直流热阴极PCVD法CH_4:N_2:H_2气氛下制备纳米金刚石膜

采用直流热阴极等离子体化学气相沉积(PCVD)技术,在CH4:H2中加入N2改变等离子体能量分布状态,提高二次形核比例,制备纳米金刚石膜。在CH4:H2气体中,在不同压力和温度下,改变通入N2的比例,分析直流热阴极等离子体放电下N2对金刚石膜生长的影响。采用拉曼光谱仪、扫描电镜(SEM)和X射线衍射分析仪(XRD)对样品进行了表征,结果表明,直流热阴极PCVD系统中,CH4:N2:H2气氛下,N2流量小于气体总流量的50%时,在6×103 Pa、850℃条件下,制备的金刚石膜样品的晶粒小于100nm、金刚石1332 cm-1特征峰展宽且强度较高、金刚石的XRD衍射峰强度也较高,具备纳米金刚石膜的基本特征。因此,利用直流热阴极PCVD方法,在较低温度和气压下,CH4:H2中加入少量N2,可以制备出纳米金刚石膜。     

不同反应气源对制备纳米金刚石膜的影响

为确定两种典型的反应气源对制备纳米金刚石膜的影响,分别以CH4/Ar/H2及CH4/N2混合气体作为反应源,用微波等离子体化学气相沉积(MWPCVD)法制备纳米金刚石薄膜.XRD和Raman分析表明两种气源条件下得到的膜材均为金刚石多晶膜,但用CH4/N2气为反应源沉积的膜材中非金刚石相成分明显更多;AFM和SEM对照分析证实所有膜层的平均晶粒尺寸及表面粗糙度均在几十纳米量级,但CH4/N2气源沉积的膜中容易形成异常长大的晶粒,不利于表面质量的提高.研究结果表明,以CH4/Ar/H2混合气体作为反应气源可制备物相组成纯度更高、表面形态更为优越的纳米金刚石膜.     

直流热阴极PCVD法间歇生长模式制备透明金刚石膜

采用直流热阴极等离子体化学气相沉积(直流热阴极PCVD)方法,通过金刚石膜的间歇生长过程,引入氮原子的作用,实现对非金刚石成份的刻蚀和金刚石膜的择优取向生长,在CH4:N2:H2气氛下制备透明金刚石膜。金刚石膜的间歇式生长分为沉积阶段和刻蚀两个阶段,沉积阶段为20 min,刻蚀阶段为1 min,沉积和刻蚀通过温度的调节来实现,总的生长时间10 h;实验中主要改变的参数是N2气比例,将N2气流量与总气体流量的比例分为高、中、低三档分别进行实验。结果在CH4:N2:H2比例为2:20:180时获得了透明金刚石膜。金刚石膜样品用Raman光谱仪、SEM和XRD进行了表征,研究表明,直流热阴极PCVD间歇生长模式下,通过引入氮原子的作用,可以制备出(111)面取向的透明金刚石膜。     

DBD-PECVD法制备CN薄膜的结构及性能研究

使用自行设计的真空系统,采用介质阻挡放电等离子体增强化学气相沉积(DBD-PECVD)法,分别以CH4/N2、C2H2/N2、C2H4/N2混合气体作为反应气体,在单晶硅片上成功制备了CN薄膜.FTIR结果证实了薄膜中碳氮原子结合成化学键,Raman结果说明薄膜中含有类金刚石结构,AFM结果表明薄膜粗糙度随放电气压的升高而逐渐增大.三种混合气体沉积的CN薄膜,以CH4/N2的沉积速度最慢,薄膜表面粗糙度最小,含H量最少;C2H2/N2的沉积速度最快,薄膜表面粗糙度最大.     

含氧碳源提高金刚石膜沉积速率的研究

采用微波等离子体化学气相法合成的金刚石膜质量好，但采用常规CH4-H2反应气体体系，金刚石膜的沉积速率较慢。为此，实验研究了C2H5OH-H2、CH3COCH3-H2等含氧体系下碳源浓度、微波功率、气体压力对金刚石膜沉积速率、表面形貌、电阻率的影响。结果表明，使用C2H5OH—H2、CH3COCH3-H2等含氧体系，金...     

用于二次电子发射阴极的纳米金刚石膜

为获得导电性和二次电子发射性能均好的金刚石阴极材料,分别以CH4/Ar/H2、CH4/N2及CH4/N2/H2混合气体作为反应气源,用微波等离子化学气相沉积(MWPCVD)法制备出不同组成结构特点的纳米金刚石薄膜.XRD和Raman检测表明3种气源条件下得到的膜材均为金刚石多晶膜,但用CH4/N2反应源沉积的膜材中非金刚石相成分明显更多;AFM分析证实所有膜层的平均晶粒尺寸均在100nm以下,属纳米晶金刚石膜.用自行设计的二次电子发射系数测量装置对比检测所得膜层的二次电子发射特性,结果表明各金刚石膜均在初级入射电子能量达约1keV时,有最高的二次发射系数(δmax);并且以CH4/Ar/H2反应源制备的金刚石相纯度最高的膜材的δmax最大,达到17左右,是适用于二次电子发射阴极的潜在材料.     

陶瓷-Teflon AF2400复合油气分离膜组件

用陶瓷超滤膜管和Teflon AF2400溶液制备陶瓷管-Teflon AF2400复合膜.测试了该复合膜组件对H2,CO,CO2,CH4,C2H6,C2H4,C2H2七种故障气体的脱气性能,并与GP100聚四氟乙烯毛细管和聚酰亚胺(PI)平板膜进行了比较.结果表明,陶瓷管-Teflon AF2400复合膜组件可在10 h内实现7种故障特征气体的油气平衡,远远快于GP100和PI膜.该组件可以在500 kPa的压力下长时间正常工作,能够满足变压器油中溶解气体在线监测的需要.     

氧气对MWPCVD制备金刚石膜的影响

在水冷反应室式微波等离子体气相沉积装置中以混合的CH4／H2／O2为反应气体,研究了O2浓度对制备金刚石膜的影响,实验发现,很低浓度的O2会显著促进金刚石的沉积,并稍稍抑制非晶C的沉积,因而沉积膜中非晶C的含量急剧下降;较高浓度的O2会同时抑制金刚石和非晶C的沉积,但由于抑制金刚石的作用更强烈,沉积膜中非晶C的含量反应有所升高,另外,O2的存在,有利于沉积颗粒较小的金刚石膜。     

氧气对MWPCVD制备金刚石膜的影响

在水冷反应室式微波等离子体化学气相沉积装置中以混合的CH4/H2/O2为反应气体,研究了O2浓度对制备金刚石膜的影响.实验发现,很低浓度的O2会显著促进金刚石的沉积,并稍稍抑制非晶C的沉积,因而沉积膜中非晶C的含量急剧下降;较高浓度的O2会同时抑制金刚石和非晶C的沉积,但由于抑制金刚石的作用更强烈,沉积膜中非晶C的含量反而有所升高.另外,O2的存在,有利于沉积颗粒较小的金刚石膜.     

高气压下温度对金刚石膜择优取向的影响

采用自主改进的圆柱谐振腔式MPCVD装置,以H2-CH4为气源、反应腔压强30kPa、微波功率6kW、CH4浓度2%,在不同的沉积温度下进行了多晶金刚石膜的制备研究。采用扫描电镜、X-射线衍射技术对所制备样品的表面形貌、物相及晶面取向进行了分析。结果表明,在高气压条件下,沉积温度由800℃升高至900℃时,金刚石膜的表面形貌由(111)晶面择优取向逐渐转向(100)晶面择优取向;沉积温度由900℃升高至1050℃时,金刚石的表面形貌由(100)晶面择优取向逐渐转向(111)晶面择优取向。     

CVD金刚石薄膜(111)与(100)取向生长的热力学分析

用非平衡热力学耦合模型计算了CVD金刚石薄膜生长过程中C2H2与CH3浓度之比[C2H2]/[CH3]随衬底温度和CH4浓度的变化关系,从理论上探讨了金刚石薄膜（111）面和（100）面取向生长与淀积条件的关系。在衬底温度和CH4浓度由低到高的变化过程中,[C2H2]/[CH3]逐渐升高,导致金刚石薄膜的形貌从（111）晶面转为（100）晶面。添加氧后C2H2与CH3浓度都将下降,但C2H2下降得更多,因而添加氧也使[C2H2]/[CH3]下降,从而有利于生长（111）晶面的金刚石薄膜。     

Low Resistance Polycrystalline Diamond Thin Films Deposited by Hot Filament Chemical Vapour Deposition

Polycrystalline diamond thin films with outgrowing diamond (OGD) grains were deposited onto silicon wafers using a hydrocarbon gas (CH4) highly diluted with H2 at low pressure in a hot filament chemical vapour deposition (HFCVD) reactor with a range of gas flow rates. X-ray diffraction (XRD) and SEM showed polycrystalline diamond structure with a random orientation. Polycrystalline diamond films with various textures were grown and (111) facets were dominant with sharp grain boundaries. Outgrowth was observed in flowerish character at high gas flow rates. Isolated single crystals with little openings appeared at various stages at low gas flow rates. Thus, changing gas flow rates had a beneficial influence on the grain size, growth rate and electrical resistivity. CVD diamond films gave an excellent performance for medium film thickness with relatively low electrical resistivity and making them potentially useful in many industrial applications.     

Morphology and texture evolution of nanostructured CaF2 films on amorphous substrates under oblique incidence flux

The morphology and biaxial texture of vacuum evaporated CaF(2) films on amorphous substrates as a function of vapour incident angle, substrate temperature and film thickness were investigated by scanning electron microscopy, x-ray pole figure and reflection high energy electron diffraction surface pole figure analyses. Results show that an anomalous [220] out-of-plane texture was preferred in CaF(2) films deposited on Si substrates at < 200?°C with normal vapour incidence. With an increase of the vapour incident angle, the out-of-plane orientation changed from [220] to [111] at a substrate temperature of 100?°C. In films deposited with normal vapour incidence, the out-of-plane orientation changed from [220] at 100?°C to [111] at 400?°C. In films deposited with an oblique vapour incidence at 100?°C, the texture changed from random at small thickness (5 nm) to biaxial at larger thickness (20 nm or more). Using first principles density functional theory calculation, it was shown that [220] texture formation is a consequence of energetically favourable adsorption of CaF(2) molecules onto the CaF(2)(110) facet.     

Si-based Multielement Thin Film Prepared by r.f. Reactive Sputtering at Room Temperature

Hydrogenatedam0rphousSi-basedthinfilmsareofinterestfortheapplicationsinelectr0nicdevicesin-cludinglightemittingdiodes,photodetect0rsandsolarenergycollectors.Theycanals0beusedasprotectivelayerspreventingcorrosionandpassivationc0atings.Silicon,carb0nnitridehydrogenatedamorph0usthinfilm(aSi:C:N:H)isoneofSi-basedfilms.Itsphysi-calandchemicalpropertiesprobablyintegratingtheexcellentcharacteristicsofa-SiC:Handa-SiN:Hfilmsareinterestingtoresearchw0rkers.Inthepresentwork,aSi:C:N:Hthinfilmswered…     

无支撑优质金刚石膜研制中的相关问题探讨

无支撑优质金刚石膜在微波真空器件和光学器件中的广泛应用,有赖于制备成本的下降和工艺的完善。结合微波等离子体化学气相沉积(MPCVD)金刚石膜的工艺研究结果,本文就沉积速率、晶面取向以及内应力的相关问题进行了初步探讨。对于给定的设备,沉积速率与多种因素有关,包括膜的质量、膜厚均匀性和有效沉积面积、以及形核的密度。在通常情况下,金刚石膜呈(111)择优取向,而样品位置下移5mm后,观察到(100)取向。对内应力的初步研究表明,CH4/H2比例较低(1.5)时,金刚石膜的内应力趋向于压应力,而(100)取向的出现则有助于使内应力降到最低。     

Low-temperature growth of nanostructured diamond films

Nanostructured diamond films are grown on a titanium alloy substrate using a two-step deposition process. The first step is performed at elevated temperature (820 degrees C) for 30 min using a H2/CH4/N2 gas mixture to grow a thin (approximately 600 nm) nanostructured diamond layer and to improve film adhesion. The remainder of the deposition involves growth at low temperature (< 600 degrees C) in a H2/CH4/O2 gas mixture. The continuation of the smooth nanostructured diamond film growth during low-temperature deposition is confirmed by in situ laser reflectance interferometry, atomic force microscopy, micro-Raman spectroscopy, and surface profilometry. Similar experiments performed without the initial nanostructured diamond layer resulted in poorly adhered films with a more crystalline appearance and a higher surface roughness. This low-temperature deposition of nanostructured diamond films on metals offers advantages in cases where high residual thermal stress leads to delamination at high temperatures.     

扩散阻挡层对Cu-Zr合金膜表面形貌与结构的影响

用磁控溅射和离子束溅射共沉积的方法，分别以TiN,TaN,ZrN为扩散阻挡层，在单晶硅片上制备了Cu-Zr合金膜，膜在400℃氮气中退火1h，研究表明，不同扩散阻挡层上Cu-Zr膜的形貌不同，沉积态膜的组成颗粒以ZrN为扩散阻挡层的最小，退火后膜的颗粒长大，且Zr向膜表面和界面处扩散，沉积态的膜具有强的（111）取向，峰形宽化明显，退火后又出现（200）、（220）、（311）衍射峰，扩散阻挡层不同时Cu-Zr合金膜的（200）与（111）的强度比值不同。     

Microcrystalline silicon films fabricated by bias-assisted hot-wire chemical vapor deposition

Microcrystalline silicon films (μc-Si:H) were deposited on stainless steel substrates by bias-assisted hot-wire chemical vapor deposition. The effect of substrate bias and substrate temperature on the crystallinity of μc-Si:H films was studied by Raman spectroscopy, X-ray diffraction and scanning electron microscopy. The results show that both the Raman peak position and the crystalline fraction of the μc-Si:H films deposited at 200 °C were obviously improved by introducing ?800 V substrate bias. The films deposited at 200 °C with ?800 V substrate bias show strongly sharpened Si (111) peak together with Si (220) and Si (311) peaks, which was different from a weak Si (111) peak for those deposited without substrate bias. By increasing the substrate temperature from 200 to 300 °C, while keeping the substrate bias at ?800 V, the crystallinity of the silicon films was further improved, and μc-Si:H films with crystalline fraction of 74 % was obtained.     

Raman spectroscopy characterization of diamond films on steel substrates with titanium carbide arc-plated interlayer

Diamond chemical vapour deposition (CVD) on steel represents a difficult task. The major problem is represented by large diffusion of carbon into steel at CVD temperatures. This leads to very low diamond nucleation and degradation of steel microstructure and properties. Recent work [R. Polini, F. Pighetti Mantini, M. Braic, M. Amar, W. Ahmed, H. Taylor, Thin Solid Films 494 (2006) 116] demonstrated that well-adherent diamond films can be grown on high-speed steels by using a TiC interlayer deposited by the PVD-arc technique. The resulting multilayer (TiC/diamond) coating had a rough surface morphology due to the presence of droplets formed at the substrate surface during the reactive evaporation of TiC. In this work, we first present an extensive Raman investigation of 2 μm, 4 μm and 6 μm thick diamond films deposited by hot filament CVD on TiC interlayers obtained by the PVD-arc technique. The stress state of the diamond was dependent on both the films thickness and the spatial position of the coating on the substrate. In fact, on the top of TiC droplets, the stress state of the diamond was much lower than that of diamond in flatter substrate areas. These results showed that diamond films deposited on rough TiC interlayers exhibited a wide distribution of stress values and that very large compressive stress exists in the diamond film grown on flat regions of steel substrates with a TiC interlayer. Diamond films could accommodate stresses as large as 10 GPa without delamination.     

掺氮类金刚石薄膜的微观结构和电导特性

用射频等离子体化学气相沉积法（RFCVD）和CH4、N2与Ar组成的混合气体制备掺氮类金刚石薄膜（a-C:H:N)。用原子力显微镜（AFM）,俄歇电子能谱（AES）,红外光谱（IR）以及显微拉曼谱（Micro-Raman)对a-C:H:N薄膜的表面形貌、组分和微观结构进行了表征。实验结果表明,薄膜中有纳米量级的颗粒存在,而且随反应气体中N2与CH4比值的增大,薄膜中氮元素的含量也随之增大,并主要以C-N键和N-H键形式存在,少量以C≡N键形式存在,还研究了热退火对a-C:H:N薄膜的电导率的影响。