CN115198163B - 一种具有拉伸塑性的多纳米相强化ods合金的制备方法 - Google Patents
一种具有拉伸塑性的多纳米相强化ods合金的制备方法 Download PDFInfo
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Abstract
本发明属于高性能金属材料制备研究领域，特别提供了一种具有拉伸塑性的多纳米相强化ODS合金的制备方法。该方法包括如下步骤，S1)将气雾化法制备的预合金粉末与Y2O3粉末按照设定成分混合均匀，在惰性气氛中进行机械合金化反应。S2)将S1)得到的粉末通过SPS烧结技术或热等静压致密化。S3)将S2)得到的样品进行固溶热处理。S4)将S3)得到的样品进行热变形处理。S5)将S4)得到的样品进行时效热处理。本发明的有益效果是，本发明的氧化物弥散强化合金中引入了高体积分数的B2相和纳米氧化物粒子进行强化，表现出优异的高温强度和良好的室温塑形，为铁素体耐热钢的制备和开发提供了一种新的方法。
Description
技术领域
本发明属于高性能金属材料制备研究领域，特别提供了一种具有拉伸塑性的多纳米相强化ODS合金的制备方法。
背景技术
与奥氏体钢和镍基高温合金相比，铁素体钢具有良好的导热性、低的膨胀系数、耐高温腐蚀和较低的成本等优点而应用在许多高温结构材料上，包括汽车排气净化装置、航天飞机的热防护结构及超超临界机组的蒸汽管道、联箱、过热管和再热器等。CsCl结构的B2相和BCC结构的铁素体晶格参数相似(分别为0.28864nm和0.28665nm)，可在基体中共格析出。铁素体的主要滑移系为{101}<111>，而具有B2相的主要滑移系是{110}<001>，当基体与NiAl析出物之间的错配足够小时，NiAl析出物将被一对1/2<111>位错剪切而产生强烈的沉淀硬化，从而使合金在宽的温度区间保持较高的强度。纳米氧化物粒子具有优异的热力学稳定性，可以在高温长时间保持粒子尺寸不增加。高温下，氧化物与位错之间的相互作用形成位错环而提高位错滑移阻力，从而提高合金的高温强度。此外，纳米氧化物还可以钉扎晶界，提高合金的晶界强度。将B2相和纳米氧化物共同引入到铁素体合金中，发挥其沉淀强化和弥散强化作用，从而使它们分别在高温区(>650℃)和中温区(550℃-650℃)发挥主要作用以改善合金的高温力学性能。
B2相的强化效果与沉淀的形貌、尺寸、体积分数等密切相关。研究表明B2相强化铁素体合金的高温性能随着沉淀体积分数的增加而提高，高体积分数的沉淀是合金保持良好高温性能的重要保证。但高体积分数的沉淀导致合金低的室温塑形而发生解理断裂。Z.k.Teng等人开发出了B2相体积分数约为17％的FBB8合金，其室温延伸率小于1％，无法满足合金室温加工塑形的要求，极大的限制了合金的应用。
发明内容
针对上述问题，本发明提供一种具有拉伸塑性的多纳米相强化ODS合金的制备方法，以解决现有技术的上述以及其他潜在问题中任一问题。
为达到上述目的，本发明的技术方案是：一种具有拉伸塑性的多纳米相强化ODS合金的制备方法，该制备方法的步骤顺序如下：
S1)将气雾化法制备的预合金粉末与一定量的Y2O3粉末混合均匀，在高纯Ar气氛中高能球磨进行机械合金化反应；
S2)将S1)得到合金粉末通过SPS烧结或热等静压致密化；
S3)将S2)得到的样品进行固溶热处理；
S4)将S3)得到的样品进行热变形处理；热变形一方面促进B2相沉淀的形核，另一方面细化晶粒，在合金冷却过程中利用纳米氧化物粒子的钉扎晶界作用阻止晶粒的长大，使基体由细小的晶粒组成，从而改善合金室温塑形；
S5)将S4)得到的样品进行时效热处理；
进一步，所述铁素体|ODS合金中高体积分数的B2相沉淀与纳米氧化物粒子均匀分布在基体中，表现出优异的高温强度和良好的室温塑形。
进一步，所述S1)的具体步骤为：
S1.1)预合金粉末成分的质量百分数为：Cr 10-14％，Ni 8-12％，Co 8-12％，Al4-8％，Mo 0-2％，Zr 0-2％，Hf 0-2％，余量为Fe和不可避免的杂质；
S1.2)合金中Y2O3粉末的质量百分数为0.3-0.5％；
S1.3)球磨工艺为：按照设定的成分配比进行称量；将粉末混合均匀后在高纯氩气气氛中高能球磨，转速为340-450转/分，球磨时间为40-60h。
进一步，所述S2)致密化的具体工艺参数为：
S2.1)采用SPS烧结制备：机械合金化粉末放入石墨磨具中进行SPS烧结，烧结温度为1050-1200℃，压力为30-50MPa，保温时间为5-10min；
S2.2)采用热等静压制备：用低碳钢将机械合金化粉末包套后进行热等静压，热等静压温度为1000-1150℃，压力为100-200MPa，保温时间为1-3h。
进一步，所述S3)固溶热处理的具体工艺参数为：
固溶热处理温度为1000-1300℃，保温时间为0.5-2h，冷却介质为空气；
进一步，所述S4)热变形处理步骤的具体工艺参数为：
S4.1)所述热变形采用轧制时，轧制温度为800-1100℃，轧制前保温时间为0.5-2h，单次变形量为5-15％，单次轧制变形以后退火5-20min，总变形量为30％-70％，轧制完成冷却方式为空冷。
S4.2)所述热变形为热挤压时，挤压温度为1000-1300℃，挤压前保温时间为0.5-2h，挤压比为(4-20):1。
进一步，所述S5)时效热处理的具体工艺参数为：
时效热处理温度为500-800℃，保温时间为0.5-240h，冷却介质为空气。
本发明的有益效果是：
1.由于采用上述技术方案，本发明的合金在预合金中引入Co，提高了B2相和基体的高温稳定性。
2.本发明引入了B2相和纳米氧化物粒子，B2相的体积分数大于20％，且B2相均匀分布在基体中。
3.本发明制备的多纳米相强化铁素体ODS合金基体由尺寸小于1μm的细晶组成，在外加载荷作用下晶粒变形更加均匀，具有优良的室温拉伸塑性，断前延伸率超过10％，满足室温加工塑形的要求。
附图说明：
图1为本发明的一种具有拉伸塑性的多纳米相强化ODS合金的制备方法的工艺流程图。
图2为采用本发明的方法具有拉伸塑性的多纳米相强化ODS合金的沉淀相FESEM图和纳米氧化物粒子的TEM图。
图3为采用本发明的方法制备得到具有拉伸塑性的多纳米相强化ODS合金的晶粒分布示意图。
图4为本发明的实施例2制备得到的具有拉伸塑性的多纳米相强化ODS合金的室温拉伸曲线示意图。
具体实施方式：
下面结合附图和具体实施例对本发明的技术方案做进一步说明。
如图1所示，本发明一种具有拉伸塑性的多纳米相强化ODS合金的制备方法，该制备方法包括如下步骤：
S1)将预合金粉末与Y2O3粉末进行机械合金化反应，得到合金粉末；
S2)将S1)得到合金粉末进行致密化处理，得到合金块体；
S3)将S2)得到的合金块体进行固溶热处理；
S4)将S3)处理后的合金块体进行热变形处理；
S5)将S4)处理后的合金块体进行时效热处理，即得到具有拉伸塑性的多纳米相强化ODS合金。
所述具有拉伸塑性的多纳米相强化ODS合金由高体积分数的B2相和氧化物共强化；且多纳米相强化ODS合金中B2相的体积分数大于20％；
所述多纳米相强化ODS合金的断前延伸率超过10％。
所述S1)中的预合金粉末为采用气雾化法制备得到；
所述的Y2O3粉末的加入量为预合金粉末的质量的0.3-0.5wt％；
所述机械合金化反应的工艺为：惰性气氛为高纯氩气，高能球磨的转速为340-450转/分，球磨时间为40-60h。
所述预合金粉末成分的质量百分数为：Cr 10-14％，Ni 8-12％，Co 8-12％，Al 4-8％，Mo 0-2％，Zr 0-2％，Hf 0-2％，余量为Fe和不可避免的杂质。
所述S2)中的致密化处理具体工艺为：
S2.1)采用SPS烧结的工艺为：机械合金化粉末放入石墨模具中，烧结温度为1050-1200℃，压力为30-50MPa，保温时间为5-10min；
S2.2)采用热等静压制备：用低碳钢将机械合金化粉末包套后进行热等静压，热等静压温度为1000-1150℃，压力为100-200MPa，保温时间为1-3h。
所述S3)中的固溶热处理参数为：
固溶热处理温度为1000-1300℃，保温时间为0.5-2h，冷却介质为空气。
所述S4)中的热变形处理参数为：
采用轧制热变形，轧制温度为800-1100℃，轧制前保温时间为0.5-2h，单次变形量为5-15％，单次轧制变形以后退火5-20min，总变形量为30％-70％，轧制完成冷却方式为空冷。
所述S4)中的热变形处理参数为：
采用热挤压实现热变形，挤压温度为1000-1300℃，挤压前保温时间为0.5-2h，挤压比为4-20:1。
所述S5)中的时效热处理参数为：
时效热处理温度为500-800℃，保温时间为0.5-240h，冷却介质为空气。
一种具有拉伸塑性的多纳米相强化ODS合金采用上述的制备方法制备得到。
实施例1：成分为Fe-12wt.％Cr-6wt.％Al-10wt.％Co-10wt.％Ni-2wt.％Mo-0.3wt.％Y2O3合金的制备
采用气雾化法制备了成分为Fe-10wt.％Cr-6wt.％Al-10wt.％Co-10wt.％Ni-2wt.％Mo的预合金粉末，根据设定成分将预合金粉末与Y2O3粉末进行称量并混合均匀，然后在高纯Ar气氛中高能球磨进行机械合金化反应，转速为400转/分，球磨时间为50h；球磨后的合金粉末通过SPS烧结进行致密化，烧结温度为1150℃，压力为40MPa，保温时间为10min。烧结致密化后的合金在1150℃保温2h然后在空气中冷却进行固溶处理。固溶处理的样品进行热挤压处理，热挤压温度为1100℃，挤压前保温时间为2h，挤压比为20:1，挤压完成后空冷得到变形样品。将变形样品在650℃时效120h，得到了成分为Fe-12wt.％Cr-6wt.％Al-10wt.％Co-10wt.％Ni-2wt.％Mo-0.3wt.％Y2O3的铁素体ODS合金。
实施例2：成分为Fe-10wt.％Cr-5wt.％Al-12wt.％Co-12wt.％Ni-1.5wt.％Mo-0.5wt.％Zr-0.3wt.％Y2O3合金的制备：
采用气雾化法制备了成分为Fe-10wt.％Cr-5wt.％Al-12wt.％Co-12wt.％Ni-1.5wt.％Mo-0.5wt.％Zr的预合金粉末，根据设定成分将预合金粉末与Y2O3粉末进行称量并混合均匀，然后在高纯Ar气氛中高能球磨进行机械合金化反应，转速为380转/分，球磨时间为45h；球磨后的合金粉末通过SPS烧结进行致密化，烧结温度为1180℃，压力为40MPa，保温时间为5min。烧结致密化后的合金在1200℃保温1h然后在空气中冷却进行固溶处理。固溶处理的样品进行热轧处理，轧制温度为900℃，轧制前保温1h，轧制单次变形量为10％，单次轧制变形后退火20min，总变形量为50％，轧制完成后空冷得到变形样品。将变形样品在700℃时效48h，得到了成分为Fe-10wt.％Cr-5wt.％Al-12wt.％Co-12wt.％Ni-1.5wt.％Mo-0.5wt.％Zr-0.3wt.％Y2O3的铁素体ODS合金。合金中沉淀相的FESEM图和纳米氧化物粒子的TEM图如图2所示，晶粒尺寸分布图如图3所示，室温拉伸曲线如图4所示，合金具有良好的室温塑形，断前延伸率超过10％。
实施例3：成分为Fe-14wt.％Cr-5wt.％Al-8wt.％Co-10wt.％Ni-1wt.％Mo-0.5wt.％Zr-0.3wt.％Y2O3合金的制备
采用气雾化法制备了成分为Fe-14wt.％Cr-5wt.％Al-8wt.％Co-10wt.％Ni-1wt.％Mo-0.5wt.％Zr的预合金粉末，根据设定成分将预合金粉末与Y2O3粉末进行称量并混合均匀，然后在高纯Ar气氛中高能球磨进行机械合金化反应，转速为450转/分，球磨时间为60h；球磨后的合金粉末通过热等静压进行致密化，用低碳钢对机械合金化粉末进行包套，然后进行热等静压，烧结温度为1150℃，压力为150MPa，保温时间为1.5h。烧结致密化后的合金在1250℃保温0.5h然后在空气中冷却进行固溶处理。固溶处理的样品进行热挤压处理，热挤压温度为1200℃，挤压前保温时间为1.5h，挤压比为15:1，挤压完成后空冷得到变形样品。将变形样品在750℃时效50h，得到了成分为Fe-14wt.％Cr-5wt.％Al-8wt.％Co-10wt.％Ni-1wt.％Mo-0.5wt.％Zr-0.3wt.％Y2O3的铁素体ODS合金。
实施例4：成分为Fe-10wt.％Cr-7wt.％Al-12wt.％Co-12wt.％Ni-2wt.％Mo-0.5wt.％Zr-0.5wt.％Hf-0.4wt.％Y2O3合金的制备
采用气雾化法制备了成分为Fe-10wt.％Cr-7wt.％Al-12wt.％Co-12wt.％Ni-2wt.％Mo-0.5wt.％Zr-0.5wt.％Hf的预合金粉末，根据设定成分将预合金粉末与Y2O3粉末进行称量并混合均匀，然后在高纯Ar气氛中高能球磨进行机械合金化反应，转速为420转/分，球磨时间为55h；球磨后的合金粉末通过热等静压进行致密化，用低碳钢对机械合金化粉末进行包套，然后进行热等静压，烧结温度为1100℃，压力为200MPa，保温时间为2h。烧结致密化后的合金在1250℃保温1h然后在空气中冷却进行固溶处理。固溶处理的样品进行热轧处理，轧制温度为1000℃，轧制前保温1h，轧制单次变形量为15％，单次轧制变形后退火15min，总变形量为60％，轧制完成后空冷得到变形样品。将变形样品在700℃时效100h，得到了成分为Fe-10wt.％Cr-7wt.％Al-12wt.％Co-12wt.％Ni-2wt.％Mo-0.5wt.％Zr-0.5wt.％Hf-0.3wt.％Y2O3的铁素体ODS合金。
本发明一种具有拉伸塑性的多纳米相强化ODS(Oxide dispersion-strengthenedalloy)合金的制备方法，其原理为：将气雾化法制备的含Co的预合金粉末与Y2O3粉末按照设定的成分混合均匀，通过高能球磨进行机械合金化，再通过热等静压或者SPS烧结技术进行致密化处理。将烧结的样品进行固溶处理、热变形处理和随后的时效处理，热变形一方面促进B2相沉淀的形核，另一方面细化晶粒，在合金冷却过程中利用纳米氧化物粒子的钉扎晶界作用阻止晶粒的长大，使基体由细小的晶粒组成，从而改善合金室温塑形，最终得到了B2相体积分数大于20％，且具有良好室温塑形的铁素体ODS(氧化物弥散强化)合金。
以上内容是结合具体的优选实施方式对本发明作的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演和替换，都应当视为属于本发明的保护范围。
Claims (4)
1.一种具有拉伸塑性的多纳米相强化ODS合金的制备方法，其特征在于，所述制备方法包括如下步骤：
S1）将预合金粉末与Y2O3粉末进行机械合金化反应，得到合金粉末；
所述预合金粉末成分的质量百分数为：Cr10-14%，Ni8-12%，Co8-12%，Al4-8%，Mo0-2%，Zr0-2%，Hf0-2%，余量为Fe和不可避免的杂质；
所述预合金粉末为采用气雾化法制备得到；
所述的Y2O3粉末的加入量为预合金粉末的质量的0.3-0.5wt%；
所述机械合金化反应的工艺为：惰性气氛为高纯氩气，高能球磨的转速为340-450转/分，球磨时间为40-60h；
S2）将S1）得到合金粉末进行致密化处理，得到合金块体；
S3）将S2）得到的合金块体进行固溶热处理；
所述固溶热处理温度为1000-1300℃，保温时间为0.5-2h，冷却介质为空气；
S4）将S3）处理后的合金块体进行热变形处理；
所述热变形处理采用轧制热变形，轧制温度为800-1100℃，轧制前保温时间为0.5-2h，单次变形量为5-15%，单次轧制变形以后退火5-20min，总变形量为30%-70%，轧制完成冷却方式为空冷；
S5）将S4）处理后的合金块体进行时效热处理，即得到具有拉伸塑性的多纳米相强化ODS合金；所述具有拉伸塑性的多纳米相强化ODS合金由高体积分数的B2相和氧化物共强化；且多纳米相强化ODS合金中B2相的体积分数大于20%；
所述多纳米相强化ODS合金的断前延伸率超过10%；
所述时效热处理温度为500-800℃，保温时间为0.5-240h，冷却介质为空气。
2.根据权利要求1所述的制备方法，其特征在于，所述S2）中的致密化处理具体工艺为：
当采用SPS烧结的工艺为：机械合金化粉末放入石墨模具中，烧结温度为1050-1200℃，压力为30-50MPa，保温时间为5-10min；
当采用热等静压制备：用低碳钢将机械合金化粉末包套后进行热等静压，热等静压温度为1000-1150℃，压力为100-200MPa，保温时间为1-3h。
3.根据权利要求1所述的制备方法，其特征在于，所述S4）中的热变形处理参数为：
采用热挤压实现热变形，挤压温度为1000-1300℃，挤压前保温时间为0.5-2h，挤压比为4-20:1。
4.一种具有拉伸塑性的多纳米相强化ODS合金，其特征在于，所述多纳米相强化ODS合金采用如权利要求1-3任意一项所述的制备方法制备得到。
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