La（Ⅲ）、Nd（Ⅲ）与甜菜碱类衍生物形成的包含（H2O）6分子簇的配合物的晶体结构

利用配体1,5-二(3-羧基吡啶基)-N-甲基二乙胺(L)合成2种稀土金属配合物{[La2L4(H2O)2](ClO4)6·6H2O}n(1)和[Nd2L4(DMF)6(H2O)2]2(ClO4)6·4H2O(2)。用红外光谱和X-射线单晶衍射表征配合物的晶体结构。结构分析表明:配合物1属于三斜晶系,P1空间群,其晶胞参数为a=1.496 6(3)nm,b=1.559 7(4)nm,c=1.956 8(4)nm,α=86.776(6)°,β=77.723(7)°,γ=87.168(7)°,Z=2。在配合物1中,一对La髥原子被2个羧基桥联,形成双核结构;双核结构进一步被羧基连接,从而形成平行于c轴的一维链。值得注意的是配合物1的晶体结构中包含着由氢键连接的6个H2O分子组成的水分子簇。配合物2属于三斜晶系,P1空间群,晶胞参数为a=1.040 8(4)nm,b=1.354 1(5)nm,c=2.975(1)nm,α=94.390(8)°,β=91.720(7)°,γ=95.230(4)°,Z=2。配合物2中4个羧基连接一对Nd髥原子,形成四轮状结构,其中2个羧基采取syn-syn双原子桥联模式,而其余2个羧基则采取单原子桥联模式。     

硫脲络合–火焰原子吸收光谱法测定低硅铝合金中的银含量

采用硫脲络合–火焰原子吸收光谱法测定低硅铝合金中的银元素含量。实验探讨了酸度及硫脲用量对银测定的影响及铝合金中基体元素与共存元素对银元素分析线的干扰情况。结果表明:选用9%的盐酸和3%的硝酸溶解试样最好,加入5 mL 50 g/L硫脲溶液可消除氯离子对试验结果的影响,基体铝元素和其它共存元素不干扰银的测定。根据低硅铝合金中银元素的含量范围,合成系列标准溶液,建立工作曲线,工作曲线的线性范围为0.05%~0.50%。银元素含量为0.30%的样品测定结果的相对标准偏差为0.15%(n=8),标准加入回收率为96.8%~98.5%。该方法操作简便、重现性好、测量结果准确可靠。     

铝基复合材料中不同形态碳分析方法的研究

本文研究铝基复合材料中碳元素不同存在形式（总碳、游离碳、碳化硅）的检测方法。 采用高频感应燃烧红外法测定总碳（2.00%～6.00%）,酸溶过滤分离-高频红外法测定游离碳（0.10%～1.50%）,重量法测定碳化硅(1%～35%)的含量。以上三个方法的精密度试验RSD%（n=8）最大分别为4.2%、1.2%、0.51%,测定游离碳和碳化硅(SiC)样品的加标回收率分别是98.5%～100.2%,99%～101%。 这三种方法都快速、可靠,已应用于铝基复合材料的实际分析工作中。     

刚玉粉、高岭土、莫来石中铝、硅的测定

主要针对三种原材料中的Al含量和Si含量的分析方法进行讨论。采用容量法对其中的Al含量进行测定,在酸性溶液中,加入过量的EDTA溶液络合铝并掩蔽残余元素。在微酸性溶液中以二甲酚橙为指示剂,用氯化锌标准溶液滴定过量的EDTA,以氟化铵络合铝而游离出等量的EDTA。再用氯化锌标准溶液滴定至溶液呈橙红色即为终点。根据氯化锌标准溶液的消耗量换算出Al2O3的含量。采用重量法对其中Si含量进行测定,将熔融后的试样进行处理,使之生成硅酸沉淀。经灼烧、称重后以硫酸、氢氟酸进行挥硅处理,再灼烧称重,根据两次质量之差换算出SiO2的含量。两种分析方法均为经典化学分析方法,其分析结果准确可靠,并且具有广泛的使用性。     

电感耦合等离子体原子发射光谱法测定钛合金中钨、铌、钽

采用电感耦合等离子体原子发射光谱法（ICP-AES）法测定钛合金中W,Nb,Ta元素的含量。样品采用盐酸、氢氟酸和硝酸溶解,并对仪器工作参数和试验条件进行了优化试验,确定了仪器最佳工作条件,考察了钛合金基体和共存元素对待测元素的影响,确定了各待测元素谱线为W207．911nm,Nb309．418nm,Ta240．063nm。选定的待测元素分析线不受合金基体和共存元素的干扰,通过基体匹配消除基体的影响。加标回收率在98％104％之间,测定结果的相对标准偏差为0．3％～2．4％（n=8）,方法的检出限为0．003-0．013μg／mL。进行了标准物质对照试验,试验结果与标准值相符。     

SiC纤维增强Ti17合金复合材料轴向残余应力的拉曼光谱和X射线衍射法对比研究

准确测量和分析SiC纤维增强Ti合金复合材料(SiC_f/Ti)中残余应力状态对优化复合材料的成型工艺和理解其失效模式具有重要意义,但其残余应力的实验测量和分析仍是一个挑战.石墨C涂层作为SiC纤维与Ti17基体合金之间必需的扩散障涂层,承载了由纤维与基体之间热不匹配引入的残余应力.本文采用显微拉曼光谱法对比测量纤维表面C涂层在复合材料中和去掉基体无应力态下G峰的峰位,通过石墨C涂层应力态下峰位移动计算出SiCf/C/Ti17复合材料中SiC纤维受到～705.0 MPa的残余压应力.采用X射线衍射方法测量了不同方向上该复合材料中基体钛合金的晶面间距以获取其空间应变,根据三轴应力模型分析了复合材料中基体钛合金沿轴向方向的残余应力为～701.3 MPa的张应力,并通过线性弹性理论转化为SiC纤维的残余压应力为～759.4 MPa.两种测试方法都确定了SiC纤维在成型过程中受到残余压应力,且获得的应力值较为接近,都可以用于对SiC_f/Ti复合材料的残余应力测量.     

Reliability assessment on interfacial failure of thermal barrier coatings

Thermal barrier coatings (TBCs) usually exhibit an uncertain lifetime owing to their scattering mechanical properties and severe service conditions. To consider these uncertainties, a reliability assessment method is proposed based on failure probability analysis. First, a limit state equa-tion is established to demarcate the boundary between failure and safe regions, and then the failure probability is calculated by the integration of a probability density function in the failure area according to the first-or second-order moment. It is shown that the parameters related to interfacial failure follow a Weibull distribution in two types of TBC. The inter-facial failure of TBCs is significantly affected by the thermal mismatch of material properties and the temperature drop in service.     

数字梯度敏感方法及其在航空透明件断裂力学中的应用

本文将数字梯度敏感方法用于航空透明件断裂力学问题研究。首先,基于透明材料的弹性-光学效应,建立了透明件应力状态与光线穿过透明件后的偏转角之间的关系。在平面应力假设下,利用最小二乘拟合建立了I型裂纹尖端应力强度因子与光学偏转角的关系。其次,通过数字梯度敏感方法搭建非接触光学测试平台,开展了带单边裂纹的航空有机玻璃试件三点弯曲实验,应用数字梯度敏感方法提取了I型裂纹尖端应力强度因子。最后,通过选择不同计算子区域和步长大小,分析了数字梯度敏感方法中的子区域和步长选择对计算结果的影响。研究结果表明,数字梯度敏感方法实验所得应力强度因子与经验公式计算所得结果偏差小于10%,通过增加最小二乘拟合项数以及合理的子区域和步长选择可以减小数字梯度敏感方法计算应力强度因子误差。     

Image analysis of atmospheric corrosion of field exposure high strength aluminium alloys

The corrosion morphology image acquisition system which can be used in the field was established. In Beijing atmospheric corrosion exposure station, the image acquisition system was used to capture the early stage corrosion morphology of five types of high strength aluminium alloy specimens. After the denoise treatment, wavelet-based image analysis method was applied to decompose the improved images and energies of sub-images were extracted as character information. Based on the variation of image energy values, the corrosion degree of aluminium alloy specimens was qualitatively and quantitatively analyzed. The conclusion was basically identical with the result based on the corrosion weight loss. This method is supposed to be effective to analysis and quantify the corrosion damage from image of field exposure aluminium alloy specimens.     

The effect of frequency and sample shape on fatigue behaviors of DZ125 superalloy

The effect of frequency and sample shape on fatigue behaviors of DZ125 superalloy are systematically studied. The results show that fatigue fracture still occurs above the cycle of 10⁸ for tests carried out at the frequency of f = 20 kHz and stress ratio R = ?1, so the traditional fatigue limit at cycle of 10⁷ is not appropriate for fatigue design. Fatigue fracture surfaces are perpendicular to stress axis for cylindrical and plate specimens, and the fatigue cracks originate from the extra surface of the specimens. Fatigue crack is apt to propagate from cutting direction to forward direction, which occurs mainly in the second propagation stage at higher stress amplitude. There is an obvious frequency effect for DZ125 superalloy. The higher the test frequency is, the more serious the effect of frequency on fatigue behaviors of the alloy. After the frequency correction, the ultra-high cycle fatigue S-N curve well coincide with the traditional fatigue S-N curve.