氧化物弥散强化铁基高温合金的制备及强化机理研究
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摘要
氧化物弥散强化铁基高温合金由于具备低肿胀、抗辐射、抗氧化、抗腐蚀及高的蠕变强度等综合性能,被认为是下一代核裂变/聚变反应堆第一壁等关键结构用材料,在国际上得到了大量研究者关注。本论文在国家自然科学基金重点项目资助下,对Fe-(12-14)Cr-3W-(0.3-0.4)Ti-(0.3-0.4)Y2O3-(1Cu)(wt.%)合金体系中的显微组织演化和力学性能开展了系统的研究工作。首先,系统研究了氧引入方式的新工艺,并对氧的存在方式及演化形式对纳米弥散相形成的作用进行了解释；同时通过对该合金体系中空位的形成及演化机制的研究和空位生成焓的测定,阐述了空位和Y-Ti-O纳米结构相的作用。其次,采用HRTEM、HAADF-STEM、TEM-EDX等分析手段对合金中的5nm左右的Y-Ti-O、铜沉淀等进行了深入的研究,阐明了其相成分组成、结构、与基体的位相关系及演化机制；最后,通过制备具有双晶尺寸分布的氧化物弥散强化铁素体钢,改善合金的韧性,同时通过微合金化过程对合金体系进行了组织改性,提高了合金的综合力学性能。主要得到的结论如下：
(1)通过紧耦合雾化过程引入氧元素,粉末氧含量与雾化介质中氧含量成线性增长关系,粉末中氧的分布由内而外依次增多,氧可部分固溶于粉末中。粉末表面的氧在热固结过程中形成由氧化物组成的原始颗粒边界,在热机械处理后,原始颗粒边界破碎,氧元素重新向基体中扩散,在基体中形成弥散分布的氧化物。合金在1400℃退火1h,空冷后的力学性能最优,室温抗拉强度和断后延伸率分别为940MPa,7%。
(2)在Fe-Cr-W-Ti-Y预合金粉末中添加1wt.%Fe203纳米颗粒,能够促进热挤压—热轧制过程中多种复合氧化物颗粒的形成。除了纳米Y2Ti2O7相,合金中还形成了微米级的Cr1.3Fe0.7O3、(Cr0.88Ti0.12)2O3和Y3Fe5O12相。微米级颗粒的形成与Fe2O3粉末在热挤压过程中团聚成型和Fe203与亲氧能力强的原子(Y、Ti、Cr)发生置换反应有关。添加少量Fe203粉末能够明显提高热挤压—热轧制粉末冶金铁基合金的显微硬度和室温、中温(550℃)抗拉强度。合金室温抗拉强度为1257MPa,比未添加Fe203粉末的合金增加了50.7%,但延伸率从13%降低至6.5%。
(3)在过饱和铁素体基体中,不共格的富Cr、Ti氧化物相与共格的Y-Ti-O纳米相共同沉淀,延长机械合金化时间可以将Cr、Ti元素回溶于基体中,有利于形成细小的均匀弥散的Y-Ti-O纳米颗粒。
(4)在14YWT和14FWT两种铁素体钢中,发现至少存在两种不同晶体学取向的Y-Ti-O纳米相,具有Y2Ti2O7结构。用Fe2O3作为携氧剂制备的纳米结构相强化铁素体钢表现出优异的综合性能。通过计算,该合金的空位生成焓约为1.11eV,明显低于纯铁的空位生成焓,为Y-Ti-O纳米相的形成提供了有利的结构条件。
(5)双晶尺寸分布晶粒组织能够有效提高纳米特征弥散强化铁素体钢的延性。通过理论计算,具有晶粒尺寸双峰粒度分布的纳米弥散强化铁素体钢的应变值比仅由纳米尺度晶粒组成的14CrODS铁素体钢要超出100%以上,理论计算与实验值符合较好。
(6)经过加铜微合金化的合金在时效10h时硬度达到峰值,此时合金中形成富铜的强化相,富铜沉淀的平均颗粒尺寸约为9.6nm,体积分数约为1022m-3。加铜微合金化可以进一步平衡合金的韧性与强度,富铜沉淀相经过500℃、300h长时间热暴露未发生明显长大。相对未加铜的双晶尺寸分布铁素体钢而言,加铜微合金化的合金强度得到很大的提高,在室温下,富铜沉淀强化的作用效果适用Orowan绕过机制。
Oxide dispersion strengthened iron-base superalloy is considered as the critical structure materials in the next generation of nuclear fission/fusion reactor, which attract a large number of researchers to carry out extensive research, due to its low-swelling, irradiatio resistance, oxidation resisitance, corrosion resistance and high creep strength. This work was supported by the National Natural Science Foundation of China. The microstructural evolution and mechanical properties of the Fe-(12-14)Cr-3W-(0.3-0.4) Ti-(0.3-0.4) Y2O3-(1Cu)(wt.%) alloy system have been investigated systematically. Firstly, the technology inducing oxygen was systematically studied in this work, as well as the effect of existence and evolution of oxygen on formation of nanoparticles was explained.The relationship between vacancy and Y-Ti-O nanoparticle was described through formation and evolution of vacancy and vacancy formation enthalpy in this alloy system. Secondly, HRTEM, HAADF-STEM, TEM-EDX analysis were used to investigate deeply on Y-Ti-O oxides and copper precipitation with mean particle sizes about5nm. Finally, the microstructures of the alloy system were modified to improve mechanical properties through micro-alloying and powder metallurgy process. Main conclusions as follows:
(1) Introducing oxygen by gas atomized process, the oxygen content in powders and that in gas atomized atmosphere was a linear growth relationship. Oxygen content in powder increased from the inside in turn. Oxygen in the powder can be part of solution. The oxygen on powder surface was formed prior particle boudary composed of oxides in the hot powder consolidation process. After the thermo-mechanical and heat treatment, crushing the original grain boundaries and oxygen resolution to the matrix occurred to form nanoscale dispersed oxides in the matrix due to the prior particle boundaries crushing. After annealling at1400℃for1h and followed by air-cooled, the room temperature tensile strength and elongation were940MPa,7%, respectively.
(2) Mixing nano-1wt.%Fe2O3particles in the Fe-Cr-W-Ti-Y pre-alloyed powder, the formation of a variety of composite oxide particles can be promoted in the hot extrusion-hot rolling process. In addition to nano Y2Ti207phase, micron-sized Cr1.3Fe0.7O3,(Cr0.88Ti0,12)203and Y3Fe5012phase were also formed. Formation micron-sized particle was related to agglomeration of Fe2O3powder in the hot extrusion process of and reaction between Fe2O3and strong pro-oxygen atoms (Y, Ti, Cr). Addtion of a small amount of Fe2O3powder can significantly improve microhardness and room temperature, intermediate temperature (550℃) tensile strength of the hot extrusion-hot rolling powder metallurgy iron-based alloy. The room temperature tensile strength of the Fe2O3addtion alloy was1257MPa, compared with the Fe2O3-free alloy that was increased by50.7%, but the elongation decreased from13%to6.5%.
(3)In the supersaturated ferrite matrix, the incoherence Cr, Ti-rich oxide phases and coherency Y-Ti-O nanoparticle were co-precipitated. Resolution of Cr, Ti elements in the matrix can be occured to by extending the mechanical alloying time, which is conducive to the formation of small uniform dispersion of Y-Ti-O nanoparticles.
(4) In14YWT and14FWT two kinds of ferritic steels, two different crystallographic orientations at least between the Y-Ti-O nanoparticles with a Y2Ti207lattice structure and the matrix have been found. The nanostructural oxide dispersion strengthened ferritic steel prepared using Fe2O3as an oxygen carrier yield an excellent mechanical properties. The vacancy formation enthalpy of the alloy was about1.11eV by calculating, which was significantly lower than the pure iron vacancy formation enthalpy of the pure iron. That provides a favorable structural conditions to formation of the Y-Ti-O nanoparticle.
(5) Bimodal grain size distribution structure can effectively improve the ductility of oxide dispersion strengthened ferritic steel. Through theoretical calculation, the ductility of bimodal grain size distribution oxide dispersion strengthened ferritic steel was exceed100%than that of only nanoscale grain14Cr ODS ferritic steel, however theoretical and experimental values was good agreement.
(6) Adding copper as micro-alloyed element in bimodal grain size alloy, the microhardness reached a peak value after aging10h at500℃. At peak aging condition, copper-rich precipitation has been formed with a mean particle size about9.6nm and volumn fraction1022m-3. The toughness and strength can be further balanced by adding copper as micro-alloyed element. The copper-rich precipitate did not significantly growth up after500℃,300h prolonged hot exposured. Not increase the relative size distribution of double-crystal copper ferrite steel. The strength of copper addtion micro-alloyed alloy has been greatly improved, comparison to that of copper-free alloy. At room temperature, copper-rich precipitation strengthening effect calculated by Orowan bypass mechanism.
(1)通过紧耦合雾化过程引入氧元素,粉末氧含量与雾化介质中氧含量成线性增长关系,粉末中氧的分布由内而外依次增多,氧可部分固溶于粉末中。粉末表面的氧在热固结过程中形成由氧化物组成的原始颗粒边界,在热机械处理后,原始颗粒边界破碎,氧元素重新向基体中扩散,在基体中形成弥散分布的氧化物。合金在1400℃退火1h,空冷后的力学性能最优,室温抗拉强度和断后延伸率分别为940MPa,7%。
(2)在Fe-Cr-W-Ti-Y预合金粉末中添加1wt.%Fe203纳米颗粒,能够促进热挤压—热轧制过程中多种复合氧化物颗粒的形成。除了纳米Y2Ti2O7相,合金中还形成了微米级的Cr1.3Fe0.7O3、(Cr0.88Ti0.12)2O3和Y3Fe5O12相。微米级颗粒的形成与Fe2O3粉末在热挤压过程中团聚成型和Fe203与亲氧能力强的原子(Y、Ti、Cr)发生置换反应有关。添加少量Fe203粉末能够明显提高热挤压—热轧制粉末冶金铁基合金的显微硬度和室温、中温(550℃)抗拉强度。合金室温抗拉强度为1257MPa,比未添加Fe203粉末的合金增加了50.7%,但延伸率从13%降低至6.5%。
(3)在过饱和铁素体基体中,不共格的富Cr、Ti氧化物相与共格的Y-Ti-O纳米相共同沉淀,延长机械合金化时间可以将Cr、Ti元素回溶于基体中,有利于形成细小的均匀弥散的Y-Ti-O纳米颗粒。
(4)在14YWT和14FWT两种铁素体钢中,发现至少存在两种不同晶体学取向的Y-Ti-O纳米相,具有Y2Ti2O7结构。用Fe2O3作为携氧剂制备的纳米结构相强化铁素体钢表现出优异的综合性能。通过计算,该合金的空位生成焓约为1.11eV,明显低于纯铁的空位生成焓,为Y-Ti-O纳米相的形成提供了有利的结构条件。
(5)双晶尺寸分布晶粒组织能够有效提高纳米特征弥散强化铁素体钢的延性。通过理论计算,具有晶粒尺寸双峰粒度分布的纳米弥散强化铁素体钢的应变值比仅由纳米尺度晶粒组成的14CrODS铁素体钢要超出100%以上,理论计算与实验值符合较好。
(6)经过加铜微合金化的合金在时效10h时硬度达到峰值,此时合金中形成富铜的强化相,富铜沉淀的平均颗粒尺寸约为9.6nm,体积分数约为1022m-3。加铜微合金化可以进一步平衡合金的韧性与强度,富铜沉淀相经过500℃、300h长时间热暴露未发生明显长大。相对未加铜的双晶尺寸分布铁素体钢而言,加铜微合金化的合金强度得到很大的提高,在室温下,富铜沉淀强化的作用效果适用Orowan绕过机制。
Oxide dispersion strengthened iron-base superalloy is considered as the critical structure materials in the next generation of nuclear fission/fusion reactor, which attract a large number of researchers to carry out extensive research, due to its low-swelling, irradiatio resistance, oxidation resisitance, corrosion resistance and high creep strength. This work was supported by the National Natural Science Foundation of China. The microstructural evolution and mechanical properties of the Fe-(12-14)Cr-3W-(0.3-0.4) Ti-(0.3-0.4) Y2O3-(1Cu)(wt.%) alloy system have been investigated systematically. Firstly, the technology inducing oxygen was systematically studied in this work, as well as the effect of existence and evolution of oxygen on formation of nanoparticles was explained.The relationship between vacancy and Y-Ti-O nanoparticle was described through formation and evolution of vacancy and vacancy formation enthalpy in this alloy system. Secondly, HRTEM, HAADF-STEM, TEM-EDX analysis were used to investigate deeply on Y-Ti-O oxides and copper precipitation with mean particle sizes about5nm. Finally, the microstructures of the alloy system were modified to improve mechanical properties through micro-alloying and powder metallurgy process. Main conclusions as follows:
(1) Introducing oxygen by gas atomized process, the oxygen content in powders and that in gas atomized atmosphere was a linear growth relationship. Oxygen content in powder increased from the inside in turn. Oxygen in the powder can be part of solution. The oxygen on powder surface was formed prior particle boudary composed of oxides in the hot powder consolidation process. After the thermo-mechanical and heat treatment, crushing the original grain boundaries and oxygen resolution to the matrix occurred to form nanoscale dispersed oxides in the matrix due to the prior particle boundaries crushing. After annealling at1400℃for1h and followed by air-cooled, the room temperature tensile strength and elongation were940MPa,7%, respectively.
(2) Mixing nano-1wt.%Fe2O3particles in the Fe-Cr-W-Ti-Y pre-alloyed powder, the formation of a variety of composite oxide particles can be promoted in the hot extrusion-hot rolling process. In addition to nano Y2Ti207phase, micron-sized Cr1.3Fe0.7O3,(Cr0.88Ti0,12)203and Y3Fe5012phase were also formed. Formation micron-sized particle was related to agglomeration of Fe2O3powder in the hot extrusion process of and reaction between Fe2O3and strong pro-oxygen atoms (Y, Ti, Cr). Addtion of a small amount of Fe2O3powder can significantly improve microhardness and room temperature, intermediate temperature (550℃) tensile strength of the hot extrusion-hot rolling powder metallurgy iron-based alloy. The room temperature tensile strength of the Fe2O3addtion alloy was1257MPa, compared with the Fe2O3-free alloy that was increased by50.7%, but the elongation decreased from13%to6.5%.
(3)In the supersaturated ferrite matrix, the incoherence Cr, Ti-rich oxide phases and coherency Y-Ti-O nanoparticle were co-precipitated. Resolution of Cr, Ti elements in the matrix can be occured to by extending the mechanical alloying time, which is conducive to the formation of small uniform dispersion of Y-Ti-O nanoparticles.
(4) In14YWT and14FWT two kinds of ferritic steels, two different crystallographic orientations at least between the Y-Ti-O nanoparticles with a Y2Ti207lattice structure and the matrix have been found. The nanostructural oxide dispersion strengthened ferritic steel prepared using Fe2O3as an oxygen carrier yield an excellent mechanical properties. The vacancy formation enthalpy of the alloy was about1.11eV by calculating, which was significantly lower than the pure iron vacancy formation enthalpy of the pure iron. That provides a favorable structural conditions to formation of the Y-Ti-O nanoparticle.
(5) Bimodal grain size distribution structure can effectively improve the ductility of oxide dispersion strengthened ferritic steel. Through theoretical calculation, the ductility of bimodal grain size distribution oxide dispersion strengthened ferritic steel was exceed100%than that of only nanoscale grain14Cr ODS ferritic steel, however theoretical and experimental values was good agreement.
(6) Adding copper as micro-alloyed element in bimodal grain size alloy, the microhardness reached a peak value after aging10h at500℃. At peak aging condition, copper-rich precipitation has been formed with a mean particle size about9.6nm and volumn fraction1022m-3. The toughness and strength can be further balanced by adding copper as micro-alloyed element. The copper-rich precipitate did not significantly growth up after500℃,300h prolonged hot exposured. Not increase the relative size distribution of double-crystal copper ferrite steel. The strength of copper addtion micro-alloyed alloy has been greatly improved, comparison to that of copper-free alloy. At room temperature, copper-rich precipitation strengthening effect calculated by Orowan bypass mechanism.
引文
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