Ti与Ag离子顺次注入SiO2合成TiO2纳米结构及其光催化活性

通过Ti离子单注入或与Ag离子顺次注入、结合后续的N₂气氛下热退火处理,在SiO₂基体的浅表面层合成TiO₂纳米结构,详细研究了该纳米结构的形貌、结构、光学特性及其光催化性能。结果表明：Ti离子单注入或与Ag离子顺次注入并经热处理后均能在SiO₂中产生TiO₂纳米颗粒,700℃退火后形成的纳米颗粒主要为锐钛矿相,继续升高退火温度,TiO₂纳米颗粒逐渐转变为金红石相。Ag的附加注入不仅能促进TiO₂纳米颗粒的生长,而且可以降低其形成的温度及光学带隙。此外,光催化实验结果还显示,Ag的附加注入能够提高所合成的TiO₂纳米颗粒光催化活性。结合光致发光和X射线光电子能谱测试结果分析并给出了附加Ag离子注入导致所合成的TiO₂ 纳米结构光催化活性提升的可能机理。     

RBS和XRD研究Fe、N共掺ZnO薄膜的制备

以Zn3N2:Fe为前驱物,用热氧化法在石英玻璃衬底上成功制备了一组Fe、N共掺杂的ZnO薄膜。用卢瑟福背散射(RBS)和X射线衍射(XRD)研究了Zn3N2:Fe在不同热氧化温度下的退火行为和结构演变。实验结果显示:刚长成的样品为Zn3N2:Fe薄膜;300oC氧化后,样品表层的Zn3N2:Fe转化为ZnO:(Fe,N),表层以下的膜层未被氧化;退火温度高于400oC时,Zn3N2:Fe薄膜全部转化为多晶结构的ZnO:(Fe,N)薄膜;500oC退火,薄膜开始向衬底扩散;600oC–700oC退火,薄膜向衬底扩散明显。在XRD灵敏度范围内,薄膜中未发现Fe团簇或与Fe相关的二次相(如Fe3O4、Fe2O3、FeO)。SQUID测量显示:在500oC退火条件下,ZnO:(Fe,N)薄膜的室温饱和磁化强度(Ms)最大。     

纳米复合永磁合金Nd9Fe85-xMnxB6的结构和磁性

利用X射线衍射(XRD)和X射线吸收精细结构(XAFS)技术对淬火速度为20m／s的退火和未退火Nd9Fe85-xMnxB6(x=0，0．5和1．0)样品分别进行了晶体结构和Fe原子局域环境的分析，并用振动样品磁强计分析了样品的磁性。结果表明：退火前，掺杂微量Mn原子对纳米复合Nd-Fe-B磁性材料的晶体结构和近邻配位无序度都有显著影响，随着Mn含量的增加，Nd2Fe14B硬磁相和α-Fe软磁相的结晶度明显增加；在温度为973K、5min退火后，Nd9Fe85-xMnxB6(x=0，0．5和1．0)磁体的主相结构基本相同，但矫顽力由339kA／m增加到398kA／m,我们认为这是由于掺杂的Mn原子影响Nd2Fe14B和α-Fe颗粒晶界的交换耦合作用所致。     

Fe-1.5wt% Cu合金中Cu纳米颗粒与微观缺陷热回复过程研究

不锈钢结构材料中Cu纳米团簇是导致核反应堆压力容器钢脆化的主要原因之一。本文用扫描电子显微镜(SEM)和正电子湮没谱学(PAT)研究材料中的纳米Cu颗粒以及微观缺陷经热处理后的回复过程。PAT测量结果表明,Fe-1.5wt%Cu合金在1 173 K高真空退火处理后,主要缺陷得以回复,合金中存在Cu纳米颗粒且能吸引并捕获热化后的局域态正电子。SEM对不同温度退火样品的微观结构进行表征,结果表明,随着退火温度的升高,合金中Cu纳米颗粒的浓度逐渐降低。1473 K退火,SEM未观测到明显的Cu纳米颗粒,而多普勒展宽能谱的W参数表明合金中仍存在微小Cu纳米颗粒。     

~(57)Fe注入铜的穆斯堡尔效应研究(Ⅱ)——注入特性和铁磁相变化

我们曾报道了在同一剂量下的~(57)Fe离子注入铜随退火温度变化的特性,观察到注入铁离子所处的三种不同位:固溶态的孤立铁原子、具有二个或更多铁原子结合在一起的固溶态原子组团(Cluster)和γ-Fe夹杂相;经一定温度退火后,固溶态的铁原子和γ-Ee分别通过凝聚和相变转变成具有体心立方结构的α-Fe;在600℃退火后α-Fe全部消失转变成固溶态铁。本文着重报道不同的~(57)Fe注入剂量对铁原子不同位的强度和它们的超精细参数的影响以及它们随不同退火温度的变化关系。     

Ag离子注入ZnO薄膜对其发光性质的影响

采用磁控溅射技术在蓝宝石基底上制备了Zn O薄膜,并对样品在氧气氛下进行了热处理,然后采用不同能量、剂量的Ag离子注入Zn O薄膜中,形成Ag纳米颗粒。利用X射线衍射、光致发光、紫外可见吸收等技术详细地研究了样品的结构与发光性质。结果表明,未注入的Zn O薄膜在380 nm和610 nm处出现发光峰,分别对应Zn O激子峰与深能级缺陷峰。Ag离子注入Zn O样品的激子发光峰增强,并在400 nm和430 nm左右处出现新发光峰,同时深能级缺陷引起的发光峰减弱。在N2气氛下退火处理后,Ag离子注入Zn O样品在400 nm处的发光峰消失,430 nm左右发光峰减弱。Ag离子注入Zn O薄膜中合成了Ag纳米颗粒,观察到了Ag纳米颗粒的等离子共振效应。对Ag纳米颗粒和离子注入产生的缺陷、Zn O发光性质的影响给出了解释。     

铁基纳米微晶薄膜巨磁阻抗效应的Mossbauer研究

本文采用Mossbauer谱学方法以及其它手段对FeCuNbSiB薄膜样品在退火过程中出现的巨磁阻抗效应发生显著变化的原因进行了探讨。研究表明,样品在退火过程中除了生长纳米晶粒α-FeSi相对提高材料的软磁性能有利外,同时随退火温度变化样品中磁矩分布方向会发生重取向。由制备态到570℃退火温度期间,薄膜样品磁矩取向发生由平行于平面为主变为垂直为主,而后再转变为平行为主。这些因素对多层膜巨磁阻抗效应的变化会产生重要影响,尤其当磁矩在垂直于平面方向分布占优势时,磁阻抗效应会显著下降。     

铁基纳米微晶薄膜巨磁阻抗效应的Mssbauer研究

本文采用 M?ssbauer 谱学方法以及其它手段对 FeCuNbSiB 薄膜样品在退火过程中出现的巨磁阻抗效应发生显著变化的原因进行了探讨。研究表明,样品在退火过程中除了生长纳米晶粒α ? FeSi相对提高材料的软磁性能有利外,同时随退火温度变化样品中磁矩分布方向会发生重取向。由制备态到 570 ℃退火温度期间,薄膜样品磁矩取向发生由平行于平面为主变为垂直为主,而后再转变为平行为主。这些因素对多层膜巨磁阻抗效应的变化会产生重要影响,尤其当磁矩在垂直于平面方向分布占优势时,磁阻抗效应会显著下降。     

一个Sm(Co,Fe,Cu,Zr)_(7.5)铸态样品的穆斯堡尔谱分析

由于R_2Co_(17)型稀土钴永磁合金具有高的磁能积、磁晶各向异性和居里温度,且较RCo_5型稀土钴永磁合金节省钐钴,因而发展成为高性能的实用的永磁体。 本文报告我们制备的一个含铁量较实用的、要求高的Sm_2(Co,Fe,Cu,Zr)_(17)永磁合金铸态样品,其成分是:26Sm-39.5Co-24.5Fe-8Cu-2Zr,在自制等加速穆斯堡尔谱仪上用~(57)Co(Pd)源测得室温下的透射谱。拟合实验谱     

热处理增强Au纳米颗粒超薄膜光电子发射的研究

本文制备了平均直径为1.4 nm的11-巯基十一烷酸(Mercaptoundecanoic acid,MUA)修饰的金纳米颗粒,随后通过硅晶片上壳聚糖薄涂层静电吸附制备了厚度约为10 nm的超薄膜,原子力显微镜(Atomic Force Microscopy,AFM)和扫描电子显微镜(Scanning Electron Microscopy,SEM)表明金纳米颗粒在薄膜中分布较为均匀且薄膜较平整。进一步采用紫外光电子能谱(Ultraviolet Photoelectron Spectroscopy,UPS)研究了不同热处理温度对超薄膜的二次电子发射能力的影响。结果表明,适度的热处理有助于超薄膜二次电子发射强度的提高,尤其是经150°C热处理的薄膜二次电子发射峰强是未处理样品的4倍,更高的热处理温度造成二次电子发射峰强度急剧下降。本文结果有助于推动有机配体金纳米颗粒超薄膜在光电子发射材料方面的应用。     

AFM Study of combinatorial Ga^＋ implanted Co7Ag93 film and its Kerr effect

In this paper,a magnetooptic chip was prepared on Si wafer by combinatorial Ga^ implantation into ion sputtered Co7Ag93 film.The surface morphology of each unit of the chip was detected by AFM,while their Kerr effect was measured by MOKE equipment.It is observed that the maximum Kerr rotation (MKP) occurs when the incident photon energy is around 3.8-3.9eV.Summarization of MKR versus implanted Ga^ dose shows that the MKR enhancement by Ga^ implantation can be characterized as incubation,enhancement and saturation regions.Considering the mutual solubility and surface morphology transition after annealing,it is suggested that Ga^ tends to form CoGa and /or CoGa3 intermetallic compounds.Before the formation of CoGa3 compounds,no apparent MKR enhancement could be observed While when the surface is half occupied by forest-like CoGa3 compounds,MKR enhancement will be saturated.By comparison of the maximum Kerr rotation with the cone areal density,it can be induced that not only the bulk concentration and structrue,but also the surface morphology plays an important role in magnetooptic Kerr effect.     

Characterisation of annealed Fe/Ag bilayers by RBS and XRD

Recently Fe/Ag thin films have been intensively investigated due to their special magnetic properties. To study the stability of the Fe–Ag interfaces very long time experiments are necessary at room temperature. To enhance the processes which take place at interfaces, high temperature annealing can be used. A detailed annealing experiment was carried out on Si-covered Fe/Ag (Ag grown on Fe) and Ag/Fe (Fe grown on Ag) polycrystalline bilayers, which were deposited on Si(1 1 1) substrates by MBE method. Heat treatments of various duration and temperature were applied in UHV conditions. Rutherford backscattering spectrometry and X-ray diffractometry were used to determine the effects of the heat treatments. In case of Fe/Ag samples, formation of iron–silicide phases was observed between the Fe layer and Si substrate, and the silver and the silicon capping layer were also completely mixed with each other. In case of the Ag/Fe samples the silver moved to the sample surface through the iron layers, while iron shifted to the substrate and mixed with silicon.     

Effect of swift heavy ion irradiation in W/Co multilayer structures

Present study reports effect of swift heavy ion irradiation on structural and magnetic properties of sputtered W/Co multilayer structures (MLS) having bilayer compositions of [W(10 Å)/Co(20 Å)]_5BL and [W(20 Å)/Co(20 Å)]_5BL. These MLS are irradiated by 120 MeV Au⁹⁺ ions up to fluence of 1 × 10¹³ ions/cm². X-ray reflectivity (XRR), wide-angle X-ray diffraction (WAXD), cross-sectional transmission electron microscopy (X-TEM) and magneto optical Kerr effect (MOKE) techniques are used for structural and magnetic characterization of pristine and irradiated MLS. Analysis of XRR data using Parratt’s formalism shows a significant increase in W/Co interface roughness. WAXD and X-TEM studies reveals that intra-layer microstructure of Co-layers in MLS becomes nano-crystalline on irradiation. MOKE study shows slight increase in coercivity at higher fluence, which may be due to increase in surface and interface roughness after recrystallization of Co-layers.     

Probing Co/Si interface behaviour by X-ray photoelectron spectroscopy （XPS） and atomic force microscopy （AFM）

In this work, we investigate the Co-Si reaction, the Co growth mode at room temperature, diffusion behaviour as well as morphology evolution during annealing on both H-terminated and clean Si（001） and Si（lll） surfaces. From in-situ X-ray photoelectron spectroscopy （XPS） investigation, ＂Co-Si＂ reaction appears to occur on both H-terminated and clean surfaces at room temperature （RT） and the silicide crystallinity is improved upon annealing. Co growth mode on H-terminated Si surfaces occurs in a pseudo layer-by-layer manner while small close-packed island growth mode is observed on the clean Si surface. Upon annealing at different temperatures, Co atom concentration decreases versus annealing time, which in part is attributed to Co atoms inward diffusion. The diffusion behaviour on both types of surfaces demonstrates a similar trend. Morphology study using ex-situ atomic force microscopy （AFM） shows that the islands formed on Si（001） surface after annealing at 700℃ are elongated with growth directions alternate between the two perpendicular [110 ] and [ 110] directions. Triangular islands are observed on Si （111） surface.     

Structural characterization of Fe/Ag bilayers by RBS and AFM

Fe/Ag thin films are intensively investigated due to their special magnetic properties. Recently a deposition-order dependent asymmetric interface has been found. When iron is grown on silver, the interface is sharp, while the growth of Ag on Fe results in a long, low-energy tail of the Ag peak in the Rutherford backscattering spectrometry (RBS) spectra. The main purpose of this paper is to show that the low-energy Ag tail is caused by grain boundary diffusion, and that, when elevating the growing temperature of the Ag layer this effect becomes more significant. Two sets of polycrystalline and epitaxial Fe/Ag bilayers were prepared simultaneously onto Si(1 1 1) and MgO(1 0 0), respectively. The iron layers were grown at 250 °C and annealed at 450 °C in both sets, while the Ag layer was grown in the first set at room temperature (RT) and in the second set at 250 °C (HT). The sample composition, the interface sharpness and the quality of the epitaxy were studied by Rutherford backscattering spectrometry (RBS) combined with channeling effect. The surface morphology was determined by atomic force microscopy (AFM). RBS spectra show that in the case of RT samples the epitaxial MgO/Fe/Ag bilayer has sharp, well-defined interface, while for the polycrystalline Si/Fe/Ag sample the silver peak has a low-energy tail. Both the Fe and Ag peaks smeared out in the case of HT samples. AFM-images show that the RT samples have a continuous Ag layer, while the HT samples have fragmented surfaces. The RBS spectra taken on the HT samples were successfully simulated by the RBS-MAST code taking into account their fragmented structures.     

The effects of the annealing time on helium implantation in Si

The modifications induced in silicon samples by helium implantation before and after isothermal annealing at 673 K have been investigated. The surface morphology has been detected by atomic force microscopy. A hillock structure is observed on the sample surface before and after annealing for 5-10 min. Surface blister formation is observed with an increasing annealing time. The variation of crystal damage with annealing time has been investigated by Rutherford backscattering/channeling. The intensity of the damage peak first increases with annealing time, reaches maximum at an annealing time of 60 min and then decreases. Helium-induced bubbles and residual defects have been observed by transmission electron microscopy, which shows that dislocations are close to the bubbles.     

Incorporation of oxygen during oxidative annealing of thermally evaporated In films

The paper describes studies on compositional, morphological and optical characteristics of thin indium oxide films prepared by annealing thermally evaporated indium metal films in 423-723 K temperature range in air. The incorporation of oxygen in the films has been probed by depth profiling oxygen using ¹⁸O(p, α)¹⁵N nuclear reaction and 3.05 MeV ¹⁶O(α, α)¹⁶O resonant scattering. The morphology of the films has been examined by atomic force microscopy while their structure by glancing incidence X-ray diffraction. As grown In films are polycrystalline and consist of well-aligned (In) hillocks. The hillocks in thin films (∼12 nm) are nanosized and conical in shape while those in thicker films (∼130 nm) are micron-sized with rather flat tops. Nanosized hillocks impart films enhanced reactivity towards oxygen. Consequently thinner films contain high amount of adsorbed oxygen in as-deposited state and undergo facile oxidation. The hillocks are obliterated in the process. The enhanced reactivity is attributed to high surface energy, generally associated with nanoparticles, and residual stress. These films exhibit high transmission (>90%) on annealing beyond 473 K. Micro-sized hillocks, on the other hand lend pronounced roughness to the films. Roughness and lower surface free energy which manifests in the form of flatter hillock tops, make the films oxidation-resistant. Depth profile measurements in thicker films show that oxidation starts at the surface and proceeds into the interiors of the film with increase in the duration of annealing. The films are deficient in oxygen, even as X-ray diffraction shows the formation of polycrystalline indium oxide. These have low transmission (<30%) and their band gaps increase with the temperature and duration of annealing. The increase in band gap is attributed to the gradual oxidation of interior regions that are initially significantly deficient in oxygen and improvement in crystallinity.     

PET薄膜中32S离子径迹的热退火效应

采用径迹蚀刻的方法研究了热处理对聚对苯二甲酸乙二醇酯（PET）薄膜中重离子径迹的热退火效应。使用113.7 MeV的³²S离子在PET薄膜中产生垂直于表面且贯穿薄膜的离子径迹。对薄膜进行局部热处理，加热温度为70～240 ℃，时间为1～300 s。薄膜经过化学蚀刻成核孔膜后使用显微镜观测。结果表明：在相同的热处理时间下，随着热处理温度的升高，PET薄膜中离子径迹的热退火效应愈加明显；在热处理温度不变的情况下，随着热处理时间的增加，退火效应亦愈加明显。     

Implantation of anatase thin film with 100 keV Fe ions: Damage formation and magnetic behaviour

We have investigated the damage morphology and magnetic properties of titanium dioxide thin films following implantation with Fe ions. The titanium dioxide films, having a polycrystalline anatase structure, were implanted with 100 keV ⁵⁶Fe⁺ ions to a total fluence of 1.3 × 10¹⁶ ions/cm². The ion bombardment leads to an amorphized surface with no indication of the presence of secondary phases or Fe clusters. The ion-beam induced damage manifested itself by a marked change in surface morphology and film thickness. A room temperature ferromagnetic behaviour was observed by SQUID in the implanted sample. It is believed that the ion-beam induced damage and defects in the polycrystalline anatase film were partly responsible for the observed magnetic response.     

Nonlinear optical properties of MeV and keV ion beam synthesized Ag nanoclusters

Ag nanoclusters embedded in silica glass matrix have been synthesized by high fluence ion implantation using both keV and MeV ion beams. In keV implantation case, optical absorption shows an intense surface plasmon resonance (SPR) peak corresponding to the Ag clusters formed in the matrix. Transmission electron microscopy (TEM) measurements carried out on identically implanted SiO₂ thin films on a TEM catcher grid shows the presence of Ag nanoclusters of size around 4 nm in the matrix. However, for the MeV implantation case, the SPR peak appears in the optical absorption spectra only after air annealing the sample at 500 °C for one hour. For the annealed samples, TEM measurements show the presence of 6 nm sized Ag nanoclusters. On the other hand the as-implanted sample shows smaller nanoclusters with a lower particle density in the matrix. Interestingly, open aperture z-scan measurements carried out on keV implanted samples did not show any nonlinear absorption, while the MeV as-implanted as well as annealed samples showed nonlinear absorption. The nonlinear absorption coefficient of the MeV annealed sample is extracted from a fit to the z-scan data considering a three photon like absorption process.