CO2 laser peeling of Al2O3 ceramic and an application for the polishing of laser cut surfaces

A laser controlled fracture peeling technique is demonstrated to smooth the Al₂O₃ ceramic surface without thermal damages. It was found that a chip can be separated and curled from the ceramic surface during a focused CO₂ continuous wave (CW) laser dual-scanning. The thickness of the curled chip is ～50 μm and the formed subsurface roughness (R_a ≈ 2 μm) is close to the surface machined by mechanical breaking (R_a = 1.84 μm). The chip formation is attributed to the controlled fracture by the residual tensile stress in the recast layer, whereas the chip curling only occurs when the melting depth is shallower than the position of lateral cracks. The peeling technique can be applied to polish the cut surface of laser fusion cutting in ceramics. The polished cut surface (R_a = 2.18 μm) is free from recast, crack and heat effects. The microstructure is similar to the base material. The material removal rate during polishing is up to 0.125 mm³/s.     

Thermal analysis of submicron nanocrystalline diamond films

The thermal properties of sub-μm nanocrystalline diamond films in the range of 0.37–1.1 μm grown by hot filament CVD, initiated by bias enhanced nucleation on a nm-thin Si-nucleation layer on various substrates, have been characterized by scanning thermal microscopy. After coalescence, the films have been outgrown with a columnar grain structure. The results indicate that even in the sub-μm range, the average thermal conductivity of these NCD films approaches 400 W m^− 1 K^− 1. By patterning the films into membranes and step-like mesas, the lateral component and the vertical component of the thermal conductivity, k_lateral and k_vertical, have been isolated showing an anisotropy between vertical conduction along the columns, with k_vertical ≈ 1000 W m^− 1 K^− 1, and a weaker lateral conduction across the columns, with k_lateral ≈ 300 W m^− 1 K^− 1.     

Influence of SiC particle addition on the nucleation density and adhesion strength of MPCVD diamond coatings on Si3N4 substrates

It is generally accepted that SiC layers are often involved in the adhesion efficiency of chemical vapour deposition (CVD) diamond films on Si-containing substrates. Si₃N₄–SiC composite substrates with different amounts of SiC particles (0–50 wt%) were then used for diamond deposition. Samples were produced by pressureless sintering (1750°C, N₂ atmosphere, 2–4 h). The diamond films were grown on a commercial MPCVD reactor using H₂/CH₄ mixtures. Despite there being no special substrate pre-treatment, the films were densely nucleated when SiC was added (N_d≈1×10¹⁰ cm⁻²) with primary nanosized (∼100 nm) particles, followed by a less dense (N_d≈1×10⁶ cm⁻²) secondary nucleation. Indentation experiments with a Brale tip of up to 588 N applied load corroborated the benefit of SiC inclusion for a strong adhesion. The low thermal expansion coefficient mismatch between Si₃N₄ and diamond resulted in very low compressive stresses in the film, as proved by micro-Raman spectroscopy.     

Thermal conductivity of diamond composites sintered under high pressures

Thermal conductivity at room temperature of diamond composites of two types: with a diamond skeleton and with diamond grains imbedded in a non-diamond matrix was evaluated in dependence of the diamond grain size (d) varied from a ten of microns to 500 μm. The thermal conductivity of the compacts with diamond skeleton obtained in the Cu–diamond system at high pressure of 8 GPa strongly increases with diamond particles size approaching the maximum value of 9 W/cm K at d ≈ 200 μm. The compacts sintered in the Cu–Ti–diamond, Al–Si–diamond and Si–diamond systems at lower pressure (2 GPa) are formed predominantly owing to the presence of the binder. It was found for these conditions that the thermal conductivity is less sensitive to the diamond grain size, reaching the value of 6 W/cm K for the composites with SiC–Si matrix.     

Formation of self-assembled platinum particles on diamond and their embedding in diamond by microwave plasma chemical vapor depositions

Single-crystalline and polycrystalline diamond films containing platinum particles with sizes of ≤ ≈ 100 nm have been formed through a self-assembling process. Pt thin films pre-deposited on diamond were found to completely change in shape to grains during a subsequent diamond overgrowth process using a microwave-plasma chemical-vapor-deposition (MPCVD) technique. The self-assembled Pt grains on flat diamond surfaces had approximately spherical particles with rather uniform sizes when the pre-deposited Pt films were sufficiently thin or less than ≈ 1 μm in thickness. The average diameter of such Pt particles, D, was well controlled simply by changing the thickness of the pre-deposited Pt film, t_pt, since D was proportional to t_pt. Such spherical Pt particles were completely embedded after sufficient diamond overgrowth. Transmission electron microscope observations revealed that most of the spherical Pt particles were well crystallized and that the interfacial structures between the diamond overlayer and the buried Pt particles were sufficiently sharp without any appreciable mixing regions.     

Effect of H2/Ar plasma on growth behavior of ultra-nanocrystalline diamond films: The TEM study

Incorporation of H₂ species into Ar plasma was observed to markedly alter the microstructure of diamond films. TEM examinations indicate that, while the Ar/CH₄ plasma produced the ultrananocrystalline diamond films with equi-axed grains (~ 5 nm), the addition of 20% H₂ in Ar resulted in grains with dendrite geometry and the incorporation of 80% H₂ in Ar led to micro-crystalline diamond with faceted grains (~ 800 nm). Optical emission spectroscopy suggests that small percentage of H₂-species (< 20%) in the plasma leads to partially etching of hydrocarbons adhered onto the diamond clusters, such that the C₂-species attach to diamond surface anisotropically, forming diamond flakes, which evolve into dendrite geometry. In contrast, high percentage of H₂-species in the plasma (80%) can efficiently etch away the hydrocarbons adhered onto the diamond clusters, such that the C₂-species can attach to diamond surface isotropically, resulting in large diamond grains with faceted geometry. The field needed to turn on the electron field emission for diamond films increases from E₀ = 22.1 V/μm (J_e = 0.48 mA/cm² at 50 V/μm applied field) for 0% H₂ samples to E₀ = 78.2 V/μm (J_e < 0.01 mA/cm² at 210 V/μm applied field) for 80% H₂ samples, as the grains grow, decreasing the proportion of grain boundaries.     

Distribution in angular mismatch between crystallites in diamond films grown in microwave plasma

High resolution electron backscattered diffraction (EBSD) has been used for analysis of grain size, texture and stress distribution on growth side of free-standing polycrystalline diamond films of different grade. The undoped and moderate boron-doped films of 0.3–0.5 mm thickness were grown by microwave plasma CVD. The highest number of stressed domains, mostly located at grain boundaries, and the largest average grain misorientation angle (θ ≈ 6°) have been found for B-doped film. Highly defected and highly [001] oriented “black” diamond exhibited much more rear stress domains, this being ascribed to angular mismatch as small as θ = 0.5° in that film. The samples of “white” diamond showed somewhat intermediate pictures, with stress observed both in bulk and on grain boundaries. Evolution of texture (columnar growth) and stress distribution with film thickness has been observed with EBSD study of film cross-sections.     

Chemical mechanical polishing of thin film diamond

The demonstration that Nanocrystalline Diamond (NCD) can retain the superior Young’s modulus (1100 GPa) of single crystal diamond twinned with its ability to be grown at low temperatures (<450 °C) has driven a revival into the growth and applications of NCD thin films. However, owing to the competitive growth of crystals the resulting film has a roughness that evolves with film thickness, preventing NCD films from reaching their full potential in devices where a smooth film is required. To reduce this roughness, films have been polished using Chemical Mechanical Polishing (CMP). A Logitech Tribo CMP tool equipped with a polyurethane/polyester polishing cloth and an alkaline colloidal silica polishing fluid has been used to polish NCD films. The resulting films have been characterised with Atomic Force Microscopy, Scanning Electron Microscopy and X-ray Photoelectron Spectroscopy. Root mean square roughness values have been reduced from 18.3 nm to 1.7 nm over 25 μm², with roughness values as low as 0.42 nm over ∼0.25 μm². A polishing mechanism of wet oxidation of the surface, attachment of silica particles and subsequent shearing away of carbon has also been proposed.     

Influence of steel substrate roughness on morphology and mesostructure of TiO2 porous layers produced by template-assisted dip coating

Mesoporous titania films were prepared by template-assisted dip coating on 1.4301 stainless-steel substrates processed by grinding and spark erosion to different degrees of roughness. The influence of substrate roughness on the morphology and mesostructure of deposited films was studied. Textures produced by grinding with roughness R_a ranging from 0.10 to 0.78 μm did not noticeably affect the pore structure as confirmed by similar pore size and a single cubic mesophase formed on grinded steel. Grinding had a modest effect on the film integrity which manifested in fractures developed in the texture depressions. Greater roughness of the steel produced by spark erosion affected the micelle self-assembly process yielding two different mesophases on a substrate of 1.08 μm roughness, and resulting in a predominant loss of templated mesostructure on a rougher (R_a = 2.69 μm) substrate surface. Film surface area expressed as m² BET per m² of the substrate planar dimensions increased with substrate roughness. Higher roughness resulted in higher photocatalytic activity of crystalline films when tested in methylene blue decomposition. Given that a moderate surface texture had a negligible effect on the film mesostructure, introducing controlled substrate roughness may serve as a technique to enhance the total film surface area.     

Synthesis of diamond using ultra-nanocrystalline diamonds as seeding layer and their electron field emission properties

A modified nucleation and growth process was adopted so as to improve the electron field emission (EFE) properties of diamonds films. In this process, a thin layer of ultra-nanocrystalline diamonds (UNCD), instead of bias-enhanced-nuclei, were used as nucleation layer for growing diamond films in H₂-plasma. The morphology of the grains changes profoundly due to such a modified CVD process. The geometry of the grains transform from faceted to roundish and the surface of grains changes from clear to spotty. The Raman spectroscopies and SEM micrographs imply that such a modified diamond films consist of UNCD clusters (~ 10–20 nm in size) on top of sp³-bonded diamond grains (~ 100 nm in size). Increasing the total pressure in CVD chamber deteriorated the Raman structure and hence degraded the EFE properties of the films, whereas either increasing the methane content in the H₂-based plasma or prolonged the growth time improved markedly the Raman structure and thereafter enhanced the EFE properties of diamond films. The EFE properties for the modified diamond films can be turned on at E₀ = 11.1 V/μm, achieving EFE current density as large as (J_e) = 0.7 mA/cm² at 25 V/μm applied field.     

Ultrasonochemical coating and characterization of TiO2-coated zirconia fine particles

Zirconia fine particles were prepared by ultrasonic spray pyrolysis (USP) and employed as a substrate for titanium/titania coating by ultrasonochemistry. The effects of several process factors on the characteristics of the prepared particles were investigated and the particles were then characterized by various techniques. This substrate was coated with various titanium concentrations (0.025–0.1 M) for two ultrasonication time periods (30 min, 2 h) by sonochemistry, and finally calcined at 1100 °C. Raman spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), particle size analysis (PSA), Fourier transformation infrared spectroscopy (FT-IR) and inductively coupled plasma-atomic emission spectroscopy (ICP-AES) comprised the techniques used to characterize them. The particles were prepared in a monodispersed spherical form with no interior cavity; their average size was shown to be 0.62 μm before calcination and 2.57 μm after calcination. The titania surface coating acted to partially stabilize the particles to a tetragonal phase. Based on the analytical results, the optimum conditions for preparing the particles were shown to be 7.5 wt% of titania as an initial solution concentration and 0.5 h of coating time.     

NUMERICAL PREDICTION OF THE PERFORMANCE OF A MANIFOLD SAMPLER WITH A CIRCULAR SLIT INLET IN TURBULENT FLOW

The performance of a bioaerosol manifold sampler with a circular slit inlet in a turbulent flow field was modeled using a 3-D numerical approach. The standard κ–ε turbulence model was used for simulating the mean turbulent flow, and the Lagrangian approach was used for predicting the particle trajectories. The ratios of wind velocities to sampler inlet velocities were from 0.5 to 3.5. Calculations were conducted for particle sizes of 2, 8, 15,and26 μm. The agreement between numerical and empirical sampling efficiencies was good. It was found that lower sampling efficiencies at high R values were associated with increased positive pitch of the velocity vectors generated at the inlet slit. Unbalanced sampling velocities between the upstream and downstream arcs were found only at high R values. At an inlet velocity of 0.8 m/s, sampling efficiencies for 15 μm particles decreased about 24% as R was increased from 0.5 to 3.5. A similar effect was observed at an inlet velocity of 0.4 m/s. Turbulence decreased sampling efficiency and was related to the sum of the magnitudes of the wind and sampling velocity vectors.     

Application of thin diamond films in low-coherence fiber-optic Fabry Pérot displacement sensor

The novel fiber-optic low coherence sensor with thin diamond films is demonstrated. The undoped and boron-doped diamond films were elaborated by the use of the microwave plasma enhanced chemical vapor deposition (μPE CVD) system. The optical signal from the Fabry–Pérot cavity made with the application of those thin films is sensitive to displacement. The sensor characterization was made in the range of 0–600 μm. The measurements were performed using two superluminescent diodes (SLD) with central wavelengths of 1290 mm and 1550 mm and the output signal was analyzed by the measurement of the modulation change of spectral pattern. Furthermore, very good coefficient of the determination R² > 0.9565 and the visibility of optical measured signal equal to 95.6% were achieved.     

Composite diamond films for short-mm wave and THz traveling wave tube windows

With an increase in frequency, the diamond thickness of the microwave windows for short-mm wave and THz traveling wave tubes (TWTs) approaches 100 μm or even tens of μm. This poses problems of mechanical strength and air tightness to the polycrystalline diamond (PCD) window. To overcome these problems, we have studied a composite diamond film that consists of PCD and ultra-nanocrystalline diamond (UNCD). First, SEM was used to examine the early growing process of UNCD on PCD. The 5 μm thick UNCD grown on 40 μm PCD exhibited a hillock structure with densely packed ≤ 20 nm granules, in contrast to the PCD layer showing randomly packed, micrometer sized grains. Then, the effect of UNCD thickness on fracture strength and thermal conductivity was studied using the test samples with thin layers of UNCD having thicknesses of 1, 2.5, 5, and 10 μm on 100 μm thick PCD films, respectively. The fracture strengths of all the films are 2–3 times higher than that of the PCD films, which is 350 ± 150 MPa. As expected, the thermal conductivity of the samples measured at ~ 20 °C decreases with an increase in UNCD thickness, particularly in the range of 0 to 2.5 μm. At a thickness of 10 μm, the thermal conductivity was found to be ~ 10 W/cm 1 K. Finally, a 100 μm sandwich-like structure with a total UNCD thickness of 10 μm was fabricated and two 180 GHz TWT windows were assembled. RF tests show that for the operating frequency range of 175 to 185 GHz, the transmission loss (S₂₁) was found to be ≤ 1.22 and ≤ 1.71 dB, respectively, indicating an excellent RF performance. Mechanical strength and air tightness of the windows were also found improved and able to meet the requirement of the device. This work provides a novel approach for fabricating relatively thin diamond films for RF applications, such as TWT windows.     

Microstructural characterization of diamond films deposited on c-BN crystals

The morphology and structure of diamond films, deposited on cubic boron nitride (c-BN) crystals by microwave-plasma-enhanced chemical vapor deposition, is studied by high-resolution scanning electron microscopy and micro-Raman spectroscopy. The c-BN crystals, with sizes of 200 to 350 μm and grown by a high-temperature/high-pressure technique, were embedded in a copper holder, and used as substrates in deposition runs of 15 min to 5 h. The nucleation centers for diamond appear as well-shaped cuboctahedral crystallites, having diameters of approximately 100 nm. With increasing deposition time the diamond crystallites grew larger, forming islands on the c-BN faces. In some cases, epitaxial growth was observed on the (111) c-BN faces where coalesced particles gave rise to very smooth regions. A number of diamond crystals with peculiar shapes are observed, such as a pseudo five-fold symmetry due to multiple twinning. Moreover, both randomly distributed carbon tubes, about 100 nm in diameter and 1 μm in length, and spherically shaped features are observed in samples prepared under the typical conditions of diamond deposition, this effect being ascribed to the influence of plasma-sputtered copper contamination. Quite unusual diamond crystals with a deep, pyramidal-shaped hole in the middle grew on the copper substrate between the c-BN crystals.     

Nucleation and growth surface conductivity of H-terminated diamond films prepared by DC arc jet CVD

High-quality polycrystalline diamond film has been extremely attractive to many researchers, since the maximum transition frequency (f_T) and the maximum frequency of oscillation (f_max) of polycrystalline diamond electronic devices are comparable to those of single crystalline diamond devices. Besides large deposition area, DC arc jet CVD diamond films with high deposition rate and high quality are one choice for electronic device industrialization. Four inch free-standing diamond films were obtained by DC arc jet CVD using gas recycling mode with deposition rate of 14 μm/h. After treatment in hydrogen plasma under the same conditions for both the nucleation and growth sides, the conductivity difference between them was analyzed and clarified by characterizing the grain size, surface profile, crystalline quality and impurity content. The roughness of growth surface with the grain size about 400 nm increased from 0.869 nm to 8.406 nm after hydrogen plasma etching. As for the nucleation surface, the grain size was about 100 nm and the roughness increased from 0.31 nm to 3.739 nm. The XPS results showed that H-termination had been formed and energy band bent upwards. The nucleation and growth surfaces displayed the same magnitude of square resistance (R_s). The mobility and the sheet carrier concentration of the nucleation surface were 0.898 cm/V s and 10¹³/cm² order of magnitude, respectively; while for growth surface, they were 20.2 cm/V s and 9.97 × 10¹¹/cm², respectively. The small grain size and much non-diamond carbon at grain boundary resulted in lower carrier mobility on the nucleation surface. The high concentration of impurity nitrogen may explain the low sheet carrier concentration on the growth surface. The maximum drain current density and the maximum transconductance (g_m) for MESFET with gate length L_G of 2 μm on H-terminated diamond growth surface was 22.5 mA/mm and 4 mS/mm, respectively. The device performance can be further improved by using diamond films with larger grains and optimizing device fabrication techniques.     

Study of light scattering on a soda lime glass eroded by sandblasting

In Saharan areas of Algeria, sandstorms can damage vehicles windshields inducing incidental light diffusion that affects the driver's visibility. Vehicles technical controllers find some difficulties with damaged windshields. The control being made visually with the naked eye, it is therefore difficult to judge when a damaged windshield is no more valid to use. In this context, we studied the influence of the surface state of a soda lime glass on the scattering of a white light. The varying parameters considered are the projected sand mass, the opening of the light beam and the distance sample-receptor. By increasing the projected sand mass up to 200 g, the optical transmission falls from 91.6 to 13% and the roughness increases from 0.035 up to 2.27 μm and then tends toward a constant level. For the as-received state, the image obtained using a CCD camera presents a net boundary and the transmission profile shows a saturation plateau. By damaging the surface, the image boundary deforms and becomes diffuse. For the highly damaged states, the image become completely blurred and the transmission profile disappears. The variation of the transmission according to roughness shows an inflection point at T = 73% and R_a = 1.5 μm. This point seems to separate two domains: a transparent field (R_a < 1.5 μm) and a blur field (R_a > 1.5 μm). The visibility limit obtained in our tests conditions is estimated at about 73%.     

Effect of XeF laser treatment on structure of nanocrystalline diamond films

Nanocrystalline diamond (NCD) films were deposited on Si substrates by microwave plasma-enhanced chemical vapor deposition (MPECVD) using methane/hydrogen/oxygen (30/169/0.2 sccm) as process gases. Subsequently a thin (0.33 μm) and a thick (1.01 μm) NCD films were irradiated with XeF excimer laser (λ = 351 nm) with 300 and 600 mJ cm^? 2 of energy densities in air. The NCD films became rougher after laser irradiations. Fraction of graphitic clusters decreased but oxygen content increased in the thin NCD film after laser irradiation. Opposite phenomena were observed for the thick NCD films. Effect of laser irradiation to oxygenation and graphitization of NCD films was correlated with structural properties of free surface and grain boundaries of the thin and thick NCD films.     

Application of the dusty plasma method for preparation of diamond ceramics

Diamond particles 3–7 μm in size sustained in plasma in a high-dispersion state were coated with cobalt by magnetron sputtering. The relative concentration of cobalt in obtained powders was 2–3 mass. %. Sintering the diamond powders with the cobalt coating under the pressure of 8 GPa and the temperatures of 2000–2100 K resulted in the production of homogeneous specimens having the density of 3.6 ± 0.1 g cm^− 3. The produced diamond compacts demonstrated high values of the ultrasonic wave propagation velocity and elastic moduli.     

Preparation of poly-lactic acid nano/microparticles using supercritical anti-solvent with enhanced mass transfer

Supercritical anti-solvent precipitation with enhanced mass transfer (SAS-EM) was applied for the production of micro and sub-microparticles of poly-lactic acid (PLA). SAS-EM technique uses an ultrasonic vibrating surface to enhance mass transfer rate between supercritical CO₂ and solvent. Without applying ultrasonic power, which is same as SAS process, PLA particles with average diameters ranging between 1 μm and 3 μm were obtained. Using SAS-EM with the power supply of 200 W, spherical PLA particles smaller than 1 μm were obtained. The particle size was able to be controlled in the range of 0.4 μm–1.0 μm, by adjusting the power supply of ultrasonic field, the system pressure and temperature.