鎂合金表面磁控濺射Al膜的制備工藝及組織性能研究
發(fā)布時(shí)間：2019-05-19 07:57
【摘要】：鎂合金是最輕的結(jié)構(gòu)材料,具有許多優(yōu)越的性能和廣闊的應(yīng)用前景,但其耐腐蝕性能較差的弱點(diǎn)是影響其應(yīng)用的重要因素。提高鎂合金的耐蝕性是當(dāng)前鎂合金開(kāi)發(fā)與研究的重要課題,其中制備涂層是改善鎂合金表面耐腐蝕性能的重要途徑。在諸多涂層制備技術(shù)中,磁控濺射技術(shù)由于具有沉積速率高、膜層均勻、密度和純度高、附著力強(qiáng)等優(yōu)點(diǎn)被認(rèn)為是制備表面涂層的最佳方法之一。基于鋁有較好的耐腐蝕性能,本工作采用磁控濺射技術(shù),在AZ91鎂合金表面制備高純鋁膜,對(duì)膜層制備的工藝、膜層微觀組織和腐蝕性能進(jìn)行了研究。首先利用正交試驗(yàn)方法,以膜層耐蝕性以及界面結(jié)合力、膜厚和粗糙度為指標(biāo),對(duì)磁控濺射鋁膜的濺射功率、基體加熱溫度、負(fù)偏壓等工藝參數(shù)進(jìn)行了優(yōu)化,得到了對(duì)實(shí)驗(yàn)指標(biāo)影響的參數(shù)順序和獲得良好綜合性能的參數(shù)組合。其后對(duì)影響性能的主要工藝參數(shù)進(jìn)行了單因素實(shí)驗(yàn),研究了各參數(shù)對(duì)膜層組織和性能的影響趨勢(shì),依據(jù)膜層腐蝕機(jī)制分析了組織對(duì)耐腐蝕性能影響的原因。正交試驗(yàn)研究結(jié)果表明,影響膜層性能的磁控濺射工藝參數(shù)主次順序?yàn)?濺射功率、基體加熱溫度、基體的負(fù)偏壓、Ar氣壓強(qiáng)和濺射時(shí)間,磁控濺射鋁膜的最優(yōu)工藝參數(shù)組合為:濺射功率60W,濺射時(shí)間120min,基體加熱溫度200℃,Ar氣壓強(qiáng)2.1Pa,基體負(fù)偏壓-150V。對(duì)鋁膜的組織觀察表明,完整的膜層可大致分為底側(cè)的等軸晶區(qū),等軸晶向柱狀晶的過(guò)渡區(qū),以及外側(cè)的柱狀晶區(qū)三個(gè)區(qū)域。改變工藝參數(shù)會(huì)使膜層的整體厚度和各區(qū)域的大小發(fā)生變化。提高濺射功率可增大膜層厚度,同時(shí)柱狀晶區(qū)域擴(kuò)大,等軸晶與柱狀晶之間的過(guò)渡層變窄。提高基體加熱溫度和延長(zhǎng)濺射時(shí)間時(shí),膜層組織將也發(fā)生類(lèi)似的變化。工藝參數(shù)對(duì)界面結(jié)合力也有明顯的影響。隨著濺射功率和基體加熱溫度的提高以及濺射時(shí)間的增加,界面結(jié)合力都呈現(xiàn)出先提高后降低的變化,當(dāng)濺射功率為60W、基體加熱溫度為200℃、濺射時(shí)間為120min時(shí),界面結(jié)合力最強(qiáng)。對(duì)試樣腐蝕過(guò)程的分析表明,磁控濺射鋁膜對(duì)鎂合金基體可以起到一定的保護(hù)作用。對(duì)于鋁膜的模擬汗液腐蝕來(lái)講,腐蝕優(yōu)先發(fā)生在膜層表面的晶界位置,并且沿晶界向膜層內(nèi)部發(fā)展,一旦膜層局部腐蝕穿透,腐蝕介質(zhì)將進(jìn)入基體和鋁膜層之間的界面,從而構(gòu)成原電池加速腐蝕的進(jìn)行,并導(dǎo)致膜層從基體上剝離。因此,膜層厚度盡可能大,且膜層以等軸晶區(qū)和過(guò)渡區(qū)為主,同時(shí)界面結(jié)合力強(qiáng),是膜層具有良好腐蝕性能的重要條件。
[Abstract]:Magnesium alloy is the mildest structural material, which has many superior properties and broad application prospects, but the weakness of its poor corrosion resistance is an important factor affecting its application. Improving the corrosion resistance of magnesium alloys is an important topic in the development and research of magnesium alloys, and the preparation of coatings is an important way to improve the corrosion resistance of magnesium alloys. Among many coating preparation technologies, magnetron sputter technology is considered to be one of the best methods to prepare surface coatings because of its high deposition rate, uniform film layer, high density and purity, strong adhesion and so on. Based on the good corrosion resistance of aluminum, high purity aluminum film was prepared on the surface of AZ91 magnesium alloy by magnetron sputter. The preparation process, microstructure and corrosion properties of the film were studied. Firstly, the process parameters such as corrosion resistance, interfacial adhesion, film thickness and roughness of magnetron sputter aluminum films were optimized by orthogonal test, such as the deposition power, substrate heating temperature and negative bias voltage of the aluminum films deposited by magnetron, and the corrosion resistance, interfacial adhesion, film thickness and roughness of the films were optimized by orthogonal test. The parameter sequence affecting the experimental index and the parameter combination with good comprehensive performance are obtained. Then the single factor experiment was carried out on the main process parameters affecting the properties, and the influence trend of each parameter on the microstructure and properties of the film was studied. According to the corrosion mechanism of the film, the reasons for the influence of microstructure on the corrosion resistance were analyzed. The results of orthogonal test show that the primary and secondary order of magnetron sputtering process parameters affecting the properties of the film is as follows: sputtering power, substrate heating temperature, negative bias voltage of substrate, Ar pressure and sputter time. The optimum technological parameters of magnetron sputter aluminum film are as follows: sputter power 60W, sputter time 120min, substrate heating temperature 200C, Ar pressure 2.1Pa, substrate negative bias voltage-150V. The observation of the microstructure of the aluminum film shows that the complete film can be roughly divided into three regions: the isometric crystal region on the bottom side, the transition zone from the isometric crystal to the columnar crystal, and the columnar crystal region on the outer side. Changing the process parameters will change the overall thickness of the film and the size of each region. Increasing the sputter power can increase the thickness of the film, at the same time, the columnar crystal region is enlarged, and the transition layer between the isometric crystal and the columnar crystal becomes narrower. When the heating temperature of the substrate is increased and the sputter time is prolonged, the microstructure of the film will change similarly. The process parameters also have obvious influence on the interfacial adhesion. With the increase of sputter power, substrate heating temperature and sputter time, the interfacial adhesion increases at first and then decreases. When the sputter power is 60W, the substrate heating temperature is 200C, and the sputter time is 120min, The interfacial adhesion is the strongest. The analysis of the corrosion process of the sample shows that the magnetron sputter aluminum film can protect the magnesium alloy matrix to a certain extent. For the simulated sweat corrosion of aluminum film, the corrosion occurs first at the grain boundary position on the surface of the film, and develops along the grain boundary to the inner layer of the film. Once the local corrosion penetration of the film layer, the corrosion medium will enter the interface between the substrate and the aluminum film. Thus, the corrosion of the original battery is accelerated and the film is peeled off from the substrate. Therefore, the thickness of the film is as large as possible, and the film is dominated by isometric crystal region and transition zone, and the interface adhesion is strong, which is an important condition for the film to have good corrosion performance.
【學(xué)位授予單位】：內(nèi)蒙古工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：TG174.44
本文編號(hào)：2480538
[Abstract]:Magnesium alloy is the mildest structural material, which has many superior properties and broad application prospects, but the weakness of its poor corrosion resistance is an important factor affecting its application. Improving the corrosion resistance of magnesium alloys is an important topic in the development and research of magnesium alloys, and the preparation of coatings is an important way to improve the corrosion resistance of magnesium alloys. Among many coating preparation technologies, magnetron sputter technology is considered to be one of the best methods to prepare surface coatings because of its high deposition rate, uniform film layer, high density and purity, strong adhesion and so on. Based on the good corrosion resistance of aluminum, high purity aluminum film was prepared on the surface of AZ91 magnesium alloy by magnetron sputter. The preparation process, microstructure and corrosion properties of the film were studied. Firstly, the process parameters such as corrosion resistance, interfacial adhesion, film thickness and roughness of magnetron sputter aluminum films were optimized by orthogonal test, such as the deposition power, substrate heating temperature and negative bias voltage of the aluminum films deposited by magnetron, and the corrosion resistance, interfacial adhesion, film thickness and roughness of the films were optimized by orthogonal test. The parameter sequence affecting the experimental index and the parameter combination with good comprehensive performance are obtained. Then the single factor experiment was carried out on the main process parameters affecting the properties, and the influence trend of each parameter on the microstructure and properties of the film was studied. According to the corrosion mechanism of the film, the reasons for the influence of microstructure on the corrosion resistance were analyzed. The results of orthogonal test show that the primary and secondary order of magnetron sputtering process parameters affecting the properties of the film is as follows: sputtering power, substrate heating temperature, negative bias voltage of substrate, Ar pressure and sputter time. The optimum technological parameters of magnetron sputter aluminum film are as follows: sputter power 60W, sputter time 120min, substrate heating temperature 200C, Ar pressure 2.1Pa, substrate negative bias voltage-150V. The observation of the microstructure of the aluminum film shows that the complete film can be roughly divided into three regions: the isometric crystal region on the bottom side, the transition zone from the isometric crystal to the columnar crystal, and the columnar crystal region on the outer side. Changing the process parameters will change the overall thickness of the film and the size of each region. Increasing the sputter power can increase the thickness of the film, at the same time, the columnar crystal region is enlarged, and the transition layer between the isometric crystal and the columnar crystal becomes narrower. When the heating temperature of the substrate is increased and the sputter time is prolonged, the microstructure of the film will change similarly. The process parameters also have obvious influence on the interfacial adhesion. With the increase of sputter power, substrate heating temperature and sputter time, the interfacial adhesion increases at first and then decreases. When the sputter power is 60W, the substrate heating temperature is 200C, and the sputter time is 120min, The interfacial adhesion is the strongest. The analysis of the corrosion process of the sample shows that the magnetron sputter aluminum film can protect the magnesium alloy matrix to a certain extent. For the simulated sweat corrosion of aluminum film, the corrosion occurs first at the grain boundary position on the surface of the film, and develops along the grain boundary to the inner layer of the film. Once the local corrosion penetration of the film layer, the corrosion medium will enter the interface between the substrate and the aluminum film. Thus, the corrosion of the original battery is accelerated and the film is peeled off from the substrate. Therefore, the thickness of the film is as large as possible, and the film is dominated by isometric crystal region and transition zone, and the interface adhesion is strong, which is an important condition for the film to have good corrosion performance.
【學(xué)位授予單位】：內(nèi)蒙古工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：TG174.44
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