化学沉淀法制备纳米Al2O3粉体中的反团聚研究

以工业用ＮＨ４Ａｌ（ＳＯ４）２．１２Ｈ２Ｏ和ＮＨ４ＨＣＯ３为原料，采用化学沉淀法制备纳米Ａｌ２Ｏ３粉体。研究了ｐＨ值、乙醇、表面活性剂等因素对Ａｌ２Ｏ３粒子尺寸的影响，并探讨了几种反团聚的机理及效果。     

In situ EELS study of dehydration of Al(OH)₃ by electron beam irradiation

The dehydration of Al(OH)₃ by an electron beam has been investigated using the time-dependent electron energy-loss spectroscopy (EELS) technique. Based on an analysis of low-loss EELS, Al L₂₃ and O K-edge, it is found that the processes are initially induced by the loss of H, followed by sputtering of O, which induce local structural changes. Some of the octahedrally coordinated Al transfer to tetrahedrally coordinated Al. The time-dependent O K-edge shows that the pre-edge peak in the O K-edge of Al(OH)₃ is induced by the formation of unpaired O, rather than an intrinsic feature of the OH bond.     

稀土强韧化陶瓷刀具材料的研制

研制出一种稀土钇强韧化Al2O3/Ti(C,N)新型陶瓷刀具材料,并对其力学性能和切削性能作了研究,表明稀土钇的适量添加能有效改善Al2O3/Ti(C,N)陶瓷刀具材料的力学性能,其抗变强度和断裂专访性分别达到1010MPa和6.1MPam^1/2。大量的切削实验表明,在切削淬硬45钢时,该刀具材料不仅具有良好的耐磨性能。而且具有较好的抗破损性能,其抗破损性能比相应不含稀土钇的Al2O3/Ti(C,N)陶瓷刀具材料高约20%。     

激光熔覆原位自生Ti-Al-Si复合涂层的微观组织和高温抗氧化性能

为提高钛合金的高温抗氧化性能,采用激光熔覆原位自生技术,在TC4钛合金表面自行设计并制备了原子百分比为Ti∶Al∶Si=41∶41∶18和Ti∶Al∶Si=35∶35∶30的两种涂层。通过XRD、OM、SEM表征了涂层的微观组织和物相组成;借助管式电阻炉测试了涂层和基体试样在800℃×24h×5次循环氧化条件下的高温抗氧化性能;结合氧化增重和氧化动力学曲线分析了涂层的高温抗氧化机理。结果表明,涂层主要由Ti5Si3、Ti7Al5Si12、Ti3Al、TiAl和TiAl3等物相组成。涂层中没有出现一般激光熔覆所产生的外延生长柱状晶组织,全部为细小等轴晶。在800℃×24h×5次循环氧化条件下,TC4基材单位面积的氧化增重约为35.1mg·cm-2,涂层的约为2.8mg·cm-2和3.3mg·cm-2。两种涂层的高温抗氧化性能较钛合金基材分别提高了12.5倍和10.6倍。激光熔覆原位自生Ti-Al-Si复合涂层能明显改善TC4钛合金的高温抗氧化性能。涂层抗氧化性改善的机理,一方面是表面生成了连续致密的TiO2、Al2O3、SiO2氧化层,阻碍了氧扩散;另一方面是提高了氧化层的黏附性,使氧化层不易从涂层表面剥落,对涂层未氧化部分起到了很好的保护作用。     

微米硬质相对相变增韧陶瓷刀具材料的影响

本文分别研究了微米TiC和微米TiN对陶瓷刀具材料Al2O3-3Y-ZrO2微观结构和力学性能的影响。结果表明,添加微米TiC后,陶瓷刀具材料的断裂韧度略有下降。添加微米TiN的陶瓷刀具材料A5Nm20Z在烧结温度为1650℃、烧结压力为30MPa和保温时间为30min时的力学性能最好,抗弯强度、断裂韧度和维氏硬度分别为845.14MPa、4.87MPa·m1/2和16.40GPa。     

Characteristics of Sputter-deposited Gadolinia-doped Ceria Thin Films on Al2O3/SiO2/Si Systems

Metal oxide films prepared by thin film technology have been reported for the potential applications on thin solid electrolyte layers for solid oxide fuel cells(SOFCs). Gadolinia-doped ceria(GDC) thin films and Al2O3 layers on SiO2/Si substrates are successively deposited by RF reactive magnetron sputtering from a cerium-gadolinium (90:10 at.%) alloy target and Al target in O2/Ar gas mixture and then perform post-thermal treatments at 300-700 ℃ and 900 ℃ for 2 h, respectively. Materials characteristics and chemical compositions of GDC films and Al2O3 layers are investigated by X-ray photoelectron spectroscopy(XPS), cross-sectional scanning electron microscopy(SEM), X-ray diffraction(XRD), and atomic force microscopy(AFM). Stoichiometric Al2O3 layers with polycrystalline structures are firstly prepared onto SiO2/Si substrates. A cubic fluorite structure with columnar crystallites of GDC films is successfully deposited on Al2O3/SiO2/Si systems. The chemical composition of 700 ℃-annealed GDC films is (Ce0.91Gd0.09)O1.94 and possesses a higher film density of 7.257 g/cm3. As a result, GDC thin films prepared by RF reactive magnetron sputtering and post-thermal treatments can be used as thin solid electrolyte layers for intermediate temperature SOFCs system as compared to the well-known yttria-stabilized zirconia(YSZ).     

二维气相色谱技术分析混合碳四馏分中微量炔烃

采用二维气相色谱技术分析了混合碳四馏分中微量炔烃——乙基乙炔（EA）和乙烯基乙炔（VA）。在第一根非极性毛细管柱上进行碳四和碳五预分离,碳五以前组分通过二维色谱预切割模式,转移到第二根多孔层Al2O3开管柱上进一步分离。由于目标化合EA、VA周围没有碳五烯烃干扰,微量EA、VA很容易定性。该方法能准确定量测定微量（10-6级）碳四炔烃。分析结果对评判催化剂加氢脱炔效果起到了重要作用。     

Al_2O_3Cu-Ti-Zr/Nb钎焊研究

使用Cu Ti Zr钎料对Al2 O3 Nb进行了钎焊试验。通过扫描电镜、能谱、X射线衍射分析了界面形貌、元素分布 ,并对反应相进行了判定。Cu70 Ti2 5 Zr5 钎料在 12 93K、10min条件下界面产生了 3种新相 :Cu2 Ti4O、Ti固溶体、CuTi,界面结构为Al2 O3 Cu2 Ti4O Ti固溶体 CuTi Cu固溶体 +CuTi。采用拉剪试验评定了强度 ,结果证实12 93K、10min ,使用Cu70 Ti2 5 Zr5 钎料的接头强度最高达到 16 2MPa ,增加或减少Ti的质量分数以及改变保温时间都会使接头抗剪强度下降。     

Field ion microscopy and 3-D atom probe analysis of Al3Zr particles in 7050 Al alloy

Field ion microscope images have been used to measure the local evaporation field of a Al3Zr particle in 7050 Al alloy. Using the matrix Al evaporation field (19 V/nm) as a reference, the evaporation field of Al3Zr has been estimated to be 36 V/nm, similar to the theoretical value for the field evaporation of Al2+ or Zr3+ ions. A strong local magnification effect from the large difference in evaporation fields between the particle and matrix has been found to cause a severe distortion of the apparent particle morphology in a three-dimensional atom probe reconstruction when using parameters based on the Al matrix. Use of the measured evaporation field for Al3Zr has allowed accurate reconstruction of the morphology of the particle. A simple worst-case analysis predicts that trajectory overlaps increase with increasing cross-section of particle, and the calculated overlaps agree well with experimental estimates of approximately 1.4-2.0 nm for variations in the particle cross-section from 7 to 12 nm. The chemical composition of Al3Zr in a 7050 Al alloy has been measured to be 64.8-67.7 at% Al, 23.6-24.8 at% Zr, 6.9-9.1 at% Zn, 0.4-0.7 at% Cu, 0.5-1.2 at% Mg, with a (Al+Zn)/Zr ratio close to 3. Specimen analysis temperatures of either 25 or 80 K show little effect on the measured chemical compositions of the particle.     

Improvement of light collection efficiency of lens-coupled YAG screen TV system for a high-voltage electron microscope

A new lens coupling television (TV) system using a YAG (Yttrium Aluminum Garnet: Y(3)Al(5)O(12) : Ce(3+)) single crystal screen has been developed for a high-voltage electron microscope (HVEM), and its performance is examined. The system, using a combination of YAG and lenses, is less damaged by high-energy electron irradiation and reduces the influence of X-rays on the image. YAG screens have not been used for lens-coupling systems, because the high refractive index (n = 1.84) of YAG results in a low light collection efficiency for emitted light. This disadvantage is overcome by combining a thin YAG disk screen (thickness; 100 microm) with a glass hemisphere whose refractive index is 1.81. We found that the light intensity is almost the same as that obtained with a conventional P22 powder screen and lenses system. The resolution is about 55 microm on the YAG screen, and this value is 1.3 times higher than that measured by the conventional system. Shading and distortion do not affect TV observation. Detection quantum efficiency, obtained after correction of the channel mixing effect, is about 0.1.     

High-resolution electron microscope observation of interface microstructure of a cast Al-Mg-Si-Bi-Pb(6262)/Al2O3p composite

High-resolution electron microscopy was employed to characterize the interface structure of a cast Al-Mg-Si-Bi-Pb aluminium(6262)-based composite reinforced by alpha alumina particles with a trace of beta alumina in order to investigate the behaviour of alloying elements in cast composites. Except for a few primary Mg2Si particles, few reaction products were detected at the interface of Al/alpha-Al2O3 due to the unfavourable reaction kinetics during the squeeze-casting process. The Mg2Si particle has an orientation relationship with alpha-Al2O3 of [011]Mg2Si//[1210]alpha-Al2O3 (111)Mg2Si//(0006)alpha-Al2O3. A significant amount of MgAl2O4 was found on the surface of the beta-Al2O3 particles, which is in contrast to the small degree of reaction found on alpha-Al2O3 particles. MgAl2O4 and beta-Al2O3 particles have the following orientation relationship: [011]MgAl2O4//[1210]beta-Al2O3 (111) MgAl2O4//(0006)beta-Al2O3. The similar crystal structure of beta-Al2O3 to MgAl2O4 favours MgAl2O4 nucleation and growth on the surface of beta-Al2O3. Interfacial energy minimization dominates the atomic structure of the interface with the result that close packed planes and directions in the Al2O3 reinforcement and reaction products are parallel to the interfaces. Bi and Pb were found in the form of metallic nanometre particles between Al2O3 particles, or between the MgAl2O4 and Al2O3 particles, or in the open channels of beta-Al2O3 filled by the Al matrix.     

选择激光烧结陶瓷粉末的研究

实验研究了Ａｌ２Ｏ３陶瓷粉末的烧结过程,介绍了激光烧结实验装置,研究了激光参数对烧结的影响和后处理工艺方法,得到了激光烧结的Ａｌ２Ｏ３陶瓷零件。     

混合纳米粒子作为润滑脂添加剂最佳配比的实验研究

在MRH-3型高速环块摩擦磨损试验机上,研究混合纳米粒子Al2O3-Al-Cu和Al2O3-Al-MgO作为润滑脂添加剂的摩擦学性能,通过减摩、表面修复以及抗极压性能实验,确定混合纳米粒子的最佳配比。结果表明:在几种纳米粒子之间的协同作用下,含有混合粒子Al2O3-Al-Cu和Al2O3-Al-MgO的润滑脂具有良好的表面修复、抗极压等摩擦学特性,混合粒子比多数单粒子在减摩方面都具有更好的效果。     

碳纳米管对Al/Al2O3复合相变蓄热材料蓄热与导热性能的影响

论文详细研究了碳纳米管对Al/A12O3复合相变蓄热材料蓄热、导热性能和循环稳定性的影响.利用XRD、TEM和DSC技术分别对碳纳米管的形貌和和蓄热材料的蓄热性能进行了表征.DSC结果表明碳纳米管的添加可略微提高材料的蓄热性能,蓄热值达到543kJ/kg.而添加量太大时,在空气中碳物种易发生氧化反应,在DSC中表现为明显的放热峰.另外,碳纳米管的添加大大提高了材料的导热性能,当碳纳米管的含量为5％时,材料的导热系数提高了30％.对蓄热材料进行升温-降温循环实验可有效提高蓄热材料的抗氧化能力,提高材料的循环稳定性.     

静电辅助气溶胶化学气相沉积法制备Al_2O_3薄膜

以乙酰丙酮铝为前驱体,N,N-二甲基甲酰胺为溶剂,采用静电辅助的气溶胶化学气相沉积(ESAVD)方法,在Si(100)衬底上制备了Al2O3薄膜,并采用场发射扫描电镜、能谱仪、X射线衍射仪和自动划痕仪等设备对制备的薄膜进行了表征。结果表明:采用ESAVD法制备的Al2O3薄膜平整致密而且晶粒细小,薄膜与基体之间及薄膜内部都未出现开裂现象;薄膜与基体的结合力约为5.56 N;沉积得到的薄膜为化学计量比为2∶3的氧化物薄膜;退火前的薄膜为非晶态,在1 200℃退火保温2 h后薄膜转变为-αAl2O3。     

热还原生成法制备Al_2O_3/Cu自生复合材料的研究

从化学反应热力学和动力学的角度,对 Ｃｕ２ Ｏ Ａｌ二元体系反应过程进行了研究,提出了用热还原生成法制备 Ａｌ２ Ｏ３／ Ｃｕ 自生复合材料的新方法,并通过基本实验和采用多种分析手段,对此方法进行了初步验证,同时制备出了此复合材料。     

氧化铝陶瓷在腐蚀环境下的摩擦磨损性能

研究了氧化铝陶瓷在HCl溶液、NaOH溶液和去离子水3种润滑介质下的摩擦磨损性能,获得其在不同滑动速度下的摩擦因数、磨损体积和表面形貌.结果表明:酸性环境抑制了硅和铝的氢氧化物膜的产生,导致在HCl溶液润滑下摩擦副的摩擦因数高,氧化铝陶瓷表面磨损严重;以NaOH溶液为润滑介质时摩擦副的摩擦表面成膜度最高,摩擦因数最低,...     

Al_2O_3-H_2O纳米流体冻结过程的数值模拟和试验研究

纳米流体作为强化换热介质,是目前的研究热点,但关于其相变过程的研究较少。利用当量比热法,在COMSOL有限元模拟软件中对质量分数为5%,不同粒径(10、20、50、100、500nm)的Al2O3-H2O纳米流体和去离子水的冻结过程进行数值模拟,并将模拟结果和试验结果进行了对比。二者具有较好一致性,表明烧杯中心和壁面附近的温度变化趋势有较大区别,中心处的温度变化更能反映样品的冻结过程;当质量分数为5%时,Al2O3-H2O纳米流体的相变时间与去离子水相比较短,且纳米流体的相变时间随Al2O3粒径的增大而增加。     

Performance of Y2O3∕Al multilayer coatings for the He-II radiation at 30.4 nm

We briefly report on the performance and stability of periodic multilayer mirrors containing Y(2)O(3) and Al layers designed for normal incidence reflection at the He-II emission line (30.4 nm). We found that Y(2)O(3)∕Al multilayer coatings had higher reflectivity (24.9%) at 30.4 nm and significantly lower reflectivity (1.3%) at 58.4 nm than the conventional coatings such as Mo∕Si. Furthermore, we investigated the temporal stability of the Y(2)O(3)∕Al multilayer coatings. Our sample was kept under vacuum, dry N(2) purge, and normal atmosphere for over three months, and there were no measurable changes in the reflectivity. These results suggest that we can use Y(2)O(3)∕Al multilayer coatings as standard mirrors for the He-II radiation.     

Al_2O_3-TiB_2陶瓷刀具材料的特性及其应用

Al_2O_3-TiB_2陶瓷刀具材料具有一系列优异性能,其硬度、韧性、导热性和耐磨性等均优于目前正在广泛使用的Al_2O_3-TiC、Al_2O_3-TiN陶瓷刀具材料。本文概述了这种陶瓷刀具材料的特性和应用情况;并对山东工业大学研制成功的牌号为LP1的Al_2O_3-TiB_2陶瓷刀具材料做了介绍。