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Three titanium (Ti) targets with different purities were used to prepare Ti films on polyimide substrates by DC magnetron sputtering. The microstructures of Ti films were characterized by a metallographic microscope, X-ray diffractometer, field emission scanning electron microscope and three-dimensional surface topography instrument. In this study, we investigated the effects of Ti target purity and microstructure on film deposition rate, surface roughness, microstructure and resistivity. The results show that the deposition rate increased with increasing Ti target purity. Ti film deposited by the high-purity (99.999%) Ti target has fewer surface particles with smaller size, lower surface roughness and lower resistivity when compared to that prepared by the Ti target of low purity (99.7%). The surface roughness of Ti film prepared by the high-purity Ti target was Sa = 121 nm, the deposition rate was 16.3 nm/min and the resistivity was 6.9 × 10−6 Ω·m. For Ti targets of the same purity, the performance of Ti film prepared by a target with equiaxed α-phase grains is better than that of Ti film prepared by a target with twins and β-phase grains.

Mo-48.2% Ag films were fabricated by direct current (DC) magnetron sputtering and annealed in an argon atmosphere. The effects of annealing on the surface morphology, resistivity and surface-enhanced Raman scattering (SERS) performance of Mo-48.2% Ag films were investigated. Results show a mass of polyhedral Ag particles grown on the annealed Mo-48.2% Ag films’ surface, which are different from that of as-deposited Mo-Ag film. Moreover, the thickness and the resistivity of Mo-48.2% Ag films gradually decrease as the annealing temperature increases. Furthermore, finite-difference time-domain (FDTD) simulations proved that the re-deposition Ag layer increases the “hot spots” between adjacent Ag nanoparticles, thereby greatly enhancing the local electromagnetic (EM) field. The Ag layer/annealed Mo-48.2% Ag films can identify crystal violet (CV) with concentration lower than 5 × 10−10 M (1 mol/L = 1 M), which indicated that this novel type of particles/films can be applied as ultrasensitive SERS substrates.

Surface science is an interdisciplinary field involving various subjects such as physics, chemistry, materials, biology and so on, and it plays an increasingly momentous role in both fundamental research and industrial applications. Despite the encouraging progress in characterizing surface/interface nanostructures with atomic and orbital precision under ultra-high-vacuum (UHV) conditions, investigating in situ reactions/processes occurring at the surface/interface under operando conditions becomes a crucial challenge in the field of surface catalysis and surface electrochemistry. Promoted by such pressing demands, high-pressure scanning tunneling microscopy (HP-STM) and ambient pressure X-ray photoelectron spectroscopy (AP-XPS), for example, have been designed to conduct measurements under operando conditions on the basis of conventional scanning tunneling microscopy (STM) and photoemission spectroscopy, which are proving to become powerful techniques to study various heterogeneous catalytic reactions on the surface. This report reviews the development of HP-STM and AP-XPS facilities and the application of HP-STM and AP-XPS on fine investigations of heterogeneous catalytic reactions via evolutions of both surface morphology and electronic structures, including dehydrogenation, CO oxidation on metal-based substrates, and so on. In the end, a perspective is also given regarding the combination of in situ X-ray photoelectron spectroscopy (XPS) and STM towards the identification of the structure−performance relationship.

Copper−chromium alloy film and Cu−Cr bulk alloy were obtained using magnetron sputtering and vacuum smelting. Experimental results indicated that Cu−Cr bulk alloy and alloy films having different residual stress and atomic diffusion exhibit a significant difference in microstructure evolution behaviors after annealing. Numerous polyhedral Cu particles and dendritic Cr particles precipitated on the surface of annealed Cu−Cr alloy film and as−cast Cu−Cr bulk alloy, respectively. Cu particles were formed under the driving of energy and residual stress in the film. The effect of annealing temperature and Cr content on the size and quantity of Cu particles is discussed. Cr particles precipitated on the bulk alloy due to the low solid solubility of Cr in Cu, and the crystallinity of Cu grains promoted the diffusion of Cr atoms. The surface−enhanced Raman scattering (SERS) intensity of the Cu−14.6%Cr alloy film was obviously higher than that of the Cu−14.2%Cr bulk alloy. The particles/film composite structure possessed the appropriate particle number, surface roughness, and interstitial gap, as opposed to the bulk material, to effectively improve SERS enhancement.

Copper–zirconium bulk alloy and Cu–Zr alloy films are prepared by vacuum smelting and magnetron sputtering, respectively, and subsequently annealing is conducted. Results show that Cu–Zr bulk alloy and alloy films exhibit significantly different microstructure evolution behaviors after annealing due to different microstructures and residual stress states. CuxZr alloy compounds disperse at the grain boundary of Cu grains in as-cast and annealed Cu–Zr bulk alloys. However, unlike bulk alloys, a large number of polyhedral Cu particles are formed on the Cu–Zr thin films’ surface upon thermal annealing. Kinetically, the residual compressive stress in the Cu–Zr films promotes the formation of Cu particles. The influencing factors and the path for mass transport in the formation of the particles are discussed. The large-specific surface area particles/film composite structure has potential applications in Surface-Enhanced Raman Scattering, catalysis, and other fields.