稀释气体对化学气相沉积SiC涂层生长行为的影响

以CH3SiCl3-H2为反应气体,采用Ar和H2作为稀释气体。在1100℃、负压条件下,由化学气相沉积制备了SiC涂层,研究了稀释气体对涂层沉积速率、形貌以及晶体结构的影响。以Ar为稀释气体时,随着稀释气体流量的增加沉积速率迅速减小;用Ar作稀释气体制备的SiC涂层相对粗糙,随着Ar流量的增加,晶粒簇之间的空隙较大,涂层变得疏松。XRD分析表明：当稀释气体Ar流量超过200ml／min时,涂层中除了β-SiC外,还逐渐出现了少量的α-SiC。以H2为稀释气体时,当H2流量增加到400ml／min时,涂层的沉积速率迅速增大;以H2为稀释气体制备的SiC涂层致密、光滑,沉积的SiC涂层全部是β-SiC,且具有非常强的(111)晶面取向,涂层中无α-SiC出现。     

SiC14-CH4-H2系统沉积碳化硅动力学与微结构

Silicon carbide was prepared from SiCl4-CH4-H2 gaseous precursors by isothermal, isobaric chemical vapor deposition (CVD) at atmospheric pressure and temperatures ranging from 900°C to 1100°C. Kinetic studies showed that carbosilane of SiH2Cl2, SiHCl3 and SiCl2 formed from decomposition of SiCl4 and CH4 contributed to the deposition of hexangular facet and granular pebble structured SiC. An average apparent activation energy of 152 kJ•mol－1 was determined. The overall CVD process was controlled not only by the surface reactions but also by complex gas phase reactions. The as-deposited thin film was characterized using scanning electron microscopy, X-ray diffraction and transmission electron microscopy, these analysis showed that the deposited thin film consisted of pure phase of the β-SiC, the growth morphology of β-SiC differs from hexangular facet to granular pebble struc-tures, which varied with substrate length and CVD temperature.     

砷化镓上生长金刚石薄膜的研究

以CH4和H2为气源,用微波辅助等离子体装置,在10.0 mm×7.0 mm的砷化镓基底上沉积了CVD金刚石薄膜,用扫描电子显微镜观察沉积效果,拉曼光谱表征沉积质量,分析薄膜附着力与砷化镓材料性能的关系。结果表明,当基体温度为600℃,气压为5 kPa,甲烷浓度为2.0%时,在砷化镓片表面上沉积出了CVD金刚石薄膜,晶粒尺寸均匀,晶形完整、规则,晶界非常清晰。     

CVI法快速制备C/SiC复合材料

为缩短CVI法制备C／SiC复合材料的工艺周期并降低成本，研究了CVI工艺过程中沉积温度、MTS（CH3SiC3)摩尔分数和气体流量对SiC沉积速率和MTS有效利用率的影响，实验结果表明：提高沉积温度，常压下1100℃时增大MTS摩尔分数（11％→19％），都有利于提高SiC沉积速率；提高沉积温度和降低反应物气体流量，能提高MTS有效利用率，在优化的工艺条件下，预制体的微观孔隙内沉积了致密的SiC基体，沉积速率达到142μm/h左右，并有效消除了基体中裂纹的形成，MTS的有效利用率为11％－27％。     

转印法制备薄膜太阳能电池用银纳米线–聚合物复合透明导电薄膜

以自制银纳米线分散液为原料,聚氨酯(PU)为可剥落树脂,在聚对苯二甲酸乙二醇酯(PET)衬底上,利用转印法制备了可用于薄膜太阳能电池的银纳米线–可剥离树脂复合透明导电薄膜,并采用四探针测试仪、紫外–可见光光度计等技术测试了其方块电阻、可见光波段透过率和雾度,分析了分散液浓度、热处理温度与时间对银纳米线透明导电薄膜光电性能的影响。结果表明:随着分散液浓度的降低,银纳米线透明导电薄膜的透过率提高,但同时方块电阻增大;热处理可显著改善透明导电薄膜的导电性,透明导电薄膜的方块电阻随着热处理温度增加、时间延长均呈现出先降低后升高的现象,透过率则随热处理温度增加而提高;在150℃热处理5 min后,银纳米线透明导电薄膜的方块电阻为42?/sq,透过率为85.7%,雾度13.52%。     

沉淀法制备氧化亚铜颗粒及其在(CH3)2SiCl2单体合成反应中应用

通过调控沉淀法中样品老化时间制备了粒径0.10~0.15, 0.5~1和1~2 mm的球状Cu2O催化剂,研究了其粒径对直接合成(CH3)2SiCl2反应性能的影响. 结果表明,在所制粒径范围内,催化剂粒径对硅粉转化率影响不大,转化率约为12%;目的产物选择性随催化剂粒径增大而逐渐降低,3种粒径的Cu2O催化剂上(CH3)2SiCl2的选择性分别为86.48%, 80.65%和74.31%. 对反应前后触体的表征显示,硅粉表面以催化剂颗粒为中心发生了辐射状刻蚀反应,且随催化剂粒径增大,反应积碳量增加.     

高气压条件下MPCVD法快速制备金刚石膜

近年来研究表明,在微波等离子体化学气相沉积法(MPCVD)制备金刚石的过程中,增大反应气压和微波功率是提高金刚石生长速率的有效途径.本文采用自主改进的圆柱谐振腔式MPCVD装置,以H2-CH4为气源,在反应气压30 kPa、微波功率5.8 kW、CH4浓度不同的条件下进行了多晶金刚石膜的制备研究,并采用扫描电镜、X-射线衍射和激光拉曼光谱技术对所制备样品的表面形貌、物相及品质进行了分析.结果表明,CH4浓度由2.5％提高至5％,金刚石膜的质量较好,沉积速率由7.5μm/h提高至27.5μm/h.     

利用溶胶-凝胶法制备SnO_2:P透明导电薄膜的研究

用溶胶-凝胶法制备SnO_2:P透明导电薄膜;探讨P掺杂量、热处理温度、镀膜次数等的对薄膜结构和光电性能的影响。结果表明:SnO_2:P薄膜保持四方金红石结构,随着P掺杂量、热处理温度和镀膜次数的增加,方块电阻先下降后上升;提高热处理温度,可以提高薄膜平整度和致密度;采用提拉法在P/Sn摩尔比为2%时,热处理温度为450℃,镀膜次数为14次时,SnO_2:P薄膜性能最佳,方块电阻为8.9 KΩ/□,可见光平均透过率约为95%;采用旋涂法在P/Sn摩尔比为2%时,热处理温度为450℃,镀膜次数为6次时,方块电阻为4.3 KΩ/□;在相同条件下,采用提拉法制备薄膜光透过率明显高于旋涂法。     

沉积温度和时间对多孔SiC薄膜的光致发光性能的影响

为了增强碳化硅(SiC)的光致发光性能,设计了三层结构的多孔SiC薄膜,衬底是单晶硅,中间层是双通阳极氧化铝(AAO)模板,顶层是SiC薄膜。采用磁控溅射工艺在AAO模板上沉积SiC薄膜,沉积温度为100~500 ℃,溅射时间为1~30 min。研究了沉积温度和沉积时间对SiC的光致发光性能的影响。结果表明:SiC薄膜为非晶态,SiC主要沉积在AAO模板的上层骨架结构上;与未经过溅射的样品相比,当衬底温度为200 ℃,溅射时间为1 min时, SiC的荧光性能增强至14.23倍;多孔SiC薄膜的荧光主要来自2.3 eV的主峰和2.8 eV的次主峰,主峰可能来自Al₂O₃的O缺陷发光与SiC本征发光,次主峰可能来自SiO₂的O缺陷发光。磁控溅射结合双通AAO模板法可应用于多孔荧光SiC薄膜的工业化快速制备。     

生长温度对激光分子束外延A1N薄膜的影响

采用激光分子束外延法在Al2O3基片上制备AlN薄膜。用反射高能电子衍射、X射线衍射和原子力显微镜研究沉积温度对薄膜微结构的影响,通过光致发光谱和透射光谱对六方AlN薄膜的光学性能进行研究。结果表明：沉积温度为450℃时,沉积的AlN薄膜为非晶态;沉积温度为650℃时,在Al2O3基片上得到c轴单一取向的的六方AlN薄膜,且AlN和Al2O3之间的外延匹配关系为AlN[1210]//Al2O3[1100],AlN[1100]//Al2O3[1210]和AlN（0001）//Al2O3（0001）,这种面内相对旋转30°,可以减小AlN薄膜与Al2O3基片之间的晶格失配度和界面能。此外,650℃沉积的AlN的透射率达到85%,禁带宽度为5.6 eV。沉积温度升高到750℃时,AlN薄膜的透射率和光学能隙变小     

Sialon结合SiC复相材料的高温氧化行为

利用X射线衍射仪、扫描电子显微镜、压汞仪和热重分析仪等方法,在1100～1500℃范围内研究了Sialon结合SiC复相材料的高温抗氧化行为.结果表明:(1)随氧化温度升高,由于氧化致密层的形成,试样氧化增重速率降低,在1500℃氧化试样由于气泡破裂严重,氧化面积增大使氧化增重率有所提高;(2)随氧化温度升高出现氧化钝化现象,使得Sialon结合SiC复相材料表现出很好的高温抗氧化性能;(3)高温氧化使得Sialon结合SiC复相材料常温抗压强度比氧化前提高;随氧化温度升高,氧化膜表面形成较多气泡和开口空洞,使耐压强度呈下降趋势.     

Structural evolution and mechanical properties of Cansas-III SiC fibers after thermal treatment up to 1700 °C

The effects of thermal treatment on the Cansas-Ⅲ SiC fibers were investigated via heating at temperatures from 900 to 1700 ℃ for 1–5 h in argon atmosphere. The composition and morphology of the SiC fibers were characterized and the tensile strength of the SiC fiber bundles was analyzed via two-parameter Weibull distribution analysis. The results showed that the thermal treatment has negligible influence on the microstructure of the SiC fibers at temperatures ≤ 1100 ℃. At temperatures ≥ 1300 ℃, the surface of the fibers became rough with some visible particles. Particularly, at 1700 °C, numbers of holes appeared. With the increasing of heating temperature and holding time, the average tensile strength of the SiC fibers decreased gradually from 1.81 to 1.01 GPa. The decreasing of tensile strength can be attributed to the increase of critical defect sizes, grain growth and phase transformation (β→α) of SiC.     

Biaxial elastic modulus of very thin diamond-like carbon (DLC) films

The biaxial elastic modulus of very thin diamond-like carbon (DLC) films was measured by the recently suggested free overhang method. The DLC films of thickness ranging from 33 to 1100 nm were deposited on Si wafers by radio frequency plasma-assisted chemical vapor deposition (r.f.-PACVD) or by the filtered vacuum arc (FVA) process. Because the substrate was partially removed to obtain sinusoidal free overhang of the DLC film, this method has an advantage over other methods in that the measured value is not affected by the mechanical properties of the substrate. This advantage is more significant for a very thin film deposited on a substrate with a large difference in mechanical properties. The measured biaxial elastic moduli were reasonable values as can be judged from the plane strain modulus of thick films measured by nanoindentation. The biaxial elastic modulus of the film deposited by r.f.-PACVD was 90±3 GPa and that of the film deposited by FVA process was 600±50 GPa. While the biaxial elastic modulus of the film deposited by FVA is independent of the film thickness, the film deposited by r.f.-PACVD exhibited decreased elastic modulus with decreasing film thickness when the film is thinner than 500 nm. Although the reason for the different behavior could not be clarified at the present state, differences in structural evolution during the initial stage of film growth seem to be the reason.     

Strength retention in scheelite coated SiC fibers: Effect of the gas composition and pre-heat treatment

Scheelite coating was deposited on SiC fiber tows from various liquid-phase precursors at 1100℃. Strength degradation of SiC fiber was found after fiber coating which was found to be caused by the stress corrosion as a result of gases generated from the decomposition of by-products remaining in the coating. A new and simple method of low temperature pre-heat treatment was adopted to eliminate the stress corrosion in the fiber coating process and to isolate the effect of different types of gases on the stress corrosion cracking of fibers. The tensile strength and fractography of samples with and without pre-heat treatment were compared. Furthermore, the effect of gas composition on the strength degradation of SiC fiber was also investigated through the control experiments.     

溶胶-凝胶法制备Sm2O3光学薄膜

以氯化钐为起始原料,采用溶胶-凝胶法在玻璃和Si(100)基板上制备了Sm2O3光学薄膜,在300～800℃对薄膜进行1～3 h热处理.采用X射线衍射、原子力显微镜和紫外-可见自记式分光光度计等对薄膜的结晶取向、显微结构和光学性能进行了表征.结果表明:Sm2O3薄膜在玻璃基板和Si(100)基板上均表现出沿(311)晶面定向生长的特征;Si基板更有利于生长致密而且结晶良好的薄膜;所制备的薄膜对紫外线有强烈吸收作用,而对可见光有较好的透过作用,随着热处理温度的升高,薄膜结晶性变好,取向性增强,光吸收性能增强,薄膜的禁带宽度减小.     

碳热还原法低温制备碳化硅微粉

以SiO2为硅源,炭黑为碳源,Fe2 O3为催化剂,采用碳热还原法在氩气保护下制备SiC微粉,研究催化剂含量,合成温度对SiC生成、形貌的影响.实验结果表明:在原料中添加Fe2 O3粉,1350℃保温3h就能产生SiC微粉;由X射线衍射分析显示,在1450℃下保温3h基本上全部转化为晶粒尺寸在50 nm左右SiC微粉;在相同温度下,随着Fe2 O3用量的增加,SiC产率增加.添加Fe2O3能加快反应速度以及提高SiC微粉的生成量.     

两步反应法制备二苯基二甲氧基硅烷

二苯基二甲氧基硅烷是新生代的聚丙烯工业中的高效催化剂的重要组成部分 ,目前我国的约 80家聚丙烯生产厂家都用到它。我们以二苯基二氯硅烷和甲醇为起始原料 ,依据反应温度、反应时间和反应物料摩尔配比的不同 ,采用两步反应法对其进行了制备研究。得到了相应的最佳制备工艺条件 ,其结果为①第一步反应 :二苯基一氯甲氧基硅烷的制备的反应温度为室温 ( 5℃～ 3 5℃ ) ,反应时间为 2 5h ,反应物料摩尔配比为Ph2 SiCl2 ∶CH3OH =1∶1 5 ;②第二步反应 :二苯基二甲氧基硅烷的制备的反应温度为 15℃以下 ,反应时间 1h ,反应分批次数为 5 ,初始摩尔配比为DCMS∶CH3OH =1∶7。