CN112267107A - Corrosion-resistant chromium-free surface treatment process - Google Patents
Corrosion-resistant chromium-free surface treatment process Download PDFInfo
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- CN112267107A CN112267107A CN202011154960.5A CN202011154960A CN112267107A CN 112267107 A CN112267107 A CN 112267107A CN 202011154960 A CN202011154960 A CN 202011154960A CN 112267107 A CN112267107 A CN 112267107A
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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
- C23C22/36—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 containing also phosphates
- C23C22/367—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 containing also phosphates containing alkaline earth metal cations
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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
- C23C22/78—Pretreatment of the material to be coated
-
- 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
- C23C22/82—After-treatment
Abstract
The invention provides a novel corrosion-resistant chromium-free surface treatment process, which solves the problems that the aluminum alloy passivation solution in the prior art contains chromium, and when the content of the chromium reaches a certain amount, the environment is polluted and the human body is damaged, and can obtain a surface treatment process which has a good passivation effect and a good corrosion-resistant effect and can bear a long-time smoke experiment by reconfiguring the passivation solution and optimizing the treatment process, wherein the surface treatment process comprises a cleaning step and a rinsing step: an activation step: passivating: and (5) drying.
Description
Technical Field
The invention relates to the technical field of aluminum alloy surface treatment, in particular to a corrosion-resistant chromium-free surface treatment process.
Background
The weight reduction of the automobile: the method has become the trend of automobile development in the world, and the overall quality of the automobile is reduced as much as possible on the premise of ensuring the strength and the safety performance of the automobile, so that the power of the automobile is improved, the fuel consumption is reduced, and the exhaust pollution is reduced. One of the most important measures is the use of lightweight materials. The density of the aluminum and the aluminum alloy is about 1/3 of steel, and the aluminum alloy are light materials which are most widely applied and are mainly used for devices such as engine brackets, cylinder bodies, steering gears, air-conditioning pumps and the like.
But because of the strong activity of aluminum, the aluminum corrodes seriously in air and other media, and has poor wear resistance. In order to overcome the defects, expand the application range and prolong the service life, the surface treatment technology of the aluminum alloy is an indispensable important link in the use of the aluminum alloy. The simplest and most effective treatment currently used is passivation.
The method is a process of placing aluminum and aluminum alloy products in a passivation solution to carry out chemical reaction under the condition of no power supply, and forming a protective film on the surface of the products. The corrosion resistance and the wear resistance of aluminum and aluminum alloy products are improved, and after passivation treatment, the thickness of a workpiece is not increased, the color is not changed, and the like, so that the product precision is ensured, and the operation is convenient. However, the passivation solutions used herein are those containing hexavalent or trivalent metals. Because hexavalent chromium is easily dissolved in water and absorbed by the land, the hexavalent chromium has obvious adverse effects on the physical and chemical properties of soil, the biological characteristics of soil (particularly soil microorganisms) and the microbial community structure, thereby affecting the ecological structure and the functional stability of the soil. Will cause harm to plants and other organisms, lead to plant decay and fall off, and finally plant wilting and withering, and simultaneously, when the concentration of hexavalent chromium in the atmosphere is more than 0.033mg/m3Respiratory inflammation can occur, leading to emphysema, bronchiectasis, and even cancer. Therefore, hexavalent chromium pollution is harmful, has wide influence range and is difficult to treat. On the basis of the existing environmental management technology level at home and abroad, even if huge manpower and financial resources are invested, the influence of the environmental management technology level on the society and the ecological environment cannot be completely eliminated. The rationale for pollution first and then treatment is not feasible. Only from the source, strict control is carried out, hexavalent chromium is replaced by chromium-free chromium, and all possibilities of pollution of hexavalent chromium are blocked, so that the fundamental way of eliminating the pollution of hexavalent chromium is to take the research and development of chromium-free passivators as a major subject.
Therefore, a novel chromium-free passivation process needs to be developed, so that the passivated aluminum alloy can bear salt spray experiments for tens to hundreds of hours.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a novel corrosion-resistant chromium-free surface treatment process which can solve the technical problems in the background art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a corrosion-resistant chromium-free surface treatment process comprises the following steps:
a cleaning step: preparing a cleaning solution, wherein the cleaning solution comprises 60% sulfuric acid, 2% ammonium bisulfate solution, 1% sodium nitrate solution, 10% hydrogen fluoride solution and an aqueous solution, and the volume ratio of the sulfuric acid to the ammonium bisulfate solution to the sodium nitrate solution to the hydrogen fluoride solution to the aqueous solution is 10-25: 1-3: 1-3: 0-1: 68-87;
putting the cleaning solution into an ultrasonic degreasing tank, heating to 30-50 ℃, putting the aluminum alloy die casting into the ultrasonic degreasing tank by adopting a slow heating mode, and carrying out ultrasonic cleaning for no more than 30 min;
rinsing:
taking out the aluminum alloy die casting subjected to ultrasonic cleaning, putting the aluminum alloy die casting into a rinsing tank for rinsing at least once, and cleaning in a turnover mode during cleaning;
an activation step:
the aluminum alloy casting is placed into the surface adjusting tank, the surface adjusting tank is internally provided with a turnover device, the aluminum alloy casting is placed into the workpiece hanging frame basket, the workpiece hanging frame basket is placed on the turnover device, the surface adjusting tank is internally provided with activating liquid, and the activating liquid comprises the following raw materials: 20g of nickel sulfate, 180g of sodium citrate, 170g of potassium sodium tartrate and 580g of aqueous solution, pouring the prepared aluminum alloy activation solution into a surface conditioning tank for heating, heating to 40-50 ℃, and performing a timed activation step, wherein in the activation, the turnover device is turned over continuously, and the turning speed is 3-7 r/min;
passivating:
preparing a passivation solution, wherein the passivation solution comprises the following raw materials: 98-100g/L of magnesium fluoride, 10-30g/L of sodium tripolyphosphate, 10-30g/L of fluozirconic acid, 23-25g/L of sodium fluosilicate, 45-65g/L of hydrochloric acid, 10-30g/L of nitric acid, 100g/L of phosphoric acid, 10-30g/L of vinyl triacetoxysilane, 30-40g/L of sulfuric acid, 30-50g/L of calcium nitrate and the balance of solvent, wherein the solvent is water, and the concentration of the passivation solution is controlled to be 2-25% according to the content of the proportion-adjusting water;
putting the prepared passivation solution into a passivation tank, heating the passivation solution from room temperature to 40 ℃, heating the passivation solution to 40 ℃ at a constant speed within 1 hour, and rotating a turnover device in the passivation tank at a rotating speed of 3-7 r/min;
rinsing after passivation is finished, wherein hot water is used for rinsing, the temperature of the hot water is 88-92 ℃, the aluminum alloy die casting is rinsed in a turnover mode, and the turnover speed is 3-7 r/min;
and (3) drying:
and (3) carrying out vacuum drying on the passivated aluminum alloy casting, heating the vacuum drying tank to above 60 ℃, vacuumizing to-0.098 MPa, and keeping the vacuum drying time for no more than 10 min.
Preferably, the temperature of the cleaning liquid in the cleaning step is raised to 30-50 ℃, the temperature is raised slowly, and the temperature is raised to the set temperature within 2 hours.
Preferably, the ultrasonic cleaning is performed at intervals, and the cleaning is continued at intervals of 5min after every 10min of ultrasonic cleaning.
Preferably, the temperature of the activating solution in the surface adjusting tank is raised to 40-50 ℃ within 1 hour, and the temperature is raised at a constant speed.
Compared with the prior art, the passivation solution prepared by the method has a good passivation effect, can ensure a long-time salt spray resistance experiment without chromium addition, and has strong corrosion resistance.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
The invention solves the problems of environmental pollution and harm to human health caused by chromium addition in the aluminum alloy passivation step in the prior art, and simultaneously, the passivation process can enable an aluminum alloy casting to bear a smoke experiment for more than dozens of hours, thereby having stronger corrosion resistance.
The invention is further described below by combining three examples, and the following three groups of experiments mainly explore the corrosion resistance of the passivation solution by preparing passivation solutions with different concentrations, and sequentially selecting the concentrations of the passivation solutions of the three groups to be 2%, 5% and 10%.
Example 1
The non-chromating surface treatment process comprises the following steps:
cleaning: the cleaning solution comprises 60% sulfuric acid, 2% ammonium bisulfate solution, 1% sodium nitrate solution, 10% hydrogen fluoride solution and water solution, wherein the volume ratio of the sulfuric acid to the ammonium bisulfate solution to the sodium nitrate solution to the hydrogen fluoride solution to the water solution is 25: 3: 3: 1: 68; putting the cleaning solution into an ultrasonic degreasing tank, heating to 50 ℃, and performing ultrasonic cleaning for no more than 30 min;
rinsing: taking out the aluminum alloy die casting, putting the aluminum alloy die casting into a rinsing tank for rinsing at least once, and cleaning in a turnover mode during cleaning;
and (3) activation: the aluminum alloy casting is placed into a surface adjusting tank, and an activating liquid is arranged in the surface adjusting tank and comprises the following raw materials: 20g of nickel sulfate, 180g of sodium citrate, 170g of potassium sodium tartrate and 580g of aqueous solution, heating to 40-50 ℃, and continuously overturning by an overturning device at the rotating speed of 3-7r/min during activation;
passivation: preparing a passivation solution, wherein the passivation solution comprises the following raw materials: 100g/L of magnesium fluoride, 30g/L of sodium tripolyphosphate, 30g/L of fluozirconic acid, 25g/L of sodium fluosilicate, 65g/L of hydrochloric acid, 30g/L of nitric acid, 120g/L of phosphoric acid, 30g/L of vinyl triacetoxysilane, 40g/L of sulfuric acid, 50g/L of calcium nitrate and 25.48Kg of water,
putting the prepared passivation solution into a passivation tank, heating the passivation solution from room temperature to 40 ℃, and rotating a turnover device in the passivation tank at a rotating speed of 3-7 r/min; after passivation is finished, rinsing and rinsing with hot water, wherein the temperature of the hot water is 88-92 ℃;
and (3) drying: and (3) carrying out vacuum drying on the passivated aluminum alloy casting, heating the vacuum drying tank to above 60 ℃, vacuumizing to-0.098 MPa, and keeping the vacuum drying time for no more than 10 min.
Example 2
The difference between the embodiment 2 and the embodiment 1 is only that the proportion of the passivating solution in the passivating step is different, and the proportion of the passivating solution is 100g/L of magnesium fluoride, 30g/L of sodium tripolyphosphate, 30g/L of fluozirconate, 25g/L of sodium fluosilicate, 65g/L of hydrochloric acid, 30g/L of nitric acid, 120g/L of phosphoric acid, 30g/L of vinyl triacetoxysilane, 40g/L of sulfuric acid, 50g/L of calcium nitrate and 9.88Kg of water.
The steps are the same as those in the embodiments, and thus are not described in detail.
Example 3
The difference between the embodiment 3 and the embodiment 1 is only that the proportion of the passivating solution in the passivating step is different, and the proportion of the passivating solution is 100g/L of magnesium fluoride, 30g/L of sodium tripolyphosphate, 30g/L of fluozirconate, 25g/L of sodium fluosilicate, 65g/L of hydrochloric acid, 30g/L of nitric acid, 120g/L of phosphoric acid, 30g/L of vinyl triacetoxysilane, 40g/L of sulfuric acid, 50g/L of calcium nitrate and 4.68Kg of water.
The steps are the same as those in the embodiments, and thus are not described in detail.
The aluminum alloys completed in the above three groups of examples were subjected to salt spray tests, wherein the concentration of sodium chloride in the salt spray test was 5% omega/v and the amount of sedimentation was 1-2mL/(80 cm)2H) air pressure of 1kg/cm3The temperature of saturated water is 47 +/-1.0 ℃, the experimental temperature is 35 +/-1.0, the pH value of the solution is 6.5-7.2, continuous spraying is adopted, the experimental time is 72 hours, and the rusty area of the surface of the aluminum alloy is observed after the experiment is finished.
The experimental results of the last three groups of examples of this experiment are: rusty area for example 1 < rusty area for example 2 < rusty area for example 3.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (4)
1. A corrosion-resistant chromium-free surface treatment process is characterized in that: the method comprises the following steps:
a cleaning step: preparing a cleaning solution, wherein the cleaning solution comprises 60% sulfuric acid, 2% ammonium bisulfate solution, 1% sodium nitrate solution, 10% hydrogen fluoride solution and an aqueous solution, and the volume ratio of the sulfuric acid to the ammonium bisulfate solution to the sodium nitrate solution to the hydrogen fluoride solution to the aqueous solution is 10-25: 1-3: 1-3: 0-1: 68-87;
putting the cleaning solution into an ultrasonic degreasing tank, heating to 30-50 ℃, putting the aluminum alloy die casting into the ultrasonic degreasing tank by adopting a slow heating mode, and carrying out ultrasonic cleaning for no more than 30 min;
rinsing:
taking out the aluminum alloy die casting subjected to ultrasonic cleaning, putting the aluminum alloy die casting into a rinsing tank for rinsing at least once, and cleaning in a turnover mode during cleaning;
an activation step:
the aluminum alloy casting is placed into the surface adjusting tank, the surface adjusting tank is internally provided with a turnover device, the aluminum alloy casting is placed into the workpiece hanging frame basket, the workpiece hanging frame basket is placed on the turnover device, the surface adjusting tank is internally provided with activating liquid, and the activating liquid comprises the following raw materials: 20g of nickel sulfate, 180g of sodium citrate, 170g of potassium sodium tartrate and 580g of aqueous solution, pouring the prepared aluminum alloy activation solution into a surface conditioning tank for heating, heating to 40-50 ℃, and performing a timed activation step, wherein in the activation, the turnover device is turned over continuously, and the turning speed is 3-7 r/min;
passivating:
preparing a passivation solution, wherein the passivation solution comprises the following raw materials: 98-100g/L of magnesium fluoride, 10-30g/L of sodium tripolyphosphate, 10-30g/L of fluozirconic acid, 23-25g/L of sodium fluosilicate, 45-65g/L of hydrochloric acid, 10-30g/L of nitric acid, 100g/L of phosphoric acid, 10-30g/L of vinyl triacetoxysilane, 30-40g/L of sulfuric acid, 30-50g/L of calcium nitrate and the balance of solvent, wherein the solvent is water, and the concentration of the passivation solution is controlled to be 2-25% according to the content of the proportion-adjusting water;
putting the prepared passivation solution into a passivation tank, heating the passivation solution from room temperature to 40 ℃, heating the passivation solution to 40 ℃ at a constant speed within 1 hour, and rotating a turnover device in the passivation tank at a rotating speed of 3-7 r/min;
rinsing after passivation is finished, wherein hot water is used for rinsing, the temperature of the hot water is 88-92 ℃, the aluminum alloy die casting is rinsed in a turnover mode, and the turnover speed is 3-7 r/min;
and (3) drying:
and (3) carrying out vacuum drying on the passivated aluminum alloy casting, heating the vacuum drying tank to above 60 ℃, vacuumizing to-0.098 MPa, and keeping the vacuum drying time for no more than 10 min.
2. The corrosion-resistant chromium-free surface treatment process according to claim 1, wherein: and heating the cleaning liquid in the cleaning step to 30-50 ℃, slowly heating, and heating to the set temperature within 2 hours.
3. The corrosion-resistant chromium-free surface treatment process according to claim 1, wherein: the ultrasonic cleaning adopts interval ultrasonic cleaning, and cleaning is continued at an interval of 5min after every 10min of ultrasonic cleaning.
4. The corrosion-resistant chromium-free surface treatment process according to claim 1, wherein: the temperature of the activating liquid in the surface adjusting tank is raised to 40-50 ℃ within 1 hour, and the temperature is raised at a constant speed.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1368563A (en) * | 2000-02-16 | 2002-09-11 | 阿托泰克德国有限公司 | Composition for removing aluminium surface stain |
| CN101275220A (en) * | 2007-03-27 | 2008-10-01 | 汉达精密电子(昆山)有限公司 | Aluminum alloy activation solution |
| CN104087924A (en) * | 2014-07-10 | 2014-10-08 | 安徽通润汽车零部件有限公司 | Metal surface passivating treatment fluid |
| CN104328409A (en) * | 2013-07-22 | 2015-02-04 | 无锡永发电镀有限公司 | Architectural aluminum profile surface environmentally-friendly passivation technology |
| CN104911577A (en) * | 2015-06-18 | 2015-09-16 | 华南理工大学 | Chromium-free alkaline passivation solution and passivation method for aluminum alloy |
| CN105154861A (en) * | 2015-07-06 | 2015-12-16 | 安徽景昌铝业有限公司 | Chromate-free passivation treatment process for aluminum profile material |
| CN110257810A (en) * | 2019-07-15 | 2019-09-20 | 江苏方成生物科技有限公司 | A kind of novel antirust agent |
-
2020
- 2020-10-26 CN CN202011154960.5A patent/CN112267107A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1368563A (en) * | 2000-02-16 | 2002-09-11 | 阿托泰克德国有限公司 | Composition for removing aluminium surface stain |
| CN101275220A (en) * | 2007-03-27 | 2008-10-01 | 汉达精密电子(昆山)有限公司 | Aluminum alloy activation solution |
| CN104328409A (en) * | 2013-07-22 | 2015-02-04 | 无锡永发电镀有限公司 | Architectural aluminum profile surface environmentally-friendly passivation technology |
| CN104087924A (en) * | 2014-07-10 | 2014-10-08 | 安徽通润汽车零部件有限公司 | Metal surface passivating treatment fluid |
| CN104911577A (en) * | 2015-06-18 | 2015-09-16 | 华南理工大学 | Chromium-free alkaline passivation solution and passivation method for aluminum alloy |
| CN105154861A (en) * | 2015-07-06 | 2015-12-16 | 安徽景昌铝业有限公司 | Chromate-free passivation treatment process for aluminum profile material |
| CN110257810A (en) * | 2019-07-15 | 2019-09-20 | 江苏方成生物科技有限公司 | A kind of novel antirust agent |
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Application publication date: 20210126 |