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1.
As a variation of high power pulsed magnetron sputtering technique, modulated pulse power (MPP) magnetron sputtering can achieve a high deposition rate while at the same time achieving a high degree of ionization of the sputtered material with low ion energies. These advantages of the MPP technique can be utilized to obtain dense coatings with a small incorporation of the residual stress and defect density for the thick coating growth. In this study, the MPP technique has been utilized to reactively deposit thick Cr2N and CrN coatings (up to 55 μm) on AISI 440C steel and cemented carbide substrates in a closed field unbalanced magnetron sputtering system. High deposition rates of 15 and 10 μm per hour have been measured for the Cr2N and CrN coating depositions, respectively, using a 3 kW average target power (16.7 W/cm2 average target power density), a 50 mm substrate to target distance and an Ar/N2 gas flow ratio of 3:1 and 1:1. The CrN coatings showed a denser microstructure than the Cr2N coatings, whereas the Cr2N coatings exhibited a smaller grain size and surface roughness than those of the CrN coatings for the same coating thickness. The compressive residual stresses in the CrN and Cr2N coatings increased as the coating thickness increased to 30 μm and 20 μm, respectively, but for thicker coatings, the stress gradually decreased as the coating thickness increased. The CrN coatings exhibited an increase in the scratch test critical load as the thickness was increased. Both CrN and Cr2N coatings showed a decrease in the hardness and an increase in the sliding coefficient of friction as the coating thickness increased from 2.5 to 55 μm. However, the wear rate of the CrN coatings decreased significantly as the coating thickness was increased to 10 μm or higher. The 10-55 μm CrN coating exhibited low wear rates in the range of 3.5-5 × 10−7 mm3 N−1 m−1. To the contrary, the Cr2N coating exhibited relatively low wear resistance in that high wear rates in the range of 3.5 to 7.5 × 10−6 mm3 N−1 m−1 were observed for different thicknesses.  相似文献   

2.
NiCrAlY bond-coat was coated on Inconel 718 substrate by air plasma spraying (APS) followed by APS ZrO2-8 wt.%Y2O3 as top-coat. Using CO2 laser of different energy densities, ceramic top-coat surface was remelted. Laser remelting with high energy density (4 J/mm2) produced a dense microstructure over the whole thickness of top-coat, while low energy density (0.67 J/mm2) laser remelting produced a ~ 50 μm thick dense layer on the top-coat surface. It was found that the volume fraction of monoclinic phase decreased from 9% in as-sprayed coating to 4% and 3% after laser remelting with high and low energy density respectively. After isothermal oxidation at 1200 °C for 200 h, the thickness of oxide layer (TGO) in the sample produced by low energy density laser remelting was ~ 5.6 μm, which was thinner than that of oxide layer in as-sprayed (~ 7.6 μm) and high energy density laser remelted (~ 7.5 μm) samples. A uniform and continuous oxide layer was found to develop on the bond-coat surface after low energy density laser remelting. Thicker oxide layer containing Cr2O3, NiO and spinel oxides was observed in both as-sprayed and high energy density laser remelted coatings. After cyclic oxidation at 1200 °C for 240 h, the weight gain per unit area of as-sprayed coating was similar to that of high energy density laser remelted coating while a significantly smaller weight gain was found in low energy density laser remelted coating.  相似文献   

3.
The pore structure in nano-porous TiO2 coatings influences the ion diffusion property and the photovoltaic performance of dye-sensitized solar cells. In this paper, TiO2 coatings were deposited by vacuum cold spray (VCS) using a strengthened nanostructured powder. The pore structure, ion diffusion, and dye infiltration properties were examined to understand the coating deposition mechanism. Results showed that the pores in the VCS TiO2 coatings presented a bimodal size distribution with two peaks at ~15 and ~50?nm. Based on the impact behavior of spray powder particles, a deposition model was proposed to explain the formation mechanism of the pores in the VCS coating using strengthened nanostructured powder. It was found that, compared to the conventional unimodal-sized nano-pores in TiO2 coatings, the bimodal-sized nano-pores contributed to a higher ion diffusion coefficient of the coatings and thereby a higher photovoltage of the solar cells.  相似文献   

4.
Seven different Al2O3-based suspensions were prepared by dispersing two nano-sized Al2O3 powders (having analogous size distribution and chemical composition but different surface chemistry), one micron-sized powder and their mixtures in a water + isopropanol solution. High velocity suspension flame sprayed (HVSFS) coatings were deposited using these suspensions as feedstock and adopting two different sets of spray parameters.The characteristics of the suspension, particularly its agglomeration behaviour, have a significant influence on the coating deposition mechanism and, hence, on its properties (microstructure, hardness, elastic modulus). Dense and very smooth (Ra ~ 1.3 μm) coatings, consisting of well-flattened lamellae having a homogeneous size distribution, are obtained when micron-sized (~ 1-2 μm) powders with low tendency to agglomeration are employed. Spray parameters favouring the break-up of the few agglomerates present in the suspension enhance the deposition efficiency (up to > 50%), as no particle or agglomerate larger than ~ 2.5 μm can be fully melted. Nano-sized powders, by contrast, generally form stronger agglomerates, which cannot be significantly disrupted by adjusting the spray parameters. If the chosen nanopowder forms small agglomerates (up to a few microns), the deposition efficiency is satisfactory and the coating porosity is limited, although the lamellae generally have a wider size distribution, so that roughness is somewhat higher. If the nanopowder forms large agglomerates (on account of its surface chemistry), poor deposition efficiencies and porous layers are obtained.Although suspensions containing the pure micron-sized powder produce the densest coatings, the highest deposition efficiency (~ 70%) is obtained by suitable mixtures of micron- and nano-sized powders, on account of synergistic effects.  相似文献   

5.
This study reported a novel treatment to improve the corrosion resistance of TiB2/A356 composites. The method was employed in combination of the molten-salt electrodeposition and subsequent electrochemical anodization technique. By means of molten-salt electrodeposition, the Al coatings were deposited on the surface of TiB2/A356 composites. It was found that the morphology of the Al coatings is closely related to the current density. Thus, under the suitable condition, a dense and uniform Al coating can be obtained, with the crystal size in the range of 0.5–2 μm and the coating thickness of ~ 9 μm. This continuous Al layer can eliminate the adverse corrosion contribution of TiB2 particles in Al matrix. The following step of anodization was designed to convert the Al film to an anodized Al oxide film for further corrosion protection. The electrochemical corrosion behavior was evaluated by potentiodynamic polarization curves and electrochemical impedance spectroscopy. These results showed the corrosion resistance was greatly enhanced in TiB2/A356 composites with an anodized Al-coating than that of the anodized composites. It is evident that the new treatment of metal electrodeposition in molten salts and following anodization is an effective method of anti-corrosion in composites.  相似文献   

6.
The direct coating of a nano-porous alumina layer on the inner surface of micro-porous alumina tubes was performed by electrophoretic deposition (EPD). A thin layer of polypyrrole (Ppy) was synthesized on the inside wall of the porous tubes by the chemical polymerization of pyrrole (Py) to give the wall electric conduction for the EPD electrode. The bimodal suspension of alumina powders with 0.6 μm and 30 nm average particle sizes was selected to control the nano-porous structure. The thickness of the coating layer was controlled by altering the applied voltage and deposition time. The interfacial connection of the coated layer and the substrate was observed by SEM before and after sintering. The pore size of the coated layer was characterized by its pore size distribution.  相似文献   

7.
In part I of this study, the dip-coat processing of mullite/gadolinium silicate (Gd2SiO5) environmental barrier coatings (EBCs) applied on α-SiC and SN282™ Si3N4 through alcohol based and sol based slurries was presented. Here, the performance of selected EBCs by evaluating their oxidation resistances during thermal cycling in simulated combustion (90% H2O-balance O2) environment between 1350 °C and RT for up to 400 cycles is being reported. Oxidation of un-coated α-SiC was severe, leading to aligned and layered porous silica scale formation (~ 17 μm thick) on its surface with frequent scale spallation when exposed to 100 cycles. Mullite/Gd2SiO5/B2O3 (83.5/11.5/5 wt.%) EBCs remained adherent to α-SiC substrate with an underlying porous silica layer formed at substrate/coating interface, which was ~ 12 μm after 100 cycles, ~ 16 μm after 200 cycles, and ~ 25 μm after 400 cycles. In contrast, α-SiC substrate coated with mullite/Gd2SiO5 (88/12 wt.%) EBC had only limited oxidation of ~ 10 μm even after 1350 °C/400 cycles. The sol based mullite/Gd2SiO5 (88/12 wt.%) EBC on α-SiC substrate after 400 cycles was adherent, but showed more interfacial damages (~ 20 μm after 400 cycles) though it had increased coating density. However, the mullite/Gd2SiO5 (88/12 wt.%) EBC (alcohol based) delaminated from the SN282™ Si3N4 substrate after 1350 °C/100 cycles, because of the formation of interconnected interfacial voids and hairline cracks. Parabolic growth kinetics for the underlying silica was observed for both the alcohol and sol based coated samples.  相似文献   

8.
In the present study, bioactive coatings enriched with micro-pores and Ca-P-Sr elements were formed on pore walls of porous titanium by micro-arc oxidation (MAO). It is found that pore size plays a significant role on the MAO treatment of porous titanium. For samples with pore size smaller than 90 μm, whatever applied voltage and treatment time were employed, MAO coatings were formed only in the near surface region. As to the sample with average pore size of 150 μm, MAO coatings were formed on both outer and inner pore walls throughout the depth. Compared with the untreated one, the specific surface area dramatically increased about 460 times. Further studies found that pore size, thickness and amounts of O, Ca, P and Sr elements of the coating on the outer pore walls were obviously higher than those on the inner pore walls. Additionally, the coating on the outer pore walls was composed of anatase and rutile TiO2 and other complex Ca-P-Sr phases, in comparison with anatase TiO2 formed on the inner pore walls. In spite of the distinct features of coatings on the different locations of pore walls, MAO-treated porous titanium overall showed a good apatite-inducing ability.  相似文献   

9.
Vacuum plasma spraying (VPS) was used to spray a Cr3C2-NiCr coating of ∼ 150, 300 and 450 μm in thickness onto a plain carbon steel substrate, employing a commercially available Cr20Ni9.5C powder. The splat microstructures observed in the coating were found to consist of a NiCr matrix with a predominant Cr3C2 phase, besides Cr7C3 and Cr2O3. The adhesion of the coating to the substrate was evaluated by means of interfacial indentation techniques. It has been found that the interfacial toughness value changes from 7.6 to 10.1 MPa m1/2 when the thickness increases from 150 to 450 μm. Also, it has been found that the parameter Kcao, determined by linear regression from the Kca versus 1 / e2 curve by means of the interfacial indentation model advanced by Chicot et al., has a value of ∼ 9.8 MPa m1/2.  相似文献   

10.
TZM alloy is a potential candidate for high temperature structural applications. However, in the preparation of this alloy by conventional melt-casting route, difficulties are encountered in achieving homogenized alloy composition in view of high melting temperature of the alloy and presence of minor alloying components. Therefore, an alternative technique of aluminothermic co-reduction was adopted to prepare TZM alloy of composition, Mo-0.5Ti-0.1Zr-0.02 °C, wt.% by simultaneous reduction of uniformly premixed oxides of MoO2, TiO2 and ZrO2 by aluminium in presence of requisite amount of carbon. The as-reduced alloy was further arc melted for consolidation. Since, TZM alloy is by nature highly susceptible to oxidation at elevated temperature in air or oxygen, therefore feasibility of development of silicide type of coating over the synthesized alloy by plasma coating technique was also examined. Silicon powder coated on TZM alloy surface by plasma spray technique was finally converted into MoSi2 coating by sintering at 1350 °C for 2-4 h duration under argon. A double layer coating structure was formed with two distinct phases. The inner thin layer was consisted of Mo2Si5 phase (~ 10 μm) followed by thick outer layer of MoSi2 (~ 150 μm). The coating showed good adhesion strength and stable oxidation with negligible mass gain (10 g/m2) at 1000 °C in air.  相似文献   

11.
Since carbon coating can effectively improve electrical wiring of Li4Ti5O12 and thus enhance its high rate performance, a novel and simple citric acid sol-gel method for in situ carbon coating is employed in this study. The effects of the amount of the carbon source in the starting xerogel on the particle size, the resistance and the electrochemical performance of the synthesized Li4Ti5O12 samples are systematically studied. The physical and electrochemical properties of the obtained samples have been characterized by XRD, TG-DSC, SEM, TEM, BET, A.C. impedance, galvanostatically charge-discharge and cyclic voltammetry tests. The results show that the initial amount of the carbon source in the starting xerogel is a critical factor which determines the content of the coated carbon and the pore volume, therefore governs the high rate performance of the Li4Ti5O12/C composites. The Li4Ti5O12/C composite with in situ carbon coating of 3.5 wt% exhibits the best electrochemical performance which delivers delithiation capacities of 143.6 and 133.5 mAh g−1 with fairly stable cycling performance even after 50 cycles at 0.5C and 1C rate, respectively.  相似文献   

12.
Nanostructured TiN/CNx multilayer films were deposited onto Si (100) wafers and M42 high-speed-steel substrates using closed-filed unbalanced magnetron sputtering in which the deposition process was controlled by a closed loop optical emission monitor (OEM) to regulate the flow of N2 gas. Multilayers with different carbon nitride (CNx) layer thickness could be attained by varying the C target current (0.5 A to 2.0 A) during the deposition. It was found that the different bilayer thickness periods (i.e. the TiN layer thickness ΛTiN was fixed at 3.0 nm while the CNx layer thickness ΛCNx was varied from 0.3 to 1.2 nm) significantly affected the mechanical and tribological properties of TiN/CNx multilayer films. These multilayer films were characterized and analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), atomic force microscopy (AFM), Rockwell-C adhesion test, scratch test, pin-on-disc tribometer, and nanoindentation measurements. XPS analyses revealed that the chemical states, such as TiN, TiC, TiNxOy and TiO2, existed in a TiN layer. Nanoindentation results showed that the hardness was highly dependent on the bilayer thickness. A maximum hardness of ~ 41.0 GPa was observed in a multilayer film at bilayer thickness ΛTiN = 3.0 nm and ΛCNx = 0.9 nm. All multilayer films exhibited extreme elasticity with elastic recoveries as high as 80% at 5 mN maximum load. The compressive stresses in the films (in a range of 1.5-3.0 GPa) were strongly related to their microstructure, which depended mainly on the incorporation of nitrogen in the films. By scratch and Rockwell-C adhesion tests, the multilayer films with smaller bilayer thicknesses (ΛTiN = 3.0 nm, ΛCNx = 0.3 and 0.6 nm) exhibited the best adhesion and cohesive strength. The critical load value obtained was as high as ~ 78 N for the films with ΛTiN = 3.0 nm, ΛCNx = 0.9 nm. The friction coefficient value for a multilayer at ΛTiN = 3.0 nm and ΛCNx = 0.9 nm was found to be low 0.11. These adhesive properties and wear performance are also discussed on the basis of microstructure, mechanical properties and tribochemical wear mechanisms.  相似文献   

13.
Sr2CeO4 blue phosphor has been prepared by the solid-state reaction method. The X-ray diffraction (XRD) study confirms the structure of the system to be orthorhombic. High resolution electron transmission microscopy reveals that Sr2CeO4 prepared by the solid state reaction method is composed of elongated spherical structures of length ∼0.2-0.6 μm and width ∼90-150 nm. The excitation spectrum shows a broad band which peaks at 275 nm. The emission spectrum shows a broad band which peaks at 467 nm when excited at 275 nm. The emission band is assigned to the energy transfer between the molecular orbital of the ligand and charge transfer (CT) state of the Ce4+ ion. The Commission International de l’Eclairage (CIE) co-ordinates are x = 0.15, and y = 0.23. The nonlinear absorption behavior of Sr2CeO4 has been investigated using the open aperture z-scan technique. The calculated effective two-photon absorption coefficient shows that the Sr2CeO4 blue phosphor is a promising optical limiting material.  相似文献   

14.
CrN-Ag composite coatings, 2 and 5 μm thick and containing 22 at.% Ag solid lubricant, were grown on Si(001) and 440C stainless steel substrates by reactive co-sputtering at Ts = 500 °C, and were covered with 200 nm thick pure CrN diffusion barrier cap layers. Annealing experiments at Ta = 625 °C, followed by quantitative scanning electron microscopy, energy dispersive x-ray spectroscopy, and Auger depth profile analyses indicate considerable Ag transport to the top surface for a barrier layer deposited at a substrate floating potential of −30 V, but negligible Ag diffusion when deposited with a substrate bias potential of −150 V. This is attributed to ion-irradiation induced densification which makes the cap layer an effective diffusion barrier. High temperature tribological sliding tests of this coating system against alumina balls at Tt = 550 °C indicate an initial friction coefficient μ = 0.43 ± 0.04 which decreases monotonically to 0.23 ± 0.03. This is attributed to the development of wear mediated openings in the barrier layer which allow Ag lubricant to diffuse to the sliding top surface. In contrast, pure CrN exhibits a constant μ = 0.41 ± 0.02 while CrN-Ag composite coatings without cap layer show a low transient μ = 0.16 ± 0.03, attributed to Ag transport to the surface, that however increases to μ = 0.39 ± 0.04 after ~ 6000 cycles as the Ag reservoir in the coating is depleted. That is, the dense CrN cap layer reduces the Ag lubricant flow rate and therefore prolongs the time when the coating provides effective lubrication. This results in a cumulative wear rate over 10,000 cycles of 3.1 × 10−6 mm3/Nm, which is 3.3 × lower than without diffusion barrier layer.  相似文献   

15.
We studied surface modification of a double layer protective coating on steel induced by single fs laser pulse irradiation in ambient air. The outer alumina (Al2O3) layer, which protects against aggressive environments, was 1.7 μm thick and the titanium aluminum nitride (TiAlN) layer in contact with the steel surface had a thickness of 1.9 μm. The pulses (λ = 775 nm, τ = 200 fs) were generated by a Ti:sapphire laser source. The pulse energy was varied from 0.32 μJ to 50 μJ, corresponding to an incident laser fluence of 0.11 J cm− 2 to 16.47 J cm− 2. The surface damage threshold was found to be 0.20 J cm− 2 and the alumina layer removal was initiated at 0.56 J cm− 2. This selective ablation of alumina was possible in a wide range of fluences, up to the maximum applied, without ablating the TiAlN layer beneath.  相似文献   

16.
The film perfection in terms of pinhole defect densities of ultra-thin Al2O3 grown by atomic layer deposition (ALD) has been quantitatively characterized. A significant defect density reduction from ~ 1.2 × 105/cm2 to ~ 90/cm2 was demonstrated for 2 nm-thick Al2O3 by using an ALD tungsten (W) buffer layer on the nickel (Ni) substrate. The reason for the defect reduction was attributed to efficient nucleation of ALD Al2O3 on ALD W. The effect of the buffer layer becomes less essential as the Al2O3 thickness increases, where the substrate surface physical conditions such as particle contamination become the main cause for defects.  相似文献   

17.
TiO2 thin films were deposited on silicon wafer substrates by low-field (1 < B < 5 mT) helicon plasma assisted reactive sputtering in a mixture of pure argon and oxygen. The influence of the positive ion density on the substrate and the post-annealing treatment on the films density, refractive index, chemical composition and crystalline structure was analysed by reflectometry, Rutherford backscattering spectroscopy (RBS) and X-ray diffraction (XRD). Amorphous TiO2 was obtained for ion density on the substrate below 7 × 1016 m− 3. Increasing the ion density over 7 × 1016 m− 3 led to the formation of nanocrystalline (~ 15 nm) rutile phase TiO2. The post-annealing treatment of the films in air at 300 °C induced the complete crystallisation of the amorphous films to nanocrystals of anatase (~ 40 nm) while the rutile films shows no significant change meaning that they were already fully crystallised by the plasma process. All these results show an efficient process by low-field helicon plasma sputtering process to fabricate stoichiometric TiO2 thin films with amorphous or nanocrystalline rutile structure directly from low temperature plasma processing conditions and nanocrystalline anatase structure with a moderate annealing treatment.  相似文献   

18.
MoSi2 - 0, 15.3, 22, and 29.3 at.% Al coatings were prepared on the nickel-based super-alloy substrates by electro-thermal explosion ultrahigh speed spraying technology. The analysis showed that the coatings had fine microstructure with grain sizes ranging from 0.5 to 2 μm. The bonding between coating and substrate was typically metallurgical cohesion. The oxidation resistance of the coating was further studied at 1100 °C in air. Al alloyed in MoSi2 coatings increased the oxidation resistance of the coatings, and the oxidation resistance of MoSi2-15.3 at.% Al coating was higher than the other two MoSi2–Al coatings. This suggested the oxidation resistance might have close relations to the obtained grain size.  相似文献   

19.
Aluminum coating was plasma sprayed on Fe-0.14-0.22 wt.% C steel substrate, and heat diffusion treatment at 923 °C for 4 h was preformed to the aluminum coating to form Fe2Al5 inter-metallic compound coating. The corrosion mechanism of the Fe2Al5 coating in molten zinc was investigated. SEM and EDS analysis results show that the corrosion process of the Fe2Al5 layer in molten zinc is as follows: Fe2Al5 → Fe2Al5Znx (η) → η + L(liquid phase) → L + η + δ(FeZn7) → L + δ → L. The η phase and the eutectic structure (η + δ) prevent the diffusion of zinc atoms efficiently. Therefore the Fe2Al5 coating delays the reaction between the substrate and molten zinc, promoting the corrosion resistance of the substrate.  相似文献   

20.
In this work, CeO2/stannate multilayer coatings on AZ91D magnesium alloy were successfully obtained by chemical conversion and sol–gel dip coating. The stannate conversion coatings were prepared from a stannate aqueous bath containing Na2SnO3, CH3COONa, Na3PO4 and NaOH at different temperatures and immersion times. Ceria films were produced on stannate/AZ91D starting from Ce(III) nitrate solutions in H2O. In some cases, the PVA was added as chelating agent. Ceria top coatings were fired at 200 °C for 1 h. Coating microstructure was examined by FE-SEM. Finally, the corrosion resistance features of the coatings were tested by the electrochemical impedance spectroscopy (EIS) in 3 wt.% NaCl solution. The effect of PVA addition was evaluated in terms of microstructure and corrosion resistance features. CeO2/stannate multilayer films, 3 μm thick, uniform, well adherent and nearly crack free were obtained. The formation of CeO2 phase was confirmed by XRD and XPS analyses. The XPS depth profiles showed a limited diffusion of Mg towards the ceramic film. The EIS tests showed a significant improvement of corrosion resistance of the multilayer coatings (~ 16.6 kΩ after 48 h in NaCl solution) with respect to the blank alloy (~ 2.4 kΩ after 48 h in NaCl solution).  相似文献   

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