Zhengtao Wu

Titanium-doped diamond-like carbon (DLC:Ti) films were deposited by magnetron sputtering. The effects of Ti concentration on the microstructure, phase composition and piezoresistive properties of the films were systematically investigated. The surface morphology, crystal structure and chemical bonding states of the samples were characterized using SEM, XRD and XPS. The piezoresistive properties were then assessed by monitoring the resistance change in the thin films using a precision resistance meter under controlled external stimulation. The results demonstrate that the sp²/sp³ ratio of the DLC:Ti films increases with rising Ti concentration, and both Ti–C and Ti–Ti chemical bonds are formed within the films. An excessive β-Ti phase forms when the Ti concentration exceeds 39.7 at.%. The electrical resistance of DLC:Ti films decreases linearly as the applied normal stress increases from 0 to 35 MPa, with a maximum piezoresistive coefficient of −9.0 × 10⁻² GPa⁻¹ achieved for the film with a Ti doping concentration of 12.9 at.%. One hundred cyclic loading–unloading tests induce the structural transition from sp³ to sp², resulting in the graphitization of DLC:Ti films. In addition, external stress facilitates the fracture of Ti–C bonds and the relaxation of residual stress in the DLC:Ti films; the β- to α-Ti phase transformation induced by external loading is also observed in the films. Cyclic piezoresistive tests reveal that the piezoresistive stability of the DLC:Ti films is enhanced with increasing Ti concentration, which is attributed to the increased formation of Ti–C bonds in the films.

Yttrium oxide (Y₂O₃) films have been widely used as protective layers in plasma etching equipment, but achieving stoichiometric films with high deposition rates remains a challenge. In this study, Y₂O₃ films were fabricated by a medium-frequency reactive magnetron sputtering (MF-RMS) technique. The oxygen flow and target control voltage were regulated through a closed-loop feedback control system, which effectively solved the problem. The microstructure, mechanical, optical, and plasma etching properties were systematically investigated. The results showed that near-stoichiometric films can achieve a relatively high deposition rate. Increasing the deposition temperature induced a structural transition in the Y₂O₃ film from a predominantly cubic phase to a mixture of cubic and monoclinic phases. For Y₂O₃ films deposited at room temperature, increasing the bias voltage increased the deposition rate but reduced hardness and elastic modulus. The Y₂O₃ film deposited at 300 °C in the near-metallic mode exhibited the highest hardness and elastic modulus, reaching 13.3 GPa and 222.0 GPa, respectively. All Y₂O₃ films exhibited excellent transmittance and resistance to plasma etching. This study provides an effective protective strategy for semiconductor etching chambers.

A new CuNi/TiB₂ thin-film thermocouple was fabricated using magnetron sputtering. A 400 nm thick CuNi interior layer was deposited on a dielectric substrate initiatory, and then covered by an 800 nm thick TiB₂ layer. The tests revealed that the TiB₂ layer had a dense and columnar cross-section. The measured hardness and elastic modulus of the TiB₂ layer were ~20.5 and 315.9 GPa, respectively. No cracking or delamination occurred at the CuNi/TiB₂ interface. The work functions of the TiB₂ and the CuNi layers were calculated to be 4.406 and 4.726 eV, respectively. The difference in work functions between the TiB₂ and the CuNi was ~0.3 eV. The CuNi/TiB₂ thin-film sensor exhibited a high Seebeck coefficient of 38.07 μV/°C with excellent linearity. The maximum service temperature of the thin-film sensor was evaluated to be ~400 °C. A further increase in temperature degraded the Seebeck coefficient due to oxidation of the TiB₂ layer.

Effects of varying Mn and Ni concentrations on the structure and piezoresistive properties of CuMnNi films deposited by magnetron sputtering with a segmented target were investigated. An increase in the Ni content refines the CuNi film grains, inducing an increase in defects such as internal micropores and a decrease in film density. At the same time, the positive piezoresistive coefficient of the film changes to negative. When 17.5 at.% Ni was added, the negative piezoresistive coefficient of the CuNi film was −2.0 × 10⁻⁴ GPa⁻¹. The doping of Ni has a weakening effect on the positive piezoresistive effect of the film. Adding Mn into Cu refines the film grains while increasing the film density. The surface roughness of the film decreases with the increase in Mn content. When the Mn content was 16.7 at.%, the piezoresistive coefficient reached the largest recorded value of 23.81 × 10⁻⁴ GPa⁻¹, and the film exhibited excellent repeatability in multiple piezoresistive tests. After the CuMn film with 16.7 at.% Mn was annealed at 400 °C for 2 h, the film grains grew slightly and the film residual stress decreased. The optimization of the film structure can reduce the scattering of electrons during transportation. The piezoresistive coefficient of the film was further improved to 35.78 × 10⁻⁴ GPa⁻¹.

The microstructure and properties of WTi alloy films with 0~23 at.% Ti prepared by magnetron sputtering were investigated. The electrical resistivity gradually increased with the increase in the Ti content. When the Ti content was 6.8 at.%, the temperature coefficient of resistance of the alloy film reached the maximum value of 19.5 × 10⁻⁴ K⁻¹, which is 3.6 times higher than that of the pure W film. After several thermal resistance tests, the temperature coefficient of resistance of the WTi alloy film with 6.8 at.% Ti decreased gradually. After five measurements, the temperature coefficient of resistance decreased gradually from 19.5 × 10⁻⁴ to 16.3 × 10⁻⁴ K⁻¹. After annealing at 500 °C for 30 min, the grain size of the WTi alloy film (6.8 at.% Ti) increased, a few pores appeared, and the density of the film decreased. The temperature coefficient of resistance decreased from 19.5 × 10⁻⁴ K⁻¹ to 14 × 10⁻⁴ K⁻¹. When the annealing time was increased to 60 min, the structure and properties of the WTi alloy film remained basically unchanged. After conducting the annealing treatment for 30 min, the WTi films showed excellent stability in the thermal resistance tests, and their temperature coefficient of resistance was basically consistent after cyclic thermal loading, which has promising application prospects for the temperature measurement of tools and dies.

Traditional dc magnetron sputtering has a low ionization rate when preparing metallic thin films. With the development of thin film science and the market demand for thin film material applications, it is necessary to improve the density of magnetron-sputtered films. High-power pulsed magnetron sputtering (HiPIMS) technology is a physical vapor deposition technology with a high ionization rate and high energy. Therefore, in this work, HiPIMS was applied to prepare metallic tungsten films and compare the surface morphology and microstructure of metallic tungsten films deposited using HiPIMS and dc magnetron sputtering (dcMS) technology under different pulse lengths, as well as related thermal resistance performance, followed by annealing treatment for comparative analysis. We used AFM, SEM, XRD, and plasma characterization testing to comprehensively analyze the changes in the TCR value, stability, repeatability and other related performance of the metallic tungsten thin-film sensor deposited by the HiPIMS technology. It was determined that the thin film prepared by the HiPIMS method is denser, with fewer defects, and the film sensor was stable. The 400 °C annealed sample prepared using HiPIMS with a 100 μs pulse length reaches the largest recorded TCR values of 1.05 × 10⁻³ K⁻¹. In addition, it shows better stability in repeated tests.

A MoN_x coating serves as an effective wear protection layer and is crucial for the investigation of its tribological characteristics at various temperatures. This study examined the tribological characteristics of MoN_x coatings that were deposited through high-power pulsed magnetron sputtering (HiPIMS) in an Ar/N₂ environment with varying N₂ partial pressures. The microstructures and mechanical properties of the coatings were elucidated using scanning electron microscopy, grazing-incidence-angle X-ray diffraction, energy-dispersive spectroscopy, and nanoindentation. The dry friction performances of the coatings at different heating temperatures were studied using a ball-on-disk tribometer. The MoN_x coating produced by HiPIMS was composed primarily of fcc−Mo₂N and featured a fine, dense column crystal with a maximum hardness of 28.8 GPa. The MoN_x coatings exhibited excellent lubrication and wear reduction properties at room temperature (RT). The dry friction performances of the MoN_x coatings at elevated temperatures were expected to depend on the growth of the MoO₃ tribolayer. At relatively low temperatures (300 °C and 400 °C), the MoO₃ tribolayer grew slowly and was not enough to provide good lubrication, causing increases in the dry friction of the coatings. However, the δ−MoN phase formed in the MoN_x coating deposited at a high N₂ partial pressure could facilitate the formation of MoO₃ and thus decreased the friction coefficient at 400 °C. At the relatively high heating temperature of 500 °C, however, the MoO₃ tribolayer grew so rapidly that the oxide layer became thick, resulting in an increase in the wear rate. It is believed that tuning the growth rate of MoO₃ via optimizing the composition and structure of the MoN_x coatings might be a useful way to improve the dry friction at various elevated temperatures.

Alternating TiB₂-dcMS and Cr-HiPIMS layers are used to fabricate TiB₂/Cr multilayer films. Introducing a 5-nm-thick Cr interlayer deposited under a substrate bias of −60 V produces slight increases in both film hardness and elastic modulus. The TEM observation indicates that the Cr grains favor epitaxial growth on the TiB₂ interlayer, forming a coherent TiB₂/Cr interface. This improves hardness. Mechanic measurement by using AFM illustrates that the coherent interface increases the elastic modulus of the Cr up to ~280 GPa, which is significantly higher than bulk material.