CN108677237B - Pretreatment liquid for magnesium alloy micro-arc oxidation, magnesium alloy micro-arc oxidation pretreatment method and micro-arc oxidation method - Google Patents
Pretreatment liquid for magnesium alloy micro-arc oxidation, magnesium alloy micro-arc oxidation pretreatment method and micro-arc oxidation method Download PDFInfo
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
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Abstract
The invention discloses a pretreatment liquid for magnesium alloy micro-arc oxidation, a magnesium alloy micro-arc oxidation pretreatment method and a micro-arc oxidation method. According to the invention, 0.03-0.1 mol/L of neodymium nitrate aqueous solution is used for carrying out pretreatment on the magnesium alloy, so that a neodymium oxide film layer is generated on the surface of the magnesium alloy, and then the magnesium alloy with the neodymium oxide film layer is subjected to micro-arc oxidation. The ceramic film obtained by the magnesium alloy micro-arc oxidation method has smoother surface, nd elements can exist in the film in a pretreatment mode, are uniformly distributed in the film, are beneficial to generating a compact ceramic film in the micro-arc oxidation process, reduce the porosity and improve the wear resistance of the film. The corrosion resistance of the magnesium alloy can be obviously improved through the ceramic film layer.
Description
Technical Field
The invention belongs to the technical field of light metal surface treatment, and particularly relates to pretreatment liquid for magnesium alloy micro-arc oxidation, a magnesium alloy micro-arc oxidation pretreatment method and a micro-arc oxidation method.
Background
The magnesium alloy has great application value in the field of materials. Due to urgent energy and environmental problems, magnesium alloys have obvious advantages and have been applied to various fields such as automobile industry, 3C industry, aerospace, metallurgy, chemical industry, modern weapons, nuclear industry, etc. The application range of the magnesium alloy is continuously expanded, but the development of the magnesium alloy is restricted by the high chemical activity and the low mechanical strength of the magnesium. Mg/Mg 2+ The standard equilibrium potential of (2) is-2.34V, and chemical and electrochemical corrosion is extremely easy to occur. Meanwhile, the self-corrosion potential of the magnesium alloy in the aqueous solution is also negative, about-1.5V, and corrosion is easier to occur relative to other metal materials.
Micro-arc oxidation technology is a newer surface treatment technology, and is receiving more and more attention. The micro-arc oxidation technology is mainly applied to valve metals such as aluminum, magnesium, titanium and alloys thereof, and the like, and the micro-arc oxidation technology is more and more attractive because of the pollution-free and clean characteristics. However, micro-arc oxidation techniques still have much work to explore in terms of corrosion resistance. Rare earth metals have extremely important applications and are an important component of new modern high-tech materials. Because rare earth elements are insoluble in a conventional electrolyte system, the rare earth elements are not easy to enter the film, and in order to solve the technical problem, the prior art adopts a pretreatment mode to enable the rare earth elements to enter the surface of the micro-arc oxidation film and improve the performance of the film. For example, the Chinese academic paper (the influence of rare earth Ce on the micro-arc oxidation and corrosion behavior of magnesium alloy) (author, cai Jingshun) discloses that a nitrate compound of rare earth element is dissolved in 30% hydrogen peroxide to prepare a pretreatment liquid, then a magnesium alloy substrate is soaked in the pretreatment liquid at 30 ℃ for 15 minutes, and the micro-arc oxidation substrate with a rare earth conversion film on the surface is prepared after cleaning and drying. However, the rare earth elements in the film prepared by the method are unevenly distributed, and the film has insufficient density and low hardness.
Disclosure of Invention
The invention solves the technical problems that: overcomes the technical defects of insufficient surface density of a ceramic film layer generated by magnesium alloy micro-arc oxidation and poor corrosion resistance of a coating in the prior art, and provides a pretreatment liquid for magnesium alloy micro-arc oxidation, a magnesium alloy micro-arc oxidation pretreatment method and a micro-arc oxidation method.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: the pretreatment liquid for magnesium alloy micro-arc oxidation is neodymium nitrate aqueous solution with the concentration of 0.03-0.1 mol/L.
Further preferably, the concentration of the pretreatment solution is 0.06-0.08 mol/L.
A magnesium alloy micro-arc oxidation pretreatment method comprises the step of immersing polished clean magnesium alloy in the pretreatment liquid for magnesium alloy micro-arc oxidation for 10-40 minutes, so that a neodymium oxide film layer is formed on the surface of the magnesium alloy.
A magnesium alloy micro-arc oxidation method comprises the following steps: in an electrolytic tank filled with electrolyte, taking magnesium alloy containing a rare earth oxide layer as an anode, taking stainless steel as a cathode, putting the stainless steel into the electrolyte, and carrying out micro-arc oxidation under the condition of continuous stirring to enable a ceramic film layer to be generated on the surface of the magnesium alloy; the magnesium alloy containing the rare earth oxide layer is prepared by the magnesium alloy micro-arc oxidation pretreatment method.
Further optimized, the electrolyte is prepared by the following steps: na is mixed with 2 SiO 3 ，KOH，Al 2 O 3 And NaF is added into deionized water and is fully dissolved and dispersed by stirring.
Further optimized, added Na 2 SiO 3 ，KOH，Al 2 O 3 And NaF have mass concentrations of Na 2 SiO 3 8～12g/L，KOH 4～6g/L，Al 2 O 3 1.6～2.4g/L，NaF 0.4～0.6g/L。
Further optimized, the device used for micro-arc oxidation is a 20kW direct current pulse micro-arc oxidation device, and the micro-arc oxidation is carried out under the following parameter conditions: the micro-arc oxidation control voltage is in a constant voltage mode of 350V, the duty ratio is 3-5%, the pulse frequency is 350-450 Hz, and the micro-arc oxidation time is 15-30 min.
Further optimized, the duty ratio is 4%, the pulse frequency is 400Hz, and the micro-arc oxidation time is 20min
The invention has the technical effects that: (1) The magnesium alloy is soaked in a neodymium nitrate pretreatment solution with the concentration of 0.03-0.1 mol/L, so that a neodymium compound film layer is formed on the surface of the magnesium alloy, and neodymium elements can exist in the film layer in a pretreatment mode and are uniformly distributed in the film layer. (2) After the magnesium alloy is pretreated by the neodymium nitrate solution, micro-arc oxidation is carried out, so that a compact ceramic film layer with smaller porosity is generated in the micro-arc oxidation process, and the thickness of the formed ceramic film layer is 17-23 mu m. (3) The surface of the prepared ceramic film layer is smoother, the ceramic film layer has high hardness, strong adhesion with the surface of a matrix and better wear resistance. (4) In Nd (NO) 3 ) 3 The magnesium alloy is pretreated in the pretreatment liquid with the concentration of 0.06mol/L to 0.08mol/L, and then micro-arc oxidation is carried out to obtain a sample, wherein the ceramic film layer is more compact, the adhesion force with the surface of the magnesium alloy is stronger, and the corrosion resistance is better. And (5) the pretreatment process is simple and is beneficial to industrial production.
Drawings
FIG. 1 is a graph showing polarization curves of a substrate and magnesium alloy micro-arc oxide films prepared in comparative example 1, comparative example 2 and examples 1 to 4;
FIG. 2 is a graph of acoustic Signal Intensity (SI) and friction force (Ff) curves and corresponding wear patterns for a ceramic film layer of a magnesium alloy micro-arc oxidized article made in comparative example 1.
FIG. 3 is a graph of acoustic Signal Intensity (SI) and friction force (Ff) curves and corresponding wear patterns for a ceramic film layer of a magnesium alloy micro-arc oxidized article made in comparative example 2.
FIG. 4 is a graph of acoustic Signal Intensity (SI) and friction force (Ff) curves and corresponding scratch patterns for a ceramic film layer of a magnesium alloy micro-arc oxidized article prepared in example 3.
FIG. 5 is a graph of acoustic Signal Intensity (SI) and friction force (Ff) curves and corresponding scratch patterns for a ceramic film layer of a magnesium alloy micro-arc oxidized article prepared in example 4.
FIG. 6 is a graph showing the abrasion of the ceramic film layer of the magnesium alloy micro-arc oxidized product prepared in comparative example 2 measured by a frictional abrasion tester.
FIG. 7 is a graph showing the abrasion of the ceramic film layer of the magnesium alloy micro-arc oxidized product prepared in example 2 measured by a frictional abrasion tester.
Detailed Description
The invention is further described in connection with the following examples in which Nd (NO) 3 ) 3 、Na 2 SiO 3 、、KOH、Al 2 O 3 And NaF are analytically pure.
Example 1
Preparation of pretreatment liquid for magnesium alloy micro-arc oxidation: nd (NO) 3 ) 3 0.0015mol was added to 50mL of deionized water, and the mixture was stirred to dissolve and disperse the mixture.
Magnesium alloy micro-arc oxidation pretreatment: firstly, a rectangular flaky KBM10 magnesium alloy substrate with the thickness of 30mm multiplied by 25mm multiplied by 3mm is firstly polished by sand paper, then deoiled, washed by deionized water and dried to obtain a polished clean magnesium alloy sheet. And then, completely immersing the polished clean magnesium alloy sheet into the pretreatment liquid, and immersing for 10min at room temperature, so that a thin neodymium oxide film layer is generated on the surface of the magnesium alloy, namely, the pretreatment of micro-arc oxidation of the magnesium alloy is completed, and the magnesium alloy containing the rare earth oxide layer is prepared.
The magnesium alloy micro-arc oxidation comprises the following steps:
(1) 30g of Na 2 SiO 3 ，15g KOH，6g Al 2 O 3 And 1.5g NaF, added into 3L deionized water, and stirred thoroughlyDissolving and dispersing to prepare electrolyte.
(3) And (3) filling the electrolyte into a 20kW direct current pulse micro-arc oxidation device, taking the magnesium alloy containing the rare earth oxide layer as an anode, taking a stainless steel plate as a cathode, putting the magnesium alloy into the electrolyte, controlling the reaction voltage to be 350V, the duty ratio to be 4%, and the pulse frequency to be 400Hz, and continuously stirring for constant current micro-arc oxidation for 20min to enable a compact ceramic film layer to be generated on the surface of the magnesium alloy. The obtained ceramic coating has smooth surface and small roughness.
Example 2:
preparation of pretreatment liquid for magnesium alloy micro-arc oxidation: nd (NO) 3 ) 3 0.003mol was added to 50mL of deionized water, and the mixture was stirred to be sufficiently dissolved and dispersed.
Magnesium alloy micro-arc oxidation pretreatment: firstly, a rectangular flaky KBM10 magnesium alloy substrate with the thickness of 30mm multiplied by 25mm multiplied by 3mm is firstly polished by sand paper, then deoiled, washed by deionized water and dried to obtain a polished clean magnesium alloy sheet. And then, completely immersing the polished clean magnesium alloy sheet into the pretreatment liquid, and immersing for 20min at room temperature, so that a thin neodymium oxide film layer is generated on the surface of the magnesium alloy, namely, the pretreatment of micro-arc oxidation of the magnesium alloy is completed, and the magnesium alloy containing the rare earth oxide layer is prepared.
The magnesium alloy micro-arc oxidation comprises the following steps:
(1) 24g of Na 2 SiO 3 ，18g KOH，7.2g Al 2 O 3 And 1.2g NaF, adding into 3L deionized water, stirring to dissolve and disperse, and making into electrolyte.
(3) And (3) filling the electrolyte into a 20kW direct current pulse micro-arc oxidation device, taking the magnesium alloy containing the rare earth oxide layer as an anode, taking a stainless steel plate as a cathode, putting the magnesium alloy into the electrolyte, controlling the reaction voltage to be 350V, the duty ratio to be 3%, and the pulse frequency to be 400Hz, and continuously stirring for constant current micro-arc oxidation for 15min to enable a compact ceramic film layer to be generated on the surface of the magnesium alloy. The obtained ceramic coating has smooth surface and small roughness.
Example 3
Preparation of pretreatment liquid for magnesium alloy micro-arc oxidation: nd (NO) 3 ) 3 0.004mol, added into 50mL deionized water, and fully dissolved and dispersed by stirring.
Magnesium alloy micro-arc oxidation pretreatment: firstly, a rectangular flaky KBM10 magnesium alloy substrate with the thickness of 30mm multiplied by 25mm multiplied by 3mm is firstly polished by sand paper, then deoiled, washed by deionized water and dried to obtain a polished clean magnesium alloy sheet. And then, completely immersing the polished clean magnesium alloy sheet into the pretreatment liquid, and immersing for 20min at room temperature, so that a thin neodymium oxide film layer is generated on the surface of the magnesium alloy, namely, the pretreatment of micro-arc oxidation of the magnesium alloy is completed, and the magnesium alloy containing the rare earth oxide layer is prepared.
The magnesium alloy micro-arc oxidation comprises the following steps:
(1) 36g of Na 2 SiO 3 ，12g KOH，6g Al 2 O 3 And 1.5g NaF, adding into 3L deionized water, stirring to dissolve and disperse, and making into electrolyte.
(3) And (3) filling the electrolyte into a 20kW direct current pulse micro-arc oxidation device, taking the magnesium alloy containing the rare earth oxide layer as an anode, taking a stainless steel plate as a cathode, putting the magnesium alloy into the electrolyte, controlling the reaction voltage to be 350V, the duty ratio to be 4%, and the pulse frequency to be 400Hz, and continuously stirring for constant current micro-arc oxidation for 20min to enable the surface of the magnesium alloy to generate a ceramic film layer. The obtained ceramic coating has smooth surface and small roughness.
Example 4
Preparation of pretreatment liquid for magnesium alloy micro-arc oxidation: nd (NO) 3 ) 3 0.005mol was added to 50mL of deionized water, and the mixture was stirred to dissolve and disperse the mixture.
Magnesium alloy micro-arc oxidation pretreatment: firstly, a rectangular flaky KBM10 magnesium alloy substrate with the thickness of 30mm multiplied by 25mm multiplied by 3mm is firstly polished by sand paper, then deoiled, washed by deionized water and dried to obtain a polished clean magnesium alloy sheet. And then, completely immersing the polished clean magnesium alloy sheet into the pretreatment liquid for 40min, so that a thin neodymium oxide film layer is formed on the surface of the magnesium alloy, namely, the magnesium alloy micro-arc oxidation pretreatment is finished, and the magnesium alloy containing the rare earth oxide layer is prepared.
The magnesium alloy micro-arc oxidation comprises the following steps:
(1) 30g of Na 2 SiO 3 ，15g KOH，4.8g Al 2 O 3 And 1.8g NaF, adding into 3L deionized water, stirring to dissolve and disperse, and making into electrolyte.
(3) And (3) filling the electrolyte into a 20kW direct current pulse micro-arc oxidation device, taking the magnesium alloy containing the rare earth oxide layer as an anode, taking a stainless steel plate as a cathode, putting the magnesium alloy into the electrolyte, controlling the reaction voltage to be 350V, the duty ratio to be 5%, and the pulse frequency to be 400Hz, and continuously stirring for constant current micro-arc oxidation for 30min to enable the surface of the magnesium alloy to generate a ceramic film layer. The obtained ceramic coating has smooth surface and small roughness.
Comparative example 1
Magnesium alloy micro-arc oxidation pretreatment: the rectangular sheet KBM10 magnesium alloy matrix with the thickness of 30mm multiplied by 25mm multiplied by 3mm is firstly polished by sand paper, then deoiled, washed by deionized water and dried, and the polished clean magnesium alloy sheet is obtained.
Micro-arc oxidation of magnesium alloy:
(1) 30g of Na 2 SiO 3 ，15g KOH，6g Al 2 O 3 And 1.5g NaF, adding into 3L deionized water, stirring to dissolve and disperse, and making into electrolyte.
(3) And (3) filling the electrolyte into a 20kW direct current pulse micro-arc oxidation device, taking the polished clean magnesium alloy sheet as an anode, taking a stainless steel plate as a cathode, putting the stainless steel plate into the electrolyte, controlling the reaction voltage to be 350V, the duty ratio to be 4%, and the pulse frequency to be 400Hz, and continuously stirring for constant current micro-arc oxidation for 20min to enable the magnesium alloy surface to generate a ceramic film layer.
Comparative example 2
Preparation of pretreatment liquid for magnesium alloy micro-arc oxidation: nd (NO) 3 ) 3 0.001mol, added to 50mL of deionized waterStirring to dissolve and disperse in the seed water.
Magnesium alloy micro-arc oxidation pretreatment: firstly, a rectangular flaky KBM10 magnesium alloy substrate with the thickness of 30mm multiplied by 25mm multiplied by 3mm is firstly polished by sand paper, then deoiled, washed by deionized water and dried to obtain a polished clean magnesium alloy sheet. And then, completely immersing the polished clean magnesium alloy sheet into the pretreatment liquid for 20min, so that a thin neodymium-bearing oxide layer is formed on the surface of the magnesium alloy, namely, the magnesium alloy micro-arc oxidation pretreatment is finished, and the magnesium alloy containing the rare earth oxide layer is prepared.
The magnesium alloy micro-arc oxidation comprises the following steps:
(1) 30g of Na 2 SiO 3 ，15g KOH，6g Al 2 O 3 And 1.5g NaF, adding into 3L deionized water, stirring to dissolve and disperse, and making into electrolyte.
(3) And (3) filling the electrolyte into a 20kW direct current pulse micro-arc oxidation device, taking the magnesium alloy containing the rare earth oxide layer as an anode, taking a stainless steel plate as a cathode, putting the magnesium alloy into the electrolyte, controlling the reaction voltage to be 350V, the duty ratio to be 4%, and the pulse frequency to be 400Hz, and continuously stirring for constant current micro-arc oxidation for 20min to enable the surface of the magnesium alloy to generate a ceramic film layer. The obtained ceramic coating has smooth surface and small roughness.
Effect examples
The ceramic film layer generated on the surface of the magnesium alloy is tested and analyzed by an energy spectrometer (EDS), and the test results are shown in Table 1. The test results showed that Nd (NO 3 ) 3 The concentration of the solution is increased, and Nd element is gradually added into the film layer. When Nd (NO) 3 ) 3 When the concentration is 0.06mol/L, the Nd element content in the film layer is the highest, and the surface is uniform.
TABLE 1 content of elemental layers for EDS test
Anode electrode determination by potentiostatic methodThe chemical curves are shown in fig. 1, and fig. 1 is a graph showing the polarization curves of the substrate and the magnesium alloy micro-arc oxide film layers prepared in comparative example 1, comparative example 2 and examples 1 to 4, and fig. 1 is a graph showing the polarization curves of the magnesium alloy micro-arc oxide film layers prepared in comparative example 1, comparative example 2, example 1, example 2, example 3 and example 4, respectively, corresponding to (a), (b), (c), (d), (e) and (f) in fig. 1. Wherein the matrix is KBM10 magnesium alloy which is not subjected to micro-arc oxidation, and the fitting data of polarization curves are shown in Table 2. Referring to fig. 1 and table 2, it can be seen that Nd (NO 3 ) 3 The corrosion resistance of the film layer is continuously improved due to the increase of the solution concentration, the corrosion potential is positively moved, the corrosion current is continuously reduced, the corrosion current is improved by three orders of magnitude relative to the substrate when the soaking concentration reaches 0.06mol/L, and the corrosion current is improved by two orders of magnitude relative to the film layer which is not pretreated.
TABLE 2 matrix, NO pretreatment and Nd (NO) 3 ) 3 Polarization curve fitting data of magnesium alloy micro-arc oxidation film layer subjected to solution pretreatment
Test of the ceramic film layer of the magnesium alloy micro-arc oxidized products prepared in comparative example 1, comparative example 2, example 2 and example 4 by using WS-2005 coating adhesion automatic scratcher test f ) And (3) curve and observing the abrasion characteristics of the ceramic membrane layer by combining an optical microscope. The test results are shown in fig. 2, 3, 4 and 5. The graph shows that the critical load of the ceramic film layer generated by the magnesium alloy through pretreatment of 0.03-0.1 mol/L neodymium nitrate solution and micro-arc oxidation is obviously improved, and the critical load is improved from 20N to 40N. As can be seen from the scratch photo, the strength of the ceramic film layer obtained by micro-arc oxidation after the pretreatment of neodymium nitrate is obviously improved, and the magnesium alloy substrate is hardly exposed, namely the film layer is more compact and has higher strength.
Samples prepared in comparative examples 1, 2, 3 and 4 were placed in a frictional wear testing machine using a load of 4.9NOn top of that, si is used 3 N 4 The ceramic balls were subjected to a frictional wear test for 30 minutes to test mass loss and wear rate of samples before and after frictional wear, and the test results are shown in table 3. And combining a scanning electron microscope, observing the abrasion conditions of the ceramic film layers of the sample of the comparative example 2 and the sample of the example 2 after the frictional abrasion test is finished, and particularly obtaining the results shown in fig. 6 and 7.
TABLE 3 mass loss and wear Rate before and after frictional wear test sample under 4.9N load
Claims (3)
1. A magnesium alloy micro-arc oxidation method is characterized in that: the method comprises the following steps: in an electrolytic tank filled with electrolyte, taking magnesium alloy containing a rare earth oxide layer as an anode, taking stainless steel as a cathode, putting the stainless steel into the electrolyte, and carrying out micro-arc oxidation under the condition of continuous stirring to enable a ceramic film layer to be generated on the surface of the magnesium alloy; the magnesium alloy containing the rare earth oxide layer is prepared by a magnesium alloy micro-arc oxidation pretreatment method; the magnesium alloy micro-arc oxidation pretreatment method comprises the steps of soaking polished clean magnesium alloy in pretreatment liquid for magnesium alloy micro-arc oxidation for 10-40 minutes, so that a neodymium oxide film layer is formed on the surface of the magnesium alloy; the pretreatment liquid for magnesium alloy micro-arc oxidation is neodymium nitrate aqueous solution with the concentration of 0.06 mol/L;
the electrolyte is prepared by the following steps: na is mixed with 2 SiO 3 ，KOH，Al 2 O 3 Adding NaF into deionized water, stirring to fully dissolve and disperse;
the added Na 2 SiO 3 ，KOH，Al 2 O 3 And NaF have mass concentrations of Na 2 SiO 3 8~12 g/L，KOH 4~6 g/L，Al 2 O 3 1.6~2.4 g/L，NaF 0.4~0.6 g/L。
2. The method for micro-arc oxidation of magnesium alloy according to claim 1, wherein the device used for micro-arc oxidation is a 20kW direct current pulse micro-arc oxidation device, and the micro-arc oxidation is performed under the following parameter conditions: the micro-arc oxidation control voltage is in a constant voltage mode of 350-V, the duty ratio is 3-5%, the pulse frequency is 350-450 Hz, and the micro-arc oxidation time is 15-30 min.
3. The method of micro-arc oxidation of magnesium alloy according to claim 2, wherein the duty cycle is 4%, the pulse frequency is 400Hz, and the micro-arc oxidation time is 20 min.
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