The effect of silicon doping on the residual stress of CVD diamond films is examined using both X-ray diffraction (XRD) analysis and Raman spectroscopy measurements. The examined Si-doped diamond films are deposited on WC-Co substrates in a home-made bias-enhanced HFCVD apparatus. Ethyl silicate (Si(OC2H5)4) is dissolved in acetone to obtain various Si/C mole ratio ranging from 0.1% to 1.4% in the reaction gas. Characterizations with SEM and XRD indicate increasing silicon concentration may result in grain size decreasing and diamond [110] texture becoming dominant. The residual stress values of as-deposited Si-doped diamond films are evaluated by both sin2ψ method, which measures the (220) diamond Bragg diffraction peaks using XRD, with ψ-values ranging from 0° to 45°, and Raman spectroscopy, which detects the diamond Raman peak shift from the natural diamond line at 1332 cm-1. The residual stress evolution on the silicon doping level estimated from the above two methods presents rather good agreements, exhibiting that all deposited Si-doped diamond films present compressive stress and the sample with Si/C mole ratio of 0.1% possesses the largest residual stress of ~1.75 GPa (Raman) or ~2.3 GPa (XRD). As the silicon doping level is up further, the residual stress reduces to a relative stable value around 1.3 GPa.
Chemical vapor deposition (CVD) diamond coated drills are fabricated by depositing diamond films on Co-cemented tungsten carbide (WC-Co) drills. The characteristics of as-deposited diamond coatings are investigated by scanning electron microscope (SEM) and Raman spectra. To evaluate the cutting performance of diamond coated drills, comparative drilling tests are conducted using diamond coated and uncoated WC-Co drills, with carbon fiber reinforced plastics (CFRPs) as the workpiece on a high-speed computer numerical control (CNC) machine. Thrust force and tool wear are measured during the drilling process. The results show that diamond coated drill exhibits better cutting performance, compared with the uncoated drill. The value of flank wear is about 70 μm after machining 90 holes, about a half of that of the WC-Co drill with 145 μm after drilling only 30 holes. The wear rate of WC-Co drill is higher than that of diamond coated drill before diamond films peeling off. The diamond coated drill achieves more predictable hole quality. The improved cutting performance of the diamond coated drill is due to the high hardness, wear resistance and low coefficient of friction.
The failure behavior of diamond-coated die was investigated experimentally and analytically through finite element method (FEM) simulation in the present work. Diamond coatings were fabricated by straight hot filament chemical vapor deposition (CVD) passing through the interior hole of the drawing die using a mixture of hydrogen and acetone as source gases. The performance tests were made under real drawing condition. Scanning electron microscopy (SEM) was used for the study of coating wear after die service. The coating wear appears on two regions of the reduction zone: one is near the entrance where the contact begins, and the other is at the end of the reduction zone. FEM simulation was made for calculating the von Mises stresses distribution on the coating and substrate during the drawing process. The present work was of great practical significance for the improvement of drawing performance of diamond-coated drawing dies.
Systematical researches were accomplished on WC-Co with different Co contents(6%,10%and 12%,mass fraction).Based on the XPS and EDX,from orthogonal pretreatment experiments,it is indicated that the acid concentration,the time of the acid pretreatment and the original Co content have significant influences on the Co-removal depth(D).Moreover,the specimen temperature,original Co content and Co-removal depth dependences of the Co evolution in nucleation,heating(in pure H2 atmosphere)and growth experiments were discussed,and mechanisms of Co evolutions were summarized,providing sufficient theoretical bases for the deposition of high-quality diamond films on WC-Co substrates,especially Co-rich WC-Co substrates.It is proven that the Co-rich substrate often presents rapid Co diffusion.The high substrate temperature can promote the Co diffusion in the pretreated substrate,while acts as a Co-etching process for the untreated substrates.It is finally found that the appropriate Co-removal depth for the WC-12%Co substrate is 8-9μm.
Xin-chang WANGCheng-chuan WANGWei-kai HEFang-hong SUN
Chemical vapor deposition （CVD） diamond films have attracted more attentions due to their excellent mechanical properties. Whereas as-fabricated traditional diamond films in the previous studies don＇t have enough adhesion or surface smoothness, which seriously impact their friction and wear performance, and thus limit their applications under extremely harsh conditions. A boron doped, undoped microcrystalline and fine grained composite diamond （BD-UM-FGCD） film is fabricated by a three-step method adopting hot filament CVD （HFCVD） method in the present study, presenting outstanding comprehensive performance, including the good adhesion between the substrate and the underlying boron doped diamond （BDD） layer, the extremely high hardness of the middle undoped microcrystalline diamond （UMCD） layer, as well as the low surface roughness and favorable polished convenience of the surface fine grained diamond （FGD） layer. The friction and wear behavior of this composite film sliding against low-carbon steel and silicon nitride balls are studied on a ball-on-plate rotational friction tester. Besides, its wear rate is further evaluated under a severer condition using an inner-hole polishing apparatus, with low-carbon steel wire as the counterpart. The test results show that the BD-UM-FGCD film performs very small friction coefficient and great friction behavior owing to its high surface smoothness, and meanwhile it also has excellent wear resistance because of the relatively high hardness of the surface FGD film and the extremely high hardness of the middle UMCD film. Moreover, under the industrial conditions for producing low-carbon steel wires, this composite film can sufficiently prolong the working lifetime of the drawing dies and improve their application effects. This research develops a novel composite diamond films owning great comprehensive properties, which have great potentials as protecting coatings on working surfaces of the wear-resistant and anti-frictional components.
A specific revised HFCVD apparatus and a novel process combining HFCVD and polishing technique were presented to deposit the micro-and nano-crystalline multilayered ultra-smooth diamond（USCD） film on the interior-hole surface of WC-Co drawing dies with aperture ranging from d1.0 mm to 60 mm.Characterization results indicate that the surface roughness values（Ra） in the entry zone,drawing zone and bearing zone of as-fabricated USCD coated drawing die were measured as low as 25.7,23.3 and 25.5 nm,respectively.Furthermore,the friction properties of USCD films were examined in both dry sliding and water-lubricating conditions,and the results show that the USCD film presents much superior friction properties.Its friction coefficients against ball-bearing steel,copper and silicon nitride balls（d4 mm）,is always lower than that of microcrystalline diamond（MCD） or WC-Co sample,regardless of the lubricating condition.Meanwhile,it still presents competitive wear resistance with the MCD films.Finally,the working lifetime and performance of as-fabricated USCD coated drawing dies were examined under producing low-carbon steel pipes in dry-sliding and water-lubricating conditions.Under the water-lubricating drawing condition,its production significantly increases by about 20 times compared with the conventional WC-Co drawing dies.
Deposition parameters that have great influences on hot filament chemical vapor deposition (HFCVD) diamond films growth on inner hole surfaces of WC?Co substrates mainly include the substrate temperature (t), carbon content (φ), total pressure (p) and total mass flow (F). Taguchi method was used for the experimental design in order to study the combined effects of the four parameters on the properties of as-deposited diamond films. A new figure-of-merit (FOM) was defined to assess their comprehensive performance. It is clarified thatt,φandp all have significant and complicated effects on the performance of the diamond film and the FOM, which also present some differences as compared with the previous studies on CVD diamond films growth on plane or external surfaces. Aiming to deposit HFCVD diamond films with the best comprehensive performance, the key deposition parameters were finally optimized as:t=830 °C,φ=4.5%,p=4000 Pa,F=800 mL/min.
