Synthesis and properties of Cr-Al-Si-N films deposited by hybrid coating system with high power impulse magnetron sputtering (HIPIMS) and DC pulse sputtering

The CrN and Cr-Al-Si-N films were deposited on Si wafer and SUS 304 substrates by a hybrid coating system with high power impulse magnetron sputtering (HIPIMS) and a DC pulse sputtering using Cr and AlSi targets under N2/Ar atmosphere.By varying the sputtering current of the AlSi target in the range of 0-2.5 A,both the Al and Si contents in the films increased gradually from 0 to 19.1% and 11.1% (mole fraction),respectively.The influences of the AlSi cathode DC pulse current on the microstructure,phase constituents,mechanical properties,and oxidation behaviors of the Cr-Al-Si-N films were investigated systematically.The results indicate that the as-deposited Cr-Al-Si-N films possess the typical nanocomposite structure,namely the face centered cubic (Cr,Al)N nano-crystallites are embedded in the amorphous Si3N4 matrix.With increasing the Al and Si contents,the hardness of the film first increases from 20.8 GPa for the CrN film to the peak value of 29.4 GPa for the Cr0.23Al0.14Si0.07 N film,and then decreases gradually.In the meanwhile,the Cr0.23Al0.14Si0.07N film also possesses excellent high-temperature oxidation resistance that is much better than that of the CrN film at 900 or 1000 °C.

Influences of working pressure on properties for TiO_2 films deposited by DC pulse magnetron sputtering

TiO2 films were deposited at room temperature by DC pulse magnetron sputtering system.The crystalline structures,morphological features and photocatalytic activity of TiO2 films were systematically investigated by X-ray diffraction（XRD）,atomic force microscopy（AFM） and ultraviolet spectrophotometer,respectively.The results indicated that working pressure was the key deposition parameter in？uencing the TiO2 film phase composition at room temperature,which directly affected its photocatalytic activity.With increasing working pressure,the target self-bias decreases monotonously.Therefore,low temperature TiO2 phase（anatase） could be deposited with high working pressure.The anatase TiO2 films deposited with 1.4 Pa working pressure displayed the highest photocatalytic activity by the decomposition of Methyl Orange solution,which the degradation rate reached the maximum（35%） after irradiation by ultraviolet light for 1 h.

Multifunctional hopeite nanocoating on Ti64 substrates by pulsed laser deposition and radio frequency magnetron sputtering for orthopedic implant applications:A comparative study

Functionalized implants demonstrate an upgraded approach in orthopedic implants,aiming to achieve long term success through improved bio integration.Bioceramic coatings with multifunctionality have arisen as an effective substitute for conventional coatings,owing to their combination of various properties that are essential for bio-implants,such as osteointegration and antibacterial character.In the present study,thin hopeite coatings were produced by Pulsed laser deposition(PLD)and radio frequency magnetron sputtering(RFMS)on Ti64 substrates.The obtained hopeite coatings were annealed at 500°C in ambient air and studied in terms of surface morphology,phase composition,surface roughness,adhesion strength,antibacterial efficacy,apatite forming ability,and surface wettability by scanning electron microscope(SEM),X-ray diffraction(XRD),atomic force microscope(AFM),tensometer,fluorescence-activated cell sorting(FACS),simulated body fluid(SBF)immersion test and contact angle goniometer,respectively.Furthermore,based on promising results obtained in the present work it can be summarized that the new generation multifunctional hopeite coating synthesized by two alternative new process routes of PLD and RFMS on Ti64 substrates,provides effective alternatives to conventional coatings,largely attributed to strong osteointegration and antibacterial character of deposited hopeite coating ensuring the overall stability of metallic orthopedic implants.

Modeling for V–O_2 reactive sputtering process using a pulsed power supply

In this article, we present a time-dependent model that enables us to describe the dynamic behavior of pulsed DC reactive sputtering and predict the film compositions of VOx prepared by this process. In this modeling, the average current J is replaced by a new parameter of Jeff. Meanwhile, the four species states of V, V2O3, VO2, and V2O5 in the vanadium oxide films are taken into consideration. Based on this work, the influences of the oxygen gas supply and the pulsed power parameters including the duty cycle and frequency on film compositions are discussed. The model suggests that the time to reach process equilibrium may vary substantially depending on these parameters. It is also indicated that the compositions of VOx films are quite sensitive to both the reactive gas supply and the duty cycle when the power supply works in pulse mode. The ＇steady-state＇ balance values obtained by these simulations show excellent agreement with the experimental data, which indicates that the experimentally obtained dynamic behavior of the film composition can be explained by this time-dependent modeling for pulsed DC reactive sputtering process. Moreover, the computer simulation results indicate that the curves will essentially yield oscillations around the average value of the film compositions with lower pulse frequency.

Deposition of Aluminium Oxide Films by Pulsed Reactive Sputtering

Pulsed reactive sputtering is a novel process used to deposit some compound films, which are not deposited by traditional D.C. reactive sputtering easily. In this paper some experimental results about the deposition of Al oxide films by pulsed reactive sputtering are presented. The hysteresis phenomenon of the sputtering voltage and deposition rate with the change of oxygen flow during sputtering process are discussed.

Effect of mid-frequency pulse therapy combined with external fixation on bone metabolism, inflammatory response and oxidative stress in patients with osteoporotic distal radial fractures

Objective:To study the effect of mid-frequency pulse therapy combined with external fixation on bone metabolism, inflammatory response and oxidative stress in patients with osteoporotic distal radial fractures.Methods: A total of 72 patients with osteoporotic distal radial fractures who were treated in the hospital between September 2015 and January 2017 were collected and divided into control group (n=36) and observation group (n=36) according to the random number table method. Control group received routine external fixation, and observation group received mid-frequency pulse therapy combined with external fixation. The differences in serum levels of bone metabolism indexes, inflammatory factors and oxidative stress indexes were compared between two groups of patients before and after treatment.Results: Before treatment, differences in serum levels of bone metabolism indexes, inflammatory factors and oxidative stress indexes were not statistically significant between the two groups. After 1 month of treatment, serum BGP, TAC and SOD levels of both groups of patients were higher than those before treatment whileβ-CTX, AKP, TRAP, CRP, IL-1β, IL-6 and MDA levels were lower than those before treatment, and serum BGP, TAC and SOD levels of observation group were higher than those of control group whileβ-CTX, AKP, TRAP, CRP, IL-1β, IL-6 and MDA levels were lower than those of control group.Conclusion: Mid-frequency pulse therapy combined with external fixation can promote fracture healing and reduce postoperative inflammatory response and oxidative stress response in patients with osteoporotic distal radial fracture.

Preparation of Thin Films by a Bipolar Pulsed-DC Magnetron Sputtering System Using Ca₃Co₄O₉and CaMnO₃Targets

The thin films were deposited on the glass substrates by an asymmetric bipolar pulsed-dc magnetron sputtering system using the Ca3Co4O9 and CaMnO3 Targets (n-type) targets of 60 mm diameter and 2.5 mm thickness. The targets were prepared from powder precursors, which obtained by a solid state reaction. Optical emissions from plasmas during sputter depositions of films were detected using a high resolution spectrometer. Thickness of thin film was estimated by Tolansky’s Fizeau fringe method and ellipsometic measurement. Crystal structures were studied from X-ray diffraction. The thermoelectric properties were assessed from Seebeck coefficient and electrical resistivity measurements at room temperature. The power factors were calculated. It was found that the optical emission spectrums showed that the Ca, Mn, Co and O atoms were sputtered from the targets onto glass substrates. As-deposited Ca-Co-O and Ca-Mn-O films thickness values were 0.435 ?m and 0.449 ?m, respectively. The X-ray diffraction patterns clearly showed amorphous nature of the as-deposited films. Determining thermoelectric properties of Ca-Co-O film gave Seebeck coefficient of 0.146 mV/K, electrical resistivity of 0.473Ω.cm, and power factor of 4.531 μW/m?K at room temperature. Ca-Mn-O film baring a high resistance was not the experimental determination of thermoelectric properties.

Effect of sputtering conditions on growth and properties of ZnO :Al films

Al-doped zinc oxide（AZO） films were deposited on glass substrates by mid-frequency magnetron sputtering. The effects of substrate rotation speed and target-substrate distance on the electrical, optical properties and microstructure and crystal structures of the resulting films were investigated by scanning electron microscopy（SEM）, atomic force microscopy（AFM）, X-ray diffraction（XRD）, spectrophotometer and Hall-effect measurement system, respectively. XRD results show that all AZO films exhibit a strong preferred c-axis orientation. However, the crystallinity of films decreases with the increase of substrate rotation speed, accompanying with the unbalanced grains grows. For the films prepared at different target-substrate distances, the uniform microstructure and morphology are observed. The highest carrier concentration of 5.9×1020 cm-3 and Hall mobility of 13.1 cm^2/（V·s） are obtained at substrate rotation speed of 0 and target-substrate distance of 7 cm. The results indicate that the structure and performances of the AZO films are strongly affected by substrate rotation speed.

Effect of harmonic magnetic field and pulse magnetic field on microstructure of high purity Cu during electromagnetic direct chill casting

The effects of two types of magnetic fields,namely harmonic magnetic field(HMF)and pulse magnetic field(PMF)on magnetic flux density,Lorentz force,temperature field,and microstructure of high purity Cu were studied by numerical simulation and experiment during electromagnetic direct chill casting.The magnetic field is induced by a magnetic generation system including an electromagnetic control system and a cylindrical crystallizer of 300 mm in diameter equipped with excitation coils.A comprehensive mathematical model for high purity Cu electromagnetic casting was established in finite element method.The distributions of magnetic flux density and Lorentz force generated by the two magnetic fields were acquired by simulation and experimental measurement.The microstructure of billets produced by HMF and PMF casting was compared.Results show that the magnetic flux density and penetrability of PMF are significantly higher than those of HMF,due to its faster variation in transient current and higher peak value of magnetic flux density.In addition,PMF drives a stronger Lorentz force and deeper penetration depth than HMF does,because HMF creates higher eddy current and reverse electromagnetic field which weakens the original electromagnetic field.The microstructure of a billet by HMF is composed of columnar structure regions and central fine grain regions.By contrast,the billet by PMF has a uniform microstructure which is characterized by ultra-refined and uniform grains because PMF drives a strong dual convection,which increases the uniformity of the temperature field,enhances the impact of the liquid flow on the edge of the liquid pool and reduces the curvature radius of liquid pool.Eventually,PMF shows a good prospect for industrialization.

Recent Developments in Magnetron Sputtering

The principle of magnetron sputtering is introduced andthe balanced and unbalanced magnetrons are compared andthe necessity of unbalanced magnetrons is explained as well. Several recent developments in plasma magnetron sputtering, i.e., unbalanced magnetron sputtering, pulsed magnetron sputtering and ion assisted sputtering, are discussed. The recent developments of unbalanced magnetron systems and their incorporation with ion sources result in an understanding in growingimportance of the magnetron sputtering technology, which makes the technology an applicable deposition process for a variety of important films, such as wear-resistant films and decorative films.

Effect of flash thermal annealing by pulsed current on rotational anisotropy in exchange-biased NiFe/FeMn film

In this paper, Ta/[NiFe（15 nm）/FeMn（10 nm）]/Ta exchange-biased bilayers are fabricated by magnetron sputtering, and their static and dynamic magnetic properties before and after rapid annealing treatment with pulsed current are charac- terized by using a vibrating sample magnetometer （VSM） and a vector network analyzer （VNA）, respectively. The exchange bias field He and static anisotropy field Hksta decrease from 118.45 Oe （10e = 79.5775 A.m-1） and 126.84 Oe at 0 V to 94.75 Oe and 102.31 Oe at 90 V, respectively, with increasing capacitor voltage, which supplies pulsed current to heat the sample. The effect of flash thermal annealing by pulsed current on the rotational anisotropy （Hrot）, the difference value between static and dynamic magnetic anisotropy, is investigated particularly. The highest Hrot is obtained in the sample annealing with 45-V capacitor （3300 μF） voltage. According to the anisotropic magnetoresistance measurements, it can be explained by the fact that the temperature of the sample is around the blocking temperature of the exchange bias system （Tb） at 45 V, the critical temperature where the formation of more unstable antiferromagnetic grains occurs.

Study of the Thin Film Pulse Transformer

A new thin film pulse transformer for using in ISND and model systems is fabricated by a mask sputtering process. This novel pulse transformer consists of four I-shaped CoZrRe nanometer crystal magnetic-film cores and a Cu thin film coil, deposited on the micro-crystal glass substrate directly. The thickness of thin film core is between 1 and 3 μm, and the area is between 4mm×6 mm and 12mm×6 mm. The coils provide a relatively high induce of 0.8 μm and can be well operated in a frequency range of 0.001~20 MHz.

ZnO:Al Films Prepared by Reactive Mid-frequency Magnetron Sputtering with Rotating Cathode

Al-doped zinc oxide （ZnO：Al,AZO） films were deposited on glass substrates using a reactive mid-frequency （MF） magnetron sputtering process with rotating cathodes.The influence of deposition parameters on structural,electrical and optical properties of AZO films is investigated.It is observed that the rotating magnetron targets exhibited a sputtered metallic surface over a wider range,and there is no re-deposition zone between the racetracks.The films deposited at static deposition mode demonstrate more homogenous in thickness and resistivity across the target surface compared with conventional rectangular targets.The films deposited under the proper conditions show a regular cone-shaped grain surface and densely packed columnar structure.The minimum resistivity of 3.16×10-4 ·cm was obtained for the film prepared at substrate temperature of 150 C,gas pressure of 640 MPa and oxygen partial pressure of 34 MPa.

High energy soliton pulse generation by a magnetron-sputtering-deposition-grown MoTe_2 saturable absorber

The pulse energy in the ultrafast soliton fiber laser oscillators is usually limited by the well-known wave-breaking phenomenon owing to the absence era desirable real saturable absorber （SA） with high power tolerance and large modulation depth. Here, we report a type of microfiber-based MoTe2 SA fabricated by the magnetron-sputtering deposition （MSD） method. High-energy wave-breaking free soliton pulses were generated with pulse duration/pulse energy/average output power of 229 fs/2.14 nJ/57 mW in the 1.5 μm regime and 1.3 ps/13.8 nJ/ 212 mW in the 2 μm regime, respectively. To our knowledge, the generated soliton pulses at 1.5μm had the shortest pulse duration and the highest output power among the reported erbium-doped fiber lasers mode locked by transition metal dichalcogenides. Moreover, this was the first demonstration of a MoTe2-based SA in fiber lasers in the 2 ltm regime, and the pulse energy/output power are the highest in the reported thulium-doped fiber lasers mode locked by two-dlmensional materials. Our results suggest that a microfiber-based MoTe2 SA could be used as an excellent photonic device for ultrafast pulse generation, and the MSD technique opens a promising route to produce a high-performance SA with high power tolerance and large modulation depth, which are beneficial for high-energy wave-breaking free pulse generation.

Microstructure and Properties of the Cr–Si–N Coatings Deposited by Combining High-Power Impulse Magnetron Sputtering(HiPIMS) and Pulsed DC Magnetron Sputtering

The Cr–Si–N coatings were prepared by combining system of high-power impulse magnetron sputtering and pulsed DC magnetron sputtering. The Si content in the coating was adjusted by changing the sputtering power of the Si target.By virtue of electron-probe microanalysis, X-ray diffraction analysis and scanning electron microscopy, the influence of the Si content on the coating composition, phase constituents, deposition rate, surface morphology and microstructure was investigated systematically. In addition, the change rules of micro-hardness, internal stress, adhesion, friction coefficient and wear rate with increasing Si content were also obtained. In this work, the precipitation of silicon in the coating was found.With increasing Si content, the coating microstructure gradually evolved from continuous columnar to discontinuous columnar and quasi-equiaxed crystals; accordingly, the coating inner stress first declined sharply and then kept almost constant. Both the coating hardness and the friction coefficient have the same change tendency with the increase of the Si content, namely increasing at first and then decreasing. The Cr–Si–N coating presented the highest hardness and average friction coefficient for an Si content of about 9.7 at.%, but the wear resistance decreased slightly due to the high brittleness.The above phenomenon was attributed to a microstructural evolution of the Cr–Si–N coatings induced by the silicon addition.

带有反向正脉冲的HiPIMS技术制备ta-C膜及性能研究

目的提高切削刀具和耐磨零件的表面硬度和摩擦性能,延长工具的使用寿命。方法基于高功率脉冲磁控溅射技术(HiPIMS),在每个脉冲周期尾部施加反向正脉冲,控制ta-C沉积过程,通过电镜测试、拉曼测试、XPS测试、纳米压痕硬度测试、摩擦磨损实验分别分析脉冲频率、反向正脉冲能量对ta-C薄膜沉积速度、膜结构、硬度、结合强度、耐磨性能的影响。结果采用钨钢为基体进行实验,将频率从4000 Hz到1500 Hz依次降低,制备涂层。在频率为4000 Hz的处理条件下制备涂层时,ta-C膜层的厚度为479.2 nm,通过XPS可知,此时sp^(3)的原子数分数达到59.53%,硬度为32.65 GPa,且得到的薄膜在12.7 N时失效,耐磨性较差,摩擦因数约为0.163。在频率为1500 Hz的处理条件下制备涂层时,涂层各项性能均有所提升,ta-C膜层的厚度为488.6 nm,通过XPS可知,此时sp^(3)的原子数分数达到63.74%,硬度为40.485 GPa,且薄膜在14.9 N时失效,耐磨性较优,摩擦因数约为0.138。结论通过调节脉冲频率,可以有效提高ta-C薄膜的沉积效率,改善膜的结构和性能。随着沉积ta-C薄膜频率的降低,薄膜中sp^(3)的含量呈现增大趋势,摩擦因数也随之降低,有效改善了ta-C膜的耐磨性。

Effect of Pulse Width and Frequency of Bias DC Voltage on the Microstructure of Pure Cr Coatings by Magnetron Sputter Ion Plating

Pure Cr coatings were deposited onto the pieces of silicon wafer at different pulse width and frequency of bias voltage by magnetron sputter ion plating.The microstructure and preferential orientation of pure Cr coatings were analyzed by SEM and XRD respectively.Results show that the diffusion ability of atoms on the coating surface was improved due to the substrate temperature rise effect caused by the ion bombardment with the pulse width increased.However,the effect of frequency of bias DC voltage on the microstructure of pure Cr coatings was particularly significant.The bombardment ions action on the coating surface were more uniformly and more dispersed compared with the nucleation rate of Cr atoms and the density of pure Cr coatings both improved with the frequency increased are the main reasons that the microstructure of pure Cr coatings changed from dense,granular columnar grain outcrops to uniformity,small nano-crystalline particles.

Phase structure of sputtered Ta coating and its ablation behavior by laser pulse heating(LPH)

Phase structure of sputtered Ta coating in the negative glow space and LPH effect were explored.The whole coating/substrate system is substrate→physically gas-absorbed Fe surface→oxygen-enriched TaOx layer→amorphous Ta→αandβdual phase→singleαphase.After LPH course,micro structure of Ta coating shows intact,only a few cracks emerge after 100 laser pulses,exhibiting thin HAZ but thick Fe/Ta ICZ,without martensitic transformation.For the electrodeposited Cr coating,continuous thermal stresses produce many extra micro-crack,substrate oxidation and martensitic transformation,leading to crack propagations and final bulk delamination,without any ICZ.