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1.
《Ceramics International》2019,45(14):17363-17375
TiWSixN films were deposited using a magnetron co-sputtering system on silicon (111), 316L stainless steel, and M2 high-speed steel substrates. The silicon target current density was varied from 0 mA/cm2 to 4.32 mA/cm2 in order to modify the Si content in the films. The microstructure and chemical composition were determined by means of X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), respectively. The surface of the films was explored via scanning electron microscopy (SEM) and atomic force microscopy (AFM). Mechanical, tribological, and thermal properties were investigated by means of the nanoindentation, ball-on-disc, and cyclic oxidation tests, respectively. Our results indicated that as the silicon target current density was increased, the microstructure changed from crystalline to amorphous, and the hardness and elastic modulus improved from initial values of 7.5 ± 0.3 GPa and 181 ± 8 GPa to 15 ± 1 GPa and 229 ± 9 GPa, respectively. Furthermore, films deposited at high silicon target current exhibited better resistance to thermal oxidation. The failure mechanism of the WTiSixN thin films under cyclic oxidation was attributed to the microstructure of the films, WO3 sublimation, and the thermal coefficient mismatch between the film and the substrate.  相似文献   

2.
The recently developed method of nanoindentation is applied to various forms of carbon materials with different mechanical properties, namely diamond, graphite and fullerite films. A diamond indenter was used and its actual shape determined by scanning force microscopy with a calibration grid. Nanoindentation performed on different surfaces of synthetic diamond turned out to be completely elastic with no plastic contributions. From the slope of the force–depth curve the Young's modulus as well as the hardness were obtained reflecting a very large hardness of 95 GPa and 117 GPa for the {100} and {111} crystal surfaces, respectively. Investigation of a layered material such as highly oriented pyrolytic graphite again showed elastic deformation for small indentation depths but as the load increased, the induced stress became sufficient to break the layers after which again an elastic deformation occurred. The Young’s modulus was calculated to be 10.5 GPa for indentation in a direction perpendicular to the layers. Plastic deformation of a thin fullerite film during the indentation process takes place in the softer material of a molecular crystalline solid formed by C60 molecules. The hardness values of 0.24 GPa and 0.21 GPa for these films grown by layer epitaxy and island growth on mica and glass, respectively, vary with the morphology of the C60 films. In addition to the experimental work, molecular dynamics simulations of the indentation process have been performed to see how the tip–crystal interaction turns into an elastic deformation of atomic layers, the creation of defects and nanocracks. The simulations are performed for both graphite and diamond but, because of computing power limitations, for indentation depths an order of magnitude smaller than the experiment and over indentation times several orders of magnitude smaller. The simulations capture the main experimental features of the nanoindentation process showing the elastic deformation that takes place in both materials. However, if the speed of indentation is increased, the simulations indicate that permanent displacements of atoms are possible and permanent deformation of the material takes place.  相似文献   

3.
C60 fullerene clusters are used as a carbon source for amorphous carbon films deposition in an electron beam excited plasma. C60 clusters are sublimated by heating a ceramic crucible containing the C60 powders up to 850 °C, which is located in a highly vacuumed process chamber. The sublimated fullerene powders are injected to the electron beam excited argon plasma and dissociated to be active species that are propelled toward the substrates. Consequently, the carbon species condense as a thin film onto the negatively biased substrates that are immersed in the plasma. Deposition rates of approximately 1.0 μm/h and the average surface roughness of 0.2 nm over an area of 400 μm2 are achieved. Decomposition of the C60 fullerene after injecting into the plasma is confirmed by optical emission spectroscopy that shows existence of small carbon species such as C2 in the plasma. X-ray diffraction pattern reveals that the microstructure of the film is amorphous, while fullerene films deposited without the plasma show crystalline structure. Raman spectroscopic analysis shows that the films deposited in the plasma are one of the types of diamond-like carbon films. Different negative bias voltages have been applied to the substrate holder to examine the effect of the bias voltage to the properties of the films. The nano-indentation technique is used for hardness measurement of the films and results in hardness up to about 28 GPa. In addition, the films are droplet-free and show superior lubricity.  相似文献   

4.
A systematic study of boron trioxide under high pressure and high temperature (HPHT) was conducted using a Chinese multi-anvil high-pressure apparatus (CHPA). The HPHT phase diagram was determined using X-ray diffraction measurements. Under high pressure (3.6–5.5?GPa) and low temperature (below 450?°C), the boron trioxide grains were reduced to the nanometer size and the hardness reaches to 13.9?GPa (5.5?GPa and 450?°C). The boroxol rings were produced only in the glass phase that was transformed from the α-B2O3 phase under HPHT. And the formation mechanism of boroxol rings was discussed according to Raman spectrum and crystal structure of α-B2O3 and β-B2O3.  相似文献   

5.
The analysis of the mechanical properties of thin films by nanoindentation has been recently subject of numerous theoretical and phenomenological studies as well as numerical simulations. In this work, we report on the application of the Winkler elastic foundation theory to analyze atomic force microscope nanoindentations of poly(n‐butyl methacrylate) films with thicknesses of 90, 196, and 485 nm. The elastic moduli of the samples were found to be 1.13 ± 0.43 GPa, 1.34 ± 0.32 GPa and 1.23 ± 0.24 GPa, respectively, after indentations of at least 50% of the film thickness. These data rely on the independent determination of the mechanical properties of 485‐nm thick films, using Sneddon's model at low penetration depth (yielding 1.27 ± 0.37 GPa). Our data show that the substrate effects begins to be noticeable only after indenting to a depth of more than 40% of the film thickness. POLYM. ENG. SCI., 2011. © 2011 Society of Plastics Engineers  相似文献   

6.
The elastic-plastic deformation of 3C-SiC thin film was investigated by a nanoindenter equipped with the Berkovich tip. Transition from pure elastic to elastic-plastic deformation was evidenced at an approximate load of 0.35 mN, when loading the sample at several peak loads ranging from 0.5 to 5 mN. The indentation size effect observed in 3C-SiC and was analyzed by Nix-Gao model. In purely elastic region, the Oliver- Pharr hardness values were 44 ± 2 GPa. In contrast, indentation size effects were evidenced in 3C-SiC specimen and the average value of Oliver-Pharr hardness in the indentation size effect region was 36 ± 2 GPa. Furthermore, depth independent or intrinsic hardness extracted from Nix-Gao was estimated as Ho = 26 ± 1 GPa which was also validated by proportional specimen resistance model, ie, H1 = 28 ± 1 and H2 = 28.5 ± 0.1 GPa. Besides, energy principle was utilized to extract Sakai Hardness as 104 GPa, which is combined elastic and elastic-plastic response. Moreover, based on energy principle, another property, ie, work of indentation was also determined to be 20 nJ/μm3. Similarly, elastic modulus had almost depicted stabilized value of 325 ± 8 GPa in pure elastic and elastic-plastic regions. In addition, plastic zone size was also estimated in elastic-plastic region using Johnson cavity model at pop-in and higher loads. Based on the first pop-in load at 0.35 mN, the distributions of shear and principal stresses were evaluated on various slip planes to elaborate the deformation behavior. Increase in loading rate from 100 to 400 μN/s increased critical pop-in load from 0.35 to 0.64 mN. This increase in critical pop-in load with increasing loading rate and values of maximum contact pressure indicates that no phase assisted transformation will occur at pop-in load. Based on theoretically calculated maximum tensile and cleavage strengths, it was affirmed that the elastic-plastic deformation occurred due to pop-in formation rather than tensile stresses. Moreover, it was also concluded on basis of Hertzian contact theory and Schmidt law that the highest possibility of slippage in 3C-SiC was along the {111} glide plane.  相似文献   

7.
Guangze Tang  Mingren Sun 《Carbon》2005,43(2):345-350
Fluorocarbon films were deposited on silicon substrate by R.F. magnetron sputtering using a polytetrafluoroethylene (PTFE) target. Structure of the deposited films was studied by X-ray photoelectron spectroscopy (XPS). Hardness, elastic modulus and scratch resistance were measured using a nanoindenter with scratch capability. -CFx (x = 1, 2, 3) and C-C units were found in the deposited fluorocarbon films. The hardness and elastic modulus of the films are strongly dependent on the R.F. power and deposition pressure. The film hardness is in the range from 0.8 GPa to 1.3 GPa while the film elastic modulus is in the range from 8 GPa to 18 GPa. Harder films exhibit higher scratch resistance. Differences in nanoindentation behavior between the deposited fluorocarbon films, diamond-like carbon (DLC) films and PTFE were discussed. The fluorocarbon films should find more applications in the magnetic storage and micro/nanoelectromechanical systems.  相似文献   

8.
Binary transition-metal nitrides (TMNs) are widely used as protective coating materials, and enhancing key performance characteristics are crucial to improving their robust and durable applications in harsh service environments. Compositional modulation via multiple elemental species offers an effective approach for optimizing physicochemical properties of TMNs, and establishing the composition–property relation is essential to the design of high-performance TMNs. In this work, we report on a comparative study of our synthesized NbN, NbMoN, and (NbMoTaW)N films and examined their microstructure, mechanical properties, and tribological and corrosion behaviors. The high-entropy (NbMoTaW)N film exhibits the highest hardness of 23.5 ± 1.35 GPa, which is ascribed to its high structural stability, increased elastic constant, and elastic modulus compared to the NbN and NbMoN films. The (NbMoTaW)N film also possesses the best wear resistance stemming from the highest H/E ratio and formation of self-lubricating MoO3 and WO3 species; moreover, this film shows the best corrosion resistance attributed to the sluggish diffusion of Cl due to lattice contraction and the structural stability caused by high-entropy effect. This work demonstrates simultaneously enhanced hardness and wear and corrosion resistance in a high-entropy TMN, opening a pathway for developing a new generation of advanced protective coating materials.  相似文献   

9.
The effect of thermal annealing on structure and mechanical properties of amorphous SiCxNy (y ≥ 0) thin films was investigated up to 1500°C in air and Ar. The SiCxNy films (2.2–3.4 μm) were deposited by reactive DC magnetron sputtering on Si, Al2O3 and α‐SiC substrates without intentional heating and at 600°C. The SiC target with small excess of carbon was sputtered at various N2/Ar gas flow ratios (0–0.48). The nitrogen content in the films changes in the range 0–43 at.%. Hardness and elastic modulus (nanoindentation), change in film thickness, film composition, and structure (Raman spectroscopy, XRD) were investigated in dependence on annealing temperature and nitrogen content. All SiCxNy films preserve their amorphous structure up to 1500°C. The hardness of all as‐deposited and both air‐ and Ar‐annealed SiCxNy films decreases with growth of nitrogen content. The annealing in Ar at temperatures of 1100°C–1300°C results in noticeable hardness growth despite the ordering of graphite‐like structure in carbon clusters in nitrogen free films. Unlike the SiC, this graphitization leads to hardness saturation of SiCN films starting above 900°C, especially for films with higher nitrogen content (deposited at higher N2/Ar). This indicates the practical hardness limit achievable by thermal treatment for SiCxNy films deposited on unheated substrates. The ordering in carbon phase is facilitated by the presence of nitrogen in the films and its extent is controlled by the N/C atomic ratio. The suppression of graphitization was observed for N/C ranging between 0.5–0.7. Films deposited at 600°C show higher hardness and oxidation resistance after annealing in comparison with those deposited on unheated substrates. Hardness reaches 40 GPa for SiC and ~28 GPa for SiCxNy (35 at.% of nitrogen). Such a high hardness of SiC film stems from its partial crystallization. Annealing of SiCxNy film (35 at.% of N) in Ar at 1400°C is accompanied by formation of numerous hillocks (indicating heterogeneous structure of amorphous films) and redistribution of film material.  相似文献   

10.
Polycrystalline Ti2AlN MAX phase films were fabricated by post-deposition annealing of Ti-Al-N film at annealing temperature in the range of 600?°C–800?°C in high vacuum. The temperature-dependent microstructure evolution from Ti-Al-N film to polycrystalline Ti2AlN film has been investigated. It was found that after post-deposition annealing above 600?°C, the as-deposited amorphous Ti-Al-N film transformed to polycrystalline Ti2AlN film. With the increase of annealing temperature from 600?°C to 700?°C, the crystallinity of polycrystalline Ti2AlN film was improved. At 800?°C, the surface Ti2AlN grains completely decomposed and transformed to TiN phase while inner grains was partial decomposed and surrounded by amorphous Al-rich phase. The polycrystalline Ti2AlN film exhibited a highest hardness of 34.1?GPa while the hardness of amorphous Ti-Al-N film was only 24.2?GPa. The mechanism of texture changes and phase transformation as well as its effect on thermal stability was also discussed.  相似文献   

11.
The phase transition of fullerene C60 under high pressure and high temperature has been widely studied, but the research on the spark-plasma sintering of C60 is limited, and the mechanical properties of synthesized materials are still unknown. In this study, a series of amorphous carbon materials were synthesized by spark-plasma sintering fullerene C60 at different temperatures. The structural characterizations showed that they were composed of multi-graphene fragments with different sizes, curvatures, and ordering degrees. The densities of the synthesized amorphous carbons were 1.3-1.4 g/cm3, which were lower than the values for graphite, but the mechanical properties were excellent. The highest compressive strength, indentation hardness, and elastic recovery of the amorphous carbons synthesized at different temperatures could reach up to ~1.25 GPa, ~3.8 GPa, and ~85.5%, respectively, which are far better than the values for commercial isotropic graphite materials.  相似文献   

12.
Diamond-like carbon (DLC) films have been deposited at atmospheric pressure by microwave-induced microplasma for the first time. Typical precursor gas mixtures are 250 ppm of C2H2 in atmospheric pressure He. Chemically resistant DLC films result if the Si (100) or glass substrate is in close contact with the microplasma, typically at a standoff distance of 0.26 mm. The films deposited under this condition have been characterized by various spectroscopic techniques. The presence of sp3 CH bonds and ‘D’ and ‘G’ bands were observed from FTIR and Raman spectroscopy, respectively. The surface morphology has been derived from SEM and AFM and shows columnar growth with column diameters of approximately 100 nm. Likely due to the low energy of ions striking the surface, the hardness and Young's modulus for the films were found to be 1.5 ± 0.3 GPa and 60 ± 15 GPa respectively with a film thickness of 2 μm. The hypothesis that a high flux of low energy ions can replace energetic ion bombardment is examined by probing the plasma. Rapid deposition rates of 4–7 μm per minute suggest that the method may be scalable to continuous coating systems.  相似文献   

13.
In this study, a novel high-entropy carbide-based ceramic cutting tool was developed. The cutting performance of three kinds of high-entropy carbide-based ceramic tools with different mechanical properties for the ISO C45E4 steel were evaluated. Although the pure (Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C0.8 ceramic cutting tool exhibited the highest hardness of 25.06 ± 0.32 GPa, the cutting performance was poor due to the chipping and catastrophic failure caused by the low toughness (2.25 ± 0.27 MPa m1/2). The (Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C0.8–15 vol% cobalt cutting tool with highest fracture toughness (6.37 ± 0.24 MPa m1/2) and lowest hardness (17.29 ± 0.79 GPa) showed the medium cutting performance due to the low wear resistance caused by the low hardness. The (Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C0.8–7.7 vol% cobalt cutting tool showed the longest effective cutting life of ∼67 min due to the high wear resistance and chipping resistance caused by the high hardness (21.05 ± 0.72 GPa), high toughness (5.35 ± 0.51 MPa m1/2), and fine grain size (0.60 ± 0.15 μm). The wear mechanisms of the cobalt-containing (Ti0.2Zr0.2Nb0.2Ta0.2Mo0.2)C0.8 ceramic cutting tools included adhesive wear and abrasive wear and oxidative wear. This research indicated that the high-entropy carbide-based ceramics with high hardness and high toughness have potential use in the field of cutting tool application.  相似文献   

14.
Interphase between the fibers and matrix plays a key role on the properties of fiber reinforced composites. In this work, the effect of interphase on mechanical properties and microstructures of 3D Cf/SiBCN composites at elevated temperatures was investigated. When PyC interphase is used, flexural strength and elastic modulus of the Cf/SiBCN composites decrease seriously at 1600°C (92 ± 15 MPa, 12 ± 2 GPa), compared with the properties at room temperature (371 ± 31 MPa, 31 ± 2 GPa). While, the flexural strength and elastic modulus of Cf/SiBCN composites with PyC/SiC multilayered interphase at 1600°C are as high as 330 ± 7 MPa and 30 ± 2 GPa, respectively, which are 97% and 73% of the values at room temperature (341 ± 20 MPa, 41 ± 2 GPa). To clarify the effect mechanism of the interphase on mechanical properties of the Cf/SiBCN composites at elevated temperature, interfacial bonding strength (IFBS) and microstructures of the composites were investigated in detail. It reveals that the PyC/SiC multilayered interphase can retard the SiBCN matrix degradation at elevated temperature, leading to the high strength retention of the composites at 1600°C.  相似文献   

15.
Thermal and elastic properties were measured for ceramics that contained as much as 96 wt% zeta phase tantalum carbide (ζ-Ta4C3−x). The ceramics were produced from tantalum hydride that was milled to reduce particle size and then blended with carbon. Powders were reaction hot-pressed at 1800°C for 2 hours under a flowing He environment, which resulted in ζ-Ta4C3−x that was about 99% dense. The main secondary phases present in the reacted ceramic were TaC and Ta2O5. ζ-Ta4C3−x had a thermal conductivity of 9.6 W/m·K and an electrical resistivity of 160 ± 4.2 μΩ-cm, which are lower and higher than those of TaC, respectively. The Young's modulus was 379 ± 5 GPa and the hardness was 5.1 ± 0.7 GPa, which are also both lower than TaC. This study is the first to report the thermal properties and elastic moduli of high-purity ζ-Ta4C3−x.  相似文献   

16.
The deposition system described for sub-30 Å and thicker carbon (ta-C) overcoat that includes two RF ion beam guns and Filtered Cathodic Arc (FCA) module mounted on a single vacuum chamber. The system is capable of flattening the Thin Film Magnetic Heads (TFMH) surface by ion beam etching; smoothing scratches, trenches, steps on boundaries of different materials, and enhancing the adhesion by ion assisted ion beam sputtering. It provides the highly controllable deposition of carbon using an FCA module with Ar-assisted arc discharge. Low-level particulates are achieved on the deposited film surface (< 5/cm2 ). It was shown that crucial impact on filtering the particles with size < 1 μm has the electrostatic field distribution across the plasma guide that can be controlled by duct bias. Mechanical and electrical properties, optical and Raman spectra of ta-C films were investigated as a function of Ar flow in the arc discharge area. At Ar flow rates 0–12 sccm, stress of the films was varied in a range 2.9–7.5 GPa while hardness and Young's Modulus stayed in ranges of 45–60 GPa, and 230–300 GPa, respectively. Density of the obtained films was greater than 2.8 g/cm3. Optical absorption and electrical conductivity of ta-C films showed a significant rise while stress came down with Ar flow. Raman G-peak was higher for ta-C films with lower stress and shifted to lower energy. The low stress films versus high stress films showed a few orders reduced electrical resistance and anisotropy of specific resistance with respect to substrate plane: ρ  ρ. In situ ellipsometric control of growing film thickness was implemented on the system. Run-to-run standard deviation was less than 1 Å for 20–25 Å thick films. High corrosion resistance of FCA coatings was exhibited. The impact of Ar gas–carbon plasma interaction on the deposition conditions and microstructure of ta-C films was discussed.  相似文献   

17.
C58 fullerene cages made by electron-impact induced fragmentation of C60 fullerenes have been assembled into several micron thick solid films by low energy cluster beam deposition onto inert substrates held at room temperature under ultrahigh vacuum. The resulting as-prepared material, RT-C58, behaves as an amorphous wide-band semiconductor. Nanoindentation was used to measure its mechanical properties revealing that RT-C58 has a higher elastic modulus E and hardness H than the reference carbon allotropes solid C60 and Highly Ordered Pyrolytic Graphite (HOPG): E(RT-C58) = 14 GPa and H(RT-C58) = 1.2 GPa. This effect can be explained by the unique intrinsic “functionalization” of C58 cages: they comprise reactive surface sites constituted by annelated pentagon rings which give rise to covalently stabilized oligomers, –C58–C58–C58, under our deposition conditions. Annealing, thick RT-C58 films up to 1100 K in ultrahigh vacuum results in HT-C58, a new material with considerably modified electronic and vibrational properties compared to the as-prepared RT-C58 film. The associated molecular transformations, including also partial cage–cage coalescence reactions, raise the overall mechanical hardness of the material: H(HT-C58) = 3.9 GPa.  相似文献   

18.
The single-phase formation and related elastic properties of (TiZrNbTaMo)C with one equimolar and twenty non-equimolar systems have been investigated by first-principles calculation. Based on the calculation results, the “composition-structure-elastic properties” correlation heatmapping predicts that Ti element is favorable for increment of hardness and Young’s modulus, while Mo element shows contrary tendency. The (TixZr2Nb2Ta2Mo4-x)C10-y (x = 1, 2, 3) have been fabricated by carbothermal reduction assisted hot-pressing sintering. The obtained experimental results validate the prediction trend of first-principles calculation. The optimization hardness and Young’s modulus is achieved at (Ti3Zr2Nb2Ta2Mo1)C10-y, and the corresponding value is 27.1 ± 0.6 GPa at 9.8 N and 490 ± 5 GPa, respectively. Noteworthily, the single-phase formation mainly depends on configuration entropy. The equimolar (Ti2Zr2Nb2Ta2Mo2)C10-y exhibits a single-phase with homogeneous chemical composition, but some element segregation can be found in the other two non-equimolar samples sintered at 2100 ℃.  相似文献   

19.
The nanomechanical properties of BiFeO3 (BFO) thin films are subjected to nanoindentation evaluation. BFO thin films are grown on the Pt/Ti/SiO2/Si substrates by using radio frequency magnetron sputtering with various deposition temperatures. The structure was analyzed by X-ray diffraction, and the results confirmed the presence of BFO phases. Atomic force microscopy revealed that the average film surface roughness increased with increasing of the deposition temperature. A Berkovich nanoindenter operated with the continuous contact stiffness measurement option indicated that the hardness decreases from 10.6 to 6.8 GPa for films deposited at 350°C and 450°C, respectively. In contrast, Young''s modulus for the former is 170.8 GPa as compared to a value of 131.4 GPa for the latter. The relationship between the hardness and film grain size appears to follow closely with the Hall–Petch equation.  相似文献   

20.
Nanocrystalline diamond (NCD) thin films have been grown by microwave plasma chemical vapor deposition (MPCVD) and investigated to determine their suitability for biomedical applications. Growth conditions were chosen to produce very uniform films over the surface of curved temporomandibular joint implants. These parameters include methane flow rates exceeding 20% of the hydrogen gas flow rate, and chamber pressure and microwave power were maintained at 30 Torr and 0.73 kW, respectively, in a Wavemat 6 kW MPCVD device. Films (3 μm thick) that completely coated 2.54-cm-diameter Ti–6Al–4V disks under these conditions exhibit mean grain size of 30.4 nm as determined by XRD peak broadening, hardness of 80 GPa as determined by nanoindentation, RMS mean roughness of 15.3±5.3 nm as determined by stylus profilometry, and film adhesion toughness (ΓC) of 158 J/m2 as determined by a Rockwell indentation method. Similar deposition performed on small Ti–6Al–4V hemispheres produce films with smaller mean grain size of 21.1 nm and correspondingly lower hardness and roughness. Overall, these films exhibit properties well suited for use in biomedical applications.  相似文献   

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