobalt nitrate to the cerium nitrate is 1: 1.
the additive is nano silica sol.
The nanometer silica sol has a particle size of 15nm, is commercially available, and is manufactured by Kohn silicon products, Inc. of Linyi City, with the model of KHAS-25.
The preparation method of the passivator for the surface treatment of the aluminum alloy material comprises the following steps: dissolving film-forming agent, complexing agent, oxidant and additive in water, stirring, and adjusting pH to 3.6-4.5 with sodium hydroxide and dilute sulfuric acid.
Example 2
The passivator for the surface treatment of the aluminum alloy material is characterized by comprising the following preparation raw materials in parts by weight: 3 parts of film forming agent, 5 parts of complexing agent, 1 part of oxidizing agent, 1 part of additive and 90 parts of water.
The film forming agent is basic chromium sulfate.
The complexing agent is a fluorine compound.
The fluorine compound is a combination of potassium fluozirconate, potassium fluoride and fluozirconic acid, wherein the mass ratio of the potassium fluozirconate to the fluozirconic acid is 5: 1: 1.5.
the oxidant is a combination of cobalt nitrate and cerium nitrate, wherein the mass ratio of the cobalt nitrate to the cerium nitrate is 1: 1.
the additive is nano silica sol.
The nanometer silica sol has a particle size of 15nm, is commercially available, and is manufactured by Kohn silicon products, Inc. of Linyi City, with the model of KHAS-25.
The preparation method of the passivator for the surface treatment of the aluminum alloy material comprises the following steps: dissolving film-forming agent, complexing agent, oxidant and additive in water, stirring, and adjusting pH to 3.6-4.5 with sodium hydroxide and dilute sulfuric acid.
Example 3
The passivator for the surface treatment of the aluminum alloy material is characterized by comprising the following preparation raw materials in parts by weight: 12 parts of film-forming agent, 15 parts of complexing agent, 6 parts of oxidizing agent, 3 parts of additive and 74 parts of water.
The film forming agent is basic chromium sulfate.
The complexing agent is a fluorine compound.
The fluorine compound is a combination of potassium fluozirconate, potassium fluoride and fluozirconic acid, wherein the mass ratio of the potassium fluozirconate to the fluozirconic acid is 5: 1: 1.5.
the oxidant is a combination of cobalt nitrate and cerium nitrate, wherein the mass ratio of the cobalt nitrate to the cerium nitrate is 1: 1.
the additive is nano silica sol.
The nanometer silica sol has a particle size of 15nm, is commercially available, and is manufactured by Kohn silicon products, Inc. of Linyi City, with the model of KHAS-25.
The preparation method of the passivator for the surface treatment of the aluminum alloy material comprises the following steps: dissolving film-forming agent, complexing agent, oxidant and additive in water, stirring, and adjusting pH to 3.6-4.5 with sodium hydroxide and dilute sulfuric acid.
Example 4
Similar to example 1, except that the film former was chromium sulfate.
Example 5
Similar to example 1, except that the complexing agent was free of potassium fluorozirconate.
Example 6
Similar to example 1, except that the complexing agent was free of potassium fluoride.
Example 7
Similar to example 1, except that the complexing agent was free of fluorozirconic acid.
Example 8
Similar to example 1, except that the oxidant was free of cobalt nitrate.
Example 9
Similar to example 1, except that the oxidizing agent was devoid of cerium nitrate.
Example 10
Similar to example 1, except that the nano-silica sol has a particle size of 120nm, and is commercially available from Korea silicon products Co., Ltd., Yiyi, model No. KHAS-12040.
Example 11
Similar to example 1, except that the nano silica sol has a particle size of 5nm, and is commercially available from Korea silicon products Co., Ltd., Korea, Shiyi, in the form of KH-515.
Evaluation of Performance
1. And (3) testing neutral salt spray resistance: the passivators for surface treatment of aluminum alloy materials prepared in examples 1 to 11 are respectively passivated to 11 pieces of completely identical aluminum materials (the aluminum materials adopted in the invention are subjected to oil removal, acid washing, sand blasting, rust removal and other steps), washed with water, treated with sealant (the raw materials for preparing the sealant comprise, by weight, 40 parts of butyl methacrylate, 30 parts of methyl methacrylate, 25 parts of butyl acrylate, 1.5 parts of methacrylic acid and 5 parts of nano silica sol), washed with water, dried to obtain the aluminum materials after surface treatment, subjected to neutral salt spray test and recorded the experimental results.
And (3) testing conditions are as follows: temperature of the test chamber: 35 ℃; the temperature of the saturator: 47 ℃; concentration of the solution: 5% NaCl (mass ratio); the pH value of the solution is as follows: 6.5-7.2(25 ℃); the settling amount of the salt spray: 1-2mL/h 80cm2(ii) a The test time is 720 hours;
the corrosion grade is divided into the following three grades: a stage: no corrosion mark or color change; b, stage: slight traces of corrosion including pitting or staining removable with slight cleaning, and surface discoloration, which have little effect on the reflectivity of the surface; c, stage: obvious discoloration or generation of yellow and black rusts or corrosion pits on the surface;
the surface treatment of the aluminum material was carried out according to the above procedure using a commercially available passivation solution (type: Saideck 650) as a comparative example in place of the passivation solution provided by the present invention, and the experimental results were recorded as shown in Table 1 below.
TABLE 1 neutral salt spray resistance test results
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Degree of corrosion | a | a | a | b | c | b |
| Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | Comparative example | |
| Degree of corrosion | b | b | c | b | b | c |
2. And (3) sulfur dioxide corrosion resistance test: the passivators for surface treatment of aluminum alloy materials prepared in examples 1 to 11 are respectively passivated to 11 pieces of completely identical aluminum materials (the aluminum materials adopted in the invention are subjected to oil removal, acid washing, sand blasting, rust removal and other steps), washed with water, treated with a sealant (the raw materials for preparing the sealant comprise, by weight, 40 parts of butyl methacrylate, 30 parts of methyl methacrylate, 25 parts of butyl acrylate, 1.5 parts of methacrylic acid and 5 parts of nano silica sol), washed with water and dried to obtain the aluminum materials subjected to surface treatment, then the aluminum materials subjected to surface treatment are subjected to sulfur dioxide corrosion resistance test according to IEC60950-22-2016 test standards, and the results are recorded.
Test conditions
(1) And (3) neutral salt spray test:
temperature of the test chamber: 35 ℃; the temperature of the saturator: 47 ℃; concentration of the solution: 5% NaCl (mass ratio); the pH value of the solution is as follows: 6.5-7.2(35 ℃); the settling amount of the salt spray: 1-2mL/h 80cm2(ii) a The test time is 168 hours;
(2) corrosion test (sulfur dioxide):
1) test parameters are as follows: the theoretical concentration of sulfur dioxide at the beginning of each test period is 0.067 volume percent, namely, 0.3L of sulfur dioxide gas is added in each test period in a test box with the volume of 450L;
2) the first stage 8h of the test period comprises a preheating second stage 16h, and comprises opening the test box to cool for 24h in total;
3) first stage of exposure conditions: temperature (40 ± 3) ° c, relative humidity about 100% (condensation water is generated on the sample), second stage: temperature (23 + -5) ° c, relative humidity (50 + -20)%, first stage + second stage is 1 cycle, test 5 cycles in total.
The sulfur dioxide corrosion resistance test comprises a neutral salt spray test and a corrosion test (sulfur dioxide), wherein the neutral salt spray test and the corrosion test (sulfur dioxide) are one cycle, and the two cycles are tested.
The surface treatment of the aluminum material was carried out according to the above procedure by using a commercially available passivation solution (type: Saideck 650) as a comparative example in place of the passivation solution provided by the present invention, and the results of the sulfur dioxide corrosion resistance test were recorded as shown in Table 2 below.
TABLE 2 Sulfur dioxide Corrosion resistance test results
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Time of etching | No corrosion | 561h | 570h | 554h | 515h | 543h |
| Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | Comparative example | |
| Time of etching | 565h | 532h | 509h | 535h | 546h | 216h |
After the surface treatment is carried out on the aluminum material by using the passivating agent and the sealing agent provided in the embodiment 1, a sulfur dioxide corrosion resistance test is carried out according to the IEC60950-22-2016 test method, and after two periods of tests, the surface of the aluminum material has no corrosion situation, which shows that the aluminum alloy material treated by the passivating solution provided by the invention has excellent neutral salt spray resistance stability and sulfur dioxide corrosion resistance.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The passivator for surface treatment of the aluminum alloy material is characterized by comprising the following raw materials in parts by weight: 3-12 parts of film-forming agent, 5-15 parts of complexing agent, 1-6 parts of oxidant, 1-3 parts of additive and 60-90 parts of water.
2. The passivator for aluminum alloy material surface treatment according to claim 1, wherein the film forming agent is selected from one or more of chromium nitrate, basic chromium sulfate and chromium chloride.
3. The passivator for aluminum alloy material surface treatment according to claim 2, wherein the film forming agent is basic chromium sulfate.
4. The passivator for aluminum alloy material surface treatment according to claim 1, wherein the complexing agent is fluorine compound.
5. The passivator for aluminum alloy material surface treatment according to claim 4, wherein the fluorine compound is selected from one or more of sodium fluoride, ammonium bifluoride, potassium fluorozirconate, potassium fluoride and fluorozirconic acid.
6. The passivator for aluminum alloy material surface treatment according to claim 1, wherein the oxidant is selected from one or more of sodium nitrate, potassium nitrate, cobalt nitrate, lanthanum nitrate, and cerium nitrate.
7. The passivator for aluminum alloy material surface treatment according to claim 6, wherein the oxidant is a combination of cobalt nitrate and cerium nitrate, wherein the mass ratio of cobalt nitrate to cerium nitrate is 1: (1-3).
8. The passivator for aluminum alloy material surface treatment according to claim 1, wherein the additive is nano silica sol.
9. The passivator for surface treatment of aluminum alloy material according to claim 8, wherein the particle size of the nano silica sol is 10-50 nm.
10. The preparation method of the passivator for aluminum alloy material surface treatment according to any one of claims 1-9, characterized in that the preparation method comprises: dissolving film-forming agent, complexing agent, oxidant and additive in water, stirring, and adjusting pH to 3.6-4.5 with sodium hydroxide and dilute sulfuric acid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112064000A (en) * | 2020-08-17 | 2020-12-11 | 尹波 | Passivation process for surface of aluminum alloy material |
| CN112080737A (en) * | 2020-08-17 | 2020-12-15 | 尹波 | Surface treatment method for communication radiator and product thereof |
| CN115074715A (en) * | 2022-06-30 | 2022-09-20 | 东风商用车有限公司 | Pretreatment zirconium agent for high-temperature-resistant coating and pretreatment method |
| CN115558914A (en) * | 2022-02-16 | 2023-01-03 | 深圳市尚笠实业有限公司 | Aluminum-based metal material surface protective agent and preparation method thereof |
-
2020
- 2020-03-26 CN CN202010224085.7A patent/CN111304643A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112064000A (en) * | 2020-08-17 | 2020-12-11 | 尹波 | Passivation process for surface of aluminum alloy material |
| CN112080737A (en) * | 2020-08-17 | 2020-12-15 | 尹波 | Surface treatment method for communication radiator and product thereof |
| CN115558914A (en) * | 2022-02-16 | 2023-01-03 | 深圳市尚笠实业有限公司 | Aluminum-based metal material surface protective agent and preparation method thereof |
| CN115074715A (en) * | 2022-06-30 | 2022-09-20 | 东风商用车有限公司 | Pretreatment zirconium agent for high-temperature-resistant coating and pretreatment method |
| CN115074715B (en) * | 2022-06-30 | 2024-01-30 | 东风商用车有限公司 | Pretreatment zirconation agent for high-temperature-resistant coating and pretreatment method |
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