阅读说明：本技术 一种铝合金阳极氧化膜封孔质量的优化方法 (Method for optimizing hole sealing quality of aluminum alloy anodic oxide film ) 是由 廖健 于 2019-09-26 设计创作，主要内容包括：本发明公开了一种铝合金阳极氧化膜封孔质量的优化方法,它包括以下步骤：S1、通过直读光谱仪定量分析其化学成分,其中面积比为铝合金型材的裸露基体面积与阳极氧化膜面积之比；S2、制定新的封孔工艺对阳极氧化膜封孔；S3、绘制不同封孔工艺对阳极氧化膜封孔质量的结果图；S4、绘制常温条件下对不同面积比的铝合金阳极氧化膜使用不同酸浸蚀失重法的失重差关系曲线图；绘制中温条件下对不同面积比的铝合金阳极氧化膜使用不同酸浸蚀失重法的失重差关系曲线图；S5、分析铝合金阳极氧化膜经过常温封孔和中温封孔后的表面宏观形貌。本发明的有益效果是：开发出能够替代磷铬酸法对阳极氧化膜封孔的酸浸失重法、不污染环境、不造成人体危害。(The invention discloses a method for optimizing hole sealing quality of an aluminum alloy anodic oxide film, which comprises the following steps: s1, quantitatively analyzing chemical components of the aluminum alloy section by a direct-reading spectrometer, wherein the area ratio is the ratio of the area of the exposed substrate of the aluminum alloy section to the area of the anodic oxide film; s2, setting a new hole sealing process to seal the hole of the anodic oxide film; s3, drawing a result graph of hole sealing quality of the anodic oxide film by different hole sealing processes; s4, drawing a weight-loss relationship curve chart of aluminum alloy anodic oxide films with different area ratios by using different acid etching weight-loss methods under normal temperature conditions; drawing a weight loss difference relation curve chart of the aluminum alloy anodic oxide films with different area ratios by using different acid etching weight loss methods under the condition of medium temperature; and S5, analyzing the surface macro morphology of the aluminum alloy anode oxide film after normal-temperature hole sealing and medium-temperature hole sealing. The invention has the beneficial effects that: the acid leaching weight loss method which can replace a phosphorus-chromic acid method to seal the hole of the anodic oxide film is developed, and the method does not pollute the environment and does not cause harm to human bodies.)

1. An optimization method for hole sealing quality of an aluminum alloy anodic oxide film is characterized by comprising the following steps: it comprises the following steps:

s1, selecting at least 8 groups of aluminum alloy sections with different surface ratios, and quantitatively analyzing chemical components of the aluminum alloy sections through an ARL-MA-283 direct reading spectrometer, wherein the area ratio is the ratio of the area of a bare substrate of the aluminum alloy section to the area of an anodic oxidation film;

s2, setting a new hole sealing process to seal the hole of the anodic oxide film, wherein the new hole sealing process comprises a phosphoric acid method and a sodium phosphomolybdate method, and the step of sealing the hole of the anodic oxide film by the phosphoric acid method comprises the step of putting the aluminum alloy section to be sealed into HNO at the temperature of 18 ~ 19 DEG C₃Soaking in solution for 9 ~ 10min, washing the aluminum alloy section by using deionized water after soaking, finally putting the aluminum alloy section into phosphoric acid solution with the temperature of 37 ~ 38 ℃, soaking for 12 ~ 13min, and washing the aluminum alloy section by using deionized water, wherein the step of sealing the anodic oxide film by using the sodium molybdate phosphate method is to put the aluminum alloy section to be sealed into HNO with the temperature of 18 ~ 19 ℃ firstly₃Soaking in solution for 9 ~ 10min, washing the aluminum alloy section with deionized water, soaking in sodium molybdate solution at 37 ~ 38 deg.C for 14 ~ 15min, and soakingWashing the aluminum alloy section with deionized water;

s3, taking three aluminum alloy section samples with the same area ratio, sealing the three samples by a phosphochromic acid method, a phosphoric acid method and a sodium phosphomolybdate method at room temperature, drying the samples after sealing the holes and measuring the weight loss mass of the samples, taking the other three aluminum alloy section samples with the same area ratio, sealing the three samples by the phosphochromic acid method, the phosphoric acid method and the sodium phosphomolybdate method at medium temperature of 58 ~ 62 ℃, drying the samples after sealing the holes and measuring the weight loss mass of the samples, and drawing a result graph of sealing the hole mass of the anodic oxide film by different sealing processes;

s4, taking three aluminum alloy sections with the same area ratio, ensuring that three aluminum alloy section samples with different area ratios are available, sealing the three samples by adopting a phosphochromic acid method, a phosphoric acid method and a sodium phosphomolybdate method respectively at normal temperature, drying and measuring the weight loss quality of the samples after sealing the holes, and drawing a weight loss difference relation curve chart of different acid etching weight loss methods for aluminum alloy anodic oxide films with different area ratios under normal temperature; taking three aluminum alloy sections with the same area ratio, ensuring that three aluminum alloy section samples with different area ratios are available, sealing the three samples by adopting a phosphochromic acid method, a phosphoric acid method and a sodium phosphomolybdate method respectively at the medium temperature, drying the three samples after sealing the holes, measuring the weight loss quality of the samples, and drawing a weight loss difference relation curve chart of the aluminum alloy anodic oxide films with different area ratios by using different acid etching weight loss methods at the medium temperature;

and S5, analyzing the surface macro morphology of the aluminum alloy anode oxide film after normal-temperature hole sealing and medium-temperature hole sealing.

Technical Field

The invention relates to an optimization method for hole sealing quality of an aluminum alloy anodic oxide film.

Background

Anodic oxidation is one of the most commonly used surface treatment methods for aluminum alloys, however, the anodic oxide film structure of aluminum alloys belongs to a honeycomb type porous structure, has high porosity and strong adsorbability, and is easily corroded by external pollution and corrosive media, so that the anodic oxide film needs to be properly sealed before being put into use. The hole sealing quality is an important index for reflecting the corrosion resistance of the anodic oxide film, and the quality of the hole sealing quality directly influences the service life of the product, so the hole sealing quality is a key detection project of the aluminum alloy anodic oxide product.

The method for detecting the hole sealing quality mainly comprises an acid etching weightlessness method, a admittance method and a dyeing spot method after acid treatment, wherein the admittance method is a quick nondestructive detection method, but the result of the method is influenced by various aspects such as an aluminum alloy material, a hole sealing process, aging time, storage conditions and the like, and the limitation is large, so the method is rarely used in China₃Soaking the aluminum alloy section bar in the solution for 9 ~ 10min, washing the aluminum alloy section bar by using deionized water after soaking, finally placing the aluminum alloy section bar in chromic acid solution at the temperature of 37 ~ 38 ℃, soaking for 14 ~ 15min, and washing the aluminum alloy section bar by using deionized water.

Into which HNO is introduced₃The pre-soaking not only strictly meets the requirements on the hole sealing quality, but also ensures that the judgment of the hole sealing quality is more sensitive, the method which is currently recognized internationally as the best method for evaluating the hole sealing quality of the aluminum alloy anode oxide film is a phosphorus chromic acid method, but hexavalent chromium belongs to a highly toxic substance, has lasting harmfulness to the environment and human bodies, has the functions of carcinogenesis and induction of gene mutation, has great influence on the environment and has lasting harmfulness.

Disclosure of Invention

The invention aims to overcome the defects of the prior art and provide the method for optimizing the hole sealing quality of the aluminum alloy anodic oxide film by using the acid leaching weight loss method, which has simple process, can replace the phosphorus chromic acid method to seal the hole of the anodic oxide film and does not pollute the environment and cause human harm.

The purpose of the invention is realized by the following technical scheme: an optimization method for hole sealing quality of an aluminum alloy anodic oxide film comprises the following steps:

s1, selecting at least 8 groups of aluminum alloy sections with different surface ratios, and quantitatively analyzing chemical components of the aluminum alloy sections through an ARL-MA-283 direct reading spectrometer, wherein the area ratio is the ratio of the area of a bare substrate of the aluminum alloy section to the area of an anodic oxidation film;

s2, setting a new hole sealing process to seal the hole of the anodic oxide film, wherein the new hole sealing process comprises a phosphoric acid method and a sodium phosphomolybdate method, and the step of sealing the hole of the anodic oxide film by the phosphoric acid method comprises the step of putting the aluminum alloy section to be sealed into HNO at the temperature of 18 ~ 19 DEG C₃Soaking in solution for 9 ~ 10min, washing the aluminum alloy section by using deionized water after soaking, finally putting the aluminum alloy section into phosphoric acid solution with the temperature of 37 ~ 38 ℃, soaking for 12 ~ 13min, and washing the aluminum alloy section by using deionized water, wherein the step of sealing the anodic oxide film by using the sodium molybdate phosphate method is to put the aluminum alloy section to be sealed into HNO with the temperature of 18 ~ 19 ℃ firstly₃Soaking the aluminum alloy section in the solution for 9 ~ 10min, cleaning the aluminum alloy section by using deionized water after soaking, finally placing the aluminum alloy section in a sodium molybdate solution at the temperature of 37 ~ 38 ℃, soaking for 14 ~ 15min, and cleaning the aluminum alloy section by using deionized water;

s3, taking three aluminum alloy section samples with the same area ratio, sealing the three samples by a phosphochromic acid method, a phosphoric acid method and a sodium phosphomolybdate method at room temperature, drying the samples after sealing the holes and measuring the weight loss mass of the samples, taking the other three aluminum alloy section samples with the same area ratio, sealing the three samples by the phosphochromic acid method, the phosphoric acid method and the sodium phosphomolybdate method at medium temperature of 58 ~ 62 ℃, drying the samples after sealing the holes and measuring the weight loss mass of the samples, and drawing a result graph of sealing the hole mass of the anodic oxide film by different sealing processes;

s4, taking three aluminum alloy sections with the same area ratio, ensuring that three aluminum alloy section samples with different area ratios are available, sealing the three samples by adopting a phosphochromic acid method, a phosphoric acid method and a sodium phosphomolybdate method respectively at normal temperature, drying and measuring the weight loss quality of the samples after sealing the holes, and drawing a weight loss difference relation curve chart of different acid etching weight loss methods for aluminum alloy anodic oxide films with different area ratios under normal temperature; taking three aluminum alloy sections with the same area ratio, ensuring that three aluminum alloy section samples with different area ratios are available, sealing the three samples by adopting a phosphochromic acid method, a phosphoric acid method and a sodium phosphomolybdate method respectively at the medium temperature, drying the three samples after sealing the holes, measuring the weight loss quality of the samples, and drawing a weight loss difference relation curve chart of the aluminum alloy anodic oxide films with different area ratios by using different acid etching weight loss methods at the medium temperature;

and S5, analyzing the surface macro morphology of the aluminum alloy anode oxide film after normal-temperature hole sealing and medium-temperature hole sealing.

The invention has the following advantages:

1. the mass loss data of the sealing quality is contrastively analyzed by a sodium phosphomolybdate method and a phosphochromic acid method, the mass loss errors of the two methods are small and are only +/-1 mg/dm²In the range and has no relation with the area of the exposed aluminum matrix, so that the sodium phosphomolybdate method can be used for replacing the hole sealing of the aluminum alloy anodic oxide film by the phosphochromic acid, thereby not polluting the environment and causing the harm to human bodies.

2. After the hole sealing is carried out on the aluminum alloy anodic oxide film by three hole sealing technologies of a phosphochromic acid method, a phosphoric acid method and sodium phosphomolybdate at normal temperature and medium temperature, the surface of the aluminum alloy anodic oxide film is detected to have no dissolution phenomenon, and the hole sealing of the aluminum alloy anodic oxide film by the sodium phosphomolybdate method can be replaced by the phosphochromic acid method under the same effect.

Drawings

FIG. 1 is a result chart of sealing quality of anodic oxide films by different sealing processes.

FIG. 2 is a graph showing the relationship between weight loss and difference of aluminum alloy anodic oxide films with different area ratios by different acid etching weight loss methods at room temperature;

FIG. 3 is a graph showing the relationship between weight loss and difference of aluminum alloy anodic oxide films with different area ratios by different acid etching weight loss methods under a medium temperature condition;

FIG. 4 is a surface macro topography diagram of an aluminum alloy anodic oxide film before normal temperature hole sealing;

FIG. 5 is a surface macro-topography diagram of an aluminum alloy anodic oxide film after hole sealing by a phosphochromic acid method under normal temperature conditions;

FIG. 6 is a surface macro topography diagram of an aluminum alloy anodic oxide film after hole sealing by a phosphoric acid method under normal temperature conditions;

FIG. 7 is a surface macro topography diagram of an aluminum alloy anodic oxide film after hole sealing by a sodium phosphomolybdate method at normal temperature;

FIG. 8 is a surface macro topography diagram of an aluminum alloy anodic oxide film before medium-temperature hole sealing;

FIG. 9 is a surface macro-topography diagram of an aluminum alloy anodic oxide film after hole sealing by a phosphochromic acid method under moderate temperature conditions;

FIG. 10 is a surface macro-topography diagram of an aluminum alloy anodic oxide film after hole sealing by a phosphochromic acid method under moderate temperature conditions;

FIG. 11 is a surface macro-topography diagram of an aluminum alloy anodic oxide film after hole sealing by a phosphochromic acid method under moderate temperature conditions;

FIG. 12 is a graph of aluminum alloy sections having different surface ratios.

Detailed Description

The invention will be further described with reference to the accompanying drawings, without limiting the scope of the invention to the following:

an optimization method for hole sealing quality of an aluminum alloy anodic oxide film comprises the following steps:

s1, selecting at least 8 groups of aluminum alloy sections with different surface ratios, and quantitatively analyzing chemical components of the aluminum alloy sections through an ARL-MA-283 direct reading spectrometer, wherein the area ratio is the ratio of the area of the bare substrate of the aluminum alloy section to the area of the anodic oxidation film, and the grouping conditions are shown in figure 12;

s2, setting a new hole sealing process to seal the hole of the anodic oxide film, wherein the new hole sealing process comprises a phosphoric acid method and a sodium phosphomolybdate method, and the step of sealing the hole of the anodic oxide film by the phosphoric acid method comprises the step of putting the aluminum alloy section to be sealed into HNO at the temperature of 18 ~ 19 DEG C₃Soaking in solution for 9 ~ 10min, washing the aluminum alloy section with deionized water, finally placing the aluminum alloy section into phosphoric acid solution with the temperature of 37 ~ 38 ℃, soaking for 12 ~ 13min, and washing the aluminum alloy section with deionized water, wherein the step of sealing the anodic oxide film by the sodium phosphomolybdate method comprises the steps of firstly sealing the hole to be sealedThe aluminum alloy section is put into HNO with the temperature of 18 ~ 19 DEG C₃Soaking the aluminum alloy section in the solution for 9 ~ 10min, cleaning the aluminum alloy section by using deionized water after soaking, finally placing the aluminum alloy section in a sodium molybdate solution at the temperature of 37 ~ 38 ℃, soaking for 14 ~ 15min, and cleaning the aluminum alloy section by using deionized water;

s3, taking three aluminum alloy section bar samples with the same area ratio, sealing the three samples by a chromic phosphate method, a phosphoric acid method and a sodium phosphomolybdate method at room temperature, drying after sealing the holes and measuring the weight loss mass of the samples, taking the other three aluminum alloy section bar samples with the same area ratio, sealing the three samples by the chromic phosphate method, the phosphoric acid method and the sodium phosphomolybdate method at medium temperature of 58 ~ 62 ℃, drying after sealing the holes and measuring the weight loss mass of the samples, drawing a result graph of the sealing mass of the anodic oxide film by different sealing processes as shown in figure 1, wherein the ordinate is the mass loss size, and it can be seen from the graph that the error of the results of the chromic phosphate method and the sodium phosphomolybdate method is relatively small, and the test result of the phosphoric acid method is slightly larger than the chromic phosphate method by 2mg/dm²The chromium trioxide and the sodium molybdate can greatly inhibit the dissolution of phosphoric acid on an aluminum matrix and play a role of a corrosion inhibitor, so that a sodium phosphomolybdate method can be used for replacing the hole sealing of a chromic acid phosphate on an aluminum alloy anode oxide film, so that the environment is not polluted and the harm to human bodies is not caused;

s4, taking three aluminum alloy sections with the same area ratio, ensuring that three aluminum alloy section samples with different area ratios are available, sealing the three samples by a phosphochromic acid method, a phosphoric acid method and a sodium phosphomolybdate method respectively at normal temperature, drying and measuring the weight loss quality of the samples after sealing, drawing a weight loss difference relation curve graph of different acid etching weight loss methods for aluminum alloy anodic oxide films with different area ratios under normal temperature as shown in figure 2, wherein the figure shows that the sodium phosphomolybdate method has less mass loss than the phosphochromic acid method, but all the mass loss is 1mg/dm²Within the range, the error is relatively small, so that a sodium phosphomolybdate method can be used for replacing the hole sealing of the phosphoric chromic acid on the aluminum alloy anode oxide film, thereby not polluting the environment and causing the harm to the human body;

taking three aluminum alloy sections with the same area ratio, ensuring that three aluminum alloy section samples with different area ratios are available, sealing the three samples by a phosphochromic acid method, a phosphoric acid method and a sodium phosphomolybdate method at a medium temperature, drying the three samples after sealing the holes, measuring the weight loss quality of the samples, drawing a weight loss difference relation curve chart of the aluminum alloy anodic oxide films with different area ratios under the medium temperature by using different acid etching weight loss methods as shown in figure 3, and showing that the mass loss result error of the sodium phosphomolybdate method and the phosphochromic acid method is smaller and is within +/-1 mg/dm²Within the range, the sodium phosphomolybdate method can be used for replacing the hole sealing of the aluminum alloy anodic oxide film by the phosphochromic acid, thereby not polluting the environment and causing the harm to the human body;

s5, analyzing a surface macro topography of the aluminum alloy anodic oxide film after normal temperature hole sealing and medium temperature hole sealing, as shown in fig. 4 and 8, respectively, a surface macro topography of the aluminum alloy anodic oxide film before normal temperature hole sealing and a surface macro topography of the aluminum alloy anodic oxide film before medium temperature hole sealing are shown, as shown in fig. 4 and 8, the aluminum alloy anodic oxide film is a honeycomb-type porous structure, as shown in fig. 5 ~, respectively, a surface macro topography after hole sealing of the aluminum alloy anodic oxide film by a phosphochromic acid method under normal temperature conditions, a surface macro topography after hole sealing of the aluminum alloy anodic oxide film by a phosphoric acid method under normal temperature conditions, and a surface macro topography after hole sealing of the aluminum alloy anodic oxide film by a sodium phosphomolybdate method under normal temperature conditions are shown, as shown in fig. 5 ~, it can be seen that no dissolution phenomenon occurs on the surface of the aluminum alloy anodic oxide film, the quality of hole sealing is further good, therefore, a sodium phosphomolybdate method can be used for replacing the phosphochromate method for the surface of the aluminum alloy anodic oxide film after hole sealing under the normal temperature condition, and the macro topography of the aluminum alloy anodic oxide film can be found by a sodium phosphomolybdate method for further, and the surface of the anode oxide film can be found that the anode oxide film after hole sealing under the medium temperature hole sealing by a sodium phosphomolybdate method, and the sodium phosphomolybdate method for the anode oxide film is used for the anode oxide film, thus the anode oxide film can be found that the anode oxide film for the anode oxide film under the anode oxide film is found that the anode oxide film under the anode oxide film is found by the sodium phosphomolybdate method for the anode.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.