两步压入法--薄膜力学性能的可靠测量方法

提出了采用力学探针测量薄膜力学性能的两步压入法.该方法通过大载荷压入展示基体变形对薄膜硬度的影响,从而选择不影响基体变形的小载荷测出薄膜的硬度和弹性模量.对高速钢基片上的TiN硬质薄膜,单晶硅片上的金属Ni薄膜和(Ti,Al)N/VN纳米多层膜的测量表明,两步压入法能够测出各种性质薄膜的力学性能,并且具有准确可靠的特点.此外,两步法对(Ti,Al)N/VN纳米多层膜的力学性能的测量表明,该体系的纳米多层膜存在硬度和弹性模量异常升高的超硬、超模量效应.     

残余压应力场中薄膜纳米测量硬度的变化与校正

利用量纲定理和有限元法系统分析了残余压应力场中薄膜硬度的变化规律,在此基础上提出了薄膜硬度的修正公式.该修正公式把有、无残余应力时的薄膜硬度比值Hr/H0、卸载功和压入总功的比值We/W、残余压应力σr和硬度的比值σr/Hr联系起来,据此,只要测定薄膜纳米压入加、卸载曲线及薄膜中的残余压应力,便可最终确定无残余应力时的薄膜硬度.     

纳米压痕测量精度的影响因素

通过比较45钢拉伸试验与纳米压痕试验得到的弹性模量,分析了影响纳米压痕测试精度的因素及其对测试结果的影响.结果表明:纳米压痕法得到的弹性模量大于拉伸试验法得到的弹性模量;压头形状与尺寸、试样表面粗糙度、定位零点等是影响测量精度的主要因素,尤其是压头尖端的不规则形状使得压头在压入材料的初始阶段与材料之间的相互作用变得复杂.     

薄膜厚度对Si基SiO2薄膜力学性能的影响

为了研究薄膜厚度对Si基SiO_2薄膜力学性能的影响规律,利用纳米压痕技术及有限元模拟方法对不同厚度的Si基SiO_2薄膜材料进行测试,分析了不同厚度薄膜的硬度及弹性模量等力学性能,讨论了不同压深膜厚比对不同厚度薄膜弹性恢复率的影响,并在试验的基础上,建立了有限元模型,模拟了不同厚度薄膜在相同压深下的载荷位移关系,分析了薄膜的弹性恢复性能。结果表明:SiO_2薄膜越厚其弹性模量越小,而薄膜的硬度在薄膜较薄时压痕的尺寸效应更明显,并利用模拟进一步分析得出薄膜越薄弹性恢复性能越好。     

用纳米压入法测量硼化铪涂层的弹性模量

用Nano IndenterⅡ对硼化铪，石英和硼化铪/硅等膜/基结构进行纳米压入测量。通过对测得的载荷一位移曲线进行处理，得到硼化铪涂层的弹性模量为188．78GPa。实验表明，较软基底对测量结果的影响较大，所得的评定值失真，用KING提出的评定模型也未获得较好的结果。因此，最大压入深度应在保证压头尖钝化和薄膜表面质量对测量结果影响不太大的情况下尽量减少最大压入深度。     

纳米压入法MEMS材料力学能测量与评定标准化的初步设想

根据纳米压入法测量与评定MEMS材料力学性能的原理,对诸如测量仪器、压头、评定模型、测试条件等影响力学性能测量精确度、测量结果的可比性的主要原因因素进行了分析。在此基础上,提出对MEMS材料力学性能测量与评定进行标准化的初步设想。     

应用纳米压痕法测试类金刚石薄膜的力学性能

纳米压痕仪被称为材料机械性质微探针,它借助于加载-卸载过程中压痕对载荷和压入深度的敏感关系,使得测试始终在薄膜材料的弹性限度内,克服了维氏法和努氏法等传统方法引起压痕边缘模糊或者碎裂的缺点,从而正确地、可靠地测试出薄膜材料的硬度和弹性模量等纳米力学性能.试验用微波电子回旋共振等离子体增强化学气相沉积技术,在不同偏压条件下制备三种类金刚石薄膜(DLC膜),用纳米压痕仪测试不同载荷下薄膜的硬度和弹性模量值.试验结果表明,材料的纳米硬度和弹性模量随着载荷的增大而逐渐减小.     

纳米压入法研究核电站-回路主管道材料的热老化行为

采用纳米压入方法对核电站一回路主管道的双相不锈钢材料热老化行为进行定量研究.通过对单独的铁素体相和奥氏体相的纳米压入实验,得到随着老化时间的增加,两者在相同压入深度时的压入载荷增加;根据动态测试技术得到的纳米硬度增加,表现为强度提高;而纳米压入塑性变形能降低,表现为韧性降低;并且不同老化时间下铁素体相的强度和韧性都要高...     

PECVD法硅基氮化硅薄膜的制备及其耐磨性研究

以N(111) 型的单晶硅片为基体,运用PECVD-2D等离子体化学气相淀积台在单晶硅片表面沉积氮化硅薄膜,通过薄膜颜色与厚度间的关系探讨了制备工艺参数对薄膜厚度的影响,用原位纳米力学测试系统对氮化硅薄膜的纳米硬度进行测定,在UMT-2型摩擦试验机上对不同制备工艺的硅基氮化硅薄膜进行耐磨寿命试验.结果表明:随着沉积温度的升高,薄膜厚度逐渐递减,SiH4和N2流量比越大,薄膜厚度越大;温度越高,薄膜硬度越大,耐磨寿命越长;随着SiH4和N2流量比的增加,薄膜硬度和耐磨寿命均先增加后减小.     

聚甲基丙烯酸甲酯薄膜的弹性模量测量研究

高聚物材料由于其易热变形、常温下状态稳定且不易被破坏等优点,是新型的存储技术———基于扫描探针显微术(SPM)的热机械超高密度信息存储技术的理想存储介质材料,存储介质的力学特性是影响热机械形成的数据斑形貌的重要因素。实验使用纳米压痕法对270nm厚聚甲基丙烯酸甲酯(PMMA)薄膜的弹性模量进行测试,采用两次保载过程,有效地消除了材料的黏性对测试结果的影响。同时研究了基底效应的影响,通过引入与深度相关的影响因子估算基底的影响,得到PMMA薄膜在常温下的弹性模量为6.5GPa。     

多晶硅微机械构件损伤的表面效应

利用电磁力驱动微拉伸装置，考察多晶硅微构件表面粗糙度和施加表面分子自组装膜(octadecyltrichlorosilane，简称OTS)对抗拉强度及断裂损伤的影响。结果表明，微构件的抗拉强度表现出依赖表面性质的表面效应。抗拉强度随表面粗糙度的增加而降低，并受环境气氛的影响。当构件表面施加表面分子自组装膜后，在以上两因素的作用下．多晶硅微构件的抗拉强度提高了32．46％。研究结果可用于微机械构件的材料表面改性设计。     

Dynamic mechanical properties of photo resist thin films

Photo resist thin films have mainly been used and investigated for versatile applications of micro electronic mechanical systems because of its outstanding aspect ratio and attainable film thickness. An accurate structure properties derived from validated material characterization is required in engineering applications. In this work, dynamic responses of photo resist thin films are tested by a nanoindentation in association with a dynamic mechanical analysis, where the thin film is coated on a silicon wafer by spin coating. The results show that the storage modulus of the photo resist thin film remains constant at the beginning and then increases as the indentation depth increases. Meanwhile, the loss modulus increases as the indentation depth increases. Varying the film thickness shows that the substrate effect plays an important role in determining the dynamic properties of thin films. However, the results agree well with the bulk material when the amplitude of nanoindentation is relatively small. It illustrates the dynamic mechanical analysis can be an efficient method to characterize the viscoelastic properties of thin films, but proper attention on the test parameters is needed.     

薄膜的力学测试技术

对薄膜力学性能的测试方法、技术以及所取得的主要成果进行简要的综合介绍。     

多元CrMoSiCN系列薄膜结构及摩擦学特性研究进展

从三元含Mo的Cr-Mo-N、Mo-Si-N、Mo-C-N薄膜到四元Cr-Mo-Si-N、Mo-Si-C-N薄膜,综述多元系列薄膜的结构、力学及摩擦学性能的研究进展;分析在不同气体压力、制备方法与参数、不同元素含量下薄膜结构的变化,阐述薄膜结构与其力学性能和摩擦学特性的关联。指出:多元Cr-Mo-Si-C-N系列薄膜结构、硬度、摩擦因数强烈受到薄膜中Mo、Si、C、N元素含量的影响,其中力学特性还与薄膜微结构紧密相关;薄膜的摩擦学特性与晶粒生长细化和作为润滑剂的无定形基质有关;在摩擦过程中发生的摩擦化学反应也有效地提高了薄膜的耐磨性。对于四元Cr-Mo-C-N和多元Cr-Mo-Si-C-N薄膜,建议进一步研究在水润滑与非润滑的不同条件下,例如在海水或者空气干摩擦环境下,是否由于薄膜结构组分的不同而有效地形成含Mo的氧化物的自润滑膜,以提高薄膜在更多场合下的适应性和减摩性。     

单轴微拉伸MEMS材料力学性能测试的系统集成

为了对微米尺度薄膜材料的力学性能进行测试,开发了一套成本较低的单轴微拉伸MEMS材料力学性能测试系统。首先,根据有限元模拟优化设计测试样片,使其能够易于夹持、准确对中,以利于应力和应变的测量。接着采用三维非硅UV-LIGA微加工技术制备了Ni薄膜样片。根据单轴拉伸测试过程和硬件构成,以Visual Basic为平台编译了一套数据采集与分析系统。最后,应用该测试系统完成对电镀Ni薄膜材料性能的测试。实验结果表明,该系统能够精确测试试样应变,精度达到0.01μm,拉伸力精度达到mN级。得到的电镀Ni薄膜材料的杨氏模量约为94.5 GPa,抗拉强度约为1.76 GPa。该系统基本满足微米尺度材料单轴微拉伸力学性能测试的需要。     

MECHANICAL DEFLECTION OF POLYSILICON MICROCANTILEVER BEAMS USING NANOINDENTATION

0INTRODUCTIONThe miniaturization of microelectronic device is now reaching the mechanical field, allowing the integration of micromechanisms together with their operation electronics in a single device. This leads to interesting perspectives in the design of monolithic microrobtic systems by the micromachining techniques directly derived from standard silicon technology. Scientists have already moved MEMS into various stages of conception and development for making laboratories on chips,…     

Atomic Force Microscope Investigation on Static Nanomechanical Properties Versus Dynamic Nanotribological Evaluation of Metal–ZrN and ZrN Thin Films

The present study offers for the first time a correlation between static nanomechanical properties (nanohardness (H), elastic modulus (E), H/E and H ³/E ² ratio) and dynamic properties (resulting from nanoscratch measurements) for Metal–ZrN thin films (Inconel–ZrN, Cr–ZrN and Nb–ZrN) as well as monolayer polycrystalline ZrN thin films. Metal–ZrN thin films have a great industrial potential, as they can combine high hardness with good elasticity and toughness making them effective for wear resistant application. Nanomechanical and nanotribological properties of Metal–ZrN and ZrN thin films deposited by DC unbalanced magnetron sputtering were investigated using an atomic force microscope interfaced with a Hysitron Triboscope. The elastic recovery of thin films under a normal load applied during nanoindentation was evaluated and correlated with elastic recovery of thin films under dynamic loading during nanoscratch measurements in order to asses which film compositions provide superior wear resistance. It is demonstrated that dynamic elastic recovery measurements correlated well with those derived from static nanoindentation tests. The nanoscratch test combines both normal and tangential loading, therefore, it is expected to be an even better predictor of wear-resistance. The AFM nanoindentation and nanoscratch measurements show superior nanomechanical and nanotribological properties for Metal–ZrN thin films when compared to polycrystalline ZrN thin films.     

SiC薄膜制备MEMS结构

采用PECVD方法制备了无定形SiC薄膜,在此基础上,以SiC为结构层,利用传统的表面硅牺牲层工艺制作了电容式谐振器以及薄膜残余应力的在片检测结构。对SiC的MEMS结构进一步进行了长时间的腐蚀,以获得SiC材料的腐蚀特性。对SiC材料的力学特性进行了研究。深入探讨了退火工艺、薄膜硅碳原子比对SiC薄膜力学特性的影响,同时对薄膜硅碳原子比与制备工艺参数(包括硅烷、甲烷流量)之间的关系进行了实验研究。     

Effect of mechanical shear on the thin‐film properties of base oil‐polymer mixtures

The thickness and frictional characteristics of thin lubricant films are known to affect the fuel economy properties of oils. The base oil and polymer compositions of the lubricant are generally considered to be critical chemical factors that can influence these thin‐film lubricant properties in new oils. However, it is important to produce lubricants with good fuel economy properties that are maintained after the lubricant is degraded. Lubricants in use can undergo oxidation and mechanical shear degradation. The effect of oxidation degradation on thin‐film physical properties has previously been studied. This paper investigates the effect of mechanical shearing on thin‐film properties. Dispersant olefin copolymers are found to reduce thin‐film friction in simple mixtures and in fully formulated oils. In simple mixtures, shearing the dispersant olefin copolymers does not affect the friction‐reducing ability of these polymers. In fully formulated oils, even though shearing diminishes to a degree the friction‐reducing ability of dispersant olefin copolymers, these copolymers can still provide significant friction reduction.