微/纳米力学测试技术及其应用

    本书系统地介绍了微／纳米力学测试技术中最常用的压入和划入技术及其典型应用。全书共分13章。测试技术方面，内容涉及接触力学、测试原理、方法、校准、仪器、力学参量、影响因素。典型应用方面，内容涉及在表面工程、微机电系统、生物、高聚物和金属玻璃等领域内的微／纳米力学行为的测试。本书可供力学、材料、物理、电子、机械、生物和化学等领域的研究人员、工程技术人员以及大专院校相关专业的师生参考。

目录

前言

第1章 绪论

1.1硬度的定义和分类

1.2纳米压入和划入技术的发展

1.3纳米压入和划入技术的特点

参考文献

第2章 压入接触力学

2.1弹性接触

2.1.1 Soeddon解

2.1.2锥形压针

2.1.3球形压针

2.1.4圆柱压针

2.2弹塑性接触

2.2.1塑性发生

2.2.2完全塑性

2.2.3材料响应

参考文献

第3章 纳米压入测试原理

3.1压入硬度和模量

3.2连续刚度测量

3.3载荷一深度数据确定的材料参数

3.3.1马氏硬度

3.3.2压入蠕变

3.3.3压入松弛

3.3.4压入弹性功和塑性功

参考文献

第4章 纳米压入测试方法

4.1压针类型

4.1.1玻氏压针

4.1.2立方角压针

4.1.3维氏压针

4.1.4努氏压针

4.1.5圆锥压针

4.1.6球形压针

4.1.7圆柱压针

4.1.8楔形压针

4.1.9考虑因素

4.2测试环节

4.2.1样品准备

4.2.2环境控制

4.2.3间距选择

4.2.4表面探测

4.2.5驱动方式

4.2.6测试步骤

4.2.7测试报告

参考文献

第5章 纳米压入的确认和校准

5.1直接确认和校准

5.2间接校准

5.3测试和校准的实例

参考文献

第6章 纳米压入和划入的测量仪器

6.1仪器技术指标的定义

6.2美国Mrs公司

6.3美国Hysitmn公司

6.4瑞士CSM公司

6.5英国MML公司

6.6澳大利亚CSIRO公司

6.7测量仪器的发展趋势

参考文献

第7章 力学参量的测量

7.1压入方式

7.1.1硬度和模量

7.1.2断裂韧度

7.1.3蠕变和粘弹行为

7.1.4压入应力??应变曲线

7.1.5加卸载曲线涉及的

部分现象

7.2划人方式

7.2.1块体材料

7.2.2薄膜材料

7.2.3粗糙度

7.3弯曲方式

7.3.1微悬臂梁静载弯曲

7.3.2微桥静载弯曲

7.3.3微结构疲劳

7.4吸引方式

7.5声发射测试

7.6温度测试

参考文献.

第8章 影响纳米压入测试的因素

8.1测试仪器的影响

8.1.1压针缺陷

8.1.2测试方法

8.1.3接触零点的确定

8.1.4载荷和位移的分辨力

8.2样品的表面状态和性质

8.2.1表面吸湿

8.2.2表面粗糙度

8.2.3残余应力

8.2.4凹陷和凸起变形

8.3纳米压入和划入测试所面临的问题

参考文献

第9章 在表面工程中的应用

9.1金属材料表面激光强化的力学表征

9.2硬质膜的力学和摩擦学性能评估

9.2.1显微硬度测试

9.2.2纳米压人测试

9.2.3纳米划入测试

9.2.4膜材的影响

参考文献

第10章 在微机电系统中的应用

10.1薄膜测试

10.1.1典型薄膜材料的硬度和模量

10.1.2薄膜疲劳

10.1.3淀积工艺对二氧化硅薄膜力学性质的影响

10.2微结构弯曲

10.2.1微结构的静态弯曲

10.2.2微结构的动态弯曲

参考文献

第11章 在生物及其相关材料中的应用

11.1人工林杉木管胞细胞壁

11.2人体腰椎骨

11.3存储液对人体牙齿微力学性能的影响

参考文献

第12章 在高聚物中的应用

12.1PMMA单轴拉伸和弯曲力学行为

12.2划入测试的理论分析

12.3韧性行为的描述

12.4脆性行为的描述

12.4.1温度效应

12.4.2应变率效应

参考文献

第13章 在金属玻璃中的应用

13.1硬度和屈服应力的关系

13.2不连续的塑性变形

13.3压痕形貌和微结构变化

13.4应变率效应

13.5钕基金属玻璃的变形行为

参考文献

附录 常见问题的回答

1测试数量

2压入间距

3压入深度

4泊松比的选择

5典型材料的参数

6断裂韧度测试压针的选择

7纳米薄膜的测试

8典型材料的压入变形行为

9显微硬度和纳米压入硬度的关系

10压入影响区及其边界效应

10.1压入影响区的有限元模拟

10.2边界距离影响的有限元模拟

10.3压人间距影响的测试

参考文献

A STUDY ON THE EFFECT OF LESIONS OF AREA-7 OF THE PARIETAL CORTEX ON THE SHORT-TERM VISUAL SPATIAL MEMORY OF RHESUS-MONKEYS (MACACA-MULATTA)

This research is focused on the contribution of area 7 to the short-term visual spatial memory. Three rhesus monkeys (Macaca mulatta) were trained in the direct delayed response task in which 5 delay intervals were used in each session. When each monkey reached the criterion of 90% correct responses in 5 successive sessions, two monkeys underwent a surgery while the other one received a sham operation as a control. In the first stage of the surgery, bilateral areas 7a, 7b and 7ip of the parietal cortex of two monkeys were precisely lesioned. After 7 days of recuperation, the monkeys were required to do the same task. The average percentage of correct responses in the lesioned animals decreased from 94.7% to 89.3% and 93.3% to 82.0% respectively (no significance, P > 0.05, n = 2). In addition, the monkeys' complex movements were mildly impaired. The lesioned monkeys were found to have difficulty picking up food from the wells. In the second stage, bilateral area 7m was lesioned. In the 5 postoperative sessions, the average percentage of correct responses in one monkey, with a relatively precise 7m lesion, decreased from 94.7% to 92.2% (no significance, P > 0.05), while the other monkey, with widely spread necrosis of lateral parietal cortex, showed an. obvious decline in performance, but still over the chance level. After 240 trials this monkey reattained the normal criterion. The results of this research suggest that the lesions of area 7 of the parietal cortex did not significantly affect the short-term visual spatial memory, which has been shown to be sensitive to lesions of the prefrontal cortex; they also support the notion of dissociation of spatial functions in the prefrontal and parietal cortices.

CHARACTERISTICS OF FATTY ACID METHYL ESTERS (FAMEs) AND ENZYMATIC ACTIVITIES IN SEDIMENTS OF TWO EUTROPHIC LAKES

Enzymatic activities and fatty acid methyl esters (FAMEs) in the sediments of two eutrophic lakes in Wuhan city were investigated. The results showed phosphatase and dehydrogenase activities in the lotus zone and plant floating bed zone were significantly lower than those in other sites, and urease activity was the highest where microorganism agents were put in. Fatty acid group compositions indicated the predominance of aerobic bacteria in the surface sediments in shallow lakes. The ratios of FAMEs specific for bacteria and Gram-positive bacteria exibited significant differences between the two lakes. The results of trans to cis indicated that the microorganisms in Lake Yuehu could adapt themselves to environmental stress better. The enzymatic activities and FAMEs showed differences in different sites, indicating that ecological restoration measures and environmental conditions could affect lake sediment to some extent. But the monitoring, work would be done in series to exactly evaluate the effect of the remediation measures.

不含桥基的茂金属烯烃聚合催化剂的合成及催化

本论文探讨了烯烃聚合催化剂的合成及其用于聚合的研究，合成的催化剂是不含桥基的IVB族的茂金属化合物。共合成了十九个茂金属化合物：（~tBuC_5H_4)CpMCl_2[M=Ti(1a)，Zr(1b)]； Me_3SiC_5H_4CpMCl_2[M=Ti(2a)， Zr(2b)]；~tBu_2C_5H_3CpMCl_2[M=Ti(3a)，Zr(3b)]；C_5H_9IndCpMCl_2[M=Ti(4a)，Zr(4b)]；PhCH_2IndCpMCl_2[M=Ti(5a)，Zr(5b)]；(~tBu_2C_5H_3)_2MCl~2[M=Ti(6a)，Zr(6b)，Hf(6c)]；(C_5H_9Ind)_2MCl_2[M=Ti(7a)，Zr(7b)，Hf(7c)]；(PhCH_2C_6H_5)_2MCl_2[M=Ti(8a)，Zr(8b)，Hf(8c)]。这十九个化合物分别通过EI-MS，~1H-NMR，IR 和元素分析进行了表征。用所合成的十九种茂金属化合物与甲基铝氧烷作为催化体系，在常温常压下，研究了乙烯聚合反应。得到的主要结论如下：（1）1a，2a， 5b 8b 催化活性最好。（2）1a 在铝钛比等于 1167 时聚合效率最高，2a 在铝钛比等于 1500 时聚合效率最高， 5b 在铝锆比大于 2955 时聚合效率最高，8b 在铝锆比等于 1667 时聚合效率最高。（3）相同的聚合条件下，催化效率是 1a＜2a，8b＜5b。（4）由聚合物的DSC表征中可见，所得聚合物的结晶度是 1a＜2a，5b＞8b。（5）由聚合物的分子量的测定可知，所得聚合物的分子量是 1a＞2a ，5b＜8b，由 8b 催化得到的聚合物的分子量最大。

PHOTOLUMINESCENCE SPECTRUM STUDY OF THE GAAS/SI EPILAYER GROWN BY USING A THIN AMORPHOUS SI FILM AS BUFFER LAYER

Recently, we reported successful growth of high-quality GaAs/Si epilayers by using a very thin amorphous Si film as buffer layer. In this paper, the impurity properties of this kind of GaAs/Si epilayers have been studied by using PL spectrum, SIMS and Hall measurement. Compared to a typical PL spectrum of the GaAs/Si epilayers grown by conventional two-step method, a new peak was observed in our PL spectrum at the energy of 1.462 eV, which is assigned to the band-to-silicon acceptor recombination. The SIMS analysis indicates that the silicon concentration in this kind of GaAs/Si epilayers is about 10(18) cm(-3). But its carrier concentration (about 4 x 10(17) cm(-3)) is lower than the silicon concentration. The lower carrier concentration in this kind of GaAs/Si epilayer can be interpreted both as the result of higher compensation and as the result of the formation of the donor-defect complex. We also found that the high-quality and low-Si-concentration GaAs/Si epilayers can be regrown by using this kind of GaAs/Si epilayer as substrate. The FWHM of the X-ray (004) rocking curve from this regrowth GaAs epilayer is 118 '', it is much less than that of the first growth GaAs epilayer (160 '') and other reports for the GaAs/Si epilayer grown by using conventional two-step method (similar to 200 '').

水菖蒲的化学成分研究和忍冬属植物的色谱分析

本论文由三章组成。第一章阐述了藏药水菖蒲的化学成分研究，共分离鉴定了39个化学成分，其中6个为新化合物。第二章报道了几种忍冬属植物的HPLC、HPLC-MS、GC分析以及抑菌活性、重金属含量测定结果。第三章概述了菖蒲属植物的研究进展。 第一章报道了水菖蒲(Acorus calamus L.)化学成分的分离纯化与结构鉴定。采用正、反相硅胶柱层析等分离方法，从水菖蒲的根中共分离出41个化合物，通过红外、质谱、核磁共振及X-ray单晶衍射等波谱方法和模拟计算方法鉴定了其中39个化合物的结构，主要为倍半萜、苯丙素、甾体类化合物。其中含有5个新的倍半萜类化合物和1系列新的甾体皂苷衍生物。经波谱分析将它们的结构鉴定为 1b, 7a(H)-cadinane-4a, 6a, 10a-triol (1), (2R,6R,7S,9S)-1(10), 4-cadinadiene-2, 9-diol (2), 1a, 5b-guaiane-10a-O-ethyl-4b, 6b-diol (7), 6b, 7b(H)-cadinane-1a, 4a, 10a-triol (13)，(1R,4R,6S,10R)-1-hydroxy-7(11)-cadinen-5, 8-dione (14)， 4′-O-正n碳酰基-3-O- β-D-葡萄糖基谷甾醇(n=14, 16, 18, 22) (15)。 第二章包括四个部分。第一部分报道了忍冬属三种植物40个样品的HPLC测定和对主要活性成分绿原酸的定量分析结果，以及运用HPLC-MS技术对色谱图中8个峰进行指认。在此基础上，考察了种植和采收多个因素对绿原酸含量的影响。第二部分报道了忍冬属三种植物27个样品的GC分析，根据样品的挥发性成分的保留时间对不同样品进行了定性比较，并考察了花期及海拔高度对植物挥发性成分的影响。第三、四部分分别阐述了灰毡毛忍冬和红腺忍冬的体外抑菌活性研究和重金属含量测定结果。 第三章全面系统地概述了菖蒲属植物的化学成分和药理活性研究进展。 This dissertation is composed by three chapters. The first chapter elaborates the phytochemical investigation of Acorus calamus L. Thirty-nine compounds including six new compounds were isolated and identified. The second chapter reports the research on genus Lonicera by HPLC, HPLC-MS and GC. Antifungal activity and heavy metals measurement of genus Lonicera were reported. The third chapter is a review about the research progress on the plant family of Acorus. The first chapter focuses on the isolation and identification of chemical constituents from Acorus calamus L.. Forty-one compounds were isolated from the root of Acorus calamus L. by repeat column chromatography over normal and reversed phase silica gel, the structure of thirty-nine compounds was identified by spectroscopic methods and computational methods, including IR, MS, NMR and X-ray. Those compounds mainly belonged to sesquiterpene, phenylpropanoid and steroid. Among them, five are new sesquiterpenes and one series are new steroid glycoside derivatives. Their structure were suggested as 1b, 7a(H)-cadinane-4a, 6a, 10a-triol (1), (2R,6R,7S,9S)-1(10), 4-cadinadiene-2, 9-diol (2), 1a, 5b-guaiane-10a-O-ethyl-4b, 6b- diol (7), 6b, 7b(H)-cadinane-1a, 4a, 10a-triol (13), (1R,4R,6S,10R)-1-hydroxy-7(11)- cadinen-5, 8-dione (14), 4′-O-carbonyl-3-O-β-D-glucosyl-sitosterol (carbonyl = tetradecanoyl, hexadecanoyl, octadecyl, docosanoyl) (15). The second chapter consists of four parts. The first part reports the HPLC analysis of forty samples of the genus Lonicera, and the quantitative investigation of chlorogenic acid in these samples by HPLC analysis. Relationship between the content of chlorogenic acid in different samples and their planting conditions and harvesting time were discussed. Furthermore, eight compounds were identified or tentatively characterized based on their mass spectra and UV spectra profiles. The second part is about qualitative analysis of the volatile constituent in twenty-seven samples of genus Lonicera by GC. The effect of planting altitude and harvesting time on the volatile constituent was also investigated. The third and fourth parts describe the antifungal activity and content of some kinds of heavy metals of L. macranthoides Hand.-Mazz. and L. hypoglauca Miq.. The third chaspter is a review about the research progress of the plant family of Acorus.

The photo-induced decarbonylation of Cp ' M(NO)(CO)(2) (M = Cr, Mo, W) with diorgano dichalcogenides (R2E2; E = S, Se; R = Me, Ph)

The photo-induced decarbonylation of Cp'Cr(NO)(CO)(2) (1a) in MeCN solution in the presence of R2E2 (E = S, Se; R = Me, Ph) leads to the formation of chalcogenolato-bridged binuclear complexes Cp-2'Cr-2(NO)(2)(mu -ER)(2) [E = S; R = Me (2a), Ph (3a); E = Se, R = Me (4a), Ph (5a)] while reactions between Cp'M(NO)(CO)(2) [M = Mo (1b), W (1c)] and Ph2E2 (E = S, Se) result in mononuclear complexes Cp'M(NO)(EPh)(2) [M = Mo; E = S (9b), Se (10b); M = W, E = S (11c), Se (12c)]. The corresponding reactions of (1b) with Me2E2 (E = S, Se) yielded both mono and binuclear complexes: Cp'Mo(NO)(SeMe)(2) (8b), Cp-2'Mo-2(NO)(2)(mu -EMe)(2) [E = S (6b), Se (7b)]. The new complexes have been characterized by i.r., H-1-, C-13-n.m.r. spectra and by electron-impact mass spectrometry.

Ferrocenylphosphine-imine ligands for Pd-catalyzed asymmetric allylic alkylation

Ferrocenylphosphine-imine ligands 6 derived front (R,S)-PPFNH2-R 5 and a variety of benzaldehydes were applied in the Pd-catalyzed asymmetric allylic alkylation of 1,3-diphenylprop-2-en-1-yl acetate 7a or pivalate 7b with dimethyl malonate. The substituent effects on the catalytic reaction were investigated, and 96% e.e. with 99% yield was achieved when the m-nitro substituted ligand 6k was used. (C) 2002 Elsevier Science Ltd. All rights reserved.