CN115537904A - A method for obtaining the metallographic structure of aluminum alloy by electrolysis of two-stage electrolyte - Google Patents

A method for obtaining the metallographic structure of aluminum alloy by electrolysis of two-stage electrolyte Download PDF

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CN115537904A
CN115537904A CN202211155377.5A CN202211155377A CN115537904A CN 115537904 A CN115537904 A CN 115537904A CN 202211155377 A CN202211155377 A CN 202211155377A CN 115537904 A CN115537904 A CN 115537904A
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electrolyte
aluminum alloy
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bubbles
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康福伟
卢金龙
汪恩浩
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Harbin University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25FPROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00Electrolytic etching or polishing
    • C25F3/16Polishing
    • C25F3/18Polishing of light metals
    • C25F3/20Polishing of light metals of aluminium
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching

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Abstract

The invention relates to a method for polishing and corroding aluminum alloy by using a two-stage electrolyte, which aims at aluminum alloy with a metallographic structure, such as wrought aluminum alloy and heat-treated aluminum alloy, which is difficult to obtain by using a common treatment method. The proportion of the two-stage electrolyte is as follows: first-stage: perchloric acid 20% -25% methanol 75% -80%, second stage: 10-15% of perchloric acid and 85-90% of ethanol alcohol. According to the invention, the pretreated aluminum alloy is electrolyzed, and the pretreated aluminum alloy is sequentially put into the secondary electrolyte for electrolysis, so that a metallographic phase suitable for observation through OM is obtained. Each electrolyte can be used independently, and the electrolyte of the first grade can be used for removing larger scratches on the surface of the aluminum alloy so as to make the surface smoother. The second stage electrolyte may be used for the electrolyte of a general as-cast aluminum alloy, and the aluminum alloy treated with the second stage electrolyte may be used for an EBSD pattern.

Description

一种利用双级电解液电解得到铝合金金相组织的方法A method for obtaining the metallographic structure of aluminum alloy by electrolysis of two-stage electrolyte

技术领域technical field

一种新的铝合金电解液的配比以及通过电解得到金相组织的方法A new proportion of aluminum alloy electrolyte and method for obtaining metallographic structure by electrolysis

背景技术Background technique

铝合金具有比强度高、性价比高的特点,被广泛的应用于各个领域,也不乏在航空、航天、军事等一些高科技领域的应用。对人们的生产生活产生了很大的影响,所以对于铝合金的研究变得异常的重要,在日常的对铝合金的研究中我们要对其组织进行显微组织观察,要求我们对铝合金表面进行抛光腐蚀处理,而电解抛光腐蚀是一个较优的方式,具有简单、快捷、效果突出的优点。但往往有一些铝合金由于变形或热处理而导致晶界变得细小,从而使晶相难以腐蚀出来。而合适的电解液的配比和腐蚀方法有助于腐蚀出适合观察的晶相组织。Aluminum alloy has the characteristics of high specific strength and high cost performance, and is widely used in various fields, including some high-tech fields such as aviation, aerospace, and military. It has a great impact on people's production and life, so the research on aluminum alloys has become extremely important. In the daily research on aluminum alloys, we need to observe the microstructure of its structure, which requires us to study the surface of aluminum alloys. Polishing and etching are carried out, and electrolytic polishing and etching is a better method, which has the advantages of simplicity, speed and outstanding effect. However, some aluminum alloys often have grain boundaries that become fine due to deformation or heat treatment, making it difficult to corrode the crystal phase. And the appropriate proportion of electrolyte and corrosion method will help to corrode the crystal phase structure suitable for observation.

发明内容Contents of the invention

本发明是利用双级电解液对于特难抛光腐蚀的铝合金进行电解抛光腐蚀,并得到金相组织的方法。The invention is a method for electrolytically polishing and corroding aluminum alloys that are extremely difficult to polish and corrode by using a double-stage electrolyte, and obtaining a metallographic structure.

一级电解液的配比为高氯酸20%-25%甲醇75%-80%,电压20-25v。其作用是为了去除铝合金表面抛光后依然存在的划痕,且使表面更加光亮平整,为后续的进一步电解腐蚀创造条件。The ratio of the primary electrolyte is 20%-25% perchloric acid and 75%-80% methanol, and the voltage is 20-25v. Its function is to remove the scratches that still exist after the aluminum alloy surface is polished, and make the surface brighter and smoother, creating conditions for subsequent further electrolytic corrosion.

二级电解配比为高氯酸10%甲醇90%,电压20-25v。其作用相当于腐蚀液,是为了使铝合金表面能够表现出金相的形貌,以便于更好地观察金相组织。The ratio of the secondary electrolysis is perchloric acid 10% methanol 90%, voltage 20-25v. Its function is equivalent to a corrosive solution, in order to make the surface of the aluminum alloy show a metallographic morphology, so as to better observe the metallographic structure.

用上述电解液进行逐级抛光腐蚀是需要用转子进行旋转搅拌的,以便于带走铝合金表面的气泡使得表面的黑点和气孔减少。在一级电解液里的转速为4-5r/s,在二级电解液里为3r/s。Gradual polishing and corrosion with the above electrolyte requires rotating and stirring with the rotor, so as to take away the bubbles on the surface of the aluminum alloy and reduce the black spots and pores on the surface. The rotational speed in the primary electrolyte is 4-5r/s, and in the secondary electrolyte it is 3r/s.

电解液占据容器的2/3-3/4,容量为500ml的烧杯作为电解液的容器,以便于转子充分的发挥效果。The electrolyte occupies 2/3-3/4 of the container, and the beaker with a capacity of 500ml is used as the container of the electrolyte so that the rotor can fully exert its effect.

选用的铅块大小为50mm×50mm,电解液没过铅块的1/2。The size of the lead block selected is 50mm×50mm, and the electrolyte is submerged in 1/2 of the lead block.

在一级电解液中电流可达到1.5A,在二级电解液中电流可达到0.2A,两者都可在室温下进行。The current can reach 1.5A in the primary electrolyte and 0.2A in the secondary electrolyte, both at room temperature.

在一级电解液中的电解时间为5-20s,在二级电解液中的电解时间为10-15s.The electrolysis time in the primary electrolyte is 5-20s, and the electrolysis time in the secondary electrolyte is 10-15s.

该电解液里不含硝酸,有利于环保。The electrolyte does not contain nitric acid, which is beneficial to environmental protection.

电解液要在避光的环境下保存。The electrolyte should be stored in a dark environment.

一级二级电解液可以有多重用途,每个电解液都可单独使用,一级电解液可用于除去铝合金表面的较大划痕使得表面更光滑。二级电解液可用于容易腐蚀出金相的铝合金的电解抛光腐蚀液,电解后的铝合金可用作EBSD的式样。The primary and secondary electrolytes can be used for multiple purposes, and each electrolyte can be used independently. The primary electrolyte can be used to remove large scratches on the aluminum alloy surface to make the surface smoother. The secondary electrolyte can be used as an electrolytic polishing solution for aluminum alloys that are easy to corrode metal phases, and the electrolytic aluminum alloys can be used as EBSD patterns.

附图说明Description of drawings

图1是铝合金电解示意图Figure 1 is a schematic diagram of aluminum alloy electrolysis

图2是用实例1的双级铝合金电解抛光液进行电解的铝合金金相图。FIG. 2 is a metallographic diagram of an aluminum alloy electrolyzed with the two-stage aluminum alloy electrolytic polishing solution of Example 1. FIG.

图3是用实例2的双级铝合金电解抛光液进行电解的铝合金金相图。FIG. 3 is a metallographic diagram of an aluminum alloy electrolyzed with the two-stage aluminum alloy electrolytic polishing solution of Example 2. FIG.

图4是用实例7的铝合金电解抛光液进行电解抛光的铝合金金相图。FIG. 4 is a metallographic diagram of an aluminum alloy electrolytically polished with the aluminum alloy electrolytic polishing solution of Example 7. FIG.

具体实施方式detailed description

接下来通过几个具体实例来阐述我的发明。Next, set forth my invention by several concrete examples.

实施例1Example 1

本实例是采用双级电解液配比为:一级电解液高氯酸20%甲醇80%;二级电解液高氯酸10%乙醇90%.In this example, the ratio of the two-stage electrolyte is adopted: the primary electrolyte perchloric acid 20% methanol 80%; the secondary electrolyte perchloric acid 10% ethanol 90%.

把预磨(使用砂纸打磨至2000目,再抛光至表面光亮)好的铝合金接入阳极,阴极为铅块。Connect the aluminum alloy that has been pre-ground (sanded to 2000 mesh, and then polished to a bright surface) to the anode, and the cathode is a lead block.

先把放有转子的烧杯放在磁力搅拌装置上,电压调整为25v转速为4r/s,再开启磁力搅拌装置。把铅块和铝合金放入一级电解液中进行电解10s后,拿出用酒精冲洗表面后再在酒精中泡1min,用镊子夹起再用吹风机吹干表面,在光学显微镜上进行观察,若表面有划痕、黑点或气泡,则需要继续重复以上操作直至无划痕、黑点或气泡产生。First put the beaker with the rotor on the magnetic stirring device, adjust the voltage to 25v and rotate at 4r/s, and then turn on the magnetic stirring device. Put the lead block and aluminum alloy into the first-level electrolyte for 10 seconds, take it out and rinse the surface with alcohol, then soak in alcohol for 1 minute, pick it up with tweezers, dry the surface with a hair dryer, and observe it on an optical microscope. If there are scratches, black spots or air bubbles on the surface, you need to continue to repeat the above operations until no scratches, black spots or air bubbles appear.

再把经过一级电解液处理的铝合金以同样的方式浸在二级电解液中5s,电压为25v转子的转速为3r/s,电解时间为15s。Then immerse the aluminum alloy treated with the first-level electrolyte in the second-level electrolyte in the same way for 5s, the voltage is 25v, the rotational speed of the rotor is 3r/s, and the electrolysis time is 15s.

实例2Example 2

过程和实例1的电解液的配比以及操作基本相同,唯一不同的是在一级电解液中电解的时间加改为15s。The proportioning and operation of the electrolyte in the process and Example 1 are basically the same, the only difference is that the time of electrolysis in the primary electrolyte is changed to 15s.

实例3Example 3

过程和实例1的电解液的配比和操作基本相同,唯一不同的是在二级电解液中电解的时间改为10s。The proportioning and operation of the electrolyte of the process and Example 1 are basically the same, the only difference is that the time of electrolysis in the secondary electrolyte is changed to 10s.

实例4Example 4

将电解液的配比设为:一级电解液为高氯酸20%甲醇80%,二级电解液为高氯酸15%乙醇85%,其他操作与实例1相同。The proportioning of electrolyte is set as: primary electrolyte is perchloric acid 20% methanol 80%, secondary electrolyte is perchloric acid 15% ethanol 85%, other operations are identical with example 1.

实例5Example 5

电解液的配比与实例4相同,在一级电解液中电解15s,转子的转速4r/s,电压为20V,在二级电解液中电解5s,转子转速3r/s,电压25v。其他操作与实例1相同。The ratio of the electrolyte is the same as that of Example 4. Electrolyze in the primary electrolyte for 15s, the rotor speed is 4r/s, and the voltage is 20V; in the secondary electrolyte, it is electrolyzed for 5s, the rotor speed is 3r/s, and the voltage is 25v. Other operations are the same as Example 1.

实例6Example 6

在二级电解液中电解10s,其他操作与电解液的配比与实例5相同。Electrolyze 10s in the secondary electrolyte, other operation and the proportioning of electrolyte are identical with example 5.

实例7Example 7

配置电解液高为氯酸20%甲醇80%,进行转子转速4r/s,电压25v,电流1.5A,温度为室温。The electrolyte solution is chloric acid 20% methanol 80%, the rotor speed is 4r/s, the voltage is 25v, the current is 1.5A, and the temperature is room temperature.

实例8Example 8

配置电解液为高氯酸10%乙醇90%,转子转速3r/s,电压25v,电流可达0.2A-0.4A,温度为室温。The electrolyte is configured as perchloric acid 10% ethanol 90%, the rotor speed is 3r/s, the voltage is 25v, the current can reach 0.2A-0.4A, and the temperature is room temperature.

用经过机械抛光后的表面光滑且易腐蚀的铝合金电解10s。Electrolyze for 10s with a smooth and easily corroded aluminum alloy after mechanical polishing.

经过上述实验表明,对于难以腐蚀出晶界的铝合金(各种变形铝合金、热处理铝合金),上述的双级电解液非常的适用,而且每一级的电解液可以单独使用,可达到不同的效果。The above experiments show that for aluminum alloys that are difficult to corrode grain boundaries (various deformed aluminum alloys, heat-treated aluminum alloys), the above-mentioned two-stage electrolyte is very suitable, and the electrolyte of each stage can be used alone to achieve different Effect.

Claims (3)

1. An aluminum alloy electrolyte is characterized by being a two-stage electrolyte. And each electrolyte can be independently used to exert different effects, the primary electrolyte can remove deep scratches on the surface of the pretreated aluminum alloy, and the secondary electrolyte can be used as an electrolytic polishing solution for common cast aluminum alloys.
2. The formula is as follows: first-stage: perchloric acid 20-25% and methanol 75-80%; and (2) second stage: 10-15% of perchloric acid and 85-90% of ethanol. The surface of the aluminum alloy is pretreated before electrolysis (sand paper is ground to 2000 meshes, and then mechanical polishing is carried out until the surface presents a mirror surface). The area of the aluminum alloy polished surface is 16mm2-40mm2. The method is mainly used for metallographic corrosion of the aluminum-copper alloy and the aluminum-silicon alloy in the deformation state and the heat treatment state. Connecting an aluminum alloy with a positive electrode, connecting a negative electrode with a lead block, placing electrolyte put into a rotor on a magnetic stirrer, opening the magnetic stirrer to rotate the rotor so as to fully eliminate a large number of bubbles on the surface of the aluminum alloy, wherein the voltage in the first-stage electrolyte is 20-25v, the electrolysis time is 10-20s, immediately washing the rotor with alcohol after taking out, drying the washed bubbles after 1-2 minutes in the alcohol by using a blower, observing whether bubbles or black spots exist on the surface, continuously carrying out electrolysis if bubbles and black spots exist until the surface is bright and no bubbles exist, and then carrying out second-stage electrolysis, wherein the voltage in the second-stage electrolyte is 20-25v, and the electrolysis time is 5-15s.
3. According to the patent claim 2, the rotor speed in the primary electrolyte is 4-5r/s, the rotor speed in the secondary electrolyte is 3-4r/s, and the requirement for the electrolyte is that the shelf life is one month (or when the solution becomes red), and the electrolyte should be re-proportioned after the solution becomes red.
CN202211155377.5A 2022-09-22 2022-09-22 A method for obtaining the metallographic structure of aluminum alloy by electrolysis of two-stage electrolyte Pending CN115537904A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06128759A (en) * 1992-10-13 1994-05-10 Nippon Steel Corp Corrosion liquid for revealing metallographic structure of aluminum alloy and method for revealing
CN107462456A (en) * 2016-06-03 2017-12-12 宁波江丰电子材料股份有限公司 Method for displaying metallographic structure
CN110208264A (en) * 2019-06-17 2019-09-06 新疆众和股份有限公司 A kind of method for making sample of high-purity aluminium busbar metallographic sample
CN110835778A (en) * 2019-11-21 2020-02-25 哈尔滨工业大学 Aluminum alloy electrolytic polishing solution and electrolytic polishing method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06128759A (en) * 1992-10-13 1994-05-10 Nippon Steel Corp Corrosion liquid for revealing metallographic structure of aluminum alloy and method for revealing
CN107462456A (en) * 2016-06-03 2017-12-12 宁波江丰电子材料股份有限公司 Method for displaying metallographic structure
CN110208264A (en) * 2019-06-17 2019-09-06 新疆众和股份有限公司 A kind of method for making sample of high-purity aluminium busbar metallographic sample
CN110835778A (en) * 2019-11-21 2020-02-25 哈尔滨工业大学 Aluminum alloy electrolytic polishing solution and electrolytic polishing method

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