AlN陶瓷衬底的SIMS和XRD测量

ＡｌＮ陶恣成分怀发对于ＡｌＮ的性能具有决定性作用，用二次离子质谱（ＳＩＭＳ）和Ｘ射线衍（ＸＲＤ）对清华大学材料系电子封装用的ＡｌＮ陶瓷进行了研究。ＳＩＭＳ谱表明ＡｌＮ衬底中除Ａｌ，Ｎ以我有Ｃ，Ｏ，Ｓｉ，Ｃａ，Ｙ等元素，其中有些是表面污染。衬底的ＳＩＭＳ深度分析表明样品Ｏ，Ｃａ，Ｙ信号都很强，且分布均匀，说明样口 含有Ｙ２Ｏ３，ＣａＯ添加剂，ＡｌＮ样品的ＸＲＤ谱与ＡｌＮ的ＪＣＰＤＳ卡片对照，在测量范     

Ti／AlN快速退火界面反应的实验研究

在电子封装用的ＡｌＮ陶瓷多晶衬底上生长２５０ｎｍ的Ｔｉ膜，并进行快速退火。用ＲＢＳ（卢瑟福背散剂）、ＡＥＳ（俄歇有谱）、ＳＩＭＳ（干净人离子质谱）ＸＲＤ（Ｘ射线衍射）等实验技术对界面反应进行了分析研究，用划痕实验测量了退火对Ｔｉ／ＡｌＮ粘附力的影响。实验结果表明：快速退火时，Ｔｉ，Ａｌ，Ｎ以及ＡｌＮ中掺杂的Ｏ均发生明显的界面扩散和界面反应，样品表面的Ｏ和ＡｌＮ衬底中掺杂的Ｏ都向Ｔｉ膜中扩散，在较低     

SIMOX材料的SIMS分析

对ＳＩＭＯＸ材料进行了ＳＩＭＳ深度剖析，研究了电荷积累效应、二次离子传输效率等实验因素对测试结果的影响，氧检测的动态范围达三个量级。对国内、外的ＳＩＭＯＸ材料做了对比研究。     

硅基GaN外延层的SIMS及XPS研究

采用真空反应法在硅基上制备出了GaN外延层。利用二次离子质谱和X射线光电子能谱对GaN外延层进行了深度剖析和表面分析。结果表明 ,外延层中Ga和N分布均匀 ;在表面处Ga发生了偏聚 ;外延层中还存在Si,O等杂质 ,但这些并未影响到GaN外延层的物相及发光性能。实验还表明 ,在外延生长前采用原位清洗可去除Si衬底表面的氧     

MCs^＋—SIMS技术在研究金属与陶瓷界面反应中的应用

近年来，实验证明ＭＣｓ＾＋－ＳＩＭＳ技术可以明显减小甚至消除ＳＩＭＳ分析中的基体效应，已成功地应用于某些半导体与金属中，适于对痕量杂质以及基体组分进行分析。现将ＭＳｃ＾＋－ＳＩＭＳ技术推广应用来表征金属与陶瓷界面反应导致的组分变化。对不同温度退火的金属（Ｔｉ）与陶瓷（Ａｌ２Ｏ３，ＡｌＮ等）界面进行了分析，成功地观察到了界面的组分变化，为其他技术进一步证实，并且获得了新的结果。     

MCs^＋—SIMS技术及其应用

强烈的基体效应一直是造成二次离了质谱（ＳＩＭＳ）难以定量分析和解释的主要原因，受其影响，常规ＳＩＭＳ，即Ｍ－ＳＩＭＳ（检测原子型二次离子Ｍ或Ｍ，Ｍ是要分析的元素）的适用范围受到了很大的限制，近几年来，上述状况已经通过一种新技术开发得到明显改善，这就是ＭＣｓ－ＳＩＭＳ技术，即在Ｃｓ一次离子轰击睛检测分子型二次离子ＭＣｓ而不是Ｍ。由于该技术明显减小甚至消除基体效应，从而开辟了ＳＩＭＳ定量分析的新途径，     

Ti/A1N快速退火界面反应的实验研究

在电子封装用的A1N陶瓷多晶衬底上生长250nm的Ti膜，并进行快速退火。用RBS（卢瑟福背散射）、AES（俄歇电子能谱）、SIMS（二次离子质谱）和XRD（X射线衍射）等实验技术对界面反应进行了分析研究，用划痕实验测量了退火对Ti／A1N界面粘附力的影响。实验结果表明：快速退火时，Ti，A1，N以及A1N中掺杂的O均发生明显的界面扩散和界面反应。样品表面的O和A1N衬底中掺杂的O都向Ti膜中扩散，在较低的退火温度下生成TiO2；在较高的退火温度下与扩散到Ti膜中的A1反应，在Ti膜中间形成Al2O3层。N向Ti中扩散，并与Ti反应生成TiN。在薄膜和衬底之间有Ti的氧化物生成。粘附力的测量结果表明：在较低的温度下进行快速退火可以明显提高Ti／A1N界面的强度，在较高的温度下，界面强度有所下降。     

砷化镓中掺硅元素的SIMS定量分析

通过对体均匀掺硅和离子注入硅样品的二次离子质谱（ＳＩＭＳ）深度剖面分析，采用均匀体标样法、剖面二次离子强度积分法和ＬＳＳ理论关系计算获得了比较一致的、且与手册值接近的ＧａＡｓ中硅元素相对灵敏度因子值。将相对灵敏度因子法应用于双能量、双剂量硅离子注入ＧａＡｓ样品及分子束外延多层ＧａＡｓ膜渗硅的ＳＩＭＳ定量分折中。从实验结果初步讨论了ＧａＡｓ中氧和碳元素的存在对２８Ｓｉ－、１０３ＳｉＡｓ－二次离子信号强度的影响，２８ＳｉＡｓ－和１０３Ｓｉ－二次离子信号强度的线性关系和可靠性。     

一种测定晶体取向及其分布的简便XRD方法

提出了旋转定向测试法，其原理是使试样的在粉末X射线衍射仪上进行θ扫描的同时绕其端面法线自转，增加了晶面法线通过衍射平面的机会。通过这种方法可直观地区分取向多晶，准单晶或者单晶体，评定研制过程中准单晶和择优取向材料的晶体品质，确定单晶，准单晶及择优取向等材料的晶面相对宏观端面的晶向偏离角和取向分散度，还可对单晶体材料进行三维晶面定向。旋转定向法测试晶体取向具有快速简便，一机多用，精度高等优点，在电子、光学、磁性，机械等材料研究领域具在广泛的应用。     

GaAs中Si的二次离子质谱定量分析

评述砷化镓中硅SIMS定量分析的进展，讨论了相对灵敏度因子法。对此种GaAs的原始参考物质，用实验确认了其可靠性。为常规定量分析研制了二次参考物质。对一些关键实验因素，如样品装载、仪器参数以及离子选择等进行了仔细研究，并评价它们对定量重复性、精确性、检测限和基体效应的影响。Cs 源入射时GaAs中Si定量分析精度在15％内；检测AsSi二次离子时，29Si的检测限达5×1014atoms／cm3。     

Residual surface oxide on ZrV getter—XPS, LEIS and SIMS study

The activated ZrV non-evaporable getter (NEG) film has been studied by means of X-ray photoelectron spectroscopy, low-energy ion scattering and secondary ion mass spectrometry. In this work, we found that the first atomic layer of the thermally activated ZrV NEG consists mainly of zirconium atoms, which are partly oxidized. The residual zirconium suboxides observed on thermally activated ZrV NEG diminish during ion sputtering of NEG surface. It indicates that residual suboxides are located mainly in the top surface layer.     

原子团离子在Al_(x)Ga(1-x)As基体组分SIMS定量分析中的应用

通过检测原子团离于MCs 和MAs－（M是基体元素）对AlxGa1-xAs基体组分进行了定量的分析，考察了MIQ－156SIMS上所测这些原子团离子的能量分布及其对分析结果的影响，并对正、负SIMS测量方法做出比较。     

Ge/Pd/n-GaAs低阻欧姆接触的SIMS分析

采用Ge／Pd／GaAs结构和快速热退火在n－GaAs上形成了低阻欧姆接触。利用H次离子质谱（SIMS）技术揭示和讨论了低欧姆接触形成的机理。比较了采用X 和CsX 信号检测的Ge，Pd，Ga和As的深度分布。结果表明采用CSX 可以提供更准确的结果和成分信息。     

SIMS and GDMS depth profile analysis of hard coatings

Rapid development in hard coating technology calls for simple construction depth profile analysers. Here we present results of depth profile analysis of a set of Ar arc plasma deposited TiN, CrN layers. The results are obtained with the use of recently constructed simple glow discharge mass spectrometer (GDMS) and compared with secondary ion mass spectrometer (SIMS). In SIMS (SAJW-05 model) we apply 5 keV Ar⁺ ion beam of about 100 μm in diameter. Digitally controlled spiral scanning of primary ion beam is performed over 1.6 mm² area. Secondary ions are extracted from the central part due to an “electronic gate” and analysed by quadrupole mass spectrometer QMA-410 Balzers (16 mm rods).GDMS analyses are performed on SMWJ-01 glow discharge prototype spectrometer. To supply discharge in 1 hPa argon we use 1.5 kV DC voltage. The analysed sample works as a cathode in a discharge cell. Area of the analysis is ∼4 mm² due to the use of secondary cathode—high purity tantalum diaphragm. Sputtered atoms are ionised, next extracted into the analytical chamber and finally analysed by the quadrupole mass analyser SRS-200 (6 mm rods).The results show that the use of simple construction GDMS analyser allows obtaining similar or even slightly better depth resolution than it can be obtained in the SIMS spectrometer. Application of glow discharge analysis opens new possibilities in direct quantitative depth profile analysis of hard coatings.     

机械镀锌层的X射线衍射分析

采用机械镀方法制备了锌镀层,运用X射线衍射技术分析了镀层的物相组成和锌粉颗粒的晶格参数。研究结果表明,机械镀锌层是由单质金属锌、锡和铁构成,镀层中没有辞、锡和铁之间的化合物或固溶体等合金相存在;由纳米亚晶构成的锌粉颗粒是镀层的主体,锌粉形成镀层后没有发生晶粒细化。     

On the application of SIMS to study the oxidation mechanisms of alumina formers

Abstract

Secondary ion mass spectrometry (SIMS) is widely used to investigate the oxidation mechanism of alumina formers, being various MeCrAl (Me=Fe, Ni, Co) alloys and β-NiAl intermetallic compound. Frequently, it is combined with dedicated oxidation exposures, mostly in atmospheres containing different amounts of oxygen tracer (¹⁸O₂) in order to investigate the scale growth mechanism. However, there are several practical aspects which have to be taken into account during planning the oxidation experiments as well as during interpretation of their results in order to avoid misleading conclusions. In particular, the effects related to the formation of non-uniform scales as well as to the relationship between the exposure conditions and the scale microstructure and morphology at various stages of its growth should be dealt with.

This paper discusses the implications of sputtering process with respect to elemental in-depth distribution profiling and the results of the oxidation mechanism investigation of various alumina formers by means of SIMS. It is shown that the obtained shapes of the SIMS profiles and images strongly depend on the choice of the exposure conditions and on the analysis parameters, including the spatial resolution. The exposure conditions are related to the scale microstructure and morphology, the evolution of which occurs during the oxidation process. Formation of duplex alumina scale is reported which comprises an inner more compact sub-layer and an outer ridged and less-compact sub-layer.