Polycrystalline Diamond Micro-Hotplates.

Micro-hotplate structures are increasingly being investigated for use in a host of applications ranging from broadband infra-red sources within absorption-based gas sensors to in situ heater stages for ultra-high-resolution imaging. With devices usually fabricated from a conductive electrode placed on top of a freestanding radiator element, coefficient of thermal expansion (CTE) mismatches between layers and electro-migration within the heating element typically lead to failure upon exceeding temperatures of 1600 K. In an attempt to mitigate such issues, a series of hotplates of varying geometry have been fabricated from a single layer of mechanically robust, high thermal conductivity, and low CTE boron-doped polycrystalline diamond. Upon testing under high vacuum conditions and characterization of the emission spectra, the resulting devices are shown to exhibit a grey-body like emission response and reach temperatures vastly in excess of conventional geometries of up to 2731 K at applied powers of ⩽100 mW. Characterization of the thermalization time meanwhile demonstrates rapid millisecond response times, while Raman spectroscopy reveals the performance of the devices is dictated by cumulative graphitization at elevated temperatures. As such, both diamond and sp2 carbon are shown to be promising materials for the fabrication of next-generation micro-hotplates.

SAW Resonators and Filters Based on Sc0.43Al0.57N on Single Crystal and Polycrystalline Diamond.

The massive data transfer rates of nowadays mobile communication technologies demand devices not only with outstanding electric performances but with example stability in a wide range of conditions. Surface acoustic wave (SAW) devices provide a high Q-factor and properties inherent to the employed materials: thermal and chemical stability or low propagation losses. SAW resonators and filters based on Sc0.43Al0.57N synthetized by reactive magnetron sputtering on single crystal and polycrystalline diamond substrates were fabricated and evaluated. Our SAW resonators showed high electromechanical coupling coefficients for Rayleigh and Sezawa modes, propagating at 1.2 GHz and 2.3 GHz, respectively. Finally, SAW filters were fabricated on Sc0.43Al0.57N/diamond heterostructures, with working frequencies above 4.7 GHz and ~200 MHz bandwidths, confirming that these devices are promising candidates in developing 5G technology.

Electropositive Nanodiamond-Coated Quartz Microfiber Membranes for Virus and Dye Filtration.

Electropositive membranes demonstrating high flux at low pressure differentials show great promise as universal separation platforms for viruses and other charged entities when centralized systems of water and power are scarce. However, the fabrication of a suitably stable membrane with optimal electrostatic characteristics remains a challenge. Here, hydrogenated detonation nanodiamond was loaded onto a quartz microfiber support membrane and coupled to the membrane surface under a high vacuum annealing process. The fabricated membranes display a zeta potential of +45 mV at pH 7 and an isoelectric point around pH 11. We show that the nanodiamond coating is robust to prolonged periods of pressurized water flow by performing extensive zeta potential measurements over time, and water filtration tests demonstrated excellent membrane retention for the electronegative dye molecule acid black 2, and at least a 6.2 log10 reduction in MS2 bacteriophage from feed waters (>99.9999%).

High-throughput nitrogen-vacancy center imaging for nanodiamond photophysical characterization and pH nanosensing.

The fluorescent nitrogen-vacancy (NV) defect in diamond has remarkable photophysical properties, including high photostability which allows stable fluorescence emission for hours; as a result, there has been much interest in using nanodiamonds (NDs) for applications in quantum optics and biological imaging. Such applications have been limited by the heterogeneity of NDs and our limited understanding of NV photophysics in NDs, which is partially due to the lack of sensitive and high-throughput methods for photophysical analysis of NDs. Here, we report a systematic analysis of NDs using two-color wide-field epifluorescence imaging coupled to high-throughput single-particle detection of single NVs in NDs with sizes down to 5-10 nm. By using fluorescence intensity ratios, we observe directly the charge conversion of single NV center (NV- or NV0) and measure the lifetimes of different NV charge states in NDs. We also show that we can use changes in pH to control the main NV charge states in a direct and reversible fashion, a discovery that paves the way for performing pH nanosensing with a non-photobleachable probe.

Facile Amine Termination of Nanodiamond Particles and Their Surface Reaction Dynamics.

Nanodiamond synthesized by the detonation method is a composite of sp3/sp2 carbon structures; amorphous and disordered-sp2 carbons populate the surface of a sp3 diamond core lattice. Because of the production process, various elemental impurities such as N, O, H, and so forth are inherent in interstitial sites or the surface carbon (sp2/amorphous) network. Herein, the reaction dynamics on the surface of ultradisperse diamond (UDD) due to the surface transformation or reconstruction during annealing in vacuum with temperatures ranging from ambient to 800 °C is described. In situ measurement of Fourier transform infrared spectroscopic analysis shows that low-temperature (<500 °C) annealing of UDD in vacuum results in isonitrile/isocyanide (-N=C:) and nitrile functionalization (-C≡N) on the surface. At temperatures ∼500 °C, the surface hydrogenation of UDD is initiated. During annealing at 780-800 °C, the nitrile group (-C≡N) is reduced to the primary amine (NH2), and isonitrile (-N=C:) turns it to be in the saturated () structure. On exposure to air, the obtained isonitrile is transformed to an N-formyl derivative (Aryl/R-NH-CHO) structure via hydrolysis. This study provides a fundamental insight into the surface reactive profile of UDD which could lead to facile surface functionalization properties and their applications in various fields such as biomedical, biosensing, drug delivery, epoxy materials process, tribology, and possibly in cyano (-C≡N/-N=C:) chemistry.

Thick, Adherent Diamond Films on AlN with Low Thermal Barrier Resistance.

The growth of >100-µm-thick diamond layers adherent on aluminum nitride with low thermal boundary resistance between diamond and AlN is presented in this work. The thermal barrier resistance was found to be in the range of 16 m2·K/GW, which is a large improvement on the current state-of-the-art. While thick films failed to adhere on untreated AlN films, AlN films treated with hydrogen/nitrogen plasma retained the thick diamond layers. Clear differences in ζ-potential measurement confirm surface modification due to hydrogen/nitrogen plasma treatment. An increase in non-diamond carbon in the initial layers of diamond grown on pretreated AlN is seen by Raman spectroscopy. The presence of non-diamond carbon has minimal effect on the thermal barrier resistance. The surfaces studied with X-ray photoelectron spectroscopy revealed a clear distinction between pretreated and untreated samples. The surface aluminum goes from a nitrogen-rich environment to an oxygen-rich environment after pretreatment. A clean interface between diamond and AlN is seen by cross-sectional transmission electron microscopy.

Author Correction: Superconducting Diamond on Silicon Nitride for Device Applications.

A correction to this article has been published and is linked from the HTML and PDF versions of this paper. The error has not been fixed in the paper.

Superconducting boron doped nanocrystalline diamond on boron nitride ceramics.

In this work we have demonstrated the growth of nanocrystalline diamond on boron nitride ceramic. We measured the zeta potential of the ceramics to select the diamond seeds. Diamond was then grown on the seeded ceramics using a microwave chemical vapour deposition system. A clear difference was found between the samples which were seeded with nanodiamond and the ones not seeded before growth. Raman spectroscopy confirmed the excellent quality of the diamond film. Dielectric measurements showed an increase in the dielectric constant of the material after diamond growth. The diamond was also doped with boron to make it superconducting. The film had a transition temperature close to 3.4 K. Similar strategies can be applied for the growth of diamond on other types of ceramics.

Superconducting Diamond on Silicon Nitride for Device Applications.

Chemical vapour deposition (CVD) grown nanocrystalline diamond is an attractive material for the fabrication of devices. For some device architectures, optimisation of its growth on silicon nitride is essential. Here, the effects of three pre-growth surface treatments, often employed as cleaning methods, were investigated. Such treatments provide control over the surface charge of the silicon nitride substrate through modification of the surface functionality, allowing for the optimisation of electrostatic diamond seeding densities. Zeta potential measurements and X-ray photoelectron spectroscopy (XPS) were used to analyse the silicon nitride surface following each treatment. Exposing silicon nitride to an oxygen plasma offered optimal surface conditions for the electrostatic self-assembly of a hydrogen-terminated diamond nanoparticle monolayer. The subsequent growth of boron-doped nanocrystalline diamond thin films on modified silicon nitride, under CVD conditions, produced coalesced films for oxygen plasma and solvent treatments, whilst pin-holing of the diamond film was observed following RCA-1 treatment. The sharpest superconducting transition was observed for diamond grown on oxygen plasma treated silicon nitride, demonstrating it to be of the least structural disorder. Modifications to the substrate surface optimise the seeding and growth processes for the fabrication of diamond on silicon nitride devices.

Air-clad suspended nanocrystalline diamond ridge waveguides.

A hybrid group IV ridge waveguide platform is demonstrated, with potential application across the optical spectrum from ultraviolet to the far infrared wavelengths. The waveguides are fabricated by partial etching of sub-micron ridges in a nanocrystalline diamond thin film grown on top of a silicon wafer. To create vertical confinement, the diamond film is locally undercut by exposing the chip to an isotropic fluorine plasma etch via etch holes surrounding the waveguides, resulting in a mechanically stable suspended air-clad waveguide platform. Optical characterization of the waveguides at 1550 nm yields an average optical loss of 4.67 ± 0.47 dB/mm. Further improvement to the fabrication process is expected to significantly reduce this waveguide loss.

Production of Metal-Free Diamond Nanoparticles.

In this paper, the controlled production of high-quality metal-free diamond nanoparticles is demonstrated. Milling with tempered steel is shown to leave behind iron oxide contamination which is difficult to remove. Milling with SiN alleviates this issue but generates more nondiamond carbon. Thus, the choice of milling materials is critically determined by the acceptable contaminants in the ultimate application. The removal of metal impurities, present in all commercially available nanoparticles, will open new possibilities toward the production of customized diamond nanoparticles, covering the most demanding quantum applications.

Effect of slurry composition on the chemical mechanical polishing of thin diamond films.

Nanocrystalline diamond (NCD) thin films grown by chemical vapour deposition have an intrinsic surface roughness, which hinders the development and performance of the films' various applications. Traditional methods of diamond polishing are not effective on NCD thin films. Films either shatter due to the combination of wafer bow and high mechanical pressures or produce uneven surfaces, which has led to the adaptation of the chemical mechanical polishing (CMP) technique for NCD films. This process is poorly understood and in need of optimisation. To compare the effect of slurry composition and pH upon polishing rates, a series of NCD thin films have been polished for three hours using a Logitech Ltd. Tribo CMP System in conjunction with a polyester/polyurethane polishing cloth and six different slurries. The reduction in surface roughness was measured hourly using an atomic force microscope. The final surface chemistry was examined using X-ray photoelectron spectroscopy and a scanning electron microscope. It was found that of all the various properties of the slurries, including pH and composition, the particle size was the determining factor for the polishing rate. The smaller particles polishing at a greater rate than the larger ones.

Positive zeta potential of nanodiamonds.

In this paper, the origin of positive zeta potential exhibited by nanodiamond particles is explained. Positive zeta potentials in nano-structured carbons can be explained by the presence of graphitic planes at the surface, which leave oxygen-free Lewis sites and so promotes the suppression of acidic functional groups. Electron Microscopy and Raman Spectroscopy have been used to show that positive zeta potential of nanodiamond is only exhibited in the presence of sp2 carbon at the surface.

Superconductivity in planarised nanocrystalline diamond films.

Chemical vapour deposition (CVD) grown boron-doped nanocrystalline diamond (B-NCD) is an attractive material for the fabrication of high frequency superconducting nanoelectromechanical systems (NEMS) due to its high Young's modulus. The as-grown films have a surface roughness that increases with film thickness due to the columnar growth mechanism. To reduce intrinsic losses in B-NCD NEMS it is crucial to correct for this surface roughness by polishing. In this paper, in contrast to conventional polishing, it is demonstrated that the root-mean-square (RMS) roughness of a 520 nm thick B-NCD film can be reduced by chemical mechanical polishing (CMP) from 44.0 nm to 1.5 nm in 14 hours without damaging the sample or introducing significant changes to the superconducting transition temperature, [Formula: see text], thus enabling the use of B-NCD films in the fabrication of high quality superconducting NEMS.

Spectroscopic Ellipsometry of Nanocrystalline Diamond Film Growth.

With the retention of many of the unrivaled properties of bulk diamond but in thin-film form, nanocrystalline diamond (NCD) has applications ranging from micro-/nano-electromechanical systems to tribological coatings. However, with Young's modulus, transparency, and thermal conductivity of films all dependent on the grain size and nondiamond content, compositional and structural analysis of the initial stages of diamond growth is required to optimize growth. Spectroscopic ellipsometry (SE) has therefore been applied to the characterization of 25-75 nm thick NCD samples atop nanodiamond-seeded silicon with a clear distinction between the nucleation and bulk growth regimes discernable. The resulting presence of an interfacial carbide and peak in nondiamond carbon content upon coalescence is correlated with Raman spectroscopy, whereas the surface roughness and microstructure are in accordance with values provided by atomic force microscopy. As such, SE is demonstrated to be a powerful technique for the characterization of the initial stages of growth and hence the optimization of seeding and nucleation within films to yield high-quality NCD.

Surface Zeta Potential and Diamond Seeding on Gallium Nitride Films.

The measurement of ζ potential of Ga-face and N-face gallium nitride has been carried out as a function of pH. Both of the faces show negative ζ potential in the pH range 5.5-9. The Ga-face has an isoelectric point at pH 5.5. The N-face shows a more negative ζ potential due to larger concentration of adsorbed oxygen. The ζ potential data clearly showed that H-terminated diamond seed solution at pH 8 will be optimal for the self-assembly of a monolayer of diamond nanoparticles on the GaN surface. The subsequent growth of thin diamond films on GaN seeded with H-terminated diamond seeds produced fully coalesced films, confirming a seeding density in excess of 1011 cm-2. This technique removes the requirement for a low thermal conduction seeding layer like silicon nitride on GaN.

Chemical Nucleation of Diamond Films.

With the large differences in surface energy between film and substrate in combination with the low sticking coefficient of hydrocarbon radicals, nanocrystalline diamond growth on foreign substrates typically results in poor nucleation densities. A seeding technique is therefore required to realize pinhole-free and thin coalesced films. In this work, a chemical nucleation method for growth of diamond on nondiamond substrates based on 2,2-divinyladamantane is shown. After treating with the carbon-containing DVA, the chemically treated wafers were exposed to low-power-density plasma, known as the incubation phase, to facilitate the formation of diamond nucleation sites followed by a high-power-density growth regime to produce coalesced films. The resulting films demonstrate high crystallinity, whereas the Raman spectra suggest high-quality diamond with low sp2 content.

Silica based polishing of {100} and {111} single crystal diamond.

Diamond is one of the hardest and most difficult to polish materials. In this paper, the polishing of {111} and {100} single crystal diamond surfaces by standard chemical mechanical polishing, as used in the silicon industry, is demonstrated. A Logitech Tribo Chemical Mechanical Polishing system with Logitech SF1 Syton and a polyurethane/polyester polishing pad was used. A reduction in roughness from 0.92 to 0.23 nm root mean square and 0.31 to 0.09 nm rms for {100} and {111} samples respectively was observed.

Observation of nonlinear dissipation in piezoresistive diamond nanomechanical resonators by heterodyne down-mixing.

We report the observation of nonlinear dissipation in diamond nanomechanical resonators measured by an ultrasensitive heterodyne down-mixing piezoresistive detection technique. The combination of a hybrid structure as well as symmetry breaking clamps enables sensitive piezoresistive detection of multiple orthogonal modes in a diamond resonator over a wide frequency and temperature range. Using this detection method, we observe the transition from purely linear dissipation at room temperature to strongly nonlinear dissipation at cryogenic temperatures. At high drive powers and below liquid nitrogen temperatures, the resonant structure dynamics follows the Pol-Duffing equation of motion. Instead of using the broadening of the full width at half-maximum, we propose a nonlinear dissipation backbone curve as a method to characterize the strength of nonlinear dissipation in devices with a nonlinear spring constant.

The diamond superconducting quantum interference device.

Diamond is an electrical insulator in its natural form. However, when doped with boron above a critical level (∼0.25 atom %) it can be rendered superconducting at low temperatures with high critical fields. Here we present the realization of a micrometer-scale superconducting quantum interference device (µ-SQUID) made from nanocrystalline boron-doped diamond (BDD) films. Our results demonstrate that µ-SQUIDs made from superconducting diamond can be operated in magnetic fields as large as 4 T independent of the field direction. This is a decisive step toward the detection of quantum motion in a diamond-based nanomechanical oscillator.