{100}织构化学气相沉积金刚石薄膜的取向生长过程

为了研究化学气相沉积（CVD）金刚石薄膜生长过程中{100}织构的形成机理,采用x射线衍射、电子背散射衍射和扫描电镜研究了CVD自支撑金刚石薄膜的宏观织构、微区晶界分布和表面形貌。结果表明：金刚石薄膜以{111}面或{100}面为生长前沿面都能够形成{100}织构,但形成的表面形貌不同;通过吸附CH3-和CH3-在{1...     

氧化铁刻蚀金刚石表面形貌的表征及形成机理

为了系统研究不同温度下氧化铁刻蚀金刚石表面的形貌及形成机理,以人造金刚石为刻蚀材料,以氧化铁作为刻蚀剂,先将金刚石洗净,然后将金刚石与氧化铁以质量比为1∶5混合均匀、压实,用氮气作为保护气氛,在650～850℃下用氧化铁刻蚀金刚石单晶表面。再用扫描电子显微镜及其3D重建技术、热重分析、X射线衍射和拉曼光谱等方法对刻蚀后金刚石单晶不同晶面的表面形貌、表面粗糙度、物相组成和刻蚀机理进行了表征与分析。首次用3D重建技术对刻蚀后金刚石不同晶面的形貌进行了立体观测,用铜基结合剂金刚石试样的抗弯强度来评估刻蚀对金刚石与结合剂间结合力的影响。结果表明:氧化铁在不同温度下均能有效刻蚀金刚石单晶,且对不同晶面的刻蚀程度和形貌是各向异性的;当刻蚀温度为650℃时,氧化铁对金刚石单晶已有一定的刻蚀;随温度的升高,刻蚀加剧;在相同条件下,金刚石单晶的{100}面刻蚀程度比{111}面严重,{100}面表面粗糙度S_a从0.84μm升至3.73μm,{111}面表面粗糙度S_a从0.77μm升高至2.01μm。刻蚀后,金刚石单晶的不同晶面形貌由金刚石本身的原子排列决定,随着刻蚀温度从650℃升至850℃,金刚石{100}面刻蚀坑从四边形变为八边形,{111}面由轻微的点状变为三棱锥形凸起。氧化铁对金刚石单晶的刻蚀机理是金刚石的氧化过程。刻蚀后,铜基结合剂金刚石试样的抗弯强度有较大的提高。     

无取向硅钢晶粒长大过程中应力对织构和晶界变化的影响

采用EBSD技术研究了有、无拉应力作用下无取向硅钢在晶粒长大过程中织构转变及晶界变化的规律。结果表明:在晶粒生长期间,无应力作用下的硅钢中,{111}〈112〉,{111}〈110〉织构组分强化,而{100}〈001〉织构组分弱化;与无拉应力作用下的情况相比,施加5MPa的拉应力时,{111}〈112〉,{111}〈110〉织构组分强化的速率下降,{100}〈001〉织构组分变化不明显。对于在晶粒生长期间持续变化的{111}〈112〉,{111}〈110〉和{100}〈001〉织构组分而言,虽然有、无拉应力作用下硅钢的{111}〈112〉和{111}〈110〉织构组分的高取向差角度晶界频率均下降,而{100}〈001〉织构组分的高取向差角度晶界频率则上升,但当有拉应力作用后,{111}〈112〉和{111}〈110〉织构组分的高取向差角度晶界频率下降的速率变小,{100}〈001〉织构组分的高取向差角度晶界频率上升的速率稍有变小。通过对无取向硅钢在晶粒长大过程中织构转变及晶界变化规律的研究,分析了合金原子在晶界的偏聚行为。     

Pr_(6)O_(11)对合成金刚石单晶各向异性的刻蚀EI北大核心CSCD

为了探究稀土氧化物对合成金刚石单晶的各向异性刻蚀,在氮气保护下,在750~950℃内用Pr_(6)O_(11)对合成金刚石单晶进行刻蚀。采用扫描电子显微分析、热重分析、X射线衍射和拉曼光谱等技术对刻蚀后金刚石单晶不同晶面的表面形貌、物相组成和刻蚀机理进行表征与分析。采用最大刻蚀深度、单颗粒抗压强度和冲击韧性来表征刻蚀前后金刚石性能的变化。结果表明:Pr_(6)O_(11)对金刚石{100}面和{111}面的刻蚀程度和形貌均不同;当温度为750℃时,Pr_(6)O_(11)对金刚石单晶已有一定程度的刻蚀,随刻蚀温度的增加,刻蚀加剧,且金刚石{111}面的刻蚀程度比{100}面严重;{111}面刻蚀坑形貌从三角形变为层状结构三角形,{100}面由轻微的四边形变为类蜂窝状刻蚀坑;{111}面最大刻蚀深度从1.12μm增加到12.54μm,而{100}面只从0.30μm增加到2.11μm;金刚石单颗粒的抗压强度由未刻蚀金刚石的576.25 N降低到最小530.06 N,冲击韧性由92.94 J/cm^(2)减小到88.53 J/cm^(2);Pr_(6)O_(11)对金刚石单晶的刻蚀机理在885℃前为催化石墨化,885℃后为催化石墨化和氧化。     

氮气氛下金刚石薄膜生长过程中的光发射谱研究

利用原位光发射谱对衬底附近的化学气相性质进行了研究．研究表明,氮气的引入使得金刚石生长的气相化学和表面化学性质发生了很大变化．含氮基团的萃取作用提高了金刚石表面氢原子的脱附速率,从而提高了金刚石膜的生长速率．而含氮基团的选择吸附使金刚石（１００）取向变得化学糙化,这种化学糙化使得（１００）晶面生长速率远大于其它晶面,最终使金刚石薄膜呈现（１００）织构．还利用化学气相沉积方法研究了氮气浓度对金刚石生长的影响,结果与光发射谱分析是一致的．     

GH4169合金楔横轧加工过程中动态再结晶及织构演变

为研究GH4169合金楔横轧加工过程中动态再结晶及织构演变规律,采用金相显微镜(OM)和电子背散射衍射(EBSD)对30%,50%两种断面收缩率下GH4169合金楔横轧件表层与心部的微观组织、晶体取向及织构进行分析。结果表明:GH4169合金楔横轧加工过程中,随着动态再结晶的发生,晶体取向逐渐变得随机化分布;轧制表层大角度晶界数量较轧件心部多,轧件表层织构强度变化不大,心部织构强度明显增强;经过楔横轧变形后织构发生转动,原始态织构类型为{001}〈110〉,{111}〈110〉,{111}〈011〉,轧制后主要织构类型为{001}〈010〉,{112}〈110〉,{110}〈111〉,{110}〈112〉;GH4169合金楔横轧件动态再结晶及织构演变规律是由楔横轧特殊变形特点决定的。     

FeNi-C-FeS体系金刚石中氮含量的研究

利用高温高压温度梯度法,在FeNi-C-FeS体系中进行了宝石级金刚石大单晶的合成研究,重点考察了FeS含量对金刚石中氮含量的影响。结果发现体系中随着掺杂FeS含量的增加,晶体品质会遭到一定程度的破坏,尤其是{100}生长区域。对晶体中氮含量而言,当掺杂FeS的量由0增加至1.25%时,{111}生长区域的氮含量与纯FeNi-C体系相比几乎没有发生变化,而{100}生长区域的氮含量却发生较大变化,远远低于纯FeNi-C体系中{100}生长区域的氮含量。这说明掺杂FeS更易对晶体的{100}生长区域产生影响,或者说S元素更容易进入{100}生长区域,这样S原子与N原子之间产生竞争,使氮原子进入金刚石的几率减少,导致{100}生长区域的氮含量急剧下降。     

高强Ti-IF钢铁素体区热轧和冷轧过程织构演变规律

为了揭示铁素体区热轧、冷轧和退火过程中高强Ti-IF钢中织构的演变过程,采用X射线衍射仪研究了铁素体区热轧及随后的冷轧和退火织构的特点.研究表明,在铁素体区热轧后,表面和中心面的织构类型和强度不尽相同,表面上的主要织构组分是剪切织构{110}<001>,而中心面上的主要织构组分是{001}<110>～{223}<110>和{111}<110>,由于织构的遗传性,冷轧和退火后的织构在表面和中心面上也不相同;经不同压下率冷轧后,织构变化趋势一致,表面上{110}<001>组分消失,{001}<110>成为最强组分,而中心面上最强组分由{001}<110>沿α取向线向{112}<110>偏移,冷轧织构由α织构和γ织构组成;退火后,表面上织构的变化与以往结论有所不同,{001}<110>～{112}<110>组分减弱,而γ取向线上的{111}<123>组分增强,{111}<112>和{111}<110>减弱.     

晶面取向对同质外延单晶金刚石生长的影响

利用微波等离子体化学气相沉积法,在天然金刚石的(100)、(110)以及(111)晶面上进行了同质外延生长单晶金刚石的研究,分析了这三个晶面上同质外延生长的特点。结果表明,不同的晶面上金刚石的生长速率和形貌显著不同。(110)晶面生长速率最快,表面由一系列大小不同的四面体组成,(100)晶面次之,呈现出排列规整的生长台阶,而(111)晶面生长速率最低,表面光滑平整,(100)和(111)的这种二维生长表面粗糙度明显小于(110)的一维生长表面,而这些特点与其生长模式密切相关。虽然在(111)晶面生长出了质量理想、表面平整的单晶金刚石,但是与(100)和(110)晶面外延生长的单晶金刚石相比,其质量还是较低。     

缓冲层Ta对退火Co/Cu/Co薄膜微观结构和界面互扩散的影响

用直流磁控溅射法在Si/SiO₂基底上制备了Co/Cu/Co薄膜和加入缓冲层的Ta/Co/Cu/Co薄膜,用扫描电子显微镜、原子力显微镜、X射线衍射和俄歇电子能谱研究了薄膜的微观结构、表面形貌、织构和界面互扩散现象。结果表明:退火后薄膜中均存在{111}和{002}衍射峰,加入缓冲层Ta后,Co/Cu/Co薄膜的衍射峰强度明显增强,并存在较强的{111}纤维织构,薄膜表面孔洞及粗糙度大幅减小。退火后薄膜界面处产生互扩散现象,层状结构被破坏。缓冲层Ta提高了薄膜与基底材料间的润湿性,可有效缓解界面互扩散现象。     

Crystal orientation changes of Ag thin films on the Si(111) substrate due to tribo-assisted recrystallization

Crystal orientation changes of Ag thin films due to the tribo-assisted recrystallization have been studied using grazing incidence X-ray diffraction with synchrotron radiation. After preparation of an Si(111) √3 × √3-Ag surface, a 5-nm-thick Ag film was deposited on the surface at the substrate temperature of 303 K in an ultra-high vacuum chamber. The friction experiments were carried out using a diamond pin-on-plate type tribometer just after the Ag deposition in the same UHV chamber. We found that the coefficient of friction of the Ag films on the Si(111) √3 × √3-Ag surface decreases from 0.07 to 0.03, with increasing reciprocal sliding cycles. In synchronization with the coefficient change, Ag{100} grains are gradually disappearing. As a result, the Ag{111} grains cover the entire surface after 50 sliding cycles. Moreover, we found that the domain size of the Ag{111} grains increases with increasing reciprocal sliding cycles by measuring the rocking curve width. These results directly show that the Ag(111) plane is the sliding plane of friction and the coefficient of friction of Ag films is determined by the fraction of the Ag(111) grains in the Ag films. Moreover, to clarify the reaction between the Ag film and the Si substrate due to the tribo-assisted recrystallization, the substrate strain has been studied by an extremely asymmetric X-ray diffraction technique using synchrotron radiation.     

AFM Study on Interface of HTHP As-grown Diamond Single Crystal and Metallic Film

The study for the interface of as-grown diamond and metallic film surrounding diamond is an attractive way for understanding diamond growth mechanism at high temperature and high pressure (HTHP), because it is that through the interface carbon atom groups from the molten film are transported to growing diamond surface. It is of great interest to perform atomic force microscopy (AFM) experiment; which provides a unique technique different from that of normal optical and electron microscopy studies, to observe the interface morphology. In the present paper,we report first that the morphologies obtained by AFM on the film are similar to those of corresponding diamondsurface, and they are the remaining traces after the carbon groups moving from the film to growing diamond. The fine particles and a terrace structure with homogeneous average step height are respectively found on the diamond(100) and (111) surface. Diamond growth conditions show that its growth rates and the temperature gradients inthe boundary layer of the molten film at HTHP result in the differences of surface morphologies on diamond planes,being rough on (100) plane and even on the (111) plane. The diamond growth on the (100) surface at HPHT could be considered as a process of unification of these diamond fine particles or of carbon atom groups recombination on the growing diamond crystal surface. Successive growth layer steps directly suggest the layer growth mechanism of the diamond (111) plane. The sources of the layer steps might be two-dimensional nuclei and dislocations.     

高能微波辐照条件下SiC晶粒的生长过程分析

利用高能真空微波辐照, 仅以SiO₂和人造石墨粉为原料, 便捷快速地合成得到结晶良好的β-SiC晶粒。在利用各种表征手段综合分析SiC晶粒微观结构的基础上, 确认高能微波辐照条件下, β-SiC晶粒的生长过程符合“光滑界面的二维形核生长”机制。借助于电子背散射衍射技术(EBSD)进行的原位解析发现, 生长最快的{211}面在晶粒长大过程中逐渐被超覆, 通过形成{421}过渡晶面而最终演变为{220}晶面, 并成为晶粒的侧面; 而生长最慢的{111}面则成为最后保留下来的六角形规则晶面。EBSD的解析结果为SiC晶粒生长过程中晶面演变提供了直接的实验证据。     

Effects of nitrogen partial pressure on microstructure,morphology and N/Ti ratio of TiN films deposited by reactive magnetron sputtering

Abstract

TiN films were deposited on Si(111) substrates at different nitrogen partial pressures with reactive magnetron sputtering. The crystal structure and preferred growth orientation of the films were determined using X-ray diffraction (XRD) analysis. Their morphology and composition were analysed using field emission scanning electron microscopy (FESEM) and energy dispersive spectroscopy (EDS). It is found that with the increase in nitrogen partial pressure, the growth of TiN films varies from the {111} preferred orientation to the {100} preferred orientation and the deposition rate of TiN films decreases. When the {111} preferred orientation is presented, TiN films reveal a kind of surface morphology of triangular pyramid with right angles; while the {100} orientation is dominant, TiN films characterise another kind of domelike surface morphology. Furthermore, the N/Ti ratio of the TiN films first increases, then decreases and increases again as nitrogen partial pressure enlarges.     

The quantitative effects of crystal habit change on the film surface form and the preferred orientation during the growth of vacuum-condensed films

Our recent systematic observations by reflection electron diffraction showed that a basic feature of film growth of high melting point materials condensed in vacuum on substrates initially at room temperature is that, after the initial thin film of randomly oriented crystals, and the growth of faces and preferred orientation of a particular type at the film surface, a new type of face and preferred orientation is often developed in further strata of deposit growth.Calculations are made showing the effect of a change in crystal habit on the film surface element distribution and the nature of the new preferred orientation which is developed.The {211} habit and orientation in gold films, in further growth after the first-developed {111} habit and orientation, is discussed as an example of the calculations, which indicate a tilt δ of approximately 25° for the {211} orientation when the vapour angle of incidence i is 45°. This agrees with our observations, confirming that the {211} orientation arises from the habit change and not from nucleation by secondary {111} twinning.     

CRYSTALLOGRAPHIC FATIGUE CRACK GROWTH IN NIMONIC AP1

Recently a controversy has developed over whether crystallographic crack growth near threshold in Ni-base superalloys occurs along {111} slip planes or {100} planes at room temperature. In this work on Nimonic API crack propagation is shown to occur on both {100} and {111} planes. The most common facet plane is {111} and this is the only orientation observed at the lowest stress intensities, but at higher stress intensities occasional {100} facets are also produced. This behaviour is compared with similar results in aluminium alloys.     

Surface topographical variation of single-crystalline diamond grown in CO-H2 plasma

Microtopographical variations of {111} and {100} crystal surfaces of single-crystalline diamond grown by microwave-plasma chemical vapour deposition of the CO-H2 reactant system were examined using scanning electron microscopy. A layer-by-layer epitaxial growth process was observed on both crystal surfaces. A number of epitaxial two-dimensional nuclei were formed at random on {111} surfaces, where small triangular growth layers spread with the same orientations as the outline of the original {111} basal plane. These spreading layers were found to leave an inverse triangular pit (so-called trigon) pattern as they joined each other. On the other hand, square growth layers spread in parallel directions to {100} basal plane, and they stacked in the 100 directions to form a pyramidal growth hillock.     

Grain-Scale Modeling of CVD of Polycrystalline Diamond Films

The evolution of grain size, grain-size distribution, morphological and crystallographic texture, surface roughness, and the contribution of various surface facets to the growth of polycrystalline diamond films is performed by carrying out a series of two-dimensional computer simulations. The films are assumed to grow from a set of randomly oriented, {100}- and {111}-faceted nuclei by the motion of their vertices (the points where the adjoining facets of the same or neighboring grains meet). The vertex velocities are found to be a function of the orientation and the growth rate of the adjoining facets. To quantify the latter, a {100} to {111} growth-rate parameter is used. The results show that the evolution of the grain size and its distribution, surface roughness, morphological and crystallographic texture, and the portion of the film grown from different surface facets are all mutually linked and governed by the magnitude of the growth-rate parameter. The latter can be controlled by the CVD processing conditions, such as the substrate temperature, reactor pressure, mole fraction of carbon-source gas (e.g., CH₄, C₂H₂).     

低偏压下化学气相沉积金刚石薄膜的生长形貌研究

在微波等离子体化学气相沉积装置中，研究了偏压电压、甲烷浓度及沉积气压对金刚石晶形显露的影响。实验结果表明，生长时施加低的衬底偏压对金刚石的晶形显露有较大的影响，正的偏压有利于(111)面显露，负偏压有利于(100)面显露。在低偏压条件下生长时，低的沉积气压和甲烷浓度有利于(111)面显露；而高的气压和甲烷浓度有利于(100)面显露。过高的甲烷浓度将恶化金刚石质量，出现菜花状组织，无明显的晶面显露。