CN102409371B - Method for detecting micro-arc oxidation arcing characteristics of alloy by using anodic polarization curve - Google Patents

Method for detecting micro-arc oxidation arcing characteristics of alloy by using anodic polarization curve Download PDF

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CN102409371B
CN102409371B CN 201110387712 CN201110387712A CN102409371B CN 102409371 B CN102409371 B CN 102409371B CN 201110387712 CN201110387712 CN 201110387712 CN 201110387712 A CN201110387712 A CN 201110387712A CN 102409371 B CN102409371 B CN 102409371B
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田修波
王晓波
巩春志
杨士勤
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Harbin Institute of Technology Shenzhen
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Abstract

利用阳极极化曲线检测合金微弧氧化起弧特性的方法,本发明涉及合金微弧氧化的方法。本发明是要解决现有的利用微弧氧化实验过程去验证电解液中添加剂的种类及用量对微弧氧化起弧特性影响的方法而造成的工作量大、浪费电能和溶液原料的技术问题。本发明的方法:测定合金在待验证电解液中的以电压U为横坐标、以电流I为纵坐标的阳极极化曲线,以是否存在钝化区来确定是否可以进行微弧氧化,以钝化区间宽窄,确定合金在电解液中微弧氧化起弧放电的电压高低,当钝化区间宽度相近时,以钝化膜层失稳前极化电流的大小确定合金在该电解液中微弧氧化起弧放电电压高低;本发明的方法为低压、低电流密度过程,节约能源。可用于预测合金微弧氧化起弧特性。

Figure 201110387712

The invention relates to a method for detecting arc-starting characteristics of alloy micro-arc oxidation by using anodic polarization curve, and the invention relates to a method for alloy micro-arc oxidation. The present invention aims to solve the technical problems of large workload, waste of electric energy and solution raw materials caused by the existing method of using the micro-arc oxidation experiment process to verify the influence of the type and amount of additives in the electrolyte on the arc-starting characteristics of the micro-arc oxidation. The method of the present invention: measure the anodic polarization curve of the alloy in the electrolytic solution to be verified with the voltage U as the abscissa and the current I as the ordinate, and whether there is a passivation zone to determine whether micro-arc oxidation can be carried out to passivate The width of the passivation interval determines the voltage level of the micro-arc oxidation arc discharge of the alloy in the electrolyte. When the width of the passivation interval is similar, the value of the polarization current before the passivation film layer becomes unstable determines the micro-arc of the alloy in the electrolyte. Oxidation arc discharge voltage is high or low; the method of the present invention is a low-voltage, low-current-density process, which saves energy. It can be used to predict the arc starting characteristics of alloy micro-arc oxidation.

Figure 201110387712

Description

利用阳极极化曲线检测合金微弧氧化起弧特性的方法The Method of Using Anode Polarization Curve to Detect the Arcing Characteristics of Alloy Micro-arc Oxidation

技术领域 technical field

本发明涉及合金微弧氧化的方法。The invention relates to a method for alloy micro-arc oxidation.

背景技术 Background technique

镁合金以其密度小、比强比刚度高、电磁屏蔽性好等优点被应用于航空、汽车和电子通讯等工业领域。但是由于镁化学性质活泼,极易氧化,在表面形成疏松多孔的氧化膜,该氧化膜对基体的保护能力差,不适合使用于大多数的腐蚀环境,其耐蚀性差的缺点制约了其进一步的应用。微弧氧化在一种在阳极氧化基础上发展起来的表面改性技术,该技术是将镁、铝、钛等金属或其合金置于电解液中,在高温高压、热化学、等离子体化学和电化学等共同作用下使材料的表面产生火花放电生成陶瓷膜层的方法。该技术具有工艺简单,对环境污染少、效率高等特点,且微弧氧化陶瓷膜具有膜基结合力强、耐磨损、耐腐蚀、耐高温氧化以及绝缘性好等优点,因此利用微弧氧化对镁合金进行表面改性前景良好。Magnesium alloys are used in industrial fields such as aviation, automobiles and electronic communications due to their advantages such as low density, high specific strength and specific stiffness, and good electromagnetic shielding. However, due to the active chemical properties of magnesium, it is very easy to oxidize, and a loose and porous oxide film is formed on the surface. The oxide film has poor protection ability for the substrate and is not suitable for use in most corrosive environments. Applications. Micro-arc oxidation is a surface modification technology developed on the basis of anodic oxidation. This technology is to place metals such as magnesium, aluminum, titanium or their alloys in the electrolyte, under high temperature and high pressure, thermochemistry, plasma chemistry and The method of generating spark discharge on the surface of the material to form a ceramic film layer under the combined action of electrochemistry and the like. This technology has the characteristics of simple process, less environmental pollution and high efficiency, and the micro-arc oxidation ceramic film has the advantages of strong film-base binding force, wear resistance, corrosion resistance, high temperature oxidation resistance and good insulation, so the use of micro-arc oxidation Surface modification of magnesium alloys is promising.

由于微弧氧化是高电压、高电流密度的工作过程,在实际生产中当一次性处理面积较大时会出现对微弧氧化电源或电网额定功率要求较高、能源利用率低等问题。电解液配方是影响微弧氧化反应的重要因素之一,适当的电解液添加剂对于降低微弧氧化的工作电压进而降低微弧氧化处理所需要的功率具有明显作用,但是由于化学添加剂种类繁多,含何种添加剂的电解液可以进行微弧氧化放电,何种添加剂有利于降低微弧氧化放电电压,都要利用高电压、高电流密度的微弧氧化实验过程去验证,这使得工作量巨大,而且浪费了大量的电能和溶液原料。Because micro-arc oxidation is a high-voltage, high-current-density working process, in actual production, when the one-time treatment area is large, there will be problems such as high requirements for the power supply of micro-arc oxidation or the rated power of the grid, and low energy utilization. The electrolyte formula is one of the important factors affecting the micro-arc oxidation reaction. Appropriate electrolyte additives have a significant effect on reducing the working voltage of the micro-arc oxidation and thus reducing the power required for the micro-arc oxidation process. Which kind of additive electrolyte can carry out micro-arc oxidation discharge, and which additive is beneficial to reduce the voltage of micro-arc oxidation discharge, must be verified by high-voltage, high-current-density micro-arc oxidation experimental process, which makes the workload huge, and A large amount of electric energy and solution raw materials are wasted.

发明内容 Contents of the invention

本发明是要解决现有的利用微弧氧化实验过程去验证电解液中添加剂的种类及用量对微弧氧化起弧特性影响的方法而造成的工作量大、浪费电能和溶液原料的技术问题,而提供利用阳极极化曲线检测合金微弧氧化起弧特性的方法。The present invention aims to solve the technical problems of large workload, waste of electric energy and solution raw materials caused by the existing method of using the micro-arc oxidation experiment process to verify the influence of the type and amount of additives in the electrolyte on the arc-starting characteristics of the micro-arc oxidation. And it provides a method for detecting arcing characteristics of alloy micro-arc oxidation by using anodic polarization curve.

本发明的利用阳极极化曲线检测合金微弧氧化起弧特性的方法按以下步骤进行:The method of utilizing the anodic polarization curve of the present invention to detect the arcing characteristics of alloy micro-arc oxidation is carried out according to the following steps:

一、制备待验证电解液;1. Prepare the electrolyte to be verified;

二、测定合金在步骤一中得到的待验证电解液中的以电压U为横坐标、以电流I为纵坐标的阳极极化曲线;Two, measure the anodic polarization curve with the voltage U as the abscissa and the current I as the ordinate in the electrolytic solution to be verified obtained in step 1;

三、经步骤二测得的阳极极化曲线上,如果不存在钝化区,则合金在该电解液中不能进行微弧氧化;如果存在钝化区,则合金在该电解液中能进行微弧氧化;钝化区间越宽,则合金在该电解液中微弧氧化起弧放电的电压越低;钝化区间宽度相近时,阳极极化曲线上钝化膜层失稳前极化电流越小,则合金在该电解液中微弧氧化起弧放电电压越低;从而得出合金微弧氧化起弧特性。3. On the anodic polarization curve measured in step 2, if there is no passivation zone, the alloy cannot undergo micro-arc oxidation in the electrolyte; if there is a passivation zone, the alloy can undergo micro-arc oxidation in the electrolyte Arc oxidation; the wider the passivation interval, the lower the voltage of the alloy in the electrolyte for micro-arc oxidation arc discharge; when the passivation interval is similar, the polarization current on the anodic polarization curve before the passivation film becomes unstable The smaller the value, the lower the arc discharge voltage of the alloy in the electrolyte, and thus the arc start characteristics of the alloy are obtained.

本发明采用电压-电流格式的阳极极化曲线来判断镁合金在电解液中能否进行微弧氧化放电及在不同种电解液中微弧氧化放电电压的高低次序,以相应电解液作为镁合金电化学极化行为时的工作液,通过阳极极化曲线,判断镁合金在该电解液中是否可以进行微弧氧化放电及在不同电解液中进行微弧氧化起弧放电时起弧电压的高低,为微弧氧化电解液添加剂的选择提供一个简单有效的参考手段。在阳极极化曲线上,如果不存在钝化区,即合金在该电解液中不能发生钝化现象,则合金在该电解液中不能进行微弧氧化放电行为;在阳极极化曲线上,如果存在钝化区,即合金在该电解液中能发生钝化现象,则合金在该电解液中能够进行微弧氧化放电行为;微弧氧化起弧电压的判定分两步进行:首先,合金在不同电解液中起弧电压的高低通过在相应电解液中的阳极极化曲线的钝化区间来判断。在阳极极化曲线上,钝化区间越宽,则在相应电解液中合金微弧氧化起弧放电电压越低;在可以进行微弧氧化起弧放电的电解液中,当合金阳极极化曲线上钝化区间宽度相近时,起弧电压的高低通过阳极极化曲线上钝化膜失稳前极化电流电流大小判断。阳极极化曲线上钝化膜层失稳前极化电流越小,则在相应电解液中合金微弧氧化起弧放电电压越低。本发明的方法中测试合金阳极极化曲线的条件相对于微弧氧化来说,是一个低压、低电流密度的过程,从而可以简化判断合金微弧氧化特性的过程,进而节约能源。The present invention adopts the anode polarization curve of the voltage-current format to determine whether the magnesium alloy can be subjected to micro-arc oxidation discharge in the electrolyte and the high and low order of the micro-arc oxidation discharge voltage in different electrolytes, and uses the corresponding electrolyte as the magnesium alloy The working solution in the electrochemical polarization behavior, through the anodic polarization curve, judge whether the magnesium alloy can perform micro-arc oxidation discharge in the electrolyte and the level of arc starting voltage when performing micro-arc oxidation discharge in different electrolytes , to provide a simple and effective reference method for the selection of additives in micro-arc oxidation electrolyte. On the anodic polarization curve, if there is no passivation zone, that is, the alloy cannot passivate in the electrolyte, the alloy cannot perform micro-arc oxidation discharge behavior in the electrolyte; on the anodic polarization curve, if There is a passivation zone, that is, the alloy can undergo passivation in the electrolyte, and the alloy can perform micro-arc oxidation discharge behavior in the electrolyte; the determination of the arc-starting voltage of the micro-arc oxidation is carried out in two steps: first, the alloy is in The level of arcing voltage in different electrolytes is judged by the passivation interval of the anodic polarization curve in the corresponding electrolyte. On the anodic polarization curve, the wider the passivation interval, the lower the alloy micro-arc oxidation arc discharge voltage in the corresponding electrolyte; When the width of the upper passivation interval is similar, the level of the arcing voltage can be judged by the magnitude of the polarization current before the passivation film is unstable on the anodic polarization curve. On the anodic polarization curve, the smaller the polarization current before the passivation film becomes unstable, the lower the arc discharge voltage of alloy micro-arc oxidation in the corresponding electrolyte. Compared with the micro-arc oxidation, the condition for testing the alloy anodic polarization curve in the method of the invention is a low-voltage, low-current-density process, thereby simplifying the process of judging the characteristics of the alloy micro-arc oxidation, thereby saving energy.

本发明可用于预测合金微弧氧化起弧特性。The invention can be used to predict the arc starting characteristics of alloy micro-arc oxidation.

附图说明 Description of drawings

图1是试验一的步骤二中测得的阳极极化曲线,其中a为第一种为浓度为10g/L的硅酸钠水溶液中AZ31镁合金的阳极极化曲线,b为第二种为浓度为10g/L的磷酸钠水溶液中AZ31镁合金的阳极极化曲线;c为第三种为浓度为10g/L的氯化钾水溶液中AZ31镁合金的阳极极化曲线;d为第四种为浓度为10g/L钼酸钠水溶液中AZ31镁合金的阳极极化曲线;e为第五种为浓度为10g/L的磷酸二氢钠水溶液中AZ31镁合金的阳极极化曲线;Fig. 1 is the anodic polarization curve that records in the step 2 of test one, and wherein a is the anodic polarization curve that the first kind is the AZ31 magnesium alloy in the sodium silicate aqueous solution of 10g/L for concentration, and b is that the second kind is Concentration is the anodic polarization curve of AZ31 magnesium alloy in sodium phosphate aqueous solution of 10g/L; c is the third kind is the anodic polarization curve of AZ31 magnesium alloy in potassium chloride aqueous solution with concentration of 10g/L; d is the fourth kind Concentration is the anodic polarization curve of AZ31 magnesium alloy in 10g/L sodium molybdate aqueous solution; e is the anodic polarization curve of AZ31 magnesium alloy in the sodium dihydrogen phosphate aqueous solution that concentration is 10g/L for the fifth;

图2是试验二的步骤二中测得的阳极极化曲线;其中f为AZ31镁合金在浓度为10g/L的硅酸钠水溶液中的阳极极化曲线;g为AZ31镁合金在浓度为10g/L的磷酸钠水溶液中的阳极极化曲线;h为AZ31镁合金在浓度为10g/L的氟化钠水溶液中的阳极极化曲线;i为AZ31镁合金在浓度为10g/L的碳酸钠水溶液中的阳极极化曲线;j为AZ31镁合金在浓度为10g/L的氢氧化钾水溶液的阳极极化曲线;k为AZ31镁合金在磷酸钠的浓度为5g/L、氢氧化钾的浓度为1g/L的混合水溶液的阳极极化曲线;l为AZ31镁合金在磷酸钠的浓度为5g/L、氢氧化钾的浓度为1g/L、氟化钠的浓度为5g/L的混合水溶液中的阳极极化曲线;m为AZ31镁合金在磷酸钠的浓度为5g/L、硅酸钠的浓度为5g/L的混合水溶液的阳极极化曲线;n为AZ31镁合金在氢氧化钾的浓度为1g/L、氟化钠的浓度为5g/L的混合水溶液中的阳极极化曲线;o为AZ31镁合金在硅酸钠的浓度为5g/L、氟化钠的浓度为5g/L的混合水溶液中的阳极极化曲线;Fig. 2 is the anodic polarization curve that records in the step 2 of test two; Wherein f is the anodic polarization curve of AZ31 magnesium alloy in the sodium silicate aqueous solution that concentration is 10g/L; G is the concentration of AZ31 magnesium alloy is 10g The anodic polarization curve in the sodium phosphate aqueous solution of /L; h is the anodic polarization curve of AZ31 magnesium alloy in the sodium fluoride aqueous solution with concentration of 10g/L; i is the sodium carbonate of AZ31 magnesium alloy in the concentration of 10g/L Anodic polarization curve in aqueous solution; j is the anodic polarization curve of AZ31 magnesium alloy in potassium hydroxide aqueous solution with concentration of 10g/L; k is the concentration of AZ31 magnesium alloy in sodium phosphate concentration of 5g/L, potassium hydroxide concentration is the anodic polarization curve of the mixed aqueous solution of 1g/L; l is the mixed aqueous solution whose concentration of sodium phosphate is 5g/L, the concentration of potassium hydroxide is 1g/L, and the concentration of sodium fluoride is 5g/L for AZ31 magnesium alloy The anodic polarization curve in; m is the anodic polarization curve of AZ31 magnesium alloy in the mixed aqueous solution whose concentration of sodium phosphate is 5g/L, and the concentration of sodium silicate is 5g/L; n is the anodic polarization curve of AZ31 magnesium alloy in potassium hydroxide The anodic polarization curve in a mixed aqueous solution with a concentration of 1g/L and a concentration of sodium fluoride of 5g/L; o is AZ31 magnesium alloy in a concentration of sodium silicate of 5g/L and a concentration of sodium fluoride of 5g/L The anodic polarization curve in the mixed aqueous solution;

图3是试验二的AZ31镁合金阳极极化曲线上钝化区间宽度图;Fig. 3 is a passivation interval width diagram on the AZ31 magnesium alloy anodic polarization curve of test two;

图4是试验二AZ31镁合金阳极极化曲线上钝化膜层失稳前极化电流图。Fig. 4 is a diagram of the polarization current on the anodic polarization curve of the second test AZ31 magnesium alloy before the passivation film becomes unstable.

具体实施方式 Detailed ways

具体实施方式一:本实施方式的利用阳极极化曲线检测合金微弧氧化起弧特性的方法按以下步骤进行:Specific implementation mode 1: The method for detecting the arcing characteristics of alloy micro-arc oxidation by using the anodic polarization curve in this embodiment is carried out according to the following steps:

一、制备待验证电解液;1. Prepare the electrolyte to be verified;

二、测定合金在步骤一中得到的待验证电解液中的以电压U为横坐标、以电流I为纵坐标的阳极极化曲线;Two, measure the anodic polarization curve with the voltage U as the abscissa and the current I as the ordinate in the electrolytic solution to be verified obtained in step 1;

三、经步骤二测得的阳极极化曲线上,如果不存在钝化区,则合金在该电解液中不能进行微弧氧化;如果存在钝化区,则合金在该电解液中能进行微弧氧化;钝化区间越宽,则合金在该电解液中微弧氧化起弧放电的电压越低;钝化区间宽度相近时,阳极极化曲线上钝化膜层失稳前极化电流越小,则合金在该电解液中微弧氧化起弧放电电压越低;从而得出合金微弧氧化起弧特性。3. On the anodic polarization curve measured in step 2, if there is no passivation zone, the alloy cannot undergo micro-arc oxidation in the electrolyte; if there is a passivation zone, the alloy can undergo micro-arc oxidation in the electrolyte Arc oxidation; the wider the passivation interval, the lower the voltage of the alloy in the electrolyte for micro-arc oxidation arc discharge; when the passivation interval is similar, the polarization current on the anodic polarization curve before the passivation film becomes unstable The smaller the value, the lower the arc discharge voltage of the alloy in the electrolyte, and thus the arc start characteristics of the alloy are obtained.

本实施方式的方法利用合金阳极极化曲线来畔的条件相对于微弧氧化来说,是一个低压、低电流密度的过程,从而可以简化判断合金微弧氧化特性的过程,进而节约能源。Compared with micro-arc oxidation, the method of this embodiment utilizes the condition of alloy anodic polarization curve, which is a process of low pressure and low current density, so that the process of judging the characteristics of alloy micro-arc oxidation can be simplified, and energy can be saved.

具体实施方式二:本实施方式与具体实施方式一不同的是步骤二中的合金为镁合金,铝合金或钛合金。其它与具体实施方式一相同。Embodiment 2: This embodiment differs from Embodiment 1 in that the alloy in step 2 is magnesium alloy, aluminum alloy or titanium alloy. Others are the same as in the first embodiment.

具体实施方式三:本实施方式与具体实施方式一或二不同的是步骤二中的阳极极化曲线是用恒电位法测定的。其它与具体实施方式一或二相同。Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the anodic polarization curve in step 2 is measured by a potentiostatic method. Others are the same as in the first or second embodiment.

具体实施方式四:本实施方式与具体实施方式与一或二不同的是步骤二中的阳极极化曲线的测定方法如下:采用CHI604C的电化学综合测试平台,采用三电极系统,参比电极为饱和的甘汞电极,辅助电极选用铂电极,被测合金做为阳极,待验证电解液作为腐蚀介质;电位测量范围为:扫描电位-2至(6~9)V,扫描速度0.01V/s,扫描前静止10S;当整个曲线扫描完毕之后得到的是常见的电压-电流对数曲线,将电位-电流对数曲线转换为电压-电流曲线即为所需要的阳极极化曲线。其它与具体实施方式一或二相同。Specific embodiment four: the difference between this embodiment and specific embodiment one or two is that the measuring method of the anodic polarization curve in step 2 is as follows: adopt the electrochemical comprehensive test platform of CHI604C, adopt three-electrode system, and reference electrode is Saturated calomel electrode, platinum electrode as the auxiliary electrode, the alloy to be tested as the anode, and the electrolyte to be verified as the corrosion medium; the potential measurement range is: scanning potential -2 to (6 ~ 9) V, scanning speed 0.01V/s , stand still for 10S before scanning; when the entire curve is scanned, the common voltage-current logarithmic curve is obtained, and the potential-current logarithmic curve is converted into a voltage-current curve, which is the required anodic polarization curve. Others are the same as in the first or second embodiment.

本发明用以下试验验证本发明的有益效果:The present invention verifies the beneficial effect of the present invention with following test:

试验一:本试验的利用阳极极化曲线检测合金微弧氧化起弧特性的方法按以下步骤进行:Test 1: In this test, the method of using the anodic polarization curve to detect the arcing characteristics of alloy micro-arc oxidation is carried out according to the following steps:

一、制备待验证电解液;其中待验证电解液有五种,第一种为浓度为10g/L的硅酸钠水溶液,第二种为浓度为10g/L的磷酸钠水溶液;第三种为浓度为10g/L的氯化钾水溶液;第四种为浓度为10g/L钼酸钠水溶液;第五种为浓度为10g/L的磷酸二氢钠水溶液;1. Prepare the electrolyte solution to be verified; among them, there are five kinds of electrolyte solutions to be verified, the first is a sodium silicate aqueous solution with a concentration of 10g/L, the second is a sodium phosphate aqueous solution with a concentration of 10g/L; the third is Concentration is the potassium chloride aqueous solution of 10g/L; The fourth kind is the concentration and is the sodium molybdate aqueous solution of 10g/L; The fifth kind is the sodium dihydrogen phosphate aqueous solution that the concentration is 10g/L;

二、恒电位法测定合金阳极极化曲线的设备及步骤为:用上海辰华仪器公司生产的CHI604C的电化学综合测试平台测定AZ31镁合金在步骤一中得到的待验证电解液中的阳极极化曲线;测试过程采用三电极系统,参比电极为饱和的甘汞电极,辅助电极选用铂电极,被测AZ31镁合金做为阳极;待验证电解液作为腐蚀介质;电位测量范围为:扫描电位-2至9V,扫描速度0.01V/s,扫描前静止10S,得到电压-电流对数曲线,再将电位-电流对数曲线转换为以电压U为横坐标、以电流I为纵坐标的阳极极化曲线;2. The equipment and steps for determining the anodic polarization curve of the alloy by the constant potential method are: use the CHI604C electrochemical comprehensive test platform produced by Shanghai Chenhua Instrument Company to measure the anode electrode in the electrolyte to be verified for the AZ31 magnesium alloy obtained in step 1 The test process uses a three-electrode system, the reference electrode is a saturated calomel electrode, the auxiliary electrode is a platinum electrode, and the AZ31 magnesium alloy to be tested is used as the anode; the electrolyte to be verified is used as the corrosion medium; the potential measurement range is: scanning potential -2 to 9V, scan speed 0.01V/s, stand still for 10S before scanning, get the voltage-current logarithmic curve, and then convert the potential-current logarithmic curve into an anode with the voltage U as the abscissa and the current I as the ordinate Polarization curve;

三、经步骤二测得的阳极极化曲线上,如果不存在钝化区,则合金在该电解液中不能进行微弧氧化;如果存在钝化区,则合金在该电解液中能进行微弧氧化;钝化区间越宽,则合金在该电解液中微弧氧化起弧放电的电压越低;钝化区间宽度相近时,阳极极化曲线上钝化膜层失稳前极化电流越小,则合金在该电解液中微弧氧化起弧放电电压越低;从而得出合金微弧氧化起弧特性。3. On the anodic polarization curve measured in step 2, if there is no passivation zone, the alloy cannot undergo micro-arc oxidation in the electrolyte; if there is a passivation zone, the alloy can undergo micro-arc oxidation in the electrolyte Arc oxidation; the wider the passivation interval, the lower the voltage of the alloy in the electrolyte for micro-arc oxidation arc discharge; when the passivation interval is similar, the polarization current on the anodic polarization curve before the passivation film becomes unstable The smaller the value, the lower the arc discharge voltage of the alloy in the electrolyte, and thus the arc start characteristics of the alloy are obtained.

其中步骤二中测得的阳极极化曲线如图1所示,其中a为第一种为浓度为10g/L的硅酸钠水溶液中AZ31镁合金的阳极极化曲线,b为第二种为浓度为10g/L的磷酸钠水溶液中AZ31镁合金的阳极极化曲线;c为第三种为浓度为10g/L的氯化钾水溶液中AZ31镁合金的阳极极化曲线;d为第四种为浓度为10g/L钼酸钠水溶液中AZ31镁合金的阳极极化曲线;e为第五种为浓度为10g/L的磷酸二氢钠水溶液中AZ31镁合金的阳极极化曲线;Wherein the anodic polarization curve recorded in step 2 is as shown in Figure 1, wherein a is the anodic polarization curve of the AZ31 magnesium alloy in the sodium silicate aqueous solution of 10g/L for the first kind of wherein a, and b is the second kind of Concentration is the anodic polarization curve of AZ31 magnesium alloy in sodium phosphate aqueous solution of 10g/L; c is the third kind is the anodic polarization curve of AZ31 magnesium alloy in potassium chloride aqueous solution with concentration of 10g/L; d is the fourth kind Concentration is the anodic polarization curve of AZ31 magnesium alloy in 10g/L sodium molybdate aqueous solution; e is the anodic polarization curve of AZ31 magnesium alloy in the sodium dihydrogen phosphate aqueous solution that concentration is 10g/L for the fifth;

从图1可以看出,c、d和e三条曲线阳极极化曲线上不存在钝化区间,因此,在浓度为10g/L的氯化钾水溶液或浓度为10g/L钼酸钠水溶液和浓度为10g/L的磷酸二氢钠水溶液中,AZ31镁合金不能进行微弧氧化起弧放电;而a和b两条阳极极化曲线上存在钝化区间,因此,在浓度为10g/L的硅酸钠水溶液或浓度为10g/L的磷酸钠水溶液中,AZ31镁合金可以进行微弧氧化起弧放电。该结果与实际所测得的结果相同。As can be seen from Figure 1, there is no passivation interval on the anodic polarization curves of the three curves of c, d and e. Therefore, in the potassium chloride aqueous solution with a concentration of 10g/L or the aqueous solution of sodium molybdate with a concentration of 10g/L In the sodium dihydrogen phosphate aqueous solution of 10g/L, the AZ31 magnesium alloy cannot be subjected to micro-arc oxidation arc discharge; and there are passivation intervals on the two anode polarization curves of a and b. Therefore, in the concentration of 10g/L silicon In sodium phosphate aqueous solution or sodium phosphate aqueous solution with a concentration of 10g/L, AZ31 magnesium alloy can be subjected to micro-arc oxidation and arc discharge. This result is the same as the actually measured result.

试验二:本试验的利用阳极极化曲线检测合金微弧氧化起弧特性的方法按以下步骤进行:Test 2: In this test, the method of using the anodic polarization curve to detect the arcing characteristics of alloy micro-arc oxidation is carried out according to the following steps:

一、制备待验证电解液;其中待验证电解液有如下十种:1. Prepare the electrolyte to be verified; among them, there are the following ten electrolytes to be verified:

(1)浓度为10g/L的硅酸钠水溶液;(1) concentration is the sodium silicate aqueous solution of 10g/L;

(2)浓度为10g/L的磷酸钠水溶液;(2) concentration is the sodium phosphate aqueous solution of 10g/L;

(3)浓度为10g/L的氟化钠水溶液;(3) Aqueous sodium fluoride solution whose concentration is 10g/L;

(4)浓度为10g/L的碳酸钠水溶液;(4) concentration is the sodium carbonate aqueous solution of 10g/L;

(5)浓度为10g/L的氢氧化钾水溶液;(5) Concentration is the potassium hydroxide aqueous solution of 10g/L;

(6)磷酸钠的浓度为5g/L、氢氧化钾的浓度为1g/L的混合水溶液;(6) The concentration of sodium phosphate is 5g/L, and the concentration of potassium hydroxide is a mixed aqueous solution of 1g/L;

(7)磷酸钠的浓度为5g/L、氢氧化钾的浓度为1g/L、氟化钠的浓度为5g/L的混合水溶液;(7) The concentration of sodium phosphate is 5g/L, the concentration of potassium hydroxide is 1g/L, the concentration of sodium fluoride is the mixed aqueous solution of 5g/L;

(8)磷酸钠的浓度为5g/L、硅酸钠的浓度为5g/L的混合水溶液;(8) The concentration of sodium phosphate is 5g/L, the concentration of sodium silicate is the mixed aqueous solution of 5g/L;

(9)氢氧化钾的浓度为1g/L、氟化钠的浓度为5g/L的混合水溶液;(9) The concentration of potassium hydroxide is 1g/L, the concentration of sodium fluoride is the mixed aqueous solution of 5g/L;

(10)硅酸钠的浓度为5g/L、氟化钠的浓度为5g/L的混合水溶液;(10) The concentration of sodium silicate is 5g/L, the concentration of sodium fluoride is the mixed aqueous solution of 5g/L;

二、恒电位法测定合金阳极极化曲线的设备及步骤为:用上海辰华仪器公司生产的CHI604C的电化学综合测试平台测定AZ31镁合金在步骤一中得到的待验证电解液中的阳极极化曲线;测试过程采用三电极系统,参比电极为饱和的甘汞电极,辅助电极选用铂电极,被测AZ31镁合金做为阳极;待验证电解液作为腐蚀介质;电位测量范围为:扫描电位-2至9V,扫描速度0.01V/s,扫描前静止10S,得到电压-电流对数曲线,再将电位-电流对数曲线转换为以电压U为横坐标、以电流I为纵坐标的阳极极化曲线;2. The equipment and steps for determining the anodic polarization curve of the alloy by the constant potential method are: use the CHI604C electrochemical comprehensive test platform produced by Shanghai Chenhua Instrument Company to measure the anode electrode in the electrolyte to be verified for the AZ31 magnesium alloy obtained in step 1 The test process uses a three-electrode system, the reference electrode is a saturated calomel electrode, the auxiliary electrode is a platinum electrode, and the AZ31 magnesium alloy to be tested is used as the anode; the electrolyte to be verified is used as the corrosion medium; the potential measurement range is: scanning potential -2 to 9V, scan speed 0.01V/s, stand still for 10S before scanning, get the voltage-current logarithmic curve, and then convert the potential-current logarithmic curve into an anode with the voltage U as the abscissa and the current I as the ordinate Polarization curve;

三、经步骤二测得的阳极极化曲线上,如果不存在钝化区,则合金在该电解液中不能进行微弧氧化;如果存在钝化区,则合金在该电解液中能进行微弧氧化;钝化区间越宽,则合金在该电解液中微弧氧化起弧放电的电压越低;钝化区间宽度相近时,阳极极化曲线上钝化膜层失稳前极化电流越小,则合金在该电解液中微弧氧化起弧放电电压越低;从而得出合金微弧氧化起弧特性。3. On the anodic polarization curve measured in step 2, if there is no passivation zone, the alloy cannot undergo micro-arc oxidation in the electrolyte; if there is a passivation zone, the alloy can undergo micro-arc oxidation in the electrolyte Arc oxidation; the wider the passivation interval, the lower the voltage of the alloy in the electrolyte for micro-arc oxidation arc discharge; when the passivation interval is similar, the polarization current on the anodic polarization curve before the passivation film becomes unstable The smaller the value, the lower the arc discharge voltage of the alloy in the electrolyte, and thus the arc start characteristics of the alloy are obtained.

其中步骤二中测得的阳极极化曲线如图2所示,图2中,f为AZ31镁合金在浓度为10g/L的硅酸钠水溶液中的阳极极化曲线;g为AZ31镁合金在浓度为10g/L的磷酸钠水溶液中的阳极极化曲线;h为AZ31镁合金在浓度为10g/L的氟化钠水溶液中的阳极极化曲线;i为AZ31镁合金在浓度为10g/L的碳酸钠水溶液中的阳极极化曲线;j为AZ31镁合金在浓度为10g/L的氢氧化钾水溶液的阳极极化曲线;k为AZ31镁合金在磷酸钠的浓度为5g/L、氢氧化钾的浓度为1g/L的混合水溶液的阳极极化曲线;l为AZ31镁合金在磷酸钠的浓度为5g/L、氢氧化钾的浓度为1g/L、氟化钠的浓度为5g/L的混合水溶液中的阳极极化曲线;m为AZ31镁合金在磷酸钠的浓度为5g/L、硅酸钠的浓度为5g/L的混合水溶液的阳极极化曲线;n为AZ31镁合金在氢氧化钾的浓度为1g/L、氟化钠的浓度为5g/L的混合水溶液中的阳极极化曲线;o为AZ31镁合金在硅酸钠的浓度为5g/L、氟化钠的浓度为5g/L的混合水溶液中的阳极极化曲线。Wherein the anodic polarization curve measured in step 2 is as shown in Figure 2, among Fig. 2, f is the anodic polarization curve of AZ31 magnesium alloy in the sodium silicate aqueous solution that concentration is 10g/L; G is the anodic polarization curve of AZ31 magnesium alloy in The concentration is the anodic polarization curve in the sodium phosphate aqueous solution of 10g/L; h is the anodic polarization curve of the AZ31 magnesium alloy in the sodium fluoride aqueous solution with the concentration of 10g/L; i is the AZ31 magnesium alloy in the concentration of 10g/L The anodic polarization curve in the sodium carbonate aqueous solution; j is the anodic polarization curve of the AZ31 magnesium alloy in the potassium hydroxide aqueous solution whose concentration is 10g/L; Potassium concentration is the anodic polarization curve of the mixed aqueous solution of 1g/L; l is AZ31 magnesium alloy in the concentration of sodium phosphate is 5g/L, the concentration of potassium hydroxide is 1g/L, the concentration of sodium fluoride is 5g/L The anodic polarization curve in the mixed aqueous solution; m is the anodic polarization curve of the mixed aqueous solution in which the concentration of sodium phosphate and sodium silicate is 5g/L for AZ31 magnesium alloy; n is the anodic polarization curve of AZ31 magnesium alloy in hydrogen The concentration of potassium oxide is 1g/L, the concentration of sodium fluoride is the anodic polarization curve in the mixed aqueous solution of 5g/L; o is AZ31 magnesium alloy in the concentration of sodium silicate is 5g/L, the concentration of sodium fluoride is Anodic polarization curve in 5g/L mixed aqueous solution.

从图2可以看出,AZ31镁合金在本试验的十种电解液中的阳极极化曲线上都存在钝化区间,因此,AZ31镁合金在这十种电解液中都可以进行微弧氧化起弧放电;本试验的方法中测试合金阳极极化曲线的条件相对于微弧氧化来说,是一个低压、低电流密度的过程,从而可以简化判断合金微弧氧化特性的过程,进而节约能源。It can be seen from Figure 2 that there are passivation intervals on the anodic polarization curves of the AZ31 magnesium alloy in the ten electrolytes in this test. Arc discharge: Compared with micro-arc oxidation, the conditions for testing the alloy anodic polarization curve in this test method are a process of low pressure and low current density, which can simplify the process of judging the characteristics of alloy micro-arc oxidation, thereby saving energy.

在不同电解液中AZ31镁合金阳极极化曲线上钝化区间宽度如图3所示,其具体数据如表1所示。The width of the passivation interval on the anodic polarization curve of AZ31 magnesium alloy in different electrolytes is shown in Figure 3, and the specific data are shown in Table 1.

表1不同电解液中AZ31镁合金阳极极化曲线上钝化区间宽度Table 1 Width of passivation interval on the anodic polarization curve of AZ31 magnesium alloy in different electrolytes

  序号 serial number   电解液 Electrolyte  钝化区间宽度(V) Passivation interval width (V)   f f   10g/L的硅酸钠 10g/L sodium silicate   4.94 4.94   g g   10g/L的磷酸钠 10g/L sodium phosphate   4.95 4.95   h h   10g/L的氟化钠 10g/L sodium fluoride   4.82 4.82 ii   10g/L的碳酸钠 10g/L of sodium carbonate   5.03 5.03   j j   10g/L的氢氧化钾 10g/L Potassium Hydroxide   5.12 5.12   k k   5g/L磷酸钠+1g/L氢氧化钾 5g/L Sodium Phosphate+1g/L Potassium Hydroxide   6.83 6.83   l l   5g/L磷酸钠+1g/L氢氧化钾+5g/L氟化钠 5g/L Sodium Phosphate+1g/L Potassium Hydroxide+5g/L Sodium Fluoride   9.95 9.95   m m   5g/L磷酸钠+5g/L硅酸钠 5g/L Sodium Phosphate+5g/L Sodium Silicate   4.82 4.82   n n   1g/L氢氧化钾+5g/L氟化钠 1g/L Potassium Hydroxide + 5g/L Sodium Fluoride   9.98 9.98   o o   5g/L硅酸钠+5g/L氟化钠 5g/L sodium silicate+5g/L sodium fluoride   9.96 9.96

在阳极极化曲线上,钝化区间越宽,则在相应电解液中AZ31镁合金微弧氧化起弧放电电压越低;则从表1初步可以看出,AZ31镁合金微弧氧化起弧放电电压U的大小顺序为:(Ul,Un,Uo)<Uk<(Uf,Ug,Uh,Ui,Uj,Um)On the anodic polarization curve, the wider the passivation interval, the lower the arc discharge voltage of AZ31 magnesium alloy micro-arc oxidation in the corresponding electrolyte; it can be seen from Table 1 that the arc discharge voltage of AZ31 magnesium alloy micro-arc oxidation The magnitude order of the voltage U is: (Ul, Un, Uo)<Uk<(Uf, Ug, Uh, Ui, Uj, Um)

当AZ31镁合金阳极极化曲线上钝化区间宽度相近时,阳极极化曲线上钝化膜层失稳前极化电流越小,则在相应电解液中镁合金微弧氧化起弧放电电压越低。When the width of the passivation interval on the anodic polarization curve of AZ31 magnesium alloy is similar, the smaller the polarization current before the passivation film on the anodic polarization curve becomes unstable, the higher the arc discharge voltage of magnesium alloy micro-arc oxidation in the corresponding electrolyte. Low.

本试验中在钝化区间宽度相近的电解液中,钝化膜层失稳前极化电流如图4所示,其具体数值如表2所示。In this test, in the electrolyte with similar passivation interval width, the polarization current before the passivation film layer becomes unstable is shown in Figure 4, and its specific values are shown in Table 2.

表2不同电解液中AZ31镁合金阳极极化曲线上钝化膜层失稳前极化电流Table 2 Polarization current before the passivation film layer is unstable on the anodic polarization curve of AZ31 magnesium alloy in different electrolytes

Figure BDA0000113878300000071
Figure BDA0000113878300000071

从表2可以看出,AZ31镁合金微弧氧化起弧放电电压U的大小顺序为:It can be seen from Table 2 that the magnitude sequence of the arc discharge voltage U of AZ31 magnesium alloy micro-arc oxidation is:

Ul<Un<Uo;Ul<Un<Uo;

Uj<Uh<Uf<Um<Ug<UiUj<Uh<Uf<Um<Ug<Ui

综合可以得出:Ul<Un<Uo<Uk<Uj<Uh<Uf<Um<Ug<UiComprehensively, it can be concluded that: Ul<Un<Uo<Uk<Uj<Uh<Uf<Um<Ug<Ui

实验结果与预测结果相同。本试验的方法中测试合金阳极极化曲线的条件相对于微弧氧化来说,是一个低压、低电流密度的过程,从而可以简化判断合金微弧氧化特性的过程,进而节约能源。The experimental results are the same as the predicted results. Compared with the micro-arc oxidation, the conditions for testing the anodic polarization curve of the alloy in this test method are a low-pressure, low-current-density process, which can simplify the process of judging the characteristics of the alloy micro-arc oxidation, thereby saving energy.

Claims (3)

1.利用阳极极化曲线检测合金微弧氧化起弧特性的方法,其特征在于利用阳极极化曲线检测合金微弧氧化起弧特性的方法按以下步骤进行:1. Utilize the method of anodic polarization curve detection alloy micro-arc oxidation arc starting characteristic, it is characterized in that utilize anodic polarization curve to detect the method for alloy micro-arc oxidation arc starting characteristic to carry out as follows: 一、制备待验证电解液;1. Prepare the electrolyte to be verified; 二、测定合金在步骤一中得到的待验证电解液中的以电压U为横坐标、以电流I为纵坐标的阳极极化曲线;Two, measure the anodic polarization curve with the voltage U as the abscissa and the current I as the ordinate in the electrolytic solution to be verified obtained in step 1; 三、经步骤二测得的阳极极化曲线上,如果不存在钝化区,则合金在该电解液中不能进行微弧氧化;如果存在钝化区,则合金在该电解液中能进行微弧氧化;钝化区间越宽,则合金在该电解液中微弧氧化起弧放电的电压越低;钝化区间宽度相近时,阳极极化曲线上钝化膜层失稳前极化电流越小,则合金在该电解液中微弧氧化起弧放电电压越低;从而得出合金微弧氧化起弧特性;3. On the anodic polarization curve measured in step 2, if there is no passivation zone, the alloy cannot undergo micro-arc oxidation in the electrolyte; if there is a passivation zone, the alloy can undergo micro-arc oxidation in the electrolyte Arc oxidation; the wider the passivation interval, the lower the voltage of the alloy in the electrolyte for micro-arc oxidation arc discharge; when the passivation interval is similar, the polarization current on the anodic polarization curve before the passivation film becomes unstable The smaller the value, the lower the arc discharge voltage of the alloy in the electrolyte; thus the arc start characteristics of the alloy are obtained; 所述的步骤二中的阳极极化曲线的测定方法如下:采用CHI604C的电化学综合测试平台,采用三电极系统,参比电极为饱和的甘汞电极,辅助电极选用铂电极,被测合金做为阳极,待验证电解液作为腐蚀介质;电位测量范围为:扫描电位-2至6V~9V,扫描速度0.01V/s,扫描前静止10S;当整个曲线扫描完毕之后得到的是常见的电压-电流对数曲线,将电位-电流对数曲线转换为电压-电流曲线即为所需要的阳极极化曲线。The measurement method of the anodic polarization curve in the described step 2 is as follows: the electrochemical comprehensive test platform of CHI604C is adopted, a three-electrode system is adopted, the reference electrode is a saturated calomel electrode, the auxiliary electrode is a platinum electrode, and the tested alloy is made of It is an anode, and the electrolyte to be verified is used as a corrosion medium; the potential measurement range is: scanning potential -2 to 6V ~ 9V, scanning speed 0.01V/s, and resting for 10S before scanning; when the entire curve is scanned, the common voltage is obtained - Current logarithmic curve, the potential-current logarithmic curve is converted into a voltage-current curve is the required anodic polarization curve. 2.根据权利要求1所述的利用阳极极化曲线检测合金微弧氧化起弧特性的方法,其特征在于步骤二中的合金为镁合金,铝合金或钛合金。2. The method according to claim 1, characterized in that the alloy in step 2 is magnesium alloy, aluminum alloy or titanium alloy. 3.根据权利要求1或2所述的利用阳极极化曲线检测合金微弧氧化起弧特性的方法,其特征在于步骤二中的阳极极化曲线是用恒电位法测定的。3. The method according to claim 1 or 2, characterized in that the anodic polarization curve in step 2 is measured by a potentiostatic method.
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CN101698957A (en) * 2009-10-29 2010-04-28 中国科学院长春应用化学研究所 Micro-arc oxidation treatment method of heat-resistant cast rare earth magnesium alloy

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