纳米SiO2／CeO2复合磨粒的制备及其抛光特性研究

以尿素[CO(NH2)2]、(NH4)2Ce(NO3)6和SiO2为原料,采用均相沉淀法制备1种新型纳米SiO2/CeO2复合磨粒,通过X射线衍射仪、X射线光电子能谱仪、飞行时间二次离子质谱仪和扫描电子显微镜等分析手段对其结构进行表征,并将SiO2/CeO2复合磨粒配置成抛光液在数字光盘玻璃基片上进行化学机械抛光试验.结果表明:所制备的SiO2/CeO2复合磨粒的平均晶粒度为19.64 nm,粒度分布均匀;经过1 h抛光后,玻璃基片的平均表面粗糙度(Ra)由1.644 nm降至0.971 nm;抛光后玻璃基片表面变得光滑、平坦,表面微观起伏较小.     

氧化硅/氧化铁复合磨粒用于硬盘基片的抛光研究

本文以HNO3、NaOH、Fe(NO3)3和SiO2浆料为原料,采用沉淀法制备了1种SiO2/Fe2O3复合磨粒,通过X射线衍射仪(XRD)、飞行时间二次离子质谱仪(TOF-SIMS)和扫描电子显微镜(SEM)对其结构进行表征,结果表明Fe2O3包覆到SiO2的表面,复合粒子具有很好的分散性.用UNIPOL-1502抛光机研究了所制备复合磨粒在镍磷敷镀的硬盘基片中的抛光性能,抛光后硬盘基片的表面粗糙度Ra由抛光前的8.87nm降至3.73nm;抛光后表面形貌的显微镜观测结果表明新制备的复合磨粒表现出较好的抛光性能.     

包覆型纳米CeO2@SiO2复合磨料的制备?表征及其抛光性能

以无水乙醇为溶剂,氨水为催化剂,利用正硅酸乙酯(TEOS)水解,并在500℃下煅烧1h,制备了SiO2粉体.将SiO2粉体作为内核浸渍到以硝酸亚铈、乙酰丙酮和正丙醇为原料制备的铈溶胶中,得到包覆型CeO2@SiO2复合粉体.利用XRD、SEM、TEM和FT-IR等测试手段,对所制备样品的物相结构、形貌、粒径大小、团聚情况进行表征.将所制备的包覆型CeO2@SiO2复合粉体配制成抛光浆料用于砷化镓晶片的化学机械抛光,用原子力显微镜(AFM)观察抛光表面的微观形貌,测量表面粗糙度.结果表明,采用浸渍工艺成功制备出单分散球形,粒径在400～450nm,负载均匀的包覆型CeO2@SiO2复合粉体.复合粉体中CeO2的包覆量随着铈溶胶中铈离子浓度的升高而增大.经包覆型CeO2@SiO2复合磨料抛光后的砷化镓晶片表面的微观起伏更趋于平缓,在1μm×1μm范围内表面粗糙度Ra值为0.819nm,获得了具有亚纳米量级粗糙度的抛光表面.     

核-壳结构PS/CeO_2复合磨料的制备及其氧化物化学机械抛光性能

以无皂乳液聚合方法制备的聚苯乙烯(PS)微球为内核,硝酸铈为铈源,六亚甲基四胺为沉淀剂,采用液相工艺制备了PS/CeO2复合颗粒.利用XRD、TEM、SAED、FESEM、EDAX等手段,对所制备样品的物相结构、形貌、粒径大小和元素成分组成进行表征.将所制备的复合磨料用于硅晶片热氧化层的化学机械抛光,用AFM观察抛光表面的微观形貌,并测量表面粗糙度.结果表明,所制备的PS/CeO2复合颗粒具有核-壳结构,呈近似球形,粒径在250～300nm,PS内核表面被粒径在5～10nm的CeO2纳米颗粒均匀包覆,壳层的厚度为10～20nm.抛光后的硅热氧化层表面在5μm×5μm范围内粗糙度Ra值和RMS值分别为0.188nm和0.238nm,抛光速率达到461.1nm/min.     

激光熔覆NiCr-ZrB2复合涂层结构及高温摩擦学性能

利用激光熔覆技术在纯钛表面制备了NiCr涂层和NiCr-ZrB2复合涂层.用X射线衍射仪、扫描电镜和高分辨透射电镜分析了涂层的组成、组织结构和晶体结构.在SRV-IV摩擦磨损试验机上对NiCr-ZrB2复合涂层从20到500℃的摩擦磨损性能进行了测试.结果表明:NiCr-ZrB2复合涂层的主要物相组成为[Ni,Ti]固溶体、Cr2Ti、ZrB2、ZrB、Ni3Cr2、Ti2Cr、TiB2和TiB;涂层厚约0.7～1.0 mm;涂层平均硬度约为HV0.21000,是纯钛基材的5.3倍;NiCr-ZrB2复合涂层的摩擦系数和磨损体积随温度的增加而减小,高温耐磨性能相对于钛基材提高约1个数量级;NiCr-ZrB2复合涂层的磨损机理为磨粒磨损和黏着磨损,高温下伴有氧化磨损和摩擦抛光现象.     

Ce0.8Zr0.2O2固溶体磨料对ZF7光学玻璃抛光性能的改善

采用改进的湿固相机械化学反应法制备出超细锆掺杂氧化铈磨料Ce1-xZrxO2(x=0,0.2),运用X射线衍射(XRD)、透射电镜(TEM)等手段表征其物相类型、外观形貌、比表面积、粒度、表面电位等物理性质,通过测定抛光速率和观察表面的微观形貌考察它们对ZF7光学玻璃的抛光性能影响.结果表明,Ce0.8Zr0.2O2固溶体磨料对ZF7光学玻璃抛光性能比纯CeO2磨料有明显的提高,抛光速率达到463 nm/min,5.0 μm×5.0 μm的范围内微观表面粗糙度Rα值达到1.054 nm,而纯CeO2磨料的抛光速率只有292 nm/min,Rα值却增大到1.441 nm.Ce0.8Zr0.2O2固溶体的抛光速率的明显增大和表面粗糙度Rα的下降主要与其负表面电位的增大和颗粒尺寸、粒度的减小密切相关.     

壳层形态对核/壳结构PS/SiO_2复合磨料抛光性能的影响

以聚苯乙烯(PS)微球为内核,通过控制正硅酸乙酯的水解过程制备具有不同壳层形态的核/壳结构PS/SiO2复合磨料,应用于二氧化硅介质层的化学机械抛光,借助AFM测量抛光表面的形貌、轮廓曲线及粗糙度.SEM和TEM结果显示:碱性水解条件下,复合磨料的壳层由SiO2纳米颗粒组成(非连续壳层);酸性条件下,复合磨料的壳层则呈无定型网状(连续壳层).抛光对比试验结果表明:复合磨料的PS弹性内核有利于降低表面粗糙度并减少机械损伤,SiO2壳层则有利于提高材料去除率,复合磨料的核/壳协同效应对于提高抛光质量具有主要影响.相对于非连续壳层复合磨料,具有连续壳层的PS/SiO2复合磨料能够得到更低的抛光表面粗糙度值(RMS=0.136 nm),且在抛光过程中表现出了更好的结构稳定性.然而,PS/SiO2复合磨料的壳层形态对抛光速率的影响则不明显.     

纳米CeO2颗粒的制备及其化学机械抛光性能研究

以硝酸铈和六亚甲基四胺为原料制备出不同粒径的纳米CeO2粉体颗粒,将纳米CeO2粉体配制成抛光液并用于砷化镓晶片的化学机械抛光.结果表明,不同尺寸的纳米磨料具有不同的抛光效果,采用粒度8 nm的CeO2磨料抛光后微观表面粗糙度最低(0.740 nm),采用粒度小于或大于8 nm的CeO2磨料抛光后其表面粗糙度值均较高.通过简化的固-固接触模型分析,认为当粒度过小时,磨料难以穿透软质层,表现为化学抛光为主,表面凹坑较多,表面粗糙度较高;当粒度大于一定值时,随着磨料粒度增加,嵌入基体部分的深度加大,使得粗糙度出现上升趋势.提出当磨料嵌入晶片表面的最大深度等于或接近于软质层厚度时,在理论上应具有最佳的抛光效果.     

缓蚀剂在铜化学机械抛光过程中的作用研究

利用柠檬酸体系抛光液研究了苯并三氮唑(BTA)缓蚀剂对铜化学机械抛光过程和抛光效果的影响,并通过X射线光电子能谱仪、紫外可见吸收光谱仪及表面电位测试和电化学分析等手段分析了抛光液中BTA缓蚀剂在铜化学机械抛光过程中的作用机理.结果表明,当H2O2存在时,抛光液中BTA作为阳极缓蚀剂吸附在抛光表面,提高了阳极铜溶解的平衡电位,并通过缩合反应生成保护膜,减小了抛光后的表面粗糙度,提高了表面质量,同时在一定程度上增加了抛光过程中的摩擦系数.另外,BTA对SiO2抛光磨粒具有一定的吸附作用,进而对抛光效果产生一定的影响,抛光磨粒表面吸附层的存在会减小抛光过程中的摩擦系数.     

水基MWCNTs/MoS2复合纳米流体的摩擦学性能研究

使用离子液体[EMIm]BF₄分散多壁碳纳米管(MWCNTs),再以[EMIm]BF₄-阿拉伯树胶(GA)为添加剂分散二硫化钼(MoS₂),二者的水溶液复配得到复合纳米流体. 采用拉曼光谱分析了MWCNTs的改性度,通过吸光度和粒度对复合纳米流体的分散与悬浮稳定性进行了表征. 对不同纳米颗粒配比的复合纳米流体润湿性能和摩擦学性能进行测试,结果表明:MWCNTs和MoS₂质量分数为0.6%、1.2%时复合纳米流体的铺展成膜能力最好,其接触角约为63.04°,相比于去离子水降低了23.55%. 摩擦磨损测试结果也表明此配比下的减摩抗磨性能最佳,平均摩擦系数为0.073,比去离子水降低了61.98%,同时体积磨损率降低了67.87%. 磨痕形貌观测表明,最优配比下磨痕浅,且表面光滑、无犁沟. X射线光电子能谱(XPS)表明MWCNTs和MoS₂共同参与摩擦并在基底成膜,由此协同实现了高效润滑.      

Measurement of the concentration diffusion coefficient for Ne-Ar, Ne-Xe, Ne-H2, Xe-H2, H2-N2 and H2-O2 gas systems

The concentration diffusion coefficient, D ₁₂, is measured for the equimolar mixtures of Ne-Ar, Ne-Xe, Ne-H₂, Xe-H₂, H₂-N₂ and H₂-O₂ binary gas systems in a two-bulb metal apparatus in the temperature range 0 C to 100 C. These values are compared with the existing data on these systems and with the predictions of the kinetic theory in conjunction with the modified Buckingham exp-six potential. Unlike the thermal diffusion coefficient, with the simple theory it is possible to predict D ₁₂ within a few percent even for systems involving polyatomic gases. The smoothed experimental D ₁₂ values are also used to obtain data for the coefficients of viscosity and thermal conductivity at round temperatures and compositions for these systems.Nomenclature C ₂ ^t relative amount of a gas in the mixture in the bulb 2 at an instant t - C ₂ relative amount of the same gas in the mixture in the bulb 2 at equilibrium - D ₁₂ diffusion coefficient - X ₁ mole-fraction of the heavier component in the mixture - _mix viscosity coefficient - _mix thermal conductivity coefficient     

Structure cellulaire de la détonation des mélanges H2–NO2/N2O4Cellular structure of the detonation of gaseous mixtures H2–NO2/N2O4

Calculations of the detonation reaction zone of gaseous reactive mixtures of NO₂/N₂O₄ as oxidizer and H₂, CH₄ or C₂H₆ as fuel, in the range of equivalence ratio Φ between 0.5 and 2, show that, for Φ?1, the chemical energy is released in two distinct and successive exothermic steps with different chemical induction times. The first exothermic stage is mainly due to the reaction NO₂+H→NO+OH, NO being the main oxidizer of the second one.The experimental study conducted on the same range of equivalence ratio (0.5?Φ?2) shows that, for Φ?1, the detonation wave of these mixtures contains a double set of cellular structures. A similar result had already been obtained with the detonation of gaseous Nitromethane, the NO₂ group being here included in the molecule. Consequently, the oxidizer NO₂ being either initially separated from the fuel or included inside the molecule of a monopropellant (Nitromethane) is responsible, because of its specific chemical kinetics, of a chemical energy release in two main steps and of the existence of a double cellular structure in the detonation wave for the same range of equivalence ratio. These results reinforce the assumption that the cellular structure of the detonation finds its origin in the strong rates of chemical energy release inside the reaction zone. To cite this article: F. Joubert et al., C. R. Mecanique 331 (2003).     

Kinetics of ultrafine coating of SiO2 nanoparticles, suspended in non-thermal CH4/C2H6 plasma

Capacitively coupled RF discharges in methane and ethane (1000–3000 Pa, 5–15 W/cm³) were used for the in-flight coating of SiO₂ nanopowders (NP) with an a-C:H layer [A. Kouprine, F. Gitzhofer, M. Boulos, A. Fridman, Polymer-like C:H thin film coating of nanopowders in capacitively coupled RF discharge, Plasma Chemistry and Plasma Processing 24 (2) (2004) 189–215]. In this present work a model of the chemical kinetics of this plasma processing has been developed, based on the GRI-Mech 3.0 mechanism [G.P. Smith, D.M. Golden, M. Frenklach, Gas Research Institute, Detailed chemical reaction mechanism. Available from: ], and calculations are performed, using the Chemkin-II code. The model includes the formation of two solid phases: an amorphous C:H coating, deposited on the suspended NP, and soot, incepted in the gas phase. Non-equilibrium plasma effects are taken into account by the rates of radical species’ production, using the reference data on the “G-value”. The CH₃ and H species appear to have key roles in surface activation and the nanofilm growth. The results demonstrate the competitive character of the formation of the two solid phases: the C:H coating is dominant under T_gas < 1400–1600 K, depending on the conditions, and soot commencing to dominate at higher temperatures. This division corresponds to the passage from non-thermal plasma conditions, with the dominance of single-valent radicals and solid phase growth on the substrate only, to the plasma thermalisation with the formation of two-valent radicals and v. inception of the solid phase. The results are validated experimentally by the observation of soot formation as a function of the gas temperature, by the mass spectrograph data on the gas composition after plasma reforming, and by the reference data on coating growth rates and induction times for soot formation.     

Spatiotemporal variations of PM2.5 and PM10 concentrations between31 Chinese cities and their relationships with SO2,NO2,CO and O3

The variations of mass concentrations of PM_2.5,PM₁₀,SO₂,NO₂,CO,and O₃ in 31 Chinese provincial capital cities were analyzed based on data from 286 monitoring sites obtained between March 22,2013 and March 31,2014.By comparing the pollutant concentrations over this length of time,the characteristics of the monthly variations of mass concentrations of air pollutants were determined.We used the Pearson correlation coefficient to establish the relationship between PM_2.5,PM₁₀,and the gas pollutants.The results revealed significant differences in the concentration levels of air pollutants and in the variations between the different cities.The Pearson correlation coefficients between PMs and NO₂ and SO₂ were either high or moderate(PM_2.5 with NO₂:r=0.256-0.688,mean r=0.498;PM₁₀ with NO₂:r = 0.169-0.713,mean r = 0.493;PM2.5 with SO₂:r= 0.232-0.693,mean r=0.449;PM₁₀ with SO₂:r = 0.131-0.669,mean r=0.403).The correlation between PMs and CO was diverse(PM_2.5:r = 0.156-0.721,mean r=0.437;PM₁₀:r=0.06-0.67,mean r= 0.380).The correlation between PMs and O₃ was either weak or uncorrelated(PM_2.5:r--0.35 to 0.089,mean r=-0.164;PM₁₀:r=-0.279 to 0.078,mean r=-0.127),except in Haikou(PM2.5:r=0.500;PM₁₀:r-0.509).     

Measurement of propagation speeds in adiabatic cellular premixed flames of CH4 + O2 + CO2

Experimental measurements of the propagation speed of adiabatic flames of methane + oxygen + carbon dioxide are presented. The oxygen content O₂/(O₂ + CO₂) in the artificial air was 31.55% and 35%. Non-stretched flames were stabilized on a perforated plate burner at atmospheric pressure. A heat flux method was used to determine propagation speeds under conditions when the net heat loss of the flame is zero. Under specific experimental conditions the flames become cellular; this leads to significant modification of the flame propagation speed. The onset of cellularity was observed throughout the stoichiometric range of the mixtures studied. Measurements in cellular flames are presented and compared with those for laminar flat flames. Cellularity disappeared when the flames became only slightly sub-adiabatic. Visual and photographic observations of the flames were performed to quantify their cellular structure. Increasing the oxygen content in the artificial air and increasing the temperature of the burner plate led to increase of the number of cells observed.     

Etude de la détonation de mélanges pauvres H2NO2/N2O4

Calculations of the detonation reaction zone of gaseous H₂NO₂/N₂O₄ mixtures in the range of equivalence ratio Φ between 0.25 and 0.7 show that for 0.25Φ0.4 the chemical energy is released in two distinct and successive exothermic steps characterised by different chemical characteristic times. As for rich mixtures, the first exothermic step is mainly due to the reaction NO₂ + H → NO + OH, but the second one is different since it results from the exothermic decomposition of NO into N₂ and O₂. For Φ=0.3 the measured detonation velocity in a tube of 52 mm internal diameter is very much smaller than the calculated value and the mean size of the cellular structure is very much larger than the value extrapolated from data obtained with mixtures of higher but close equivalence ratio. All these results show that the detonation, though self-sustained and steady, is ‘non-ideal’, i.e. it is supported only by a part of the available chemical energy, that provided mainly by the first exothermic step. To cite this article: D. Desbordes et al., C. R. Mecanique 332 (2004).     

KH2PO4/SiO2复合粉体抑制铝粉爆燃效果及机理分析

为研究KH₂PO₄/SiO₂复合粉体抑爆剂对铝粉爆燃的抑制作用,采用球磨机将KH₂PO₄和SiO₂混合研磨制备出新型的KH₂PO₄/SiO₂复合粉体抑爆剂。在哈特曼管实验装置上,开展爆燃火焰传播抑制实验,结果表明:随着KH₂PO₄/SiO₂复合粉体抑爆剂含量的增加,爆燃火焰传播长度和速度逐渐减小,当添加质量比10∶6的KH₂PO₄/SiO₂复合粉体抑爆剂时,可实现铝粉爆燃火焰传播的抑制。在20 L球形爆炸装置上,开展复合粉体抑爆剂抑制铝粉爆炸压力测试实验,结果表明:随着KH₂PO₄/SiO₂复合粉体抑爆剂含量的增加,铝粉爆炸最大爆炸压力p_max和最大爆炸压力上升速率(dp/dt)_max逐渐减小,当添加质量比10∶9的KH₂PO₄/SiO₂复合粉体抑爆剂时,可实现铝粉爆燃的完全抑制。通过KH₂PO₄粉体、SiO₂粉体与复合粉体抑爆剂对比可知,复合粉体抑爆剂对铝粉火焰传播和爆炸压力的抑制效果都优于单体粉体抑爆剂。通过对铝粉在空气中燃烧的热分析研究,从化学和物理两个方面分析了KH₂PO₄/SiO₂复合粉体抑爆剂对铝粉爆燃的抑制机理。     

等离子喷涂Al2O3/TiO2纳米复合涂层的制备、结构及摩擦学性能

采用喷雾干燥法对溶胶-凝胶法合成的系列A l2O3/TiO2纳米复合粉体进行造粒,使用等离子喷涂技术制备系列A l2O3/TiO2纳米复合涂层.对涂层结构和形貌分析表明所制备的A l2O3/TiO2纳米复合涂层形成了具有熔融区和半熔融区的双区形态的纳米复合结构.使用UMT-2MT试验机研究了复合涂层的摩擦磨损性能,结果表明复合涂层的磨损率随TiO2含量的增加表现出先降低而后增大的趋势,TiO2质量百分数为10%的纳米复合涂层的磨损率最低;而涂层的摩擦系数随TiO2含量的增加变化不大.复合涂层的磨损机制为裂纹扩展导致的磨损剥落.     

Ar稀释C2H2+2.5O2预混气高频爆轰的端面结构

为了研究预混气爆轰的内部结构,对不同浓度的Ar稀释的C₂H₂+2.5O₂预混气进行爆轰实验和数值计算。首先,在内径63.5 mm的管道内进行爆轰实验,使用烟熏玻璃记录了不同初始压力下C₂H₂+2.5O₂预混气的爆轰端面结构。使用数字化图像处理技术来分析烟熏玻璃记录的三波点轨迹,以减少人为误差。然后,观察实验结果并描绘规则图形,图像识别程序经过验证后,用于分析实验结果。从端面结构中对封闭图形进行圆的拟合,用胞格半径方差来表示胞格大小的均匀程度;用相邻胞格圆心距的方差来表示胞格分布的规则程度。通过对比不同Ar稀释下半径方差和圆心距方差随胞格数量的变化,给出不同浓度Ar稀释下C₂H₂+2.5O₂预混气的端面胞格尺寸及分布规律,随着Ar浓度的升高,预混气端面胞格分布更加规律。