单晶硅化学机械抛光划痕演变研究

化学机械抛光法是制作超光滑单晶硅镜片的常用工艺,抛光过程中的各类杂质粒子经常会导致加工表面产生划痕,降低镜片的表面质量。为系统研究不同晶向单晶硅表面塑性划痕与抛光液中杂质的关系,设计了金刚石微粉掺杂抛光Si(111)、Si(110)和Si(100)晶面的实验。利用轮廓仪测量了不同晶向、不同掺杂浓度下的划痕形貌,并通过计算载荷归一化后的划痕宽度分布、划痕深度分布、粗糙度和二维功率谱密度来评估划痕形貌。结果显示,抛光液中杂质粒子粒径、硅片表面的划痕宽度均服从正态分布。随着杂质粒子浓度的增加,划痕形貌从非周期性特征转变为周期性波动,粗糙度出现突跃点。此外,在同浓度金刚石微粉掺杂情况下,Si(110)面在划痕产生初期有更好的杂质粒子容忍度。     

水稻中的纳米硅及其紫外吸收

为了了解水稻中硅的亚显微结构及其紫外吸收特性,根据强酸不会腐蚀SiO₂玻璃的事实,选择湿消化方法分离水稻中的硅体。以浓硫酸和硝酸混合液分别处理水稻叶片和稻壳,经多级沉降分离出其中的硅体。X射线光电子能谱结果表明硅体距离表面10 nm以内碳相对质量为35.05%,远高于硅体表面(5.88%),说明硅质壁能够阻止强酸进入硅体内部,避免硅体内氧化,保持硅体结构完整和相对独立的理化性质。电镜显示硅体SiO₂结构致密,由1～2 nm的SiO₂凝胶粒子粘聚而成,纳米颗粒相互融合组成排列方向一致的纳米棒,内部还有微米尺度(≤1μm)和纳米尺度(≤1～2 nm)的隙孔。颖壳硅体最大吸收位于285 nm;叶片纳米硅对紫外辐射的吸收极其有限,表明水稻颖壳和叶片硅体对紫外辐射具有不同的抵抗机制。     

激光轰击过程中纳米碳管复合光限幅材料组成及结构的演变研究

光限幅材料在激光轰击过程中的稳定性将在很大程度上决定其实用化价值。文章采用红外(IR)光谱、拉曼(Raman)光谱、透射电子显微镜(TEM)及孔结构分析等测试方法对纳米碳管(CNTs)复合光限幅材料在激光轰击过程中组成、结构的演变进行跟踪研究。结果表明,在强激光轰击下,复合体系中二氧化硅(SiO₂)基质的组成未发生显著改变且网络结构趋于完整,具有较好的稳定性。掺杂CNTs石墨化程度提高,SiO₂凝胶玻璃基质对其起一定的保护作用。轰击过程产生的热效应使得SiO₂颗粒长大,由其堆积而成的孔随之增大。     

一维电介质-金属光子晶体的光学特性研究

利用传输矩阵方法,研究了一维电介质-金属光子晶体的光学特性,该光子晶体通过在Si/SiO₂组成的电介质型光子晶体中插入一定厚度Al层形成。计算结果表明,金属层的引入可以有效提高反射效率,[Si(46 nm)/SiO₂(60 nm)/Al(10 nm)/SiO₂(60 nm)]5结构的单位周期传输衰减从[Si(46 nm)/SiO₂(120 nm)]5的7.2 dB增大到了20 dB;可以得到更宽频率范围的全方向反射带隙,例如[Si(46 nm)/SiO₂(60 nm)/Al(30 nm)/SiO₂(60 nm)]5结构即可提供550 nm带宽的全方向反射;同时讨论了金属吸收、金属层厚度及插入位置对其光学特性的影响。这种电介质-金属光子晶体有望作为性能优异的光学反射镜得到应用。     

磁性复合流体分散性及其对BK 7光学玻璃抛光性能的影响

针对BK7光学玻璃材料去除率和抛光质量不断提高的需求,提出通过减少磁性复合流体(MCF)抛光液颗粒的团聚、提高MCF分散性,配制性能优良的抛光液,提高BK7光学玻璃的MCF抛光性能.MCF中添加不同质量分数的高分子类分散剂聚乙烯醇(PVA),采用激光粒度分布仪测试MCF抛光液中颗粒的粒径分布和中位粒径,探究不同PVA浓度的抛光液对BK7光学玻璃抛光性能的影响.试验结果表明:当PVA质量分数为3%时,中位粒径达到最小值5.854μm,MCF的分散性最好,对光学玻璃的抛光性能大幅提高,当PVA质量分数为5%时,经MCF抛光10min后材料去除率达到最大值26.4×10~(-4)g/min,表面粗糙度达到最小值8.23nm.MCF中添加适量PVA能够减少抛光液颗粒的团聚,提高MCF的分散性,提升BK7光学玻璃的磁性复合流体抛光性能.     

Eu掺杂SiO2纳米基质的发光特性

采用溶胶-凝胶(sol-gel)法制备了Eu掺杂的SiO₂干凝胶,分别用光致发光(PL)光谱、透射电镜(TEM)、扫描电镜(SEM)、红外吸收(IR)谱等分析手段对样品进行了表征,研究了SiO₂的基质中Eu³⁺、Eu²⁺的发光特性以及退火温度对发射光谱的影响,并对其发光机理进行了分析。结果表明,样品掺杂均匀,颗粒尺寸大约在50~80 nm,硼(B)离子进入SiO₂网格,成为了基质的一部分,改变了基质的网络结构。当采用258 nm激发样品时,随着退火温度的升高,红光发射强度先增强后减弱。对于经800 ℃退火处理的样品红光发射最强,出现了576 nm(⁵D₀ →⁷F₀),620 nm(⁵D₀ →⁷F₂),658 nm(⁵D₀ →⁷F₃)3条谱线,其中主峰位于 620 nm红光发射,对应于Eu³⁺离子的⁵D₀ →⁷F₂超灵敏跃迁,进一步说明B离子参与到基质中,形成了Si—O—B键,导致Eu³⁺离子所处配位环境的对称性降低,从而有利于Eu³⁺离子的特征发射;当采用271 nm激发样品时,随着退火温度的升高,蓝光发射强度先增强后减弱,经850 ℃退火的样品400~500 nm蓝光发射最强,归属于Eu²⁺的5d→4f的跃迁发射,证明在铝离子(Al³⁺)存在的情形下,在高温退火过程中Al³⁺部分取代Si⁴⁺形成AlO^-₄基团,掺杂Eu³⁺填补AlO^-₄基团附近的空位,增加了Eu³⁺周围的AlO^-₄四面体中氧原子的电子给予能力,使得Eu³⁺还原成Eu²⁺,从而得到了较强的蓝光发射。但是,当退火温度达到900 ℃时,由于稀土离子发生位置的迁移形成团簇红光和蓝光都明显地降低。     

庞西垌花岗质复式岩体X射线荧光光谱、等离子体质谱分析及其对岩浆分异的指示意义

云开地块西南缘的庞西垌复式岩体由外而内、由上而下依次为花岗片麻岩、片麻状花岗岩和花岗岩,即由高级变质岩渐变过渡至岩浆岩。X射线荧光光谱、等离子体质谱对三类岩石的分析结果表明,三类岩石皆属于过铝质岩石系列,造岩组分和微量元素具有渐变过渡的特征。在花岗片麻岩演化为花岗岩的熔融、分异过程中,Al₂O₃,CaO,MgO与TiO₂等造岩组分含量逐渐增高,SiO₂含量逐渐降低;稀土元素总量整体升高,稀土元素中轻稀土含量逐渐增高,而重稀土含量逐渐降低,显示出轻重稀土分异增强的特征,在多期演化过程中,形成了具有亲缘演化基因的庞西垌花岗质岩石系列。这表明云开地块表变质壳岩石的重熔可能是花岗质岩石的重要成因。其演化机制可能是,表壳岩石在发生熔融之后SiO₂最先脱离母岩不断熔出,重稀土可能随着SiO₂熔体逐渐向上富集;而Al₂O₃,CaO,MgO,TiO₂以及轻稀土相对SiO₂则向下富集。     

喷雾热解法制备红色发光粉LiEu(SiO2)1/6W2O8的研究

采用喷雾热解法制备红色荧光粉LiEu(SiO₂)_1/6W₂O₈。研究了反应温度、前驱体溶液浓度、载气流速对实验结果的影响。通过扫描电镜、X射线衍射、激发和发射光谱对所制样品进行了研究,发现样品颗粒呈实心类球形、结晶度好、表面光滑、发光强度较高、粒径平均1.5μm左右且分布较窄。该类荧光粉激发主峰位于396nm,发射主峰位于615nm。LiEu(SiO₂)_1/6W₂O₈发光的色坐标为:x=0.667 9,y=0.3310,与NTSC的红色标准基本一致,该荧光粉色纯度非常高,适用于制造紫光芯片激发的白光LED。用喷雾热解法制备红色荧光粉LiEu(SiO₂)_1/6W₂O₈的研究尚未见报道。     

一种新型平板彩色显示器件的制备和光谱分析

以MEH-PPV(聚[2-甲氧基-5-(2′-乙基己氧基-对苯乙烯)])和Alq₃作为发光层, 成功制备出ITO/SiO₂/MEH-PPV/SiO₂/Al结构和ITO/SiO₂/Alq₃ /SiO₂/Al结构的固态阴极射线器件。通过分析SSCL光谱,认为这些高速电子激发有机材料后形成Frenkel激子。当器件两个电极之间加的电压比较低时,有机薄膜层的场强也比较低,这些激子被解离的概率很小,从而产生的是激子发光的长波发射;当器件两个电极之间加的电压比较高时,有机薄膜层的场强很高, 在有机层形成的激子大部分被解离, 解离后的电子直接跃迁至LUMO(lowest unoccupancied molecular orbit),这些电子弛豫后从LUMO能级到HOMO(highest occupancied molecular orbit )能级直接辐射跃迁, 接着重新复合发光,从而产生短波发射。制作的固态阴极射线器件可以实现全色发光, 提高发光效率和加强蓝光发射。作者可以预期所研制出的这种SSCL器件必将引发平板显示领域一场新的革命性变革。     

ZnO/SiO2 复合薄膜的光学性能

采用溶胶-凝胶法在玻璃衬底上制备ZnO/SiO₂复合薄膜,分别用XRD、TEM、SEM对样品的结构和形貌进行表征,并研究了不同ZnO含量对复合薄膜透过率及荧光特性的影响。结果表明,样品经500 ℃退火处理生成了SiO₂和ZnO,其晶粒尺寸为18.7 nm,薄膜具有双层结构。复合薄膜的透过率随着其中ZnO含量的增加而降低,禁带宽度减小,光学吸收边红移。样品在355 nm波长激发下产生了384 nm的紫外发射峰和440 nm的蓝光发射带,并随ZnO含量的增加而增强,它们分别来自ZnO的电子-空穴复合发光和缺陷发光,及ZnO/SiO₂复合薄膜双层结构的缺陷发光。     

纳米磷化镓粉体中混杂石墨和金刚石微晶的拉曼光谱分析

利用Raman光谱并结合能量色散X射线显微分析(EDX)和X射线衍射图谱(XRD)对混杂于纳米磷化镓粉体内的石墨和金刚石纳米微晶进行了分析。结果表明,在纳米GaP粉体Raman光谱中,位于1324 cm-1和1572 cm-1的两个宽强散射谱带分别归属于金刚石的F2g模和石墨的E2g模振动。EDX结果证实纳米GaP粉体材料中含有碳元素。XRD图谱中出现了石墨和金刚石的低晶面指数衍射峰。     

Raman and X‐ray diffraction analysis on unburned carbon powder refined from fly ash

The bonding and crystalline structures of oil‐fried fly ash collected from a power plant were analyzed by using Raman spectroscopy and X‐ray diffraction (XRD), respectively. These carbon powders underwent a series of annealing treatment for graphitization and crystallization. In Raman spectra, the refined, unburned carbon contains clearly the D, G and D′ peaks under 2000 or 2700 °C treatment. The Raman spectral line shape of refined, unburned carbon heated at 2700 °C is similar to that of commercial graphite made from graphitization process. In the XRD spectra, the refined, unburned carbon contains (002), (100) and (004) diffraction peaks under heating at 2000 or 2700 °C. The XRD spectral line shape of refined, unburned carbon heated at 2700 °C is similar to that of a commercial graphite bar. The quantitative graphitization level from Raman spectra and crystallization degree from XRD spectra on refined, unburned carbon powders serve as preliminary guide for the qualitative evaluation of these unburned carbon powders. Copyright © 2009 John Wiley & Sons, Ltd.     

Raman identification of lonsdaleite in Popigai impactites

Micro‐Raman spectroscopy and X‐ray diffraction method (XRD) were used to characterize impact carbonaceous rocks excavated from the Popigai crater (Siberia). The deconvolution of the first‐order Raman spectra of the rocks containing different amounts of carbon phases (diamond, lonsdaleite and graphite) allowed the identification of lonsdaleite spectrum. The most intensive band at 1292–1303 cm⁻¹ was ascribed to A_1g vibration mode of lonsdaleite, whereas the less intense band at 1219–1244 cm⁻¹ was attributed, in agreement with previously reported ab initio calculations, to E_2g vibration mode. The established correlation between the intensities of Raman and XRD peaks permits a rough estimation of lonsdaleite/diamond phase ratio in the impact rocks using micro‐Raman measurements. The second‐order Raman spectra of lonsdaleite–diamond rocks were recorded. Copyright © 2014 John Wiley & Sons, Ltd.     

炸药爆轰合成纳米金刚石的拉曼光谱和红外光谱研究

用负氧平衡炸药爆轰法合成纳米金刚石,并用粉末X射线衍射(XRD)仪、激光Raman光谱仪和红外光谱仪等分析仪器对其结构进行表征。XRD结果表明,纳米金刚石为立方结构,由于其内部结构的高密度缺陷、杂质原子的夹杂使谱线偏离,晶格常数比静压合成的大颗粒金刚石大0.72%。由于金刚石晶粒细小,Raman光谱特征峰产生宽化,并且向小波数方向偏移了3 cm-1,此外在纳米金刚石中还含有极少量的石墨。红外光谱测试结果中,3 422 cm-1吸收峰为O—H伸缩振动峰;在1 634 cm-1出现了H₂O的弯曲振动峰,表明在纳米金刚石样品粉末中含有水分;2 930和2 857 cm-1是CH₂的反对称和对称伸缩振动吸收峰;2 971 cm-1是CH₃的反对称伸缩振动吸收峰,说明样品中存在极少量的碳氢化合物;1 788 cm-1吸收峰为CO伸缩振动吸收峰。文章从纳米金刚石的生成机理上分析了产生这些峰位的原因,结果表明纳米金刚石属于Ⅰ型金刚石,在它之中含有ⅠaA型和Ⅰb型金刚石,ⅠaA型金刚石的含量比Ⅰb型金刚石多。     

Preparation of nanodiamonds by laser irradiation of graphite

Graphite powders were irradiated by pulsed laser at room temperature and normal pressure and then boiled in perchloric acid. Samples were characterized by high-resolution transmission electron microscopy (HRTEM), electron diffraction pattern (EDP), X-ray diffraction (XRD) pattern, and Raman spectroscopy.The analyses on the HRTEM images, EDP, and XRD show that the diamond particles with a size of about 5 nm are obtained. The shifting and broadening of the diamond peak in Raman spectrum indicate that there are high defect density and residual internal stress in synthetic diamond.     

Growth and Characteristics of Freestanding Hemispherical Diamond Films by Microwave Plasma Chemical Vapor Deposition

Freestanding hemispherical diamond films have been fabricated by microwave plasma chemical vapor deposition using graphite and molybdenum （Mo） as substrates. Characterized by Raman spectroscopy and scanning electron microscopy, the crystalline quality of the films deposited on Mo is higher than that on graphite, which is attributed to the difference in intrinsic properties of the two substrates. By decreasing the methane concentration, the diamond films grown on the Mo substrate vary from black to white, and the optical transparency is enhanced. After polishing the growth side, the diamond films show an infrared transmittance of 35-60% in the range 400-4000 cm^- 1.     

Investigating the mechanisms of diamond polishing using Raman spectroscopy

Recent research has shown that a phase transformation of diamond to a different form of carbon is involved when diamonds are polished in the traditional fashion. The question as to how this phase transformation is activated and maintained to produce high wear rates is of great technological interest since it may radically change the way we view the processing of diamond. This paper describes the use of Raman spectroscopy to examine debris produced on the diamond polishing wheel, both during its preparation and during polishing. In addition, polished diamond surfaces were examined for the possible existence of non-diamond surface layers in an attempt to identify material removal mechanisms. Raman spectroscopy proves ideal for these analyses because its relatively high spatial resolution is well suited to the analysis of small wear features and debris particles, and because of the wealth of information it reveals about chemical structure. This level of structural information has been lacking in previous analyses of diamond polishing debris. In addition to the non-diamond carbon found in the wear debris, significant quantities of two iron oxides, magnetite (Fe₃O₄) and haematite (α-Fe₂O₃), were also found. An interesting observation was that a transformation from magnetite to haematite could be induced either by using high power laser excitation or by frictional heating during polishing. It is suggested that some of the Raman peaks previously attributed to lonsdaleite might better be explained by the presence of these oxides.     

膨胀石墨的Raman光谱研究

以波长为514.5nm的激光对550-920℃制备的膨胀石墨进行了Raman光谱研究,结果表明:膨胀石墨的Raman光谱与高取向热解石墨基本相同,分别在~1350、~1580、~2445、~2725、~3248和~4300cm-1处出现了相应的Raman位移;其中位于~1350、~2445和~4300cm-1的Raman峰位随着制备温度的不同会发生较大的移动,而不同温度制备的膨胀石墨位于~1580、~2725、~3248cm-1处的三个Ra-man峰位基本接近;~2725 cm-1处的二阶模包含两个分别位于2707和2730cm-1处的Raman峰。膨胀石墨的D模与G模强度比ID/IG随着温度升高下降,而D线的二阶模D*峰强ID*与IG的比值ID*/IG的大体变化趋势是随着温度升高而增大。     

Synthesis of carbides in the arc plasma

A method of synthesis of iron, silicon, titanium, and tungsten carbides in an argon arc between graphite electrodes is developed. It is found that iron, silicon, and titanium atoms introduced into the interelectrode gap cause the voltage drop across the gap to decrease, whereas tungsten atoms increase this voltage. The X-ray diffraction analysis of synthesized powders reveals carbide and graphite crystallites. Their relative concentrations are estimated from the intensities of the respective reflection peaks. The morphological examination of the synthesized particles shows that titanium carbide particles are the largest and iron carbide ones are the finest. Raman spectra taken of the powders confirm the presence of graphite and carbide crystallites.     

Growth mechanism and photoluminescence of the SnO2 nanotwists on thin film and the SnO2 short nanowires on nanorods

SnO2 nanotwists on thin film and SnO2 short nanowires on nanorods have been grown on single silicon substrates by using Au-Ag alloying catalyst assisted carbothermal evaporation of SnO2 and active carbon powders.The morphology and the structure of the prepared nanostructures are determined on the basis of field-emission scanning electron microscopy(FESEM),transmission electron microscopy(TEM),selected area electronic diffraction(SAED),high-resolution transmission electron microscopy(HRTEM),x-ray diffraction(XRD),Raman and photoluminescence(PL) spectra analysis.The new peaks at 356,450,and 489 nm in the measured PL spectra of two kinds of SnO2 nanostructures are observed,implying that more luminescence centres exist in these SnO2 nanostructures due to nanocrystals and defects.The growth mechanism of these nanostructures belongs to the vapour-liquid-solid(VLS) mechanism.