CN114892093B - 一种高强韧性匹配氧化物颗粒弥散钢及其制备方法和应用 - Google Patents
一种高强韧性匹配氧化物颗粒弥散钢及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种高强韧性匹配氧化物颗粒弥散钢及其制备方法和应用,属于新型结构材料技术领域。所述高强韧性匹配氧化物颗粒弥散钢的组分按质量百分数计,包括:Cr11.0‑13.0%,W1.0‑2.0%,V0.1‑0.2%,Y0.3‑0.4%,O0.05‑0.15%,Si1.5‑2.5%,C≤0.0016%,其余为Fe和不可避免的杂质。本发明采用粉末冶金的制备方式,通过引入较高含量的硅元素和使用特殊的热处理制度引入高密度具有完整核壳结构的氧化物颗粒,制备出一种高强韧性匹配氧化物颗粒弥散钢。该合金满足了核反应堆燃料包壳材料的强韧性要求,具有极高的商用价值和广阔的发展前景。
Description
技术领域
本发明涉及新型结构材料技术领域,特别涉及一种高强韧性匹配氧化物颗粒弥散钢及其制备方法和应用。
背景技术
鉴于核事故发生后的严重后果,核工业领域对核反应堆的燃料包壳材料的事故容错率及相关服役性能提出了更高的要求,其中包括高温耐辐照损伤性能、高强度、高韧性等性能要求。
传统的核反应堆燃料包壳材料为锆合金材料。锆合金材料具有非常优异的服役性能,但是其事故容错率很低,事故发生时锆合金与水蒸气接触迅速产生大量氢气并引发氢爆的特性带来了极大隐患。氢爆也正是福岛核事故造成大范围影响的主要原因之一。因此,核工业领域将对事故容错率较高的氧化物颗粒弥散(ODS)钢的开发提上日程。ODS钢中高密度的氧化物弥散颗粒具有捕捉辐照缺陷,抑制辐照损伤的特性,具有非常优异的高温耐辐照损伤性能。因此ODS钢成为了建造先进四代反应堆和核聚变反应堆中最具有商业前景的核燃料包壳材料,具有广阔的发展和应用前景。但是目前所开发的ODS钢始终具有强度高、塑性较差的缺点。
发明内容
为解决上述问题,本发明提供了一种高强韧性匹配氧化物颗粒弥散钢及其制备方法和应用。通过使用特殊的热处理步骤,引入高密度具有完整核壳结构的氧化物颗粒,开发出了一种兼具高强度和高韧性的氧化物颗粒弥散钢。
为实现上述目的,本发明提供了如下技术方案:
本发明技术方案之一:提供一种高强韧性匹配氧化物颗粒弥散钢,组分按质量百分数计,包括:Cr 11.0-13.0%,W 1.0-2.0%,V 0.1-0.2%,Y 0.3-0.4%,O 0.05-0.15%,Si 1.5-2.5%,C≤0.0016%,其余为Fe和不可避免的杂质。
本发明技术方案之二:提供一种上述高强韧性匹配氧化物颗粒弥散钢的制备方法,包括以下步骤:
将按照合金成分配比取Cr、W、V和Fe制成预合金粉末,再与Si粉末、Y粉末和Y2O3粉末混合,依次经球磨,烧结,锻造,热处理,淬火,得到高强韧性匹配氧化物颗粒弥散钢。
优选地,所述预合金粉末的粒径为5-30μm;所述Si粉末的粒径为1-5μm;所述Y粉末的粒径为1-5μm;所述Y2O3粉末的粒径为1-5μm。
优选地,所述烧结采用的是热等静压烧结工艺。
优选地,所述锻造采用热锻+温锻两步法,热锻在1150℃保温1h后自由锻造,采用正交锻造的方法,锻造比为2:1,锻造后自然冷却,温锻在800℃保温3-5h后锻造,采用模锻正交锻造的方法,锻造比为2:1,锻造后埋沙冷却。
优选地,所述热处理的温度为1150-1250℃,时间为20min。
优选地,所述淬火的温度为20℃。
优选的,在球磨过程中持续通入氩气,且研磨球选用玛瑙球。保持气氛清洁并且避免C元素的引入,使合金材料的C含量控制在较低水平。
本发明技术方案之三:提供一种上述高强韧性匹配氧化物颗粒弥散钢在制备核反应堆燃料包壳材料、航空发动机结构材料和发电厂蒸汽运输管道结构材料中的应用。
本发明的有益技术效果如下:
本发明提供了一种高强韧性匹配氧化物颗粒弥散钢及其制备方法和应用。通过使用特定的热处理步骤和两步法锻造,在该高强韧性匹配氧化物颗粒弥散钢中引入了稳定的高密度具有完整核壳结构的氧化物颗粒,其中壳成分为无定形态的富铬/钒壳,核成分为钇硅氧化物,氧化物颗粒周围的无定形态富铬/钒壳硬度低,缓解了颗粒周围的应力集中,提高了高强韧性匹配氧化物颗粒弥散钢的韧性。
同时,高强韧性匹配氧化物颗粒弥散钢中添加的较高含量的硅元素析出了大量钇硅氧化物,提高了高强韧性匹配氧化物颗粒弥散钢的强度;硅元素和核壳结构同时作用,使制得的高强韧性匹配氧化物颗粒弥散钢同时获得较高的强度和韧性。
本发明采用粉末冶金的制备方式,通过使用不同于经验值(现有技术中,只有在低温下短时间保温才能得到该结构的氧化物颗粒)的热处理制度,引入高密度具有完整核壳结构的氧化物颗粒,制备了一种高强韧性匹配氧化物颗粒弥散钢。该合金满足了核反应堆燃料包壳材料的强韧性要求,具有极高的商用价值和广阔的发展前景。
附图说明
图1为实施例1制备的高强韧性匹配氧化物颗粒弥散钢的明场像透射电子显微结构图。
图2为实施例1制备的高强韧性匹配氧化物颗粒弥散钢的高密度的核壳结构氧化物颗粒的高角环形暗场像透射电子显微结构图。
图3为实施例1制备的高强韧性匹配氧化物颗粒弥散钢中Fe、Cr、W、Y、Si、V、O元素的能量弥散X射线面分布图。
具体实施方式
现详细说明本发明的多种示例性实施方式,该详细说明不应认为是对本发明的限制,而应理解为是对本发明的某些方面、特性和实施方案的更详细的描述。应理解本发明中所述的术语仅仅是为描述特别的实施方式,并非用于限制本发明。
另外,对于本发明中的数值范围,应理解为还具体公开了该范围的上限和下限之间的每个中间值。在任何陈述值或陈述范围内的中间值,以及任何其他陈述值或在所述范围内的中间值之间的每个较小的范围也包括在本发明内。这些较小范围的上限和下限可独立地包括或排除在范围内。
除非另有说明,否则本文使用的所有技术和科学术语具有本发明所述领域的常规技术人员通常理解的相同含义。虽然本发明仅描述了优选的方法和材料,但是在本发明的实施或测试中也可以使用与本文所述相似或等同的任何方法和材料。
关于本文中所使用的“包含”、“包括”、“具有”、“含有”等等,均为开放性的用语,即意指包含但不限于。
实施例1
本实施例按照Cr 12%,W 1.5%,V 0.15%,Y 0.35%,O 0.12%,Si 1.5%,C≤0.0016%,其余为Fe的质量百分比设计高强韧性匹配氧化物颗粒弥散钢。
具体制备步骤如下:
(1)采用气雾化粉技术制备粒径为15μm的Cr、W、V和Fe粉末,按质量配比称取,混合,作为预合金粉末;
(2)将预合金粉末与高强韧性匹配氧化物颗粒弥散钢总质量1.5%的Si粉(粒径3μm)、高强韧性匹配氧化物颗粒弥散钢总质量0.08%的Y粉(粒径3μm)和高强韧性匹配氧化物颗粒弥散钢总质量0.35%的Y2O3粉(粒径4μm)混合均匀,放入大型球磨机中球磨,转速设置为200rpm,球粉比为10:1,球磨60h,球磨过程中持续通入氩气,研磨球选用玛瑙球;
(3)将步骤(2)球磨后的粉末装罐密封,放入热等静压炉烧结固化,温度为1150摄氏度,压力为15MPa,时间为2h;
(4)将固化后的钢块采用热锻+温锻两步法锻造为饼状钢坯,热锻在1150℃保温1h后自由锻造,采用正交锻造的方法,锻造比为2:1,锻造后自然冷却,温锻在800℃保温4h后锻造,采用模锻正交锻造的方法,锻造比为2:1,锻造后埋沙冷却;
(5)将步骤(4)所得钢坯转移至马弗炉中1200℃热处理20min;冷却至700℃后取出,放入温度为20℃的水中急速淬火,得到高强韧性匹配氧化物颗粒弥散钢。
实施例1制备的高强韧性匹配氧化物颗粒弥散钢的明场像透射电子显微结构图见图1,从图1中可以看出,实施例1制备的高强韧性匹配氧化物颗粒弥散钢中存在高密度的核壳结构氧化物颗粒。
实施例1制备的高强韧性匹配氧化物颗粒弥散钢的高密度的核壳结构氧化物颗粒的高角环形暗场像透射电子显微结构图见图2。从图2中可以看出,实施例1制备的高强韧性匹配氧化物颗粒弥散钢中存在高密度的核壳结构氧化物颗粒均匀分布在晶界内和晶界上。
实施例1制备的高强韧性匹配氧化物颗粒弥散钢中Fe、Cr、W、Y、Si、V、O元素的能量弥散X射线面分布图见图3。从图3中可以看出实施例1制备的高强韧性匹配氧化物颗粒弥散钢中存在高密度的核壳结构氧化物颗粒成分为钇硅氧化物。
经测定,实施例1制备的高强韧性匹配氧化物颗粒弥散钢在室温下的拉伸强度为985MPa,塑性为22.3%;在700℃下的拉伸强度为289MPa,塑性为27.1%。
实施例2
本实施例按照Cr 12.0%,W 1.5%,V 0.15%,Y 0.35%,O 0.12%,Si 2.0%,C≤0.0016%,其余为Fe的质量百分比设计高强韧性匹配氧化物颗粒弥散钢。
具体制备步骤如下:
(1)采用气雾化粉技术制备粒径为15μm的Cr、W、V和Fe粉末,按质量配比称取,混合,作为预合金粉末;
(2)将预合金粉末与高强韧性匹配氧化物颗粒弥散钢总质量2.0%的Si粉(粒径3μm)、高强韧性匹配氧化物颗粒弥散钢总质量0.08%的Y粉(粒径3μm)和高强韧性匹配氧化物颗粒弥散钢总质量0.35%的Y2O3粉(粒径4μm)混合均匀,放入大型球磨机中球磨,转速设置为200rpm,球粉比为10:1,球磨60h;
(3)将步骤(2)球磨后的粉末装罐密封,放入热等静压炉烧结固化,温度为1150摄氏度,压力为15MPa,时间为2h;
(4)将固化后的钢块采用热锻+温锻两步法锻造为饼状钢坯,热锻在1150℃保温1h后自由锻造,采用正交锻造的方法,锻造比为2:1,锻造后自然冷却,温锻在800℃保温4h后锻造,采用模锻正交锻造的方法,锻造比为2:1,锻造后埋沙冷却;
(5)将步骤(4)所得钢坯转移至马弗炉中1200℃热处理20min;冷却至700℃后取出,放入温度为20℃的水中急速淬火,得到高强韧性匹配氧化物颗粒弥散钢。
经测定,实施例2制备的高强韧性匹配氧化物颗粒弥散钢在室温下的拉伸强度为1128MPa,塑性为21.7%;在700℃下的拉伸强度为333MPa,塑性为26.9%。
实施例3
本实施例按照Cr 12.0%,W 1.5%,V 0.15%,Y 0.35%,O 0.12%,Si 2.5%,C≤0.0016%,其余为Fe的质量百分比设计高强韧性匹配氧化物颗粒弥散钢。
具体制备步骤如下:
(1)采用气雾化粉技术制备粒径为15μm的Cr、W、V和Fe粉末,按质量配比称取,混合,作为预合金粉末;
(2)将预合金粉末与高强韧性匹配氧化物颗粒弥散钢总质量2.5%的Si粉(粒径3μm)、高强韧性匹配氧化物颗粒弥散钢总质量0.08%的Y粉(粒径3μm)和高强韧性匹配氧化物颗粒弥散钢总质量0.35%的Y2O3粉(粒径4μm)混合均匀,放入大型球磨机中球磨,转速设置为200rpm,球粉比为10:1,球磨60h;
(3)将步骤(2)球磨后的粉末装罐密封,放入热等静压炉烧结固化,温度为1150摄氏度,压力为15MPa,时间为2h;
(4)将固化后的钢块采用热锻+温锻两步法锻造为饼状钢坯,热锻在1150℃保温1h后自由锻造,采用正交锻造的方法,锻造比为2:1,锻造后自然冷却,温锻在800℃保温4h后锻造,采用模锻正交锻造的方法,锻造比为2:1,锻造后埋沙冷却;
(5)将步骤(4)所得钢坯转移至马弗炉中1200℃热处理20min;冷却至700℃后取出,放入温度为20℃的水中急速淬火,得到高强韧性匹配氧化物颗粒弥散钢。
经测定,实施例3制备的高强韧性匹配氧化物颗粒弥散钢在室温下的拉伸强度为1477MPa,塑性为20.9%;在700℃下的拉伸强度为395MPa,塑性为25.3%。
对比例1
高强韧性匹配氧化物颗粒弥散钢的制备:
与实施例1相比,区别在于省略步骤(4),其他操作与实施例1相同。
经测定,对比例1制备的高强韧性匹配氧化物颗粒弥散钢在室温下的拉伸强度为786MPa,塑性为10.1%;在700℃下的拉伸强度为217MPa,塑性为11.5%。这是由于省略步骤(4)后,钢中不具有特殊的核壳结构或核壳结构数量降低,导致强韧性下降。这是由于省略步骤(4)后,钢中不具有特殊的核壳结构的氧化物颗粒或具有核壳结构的氧化物颗粒数量降低,导致强韧性下降。
对比例2
高强韧性匹配氧化物颗粒弥散钢的制备:
与实施例1相比,区别在于省略步骤(5),其他操作与实施例1相同。
经测定,对比例2制备的高强韧性匹配氧化物颗粒弥散钢在室温下的拉伸强度为815MPa,塑性为11.9%;在700℃下的拉伸强度为225MPa,塑性为14.7%。这是由于省略步骤(5)后,钢中具有特殊的核壳结构的氧化物颗粒数量显著降低,导致强韧性下降。
对比例3
高强韧性匹配氧化物颗粒弥散钢的制备:
与实施例1相比,区别在于步骤(5)中热处理温度为900℃,其他操作与实施例1相同。
经测定,对比例2制备的高强韧性匹配氧化物颗粒弥散钢在室温下的拉伸强度为868MPa,塑性为13.4%;在700℃下的拉伸强度为266MPa,塑性为20.5%。这是由于步骤(5)中热处理温度对钢的显微结构存在显著影响,导致特殊的核壳结构的氧化物颗粒未能析出或消失,导致强韧性下降。
以上所述的实施例仅是对本发明的优选方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案做出的各种变形和改进,均应落入本发明权利要求书确定的保护范围内。
Claims (5)
1.一种高强韧性匹配氧化物颗粒弥散钢,其特征在于,组分按质量百分数计,包括:Cr11.0-13.0%,W 1.0-2.0%,V 0.1-0.2%,Y 0.3-0.4%,O 0.05-0.15%,Si 1.5-2.5%,C≤0.0016%,其余为Fe和不可避免的杂质;
所述高强韧性匹配氧化物颗粒弥散钢的制备方法包括以下步骤:
将按照合金成分配比取Cr、W、V和Fe制成预合金粉末,再与Si粉末、Y粉末和Y2O3粉末混合,依次经球磨,烧结,锻造,热处理,淬火,得到高强韧性匹配氧化物颗粒弥散钢;
所述锻造采用热锻+温锻两步法,热锻在1150℃保温1h后自由锻造,采用正交锻造的方法,锻造比为2:1,锻造后自然冷却,温锻在800℃保温3-5h后锻造,采用模锻正交锻造的方法,锻造比为2:1,锻造后埋沙冷却;
所述热处理的温度为1150-1250 ℃,时间为20min;
所述淬火的温度为20℃。
2.一种权利要求1所述高强韧性匹配氧化物颗粒弥散钢的制备方法,其特征在于,包括以下步骤:
将按照合金成分配比取Cr、W、V和Fe制成预合金粉末,再与Si粉末、Y粉末和Y2O3粉末混合,依次经球磨,烧结,锻造,热处理,淬火,得到高强韧性匹配氧化物颗粒弥散钢;
所述锻造采用热锻+温锻两步法,热锻在1150℃保温1h后自由锻造,采用正交锻造的方法,锻造比为2:1,锻造后自然冷却,温锻在800℃保温3-5h后锻造,采用模锻正交锻造的方法,锻造比为2:1,锻造后埋沙冷却;
所述热处理的温度为1150-1250 ℃,时间为20min;
所述淬火的温度为20℃。
3.根据权利要求2所述的制备方法,其特征在于,所述预合金粉末的粒径为5-30μm;所述Si粉末的粒径为1-5μm;所述Y粉末的粒径为1-5μm;所述Y2O3粉末的粒径为1-5μm。
4.根据权利要求2所述的制备方法,其特征在于,所述烧结采用热等静压烧结工艺。
5.权利要求1所述高强韧性匹配氧化物颗粒弥散钢在制备核反应堆燃料包壳材料、航空发动机结构材料或发电厂蒸汽运输管道结构材料中的应用。
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