This study investigates the effect of ZrB$_2$ additions on the microstructure, thermal stability, and thermo-mechanical wear behaviour of polycrystalline diamond. Following high-pressure high-temperature (HPHT) sintering, the ZrB$_2$-PCD material showed a full conversion of the binder phase to cobalt-boride (Co2B and Co$_{23}$B$_6$) phases. In-situ PXRD and TEM vacuum annealing experiments observed that the onset of bulk graphitisation occurred above $1000^{\circ}C$ for the ZrB$_2$-PCD material, compared to $850^{\circ}C$ for the STD-PCD material. The ZrB$_2$-PCD tools showed excellent thermo-mechanical wear behaviour, exhibiting increased durability and a steady wear scar progression during high-temperature dry-VTL testing. However, lowered abrasion wear resistance was observed for the ZrB2-PCD tools during low-temperature wet-VTL testing, probably due the reduced diamond contiguity in the ZrB2 additive sample. Further optimisation of the ZrB$_2$ additive phase content, mixing methodology, or sintering conditions could be explored to improve the abrasive wear resistance of this novel PCD material.
We report on measurements of the temperature dependence of resistivity, $ρ(T)$, for single crystal samples of ZrB$_{12}$, ZrB$_{2}$ and polycrystalline samples of MgB$_{2}$. It is shown that cluster compound ZrB$_{12}$ behaves like a simple metal in the normal state, with a typical Bloch -- Grüneisen $ρ(T)$ dependence. However, the resistive Debye temperature, $T_{R}=300 K$, is three times smaller than $T_{D}$ obtained from specific heat data. We observe the $T^{2}$ term in $ρ(T)$ of these borides, which could be interpreted as an indication of strong electron-electron interaction. Although th…
In this work, Ni50Al50 alloy is taken into consideration as potential brazing material for joining ZrB2 ultra-high temperature ceramic. The results of experimental study on high temperature interfacial phenomena between molten binary Ni50Al50 alloy and polycrystalline ZrB2, are shown. A sessile drop method combined with a capillary purification procedure was applied to investigate the wetting behavior of Ni50Al50/ZrB2 couple during holding for 400 seconds at temperature of 1688°C (i.e. at T=1.02Tm). It was found that the molten Ni50Al50 rapidly wets and spreads over the surface of ZrB2, while …
The letter introduces a diagram that rationalizes tunneling atomic force microscopy (TUNA) observations of electron emission from polycrystalline diamonds as described in recent publications. The direct observations of electron emission from grain boundary sites by TUNA could indeed be evidence of electrons originating from grain boundaries under external electric fields. At the same time, from the diagram it follows that TUNA and field emission schemes are complimentary rather than equivalent for results interpretation. It is further proposed that TUNA could provide better insights into emiss…
Quantum-mechanical molecular-dynamics simulations are carried out to explore possible precursor states of nano-polycrystalline diamond, a novel ultra-hard material produced directly from graphite. Large-scale simulation with 10^5 atoms is realized by using the ' order-N' simulation code 'ELSES' (http://www.elses.jp). The simulation starts with a diamond structure that contains initial structural defects and results in a mixture of graphite(sp^2)-like and diamond(sp^3)-like regions as nano-meter-scale domains. We speculate that the domains are metastable and are possible candidates of the precu…
The chemical vapor deposition of polycrystalline diamond (PCD) films is typically done on substrates seeded with diamond nanoparticles. Specular laser reflectance and a continuous film model have been used to monitor the thickness of these films during their deposition. However, most seeds are isolated during the early stages of the deposition, which questions the utility of applying such a continuous film model for monitoring deposition before film formation. In this work, we present a model based on the Rayleigh theory of scattering for laser reflectance at substrates with growing nanodiamon…
We report on wide-field optically detected magnetic resonance imaging of nitrogen-vacancy centers (NVs) in type IIa polycrystalline diamond. These studies reveal a heterogeneous crystalline environment that produces a varied density of NV centers, including preferential orientation within some individual crystal grains, but preserves long spin coherence times. Using the native NVs as nanoscale sensors, we introduce a 3-dimensional strain imaging technique with high sensitivity ( $< 10^{-5}$ Hz$^{-1/2}$) and diffraction-limited resolution across a wide field of view.
Quantum information processing and integrated nanophotonics require robust generation of single photon emitters on demand. In this work we demonstrate that diamond films grown by microwave plasma chemical vapour deposition on a silicon substrate host bright, narrowband single photon emitters in the visible to near infrared spectral range. The emitters possess fast lifetime, absolute photostability, and exhibit full polarization at excitation and emission. Pulsed and continuous laser excitations confirm their quantum behaviour at room temperature, while low temperature spectroscopy is done to i…
Polycrystalline diamond films with systematic change in microstructure that varies from microcrystalline to nanocrystalline structure are synthesized on Si by hot filament chemical vapor deposition. The morphology and structural properties of the grown diamond films are analyzed using field emission scanning electron microscope (FESEM), atomic force microscope (AFM), X-ray diffraction and Raman spectroscopy. The average roughness and grain size of the diamond films decrease with increase in CH4 to H2 ratio from 0.5 to 3 %. Also, structural disorder in these diamond films increases with decreas…
The surface topography of diamond coatings strongly affects surface properties such as adhesion, friction, wear, and biocompatibility. However, the understanding of multi-scale topography, and its effect on properties, has been hindered by conventional measurement methods, which capture only a single length scale. Here, four different polycrystalline diamond coatings are characterized using transmission electron microscopy to assess the roughness down to the sub-nanometer scale. Then these measurements are combined, using the power spectral density (PSD), with conventional methods (stylus prof…
Dielectric resonators are key components for many microwave and millimetre wave applications, including high-Q filters and frequency-determining elements for precision frequency synthesis. These often depend on the quality of the dielectric material. The commonly used material for building the best cryogenic microwave oscillators is sapphire. However sapphire is becoming a limiting factor for higher frequencies design. It is then important to find new candidates that can fulfil the requirements for millimetre wave low noise oscillators at room and cryogenic temperatures. These clocks are used …
In this paper, we describe the modification of Nanoscale Impedance Microscopy (NIM), namely, a combination of contact-mode atomic force microscopy with local impedance measurements. The postulated approach is based on the application of multifrequency voltage perturbation instead of standard frequency-by-frequency analysis, which among others offers more time-efficient and accurate determination of the resultant impedance spectra with high spatial resolution. Based on the impedance spectra analysis with an appropriate electric equivalent circuit, it was possible to map surface resistance and c…
Time-domain Brillouin scattering technique, also known as picosecond ultrasonic interferometry, which provides opportunity to monitor propagation of nanometers to sub-micrometers length coherent acoustic pulses in the samples of sub-micrometers to tens of micrometers dimensions, was applied to depth-profiling of polycrystalline aggregate of ice compressed in a diamond anvil cell to Megabar pressures. The technique allowed examination of characteristic dimensions of elastic inhomogeneities and texturing of polycrystalline ice in the direction normal to the diamond anvil surfaces with sub-microm…
Chemical-Vapor-Deposition (CVD) diamond films were prepared using a variation of nitrogen addition into the gas source admixture by a direct current CVD method. The influence of nitrogen addition on the crystallographic texture and grain shape evolution in heteroepitaxial polycrystalline diamond films was investigated using high-resolution electron backscattering diffraction (HR-EBSD) and X-ray diffraction (XRD). The analysis reveals that an addition of 1.5% N2 to the CH4 gas flow leads to a strong enhancement of a {110} fiber texture. The phenomenon is discussed in terms of a competitive grow…
A suspended system for measuring the thermal properties of membranes is presented. The sensitive thermal measurement is based on the 3$ω$ dynamic method coupled to a V$\ddot{o}$lklein geometry. The device obtained using micro-machining processes allows the measurement of the in-plane thermal conductivity of a membrane with a sensitivity of less than 10nW/K (+/-$5x10^{-3}$Wm$^{-1}K^{-1}$ at room temperature) and a very high resolution ($ΔK/K =10^{-3}$). A transducer (heater/thermometer) centered on the membrane is used to create an oscillation of the heat flux and to measure the temperature osc…
Ultra-nanocrystalline diamond is a polycrystalline material, having crystalline diamond grains of sizes in the nanometer regime. We study the structure and mechanical properties of this material as a function of the average grain size, employing atomistic simulations. From the calculated elastic constants and the estimated hardness, we observe softening of the material as the size of its grains decreases. We attribute the observed softening to the enhanced fraction of interfacial atoms as the average grain size becomes smaller. We provide a fitting formula for the scaling of the cohesive energ…
We present atomistic simulations for the mechanical response of ultra nanocrystalline diamond, a polycrystalline form of diamond with grain diameters of the order of a few nm. We consider fully three-dimensional model structures, having several grains of random sizes and orientations, and employ state-of-the-art Monte Carlo simulations. We calculate structural properties, elastic constants and the hardness of the material; our results compare well with experimental observations for this material. Moreover, we verify that this material becomes softer at small grain sizes, in analogy to the obse…
Diamond provides superior optical and mechanical material properties, making it a prime candidate for the realization of integrated optomechanical circuits. Because diamond sub- strates have matured in size, efficient nanostructuring methods can be used to realize full-scale integrated devices. Here we review optical and mechanical resonators fab- ricated from polycrystalline as well as single crystalline diamond. We present relevant material properties with respect to implementing optomechanical devices and compare them with other material systems. We give an overview of diamond integrated op…
Substantial developments have been achieved in the synthesis of chemical vapour deposition (CVD) diamond in recent years, providing engineers and designers with access to a large range of new diamond materials. CVD diamond has a number of outstanding material properties that can enable exceptional performance in applications as diverse as medical diagnostics, water treatment, radiation detection, high power electronics, consumer audio, magnetometry and novel lasers. Often the material is synthesized in planar form, however non-planar geometries are also possible and enable a number of key appl…
Nano-polycrystalline diamond (NPD) and nanotwinned diamond (NtD) were successfully synthesized in multi-anvil high pressure apparatus at high pressure and high temperature (HPHT) conditions using precursors of onion carbons. We found that the choices of distinct onion carbons with hollow or multi-cored microstructures lead to the synthesis of different diamond products of NPD or NtD ones. High quality NtD with an average twin size of 6.8 nm has been synthesized whose Vickers hardness reaches as high as 180 GPa as measured by indentation hardness experiment. The existence of stacking faults oth…
Radio-Frequency Gasket for Studies of Superconductivity in Diamond Anvil Cells
Center for High Pressure Science & Technology Advanced Research(高压科学前沿技术先进研究中心);Shanghai Key Laboratory of Material Frontiers Research in Extreme Environments (MFree)(极端环境下材料前沿研究上海市重点实验室(MFree));Shanghai Advanced Research in Physical Sciences (SHARPS)(上海物理科学先进研究中心(SHARPS))
Single-photon sources are a fundamental element for developing quantum technologies, and sources based on colour centres in diamonds are among the most promising candidates. The well-known NV centres are characterized by several limitations, thus few other defects have recently been considered. In the present work, we characterize in detail native efficient single colour centres emitting in the near infra-red in both standard IIa single-crystal and electronic-grade polycrystalline commercial CVD diamond samples. In the former case, a high-temperature annealing process in vacuum is necessary to…
Thermal conductivity of nanocrystalline and ultra-nanocrystalline films is analyzed with effective medium theory (EMT) models. The existing EMT models use the spherical inclusion approximation. Although this approximation works quite well it is inconsistent, mostly with respect to the maximal packing of 74{\%}, which may be unrealistic for polycrystalline films. To check the consistency of these models we devise an EMT model with arbitrarily shaped inclusions. We pick the EMT model with cubic inclusions and we compare its results with the results of the EMT model with spherical inclusions. It …
In situ high-pressure energy dispersive x-ray diffraction experiments on polycrystalline powder TiN with NaCl-type structure have been conducted with the pressure up to 30.1 GPa by using the diamond anvil cell instrument with synchrotron radiation at room tempearture. The experimental results suggested that an isostructural phase transition might exist at about 7 GPa as revealed by the discontinuity of V/V0 with pressure.
The maximum output power of GaN-based high-electron mobility transistors is limited by high channel temperature induced by localized self-heating which degrades device performance and reliability. With generated heat fluxes within these devices reaching magnitude close to ten times of that at the sun surface, chemical vapor deposition (CVD) diamond is an attractive candidate to aid in the extraction of this heat in order to keep the operating temperatures of these high power electronics as low as possible. Due to the observed inhomogeneous structure, CVD diamond membranes exhibit a 3D anisotro…
Understanding the impact of lattice imperfections on nanoscale thermal transport is crucial for diverse applications ranging from thermal management to energy conversion. Grain boundaries (GBs) are ubiquitous defects in polycrystalline materials, which scatter phonons and reduce thermal conductivity. Historically, their impact on heat conduction has been studied indirectly through spatially-averaged measurements, that provide little information about phonon transport near a single GB. Here, using spatially-resolved time-domain thermoreflectance (TDTR) measurements in combination with electron …
Hexagonal boron nitride (h-BN) is unique among two-dimensional materials, with a large band gap (~6 eV) and high thermal conductivity (>400 W/m/K), second only to diamond among electrical insulators. Most electronic studies to date have relied on h-BN exfoliated from bulk crystals; however, for scalable applications the material must be synthesized by methods such as chemical vapor deposition (CVD). Here, we demonstrate single- and few-layer h-BN synthesized by CVD on single crystal platinum and on carbon nanotube (CNT) substrates, also comparing these films with h-BN deposited on the more com…