纳米TiO2薄膜的低温等离子体制备技术

以四氯化钛为源物质,氩气为载气,氧气为反应气体,利用低温等离子体增强化学气相沉积在硅基表面制备出了TiO2薄膜。使用场发射扫描电子显微镜、X射线衍射仪等检测分析表征TiO2薄膜的性能与性质,并探讨了工艺条件如基片材料、沉积时间和基片温度对薄膜性能的影响。结果表明：制备的薄膜表面光滑均匀,结构致密,最小晶粒尺寸约15 nm;薄膜的晶型主要依赖于沉积温度,低于300 ℃沉积的薄膜是无定形的,300 ℃之上沉积的薄膜是锐钛矿结构。     

The structure and optical characters of the ZnO film grown on GaAs/Al2O3 substrate

In this paper ZnO films are grown on GaAs/Al₂O₃ substrates at different temperature by metal-organic chemical vapor deposition (MOCVD). The GaAs/Al₂O₃ substrates are formed by depositing GaAs layer (∼35 nm) on the Al₂O₃ substrate. The results of X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) demonstrate that most of the Ga and As atoms form Ga-As bond and the GaAs layer does not present any orientation. The characters of the ZnO films grown on GaAs/Al₂O₃ substrates are investigated by XRD, photoluminescence (PL), atomic force microscopy (AFM) and Raman scattering. Compared with ZnO film grown on Al₂O₃ substrate, ZnO film prepared by our fabrication scheme has good crystal and optical quality. Meanwhile its grain size becomes bigger according to the AFM image. Raman analysis indicates that the intrinsic defects and the in-plane tensile stress are obviously reduced in ZnO/GaAs/Al₂O₃ samples.     

Nanomechanical characteristics of SnO2:F thin films deposited by chemical vapor deposition

The nanoindentation characterizations and mechanical properties of fluorine-doped tin oxide (SnO₂:F) films deposited on glass substrates, using chemical vapor deposition (CVD) method, were studied, which included the effects of the indentation loads, the loading time and the hold time on the thin film. The surface roughness, fractal dimension and frictional coefficient were also studied by varying the freon flow rates. X-ray diffraction (XRD), atomic force microscopy (AFM) and frictional force microscopy (FFM) were used to analyze the morphology of the microstructure. The results showed that crystalline structure of the film had a high intensity (1 1 0) peak orientation, especially at a low freon flow rate. According to the nanoindentation records, the Young's modulus ranged from 62.4 to 75.1 GPa and the hardness ranged from 5.1 to 9.9 GPa at a freon flow rate of 8000 sccm. The changes in measured properties were due to changing loading rate.     

Deposition and characterization of carbon nitride films from hexamethylenetetramine/N2 by microwave plasma-enhanced chemical vapor deposition

Carbon nitride thin films were deposited on Si(1 0 0) substrate by microwave plasma-enhanced chemical vapor deposition (PECVD). Hexamethylenetetramine (HMTA) was used as carbon and nitrogen source while N₂ gas was used as both nitrogen source and carrier gas. The sp³-bonded C---N structure in HMTA was considered significantly in the precursor selection. X-ray diffraction analysis indicated that the film was a mixture of crystalline - and β-C₃N₄ as well as graphitic-C₃N₄ and β-Si₃N₄ which were not easily distinguished. Raman spectroscopy also suggested the existence of - and β-C₃N₄ in the films. X-ray photoelectron spectroscopy study indicated the presence of sp²- and sp³-bonded C---N structures in the films while sp³C---N bonding structure predominated to the sp² C---N bonding structure in the bulk composition of the films. N was also found to be bound to Si atoms in the films. The product was, therefore, described as CN_x:Si, where x depends on the film depth, with some evidences of crystalline C₃N₄ formation.     

等离子体增强化学气相沉积法实现硅纳米线掺硼

用等离子体增强化学气相沉积(PECVD)方法成功实现硅纳米线的掺B.选用Si片作衬底，硅烷 （SiH4）作硅源，硼烷（B2H6）作掺杂气体， Au作催化剂，生长温度440℃.基于气-液-固(VLS)机制，探讨了掺B硅纳米线可能的生长机制.PECVD法化学成分配比更灵活，更容易实现纳米线掺杂，进一步有望生长硅纳米线pn结，为研制纳米量级器件提供技术基础. 关键词： 硅纳米线 化学气相沉积 纳米器件     

Electrical characterisation of phosphorus-doped ZnO thin films grown by pulsed laser deposition

Phosphorus-doped ZnO films were grown by pulsed laser deposition using a ZnO:P₂O₅-doped target as the phosphorus source with the aim of producing p-type ZnO material. ZnO:P layers (with phosphorus concentrations of between 0.01 to 1 wt%) were grown on a pure ZnO buffer layer. The electrical properties of the films were characterised from temperature dependent Hall-effect measurements. The samples typically showed weak n-type conduction in the dark, with a resistivity of 70 Ω cm, a Hall mobility of μ_n0.5 cm² V ⁻¹ s⁻¹ and a carrier concentration of n3×10¹⁷ cm⁻³ at room temperature. After exposure to an incandescent light source, the samples underwent a change in conduction from n- to p-type, with an increase in mobility and decrease in concentration for temperatures below 300 K.     

Catalyst-free growth of well-aligned arsenic-doped ZnO nanowires by chemical vapor deposition method

ZnO nanowires with different arsenic concentration were grown on Si (1 0 0) substrates by chemical vapor deposition method without using catalyst. Zn/GaAs mixed powders were used as Zn and As source, respectively. Oxygen was used as oxidant. The images of scanning electron microscope show that the arsenic-doped ZnO nanowires with preferred c-axial orientation were obtained, which is in well accordance with the X-ray diffraction analysis. The arsenic related acceptor emission was observed in the photoluminescence spectra at 11 K for all arsenic-doped ZnO samples. This method for the preparation of arsenic-doped ZnO nanowires may open the way to realize the ZnO nanowires based light-emitting diode and laser diode.     

MgB2 超薄膜的制备和性质研究

利用混合物理化学气相沉积法在6H-SiC(001)衬底上制备干净的MgB₂超导超薄膜.在本底气体压强、载气氢气流量等条件一定的情况下,改变B₂H₆流量及沉积时间,制备得到不同厚度的系列MgB₂超薄膜样品,并研究了超导转变温度T_c、剩余电阻率ρ_(42K)、上临界磁场H_c2等与膜厚的关系.该系列超薄膜沿c轴外延生长,随膜厚度的变小,T_c(0)降低,ρ_(42K)升高.膜在衬底上的生长遵循Volmer-Weber岛状生长模式.对于厚度为7.5 nm的MgB₂超薄膜,T_c(0) =32.8 K,ρ_(42K) =118 μΩcm,是迄今为止所观测到的厚度为7.5 nm的MgB₂超薄膜最高的T_c值;对于厚度为10 nm的MgB₂膜,T_c(0)=35.5 K,ρ_(42K)=17.7 μΩcm,上临界磁场μ₀H_c2估算为12 T左右,零磁场、4 K时的临界电流密度J_c=1.0×10⁷ A/cm²,是迄今为止10 nm厚MgB₂超薄膜的最高J_c值,且其表面连接性良好,均方根粗糙度为0.731 nm.这预示MgB₂超薄膜在超导纳米器件上具有广阔的应用前景. 关键词： 2超薄膜')" href="#">MgB₂超薄膜 薄膜生长 氢气流量 混合物理化学气相沉积     

Influence of laser power on the orientation and microstructure of CeO2 films deposited on Hastelloy C276 tapes by laser chemical vapor deposition

CeO₂ films were prepared on LaMnO₃/MgO/Gd₂Zr₂O₇ multi-coated Hastelloy C276 tapes by laser chemical vapor deposition at different laser power (P_L) from 46 to 101 W. Epitaxial (1 0 0) CeO₂ films were prepared at P_L = 46-93 W (deposition temperature, T_dep = 705-792 K). Epitaxial CeO₂ films had rectangular-shaped grains at P_L = 46-77 W (T_dep = 705-754 K), while square-shaped grains were obtained at P_L = 85-93 W (T_dep = 769-792 K). CeO₂ films showed a columnar microstructure. Epitaxial (1 0 0) CeO₂ films with rectangular grains exhibited full width at half maximum of ω-scan on (2 0 0) reflection and ?-scan on (2 2 0) reflection of 3.4-3.2° and 6.0-7.2°, respectively. The deposition rate of the epitaxial (1 0 0) CeO₂ films had a maximum of 4.6 μm h⁻¹ at P_L = 77 W (T_dep = 754 K).     

Effects of high-temperature annealing on magnetic properties of V-doped GaN thin films grown by MOCVD

Metal organic chemical vapor deposition (MOCVD) has been used to grow vanadium-doped GaN (GaN:V) on c-sapphire substrate using VCl₄ as the V source. The as-grown GaN:V exhibited a saturated magnetic moment (M_s) of 0.28 emu/cm³ at room temperature. Upon high-temperature annealing treatment at 1100 °C for 7 min under N₂ ambient, the M_s of the GaN:V increased by 39.28% to 0.39 emu/cm³. We found that rapid thermal annealing leads to a remarkable increase in surface roughness of the V-doped GaN as well as the electron concentration. The annealing also leads to a significant increase in the Curie temperature (T_C), we have identified Curie temperatures about 350 K concluded from the difference between the field-cooled and zero-field-cooled magnetizations. Structure characterization by x-ray diffraction indicated that the ferromagnetic properties are not a result of secondary magnetic phases.     

一种简单的化学气相沉积法制备大尺寸单层二硫化钼

最近单层二硫化钼以其直接带隙的性质及在电子器件、催化、光电等领域中的潜在应用而备受关注.化学气相沉积法能够制备出高质量、大尺寸且性能优良的单层二硫化钼,但其制备工艺比较复杂.本文采用简化的化学气相沉积法在蓝宝石衬底上制备出了大尺寸的单晶二硫化钼.清洗衬底时,只需要简单的清洁,不需要用丙酮、食人鱼溶液(H_2SO_4/H_2O_2=3:1)等处理,这样既减少了操作步骤,又避免了潜在的危险.升温时直接从室温加热到生长的温度,不必分段升温,并且采用常压化学气相沉积法,不需要抽真空等过程,使得实验可以快捷方便地进行.光学显微镜、拉曼光谱和光致发光谱的结果表明,生长的二硫化钼为规则的三角形单层,边长为50μm左右,远大于机械剥离的样品.     

Nucleation mechanism and morphology evolution of MoS_2 flakes grown by chemical vapor deposition

We study the nucleation mechanism and morphology evolution of MoS_2 flakes grown by chemical vapor deposition(CVD)on SiO_2/Si substrates with using S and MoO_3 powders.The MoS_2 flake is of monolayer with triangular nucleation,which might arise from the initial MoO_3-xthat is deposited on the substrate,and then bonded with S to form MoS_2 flake.The ratio of Mo and S is higher than 1:2 at the beginning with Mo terminated triangular nucleation formed.After that,the morphology of MoS_2 flake evolves from triangle to similar hexagon,then to truncated triangle which is determined by the faster growth speed of Mo termination than that of S termination under the S rich environment.The nucleation density does not increase linearly with the increase of reactant concentration,which could be explained by the two-dimensional nucleation theory.     

Control of diameter of ZnO nanorods grown by chemical vapor deposition with laser ablation of ZnO

We made a study of controlling diameters of well-aligned ZnO nanorods grown by low-pressure thermal chemical vapor deposition combined with laser ablation of a sintered ZnO target, which was developed by us. Until now, it has been impossible to control diameters of ZnO nanorods, while the growth orientation was maintained well-aligned. In this study we developed a multi-step growth method to fabricate well-aligned nanorods whose diameters could be controlled. Metal Zn vapor and O₂ are used as precursors to grow ZnO nanorods. N₂ is used as a carrier gas for the precursors. A substrate is an n-Si (111) wafer. A sintered ZnO target is placed near the substrate and ablated by a Nd–YAG pulsed laser during ZnO nanorod growth. The growth temperature is 530 C and the pressure is 66.5 Pa. A vertical growth orientation of ZnO nanorods to the substrate is realized in the first-step growth although the diameter cannot be controlled in this step. When an O₂ flow rate is 1.5 sccm, well-aligned nanorods with 100 nm diameter are grown. Next, the second-step nanorods are grown on only the flat tip of the first-step nanorods. The diameters of the second-step nanorods can be controlled by adjusting the O₂ flow rate, and the growth direction is kept the same as that of the first-step nanorods. When the O₂ flow rate in second-step growth is smaller than 0.6 sccm, the diameter of the second-step nanorods is 30–50 nm. When the O₂ flow rate is between 0.75 and 3.0 sccm, the diameter is almost same as that of the first-step nanorods. When the O₂ flow rate is larger than 4.5 sccm, the diameter is increased with increasing O₂ flow rate. Further, the third-step ZnO nanorods with gradually increased diameters can be grown on the second-step nanorods with 1.5 sccm O₂ flow rate and without laser ablation.     

Influence of TaCl5 partial pressure on texture structure of TaC coating deposited by chemical vapor deposition

TaC was deposited on graphite substrate with different TaCl₅ partial pressure at 800 °C and 1200 °C by chemical vapor deposition. Microstructures and texture structures of the prepared coatings were researched with X-ray diffraction and scanning electronic microscopy. When the coating deposition process is controlled by surface reaction kinetics (800 °C), TaCl₅ partial pressure had little influence on the microstructure and texture structure of the coating. When the coating formation process is controlled by diffusion kinetics (1200 °C), the microstructure, texture structure of the prepared TaC grains vary greatly with TaCl₅ partial pressure. In the diffusion controlled process, the increasing of TaCl₅ partial pressure will result in the changing of gas supersaturation, and then the occurrence of secondary nucleation, which is the main reason for the changing of coating morphology and texture structure. With the help of competitive growth in (1 0 0) and (1 1 1) directions, the formation mechanism of the different texture coatings are discussed in detail. In addition, a diffusion model of deposition species around step-edge-corner was also proposed to explain the growth mechanism of the texture coatings.     

Effects of sapphire substrates surface treatment on the ZnO thin films grown by magnetron sputtering

The surface treatment effects of sapphire substrate on the ZnO thin films grown by magnetron sputtering were studied. The sapphire substrates properties have been investigated by means of atomic force microscopy (AFM) and X-ray diffraction rocking curves (XRCs). The results show that sapphire substrate surfaces have the best quality by CMP with subsequent chemical etching. The surface treatment effects of sapphire substrate on the ZnO thin films were examined by X-ray diffraction (XRD) and photoluminescence (PL) measurements. Results show that the intensity of (0 0 2) diffraction peak of ZnO thin films on sapphire substrates treated by CMP with subsequent chemical etching was strongest, FWHM of (0 0 2) diffraction peak is the narrowest and the intensity of UV peak of PL spectrum is strongest, indicating surface treatment on sapphire substrate preparation may improve ZnO thin films crystal quality and photoluminescent property.     

衬底对化学气相沉积法制备氧化硅纳米线的影响

通过化学气相沉积法在不同衬底上制备了大量的氧化硅纳米线.选用衬底为Si片、带有约100nm厚SiO2氧化层Si片和石英片.利用场发射扫描电子显微镜(SEM)和透射电镜(TEM，配备有能谱仪)对样品的表面形貌、结构和成分进行研究.结果表明：这些纳米线都为非晶态，但在不同衬底上生长的纳米线形貌、尺寸和化学成分不同.讨论了各种衬底对不同特征氧化硅纳米线生长的影响. 关键词： 化学气相沉积 纳米线 纳米颗粒     

Atmospheric pressure plasma treatment on graphene grown by chemical vapor deposition

We demonstrate the surface treatment of graphene using an atmospheric pressure plasma jet (APPJ) system. The graphene was synthesized by a thermal chemical vapor deposition with methane gas. A Mo foil and a SiO₂ wafer covered by Ni films were employed to synthesize monolayer and mixed-layered graphene, respectively. The home-built APPJ system was ignited using nitrogen gas to functionalize the graphene surface, and we studied the effect of different treatment times and interdistance between the plasma jet and the graphene surface. After the APPJ treatment, the hydrophobic character of graphene surface changed to hydrophilic. We found that the change is due to the formation of functionalities such as hydroxyl and carboxyl groups. Furthermore, it is worth noting that the nitrogen plasma treatment induced charge doping on graphene, and the pyridinic nitrogen component in the X-ray photoelectron spectroscopy spectrum was significantly enhanced. We conclude that the atmospheric pressure plasma treatment enables controlling the graphene properties without introducing surface defects.     

纳米TiO_2薄膜的低温等离子体制备技术

以四氯化钛为源物质,氩气为载气,氧气为反应气体,利用低温等离子体增强化学气相沉积在硅基表面制备出了TiO2薄膜。使用场发射扫描电子显微镜、X射线衍射仪等检测分析表征TiO2薄膜的性能与性质,并探讨了工艺条件如基片材料、沉积时间和基片温度对薄膜性能的影响。结果表明:制备的薄膜表面光滑均匀,结构致密,最小晶粒尺寸约15 nm;薄膜的晶型主要依赖于沉积温度,低于300℃沉积的薄膜是无定形的,300℃之上沉积的薄膜是锐钛矿结构。     

Well-aligned ZnO nanowires grown on Si substrate via metal–organic chemical vapor deposition

ZnO nanowires were grown on silicon substrate by metal–organic chemical vapor deposition (MOCVD) without catalysts. The scanning electron microscopy (SEM) observations along with X-ray diffraction (XRD) results suggest that the ZnO nanowires are single crystals vertically well-aligned to silicon substrate. Room-temperature photoluminescence (PL) measurement reveals strong UV emission and weak green emission, which demonstrates that the nanowires are of good optical properties. The mechanism of the catalyst-free growth of ZnO nanowires on silicon substrate is proposed.     

混合物理化学气相沉积法制备MgB$lt;sub$gt;2$lt;/sub$gt;单晶纳米晶片的研究

利用混合物理化学气相沉积法在石墨衬底上制备出了晶形为六角结构、厚度不同、径向尺寸不一的MgB₂单晶纳米晶片. 利用纳米定向转移技术将此晶片转移到了碳支持膜铜网上, 以便对其精细结构等物性进行表征. 电输运测量和磁性测量结果都表明晶片具有超导电性: T_conset=38 K, T_c(0)=33 K. 扫描电子显微镜图像表明, 晶片表面平整、厚度分布在几个纳米到200 nm之间, 宽度从几微米到上百微米; 高分辨透射电镜图像显示出晶片具有周期性晶格条纹. 选区电子衍射数据与MgB₂已有的单晶衍射数据相符. 这些测量结果证实了其确为高质量单晶MgB₂超导纳米晶片. 本文不仅提出了一种全新的制备单晶MgB₂的方法, 也观察到了纳米尺度MgB₂单晶的零电阻现象, 为后续的磁通钉扎、纳米力学性能等领域的深入研究提供了合适的素材. 关键词： 2')" href="#">单晶MgB₂ 超导纳米晶片 零电阻 混合物理化学气相沉积法