CN117444234A - 一种实现fcc结构多主元合金力学性能提升的激光增材制造方法 - Google Patents
一种实现fcc结构多主元合金力学性能提升的激光增材制造方法 Download PDFInfo
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Abstract
一种实现FCC结构多主元合金力学性能提升的激光增材制造方法属于金属材料和增材制造技术领域。激光增材制造用粉末为复合粉末材料,其包括一种多主元预合金粉末和硼化物粉末,其中,所述的预合金粉末成分包含Fe、Ni、Co、Cr、Mn中的至少三种元素且等摩尔比,质量分数99.5–99.95wt.%,硼化物粉末为硼铁或硼化铬中的一种,质量分数为0.05–0.5wt.%;激光增材制造方法为激光粉末床熔融工艺,制备得到的FCC结构多主元合金,屈服强度≥800MPa,抗拉强度≥1050MPa,断裂延伸率≥20%,合金由激光增材制造一步成形,无需任何后处理工艺,有助于实现具有复杂形状的结构件,具有广阔的应用前景。
Description
技术领域
本发明涉及一种提升FCC结构多主元合金力学性能的激光增材制造方法,属于金属材料和增材制造技术领域。
背景技术
传统合金以单一元素为主,通常质量百分比大于50%,同时添加少量合金元素形成。而多主元合金也称为高熵合金,突破了这种传统的合金设计理念,是一种采用多种元素作为主元的新型合金,每种元素含量5–35wt.%。相比于传统合金,高熵合金由于具有高熵效应、迟滞扩散效应、晶格畸变效应以及鸡尾酒效应等,且通常表现出简单的单相固溶体结构,如FCC、BCC或HCP,这会赋予合金多种优异的性能,包括力学性能、耐磨、耐腐蚀和热稳定性等。
尽管多主元合金容易获得优异的综合性能,但已报道的具有FCC单相结构的合金通常强度较低,极大地限制了多主元的工程应用。例如,传统铸造方法制备的FCC结构CoCrFeNiMn高熵合金,其抗拉强度仅为400MPa。有报道指出,可通过在FCC基体中引入纳米尺度的共格析出相,以达到提高强度的目的。例如,在CoCrFeNi单相FCC高熵合金中添加少量的Ti和Al,并结合形变热处理等复杂后处理工艺,促使FCC基体中析出共格的纳米尺度L12析出相,从而使合金的强度大幅提升,屈服强度达到1005MPa,但合金中仍存在大量的脆性Laves相,一方面限制了合金强度的进一步提高,另一方面也使合金塑性显著下降,有些甚至不足10%,此外复杂的形变热处理工艺等也限制了其更为广泛的推广应用。
目前多主元合金制备以传统的铸造工艺为主,包括熔化、轧制、热处理等一系列复杂的步骤,且无法设计加工复杂的零部件,在一定程度上制约了高熵合金的发展和应用。激光粉末床熔融技术作为一种高效率的激光增材制造技术,具有很大的应用潜力,且能够成形具有复杂几何形状的零部件。但目前采用激光增材制造制备的FCC多主元合金仍存在强度不足或强塑性不匹配等问题,制约了其作为复杂结构件材料的工程应用。
发明内容
针对现有技术的问题,本发明的目的是提供一种可以提升FCC结构多主元合金力学性能激光增材制造方法及所用复合材料。通过改变激光粉末床熔融多主元合金原材料,并利用激光能量密度大、光斑小和冷速快的特点,配合工艺参数优化,调控多主元合金熔池熔化状态和凝固条件,实现降低粗大枝晶数量、细化晶粒尺寸和亚结构组织的目的,直接成形获得成分均匀、致密度高、晶粒尺寸细小、组织均匀以及力学性能优异的多主元合金。
本发明的目的是通过如下的技术方案实现的:
一种实现FCC结构多主元合金力学性能提升的激光增材制造方法,其特征在于:所述激光增材制造用粉末为复合粉末材料,其包括一种多主元预合金粉末和硼化物粉末,其中,所述的预合金粉末成分包含Fe、Ni、Co、Cr、Mn中的至少三种元素且等摩尔比,质量分数99.5–99.95wt.%,硼化物粉末为硼铁或硼化铬中的一种,质量分数为0.05–0.5wt.%;包括如下制备步骤:
步骤1:对等摩尔比或近等摩尔比的多主元预合金粉末和硼化物粉末机械混合均匀,并在真空干燥箱内,95℃条件下干燥3小时;
步骤2:利用激光粉末床熔融增材制造技术对步骤1所得粉末进行激光增材制造成形,工艺参数为:激光功率:85–120W,扫描速度:800–1000mm/s,扫描间距:0.04–0.05mm,层厚:0.03mm,层间旋转67°,基板预热80–100℃,保护气体为氩气。
优选地,所述激光增材制造用复合粉末材料中的预合金粉末为气雾化制备的球形粉末,纯度≥99.5wt.%,粒径为25–45μm。
优选地,所述激光增材制造用复合粉末材料中的硼化物粉末中硼含量在18–25wt.%,硼化物粉末粒径为15–38μm。
优选地,激光增材制造一步成形,无需任何后处理工艺。
本发明所述方法制备得到的多主元合金,其特征在于:合金致密度大于98.5%。
优选地,所述多主元合金为单相FCC结构。
优选地,所述多主元合金力学性能优异。
本发明的有益效果
本发明提出一种提升FCC结构多主元合金力学性能的激光增材制造方法,合金性能的提升主要得益于所述材料与激光增材制造方法的相辅相成。所述复合材料包括一种多主元预合金粉末和硼化物粉末,将二者混合均匀,作为激光粉末床熔融的原材料。为保证制备的合金仍保持优异的塑性变形能力,故而要求合金的相结构主要为单相FCC结构。预合金粉末成分包含Fe、Ni、Co、Cr、Mn中的至少三种元素且等摩尔比或近等摩尔比,目的是保证足够的系统熵,促进形成单相固溶体。微量外添加硼化物的复合设计是从两方面考虑,一是利用高能量激光热源,使其在熔池内熔化,一方面引入的异质粒子可以增加形核质点,抑制合金晶粒长大,同时增加亚结构的形成,另一方面可以补充部分金属元素进熔池,保证系统熵。但异质粒子的含量需要结合预合金粉末的比例以及激光能量进行设计调配。含量过低则效果不明显,过高则会有大量硼化物或者脆性金属间化合物在晶界析出,影响合金整体力学性能表现。同时激光粉末床熔融工艺也至关重要,熔池能量过高则易形成粗大枝晶或柱状晶组织进而降低力学性能,熔池能量过低则会熔化程度不够或组织不均匀,且产生较多缺陷。因此,复合材料中两种粉末比例及其与激光粉末床熔融工艺的合理调配至关重要。
本发明与常规方法制备的FCC结构多主元合金相比:
1)本发明所述的方法,通过工艺参数优化制备得到的多主元合金相结构主要由FCC相组成,组织均匀致密,相较于铸态样品晶粒尺寸更为细小;
2)本发明制备得到的FCC结构多主元合金,相较于常规铸造后加大形变处理与退火结合的复杂后处理工艺,本发明的方法得到的合金不需要任何后处理,就可以获得优异的力学性能,合金屈服强度≥800MPa,抗拉强度≥1050MPa,断裂延伸率≥20%;
2)本发明提供的激光增材制造方法操作简单,可以制备复杂形状的构件,且构件表面质量好,表面无明显氧化,有益于直接工程应用,有更广阔的应用前景。
附图说明
图1为实施例5以及对比例1的X射线衍射(XRD)谱图。
图2为实施例5的平行于成形方向的截面金相图。
图3为对比例1的平行于成形方向的截面金相图。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步阐述,其中,所述方法如无特别说明均为常规方法,所述原材料如无特别说明均能从公开商业途径而得。
以下实施例中:
(1)复合材料中多主元预合金粉末包含Fe、Ni、Co、Cr、Mn中的至少三种元素且等摩尔比,并采用气雾化制粉技术制备得到且纯度≥99.5wt.%;硼化物粉末中硼含量为18–20wt.%。
(2)对等摩尔比的多主元预合金粉末和硼化物粉末的粒度进行筛分,机械混合均匀,并在干燥箱内干燥2–3小时。
(3)激光粉末床熔融设备为EOS公司的M100型,基板选用316L不锈钢。
对实施例中所制备的多主元合金进行的组织结构表征和力学性能测试:
(1)物相分析:采用的是布鲁克公司的X射线衍射仪(D8 ADVANCE),测试样品尺寸为10×10×2mm3;
(2)微观组织:采用奥林巴斯OLMPUS-PMG3型光学显微镜和Image-J图像分析软件;
(3)准静态拉伸力学性能测试:采用CMT4305型微机电子万能试验机进行室温准静态拉伸试验,测试试样依据金属材料室温拉伸试验方法(GB/T228.1-2010)国家标准中有关规定制成工字试样,样品厚1.0mm,宽3.14mm,平行段长度10mm,标距长度5mm,应变率为10- 3s-1。
实施例1
本实施例中复合材料包括多主元合金FeNiCr粉末和质量分数为0.5wt.%的硼铁粉末,多主元合金FeNiCr粉末粒径为25–38μm,硼铁粉末粒径为15–38μm;激光粉末床熔融工艺参数为:激光功率:85W,扫描速度:800mm/s,扫描间距:0.04mm,层厚:0.03mm,层间旋转67°,基板预热80℃。
实施例2
本实施例中复合材料包括多主元合金FeNiCr粉末和质量分数为0.5wt.%的硼铁粉末,多主元合金FeNiCr粉末粒径为38–45μm,硼铁粉末粒径为15–38μm;激光粉末床熔融工艺参数为:激光功率:100W,扫描速度:1000mm/s,扫描间距:0.05mm,层厚:0.03mm,层间旋转67°,基板预热90℃。
实施例3
本实施例中复合材料包括多主元合金FeNiCoCr粉末和质量分数为0.25wt.%的硼铁粉末,多主元合金FeNiCoCr粉末粒径为25–45μm,硼铁粉末粒径为15–38μm;激光粉末床熔融工艺参数为:激光功率:100W,扫描速度:1000mm/s,扫描间距:0.05mm,层厚:0.03mm,层间旋转67°,基板预热90℃。
实施例4
本实施例中复合材料包括多主元合金FeNiCoCrMn粉末和质量分数为0.15wt.%的硼铁粉末,多主元合金FeNiCoCrMn粉末粒径为25–45μm,硼铁粉末粒径为15–38μm;激光粉末床熔融工艺参数为:激光功率:100W,扫描速度:1000mm/s,扫描间距:0.05mm,层厚:0.03mm,层间旋转67°,基板预热90℃。
实施例5
本实施例中复合材料包括多主元合金FeNiCoCrMn粉末和质量分数为0.05wt.%的硼铁粉末,多主元合金FeNiCoCrMn粉末粒径为25–38μm,硼铁粉末粒径为15–38μm;激光粉末床熔融工艺参数为:激光功率:85W,扫描速度:1000mm/s,扫描间距:0.04mm,层厚:0.03mm,层间旋转67°,基板预热80℃。
实施例6
实施例中复合材料包括多主元合金FeNiCoCrMn粉末和质量分数为0.15wt.%的硼化铬粉末,多主元合金FeNiCoCrMn粉末粒径为25–38μm,硼化铬粉末粒径为15–25μm;激光粉末床熔融工艺参数为:激光功率:110W,扫描速度:800mm/s,扫描间距:0.04mm,层厚:0.03mm,层间旋转67°,基板预热90℃。
实施例7
本实施例中复合材料包括多主元合金FeCoCrMn粉末和质量分数为0.20wt.%的硼化铬粉末,多主元合金FeCoCrMn粉末粒径为25–45μm,硼化铬粉末粒径为15–25μm;激光粉末床熔融工艺参数为:激光功率:85W,扫描速度:900mm/s,扫描间距:0.05mm,层厚:0.03mm,层间旋转67°,基板预热80℃。
对比例1
本对比例中合金材料为多主元合金FeNiCoCrMn粉末,粒径为25–38μm,不包含硼化物粉末;激光粉末床熔融工艺参数为:激光功率:85W,扫描速度:1000mm/s,扫描间距:0.04mm,层厚:0.03mm,层间旋转67°,基板预热80℃。
对比例2
本对比例中复合材料包括多主元合金FeNiCoCrMn粉末和质量分数为0.85wt.%的硼铁粉末,多主元合金FeNiCoCrMn粉末粒径为25–38μm,硼铁粉末粒径为15–38μm;激光粉末床熔融工艺参数为:激光功率:120W,扫描速度:1100mm/s,扫描间距:0.06mm,层厚:0.02mm,层间旋转67°,基板预热80℃。
实施例5、对比例1的XRD测试结果如图1所示,从图中可得出所述合金材料的相结构;实施例5、对比例1的纵截面金相形貌分别如图2和图3所示,从图中可得出激光增材制造用复合材料和制备工艺合理调配益于消除熔池粗大直径或柱状晶形成,有利于获得更好的综合力学性能。实施例1-8与对比例1-2的多主元合金材料相结构结果、熔池宽深比和拉伸性能测试结果如表1所示。其中,熔池宽深比是根据制备得到样品的纵截面金相通过图像法测得,宽深比可以反应熔池熔化情况,工艺参数匹配得当则宽深比较大,预示熔池内合金熔化较为充分,过小或小于1则代表熔化不均匀充分,但也不宜过大,过大则可能引起熔池内温度过高,重熔效果明显造成晶粒二次生长,并影响成形质量,所以工艺参数匹配需要合理。
表1
综上所述,发明包括但不限于以上实施例,凡是在本发明的精神和原则之下进行的任何等同替换或局部改进,都将视为在本发明的保护范围之内。
Claims (7)
1.一种实现FCC结构多主元合金力学性能提升的激光增材制造方法,其特征在于:所述激光增材制造用粉末为复合粉末材料,其包括一种多主元预合金粉末和硼化物粉末,其中,所述的预合金粉末成分包含Fe、Ni、Co、Cr、Mn中的至少三种元素且等摩尔比,质量分数99.5–99.95wt.%,硼化物粉末为硼铁或硼化铬中的一种,质量分数为0.05–0.5wt.%;包括如下制备步骤:
步骤1:对等摩尔比或近等摩尔比的多主元预合金粉末和硼化物粉末机械混合均匀,并在真空干燥箱内,95℃条件下干燥3小时;
步骤2:利用激光粉末床熔融增材制造技术对步骤1所得粉末进行激光增材制造成形,工艺参数为:激光功率:85–120W,扫描速度:800–1000mm/s,扫描间距:0.04–0.05mm,层厚:0.03mm,层间旋转67°,基板预热80–100℃,保护气体为氩气。
2.根据权利要求1所述的一种实现FCC结构多主元合金力学性能提升的激光增材制造方法,其特征在于:所述激光增材制造用复合粉末材料中的预合金粉末为气雾化制备的球形粉末,纯度≥99.5wt.%,粒径为25–45μm。
3.根据权利要求1所述的一种实现FCC结构多主元合金力学性能提升的激光增材制造方法,其特征在于:所述激光增材制造用复合粉末材料中的硼化物粉末中硼含量在18–25wt.%,硼化物粉末粒径为15–38μm。
4.根据权利要求1-3任一项所述的一种实现FCC结构多主元合金力学性能提升的激光增材制造方法,其特征在于:激光增材制造一步成形,无需任何后处理工艺。
5.应用如权利要求1–4中任一所述方法制备的多主元合金,其特征在于:合金致密度大于98.5%。
6.根据权利要求5所述的多主元合金,其特征在于:所述多主元合金为单相FCC结构。
7.根据权利要求5所述的多主元合金,其特征在于:多主元合金屈服强度≥800MPa,抗拉强度≥1050MPa,断裂延伸率≥20%。
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