CN116219295B - 一种激光增材制造用双相不锈钢粉末和原位激光增材制造双相不锈钢的方法 - Google Patents
一种激光增材制造用双相不锈钢粉末和原位激光增材制造双相不锈钢的方法 Download PDFInfo
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- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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Abstract
本发明公开了一种激光增材制造用双相不锈钢粉末和原位激光增材制造双相不锈钢的方法,属于双相不锈钢技术领域。本发明中激光粉末增材制造双相不锈钢所用粉末合金元素为Cr,Ni,Mo,Si,Mn,C,N,O,余量为Fe和不可避免的杂质。采用原位激光送粉增材设备,进行原位激光增材制造双相不锈钢。本发明实现了激光增材制造很快的冷却速率下依然可以保证铁素体向奥氏体转变,从而保证双相不锈钢中铁素体和奥氏体的相比例,最终得到铁素体含量在40~50%的双相不锈钢,实现双相不锈钢的原位增材制造,无需后续热处理。
Description
技术领域
本发明属于双相不锈钢技术领域,具体涉及一种激光增材制造用双相不锈钢粉末和原位激光增材制造双相不锈钢的方法。
背景技术
双相不锈钢(DSS)是指微观组织由铁素体与奥氏体两相构成的不锈钢,其中一相所占比例约为45%~55%,其中含量少的一相含量至少占30%。由于具有铁素体和奥氏体两相的微观组织,因此双相不锈钢结合了铁素体和奥氏体不锈钢的优点,是一种兼具高强度和高耐腐蚀性的一类不锈钢,被广泛应用于石油、化工、造纸、海洋、能源、建筑等行业。超级双相不锈钢是指抗点蚀当量(PREN=Cr%+3.3Mo%+16N%)值大于40的一类高镍、高铬、高钼的高合金超级双相不锈钢。
增材制造技术又被称为3D打印,其通过将复杂三维结构分割为薄层,通过逐层二维成形叠加制造的方式实现零件的制造。由于其特殊的成形机制,增材制造技术对于构件的几何适应性极强,理论上可以制造任何复杂形状的三维构件。金属材料增材制造的热源主要有电弧、激光和电子束等。目前双相不锈钢的增材制造的实现方法主要集中在电弧熔丝增材制造,很少有采用激光粉末增材制造的方法原位增材制造双相不锈钢。其中主要的原因是由于激光能量密度高,快速加热-熔化-凝固双相不锈钢,其凝固微观组织以铁素体为主,没有足够的时间完成铁素体向奥氏体的转变,因此很难实现奥氏体/铁素体比例接近1:1。相比较于激光粉末增材制造的方法,电弧熔丝增材制造冷却速率显著降低,冷却至室温的凝固组织可以得到约40%~60%奥氏体,从而实现双相不锈钢的原位增材制造。
综上可知,激光粉末增材制造双相不锈钢的难点的主要是激光能量密度高,熔池金属凝固速度太快导致的。这是由于激光热源性质决定的,难以改变。然而,相较于电弧增材制造,激光粉末增材制造成形质量好、精度高、后续加工少,且随着激光产业迅猛发展,激光增材制造的成本也越来越低,因此激光粉末增材制造双相不锈钢是未来发展的一个趋势。实现双相不锈钢的原位激光增材制造具有很高的实际应用价值。
发明内容
本发明的目的在于克服现有的不足,设计一种双相不锈钢的粉末成分,实现双相不锈钢的激光原位增材制造,其奥氏体/铁素体比例接近1:1,并提供了一种原位激光增材制造的双相不锈钢的方法,实现采用激光热源粉末增材制造的奥氏体/铁素体双相组织的原位合成,无需后续的热处理。
根据不锈钢焊接冶金凝固的理论,影响增材制造双相不锈钢凝固微观组织转变的因素不仅包含工艺因素(凝固速度),还有冶金因素(材料成分)。微调双相不锈钢的成分,使其与激光粉末增材制造方法快速凝固的特点相匹配,有望实现原位的双相不锈钢增材制造。对于典型的2507型双相不锈钢(Cr:25%,Ni:7%,Mo:3~5%,N:0.22~0.34%),其凝固顺序为,首先从液相中析出高温铁素体(δ相),随后发生奥氏体(γ相)转变(δ→γ),冷却至室温,最后得到奥氏体和铁素体双相组织,其中铁素体的含量在50%左右。但是由于激光增材制造快速凝固的工艺特点,其凝固速度远高于常规的铸造过程,导致铁素体向奥氏体转变不完全(δ→γ),因此凝固组织以铁素体居多。铁素体含量高会导致双相不锈钢的韧性降低、腐蚀性差等问题。目前现有的报道中,激光增材制造双相不锈钢为了保证其性能,往往需要后续热处理调节奥氏体和铁素体的相比例。因此本发明的基本原理为通过提高Nieq(其中Nieq=Ni%+35C%+20N%),扩大奥氏体相区,使之于激光增材快速凝固的特点相匹配,在激光增材制造很快的冷却速率下依然可以保证铁素体向奥氏体转变(δ→γ),从而保证双相不锈钢中铁素体和奥氏体的相比例,实现双相不锈钢的原位增材制造。
为了实现上述目的,本发明中激光粉末增材制造双相不锈钢所用粉末合金元素含量为Cr:24.5~26.0%,Ni:8~8.5%,Mo:3.5~5%,Si:0.3~0.5%,Mn:0.7~1%,C<0.025%,N:0.25~0.34%,O<0.03%,余量为Fe和不可避免的杂质。其中Creq/Nieq=1.95~2.1(Creq=Cr%+Mo%+0.7Nb%,Nieq=Ni%+35C%+20N%)。所述粉末为球形粉末,粒径为15~53或者45~105μm。上述粉末的微观形貌如图1所示。所用双相不锈钢的粉末相比于商用的2507型不锈钢成分中Ni含量提高1%~1.5%。
本发明中采用的激光粉末增材制造设备为常规的激光送粉增材设备,包括激光器、水冷机、光纤、保护气(氩气或氮气)、激光熔覆头、六轴机器人和送粉器组成。
一种原位激光增材制造双相不锈钢的方法,包括以下步骤:
第一步是材料准备。基板采用不锈钢材质,将基板表面打磨直至无氧化物,用丙酮将基板表面的油污清洗干净,采用喷砂机进行表面喷砂处理。将烘干后的粉末装入送粉器。
第二步是进行激光增材。首先进行参数设置。激光功率1200~2500W,送粉速率8~20g/min,光斑直径3~4mm,激光扫描速率5~10mm/s,两道搭接率为40~50%,层间抬升量1~2.5mm,保护气为氩气或者氮气亦或者二者混合,保护气流量25~35L/min,采用氮气做保护气可以减少粉末中氮含量的损失。然后激光连续沉积获得预定尺寸的双相不锈钢块体,冷却至室温。
第三步是检测样品中铁素体的含量。试样中铁素体相的含量采用GB/T1954-2008《铬镍奥氏体不锈钢焊缝铁素体含量的测量方法》中磁性法测量。在上述增材制造双相不锈钢块体中切取横截面试样,将横截面打磨至光亮。在增材试样的横截面上选择10个位置测得其铁素体含量,取其平均值为检测结果。采用上述方法激光增材制造获得的双相不锈钢样品中铁素体含量在40~50%之间。
第四步是对双相不锈钢中的奥氏体和铁素体进行微观表征。在上述增材制造双相不锈钢块体中切取5×10×20mm的试样若干,选择横截面粗磨、精磨、抛光、草酸电解腐蚀制作金相试样,用于观察样品中奥氏体和铁素体的比例和形貌,其光学显微镜的微观形貌如图2所示。在金相照片可以看到铁素体、晶粒内奥氏体、晶界奥氏体。同时部分样品的横截面粗磨、精磨、高氯酸电解抛光制作电子背散射衍射(EBSD)试样,用于分析分析局部的奥氏体和铁素体的双相比例。EBSD相比例图(图3)可以看出局部铁素体的比例为52.5%,也验证了磁性法测得铁素体含量的准确性。
附图说明
图1为双相不锈钢粉末形貌照片;
图2为激光增材制造双相不锈钢的微观组织,(a)是激光增材制造双相不锈钢的微观组织(200X),(b)是激光增材制造双相不锈钢的微观组织(500X);
图3为激光增材制造双相不锈钢的EBSD相比例图;
图4为工艺参数1下的激光增材制造双相不锈钢微观组织图,(a)是工艺参数1激光增材制造双相不锈钢微观组织光镜照片(500X),(b)是工艺参数1激光增材制造双相不锈钢EBSD相比例图;
图5为工艺参数2激光增材制造双相不锈钢微观组织图,(a)是工艺参数2激光增材制造双相不锈钢微观组织光镜照片(500X),(b)是工艺参数1激光增材制造双相不锈钢EBSD相比例图;
图6为工艺参数3激光增材制造双相不锈钢的微观组织图,(a)是工艺参数3激光增材制造双相不锈钢微观组织光镜照片(500X),(b)是工艺参数3激光增材制造双相不锈钢EBSD相比例图。
具体实施方式
特别说明,本发明实施例中所用的方法除参数外均相同,具体为:
一种原位激光增材制造双相不锈钢的方法,包括以下步骤:
第一步是材料准备。基板采用不锈钢材质,将基板表面打磨直至无氧化物,用丙酮将基板表面的油污清洗干净,采用喷砂机进行表面喷砂处理。将烘干后的粉末装入送粉器。
第二步是进行激光增材。首先进行参数设置。激光功率1200~2500W,送粉速率8~20g/min,光斑直径2~4mm,激光扫描速率5~10mm/s,两道搭接率为40~50%,层间抬升量1~2.5mm,保护气为氩气或者氮气亦或者二者混合,保护气流量25~35L/min,采用氮气做保护气可以减少粉末中氮含量的损失。然后激光连续沉积获得预定尺寸的双相不锈钢块体,冷却至室温。
第三步是检测样品中铁素体的含量。试样中铁素体相的含量采用GB/T1954-2008《铬镍奥氏体不锈钢焊缝铁素体含量的测量方法》中磁性法测量。在上述增材制造双相不锈钢块体中切取横截面试样,将横截面打磨至光亮。在增材试样的横截面上选择10个位置测得其铁素体含量,取其平均值为检测结果。采用上述方法激光增材制造获得的双相不锈钢样品中铁素体含量在40~50%之间。
第四步是对双相不锈钢中的奥氏体和铁素体进行微观表征。在上述增材制造双相不锈钢块体中切取5×10×20mm的试样若干,选择横截面粗磨、精磨、抛光、草酸电解腐蚀制作金相试样,用于观察样品中奥氏体和铁素体的比例和形貌,其光学显微镜的微观形貌如图2所示。在金相照片可以看到铁素体、晶粒内奥氏体、晶界奥氏体。同时部分样品的横截面粗磨、精磨、高氯酸电解抛光制作电子背散射衍射(EBSD)试样,用于分析分析局部的奥氏体和铁素体的双相比例。EBSD相比例图(图3)可以看出局部铁素体的比例为52.5%,也验证了磁性法测得铁素体含量的准确性。
实施例1
激光功率1500W,送粉速率12g/min,光斑直径3mm,激光扫描速率10mm/s,两道搭接率为50%,层间抬升量1.4mm,保护气为氩气,保护气流量25L/min,冷却至室温。选择样品的横截面,采用磁性法测得平均铁素体的含量为47%。磁性法测得结果见表2。切取样品,粗磨、精磨、抛光腐蚀后其微观组织光学显微镜照片如图4中(a)所示,切取样品,粗磨、精磨、电解抛光后EBSD相比例图表征如图4中(b)所示,样品中铁素体的含量为46.5%,与磁性法测得铁素体含量相近。
实施例2
激光功率1500W,送粉速率12g/min,光斑直径3mm,激光扫描速率10mm/s,两道搭接率为50%,层间抬升量1.4mm,保护气为氮气和氩气各50%,保护气流量25L/min,冷却至室温。选择样品的横截面,采用磁性法测得平均铁素体的含量为42%。磁性法测得结果见表2。切取样品,粗磨、精磨、抛光腐蚀后其微观组织光学显微镜照片如图5中(a)所示,切取样品,粗磨、精磨、电解抛光后EBSD相比例图表征如图5中(b)所示,样品中铁素体的含量为40.5%,与磁性法测得铁素体含量相近。
实施例3
激光功率1500W,送粉速率9g/min,光斑直径3mm,激光扫描速率5mm/s,两道搭接率为50%,层间抬升量1.7mm,保护气为氩气,保护气流量25L/min,冷却至室温。选择样品的横截面,采用磁性法测得平均铁素体的含量为49%。磁性法测得结果见表2。切取样品,粗磨、精磨、抛光腐蚀后其微观组织光学显微镜照片如图6中(a)所示,切取样品,粗磨、精磨、电解抛光后EBSD相比例图表征如图6中(b)所示,样品中铁素体的含量为49.4%,与磁性法测得铁素体含量相近。
尽管上述实施例对本发明做出了详尽的描述,但它仅仅是本发明一部分实施例,而不是全部实施例,人们还可以根据本实施例在不经创造性前提下获得其他实施例,这些实施例都属于本发明保护范围。
Claims (2)
1.一种原位激光增材制造双相不锈钢的方法,其特征在于,包括以下步骤:
(1)以不锈钢材质为基板,将基板表面打磨干净并清洗后,进行喷砂处理;
(2)将烘干后的粉末装入送粉器,进行激光增材,并设定参数:激光功率1200~2500W,送粉速率8~20g/min,光斑直径3~4mm,激光扫描速率5~10mm/s,两道搭接率为40~50%,层间抬升量1~2.5mm,然后激光连续沉积获得预定尺寸的双相不锈钢块体,冷却至室温,得到铁素体含量在40~50%的双相不锈钢;所述双相不锈钢所用的粉末合金元素含量为Cr:24.5~26.0%,Ni:8~8.5%,Mo:3.5~5%,Si:0.3~0.5%,Mn:0.7~1%,C<0.025%,N:0.25~0.34%,O<0.03%,余量为Fe和不可避免的杂质;
进行激光增材时,设定保护气为氩气和/或氮气,保护气流量25~35L/min;
令Creq=Cr%+Mo%+0.7Nb%,Nieq=Ni%+35C%+20N%,Creq/Nieq=1.95~2.1。
2.根据权利要求1所述方法,其特征在于,在步骤(1)中,将基板表面打磨直至无氧化物,用丙酮将基板表面的油污清洗干净。
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