热时效对RPV模拟钢的微结构与冲击性能的影响
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摘要
核电具有低污染、效益高的特点，在缓解能源危机的同时可以降低碳的排放，是当今世界上大规模可持续供应的主要能源之一。核反应堆压力容器（RPV）是压水堆核电站中不可更换的大型关键部件，由Mn-Ni-Mo低合金铁素体钢（A508--III钢）制成，在服役工况下，经过长期中子辐照后会引起韧脆转变温度升高，这是影响RPV安全运行的关键因素，也是核电站寿命的决定性因素。RPV钢的辐照脆化效应主要是由于中子辐照损伤产生晶体缺陷，并诱发高数量密度纳米富Cu相的析出所造成的。
如果用中子辐照试验来研究RPV钢中纳米富Cu相的析出费用太高，实验操作也很不方便，而采用低温热时效的办法也可以使过饱和固溶的Cu以纳米富Cu相形式析出，但是时效时间过长。为了加速纳米富Cu相的析出，本工作以提高了Cu含量的RPV模拟钢为研究对象，模拟钢经过880℃水淬和660℃调质处理后，在370℃长期时效不同时间，然后采用透射电镜（TEM），高分辨透射电镜（HRTEM）、能谱（EDS），原子探针层析技术（APT）和冲击试验等方法研究了时效后RPV模拟钢的显微组织，纳米富Cu相的析出过程以及晶体结构演化特点，界面上合金元素及杂质元素的偏聚特征以及纳米富Cu相的析出对韧脆转变温度的影响等，得出了以下主要结论：
（1）首次观察到纳米富Cu相在析出成核过程中Cu原子沿着α-Fe基体的{110}晶面以2层或3层为周期发生偏聚，并导致晶格畸变的各向异性，而后，富Cu区会在bcc结构的{110}晶面上发生切变形成了ABC/BCA/CAB/ABC排列的多孪晶9R结构。首次观察到同一个富Cu相中bcc，正交9R和单斜9R结构并存的现象，说明了这种结构演化过程的复杂性。最后富Cu相由9R结构转变为fcc或者fct结构。
（2）研究了RPV模拟钢中不同的溶质或杂质原子在晶界处的偏聚特征。确定了它们偏聚倾向由强到弱依次为C>P>Mo>Si>Mn>Ni，Cu在晶界处会出现贫化现象，C在晶界上偏聚的宽度最宽。证实了C和P在晶界偏聚存在竞争现象，观察到Si的偏聚与晶界的特性有关。
（3）观察到溶质或杂质原子在相界面处的偏聚特性与在晶界处的不同，Ni，Si和P元素会偏聚在α-Fe和渗碳体的相界面上， Mn，Mo和S原子会富集在渗碳体中，Cu被排除在渗碳体之外，且不会在相界面上偏聚。而在富Cu相与α-Fe的相界面处，Ni和Mn有明显的偏聚，C，P，Mo，Si倾向偏聚在相界面的α-Fe一侧，且偏聚的程度比晶界处的低。
（4）通过热时效模拟的办法证实了纳米富Cu相的析出确实会导致材料的韧脆转变温度（DBTT）升高，样品在370℃经过13200h时效后，析出纳米富Cu相的数量密度达到7.1×10~(22)m~(-3)，这时DBTT从-100℃上升到-45℃，提高了55℃，但热时效得到的纳米富Cu相的数量密度比中子辐照引起的低，并且材料的基体也没有受到中子辐照损伤，因而DBTT上升的幅度并不像中子辐照引起的那样高。
（5）用4%-硝酸酒精溶液作腐蚀液可以将小至3nm的富Cu相从α-Fe中萃取出来。在不同时效时间的样品中，观察到了不同尺寸、Cu含量有一定差别的bcc，9R或fcc结构的纳米富Cu相，它们在长大过程中的晶体结构转变与尺寸大小以及Cu含量之间没有严格的依赖关系。纳米富Cu相中都不同程度的含有Fe，Ni和Mn，但是这些纳米富Cu相仍为单相固溶体，而不像块体合金中那样是多相组织。
Nuclear power has the features of low pollution and high efficiency. It eases theenergy crisis, and reduces the carbon emissions at the same time. Reactor pressurevessel (RPV) is nonreplaceable major component of the pressurized water reactor(PWR) in power plants. RPVs are usually made of low alloy ferritic steels and A508class3(A508-Ⅲ) steel is one type of these materials. After long-term service underthe neutron irradiation, the RPV steel becomes embrittled and the shift in theductile-to-brittle transition temperature (DBTT) which is the main parameter used tomeasure the embrittlement degree of RPV increases. The irradiation-inducedembrittlement of RPV steel is presently the main impact factor of ensuring theoperation safety and assessing operation lifetime of nuclear power plants. Theembrittlement effect of RPV steel is mainly correlated with the formation of highnumber density Cu-rich nanophases induced by the crystal defects in theneutron-irradiated steel.
If the experiments were carried out in the way of neutron irradiation to investigatethe precipitation of Cu-rich nanophases in RPV steel, besides the high costs, it wouldbe very inconvenient to operate the experiments since the irradiated specimens havestrong radioactivity. The Cu-rich nanophases can also precipitate in RPV steelthermally aged at290℃if the content of residual Cu element is less than0.08wt.%,but it will take too much time more than20years. In order to reduce theexperimental period and simultaneously accelerate the precipitation of Cu-richnanophases, experiment was performed by using RPV model steel containing higherCu content than commercially available A508-Ⅲ steel. The specimens of RPVmodel steel were tempered at660℃for10h followed air cooling after heattreatment at880℃for30min and water quenching, then they were isothermallyaged at370℃for different time. Several techniques (such as conventional transmission electron microscopy, high resolution transmission electron microscopy,energy spectrum, atom probe tomography and so on) were used to investigate themicrostructure, the precipitation process and structural evolution of the Cu-richnanophases, the interfaces segregation of solute or impurity atoms as well as theeffect of the precipitation of Cu-rich nanophases on the DBTT in PRV model steelduring thermal aging at370℃temperature. The following conclusions can bedrawn:
(1) It is the first time to observe that the Cu atoms can segregate on the {110}planes of the α-Fe matrix in a period of two or three layers during the nucleationprocess of Cu-rich nanophase. The periodical segregation also causes the internalstress and the lattice distortion to be anisotropic. It is also observed that the Cu-richregions undergo a transformation from bcc structure to multi-twined9R structure bymeans of a shear along the {110} plane of bcc structure, while the interface betweenthe Cu-rich nanophase and the α-Fe matrix is coherent. It is firstly observed that thesame Cu-rich nanophase consists of bcc,9R orthorhombic structure and9Rmonoclinic structure segments. The coexistence of multi-structure within the sameCu-rich nanophase suggests that the structural evolution of Cu-rich nanophase is verycomplicated. Finally, the Cu-rich nanophases transformed to fcc or fct single structurefrom9R structure.
(2) The segregation of solute or impurity atoms at the grain boundaries wascharacterized. The sequence of segregation tendency for different atoms from strongto weak is C> P> Si> Mn> Mo> Ni, whilst Cu atoms were clearly depleted at thegrain boundaries. There is a competitive interaction between C and P atoms that thesegregation amount of P and C atoms is inversely correlated with each other. Si atomsalso segregate to the grain boundaries, but it depends on the characteristic of the grainboundaries. The segregation of Si atoms to some grain boundary is obvious, but itdoes not to others. The C segregation range at grain boundaries is the widest.According to the width of the composition profiles at the half intensity for different atoms at the grain boundaries, the segregation range of C atoms is1.5times widerthan that of Mn. Ni and Mo atoms.
(3) It is observed that the segregation characteristics of the solute or impurity atomsat the phase interfaces are different from that at the grain boundaries. Ni, Si, P atomssegregate on the interfaces between cementites and the α-Fe matrix, and Mn, Mo, Satoms enrich in the cementites. Cu atoms are ejected from the cementites, but the Cusegregation on the interface is not detected. Ni and Mn atoms evidently segregate tothe interfaces between the Cu-rich phase and the α-Fe matrix, while C, P, Mo, Siatoms prefer to segregate towards the α-Fe matrix near the interfaces, but theirsegregation amount at the interfaces of Cu-rich phase and the α-Fe matrix is less thanthat at the grain boundaries.
(4) The precipitation of the Cu-rich nanophases indeed can lead to the shift ofDBTT towards higher temperature for the RPV model steel by thermal aging. TheCu-rich nanophases precipitate on dislocations in the specimen aged at370℃for3000h, and the clusters become a little coarsened when the aging time is extended to13200h. For the specimens aged for1150h, Cu-rich nanophases were on thenucleation stage assessed by TEM as well as APT analysis, and they did not have aneffect on the DBTT of the RPV model steel. For the specimens aged for3000h,Cu-rich nanophases precipitated with an average equivalent diameter of1.5nm and anumber density of4.2×10~(22)m~(-3). and it results in the increase of the DBTT from-100℃to-60℃. For the specimens aged for13200h, Cu-rich nanophasesslightly coarsened to2.4nm of the average equivalent diameter, while the numberdensity is similar to that of the specimens aged for3000h. In this case the DBTTrose to-45℃. The Cu concentration in the α-Fe matrix for the specimen aged for13200h is still more than the limitation of Cu solubility in the α-Fe matrix at370℃.It means that the precipitation of Cu-rich nanophases does not reach the equilibriumstate. The precipitation of Cu-rich nanophases induced by thermal aging reveals asmaller impact on the DBTT than that by neutron irradiation. From the thermal aging aspect, the much lower number density of Cu-rich clusters and the absence of thedefects induced by neutron irradiation in the matrix could account for thisphenomenon.
(5) The Cu-rich precipitations with the diameter larger than3nm could beextracted from the α-Fe matrix by carbon replica using the etchant of4%nitric acidalcohol solution. As to the specimens aged for different time, a different crystalstructure of bcc,9R and fcc can be observed for Cu-rich nanophases with differentsize and different Cu contents, but the crystal structure of the Cu-rich nanophasesdoes not directly depend on the size and Cu content of them. The Cu-richnanophases contain Fe, Mn and Ni with varying degree while the Cu-richnanophases are all homogeneously solid solution determined by high resolutionlattice image, which is not like the multi-phases in the bulk materials ofCu-Fe-Mn-Ni alloys.
如果用中子辐照试验来研究RPV钢中纳米富Cu相的析出费用太高，实验操作也很不方便，而采用低温热时效的办法也可以使过饱和固溶的Cu以纳米富Cu相形式析出，但是时效时间过长。为了加速纳米富Cu相的析出，本工作以提高了Cu含量的RPV模拟钢为研究对象，模拟钢经过880℃水淬和660℃调质处理后，在370℃长期时效不同时间，然后采用透射电镜（TEM），高分辨透射电镜（HRTEM）、能谱（EDS），原子探针层析技术（APT）和冲击试验等方法研究了时效后RPV模拟钢的显微组织，纳米富Cu相的析出过程以及晶体结构演化特点，界面上合金元素及杂质元素的偏聚特征以及纳米富Cu相的析出对韧脆转变温度的影响等，得出了以下主要结论：
（1）首次观察到纳米富Cu相在析出成核过程中Cu原子沿着α-Fe基体的{110}晶面以2层或3层为周期发生偏聚，并导致晶格畸变的各向异性，而后，富Cu区会在bcc结构的{110}晶面上发生切变形成了ABC/BCA/CAB/ABC排列的多孪晶9R结构。首次观察到同一个富Cu相中bcc，正交9R和单斜9R结构并存的现象，说明了这种结构演化过程的复杂性。最后富Cu相由9R结构转变为fcc或者fct结构。
（2）研究了RPV模拟钢中不同的溶质或杂质原子在晶界处的偏聚特征。确定了它们偏聚倾向由强到弱依次为C>P>Mo>Si>Mn>Ni，Cu在晶界处会出现贫化现象，C在晶界上偏聚的宽度最宽。证实了C和P在晶界偏聚存在竞争现象，观察到Si的偏聚与晶界的特性有关。
（3）观察到溶质或杂质原子在相界面处的偏聚特性与在晶界处的不同，Ni，Si和P元素会偏聚在α-Fe和渗碳体的相界面上， Mn，Mo和S原子会富集在渗碳体中，Cu被排除在渗碳体之外，且不会在相界面上偏聚。而在富Cu相与α-Fe的相界面处，Ni和Mn有明显的偏聚，C，P，Mo，Si倾向偏聚在相界面的α-Fe一侧，且偏聚的程度比晶界处的低。
（4）通过热时效模拟的办法证实了纳米富Cu相的析出确实会导致材料的韧脆转变温度（DBTT）升高，样品在370℃经过13200h时效后，析出纳米富Cu相的数量密度达到7.1×10~(22)m~(-3)，这时DBTT从-100℃上升到-45℃，提高了55℃，但热时效得到的纳米富Cu相的数量密度比中子辐照引起的低，并且材料的基体也没有受到中子辐照损伤，因而DBTT上升的幅度并不像中子辐照引起的那样高。
（5）用4%-硝酸酒精溶液作腐蚀液可以将小至3nm的富Cu相从α-Fe中萃取出来。在不同时效时间的样品中，观察到了不同尺寸、Cu含量有一定差别的bcc，9R或fcc结构的纳米富Cu相，它们在长大过程中的晶体结构转变与尺寸大小以及Cu含量之间没有严格的依赖关系。纳米富Cu相中都不同程度的含有Fe，Ni和Mn，但是这些纳米富Cu相仍为单相固溶体，而不像块体合金中那样是多相组织。
Nuclear power has the features of low pollution and high efficiency. It eases theenergy crisis, and reduces the carbon emissions at the same time. Reactor pressurevessel (RPV) is nonreplaceable major component of the pressurized water reactor(PWR) in power plants. RPVs are usually made of low alloy ferritic steels and A508class3(A508-Ⅲ) steel is one type of these materials. After long-term service underthe neutron irradiation, the RPV steel becomes embrittled and the shift in theductile-to-brittle transition temperature (DBTT) which is the main parameter used tomeasure the embrittlement degree of RPV increases. The irradiation-inducedembrittlement of RPV steel is presently the main impact factor of ensuring theoperation safety and assessing operation lifetime of nuclear power plants. Theembrittlement effect of RPV steel is mainly correlated with the formation of highnumber density Cu-rich nanophases induced by the crystal defects in theneutron-irradiated steel.
If the experiments were carried out in the way of neutron irradiation to investigatethe precipitation of Cu-rich nanophases in RPV steel, besides the high costs, it wouldbe very inconvenient to operate the experiments since the irradiated specimens havestrong radioactivity. The Cu-rich nanophases can also precipitate in RPV steelthermally aged at290℃if the content of residual Cu element is less than0.08wt.%,but it will take too much time more than20years. In order to reduce theexperimental period and simultaneously accelerate the precipitation of Cu-richnanophases, experiment was performed by using RPV model steel containing higherCu content than commercially available A508-Ⅲ steel. The specimens of RPVmodel steel were tempered at660℃for10h followed air cooling after heattreatment at880℃for30min and water quenching, then they were isothermallyaged at370℃for different time. Several techniques (such as conventional transmission electron microscopy, high resolution transmission electron microscopy,energy spectrum, atom probe tomography and so on) were used to investigate themicrostructure, the precipitation process and structural evolution of the Cu-richnanophases, the interfaces segregation of solute or impurity atoms as well as theeffect of the precipitation of Cu-rich nanophases on the DBTT in PRV model steelduring thermal aging at370℃temperature. The following conclusions can bedrawn:
(1) It is the first time to observe that the Cu atoms can segregate on the {110}planes of the α-Fe matrix in a period of two or three layers during the nucleationprocess of Cu-rich nanophase. The periodical segregation also causes the internalstress and the lattice distortion to be anisotropic. It is also observed that the Cu-richregions undergo a transformation from bcc structure to multi-twined9R structure bymeans of a shear along the {110} plane of bcc structure, while the interface betweenthe Cu-rich nanophase and the α-Fe matrix is coherent. It is firstly observed that thesame Cu-rich nanophase consists of bcc,9R orthorhombic structure and9Rmonoclinic structure segments. The coexistence of multi-structure within the sameCu-rich nanophase suggests that the structural evolution of Cu-rich nanophase is verycomplicated. Finally, the Cu-rich nanophases transformed to fcc or fct single structurefrom9R structure.
(2) The segregation of solute or impurity atoms at the grain boundaries wascharacterized. The sequence of segregation tendency for different atoms from strongto weak is C> P> Si> Mn> Mo> Ni, whilst Cu atoms were clearly depleted at thegrain boundaries. There is a competitive interaction between C and P atoms that thesegregation amount of P and C atoms is inversely correlated with each other. Si atomsalso segregate to the grain boundaries, but it depends on the characteristic of the grainboundaries. The segregation of Si atoms to some grain boundary is obvious, but itdoes not to others. The C segregation range at grain boundaries is the widest.According to the width of the composition profiles at the half intensity for different atoms at the grain boundaries, the segregation range of C atoms is1.5times widerthan that of Mn. Ni and Mo atoms.
(3) It is observed that the segregation characteristics of the solute or impurity atomsat the phase interfaces are different from that at the grain boundaries. Ni, Si, P atomssegregate on the interfaces between cementites and the α-Fe matrix, and Mn, Mo, Satoms enrich in the cementites. Cu atoms are ejected from the cementites, but the Cusegregation on the interface is not detected. Ni and Mn atoms evidently segregate tothe interfaces between the Cu-rich phase and the α-Fe matrix, while C, P, Mo, Siatoms prefer to segregate towards the α-Fe matrix near the interfaces, but theirsegregation amount at the interfaces of Cu-rich phase and the α-Fe matrix is less thanthat at the grain boundaries.
(4) The precipitation of the Cu-rich nanophases indeed can lead to the shift ofDBTT towards higher temperature for the RPV model steel by thermal aging. TheCu-rich nanophases precipitate on dislocations in the specimen aged at370℃for3000h, and the clusters become a little coarsened when the aging time is extended to13200h. For the specimens aged for1150h, Cu-rich nanophases were on thenucleation stage assessed by TEM as well as APT analysis, and they did not have aneffect on the DBTT of the RPV model steel. For the specimens aged for3000h,Cu-rich nanophases precipitated with an average equivalent diameter of1.5nm and anumber density of4.2×10~(22)m~(-3). and it results in the increase of the DBTT from-100℃to-60℃. For the specimens aged for13200h, Cu-rich nanophasesslightly coarsened to2.4nm of the average equivalent diameter, while the numberdensity is similar to that of the specimens aged for3000h. In this case the DBTTrose to-45℃. The Cu concentration in the α-Fe matrix for the specimen aged for13200h is still more than the limitation of Cu solubility in the α-Fe matrix at370℃.It means that the precipitation of Cu-rich nanophases does not reach the equilibriumstate. The precipitation of Cu-rich nanophases induced by thermal aging reveals asmaller impact on the DBTT than that by neutron irradiation. From the thermal aging aspect, the much lower number density of Cu-rich clusters and the absence of thedefects induced by neutron irradiation in the matrix could account for thisphenomenon.
(5) The Cu-rich precipitations with the diameter larger than3nm could beextracted from the α-Fe matrix by carbon replica using the etchant of4%nitric acidalcohol solution. As to the specimens aged for different time, a different crystalstructure of bcc,9R and fcc can be observed for Cu-rich nanophases with differentsize and different Cu contents, but the crystal structure of the Cu-rich nanophasesdoes not directly depend on the size and Cu content of them. The Cu-richnanophases contain Fe, Mn and Ni with varying degree while the Cu-richnanophases are all homogeneously solid solution determined by high resolutionlattice image, which is not like the multi-phases in the bulk materials ofCu-Fe-Mn-Ni alloys.
引文
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[4] Miller M K, Russell K F, Sokolov M A, Nanstad R K. Atom probe tomography of radiation-sensitive characterization KS-01weld[J]. Journal of Nuclear materials,2003;320:177-183.
[5] Miller M K, Nanstad P K, Sokolov M A, Russell K F. The effects of irradiation, annealing andreirradiation on RPV steels[J]. Journal of Nuclear materials,2006;351:216-222.
[6] Miller M K, Russell K F. Embrittlement of RPV steels: An atom probe tomographyperspective [J]. Journal of Nuclear materials,2007;371:145-160.
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