Skutterudite类化合物晶粒长大规律和放电等离子体烧结的研究

用熔融-退火-放电等离子体烧结法(SPS)制备了晶粒尺寸均匀致密度高的La0.75Fe3CoSb12热电合金.研究了退火时间和温度对skutterudite合金晶粒长大的影响,晶粒生长动力学指数n=2.7,表观生长激活能Q=381±30 kJ/mol.晶粒长大主要受扩散机制控制. SPS的致密度随烧结时间的延长和温度的升高而增加, SPS后微观组织的观察表明,通过控制退火温度可有效地控制合金最终的晶粒尺寸.     

不同均匀化退火时1235铝的晶粒长大动力学研究

研究了不同均匀化退火时1235铝晶粒长大过程。结果表明:退火温度不同,晶粒长大的速度就不同,当退火温度下降至440℃后,晶粒长大的速度有所下降。基于线性拟合求得了540、440℃下的晶粒生长动力学方程。求得了1235铝的晶粒长大激活能,其值为245.58kJ/(mol·K),它比纯铝的晶界自扩散激活能要高。金属中的杂质和合金元素对晶粒长大有阻碍作用,因而完成晶粒长大过程需要更大的驱动力。     

W17.9Ni65.6B13.5V3非晶合金的非等温晶化动力学研究

采用单辊急冷法制备了W17.9Ni65.6B13.5V3非晶薄带,并用X射线衍射(XRD)和示差扫描量热分析仪(DSC)研究了该非晶合金的变温晶化动力学。结果表明：玻璃转变温度Tg、晶化起始温度Tx和晶化峰值温度Tp均随着升温速率的增加而提高,具有明显的动力学效应;利用Kissinger方程和Ozawa方程求出的W17.9Ni65.6B13.5V3非晶合金的晶化激活能Ex分别达456.9kJ/mol和471.1kJ/mol,非晶合金具有较强的热稳定性;利用Kissinger方程和Ozawa方程计算得到的晶化激活能Ex均小于晶体长大激活能Ep,表明形核过程比晶粒长大过程更容易,该非晶合金在一定条件下退火容易获得超细晶粒组织。     

退火处理对TA15合金晶界取向差演化特性的影响

利用背散射电子衍射(EBSD)及透射电子显微镜(TEM)技术研究TA15合金不同温度退火后晶界取向差变化情况.结果表明,800 ℃退火处理有少量小角晶界转化为大角晶界;退火温度提高到950 ℃,大角晶界分数大幅度增加;小角晶界转化为大角晶界的平均激活能为151.4 kJ/mol,等于α钛的自扩散激活能,说明了小角晶界向大角晶界转变是由钛原子的自扩散控制;TEM观察结果表明,800 ℃退火处理后亚晶界变为具有六方网络的位错网络,950 ℃退火处理则得到大量的等轴晶.     

往复挤压ZK60合金的低温准超塑性(英文)

通过2道次往复挤压制备细晶ZK60合金,在443~523K和初始应变速率为3.310-4~3.310-2s-1的范围内测试合金的低温超塑性。结果表明:往复挤压ZK60合金的平均晶粒尺寸约为5.0m,分布于基体内的破碎二次相颗粒和沉淀颗粒尺寸分别为不大于175nm和50nm。该合金具有低温准超塑性,在523K和3.310-4s-1应变速率下伸长率最大,为270%;在443和473K时,应变速率敏感系数m小于0.2;在523K时m为0.42。当温度不高于473K和523K时,超塑性变形激活能分别不高于63.2kJ/mol和110.6kJ/mol。当低于473K时,主要的超塑性流变机制为晶内滑移;在523K时,主要的超塑性变形机制为晶界滑移,由晶界扩散控制的位错蠕变为主要的兼容机制。     

固溶处理对GH4169合金组织与性能的影响

研究了热处理温度和保温时间对GH4169合金晶粒长大规律和硬度的影响.结果表明,δ相对晶粒长大有显著阻碍作用,在低于δ相完全溶解温度热处理时,未溶解的δ相使晶粒长大缓慢;在高于δ相完全溶解温度热处理时,合金为单相奥氏体组织,晶粒随温度的升高迅速长大.晶粒长大动力学表明:在热处理温度高于1050℃时的晶粒长大激活能为157.6kJ/mol,晶粒长大机理为Ni基合金的晶界扩散过程所控制,同时也建立了相应的晶粒长大动力学方程.     

软磁锰锌铁氧体的晶粒生长动力学实验分析

用共沉淀相转化法合成出的纳米锰锌铁氧体粉体经柠檬酸进行表面处理,压制成环型后经两步烧结得到烧结样品.用XRD、SEM以及VSM等方法对烧结样品进行了表征,并用球模型烧结方程探讨了烧结过程中的晶粒生长机制,结果表明锰锌铁氧体的晶粒生长指数,n≈2,表观生长激活能Q=71.14 kJ/mol,由此可知锰锌铁氧体在烧结过程中的晶粒生长主要受晶界迁移机制控制.当烧结温度为1000℃时,锰锌铁氧体样品已达到理论密度的94%,其磁性能较好.     

大塑性变形制备的非晶镍钛形状记忆合金的晶化(英文)

局部包套压缩大塑性变形能够实现镍钛形状记忆合金的完全非晶化,其中少量残留的纳米晶相分布在非晶基体上。研究非晶镍钛合金在573、723和873 K退火条件下的晶化机制。采用约翰逊-迈尔方程描述非晶镍钛合金的晶化动力学行为。在573和723 K的退火条件下,可以获得具有完全纳米晶相的镍钛形状记忆合金,在该纳米晶镍钛形状记忆合金中,马氏体相变由于晶界的约束而受到了抑制。在873 K的退火条件下,非晶镍钛合金的晶化产生了晶粒粗大的镍钛形状记忆合金样品。在室温条件下的粗晶镍钛样品中,可以观察到马氏体复合孪晶,而且发现马氏体孪晶在晶界优先形核,并且向两个不同的晶粒内部长大。局部包套压缩大塑性变形结合后续退火工艺为制备纳米晶镍钛形状记忆合金提供了一种新的途径。     

双脉冲电沉积纳米晶Ni-CeO2复合镀层的微观结构及其高温抗氧化性能

在超声波振荡环境下,用双脉冲电源在Watt-Ni电解液体系中电沉积了纳米晶Ni CeO₂复合镀层,采用E-S:EM,TEM和XRD对镀层的形貌,微观结构及相组成进行分析;通过循环氧化增重曲线和DSC曲线,比较研究了纯Ni镀层和NiCeO₂复合镀层的高温抗氧化性能与热稳定性.结果表明,超声波振荡能有效抑制纳米颗粒在镀液中的团聚;添加20 g/L CeO₂,可使Ni晶粒细化;在873 K空气中退火处理2 h,复合镀层中的CeO₂沿裂纹扩展间隙处析出并形成含有稀土元素的弥散相,可起到钉扎晶界和阻止热裂纹萌生的作用.晶界作为Ni的快速扩散通道,促进稀土弥散相沿晶界析出并形成连续的致密氧化膜,能有效抑制O与Ni原子在氧化膜中互扩散,从而降低镀层的氧化速率.通过测定不同升温速率下镀层DSC曲线的吸热峰对应温度,由Kissinger方程求得Ni CeO₂复合镀层中Ni晶粒长大的表观活化能为243.3 kJ/mol,明显高于纯Ni的晶粒长大表观活化能（159.2 kJ/mol）,吸热峰对应温度也较纯Ni镀层提高约130 K,因此Ni-CeO₂复合镀层具有更高的热稳定性.     

固溶处理对GH4169合金组织与性能的影响

研究了热处理温度和保温时问对GH4169合金晶粒长大规律和硬度的影响。结果表明，δ相对晶粒长大有显著阻碍作用，在低于δ相完全溶解温度热处理时，未溶解的δ相使晶粒长大缓慢；在高于δ相完全溶解温度热处理时，合金为单相奥氏体组织，晶粒随温度的升高迅速长大。晶粒长大动力学表明：在热处理温度高于1050℃时的晶粒长大激活能为157．6kJ／mol，晶粒长大机理为Ni基合金的晶界扩散过程所控制同时也建立了相应的晶粒长大动力学方程。     

Thermal stability of nanocrystalline in surface layer of magnesium alloy AZ91D

Isothermal and isochronal annealing was conducted to study the thermal stability of the nanocrystalline in the surface layer of Mg alloy AZ91D induced by high-energy shot peening(HESP) .Field emission scanning electron microscope(FESEM) and X-ray diffractometer were used to characterize the microstructure.Results showed that nanocrystalline produced by HESP on the surface layer of the magnesium alloy AZ91D was 60-70 nm on average.The nanocrystalline could remain stable at about 100℃,and grew up slowly between 100℃ and 200℃.When the annealing temperature reached 300℃,the growth rate of the nanocrystalline increased significantly.The kinetic coefficient n of the nanocrystalline growth was calculated to be 2-3 and the grain growth activation energy Q=39.7 kJ/mol,far less than the self-diffusion activation energy of magnesium atoms in the coarse polycrystalline material.     

Thermal stability of nanocrystalline layer prepared by surface mechanical attrition in 0Cr18Ni9Ti stainless steel

By means of surface mechanical attrition (SMA), a nanostructured surface layer was formed on a 0Cr18Ni9Ti austenite stainless steel plate. A strain-induced martensite transformation was observed during SMA treatment, and a single magnetic martensite phase layer with thickness of about 30 μm was gotten. The grain growth and phase transformations in the nanocrystalline layer are investigated during heating. The grain growth exponent for nanocrystalline polycrystalline steel is estimated. The kinetics mechanism governing the grain growth in the nanocrystalline layer is discussed. The martensite in the surface layer is quite stable and the temperature at which the reverse transformation of martensite to austenite starts during heating is about 500 ℃.     

Diffusion of chromium in nanocrystalline iron produced by means of surface mechanical attrition treatment

By means of surface mechanical attrition treatment (SMAT) to a pure iron plate, a nanometer-grained surface layer without porosity and contamination was fabricated. The average grain size in the top surface layer (of 5 μm thick) is about 10–25 nm, and the grain size stability can be maintained up to 653 K. Cr diffusion kinetics in the nanocrystalline Fe phase was measured by using second ion mass spectrometry within a temperature range of 573–653 K. Experimental results showed that diffusivity of Cr in the nanocrystalline Fe is 7–9 orders of magnitude higher than that in Fe lattice and 4–5 orders of magnitude higher than that in the grain boundaries (GBs) of α-Fe. The activation energy for Cr diffusion in the Fe nanophase is comparable to that of the GB diffusion, but the pre-exponential factor is much higher. The enhanced diffusivity of Cr may originate from a large volume fraction of non-equilibrium GBs and a considerable amount of triple junctions in the present nanocrystalline Fe sample processed by means of the SMAT technique.     

Grain growth and thermal stability of nanocrystalline Ni–TiO2 composites

The grain growth and thermal stability of nanocrystalline Ni–TiO₂ composites were systematically investigated. The nanocrystalline Ni–TiO₂ composites with different contents of TiO₂ were prepared via electroplating method with the variation of TiO₂ nano-particles concentration. The effect of TiO₂ content on the grain size, phase structure and microhardness was investigated in detail. The corresponding grain growth and diffusion mechanisms during the heating process were also discussed. The optimal microhardness of HV₅₀ 270 was achieved for the composite with addition of 20 g/L TiO₂ nano-particles after annealing at 400 °C for 90 min. The calculation of the activation energy indicated that lattice diffusion dominated at high temperatures for the nanocrystalline Ni–TiO₂ composites. It was indicated that the increase of TiO₂ nano-particles content took effect on restricting the grain growth at high temperatures by increasing the grain growth activation energy.     

Pressure-composition-isotherm behavior of nano-/amorphous Mg<Subscript>2</Subscript>NiH<Subscript>x</Subscript>

It has recently been shown that the hydriding properties of the nanocrystalline metal hydrides are far superior to those of the polycrystalline ones. Especially in the case of the Mg-based hydrogen storage alloys, nanostructural modifications have been studied for the purpose of improving their hydrogenation kinetics. In previous studies, I reported on the successful fabrication of Mg₂NiH_x from Mg and Ni chips with hydrogen induced mechanical alloying (HIMA). Observation of the microstructure showed that the synthesized particles (processed with a 66:1 ball to chips mass ratio and 96 hr HIMA) are composed of amorphous and nanocrystalline composite phases with a grain size of less than 10 nm. The aim of the present work was to examine the hydriding/dehydriding behavior of nanocrystalline metal hydrides using a Sieverts type automatic pressure-composition-isotherm (PCI) apparatus at 393, 423, 453, 483, 513 and 543 K. The specimen was characterized by X-ray diffraction after PCI measurement. The influence of hydrogenation behavior on the phase transition of nano-/amorphous Mg₂Ni is a key factor in commercial application. The particles synthesized at 66:1 BCR and 96 hr HIMA revealed a good hydrogen capacity of 2.25 mass% at 483 K.     

Thermal Stability of Nanocrystalline AZ31 Magnesium Alloy Fabricated by Surface Mechanical Attrition Treatment

A nanocrystalline layer(NL) was fabricated on the surface of AZ31 magnesium(Mg) alloy sheet by surface mechanical attrition treatment(SMAT). The microstructure of the Mg alloy was characterized by optical microscopy,X-ray diffraction and microhardness test. The results showed that both the microstructure and microhardness of AZ31 Mg alloy sheet after SMAT revealed a gradient distribution along depth from surface to center. The thermal stability of the NL was investigated through characterizing the microstructure evolution during the post-isothermal annealing treatment within the temperature range from 150 to 250 ℃. The NL exhibits a certain degree of thermal stability below 150 ℃, while it disappears quickly when annealing at the temperature range of 200–250 ℃. The grain growth kinetics of the nanocrystalline of AZ31 Mg alloy induced by SMAT was investigated. The activation energy of nanocrystalline AZ31 Mg alloy was obtained with a value of 92.8 k J/mol.     

Ordering and grain growth in nanocrystalline Fe75Si25 alloy

The grain growth and ordering behaviors in nanocrystalline Fe₇₅Si₂₅ powders produced by mechanical alloying was studied. In the temperature range 573–703 K, the disordered α-Fe(Si) showed only limited growth with a small activation energy of 32.3 kJ mol⁻¹. However, in the range 773–853 K ordering to DO₃ structure occurred accompanied by a sharp increase in average grain size to a maximum value that depended on the temperature. A grain growth model available in the literature for nanocrystalline materials yielded a good fit to the experimental data. Activation energy of 278.9 kJ mol⁻¹ determined using this model for grain growth is similar to that for lattice diffusion of Si in DO₃ Fe₃Si. The reason for the concurrence of ordering and grain growth is attributed to the Si desegregation at grain boundaries upon ordering transformation. The levels of segregation are estimated from lattice parameter measurements.     

Synthesis and grain growth kinetics of in-situ FeAl matrix nanocomposites （ Ⅱ ）： Structural evolution and grain growth kinetics of mechanically alloyed Fe-Al-Ti-B composite powder during heat treatment

Morphological changes, structural evolutions and grain growth kinetics of mechanically alloyed（MAed） Fe50Al50, Fe42.5Al42.5Ti5B10 and Fe35Al35Ti10B20 （mole fraction, %） powders were investigated by XRD and SEM, when being isothermally annealed at 1 073-1 373 K. The effect of different Ti and B addition on the grain growth of FeAI phase was also discussed. The results show that the nanocrystalline FeAI and in-situ TiB2/FeAl nanocomposite powders can be synthesized by subsequent heat treatment. Besides the relaxation of crystal defects and lattice stress, the transformation from Fe-based solid solution into B2-FeAl and TiB2 occurs upon heating of the MA-processed alloys. Although the grain growth takes place, the grain sizes of both FeAl and TiB2 are still in nanometer scale. The activation energies for the nanocrystalline FeAl growth in the three alloys are calculated to be 534.9, 525.6 and 1 069.6 kJ/mol respectively, according to kinetics theory of nanocrystalline growth. Alloys with different TiB2 contents exhibit unequal thermal stability. The presence of higher content TiB2 plays significant role in the impediment of grain growth.     

Synthesis and grain growth kinetics of in-situ FeAl matrix nanocomposites (Ⅱ): Structural evolution and grain growth kinetics of mechanically alloyed Fe-Al-Ti-B composite powder during heat treatment

Morphological changes, structural evolutions and grain growth kinetics of mechanically alloyed(MAed) Fe50Al50, Fe42.5Al42.5Ti5B10 and Fe35Al35Ti10B20 (mole fraction, %) powders were investigated by XRD and SEM, when being isothermally annealed at 1 073-1 373 K. The effect of different Ti and B addition on the grain growth of FeAl phase was also discussed. The results show that the nanocrystalline FeAl and in-situ TiB2/FeAl nanocomposite powders can be synthesized by subsequent heat treatment. Besides the relaxation of crystal defects and lattice stress, the transformation from Fe-based solid solution into B2-FeAl and TiB2 occurs upon heating of the MA-processed alloys. Although the grain growth takes place, the grain sizes of both FeAl and TiB2 are still in nanometer scale. The activation energies for the nanocrystalline FeAl growth in the three alloys are calculated to be 534.9, 525.6 and 1 069.6 kJ/mol respectively, according to kinetics theory of nanocrystalline growth. Alloys with different TiB2 contents exhibit unequal thermal stability. The presence of higher content TiB2 plays significant role in the impediment of grain growth.