Metallic glasses are structurally disordered alloys whose compositions are designed to impede crystallization upon cooling from the liquid state.BMGs are firstly developed in the early 1990s.Owing to their superior properties,e.g.,very high corrosion and wear resistance,great yield strength and elastic limit,studies on BMGs are of significance.Annealing or thermal treatment of metallic glasses at near glass transition temperature triggers relaxation and often hampers their performances in service.Rejuvenation treatment of MGs by thermal cycling is recently intensively investigated.However,the mechanism responsible for the structural rejuvenation still remains elusive.In this thesis,we conduct systematic studies of on the rejuvenation effect of a Zr-based metallic glass annealed at near glass transition temperature for various durations,subjected to thermo-cycling treatment and a growth behavior of AuCuSi alloy film by in-situ grazing incidence small angle X-ray scattering.It is found that well relaxed samples after long-term annealing are almost unaffected by thermal cycling treatment.In contrast,while short-term annealed samples exhibit large rejuvenation effect by thermo-cycling treatment.Using synchrotron X-ray diffraction,we find that thermal cycling results in a disordering at the short-range scale,where the rejuvenation effect is large in a heterogeneous sample.More interestingly,the thermo-cycling treatment on intermediate structure with 20 h-annealed sample relatively exhibits a high degree rejuvenation effect,as compared to shorter and longer annealed samples.This finding indicates that the activation barrier for rejuvenation strongly depends on the original structural states,e.g.,free volume,inherent stress and structural heterogeneity.Multi-alloy coatings and films and studies have become growing of importance in recent days,especially for corrosion and wear resistance coatings,soft magnetic thin films and micro-electromechanical systems(MEMSs).Yet,high quality structural data in sub-micron scale is still missing due to experimental difficulty.While it is intensively researched and found that properties of thin film alloy changes with thickness of the film,the lack of understanding limits its performance.Thus,the understanding of how the atomic cluster link together during sputter process is indispensable step for moving forwards.Here,we take great advantages of in-situ grazing incidence small-angle X-ray scattering(GISAXS)measurements for investigating an AuCuSi alloy on a silicon oxide layer on a silicon substrate during sputter deposition.A further big advantage of synchrotron radiation with high statistics allows us to understand details of growth kinetics of cluster growth and initial nucleation during continuing deposition.This work combines X-ray reflectivity(XRR),Grazing incident wide angle scattering(GIWAXS),Ultra Violet-Visble spectroscopy(UV-Vis)and measurements,enables solid understanding for atomic scale evolution.