Understanding Dielectric Breakdown and Related Tool Wear Characteristics in Nanoscale Electro-Machining Process

To address the need to produce sub-50 nm scale features for manufacturing of nano/bio devices and systems, a nanoscale electro-machining (nano-EM) process is being studied. This paper reports unique field induced effects on a tungsten tool. During machining, the tungsten atoms leave the active tool tip in the form of clusters. Upon machining, the tool tip end radius was sharper (∼20 nm after in comparison with ∼35 nm before). The tool surface was chemically modified to a nanocrystalline matrix of tungsten oxide and tungsten carbide. The tool sharpening and the formation of the nanocrystalline matrix are expected to prolong the tool life in the nano-EM process in a manufacturing environment.     

Hard and superhard TiAlBN coatings deposited by twin electron-beam evaporation

Superhard nanostructured coatings, prepared by plasma-assisted chemical vapour deposition (PACVD) and physical vapour deposition (PAPVD) techniques, such as vacuum arc evaporation and magnetron sputtering, are receiving increasing attention due to their potential applications for wear protection. In this study nanocomposite (TiAl)B_xN_y (0.09 ≤ x ≤ 1.35; 1.07 ≤ y ≤ 2.30) coatings, consisting of nanocrystalline (Ti,Al)N and amorphous BN, were deposited onto Si (100), AISI 316 stainless steel and AISI M2 tool steel substrates by co-evaporation of Ti and hot isostatically pressed (HIPped) Ti-Al-B-N material from a thermionically enhanced twin crucible electron-beam (EB) evaporation source in an Ar plasma at 450 °C. The coating stoichiometry, relative phase composition, nanostructure and mechanical properties were determined using X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD), in combination with nanoindentation measurements. Aluminium (∼ 10 at.% in coatings) was found to substitute for titanium in the cubic TiN based structure. (Ti,Al)B_0.14N_1.12 and (Ti,Al)B_0.45N_1.37 coatings with average (Ti,Al)N grain sizes of 5-6 nm and either ∼ 70, or ∼ 90, mol% (Ti,Al)N showed hardness and elastic modulus values of ∼ 40 and ∼ 340 GPa, respectively. (Ti,Al)B_0.14N_1.12 coatings retained their ‘as-deposited’ mechanical properties for more than 90 months at room temperature in air, comparing results gathered from eight different nanoindentation systems. During vacuum annealing, all coatings examined exhibited structural stability to temperatures in excess of 900 °C, and revealed a moderate, but significant, increase in hardness. For (Ti,Al)B_0.14N_1.12 coatings the hardness increased from ∼ 40 to ∼ 45 GPa.     

A pinless embedded tool used in FSSW and FSW of aluminum alloy

A pinless tool design was proposed to achieve high butt tensile strength in aluminum alloy sheets (∼3 mm thick) in friction stir welding (FSW), where a 7 mm long cylindrical insert rod made of aluminum alloy was tightly embedded into a hollow cylindrical tool. The effects of rod diameter (d) on the welding properties and mechanism of weld formation were investigated. For friction stir spot welding (FSSW), the maximum rate of temperature rise was about 12.8 °C/s, and the failure load was about 2 kN for this pinless tool (d = 10 mm), with these being about 7.4 °C/s and 1.35 kN for the plain one. For FSW, the failure load was about 1.46 kN for this tool, and about 0.72 kN for the plain one. The abutting edges of sheets with a thickness of 3 mm could be welded using this pinless tool.     

Effect of sintering temperature and time on densification, microstructure and properties of the PZT/ZnO nanowhisker piezoelectric composites

Lead zirconate titanate (PZT) based piezoelectric composites embedded with ZnO nanowhiskers (ZnO_w) were investigated to clarify the optimal sintering condition for densification, microstructure, and electrical properties. The samples are characterized by X-ray diffraction analysis and scanning electron microscopy. The results show that the increase of the sintering temperature and time is quite effective in improving the densification and piezoelectric properties of the PZT/ZnO_w composites. However, the relative density and piezoelectric properties deteriorate as the composites are sintered over the optimal sintering condition. Particularly, the PZT/ZnO_w composites sintered at 1150 °C for 2 h show excellent electrical properties of piezoelectric constant d₃₃ ∼ 471 pC/N, relative dielectric constant ? ∼ 3838, planar electromechanical coupling factor k_p ∼ 0.543, remnant polarization P_r ∼ 23.2 μC/cm² and coercive field E_c ∼ 9.2 kV/cm.     

Workpiece surface integrity when slot milling γ-TiAl intermetallic alloy

Slot milling is presented as a potential manufacturing route for aerospace component feature production when machining γ-TiAl intermetallic alloy Ti–45Al–2Mn–2Nb + 0.8 vol.% TiB₂XD using 2 mm diameter AlTiN coated WC ball nose end milling cutters. When operating with flood cutting fluid at v = 88 m/min, f = 0.05 mm/tooth, d = 0.2 mm, maximum flank wear was ∼65 μm after 25 min. SEM micrographs of slot surfaces show re-deposited/adhered and smeared workpiece material to a length of ∼50 μm. Brittle fracture of the slot edges was restricted to <10 μm with sporadic top burr formation observed up to ∼20 μm. Cross sectional micrographs of the slot sidewalls showed bending of the lamellae limited to within 5 μm.     

Profiled Superabrasive Grinding Wheels for the Machining of a Nickel Based Superalloy

Machining data are presented for small diameter, profiled (fir tree root form), single layer/electroplated CBN (B46, B76 and 91) and diamond (D46) grinding wheels, when cutting Udimet 720. Spindles operating at 60,000 and 90,000 rpm were employed, with a synthetic polyalphaolefine (PAO) oil based fluid in a down grinding mode on single sided specimens. Operating parameters were selected to reflect finishing conditions. Measured tool wear was lower for CBN grit as compared to diamond however workpiece roughness was lower with Ra approaching 0.75 μm when using D46 wheels. Higher rotational speed produced lower grinding wheel wear. No workpiece burning was observed irrespective of grit type at the conditions tested.     

Polymorphic phase transition-induced electrical behavior of BiCoO3-modified (K0.48Na0.52)NbO3 lead-free piezoelectric ceramics

(1 − x)(K_0.48Na_0.52)NbO₃-xBiCoO₃ [KNN-xBC] lead-free piezoelectric ceramics were prepared by the conventional solid-state sintering method. The effects of the BiCoO₃ addition on the phase structure, dielectric, piezoelectric and ferroelectric properties of KNN-xBC ceramics were systematically investigated. The polymorphic phase transition (PPT) from rhombohedral to orthorhombic phase around room temperature was identified in the composition range of 0.01 ≤ x ≤ 0.02, and the improved electrical properties were induced by this PPT. The KNN-0.01BC ceramics near PPT exhibit optimum electrical properties: d₃₃ ∼ 165 pC/N, k_p ∼ 0.40, P_r ∼ 31.0 μC/cm², and E_c ∼ 12.6 kV/cm. These results indicate that the enhanced piezoelectric properties for alkali niobate can be achieved by forming the coexistence of rhombohedral and orthorhombic phases.     

Internal structure of clusters of partially coherent nanocrystallites in Cr-Al-N and Cr-Al-Si-N coatings

Nano-sized clusters consisting of strongly preferentially oriented, partially coherent nanocrystallites were observed in Cr-Al-N and Cr-Al-Si-N coatings deposited using cathodic arc evaporation. Microstructure analysis of the coatings, which was done using the combination of X-ray diffraction (XRD) and transmission electron microscopy with high resolution (HRTEM), revealed furthermore stress-free lattice parameters, size and local disorientation of crystallites within the nano-sized clusters in dependence on the aluminium and silicon contents, mean size of these clusters and the kind of structure defects. Within the face-centred cubic (fcc) Cr_{1 − x − y}Al_xSi_yN phase, the stress-free lattice parameter was described by the equation a = (0.41486 − 0.00827 · x + 0.034 · y) nm. The size of individual crystallites decreased from ∼ 11 nm in Cr_0.92Al_0.08N to ∼ 4 nm in Cr_0.24Al_0.65Si_0.10N. These nanocrystallites formed clusters with the mean size between 36 and 56 nm. The mutual disorientation of the partially coherent nanocrystallites forming the clusters increased with increasing aluminium and silicon contents from 0.5° to several degrees. The disorientation of neighbouring nanocrystallites was explained by the presence of screw dislocations and by presence of phase interfaces in coatings containing a single fcc phase and several phases, respectively.     

Effect of dwell time during sintering on piezoelectric properties of (Ba0.85Ca0.15)(Ti0.90Zr0.10)O3 lead-free ceramics

In this letter, the effect of dwell time (1-6 h) during sintering on the piezoelectric properties is investigated for the (Ba_0.85Ca_0.15)(Ti_0.90Zr_0.10)O₃ ceramics. All ceramics sintered at different dwell time are of a pure phase, and its structure distortion is induced by too long dwell time. Their dielectric constant and remanent polarization increases and the coercive field decreases with increasing dwell time. An enhanced piezoelectric behavior (d₃₃ ∼ 492 pC/N and k_p ∼ 51.5%) is demonstrated for the BCTZ ceramic with an optimum dwell time of 5 h, owing to the structure distortion together with a dense microstructure and a larger grain size.     

Microstructure, ferroelectric, and piezoelectric properties of (1 − x − y)Bi0.5Na0.5TiO3-xBaTiO3-yBi0.5Ag0.5TiO3 lead-free ceramics

Lead-free (1 − x − y)Bi_0.5Na_0.5TiO₃-xBaTiO₃-yBi_0.5Ag_0.5TiO₃ (BNT-BT-BAT-x/y, x = 0-0.10, y = 0-0.075) piezoelectric ceramics were synthesized by conventional oxide-mixed method. The microstructure, ferroelectric, and piezoelectric properties of the ceramics were investigated. Results show that a morphotropic phase boundary (MPB) between rhombohedral and tetragonal phases of BNT-BT-BAT-x/0.04 ceramics is formed at x = 0.06-0.08. The addition of BAT has no obvious change on the crystal structure of BNT-BT ceramics while it causes the grain size of the ceramics to become more homogenous. Near the MPB, the ceramics with x = 0.06 and y = 0.05-0.06 possess optimum electrical properties: P_r ∼ 42.5 μC/cm², E_c ∼ 32.0 kV/cm, d₃₃ ∼ 172 pC/N, k_p ∼ 32.6%, and k_t ∼ 52.6%. The temperature dependences of k_p and polarization versus electric hysteresis loops reveal that the depolarization temperature (T_d) of BNT-BT-BAT-0.06/y ceramics decreases with increasing y. In addition, the polar and non-polar phases may coexist in the BNT-BT-BAT-x/y ceramics above T_d.     

Micro-electrical discharge machining of polycrystalline diamond using rotary cupronickel electrode

Cupronickel was used as the electrode material to fabricate microstructures on polycrystalline diamond by electrical discharge machining (EDM). The electrodes were shaped into tiny rotary wheels driven by the flow of EDM fluid. Results showed that material removal rate was improved by a factor of five compared to conventional electrode materials. Raman spectroscopy and energy dispersive X-ray spectroscopy indicated that graphitization of diamond and diffusion-based chemical reactions between nickel and diamond dominated the EDM process. Effects of electrode rotation rate and discharge energy on the EDM characteristics were clarified. High form accuracy (∼0.5 μm/1 mm) and low surface roughness (∼0.1 μm Ra) were obtained.     

Synthesis and magnetic properties of nickel nanoparticles deposited on the silicon nanowires

Nickel (Ni) nanoparticles with sizes of ∼35 nm were deposited on the surface of silicon nanowires (SiNWs) by electroless plating technique. The magnetic properties of Ni/SiNWs were investigated. The blocking temperature (T_B) of 370 K was obtained and confirmed by field-cooled (FC) and zero-field-cooled (ZFC) plots. The M-H hysteresis loops from 5 K to 400 K were measured. The saturation magnetization value was ∼4.5 emu/g and the coercivity was ∼375.3 Oe for the loop at 5 K, respectively. While for the loop at 400 K, these values were of ∼2.6 emu/g and ∼33.3 Oe, respectively. The temperature dependence of coercivity followed by the relation H_C(T) = H_C0[1 − (T/T_B)^1/2], indicating a superparamagnetic behavior. The magnetization of superparamagnetic grains in a magnetic field H was better described by Langevin function at 400 K. These novel magnetic properties of Ni/SiNWs were possibly attributed to the paramagnetic defects on the surface of SiNWs.     

Effect of corrosion severity on fatigue evolution in Al-Zn-Mg-Cu

The effect of existing-localized corrosion on fatigue cracking of 7075-T6511 was established using crack surface marker-band analysis and a fracture mechanics model. The substantial reduction of fatigue life due to EXCO solution L-S surface pre-corrosion is nearly independent of exposure time after initial-sharp degradation, scaling with the evolution of pit-cluster size and initial stress intensity range with exposure time. Independent of exposure time, formation of a resolvable fatigue crack (∼10 μm) accounts for a similar-low (∼5%) fraction of total fatigue life at low stress range (σ_max = 150 MPa, R = 0.1). Crack formation occurs at microscopic protrusions into the corroded volume. A corrosion-modified-equivalent initial flaw size (CM-EIFS); predicted with the AFGROW tool using measured initial aspect ratio, initiation cycles, and total fatigue life inputs; accurately represents the corrosion damage effect on fatigue for a range of exposures. The similar deleterious effect of several corroding environments for various-exposed surfaces is described by a lower-bound CM-EIFS with a 300 μm depth and 1200 μm surface length suggesting fatigue is governed by a microscopic pit-based topography. Either an approximate lower-bound, or specific CM-EIFS calibrated by limited measurements of fatigue life for service-environment exposed specimens, can be used to assess the impact of corrosion in a damage tolerant framework. Complexities (e.g., local H embrittlement, 3D pit geometry, topography dependent initiation, and microstructure sensitive small-crack growth) do not compromise the CM-EIFS estimation, but must be better understood for refined modeling.     

Microstructure, mechanical, EPR and optical properties of lithium disilicate glasses and glass-ceramics doped with Mn ions

The microstructure, mechanical, EPR and optical properties of transparent MnO₂ doped lithium disilicate (LDS) glass-ceramics prepared by melt quenching and controlled crystallization, have been studied. The microstructure of the glass-ceramics has been characterized using FE-SEM, TEM, FT-IR and XRD techniques. FE-SEM micrographs show elongated, highly interlocked, dense (∼80 vol.%) nanocrystals of LDS with an average size ∼100 nm. XRD and FT-IR studies reveal that the only crystalline phase formed after heat-treatment at 700 °C for 1 h is LDS. A good combination of average microhardness ∼5.6 GPa, high fracture toughness ∼2.8 MPa m^1/2, 3-point flexural strength ∼250 MPa and moderate elastic modulus 65 GPa has been obtained. The EPR spectra of both LDS glasses and glass-ceramics exhibit resonance signals with effective g values at g = 4.73, g = 4.10, g = 3.3, and g = 1.98. The resonance signal at g = 1.98 is found to be more intense than the other signals and exhibits hyperfine structure at lower concentration of manganese. From the observed spectrum, the spin-Hamiltonian parameters have been evaluated. In glass samples the optical absorption spectrum exhibits a broad band around ∼20,320 cm⁻¹ which has been assigned to the transition ⁶A_1g(S) → ⁴A_1g(G) ⁴E_g(G)-of Mn²⁺ ions. The cerammed samples upon 394 nm excitation emit a green luminescence (565 nm, ⁴T_1g → ⁶A_1g(G) transition of Mn²⁺ ions), and a weak red emission (710 nm). From the ultraviolet absorption edges, the optical bandgap energies (E_opt) were evaluated and are discussed.     

Thermal stability of superhard Ti-B-N coatings

Ternary transition-metal boron nitride Ti-B-N offers outstanding hardness and thermal stability, which are increasingly required for wear resistant applications, as the protective coatings are subjected to high temperature, causing thermal fatigue. Ti-B-N coatings with chemical compositions close to the quasibinary TiN-TiB₂ tie line and boron contents below ∼ 18 at.% contain a crystalline supersaturated NaCl structure phase, where B substitutes for N. Annealing above the deposition temperature causes precipitation of TiB₂, which influence dislocation mobility and hence the hardness of TiB_0.40N_0.83 remains at a very high level of ∼ 43 GPa with annealing temperature T_a up to 900 °C. Growth of Ti-B-N coatings with B contents above ∼ 18 at.% results in the formation of nm sized TiN and TiB₂ crystallites embedded in a high volume fraction of disordered boundary layer. The compaction of this disordered phase during annealing results in a hardness increase of TiB_0.80N_0.83 coatings from the as-deposited value of ∼ 37 GPa to ∼ 42 GPa at T_a = 800 °C. Excess B during growth of TiB_2.4 coatings causes the formation of bundles of ∼ 5 nm wide TiB₂ subcolumns encapsulated in a B-rich tissue phase. This nanocolumnar structure is thermally stable up to temperatures of ∼ 900 °C, and consequently the hardness remains at the very high level of ~ 48 GPa, as nucleation and growth of dislocations is inhibited by the nm sized columns. Furthermore, the high cohesive strength of the B-rich tissue phase prevents grain boundary sliding.     

Nanocrystals of a new complex perovskite dielectric Ba2TmSbO6

Nanocrystals of a new complex perovskites ceramic oxide, barium thulium antimony oxide - Ba₂TmSbO₆, were synthesized using a single step auto-ignition combustion process. The combustion product was single phase and composed of aggregates of nanocrystals of sizes in the range 20-50 nm. Ba₂TmSbO₆ crystallized in cubic perovskite structure with lattice parameter, a = 8.4101 Å. The polycrystalline fluffy combustion product was sintered to high density (∼97%) at ∼1450 °C for 4 h. Resistivity of the sintered specimen was ∼5 MΩ/cm. The Ba₂TmSbO₆ has dielectric constant (?′) and dielectric loss (tan δ) of 17 and ∼10⁻⁴ at 5 MHz; the new material would probably be developed as a low-loss dielectric material.     

Micro grinding tool for manufacture of complex structures in brittle materials

This paper presents a novel micro shaft grinding tool with cylindrical tool tip diameter between 13 μm and 100 μm. The manufacturing of the tool itself is carried out on a prototype desktop machine. The shaping of the tool is accomplished by grinding the tool tip directly onto the cylindrical carbide tool shank. During tool grinding, the tool shank rotates in a micro spindle with air-lubricated bearings, leading to high concentricity and low run-out. The tool tip is electrically nickel plated with diamond grains. During first experimental tests of the tool, very low surface roughness values and sharp edges without burrs were achieved.     

Structural, optical and EPR studies on ZnO:Cu nanopowders prepared via low temperature solution combustion synthesis

Cu (0.1 mol%) doped ZnO nanopowders have been successfully synthesized by a wet chemical method at a relatively low temperature (300 °C). Powder X-ray diffraction (PXRD) analysis, scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Fourier transformed infrared (FTIR) spectroscopy, UV-Visible spectroscopy, Photoluminescence (PL) and Electron Paramagnetic Resonance (EPR) measurements were used for characterization. PXRD results confirm that the nanopowders exhibit hexagonal wurtzite structure of ZnO without any secondary phase. The particle size of as-formed product has been calculated by Williamson-Hall (W-H) plots and Scherrer's formula is found to be in the range of ∼40 nm. TEM image confirms the nano size crystalline nature of Cu doped ZnO. SEM micrographs of undoped and Cu doped ZnO show highly porous with large voids. UV-Vis spectrum showed a red shift in the absorption edge in Cu doped ZnO. PL spectra show prominent peaks corresponding to near band edge UV emission and defect related green emission in the visible region at room temperature and their possible mechanisms have been discussed. The EPR spectrum exhibits a broad resonance signal at g ∼ 2.049, and two narrow resonances one at g ∼ 1.990 and other at g ∼ 1.950. The broad resonance signal at g ∼ 2.049 is a characteristic of Cu²⁺ ion whereas the signal at g ∼ 1.990 and g ∼ 1.950 can be attributed to ionized oxygen vacancies and shallow donors respectively. The spin concentration (N) and paramagnetic susceptibility (χ) have been evaluated and discussed.     

Low-loss microwave dielectrics using rock salt oxide Li2MgTiO4

Rock-salt-structured Li₂MgTiO₄ ceramic was prepared by the conventional mixed oxide route and its microwave dielectric properties were investigated. The microstructures of the ceramics were characterized by SEM. The dielectric properties of the ceramics exhibited a significant dependence on the sintering condition and crystal structure. A new microwave dielectric material, Li₂MgTiO₄ sintered at 1360 °C has a dielectric constant (?_r) of ∼17.25, a Q × f of ∼97,300 GHz (where f = 9.86 GHz, is the resonant frequency) and a τ_f of ∼-27.2 ppm/°C. The microwave dielectric properties of the ceramic are reported for the first time.     

Hydrogen absorption and desorption characteristics of high coercivity NdDyFeCoNbCuB sintered magnet. I. Low temperature hydrogen decrepitation treatments

Hydrogen absorption/adsorption properties of high coercivity NdDyFeCoNbCuB sintered magnets were determined. Hydrogenation kinetics were analyzed using both differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Hydrogenation of the Nd-rich intergranular phase results in a rather broad and large peak at ∼100 ± 50 °C, then the tetragonal main phase (Φ phase) reacts readily close to 195 °C. The disproportionation process of the whole magnet initiates at T ∼ 500 °C, then accelerates in the vicinity of 600 °C and finally ends at T ∼ 780 °C. Furthermore, the first hydrogenation reaction, which is associated with the hydrogen diffusion in the bulk via the intergranular Nd-rich phase, was seen to proceed quite differently depending on the heating rate, or the applied plateau temperature. While hydrogen absorption at 50 °C is rather slow, it results in higher hydrogen uptake than at 150 °C, though there it happens much faster. Three modes of hydrogenation of sintered magnets are discussed in terms of practical operability. Using the optimized hydrogen decrepitation/desorption annealing route leads to a demonstration that the anisotropic NdDyFeCoNbCuB powders obtained by the HD/D technique have recovered most of the magnetic performance initially displayed in the bulk magnets.