ECAP加工与热处理对工业纯铁点蚀行为的影响

通过多道次等通道转角挤压(ECAP)和退火热处理,制备不同组织结构状态的超细晶工业纯铁,采用透射电镜观察微观组织结构特征,并用电化学极化和阻抗谱技术表征超细晶纯铁在含氯离子的钝化介质中点蚀行为。结果表明:随着ECAP加工道次增加,低道次形成的高位错密度板条状结构转变为低位错密度等轴晶;ECAP样退火热处理后,位错减少、大角度晶界增加。ECAP加工道次对纯铁自钝化性能影响不大,开路电位和极化电阻变化均较小;耐点蚀性能与加工道次有关,点蚀电位随加工道次先下降后升高;退火处理后自钝化性能和耐蚀性提高,开路电位、极化电阻和点蚀电位均明显增大。     

基于矫顽力与剩磁的铁磁性材料应力测量

铁磁性材料的磁滞回线代表其在外加磁场下的基本磁特性,磁滞回线反映的磁特性参数磁导率μ、矫顽力H_C、剩磁M_R能灵敏地反应铁磁性材料的微观组织结构。针对铁磁性材料受应力易发生形变的问题,该文研究铁磁性材料内部磁畴结构和所受应力的关系,利用应力引起的磁特性参数的变化确定材料所受的应力大小,基于U型磁轭的电磁检测原理,测量激励线圈中的电流值和感应线圈上的电压值,采集被测磁回路的磁滞回线并计算矫顽力、剩磁。结果表明:矫顽力数值会随拉力的增大而升高,剩磁随拉力的增大呈阶段性变化,利用矫顽力与剩磁可以实现铁磁性材料的受力分析。     

高能球磨FeCo+MnO的结构与磁性研究

用高能球磨采用两种方案制备了FeCo MnO体系,并用X射线衍射和振动样品磁强计对其结构和磁性质做了分析.发现采用直接氧化Mn而得到MnO的方法,所得体系的MnO较纯;而通过分解MnCO3得到MnO的体系,MnO纯度较低,有较多Mn3O4杂质,两种方法制备的FeCo MnO体系的矫顽力和剩磁比都比单纯FeCo体系的增加很多,且前一种方法比后一种方法制备的FeCo MnO体系的矫顽力和剩磁比较大.然后研究了球磨时间及退火处理对FeCo MnO体系矫顽力及剩磁比的影响,发现球磨时间为120h体系的矫顽力和剩磁比最大;经过退火处理后,体系的矫顽力和剩磁比都有较大幅度的增加.     

铂丝位错特性对标准铂电阻温度计稳定性影响的研究

铂丝的位错是影响标准铂电阻温度计性能稳定性的重要因素之一。从微观角度出发,借助X射线衍射(XRD)分析方法,开展了退火时间对铂丝位错密度影响的研究,并利用标准铂电阻温度计退火实验数据进行了验证。结果表明:实际用于标准铂电阻温度计直径为0.07mm的新制铂丝(纯度99.999%)平均位错密度随着退火时间呈指数减小,经过100h退火后位错密度从1012cm^-2下降到1011cm^-2,300h后其位错密度基本保持稳定;新制标准铂电阻温度计在退火前300h其水三相点电阻值明显减小,退火300h后水三相点值变化量小于3mK并趋于平稳,此结果从热处理时间上与铂丝位错实验结果基本吻合。研究结果为标准铂电阻温度计制作工艺的提升及计量检定规程的修订提供技术支撑     

基于位错密度分析的Ti-8Al-1Mo-1V钛合金片层组织在热轧及退火过程中的演变机制

采用金相(OM)、电子背散射衍射(EBSD)、透射电子显微镜(TEM)等手段研究了Ti-8Al-1Mo-1V钛合金片层组织在热轧及轧后退火过程中的组织演变规律及机制。研究结果表明:热轧及轧后退火难以实现片层α相的球化,仅能实现α相的连续化分布及β相的球化。热轧过程中位错密度无法有效累积是造成片层α相再结晶驱动力缺失的主要原因。同较粗的片状α相相比,在相同轧制力下,细小β相更易破断,并在随后的退火过程中实现扩散球化。根据分析,本工作提出了Ti-8Al-1Mo-1V钛合金片层组织热轧+退火过程中的组织演变机制。此外研究发现,Ti811钛合金片层组织在热轧过程中可形成织构指数为■的板织构。     

真空感应熔炼半导体用热轧NiCr靶微观组织和磁性能分析

采用真空感应熔炼方法制备了半导体用NiCr溅射靶,并对其开展不同变形量下的热轧,分析了NiCr合金受到热轧作用后发生的组织形态变化与磁性能改变。研究结果表明:NiCr合金中形成了呈现面心立方结构的镍基固溶体,合金受到热轧作用后发生了晶粒明显细化现象。随着热轧变形量的逐渐增大,(101)晶面择优取向程度先提高后减小,在热轧阶段组织晶粒发生了转动。随着热轧变形增加,观察到位错出现在晶粒内,部分区域发生了位错的相互缠结,晶粒内形成了小角度晶界。热轧后的试样在磁滞回线中心部位存在更多数量的磁滞回线,增大了矫顽力和剩余磁感应强度。随着热轧变形程度的提高,合金矫顽力Hc随之提高,获得更高磁透率,而剩磁Br先逐渐增大后减小,当热轧变形程度达到10%时,Br出现了迅速增大,之后Br不断下降。     

CGO硅钢初次再结晶组织及织构演变规律

对3%(质量分数)Si CGO硅钢冷轧板进行初次再结晶退火实验,设置不同的退火保温时间,将退火后的样品分别使用OM,TEM及EBSD进行分析,观察其微观组织、位错及织构分布,研究CGO硅钢初次再结晶过程中组织及织构的演变规律。结果表明:随着退火保温时间的延长,回复再结晶的程度增加,当保温时间延长至300s时,再结晶基本完成且呈现等轴晶状态,随着保温时间的延长,组织中位错密度降低。初次再结晶退火保温时间对初次再结晶织构分布有影响:随着保温时间的延长,{111}〈112〉和{110}〈112〉织构含量不断下降,{111}〈110〉织构的含量先减少后增加,立方及旋转立方组分基本保持不变,Goss织构组分逐渐增多。当保温时间较短时,晶粒取向差主要为小角度晶界并存在大量亚晶,随着保温时间的延长,大角度晶界逐渐增多。     

135°ECAP+旋锻变形工业纯钛的热稳定性研究

对经过135°ECAP+旋锻变形后的工业纯钛100,150,200,250,300,350,400,450℃和500℃下保温1h退火。采用透射电子显微镜(TEM)、扫描电子显微镜(SEM)、拉伸试验机及显微硬度仪等技术研究ECAP+旋锻变形工业纯钛退火后的组织与性能变化。结果表明:在400℃以下退火时,显微组织中位错密度降低,晶界逐渐清晰,变形组织未发生明显变化,材料的抗拉强度和显微硬度略有降低,伸长率增加不明显;在400℃以上退火时,随着退火温度的升高,发生再结晶,晶粒尺寸明显增大,平均晶粒尺寸约为5μm,材料的抗拉强度和显微硬度均出现明显降低,伸长率增加。拉伸断口表明,ECAP+旋锻变形退火后工业纯钛的拉伸断裂均为韧性断裂。随着退火温度的升高,韧窝尺寸变大,韧窝深度变深。     

CSP工艺热轧低碳钢板的强化机制

采用金相显微镜、H—800透射电镜和正电子湮没方法分析了CSP热轧低碳钢板金相组织、析出物形貌、尺寸、分布及位错密度。结果表明:CSP工艺热轧低碳钢板的晶粒较为细小,约为5.3μm;当累积变形量较小、变形温度较高时,析出物主要在晶界上,数量少见比较粗大,其尺寸大多大于150nm;当累积变形量较大、变形温度较低时,析出物主要在晶内,细小、弥散且数量较多,其尺寸大多为20～100nm,析出物主要为Al_2O_3、MnS或Cu_7S_4;随着累积变形量的增加,位错密度明显增加,终轧后轧件的位错密度约为6.35×10~(14)m~(-2)。晶粒细化、析出物弥散分布及位错密度增加是CSP工艺热轧低碳钢板强度高的决定因素。     

块状纳米晶Sm2Co17烧结磁体的研究

采用高能球磨和放电等离子烧结技术制备了致密纳米晶Sm2Co17烧结磁体,研究了粉末和烧结磁体的结构和磁性能.球磨粉末在低温退火(<1023K)时,主相为TbCu7结构;高温退火(>1023K)时,主相为Th2Zn17结构.退火温度从923K增加到1223K,粉末的矫顽力从0.99T下降到0.12T.烧结磁体也具有TbCu7结构,磁体平均晶粒尺寸约为35nm.室温时磁体的剩磁为0.65T,矫顽力达0.87T.烧结磁体具有较好的高温性能,573K时的剩磁为0.6T,矫顽力为0.32T.     

He+ 辐照对CLAM钢焊缝微观组织和性能的影响

在室温下用强度为70 keV的He⁺辐照CLAM钢焊缝,使用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和连续刚度纳米压痕技术(CSM)对其表征,研究了He⁺辐照对CLAM钢焊缝的微观组织和性能的影响。结果表明,随辐照剂量的增大焊缝表面黑色孔洞的尺寸增大、密度提高;辐照剂量为1×10¹⁷ ions·cm^-2时,在两种焊缝中形成的位错环的尺寸分别约为18.97 nm、15.73 nm,数密度分别约为2.24×10²¹ m^-3、1.78×10²¹ m^-3,氦泡引起的辐照肿胀率分别约为1.7%和0.4%;辐照缺陷(位错环、氦泡)导致的辐照硬化率分别为49.0%和29.9%。与焊态焊缝相比,调质处理态焊缝的辐照损伤较弱,在一定程度上表明经调质处理后焊缝的抗辐照性能有所提高。     

挤压态6013-T4铝合金在动态冲击载荷下的变形行为及其微观机理

使用霍普金森压杆试验装置进行挤压态6013-T4铝合金的室温动态压缩实验,应变速率为1×10³~3×10³ s^-1。结果表明,6013-T4铝合金在动态压缩过程中表现出明显的应变硬化和正应变速率敏感性;随着应变和应变速率的提高位错密度增大,在高应变速率和大应变量变形后试样的位错塞积显著。在相同的变形条件下0°方向试样的应力总是最高,而45°方向试样的应力最低。挤压态6013-T4合金的主要织构类型为{112}<111>和{110}<111>。对于{112}<111>织构,0°、45°和90°方向的最大施密特因子分别为0.27、0.49和0.41。对于{110}<111>织构,最大施密特因子分别为0.27、0.43和0.41。0°方向的施密特因子最小,使该方向的应力水平较高。在相同的应变速率和应变量条件下动态压缩变形时,0°方向试样的位错密度更高。在冲击件的材料选择和结构设计中有必要考虑材料的应变速率敏感性、力学性能各向异性以及微观组织的演变。     

Si3N4/FePd/Si3N4薄膜的晶体结构和磁性能研究

采用磁控溅射的方法制备了Si₃N₄/FePd/Si₃N₄三层膜, 研究了非磁性材料Si₃N₄作为插入层对磁记录FePd薄膜结构与磁性能的影响。结果表明, 热处理后Si₃N₄分布在FePd纳米颗粒之间, 抑制了FePd晶粒的生长, 与纯FePd薄膜相比, Si₃N₄/FePd/Si₃N₄薄膜的颗粒明显得到细化; 通过添加Si₃N₄层, FePd薄膜的晶体学参数c/a从0.960减小到0.946, 表明Si₃N₄可以有效促进FePd薄膜的有序化进程, 同时提升了矫顽力和剩磁比, 分别提高到249 kA/m、0.86; 随着600℃退火时间的进一步延长, 添加Si₃N₄的薄膜磁性没有迅速下降, 在较宽的热处理时间范围内磁性能保持在比较高的水平, 提高了抗热影响的能力。Si₃N₄作为插入层对FePd薄膜的磁性能具有较大的提升作用, 这对磁记录薄膜的发展具有重要意义。     

氢气氛退火对硅上低温外延制备的硅锗薄膜性能的影响

采用反应型热化学气相沉积系统在硅(100)衬底上外延生长富锗硅锗薄膜。四氟化锗作为锗源, 乙硅烷作为还原性气体。通过设计表面反应, 在低温条件下(350℃)制备了高质量的富锗硅锗薄膜。研究了氢退火对低温硅锗外延薄膜微结构和电学性能的影响。结果发现退火温度高于700℃时, 外延薄膜的表面形貌随着退火温度的升高迅速恶化。当退火温度为650℃时, 获得了最佳的退火效果。在该退火条件下, 外延薄膜的螺旋位错密度从3.7×10⁶ cm^-2下降到4.3×10⁵ cm^-2, 表面粗糙度从1.27 nm下降到1.18 nm, 而外延薄膜的结晶质量也有效提高。霍尔效应测试表明, 经退火处理的样品载流子迁移率明显提高。这些结果表明, 经过氢退火处理后, 反应型热化学气相沉积制备的低温硅锗外延薄膜可以获得与高温下硅锗外延薄膜相比拟的性能。     

Aging effect on coercivity of iron oxide thin films

Changes in magnetic properties for Fe_3-x□_x O₄ (x: oxidation degree) thin films made by reactive sputtering and subsequent heat treatments have been examined under room temperature aging and constant temperature annealing. Aging causes variations in coercivity of insufficiently oxidized films which have a specific resistance of less than 1×10¹ Ω·cm, while the coercivity of γ-Fe₂O₃ (x=1/3) did not change. This phenomenon did not depend on additive elements or preparation method. Other magnetic properties such as saturation magnetization, residual magnetization, squareness ratio and coercive squareness, were not affected by aging for any Fe_3-x □_xO₄ composition. The activation energy for a coercivity change is 0.72-0.95 eV near room temperature for films with a specific resistance below 1×10¹ Ω·cm. It was confirmed that only the coercivity varied at 20°C, while both coercivity and the degree of oxidation changed with annealing at 100°C     

n型SnS热电材料的制备与性能研究

SnS由低毒、廉价、高丰度的元素组成, 在热电研究领域受到广泛关注。采用机械合金化(MA)结合放电等离子烧结(SPS)工艺制备了n型SnS_1-xCl_x(x=0, 0.02, 0.03, 0.04, 0.05, 0.06)多晶块体热电样品, 并研究了Cl^-掺杂量对SnS物相、微观结构以及电热输运性能的影响。结果表明: Cl^-的引入会提高电子浓度, 使SnS由本征p型转变为n型半导体。随着Cl^-掺杂量的增加, n型SnS半导体室温下的霍尔载流子浓度从6.31×10¹⁴ cm^-3 (x=0.03)增加到7.27×10¹⁵cm^-3 (x=0.06)。x=0.05样品在823 K取得最大的电导率为408 S·m^-1, 同时具有较高的泽贝克系数为-553 μV•K^-1, 使其获得最大功率因子为1.2 μW·cm^-1·K^-2。Cl^-的掺入会引入点缺陷, 散射声子, 使晶格热导率κ_lat由0.67 W·m^-1·K^-1(x=0)降至0.5 W·m^-1·K^-1 (x=0.02)。x=0.04样品在823 K获得了最大ZT为0.17, 相比于x=0样品(ZT~0.1)提高了70%。     

Magnetic Hysteresis Loop Technique as a NDE Tool for the Evaluation of Microstructure and Mechanical Properties of 2.25Cr–1Mo Steel

This study intends to understand the effect of short-term overheating on microstructure modifications, and variation in mechanical and magnetic properties of boiler tubes. It is based on the hypothesis that short-term overheating on boiler tubes leads to microstructural changes degrading their mechanical properties, thus resulting in their failure. As part of this study, fresh 2.25Cr–1Mo boiler tube samples were heat treated in the range of 700–950 \(^{\circ }\hbox {C}\). Magnetic hysteresis loop (MHL) measurements were carried for the non-destructive evaluation (NDE) of the mechanical properties that get altered due to microstructural modifications. For comparison, MHL was also carried out on a service-exposed boiler tube, which had failed due to short-term overheating. The magnetic parameters were correlated with the change in microstructure and micro-hardness of the samples. A decrease in coercivity, remanence, maximum induction and micro hardness were found at the lower soaking temperatures, due to: easy magnetic domain wall and dislocation motions for the stress relaxation; annihilation and recovery of dislocations; increase in inter carbide distance; and the decrease in the number density of carbides for the coarsening of carbides. A subsequent increase in coercivity, remanence and maximum inductions along with hardness are due to the nucleation and growth of fresh bainitic phase, obstructing the magnetic domain wall and dislocation motion. A drastic decrease in coercivity for the service-exposed tube is due to the transformation of MX type carbides to \(\hbox {M}_{23}\hbox {C}_{6}\) type and accumulation of such carbides at the grain boundaries along with the decrease in number density of the carbides. The presence of scale has less effect on the coercivity, but its demagnetizing effect largely decreases the remanence and maximum induction. The results of the study show that the MHL can be a suitable NDE technique for the evaluation of change in microstructure and degradation of mechanical properties in power plant steels.     

The microstructure and magnetic properties of NdFeB magnets directly solidified at a low cooling rate

Nd_12.5Fe₈₂B_5.5 ribbons have been prepared by a melt spinning technique at a wheel speed ranging from 5 to 22 m/s. It was found that the wheel speed v_R dramatically influences the microstructure and magnetic properties of the ribbons. At an optimized v_R, a structure with single-phase Nd₂Fe₁₄B and an enhanced coupling between grains give rise to excellent magnetic properties. For example, the coercivity, remanence ratio, and maximum energy product of the best sample quenched at a wheel speed of 13 m/s are 1227.4 kA/m, 0.76, and 182.6 kJ/m³, respectively. In comparison with the samples from under- and over-quenched conditions and all the samples with annealing, the as-quenched sample fabricated at the optimized wheel speed has the best magnetic properties.     

Analysis of strain rate dependence of tensile elongation for a mechanical milling Al–1.1Mg–1.2Cu alloy tested at 748 K from a dislocation dynamics viewpoint

Tensile deformation was carried out for a mechanically milled and thermo-mechanically treated Al–1.1Mg–1.2Cu (at.%) alloy at 748 K and three nominal strain rates of 10⁻³, 10⁰, and 10² s⁻¹. Despite the prevailing belief that superplasticity occurs by grain boundary sliding which requires slow strain rates at high temperatures, the maximum elongation was observed at the intermediate strain rate of 10⁰ s⁻¹, neither at the lowest nor the highest strain rates. In order to explain this phenomenon, the true stress–true strain behaviors at these three nominal strain rates were analyzed from a viewpoint of dislocation dynamics by computer-simulation with four variables of the thermal stress component σ*, dislocation immobilization rate U, re-mobilization probability of unlocked, immobile dislocations Ω and dislocation density at yielding ρ₀. It can then be concluded that the large elongation (>400% in nominal strain) at the intermediate strain rate is produced by a combination of a very large Ω and a moderate U, resulting in a large strain rate sensitivity m value.     

A Low-Field Scaling Rule of Minor Hysteresis Loops in Plastically Deformed Steels

A scaling rule of magnetic minor hysteresis loops at low applied fields has been examined in plastically deformed low carbon steel and pure Ni. It was found that a power law between hysteresis loss and remanence of a minor loop holds true over the wide range of magnetization from the very low to intermediate range unlike the well-known Steinmetz law. The power-law exponent was an almost constant value of 1.35 being independent of the types of magnetic materials, the level of plastic deformation, and sample shape. The coefficient of the scaling rule increases with deformation and is in linear proportion to coercivity. This behavior was qualitatively explained on the basis of the Rayleigh law and NÉel theory.