Si基底磁控溅射制备CrN薄膜的表面形貌与生长机制

在Si基底上采用直流磁控溅射法制备CrN薄膜,利用原子力显微镜(AFM)、扫描电镜(SEM)和X射线衍射仪(XRD)分析薄膜表面形貌和物相成分,探讨薄膜生长的动力学过程.结果表明只有当生长时间足够(1800s)时,才能形成具有CrN相的薄膜.随着CrN薄膜的生长,薄膜表面晶粒由三棱锥发展为三棱锥与胞状共存状,薄膜表面粗糙度逐渐增大,动力学生长指数β=0.50.     

Fabrication of hexagonal gallium nitride films on silicon (111) substrates

Hexagonal gallium nitride films were successfully fabricated through ammoniating Ga2O3 films deposited on silicon (111) substrates by electrophoresis. The structure, composition, and surface morphology of the formed films were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The measurement results reveal that the polycrystalline GaN films with hexagonal wurtzite structure were successfully grown on the silicon (111) substrates. Preliminary results suggest that varying the ammoniating temperature has obvious effect on the quality of the GaN films formed with this method.     

Li掺杂对Mn-ZnO薄膜结构, 电学和磁学性能的影响

利用磁控溅射法在Si(110)基片上制备了Zn0.95-xLixMn0.05O(x=0,0.05)薄膜,研究了Li掺杂对Mn-ZnO薄膜结构、电学和磁学性能的影响。XRD结果表明,样品薄膜具有高度的c轴择优取向,并且没有发现其他杂相。AFM表明,Li掺入Mn-ZnO使得薄膜颗粒均匀、质地致密。霍尔测试表明,Li掺入Mn-ZnO使载流子浓度增加,然而没有改变其n型导电类型。磁性测试表明,Li掺入Mn-ZnO使得室温铁磁性增强,可由束缚极化极子(BMP)模型解释。     

Pretreatment of glass substrates by Ar/O2 ion beams for the as-sputtered rough Al doped zinc oxide thin films

Textured TCO surfaces are required in silicon thin film solar cells to gain efficient light trapping. Nowadays, magnetron sputtered ZnO:Al films are usually etched in HCl solution to obtain textured surface. This study introduces a method to achieve as-grown rough ZnO:Al films by ion beam pretreatment of the glass substrate. The reference ZnO:Al films deposited on untreated glass are composed of well aligned columnar grains. In contrast, in the as-grown rough films, additional large conical grains are observed. The large grains exhibit faster growth rate than the surrounding columnar grains, and therefore overgrow the columnar grains gradually and finally cover the whole surface. In order to investigate the ZnO:Al film structural properties, transmission electron microscopy and X-ray diffraction are employed. The crystal orientations of these two types of grains are further analyzed by selected area diffraction patterns. The columns in the as-grown rough ZnO:Al are similarly textured as the reference ZnO:Al film on untreated glass. The c-axis is well aligned nearly perpendicular to the substrate surface, but a tilt of 10° was observed with respect to the growth direction. The large conical grains show no strong out of plane texture and random in plane orientation.     

溅射方法和基体材料对氧化钛薄膜微观结构的影响

目的研究不同溅射方法和基体材料对沉积氧化钛薄膜的晶体结构、化学价态、表面形貌的影响。方法采用高功率脉冲磁控溅射(HPPMS)和直流磁控溅射(DCMS)在316L不锈钢和硅片表面制备了氧化钛薄膜。采用等离子光发射谱检测了沉积薄膜时的等离子体特征。采用X射线衍射仪(XRD)、X射线光电子能谱(XPS)、原子力显微镜(AFM)和扫描电子显微镜(SEM),分别评价氧化钛薄膜的晶体结构、化学价态、晶粒尺寸和表面粗糙度。结果等离子体特征显示,沉积氧化钛薄膜时,HPPMS比DCMS具有更高的离化率和等离子体密度。XRD结果显示,在相同的平均溅射功率下,采用HPPMS和DCMS方法,均在不锈钢表面制备出纯金红石结构的氧化钛薄膜,而在硅片表面得到的氧化钛薄膜为金红石、锐钛矿混合结构,且采用HPPMS比DCMS技术制备的氧化钛薄膜含有更高的金红石含量。XPS结果显示,两种方法在所有基体表面均制备出了含有氧缺位的氧化钛薄膜。采用HPPMS和DCMS制备氧化钛薄膜时,不锈钢基体沉积的薄膜中,Ti3+/Ti4+比值均高于Si基体上的薄膜。SEM和硬度测试结果显示,HPPMS制备的氧化钛薄膜为等轴晶,晶粒较小,硬度较高。DCMS制备的氧化钛薄膜具有柱状晶的结构,晶粒较大。AFM的结果显示,采用不同溅射方法制备的氧化钛薄膜表面粗糙度没有明显差别。结论不同溅射方法和基体材料导致了薄膜沉积时样品表面离子轰击能量的差异,因此影响了氧化钛薄膜的晶体结构、化学价态和晶粒尺寸。     

磁过滤阴极弧法制备CrCN薄膜结构与组分研究

目的通过磁过滤阴极弧沉积技术制备质量优异的CrCN涂层。研究乙炔/氮气混合气体流量以及基底偏压对薄膜结构和成分的影响。方法采用磁过滤真空阴极弧沉积技术,在20~100 m L/min变化的乙炔/氮气混合气体流量参数下沉积CrCN复合薄膜。通过X射线衍射、场发射电子显微镜、扫描探针显微镜、X射线光电子能谱仪、透射电镜,对薄膜的物相结构和形貌进行分析。结果随着气体流量的增加,CrCN复合薄膜的晶粒逐渐减小最终向非晶化转变。TEM结果表明,在CrCN复合薄膜中有大量几纳米到十几纳米的纳米晶浸没在非晶成分中。SPM表明,随着基底偏压由–200 V增大到–150 V,CrCN薄膜的表面粗糙度Sa由0.345 nm上升至4.38 nm。XPS、TEM和XRD数据表明,薄膜中Cr元素主要以单质Cr、Cr N以及Cr3C2的形式存在。结论采用磁过滤真空阴极弧沉积技术制备的CrCN复合薄膜具有纳米晶-非晶镶嵌结构。该方法沉积的CrCN薄膜的表面粗糙度与基底负偏压有关。混合气体的流量变化对薄膜组分的变化几乎无影响。     

Preparation and characterization of Ca0.18Na0.32Bi0.50TiO3 ferroelectric thin films by metalorganic solution deposition

Ca_0.18Na_0.32Bi_0.50TiO₃ (CNBT) ferroelectric thin films were prepared by metalorganic solution deposition on silicon substrate and annealed at different temperatures. The morphology and structure of the films were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The crystal structure of Ca-doped Na_0.50Bi_0.50TiO₃ films shows no obvious lattice distortion compared with that of un-doped one. The optimal heat treatment process for CNBT films were determined to be high-temperature drying at 400 °C for no less than 15 min followed by annealing at 600 °C for 5 min, which leads to the formation of compact films with uniform grains of 30–50 nm. Ferroelectric property measurement shows that the remanent polarization of CNBT films is 18 times higher than that of un-doped Na_0.50Bi_0.50TiO₃ (NBT) thin films.     

LaNiO3/石墨烯复合薄膜的制备及光催化性能

采用改进的Hummer法制备出薄层石墨烯材料,采用溶胶-凝胶法结合旋转涂膜技术以玻璃基底制备出石墨烯基LaNiO3复合薄膜。采用X射线衍射(XRD)仪,透射电镜(TEM),扫描电镜(SEM),拉曼光谱,X射线衍射光电子能谱(XPS)、紫外-可见(UV-Vis)吸收光谱和荧光光谱(PL)等测试手段对复合薄膜进行表征。结果表明,晶粒粒径约为20 nm的LaNiO3较均匀地生长在了石墨烯片上。光催化性能研究表明,LaNiO3/石墨烯复合薄膜的光催化活性显著优于LaNiO3薄膜,当石墨烯的含量约为4%时,复合薄膜4 h内对酸性红的降解效率比LaNiO3薄膜提高了1倍。     

Zn掺杂CdO薄膜的溅射法制备和光电性能研究

目的通过向CdO薄膜中掺杂ZnO,在尽量不影响其电学性质的前提下,拓宽禁带宽度并改善性能。方法通过磁控射频溅射分别在玻璃基底和硅111基底上沉积了一系列Cd_(1-x)Zn_xO透明导电薄膜。利用XRD、紫外可见分光光度计和霍尔效应测量仪,测试了薄膜的结构、光学和电学性能。结果随着Zn掺杂含量的增加,薄膜结构会发生变化:x0.25时,薄膜结果为岩盐相;0.25x0.5时,薄膜结构为混合相;x0.5时,薄膜结构变成了纤锌矿相。掺杂Zn后,薄膜吸收边可以提升到3eV左右,同时其电阻率为6.69×10~(-4)?·cm,载流子浓度为7.92×10~(20) cm~(-3),与纯CdO薄膜电学性质相近。结论对CdO薄膜进行一定量的ZnO掺杂,可以在不影响其电学性质的前提下提高禁带宽度,从而使薄膜具有良好的光电性能。     

Free-Cyanide Synthesis and Characterization of Cu–Zn Alloy by an Electrodeposition-Annealing Route

Substitution of cyanide in electroplating is a current challenge. We present an alternative method aiming to reduce the toxicity and the cost of electroplating of Cu–Zn alloy (usually prepared from cyanide baths) while maintaining the decorative qualities and anticorrosive properties of the coating. For this purpose, Cu–Zn alloys were obtained in two steps from non-cyanide electrolytes. First, a copper layer electrodeposited onto a nickel under-layer, followed by a thin layer of zinc from three different simple non-cyanide zinc baths. The Zn/Cu/Ni sandwich system was then subjected to heat treatment at a temperature of 400°C, to ensure the diffusion of zinc into the copper layer to give the desired Cu–Zn alloy structure. The synthesized films were characterized by using X-ray diffraction XRD, scanning electron microscopy and energy dispersive X-ray spectroscopy (EDS). XRD demonstrated that the electrodeposited films are crystalline and present the Cu_0.7Zn_0.3 phase with preferential (111) orientation. An analysis of XRD patterns revealed that after heat treatment, the Cu–Zn alloys were composed of a predominating α-phase structure. The morphology and composition of the coatings depends on the zinc plating bath type. After annealing, well defined pseudospherical Cu–Zn grains were formed covering the entire substrate surface. The EDS analysis indicated the formation of Cu_0.7Zn_0.3 brass alloys. The results showed the feasibility of this low-cost new route for the preparation of good quality Cu–Zn alloys from cyanide-free electrolytes.     

钴硼合金功能膜的制备与结构分析

以ＮａＢＨ４为还原剂用化学沉积方法成功制备了钴硼合金功能膜。通过大量试验,优化出一种沉积速率较快的镀液配方与工艺。采用ＸＲＤ、ＴＥＭ等仪器对沉积膜的镀态结构和组织性能进行了测试,研究了合金的沉积速率与结构。试验获得的合金膜显微硬度较高,表面光亮致密,且与基体结合牢固;虽然ＸＲＤ的检测结果显示沉积膜为非晶态结构,ＴＥＭ的进一步分析表明,沉积膜是非晶态＋晶态的过渡态结构,从而对钴硼合金沉积膜作了较为全面的评价。     

Si（111）衬底上生长GaN晶环的研究

利用热壁化学气相沉积在Si(111)衬底上获得GaN晶环，采用扫描电镜(SEM)、选择区电子衍射(SAED)、X射线衍射(XRD)，光致发光(PL)谱和傅里叶红外吸收谱(FTIR)对晶环的组成、结构、形貌和光学特性进行分析。初步结果证明：在Si(111)衬底上获得择优生长的六方纤锌矿结构的GaN晶环。SEM显示在均匀的薄膜上出现直径约为10μm的5品环，由XRD和SAED的分析证实晶环呈六方纤矿多晶结构，FTIR显示GaN薄膜的主要成分为GaN，同时含有少量的C污染，PL测试表明晶环呈现不同于GaN薄膜的发光特性。     

HWCVD与RF-PECVD复合技术制备微晶硅薄膜的性能*

采用热丝化学气相沉积(HWCVD)和射频等离子体化学气相沉积(RF-PECVD)相结合的技术,在普通载玻片和聚酰亚胺衬底上沉积制备微晶硅薄膜。系统考查了热丝到衬底的距离对沉积薄膜结构和性能的影响规律,用拉曼光谱仪、X-射线衍射仪(XRD)、紫外可见光纤光谱仪对薄膜的晶化率、微观结构和光学性能进行研究。结果表明:薄膜沉积速率最高可达到0.73nm/s,晶化率和禁带宽度分别可以在0%～78%和0.86～1.28eV变化,射频等离子体的引入有助于多晶硅薄膜的(220)择优生长,HWCVD的引入有助于薄膜晶化。     

磁控溅射和退火制备ZnO/SiO2复合薄膜

采用射频磁控溅射和退火处理的方法在单晶硅衬底上制备了ZnO/SiO2复合薄膜,利用X射线衍射(XRD)、扫描电镜(SEM)、能谱分析(EDS)和接触角测量等测试手段研究溅射气压、溅射功率、氧氩比和退火温度等对复合薄膜成分组成、组织结构及润湿性能的影响。研究表明,复合薄膜中主要有ZnO、SiO2、Zn2SiO4 3种物相,且分别以六方纤锌矿结构、无定形态和硅锌矿型等形式存在。随着溅射和退火工艺的改变,复合薄膜的接触角在41°～146°间变化,组织形态由颗粒状向纳米竹叶状变化。溅射气压0.5 Pa,溅射功率120 W,氧氩比(O2∶Ar)为0∶30,退火温度为700℃的条件下获得具有六方纤锌矿结构的ZnO纳米组织,该组织呈现出竹叶状,在薄膜表面交错排列形成了无序多空隙的微观形貌,使复合薄膜具有超疏水性,接触角为146°。     

Mo电极上磁控反应溅射AlN薄膜

采用射频反应磁控溅射法在Mo电极上沉积了AlN薄膜.研究了溅射气压、靶基距、溅射功率、衬底温度及N_2含量等不同工艺条件对AlN薄膜择优取向生长的影响.用XRD分析了薄膜的择优取向,用原子力显微镜、高分辨场发射扫描电镜表征了薄膜的形貌.实验结果表明,靶基距和溅射气压的减小,衬底温度及溅射功率的升高有利于AlN(002)晶面的择优取向生长.氮氩比对AlN薄膜择优取向生长影响较小,N_2≥50%(体积分数)时均可制得高c轴择优取向的AlN薄膜.经优化工艺参数制备的AlN柱状晶薄膜适用于体声波谐振滤波器的制备.     

Electroless deposition of Cu on multiwalled carbon nanotubes

Copper has been deposited on the surface of multiwailed carbon nanombes （MWNTs） and inside MWNTs by electroless deposition. The as-prepared Cu-MWNT composite materials have been characterized by X-ray diffractometer （XRD）, transmission electron microscopy （TEM）, and electrochemical measurement. XRD analyses showed that Cu was a face-centered cubic （fcc） structure. The average size of Cu was calculated by Scherrer＇s formula from XRD data, and it was 11 nm. TEM revealed that Cu grains on the surface of MWNTs were uniform with the sizes of about 30-60 nm. The electrochemical measurement indicated that Cu-MWNT composite materials possessed fine electron conductivity.     

钼酸铋薄膜的化学溶液制备技术及其性能表征

使用化学溶液制各技术在硅(100)衬底上制备出符合化学计量比的钼酸铋(α相)薄膜.采用X射线衍射(XRD)分析的研究结果表明,所制备的薄膜具有单一的单斜晶相结构利用原子力显微镜(AFM)对其表面形貌进行表征,验证了实验过程中溶剂的改变对薄膜结构和表面形貌产生的影响;使用荧光发射仪研究了薄膜在室温下的发光特性.结果表明,通过化学溶液制备技术可以制备出具有单一晶相的钼酸铋(α相)薄膜,该薄膜具有良好的光致发光特性.     

SPS制备SmCo7-xFex块状纳米晶磁体的研究

采用高能球磨法制得SmCo7-xFex非晶粉末,然后采用放电等离子技术将其烧结为块状纳米晶磁体,对磁体的微观结构和磁性能进行了观察和测试.结果表明,SmCo7-xFex球磨5 h后成为非晶粉末,经SPS烧结后得到1:7相.TEM观察表明,磁体晶粒尺寸在20～50 nm.另外,磁体具有较好的磁性能,当x=0.4时,矫顽力为992.8 kA/m,剩磁为0.634T,(BH)max为69.75KJ/m3.     

Microstructure and hardness of hollow cathode discharge ion-plated titanium nitride film

Titanium nitride (TiN) films were deposited on 304 stainless steel substrate by hollow cathode discharge (HCD) ion-plating technique. The preferred orientation and microstructure were studied by x-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. Microhardness of the TiN film was measured and correlated to the microstructure and preferred orientation. The results of TEM study showed that the microstructure of TiN film contains grains with nanometer scale. As the film thickness increases, the grain size of TiN increases. The x-ray results show that TiN(111) is the major preferred orientation of the film. The hardness of TiN film is primarily contributed from TiN(111) preferred orientation.     

Co/C与Co-Pt/C膜的微结构研究

利用磁控溅射方法制备Co/C和Co-Pt/C薄膜.用X射线衍射谱(XRD)和透射电子显微镜(TEM)测量样品结构和微观形貌.对Co/C和Co-Pt/C晶粒的大小进行计算,表明Co/C颗粒膜Co是以团簇的形式镶嵌在C层中的,面心立方(fcc)COPt3和面心四方(fct)Copt两个稳定有序相在Co-Pt/C薄膜中很好地...