纳米CeO2在水相介质中的分散性能研究

通过对纳米CeO2悬浮液体系中颗粒的表面电性进行测定,采用无机电解质类分散剂(SHP)和非离子型表面活性剂聚乙烯吡咯烷酮(PVP)对纳米CeO2粉体进行了分散实验,研究了超声分散时间及表面活性剂浓度对纳米CeO2粉体在水相介质中分散性能的影响.结果表明,随超声时间的增加,纳米CeO2粉体的分散性增强;随分散剂浓度的增加,纳米CeO2粉体的分散性呈先增后减的变化规律.纳米CeO2粉体在水相介质中的分散工艺为:超声时间20min,浓度为2.0%的SHP.     

超声辐射醇水体系制备纳米CeO2粉体及其抛光性能研究

在超声辐射条件下,使用正丁醇/水反应体系通过均相沉淀法制备了纳米CeO2粉体;将所制备的纳米CeO2粉体作为磨料对硅晶片进行抛光,用原子力显微镜观察抛光表面的微观形貌并测量表面粗糙度;研究了超声场以及醇/水反应体系对纳米CeO2粉体粒径和团聚情况的影响,考察了纳米CeO2磨料对硅晶片的抛光效果。结果表明:超声辐射以及醇/水反应体系均有利于制备出粒径更小,且分散性更好的纳米CeO2粉体;使用纳米CeO2磨料抛光的硅晶片表面最终在2μm×2μm范围内的微观粗糙度值为Ra0.108nm,而且抛光表面非常平整。     

双液超声雾化反应制备纳米CeO_2粉体

以硝酸铈和碳酸氢铵为原料,用双液超声雾化反应法制备了纳米CeO2粉体;用X射线衍射仪和透射电子显微镜分析了雾化温度、焙烧温度、雾化液浓度、表面活性剂等因素对粉体颗粒尺寸和形貌的影响.结果表明:前驱体的物相组成与雾化温度有关,雾化温度60℃时制备的纳米CeO2颗粒团聚现象较轻、均匀性好;培烧温度的提高会使纳米CeO2颗粒迅速长大,比表面积大大减小,200℃焙烧较好;雾化液浓度的减小对颗粒尺寸影响不大,但会使其团聚状况有明显减轻,优化的浓度为0.2 mol·L-1;表面活性剂的加入有利于降低雾化液的表面张力,加入体积分数10%乙醇+0.5%聚乙二醇后,有利于生成更细小、粒径更加均匀的球形颗粒;在以上最佳工艺条件下制备的CeO2颗粒尺寸为3 Nm.     

分散剂对蛇纹石在乙醇中分散性能的影响

通过对高能球磨法制备的超细蛇纹石Zeta电位的测量,选用不同分散剂,分别研究了不同超声时间和分散剂加入量条件下,聚乙烯吡咯烷酮(PVP)、油酸(OA)、十二烷基苯磺酸钠(SDBS)和三乙醇胺(TEA)4种分散剂对蛇纹石粉体在无水乙醇中分散性能的影响。并对PVP作用的蛇纹石粉体进行了红外表征。研究结果表明,粉体的分散效果随着超声时间和表面活性剂加入量的增加呈现先增大后减小的趋势;不同分散剂分散效果从高到低顺序依次为PVP,油酸,十二烷基苯磺酸钠,三乙醇胺。最佳分散工艺为:pH=10,PVP质量分数2.5%,超声功率560W,超声时间43min。     

SiCp/Cu复合材料的显微组织和力学性能

采用非均相沉淀包裹法制得铜包SiC复合粉体,利用热压烧结工艺制备了含有体积分数为20%～65%SiC颗粒的SiCp/Cu复合材料.用X射线衍射仪、扫描电镜、能谱分析等测试方法对试样进行了成分和微观形貌分析.结果表明:包裹法制得的SiCp/Cu复合材料中基体铜形成连续的结构,SiC分散较均匀;随着SiC含量的增加,试样孔隙率提高,抗弯强度下降;而硬度则先增后降,并在SiC体积分数为35%时出现最大值;所有试样均表现为脆性断裂.     

Ti2AlC粉末粒径分布对TiC0.5-Al2O3/Cu复合材料组织及性能的影响

通过不同时间的湿法球磨得到不同粒径分布的Ti₂AlC粉末,再与Cu₂O粉末和铜粉末混合,利用放电等离子烧结技术制备TiC_0.5-Al₂O₃/Cu复合材料,研究了Ti₂AlC粉末粒径分布对其组织和性能的影响。结果表明：随着Ti₂AlC粉末中亚微米级颗粒体积分数由0增加到70.27%,复合材料中增强相颗粒TiC_0.5和Al₂O₃在基体中分散更均匀,但是当亚微米级颗粒体积分数为98.07%时,增强相颗粒出现聚集现象;随着亚微米级颗粒体积分数的增加,复合材料的导电率与相对密度先减小后增大,硬度与屈服强度则先升后降,当亚微米级颗粒体积分数为70.27%时,复合材料综合性能最优异。     

醇水均匀沉淀法制备纳米CeO2粉体工艺及机理研究

在醇-水体系中以六亚甲基四胺（HMT）为缓释沉淀荆制备了纳米CeO2粉体，并用TEM和BET对其进行了表征，考察了制备过程中工艺参数对CeO2粉体颗粒大小及团聚的影响，并对影响机理进行了探讨。结果表明：在较佳工艺条件下制备的纳米CeO2平均尺寸约为8nm，与传统的水溶液均匀沉淀法相比较，该方法得到的粉体粒径更小，且分散性好。     

表面活性剂含量对氧化铈/氧化硅复合磨料分散性的影响

以乙醇为溶剂及表面活性剂,以氨水为催化剂,利用正硅酸乙酯的水解得到氧化硅颗粒,并分析乙醇质量92%时制备的氧化硅颗粒呈球形,粒径分布均匀,表面光滑,呈单分散状态;乙醇质量分数为96%时制备的氧化硅颗粒粒径分布范围大,并且小颗粒团聚一体,聚集到大颗粒上.基于理想的氧化硅颗粒,利用化学沉淀法制备CeO2/SiO2复合磨料,并通过透射电子显微镜(TEM)及X射线衍射仪(XRD)对制备的样品进行表征.结果表明,制备的CeO 2/SiO2复合磨料为球形,粒径为150分数对制备的氧化硅颗粒以及氧化铈/氧化硅复合磨料分散性的影响.结果表明:水解体系中乙醇质量分数为71%时制备的氧化硅颗粒基本呈球形,粒径分布范围大,呈少量单分散状态;乙醇质量分数为~250 n m ,具有草莓状核壳的包覆结构,作为抛光磨料可以提高抛光表面质量.     

工艺参数对醇水均匀沉淀法制备纳米CeO2颗粒粒径的影响

在醇水混合体系中以乙醇为溶剂,六次甲基四胺(HMT)为缓释沉淀剂采用均匀沉淀法制备了纳米CeO2粉体,用透射电子显微镜(TEM)、X射线衍射仪(XRD)等方法对纳米颗粒进行了表征,研究了醇水比、反应温度、反应时间对纳米颗粒粒径的影响.结果表明:随着乙醇含量的增加,纳米颗粒粒径逐渐减小,随着反应温度的升高和反应时间的延长,纳米颗粒粒径增大.     

水热法合成棒束状纳米CeO_2粉体及其催化性能

在醇-水体系中以P123为模板、硝酸铈和草酸为原料,利用水热法制备了棒束状纳米CeO2粉体,研究了反应温度、硝酸铈与草酸的物质的量比(nCH)、溶液pH以及反应时间对CeO2粉体颗粒的影响,确定了制备棒束状纳米CeO2粉体的最佳工艺参数;将最佳工艺参数下制得的CeO2对酸性品红溶液进行催化降解试验,并与块状CeO2催化降解结果进行对比。结果表明:制备棒束状纳米CeO2的最佳工艺参数为200℃、nCH=2∶3、pH=1、反应时间360 min;在此最佳工艺参数下制备的棒束状纳米CeO2对酸性品红溶液的催化活性比普通块状CeO2的大大提高。     

剪切增稠抛光磨料液的制备及其抛光特性

为了实现对工件的剪切增稠抛光(STP),采用机械混合与超声波分散法制备了一种Al2O3基STP磨料液,并研究了它们的抛光特性。利用应力控制流变仪考察其流变性能,通过扫描电镜和光学轮廓仪研究了单晶硅加工后表面显微组织的变化,并测量其表面粗糙度。结果表明:STP磨料液具有剪切变稀和可逆的剪切增稠特性,达到临界剪切速率后,会形成Al2O3"粒子簇";当剪切速率增大至1000s-1,储能模量,耗能模量和耗散因子都增至最大值,此时主要表现为类似固体的弹性行为,有利于形成类似"柔性固着磨具"。在STP加工单晶硅过程中,采用塑性去除的材料去除方式。随着抛光时间的延长,硅片去除速率先增大后减小;表面粗糙度不断减小并趋于稳定。实验显示,磨粒浓度不宜过高,否则会因剪切增稠效应造成黏度过大,导致流动性差而影响抛光质量。当Al2O3质量分数为23%时,抛光25min后,硅片表面粗糙度Ra由422.62nm降至2.46nm,去除速率达0.88μm/min,表明其能实现单晶硅片的高效精密抛光。     

大尺寸单晶金刚石衬底抛光技术研究现状与展望

近些年来,化学气相沉积（Chemical vapor deposition,CVD）单晶金刚石在电子学领域的应用令人瞩目,这得益于CVD单晶金刚石在生长技术和半导体掺杂技术上的进展。一直以来,成熟的衬底加工技术是半导体材料得以应用的基础,其中超精密抛光作为晶圆衬底加工的最后一道工序,直接决定了晶圆表面粗糙度和亚表面损伤程度。可以预见,超精密抛光技术将会在制备大尺寸高质量金刚石衬底中发挥重要作用。对目前国内外现有的单晶金刚石抛光方法进行综述,以制备大尺寸高质量单晶金刚石衬底为目标,从加工设备、工艺参数、加工精度、加工效率和材料去除机理等方面进行分析,总结各种抛光方法的优势和缺点,展望未来大尺寸单晶金刚石衬底抛光技术的发展趋势。目前鲜有针对大尺寸单晶金刚石抛光技术的综述,本文为国内学者展开单晶金刚石抛光相关工作的研究提供综述资料。     

Power law approximations to gas volume fraction and velocity profiles in low void fraction vertical gas–liquid flows

A dual sensor conductance probe was used to measure the distributions of the local gas volume fraction and the local gas axial velocity in vertical upward, bubby air–water flows in which the mean gas volume fraction was less than 0.1. Very limited data are available in the literature for such low volume fraction flows. The measured local gas volume fraction and velocity distributions were approximated by power law functions. The power law exponents associated with the measured local gas volume fraction profiles were found to be up to 30% higher than values predicted in the literature. The power law exponents associated with the measured local gas velocity profiles were also found to be somewhat higher than values predicted in the literature. The power law exponents for the measured local gas volume fraction and local axial gas velocity distributions at a given flow condition were combined to obtain an estimate of the ‘Zuber–Findlay’ distribution parameter C₀ at that flow condition. The mean value of C₀ for all of the flow conditions investigated was 1.09. This value of C₀ was found to give good agreement with the gradient of a plot of the mean gas velocity versus the homogeneous velocity u_h, where and u_h were obtained from reference measurements. This agreement is evidence for the good accuracy of the measured volume fraction and velocity profiles. Finally, the paper casts doubt upon previously published criteria regarding the optimum axial sensor separation in dual sensor probes.     

Microstructural analysis of Al alloys dispersed with TiB2 particulate for MMC applications

A dispersion of TiB₂ particulates in an Al alloy matrix was formed via the in-situ reaction between mixtures of K₂TiF₆ (K₂ZrF₆), KBF₄ and molten aluminium. The dispersion of the ceramic phase in the aluminium matrix was also achieved in some experiments by adding exogenous TiB₂ particles to the fluoride melt in contact with molten aluminium.
In this work, we have examined the microstructure of the as-cast metal matrix composites using analytical electron microscopy and X-ray diffraction techniques. The phases formed as a result of the reaction between the molten fluoride flux and liquid aluminium have been identified. These were (Ti, Zr, Al)B₂, Al₃Ti and possibly AlB₁₂ in the Al-matrix, and KAlF₄ and KMgF₃ in the solidified flux. The mechanism of formation of TiB₂ and Al₃Ti is explained. The role of alloying elements is also explained in the context of interfacial chemistry and dispersion.     

The effects of iron particles on the friction and wear mechanisms of ceramics in ethanol

For the combinations of an Si₃N₄ pin and five kinds of ceramic disk (SiC, Si₃N₄, Al₂O₃, ZrO₂, TiC), a friction and wear test was carried out in ethanol and in ethanol containing iron particles (1 wt.%, average diameter d = 200 nm, D = 12 μm under cohered condition) under a load in the range 5.88–11.50 N, at a sliding velocity of 0.138–0.196 m s⁻¹. A topographical analysis was also performed on the microasperities of the wear surfaces to estimate the behavior of the iron particles, and the degree of surface damage. As a result, the following facts were found. (1) The addition of iron particles in ethanol decreased both the wear rates of SiC and TiC disks and the mating pins, and also decreased the wear rate of the Al₂O₃ disk but increased that of the mating pin. The addition increased the wear rates of both ZrO₂ and Si₃N₄ disks and the mating pins. (2) The average coefficients of friction with the addition of iron particles were greater than those without iron particles. (3) The wear rates of pin and disk depended on the topographies of wear surfaces and the wear index Γ.     

Observation of removal of an Fmoc protecting group by scanning tunneling microscopy

We demonstrate here by imaging successive surface reactions in self-assembled monolayers (SAMs) on Au(1 1 1) at molecular scale with a scanning tunneling microscope (STM): (i) SAM matrices formation with 1-octanethiol on Au(1 1 1) in ethanol, (ii) insertion of N-Fmoc-aminooctanethiol into the SAM matrices in ethanol, and (iii) removal of the Fmoc protecting group with tris(2-aminoethyl)amine (TAEA). The total reaction is formation of SAMs containing a small amount of NH₂ terminated molecules in the CH₃ terminated SAM matrices. After the reaction of the protecting group with TAEA, STM imaging revealed the decrease in heights of the inserted molecules on average. We attributed this observation to removal of the protecting group by taking account of a convolution of electronic and topographic contributions to observed STM heights. Apparent areas of the terminal groups, however, became larger on removal. The increase in the areas was attributed to water adsorption to the NH₂ terminal group under air.     

Preparation of ultrafine α-AlO using precipitation-azeotropic distillation method

Ammonium aluminum carbonate hydroxide (AACH) was prepared by a precipitation-azeotropic distillation method, which uses aluminum sulfate as the Al source and ammonium carbonate as the precipitant. Then, AACH was calcined into ultrafine ?-Al₂O₃ powder. The factors that influence the dispersion property of ultrafine ?-Al₂O₃ powder are discussed in this paper, such as the methods of adding materials, surfactant, and drying methods. The changes of the structure and property of ultrafine alumina in the thermal treatment process are also studied. The morphological structure and properties of AACH are characterized by DTA/TGA, SEM, XRD, and ICP measurements. The results show that ultrafine ?-Al₂O₃ powder with a uniform particle size and well-distributed property can be synthesized only after aluminum sulfate atomizes into ammonium carbonate, proper amount of PEG1000 is added as the dispersant, and the product is treated by azeotropic distillation. The phase transformation of alumina during the calcination process can be described as amorphous Al₂O₃ → ?-Al₂O₃ → ?-Al₂O₃ → ?-Al₂O₃. The crystal grain size and density of ultrafine alumina powder increase with the increase of the calcination temperature. After AACH has been calcined at 1200°C for 2 h, the ultrafine ?-Al₂O₃ with uniform particle size, spherical shape, and more than 99.97% purity is obtained and its powder is well dispersed.     

电纺氧化锌纳米纤维乙醇、丙酮气敏传感器

研究了用静电纺丝技术制造微纳气体传感器的方法。采用PVP（Polyvinyl Pyrrolidone）/Zn（Ac）₂和PEO（Polyoxyethylene ）/Zn（Ac）₂两种混合溶液作为原料,通过电纺喷射获得了复合前驱体纳米纤维;在空气中加热至500℃去除聚合物,并使Zn（Ac）₂受热分解、氧化获得ZnO纳米纤维;利用X射线衍射术（XRD）对ZnO纳米纤维进行成分表征;最后实验检测了ZnO纳米纤维气敏传感器对乙醇和丙酮气体的传感特性。结果显示：以PVP/Zn（Ac）₂、PEO/Zn（Ac）₂复合纳米纤维为前驱体制得的ZnO纳米纤维平均直径分别为308 nm、184 nm;这种纳米纤维经加热氧化可获得高纯度ZnO纳米纤维;在室温条件ZnO纳米纤维气敏传感器对目标气体传感响应时间小于1 s,其传感灵敏值随着气体浓度的增大而升高。另外,以PEO/Zn（Ac）₂为前驱体制得的ZnO纳米纤维表面粗糙、比表面积大,具有较高的传感灵敏值,对于乙醇、丙酮两种目标气体的最高灵敏值分别为215.69和118.13。得到的结果表明：静电纺丝技术的引入为半导体微纳气敏传感器的集成制造提供了有效的方法。     

离子束溅射氧化钽薄膜的光学带隙特性

Ta_2O_5薄膜是可见光到近红外波段中重要的高折射率薄膜材料之一。本文针对离子束溅射制备Ta_2O_5薄膜的光学带隙特性开展了实验研究工作,基于Cody-Lorentz模型表征了薄膜的光学带隙特性,重点针对薄膜的禁带宽度和Urbach带尾宽度与制备参数之间的相关性进行研究。研究结果表明:在置信概率95%以上时,对Ta_2O_5薄膜禁带宽度影响的制备参数,权重大小依次为氧气流量、基板温度、离子束电压;而对Ta_2O_5薄膜Urbach带尾宽度影响的制备参数,权重大小依次为基板温度和氧气流量。对于Ta_2O_5薄膜在超低损耗激光薄膜和高损伤阈值激光薄膜领域内应用,本文的研究结果给出了同步提高薄膜的禁带宽度和降低带尾宽度的重要工艺参数选择方法。     

Electron microscopy study of different stages of oxidation of Ti-47Al-2Nb-2Cr-0.15B and Ti-45Al-15Nb at 900°C

The initial stage of oxidation of Ti-47Al-2Nb-2Cr-0.15B and Ti-45Al-15Nb alloys was studied. Studies reveal that the X and NbCr₂ phases will form in advance in the transition layer of the 2Nb2Cr alloy compared with the 15Nb alloy. The adherence between the nitride layer and underling layer is good. However, an obvious boundary exists between the mixed layer and the inner layer. The recrystallizing of the base alloy leads to an increase of the volume fraction of grain boundaries that can increase the oxidation rate at the initial oxidation stage. An Nb-based compound forms in the transition layer, which can prevent the formation of X phase.