AES studies of palladium films formed on copper and mica

Thin epitaxial films of palladium were grown on epitaxial copper films and cleaved mica in ultra high vacuum. The growth modes of these films were investigated by Auger electron spectroscopy (AES), low energy electron diffraction (LEED), transmission electron microscopy (TEM), and TEM replica techniques. Layer by layer growth of Pd on Cu and mica was observed and inelastic mean free paths of Auger electrons for energies of 60 eV (Cu MMM) and 329 eV (Pd MNN) were calculated. These values were 5.7 and 6.9 Å respectively. The thermal stability of monocrystalline and polycrystalline Pd/Cu bilayer films at 483 K was also investigated by AES and TEM. It was found that Pd agglomerates on the Cu at this temperature to form a Stranski-Krastanov growth morphology. The agglomeration is much more rapid on polycrystalline films, suggesting that high surface diffusivity paths (grain boundaries and possibly other defects) enhance the surface diffusion of Pd on Cu.     

热处理对MgO基片的表面形貌以及对CeO_2和Tl-2212薄膜生长的影响

研究了MgO基片在高温退火时表面形貌和表面结构的变化,以及它对CeO2缓冲层和Tl-2212超导薄膜生长的影响。原子力显微镜(AFM)研究表明,在流动氧环境中1100℃温度下退火,MgO的表面首先由未退火时的皱褶形貌,演化为光滑表面,随着退火时间的延长,表面形貌最终演化为具有光滑基底的独立生长峰结构。XRD测试表明,通过高温热处理可以大幅度提高MgO基片表面结晶的完整性。在1100℃温度下热处理8小时的MgO基片上可以生长出具有高度c轴取向的CeO2(001)缓冲层。然后在此缓冲层上制备了厚度为500nm的外延Tl-2212超导薄膜,其临界转变温度(Tc)达到108.6K,液氮温度下临界电流密度(Jc)为2.8mA/cm2,微波表面电阻Rs(77K,10GHz)约为360.9μΩ。     

MgO单晶基片上YBCO高温超导薄膜的制备

在2英寸MgO(001)单晶基片上,采用直流溅射法,通过基片高温退火,成功制备了性能优越的YBa2C3O7-δ(YBCO)双面超导薄膜,能够满足超导滤波器的设计要求。X射线衍射(XRD)分析表明经过退火的基片上生长的YBCO薄膜与基片有单一的外延取向关系;用原子力显微镜(AFM)和高能电子衍射(RHEED)分析高温退火对基片表面状况的改变。结果表明制备的YBCO薄膜具有很好的超导电性,薄膜临界电流密度Jc(77K,0T)≈2.5×106A/cm2,微波表面电阻Rs(10GHz,77K)≈0.16mΩ。     

Strain induced epitaxial relationships of Cr on Co/Pd(111)

The growth and structure of Co ultra-thin films on Pd(111) and Cr on Co/Pd(111) have been analyzed by grazing incidence X-ray diffraction and low energy electron diffraction. It is shown that the in-plane lattice constant of the epitaxial Co film depends on the growth temperature. Although the strain decreases as a function of the Co film thickness, it persists for 20 monolayer (ML) films or even thicker. When Cr is deposited at room temperature on a strained Co film (10 to 20 ML thick) a Kurdjumov–Sachs epitaxial relationship is observed, whereas when Cr is deposited on a Co(0001) single-crystal or on a very thick Co film on Pd(111), a Nishyama–Wassermann orientation is obtained.     

Growth of epitaxial thin Pd(1 1 1) films on Pt(1 1 1) and oxygen-terminated FeO(1 1 1) surfaces

Thin Pd films (1-10 monolayers, ML) were deposited at 35 K on a Pt(1 1 1) single crystal and on an oxygen-terminated FeO(1 1 1) monolayer supported on Pt(1 1 1). Low energy electron diffraction, Auger electron spectroscopy, and Kr and CO temperature programmed desorption techniques were used to investigate the annealing induced changes in the film surface morphology. For growth on Pt(1 1 1), the films order upon annealing to 500 K and form epitaxial Pd(1 1 1). Further annealing above 900 K results in Pd diffusion into the Pt(1 1 1) bulk and Pt-Pd alloy formation. Chemisorption of CO shows that even the first ordered monolayer of Pd on Pt(1 1 1) has adsorption properties identical to bulk Pd(1 1 1). Similar experiments conducted on FeO(1 1 1) indicate that 500 K annealing of a 10 ML thick Pd deposit also yields ordered Pd(1 1 1). In contrast, annealing of 1 and 3 ML thick Pd films did not result in formation of continuous Pd(1 1 1). We speculate that for these thinner films Pd diffuses underneath the FeO(1 1 1).     

Study of ultrathin iron silicide films grown by solid phase epitaxy on the Si(001) surface

Ultrathin films of iron silicide have been grown by high-temperature annealing of 0.14-to O.5O-nm-thick Fe films deposited on the Si(001) surface at room temperature. It has been found that annealing leads to the formation of nanoislands of iron silicide on the surface, so that their type depends on the thickness of the Fe film. High-energy electron diffraction and atomic force microscopy measurements have revealed that the deposition of Fe films less than 0.32 nm thick on the Si(001) surface stimulates epitaxial growth of both three-dimensional β-FeSi₂ and two-dimensional γ-FeSi₂ islands. It has been found that, for Fe coverages of more than 0.32 nm thick, a complete transition to solide phase epitaxy is observed only for two-dimensional β-FeSi₂ islands. The effect of prolonged annealing at 850°C on the morphology of the surface of the iron silicide film has been investigated.     

Study of the structural perfection and distribution/redistribution of silicon in epitaxial GaAs films grown by molecular beam epitaxy on (100), (111)A, and (111)B substrates

Silicon distribution before and after thermal annealing in thin doped GaAs layers grown by molecular beam epitaxy on (100)-, (111)A-, (111)B-oriented substrates is studied by X-ray diffraction and SIMS. The surface morphology of the epitaxial films inside and outside an ion etch crater that arises during SIMS measurements is studied by atomic force microscopy. Distinctions in the surface relief inside the crater for different orientations have been revealed. Observed differences in the doping profiles are explained by features of the surface relief developing in the course of ion etching in SIMS measurements and by enhanced Si diffusion via growth defects.     

Comparative AES and RHEED study of the formation of Pd silicide on clean and oxide covered Si(100) and (111) surfaces

The formation and epitaxial orientation of Pd silicide on clean and native oxide covered Si(100) and (111) surfaces was studied by Auger electron spectroscopy (AES) and reflection high energy electron diffraction (RHEED). Pd was vapor deposited in UHV on to the substrates up to thicknesses of about 6 nm. On clean Si substrates, ultra-thin Pd deposits reacted to form Pd₂Si already at room temperature, as detected by a characteristic splitting of the Si LVV Auger peak. However, a polycrystalline structure with very small crystallite sizes was indicated by diffuse ring patterns in RHEED. When the initial thickness of the Pd deposit exceeded about 3 nm, the diffraction ring pattern of unreacted metal developed. During annealing of room temperature deposits of Pd, the (100) and (111) substrates behaved differently. Larger crystallites formed on Si(100), but the films remained polycrystalline, though textured. On Si(111), virtually perfect epitaxial re-orientation of the silicide was found. When the substrates were initially covered with native oxide of about 2 nm thickness, silicide formation started at about 200°C, resulting in polycrystalline, but strongly textured Pd₂Si. Upon further annealing at temperatures up to 600°C, an additional phase of epitaxially oriented Pd₂Si developed on Si(111), similar to that on clean Si(100). In all experiments, extended annealing at temperatures above 250°C caused segregation of Si to the surface. This was accompanied by the development of an additional peak in the Auger electron spectra at about 313 eV, which we assign to a plasmon loss of δE = 17 eV in the Si overlayer, being excited by Pd Auger electrons of energy 330 eV.     

GaAs(100)衬底上C60单晶膜的取向生长

利用双温区真空蒸发沉积技术成功地在GaAs（100）衬底上实现了完全（111）取向的C₆₀单晶膜的生长．用扫描电子显微镜和Ｘ射线衍射技术对C₆₀单晶膜的形貌和结构进行了分析．结果表明：能实现C₆₀取向生长的衬底温度范围很窄，温度过高或过低都易造成晶粒的取向无序．对实验结果做出了合理的解释，并讨论了C₆₀单晶膜的生长机制 关键词：     

在Pd/Cu(100)表面上外延的超薄Co膜的结构和磁性

利用脉冲激光溅射(PLD)和分子束外延(MBE)方法制备了超薄膜系统 Co/Pd/Cu(100).脉冲激 光溅射生长的单原子Pd层呈现了很好的二维生长模式.在这个Pd表面上，分子束外延生长的C o层直至12个原子层都表现了层-层生长模式.利用俄歇电子谱(AES)和低能电子衍射(LEED)研 究了该系统的表面结构.利用低温磁光克效应(MOKE)研究了系统的磁学性质.结构研究表明， Co层由于面内晶格失配应力而具有一个四方正交结构；与对比样品Co/Cu(100)的比较研究说 明Pd层的存在强烈地改善了Co膜的起始生长模式和结构.磁光克效应测量表明，Pd层的存在 改变了Co层的磁学性质. 关键词： 薄膜的磁性质 组织与形貌 界面磁性     

Annealing effects of sapphire substrate on properties of ZnO films grown by magnetron sputtering

The annealing effects of sapphire substrates on the quality of epitaxial ZnO films grown by dc reactive magnetron sputtering were studied. The atomic steps formed on (0001) sapphire (α-Al₂O₃) substrates surface by annealing at high temperature were analyzed by atomic force microscopy. Their influence on the growth of ZnO films was examined by X-ray diffraction and photoluminescence measurements. Experimental results indicate that the film quality is strongly affected by annealing treatment of the sapphire substrate surface. The optimum annealing temperature of sapphire substrates for ZnO grown by magnetron sputtering is 1400 °C for 1 h in air. PACS 81.40.Ef; 68.55.Jk; 81.05.Dz; 81.15.Cd     

Structural manipulation of ultrathin organic films on metal surfaces: the case of decane thiol/Au(111)

3 (CH₂)₉]SH) have been adsorbed on Au(111) single crystals both via vacuum deposition and from an ethanolic solution. The epitaxial structure of the ultrathin organic films has been identified at room temperature via low-energy electron diffraction to be c(4×2)R30° for the solution grown film and rectangular c(23×) for the vacuum deposited film. These structures correspond to molecules adsorbed on the surface with their carbon chains flat on the surface (vacuum deposited) and nearly perpendicular (solution grown). It is demonstrated that this orientation can be changed reversibly in vacuum via either annealing the films or exposing them to additional gas. Received: 7 February 1997/Accepted: 27 May 1997     

Influence of preparation conditions on the depth-dependent composition of AuPd nanoparticles grown on planar oxide surfaces

The high resolution depth profiling capabilities of medium energy ion scattering are employed to determine the depth dependent composition of Au/Pd nanoparticles grown on thin silica films on Si(100) as functions of Au/Pd composition, total metal loading and annealing temperature. We show that, despite the fact that Au is deposited prior to Pd, the surface of the particles is generally enriched in Au compared to the bulk composition. The extent of this Au enrichment decreases with annealing temperature. In addition, we examine the influence of the adsorption of acetic acid on the surface composition of Au/Pd particles grown on thin alumina films on NiAl(110). We find that acetic acid causes limited segregation of Pd to the bimetallic surface of relatively Au-rich particles.     

A leed-aes study of thin Pd films on Si(111) and (100) substrates

A system Pd (deposit)-Si (substrate) has been studied by LEED and AES. Pd₂Si formed on Si(111) became epitaxial after a short time of annealing at a temperature between 300 and 700°C, while the Pd₂Si formed on Si(100) did not, in both cases the surfaces of the Pd₂Si being covered with a very thin Si layer. A sequence of superstructures (3√3 × 3√3), (1 × 1), and (2√3 × 2√3) was observed successively in Pd/Si(111) as the annealing temperature was increased. A (√3 × √3) structure was obtained by sputtering the 3√3 surface slightly. It was found that the √3 structure corresponds to Pd²Si(0001)-(1 × 1) grown epitaxially on Si(111), and that the 3√3 structure comes from the thin Si layer accumulated over the silicide surface, while the 2√3 and 1 structures arise from a submonolayer of Pd adsorbed on Si(111). Superstructures observed on a Pd/Si(100) system are also studied.     

Study of the features of BaF<Subscript>2</Subscript> heteroepitaxy on CaF<Subscript>2</Subscript>/Si(100) layers obtained in the high-temperature growth mode

The surface morphology of BaF₂ epitaxial films grown by MBE (molecular beam epitaxy) in various modes on the surface of CaF₂/Si(100) is investigated by AFM. The CaF₂ layers on Si(100) are obtained in the high-temperature growth mode (Т _S = 750°C). It is shown that the epitaxy of BaF2 at a temperature of 600°C at the initial stage of growth leads to the formation of defects such as perforations in the epitaxial film, while epitaxy at a temperature of 750°C provides a defect-free film with a surface morphology suitable for the subsequent growth of semiconductors of IV–VI type and solid solutions based on them.     

On new two-dimensional structures produced on the Si (111) and Si (100) surface upon molecular-beam epitaxy of cobalt and silicon

Highly perfect epitaxial heterostructure CoSi₂ films have been grown on the surface of Si (111) and Si (100) single crystals by the method of molecular-beam epitaxy. The optimal regimes of the film growth with different thicknesses have been determined. It has been shown that short-term annealing of epitaxial films at T = 900–950 K leads to the formation of new CoSi₂/Si(111)-2 × 2 and CoSi₂/Si(100)−2 × 4 superstructures.     

ZnO-Si不同退火条件对生长ZnSe薄膜的影响

研究了作为缓冲层的ZnO薄膜在不同的退火时间、退火温度下退火对Si衬底上生长ZnSe膜质量的影响。当溅射有ZnO膜的Si(111)衬底的退火条件变化时，从X射线衍射谱（XRD）和光致发光谱（PL）中可见，ZnSe(111)膜的晶体质量有较大的变化。变温的PL谱表明，Si衬底上生长的具有ZnO缓冲层的ZnSe膜的近带边发射峰起源于自由激子发射。     

Structure and composition of gallium nitride films produced by processing gallium arsenide single crystals in atomic nitrogen

Thin GaN films are grown on (001) single-crystal GaAs substrates processed in an atmosphere of active nitrogen radicals. Auger electron spectroscopy is applied to take the depth profiles of the basic chemical elements that enter into the composition of the epitaxial GaN films and single-crystal GaAs substrates. It is found that the surface composition of the GaN films is characterized by considerable nonstoichiometry (the excess nitrogen achieves ≈9%), which is caused by the presence of atomic nitrogen in the discharge chamber. With a high-resolution X-ray diffraction method, the structural perfection of the epitaxial layers is investigated. It is shown that low-temperature annealing (at temperatures below 700°C) is responsible for the formation of cubic GaN films on the (001) surface of cubic GaAs, whereas higher temperature annealing results in the growth of the hexagonal films.     

Effects of sapphire substrate annealing on ZnO epitaxial films grown by MOCVD

The annealing effects of sapphire substrate on the quality of epitaxial ZnO films grown by metalorganic chemical vapor deposition (MOCVD) were studied. The atomic steps formed on (0 0 0 1) sapphire (α-Al₂O₃) substrate surface by annealing at high temperature was analyzed by atomic force microscopy (AFM). The annealing effects of sapphire substrate on the ZnO films were examined by X-ray diffraction (XRD), AFM and photoluminescence (PL) measurements. Experimental results indicate that the film quality is strongly affected by annealing treatment of the sapphire substrate surface. The optimum annealing temperature of sapphire substrates is given.     

Interfacial reactions of ultrahigh vacuum deposited ytterbium thin films on silicon

Epitaxial ytterbium silicide thin films were grown on (111)Si by ultrahigh vacuum deposition and subsequent thermal annealing. The epitaxial YbSi(2-x) thin films consist of various kinds of defects such as vacancies, stacking faults, and pinholes. The vacancies were ordered so as to relax the compressive stress in Si sublattice of YbSi(2-x) thin films. The vacancy ordering structure is of an out-of-step structure with higher vacancy concentration after higher temperature annealing so that the compressive stress was further relaxed. A high density of stacking faults was present in the epitaxial YbSi(2-x) thin films. The stacking faults were annihilated by high temperature annealing. Pinholes also formed in the epitaxial YbSi(2-x) thin films and could be avoided by appropriate fabrication process. The epitaxial YbSi(2-x) thin films were thermally stable up to 1000 degrees C.