CN113249625A - 一种高比强度镁锂基复合材料及其制备方法 - Google Patents
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Abstract
本发明提供一种高比强度镁锂基复合材料及其制备方法,该材料以超轻镁锂合金LA141作为基体,多壁碳纳米管为增强体,由以下方法制备而成:(1)利用电泳沉积技术制备MWCNTs膜层;(2)累积叠轧制备LA141/MWCNTs板材;(3)搅拌摩擦加工制备LA141/MWCNTs复合材料。本发明的镁锂基复合材料及其制备方法,通过采用电泳沉及技术、累积叠轧技术和搅拌摩擦加工相结合,从而实现了镁锂基复合材料的制备。该方法操作简单,成本较低,制备出了具有超细晶、增强体分布均匀和比强度较高的复合材料。
Description
技术领域
本发明涉及一种镁锂基复合材料及其制备方法,具体涉及一种高比强度镁锂基复合材料及其制备方法。
背景技术
研究发现通过在Mg中添加Li元素,可以使密度降低至1.35-1.65g/cm3,比普通镁合金轻1/4-1/3,由于其低密度的特点,镁锂合金被人们称为超轻合金。此外通过Li元素的添加使Mg的晶格结构从密排六方(hcp)变为体心立方(bcc),由于体心立方结构的滑移系较密排立方结构多,因此提高金属镁的塑性变形能力。由镁理合金的二元相图可知,当Li含量小于5.70%时,合金中仅存α-Mg相;当Li含量为5.70~10.3%时,合金中存在α-Mg相和β-Li相,为双相镁锂合金;当Li元素含量大于10.3%时,合金中仅存β-Li相。镁锂合金除了低密度的特点,同时还具备较好比刚度、比强度以及良好阻尼性能和电磁屏蔽性能,在航天航空、国防军工领域、汽车领域以及3C行业有着广泛的用途。虽然镁锂合金具有低密度等诸多优点,但是相比于其他合金强度较低,限制了其运用的范围,因此急需提高其强度扩大其使用的范围。
碳纳米管具有优异的力学性能以及良好的热学性能和电学性能,对于复合材料而言是一种理想的增强体。碳纳米管增强金属基复合材料具有较高的比强度和比刚度,而且具有潜在的优良导电和导热性能,在航空航天、汽车制造、3C等领域有着广泛的应用前景。由于碳纳米管之间范德华力作用强,导致其在金属基体材料中发生团聚,不能很好地体现出其优异的增强作用,因此在制备碳纳米管增强金属基复合材料时,如何分散碳纳米管成为大家关注的关键技术问题。
搅拌摩擦加工是一种以搅拌摩擦焊为基础发展的一种剧烈塑性变形加工技术,在复合材料制备、材料改性等方面有着广泛的用途。由于该技术具有较大的塑性变形,因此在制备复合材料过程中不仅可以显著细化基体材料的微观组织,与传统的塑性变形加工相比,搅拌摩擦加工技术在过程中使材料发生剧烈塑性变形,在搅拌头的作用下材料发生塑性流动,显微组织发生混合和破碎,使增强体颗粒在基体中的分布更加均匀。搅拌摩擦加工技术是一种高效、绿色的固相加工技术,与其他制备方法相比,具有操作方便、成本低、不良界面反应少等优点。
发明内容
镁锂合金LA141塑性变形能力好,适合累积叠轧和搅拌摩擦加工;高锂含量合金的晶粒粗大,有必要采用剧烈塑性变形进行晶粒细化;MWCNTs表面活性大,容易团聚,搅拌摩擦加工有利于使其均匀分布。本发明的目的在于提供一种高比强度镁锂基复合材料及其制备方法。该方法制备的复合材料不仅增强体(MWCNTs)在基体材料分布均匀,而且使基体材料(LA141)晶粒得到明显的细化,从而使该复合材料具备较高的比强度。
本发明的目的是这样实现的:
本发明将电泳沉积技术、累积叠轧技术和搅拌摩擦加工的优点结合起来,开发出新的工艺流程。首先利用电泳沉积技术在基体板材上制备出宏观均匀分散的碳纳米管膜层,然后利用累积叠轧技术对具有碳纳米管膜层的基体板材(LA141)进行预成型,制备出具体较高体积分数碳纳米管的LA141/MWCNTs预制板材,最后利用搅拌摩擦加工所用搅拌头的旋转和给进所产生剧烈的塑性变形,让基体材料在高速运动的搅拌头作用下发生塑性流动,与增强体材料发生混合,从而使增强体在基体中均匀分布,此外,由于搅拌摩擦的剧烈塑性变形作用,使得基体材料的晶粒发生明显的细化。
本发明通过以下技术方案实现:
一种高比强度镁锂基复合材料,其特征在于:该方法以超轻镁锂合金LA141作为基体,多壁碳纳米管为增强体。一种高比强度镁锂基复合材料的制备方法,其特征在于,以下制备步骤:
(1)利用电泳沉积技术制备MWCNTs膜层;
(2)累积叠轧制备LA141/MWCNTs板材;
(3)搅拌摩擦加工制备LA141/MWCNTs复合材料。
其具体制备步骤如下:
(1)利用电泳沉积技术制备MWCNTs膜层:
将镁锂合金铸锭切成厚度为20mm块状板材,然后在250℃下保温30min进行预轧制,每道次下压量为10%,并且每次间隔保温5min,直至轧制到2mm。然后将轧制得到的板材切成片状板材用于制备膜层;采用1gMWCNTs、0.4gAl(NO3)3、0.1g聚乙烯吡咯烷酮(PVP)溶于400ml体积比1:1的无水乙醇和丙酮的混合液中,然后超声分散8h,获得悬浮性较好的电泳液。然后以LA141镁锂合金作为阴极,相同尺寸的不锈钢片作为阳极,在30V的电压和0.5A的电流下进行电泳沉积5-10min,然后将沉积完成的试样自然干燥1-2h,获得所需MWCNTs膜层。
(2)累积叠轧制备LA141/MWCNTs板材:
将电泳沉积后具有MWCNTs膜层的板材块进行叠层堆垛,在250℃下保温10min,以60%的下压量进行累积叠轧结合,获得由初始厚度14mm下压制成5mm的LA141/MWCNTs板材。
(3)搅拌摩擦加工制备LA141/MWCNTs复合材料:
将LA141/MWCNTs板材进行搅拌摩擦加工,其工艺参数为:搅拌头旋转速度为900~1100r/min、给进速度为30~50mm/min,倾斜角度为2.5°,下压量为0.1mm;在上述工艺参数下制备出LA141/MWCNTs复合材料。
所述碳纳米管为多壁碳纳米管,纯度为>95wt%,内径为3-5nm,外径为8-15nm,长度为3-12μm。
所述LA141合金成分及其百分含量为:Li:13%-14%,Al:0.9%-1%,其余为Mg。
与现有技术相比,本发明的有益效果是:
本发明的镁锂基复合材料及其制备方法,通过采用电泳沉及技术、累积叠轧技术和搅拌摩擦加工相结合,从而实现了镁锂基复合材料的制备。该方法操作简单,成本较低,制备出了具有超细晶、增强体分布均匀和比强度较高的复合材料。
附图说明
图1是碳纳米膜层的SEM图。
图2是搅拌摩擦加工示意图。
图3是该复合材料的TEM图。
图4是基体合金(铸态、轧制态)和该复合材料的应力-应变曲线。
具体实施方式
下面结合附图与具体实施方式对本发明作进一步详细描述。
本发明涉及一种镁锂基复合材料及其制备方法,具体涉及一种高比强度镁锂基复合材料及其制备方法。具体步骤如下:
(1)将基体LA141铸锭在200℃下进行12h的均化处理。
(2)将均化好的基体LA141铸锭切成尺寸为110mm×40mm×20mm块状板材,砂纸打磨至表面光滑,然后在250℃下保温30min进行预轧制,每道次下压量为10%并且每次间隔保温5min,直至轧制到2mm。然后将轧制得到的板材切成尺寸为150mm×130mm×2mm片状板材,利用砂纸打磨除去表面的氧化层利用无水乙醇进行清洗,用于膜层制备备用;采用1gMWCNTs、0.4gAl(NO3)3、0.1g聚乙烯吡咯烷酮(PVP)溶于400ml体积比1:1的无水乙醇和丙酮的混合液中,先用玻璃棒不断搅拌,让碳管溶于混合液体中,然后利用超声分散,共8h,获得悬浮性较好的电泳液。然后以LA141镁锂合金作为阴极,相同尺寸的不锈钢片作为阳极,在30V的电压和0.5A的电流下进行电泳沉积5min,然后将沉积完成的试样自然干燥1h,获得所需MWCNTs膜层。
(3)取7块具有MWCNTs膜层的板材,将没有膜层的一侧进行打磨,使其露新鲜的金属,然后用打磨的一侧与沉积有碳管膜层的一侧进行叠层堆垛,在250℃下保温10min,以轧辊转速为500r/min,以60%的下压量进行轧制结合,获得由初始厚度14mm下压制成5mm的LA141/MWCNTs板材。
将LA141/MWCNTs板材切割成尺寸为150mm×140mm×5mm的板材,利用砂纸打磨除去板材表面的氧化层,然后利用搅拌焊机沿着垂直于轧制方向对板材进行搅拌摩擦加工,其工艺参数为:搅拌头旋转速度为900~1100r/min、给进速度为30~50mm/min,倾斜角度为2.5°,下压量为0.1mm;在上述工艺参数下加工制备出LA141/MWCNTs复合材料。
(4)对制备的镁锂基复合材料力学性能进行检测、分析、表征。
结果表明,经过搅拌摩擦加工后,基体合金LA141晶粒得到明显的细化,由于在制备过程中采用了电泳沉积技术,制备出了均匀的膜层,经过搅拌摩擦加工后使增强体在基体中分布均匀。本发明的镁锂基复合材料最高抗拉强度为260MPa,分别比均火态和轧制态的试样的抗拉强度高出110MPa和100MPa。此外本发明的复合材料其具有较高的比强度为192.59kNm/kg。
本发明以LA141镁锂合金作为基体材料,碳纳米管作为增强,通过采用电泳沉积技术、累积叠轧技术和搅拌摩擦加工相结合,制备了镁锂基复合材料。该方法操作简单,成本较低,制备出了具有超细晶、增强体分布均匀的复合材料,从而大幅度的提高了LA141镁锂合金的比强度。
Claims (10)
1.一种高比强度镁锂基复合材料,其特征在于:该材料以超轻镁锂合金LA141作为基体,多壁碳纳米管为增强体,由以下方法制备而成:
(1)利用电泳沉积技术制备MWCNTs膜层;
(2)累积叠轧制备LA141/MWCNTs板材;
(3)搅拌摩擦加工制备LA141/MWCNTs复合材料。
2.根据权利要求1所述的高比强度镁锂基复合材料,其特征在于:所述步骤(1)具体为:
将镁锂合金铸锭切成厚度为20mm块状板材,然后在250℃下保温30min进行预轧制,每道次下压量为10%,并且每次间隔保温5min,直至轧制到2mm;然后将轧制得到的板材切成片状板材用于制备膜层;采用1gMWCNTs、0.4gAl(NO3)3、0.1g聚乙烯吡咯烷酮(PVP)溶于400ml体积比1:1的无水乙醇和丙酮的混合液中,然后超声分散8h,获得悬浮性较好的电泳液;然后以LA141镁锂合金作为阴极,相同尺寸的不锈钢片作为阳极,在30V的电压和0.5A的电流下进行电泳沉积5-10min,然后将沉积完成的试样自然干燥1-2h,获得所需MWCNTs膜层。
3.根据权利要求1所述的高比强度镁锂基复合材料,其特征在于:所述步骤(2)具体为:
将电泳沉积后具有MWCNTs膜层的板材块进行叠层堆垛,在250℃下保温10min,以60%的下压量进行累积叠轧结合,获得由初始厚度14mm下压制成5mm的LA141/MWCNTs板材。
4.根据权利要求1所述的高比强度镁锂基复合材料,其特征在于:所述步骤(3)具体为:
将LA141/MWCNTs板材进行搅拌摩擦加工,其工艺参数为:搅拌头旋转速度为900~1100r/min、给进速度为30~50mm/min,倾斜角度为2.5°,下压量为0.1mm;在上述工艺参数下制备出LA141/MWCNTs复合材料。
5.根据权利要求1所述的高比强度镁锂基复合材料,其特征在于:所述碳纳米管为多壁碳纳米管,纯度为>95wt%,内径为3-5nm,外径为8-15nm,长度为3-12μm,所述LA141合金成分及其百分含量为:Li:13%-14%,Al:0.9%-1%,其余为Mg。
6.一种高比强度镁锂基复合材料的制备方法,其特征在于,包括以下步骤:
(1)利用电泳沉积技术制备MWCNTs膜层;
(2)累积叠轧制备LA141/MWCNTs板材;
(3)搅拌摩擦加工制备LA141/MWCNTs复合材料。
7.根据权利要求1所述的高比强度镁锂基复合材料的制备方法,其特征在于:所述步骤(1)具体为:将镁锂合金铸锭切成厚度为20mm块状板材,然后在250℃下保温30min进行预轧制,每道次下压量为10%,并且每次间隔保温5min,直至轧制到2mm;然后将轧制得到的板材切成片状板材用于制备膜层;采用1gMWCNTs、0.4gAl(NO3)3、0.1g聚乙烯吡咯烷酮(PVP)溶于400ml体积比1:1的无水乙醇和丙酮的混合液中,然后超声分散8h,获得悬浮性较好的电泳液;然后以LA141镁锂合金作为阴极,相同尺寸的不锈钢片作为阳极,在30V的电压和0.5A的电流下进行电泳沉积5-10min,然后将沉积完成的试样自然干燥1-2h,获得所需MWCNTs膜层。
8.根据权利要求1所述的高比强度镁锂基复合材料的制备方法,其特征在于:所述步骤(2)具体为:将电泳沉积后具有MWCNTs膜层的板材块进行叠层堆垛,在250℃下保温10min,以60%的下压量进行累积叠轧结合,获得由初始厚度14mm下压制成5mm的LA141/MWCNTs板材。
9.根据权利要求1所述的高比强度镁锂基复合材料的制备方法,其特征在于:所述步骤(3)具体为:将LA141/MWCNTs板材进行搅拌摩擦加工,其工艺参数为:搅拌头旋转速度为900~1100r/min、给进速度为30~50mm/min,倾斜角度为2.5°,下压量为0.1mm;在上述工艺参数下制备出LA141/MWCNTs复合材料。
10.根据权利要求1所述的高比强度镁锂基复合材料的制备方法,其特征在于:所述碳纳米管为多壁碳纳米管,纯度为>95wt%,内径为3-5nm,外径为8-15nm,长度为3-12μm,所述LA141合金成分及其百分含量为:Li:13%-14%,Al:0.9%-1%,其余为Mg。
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