A Study of the Radiation Tolerance and Timing Properties of 3D Diamond Detectors.

We present a study on the radiation tolerance and timing properties of 3D diamond detectors fabricated by laser engineering on synthetic Chemical Vapor Deposited (CVD) plates. We evaluated the radiation hardness of the sensors using Charge Collection Efficiency (CCE) measurements after neutron fluences up to 1016 n/cm2 (1 MeV equivalent.) The radiation tolerance is significantly higher when moving from standard planar architecture to 3D architecture and increases with the increasing density of the columnar electrodes. Also, the maximum applicable bias voltage before electric breakdown increases significantly after high fluence irradiation, possibly due to the passivation of defects. The experimental analysis allowed us to predict the performance of the devices at higher fluence levels, well in the range of 1016 n/cm2. We summarize the recent results on the time resolution measurements of our test sensors after optimization of the laser fabrication process and outline future activity in developing pixel tracking systems for high luminosity particle physics experiments.

A single-crystal diamond X-ray pixel detector with embedded graphitic electrodes.

The first experimental results from a new transmissive diagnostic instrument for synchrotron X-ray beamlines are presented. The instrument utilizes a single-crystal chemical-vapour-deposition diamond plate as the detector material, with graphitic wires embedded within the bulk diamond acting as electrodes. The resulting instrument is an all-carbon transmissive X-ray imaging detector. Within the instrument's transmissive aperture there is no surface metallization that could absorb X-rays, and no surface structures that could be damaged by exposure to synchrotron X-ray beams. The graphitic electrodes are fabricated in situ within the bulk diamond using a laser-writing technique. Two separate arrays of parallel graphitic wires are fabricated, running parallel to the diamond surface and perpendicular to each other, at two different depths within the diamond. One array of wires has a modulated bias voltage applied; the perpendicular array is a series of readout electrodes. X-rays passing through the detector generate charge carriers within the bulk diamond through photoionization, and these charge carriers travel to the nearest readout electrode under the influence of the modulated electrical bias. Each of the crossing points between perpendicular wires acts as an individual pixel. The simultaneous read-out of all pixels is achieved using a lock-in technique. The parallel wires within each array are separated by 50 µm, determining the pixel pitch. Readout is obtained at 100 Hz, and the resolution of the X-ray beam position measurement is 600 nm for a 180 µm size beam.

Fast beam monitor diamond-based devices for VUV and X-ray synchrotron radiation applications.

The improved performance of third-generation light sources and the advent of next-generation synchrotron radiation facilities require the use of extremely precise monitoring of the main photon-beam parameters, such as position, absolute and relative intensity, and temporal structure. These parameters, and associated real-time feedbacks, are fundamental at the beamline control level and at the machine control level, to improve the stability of the photon beams and to provide bunch-to-bunch quantitative information. Fast response time, high radiation hardness and visible-blind response are main features of photon-beam monitors for VUV and X-ray synchrotron radiation beamlines; hence diamond-based detectors are outstanding candidates. Here, results are presented of an extensive measurement campaign aiming at optimizing the capabilities of diamond detectors to discern time structures below the 100 ps timescale. A custom-built device has been fabricated and tested at the Italian Synchrotron Radiation Laboratory Elettra in Trieste. The results obtained show that diamond is an excellent material for ultra-fast photon pulses with picosecond time resolution; finally the possibilities for application at free-electron laser sources are discussed.

Characterizing transmissive diamond gratings as beam splitters for the hard X-ray single-shot spectrometer of the European XFEL.

The European X-ray Free Electron Laser (EuXFEL) offers intense, coherent femtosecond pulses, resulting in characteristic peak brilliance values a billion times higher than that of conventional synchrotron facilities. Such pulses result in extreme peak radiation levels of the order of terawatts cm-2 for any optical component in the beam and can exceed the ablation threshold of many materials. Diamond is considered the optimal material for such applications due to its high thermal conductivity (2052 W mK-1 at 300 K) and low absorption for hard X-rays. Grating structures were fabricated on free-standing CVD diamond of 10 µm thickness with 500 µm silicon substrate support. The grating structures were produced by electron-beam lithography at the Laboratory for Micro- and Nanotechnology, Paul Scherrer Institut, Switzerland. The grating lines were etched to a depth of 1.2 µm, resulting in an aspect ratio of 16. The characterization measurements with X-rays were performed on transmissive diamond gratings of 150 nm pitch at the P10 beamline of PETRA III, DESY. In this paper, the gratings are briefly described, and a measured diffraction efficiency of 0.75% at 6 keV in the first-order diffraction is shown; the variation of the diffraction efficiency across the grating surface is presented.

A Solar-Blind UV Detector Based on Graphene-Microcrystalline Diamond Heterojunctions.

An ultraviolet detector is demonstrated through a whole-wafer, thin diamond film transfer process to realize the heterojunction between graphene and microcrystalline diamond (MCD). Conventional direct transfer processes fail to deposit graphene onto the top surface of the MCD film. However, it is found that the 2 µm thick MCD diamond film can be easily peeled off from the growth silicon substrate to expose its smooth backside for the graphene transfer process for high-quality graphene/MCD heterojunctions. A vertical graphene/MCD/metal structure is constructed as the photodiode device using graphene as the transparent top electrode for solar-blind ultraviolet sensing with high responsivity and gain factor. As such, this material system and device architecture could serve as the platform for next-generation optoelectronic systems.

Ultra-thin optical grade scCVD diamond as X-ray beam position monitor.

Results of measurements made at the SIRIUS beamline of the SOLEIL synchrotron for a new X-ray beam position monitor based on a super-thin single crystal of diamond grown by chemical vapor deposition (CVD) are presented. This detector is a quadrant electrode design processed on a 3 µm-thick membrane obtained by argon-oxygen plasma etching the central area of a CVD-grown diamond plate of 60 µm thickness. The membrane transmits more than 50% of the incident 1.3 keV energy X-ray beam. The diamond plate was of moderate purity (∼1 p.p.m. nitrogen), but the X-ray beam induced current (XBIC) measurements nevertheless showed a photo-charge collection efficiency approaching 100% for an electric field of 2 V µm(-1), corresponding to an applied bias voltage of only 6 V. XBIC mapping of the membrane showed an inhomogeneity of more than 10% across the membrane, corresponding to the measured variation in the thickness of the diamond plate before the plasma etching process. The measured XBIC signal-to-dark-current ratio of the device was greater than 10(5), and the X-ray beam position resolution of the device was better than a micrometer for a 1 kHz sampling rate.

Magnetic Resonance Study of Bulky CVD Diamond Disc.

Diamonds produced using chemical vapor deposition (CVD) have found many applications in various fields of science and technology. Many applications involve polycrystalline CVD diamond films of micron thicknesses. However, a variety of optical, thermal, mechanical, and radiation sensing applications require more bulky CVD diamond samples. We report the results of a magnetic resonance and structural study of a thick, sizable polycrystalline CVD diamond disc, both as-prepared and treated with e-beam irradiation/high-temperature annealing, as well as gamma irradiation. The combination of various magnetic resonance techniques reveals and enables the attribution of a plentiful collection of paramagnetic defects of doublet and triplet spin origin. Analysis of spectra, electron, and nuclear spin relaxation, as well as nuclear spin diffusion, supports the conclusion of significant macro- and micro-inhomogeneities in the distribution of nitrogen-related defects.

A Highly Versatile X-ray and Electron Beam Diamond Dosimeter for Radiation Therapy and Protection.

Radiotherapy is now recognized as a pillar in the fight against cancer. Two different types are currently used in clinical practice: (1) external beam radiotherapy, using high-energy X-rays or electron beams, both in the MeV-range, and (2) intraoperative radiotherapy, using low-energy X-rays (up to 50 keV) and MeV-range electron beams. Versatile detectors able to measure the radiation dose independently from the radiation nature and energy are therefore extremely appealing to medical physicists. In this work, a dosimeter based on a high-quality single-crystal synthetic diamond sample was designed, fabricated and characterized under low-energy X-rays, as well as under high-energy pulsed X-rays and electron beams, demonstrating excellent linearity with radiation dose and dose-rate. Detector sensitivity was measured to be 0.299 ± 0.002 µC/Gy under 6 MeV X-ray photons, and 0.298 ± 0.004 µC/Gy under 6 MeV electrons, highlighting that the response of the diamond dosimeter is independent of the radiation nature. Moreover, in the case of low-energy X-rays, an extremely low limit of detection (23 nGy/s) was evaluated, pointing out the suitability of the device to radiation protection dosimetry.

Ion Microprobe Study of the Polarization Quenching Techniques in Single Crystal Diamond Radiation Detectors.

Synthetic single crystal diamond grown using the chemical vapor deposition technique constitutes an extraordinary candidate material for monitoring radiation in extreme environments. However, under certain conditions, a progressive creation of space charge regions within the crystal can lead to the deterioration of charge collection efficiency. This phenomenon is called polarization and represents one of the major drawbacks associated with using this type of device. In this study, we explore different techniques to mitigate the degradation of signal due to polarization. For this purpose, two different diamond detectors are characterized by the ion beam-induced charge technique using a nuclear microprobe, which utilizes MeV energy ions of different penetration depths to probe charge transport in the detectors. The effect of polarization is analyzed by turning off the bias applied to the detector during continuous or discontinuous irradiation, and also by alternating bias polarity. In addition, the beneficial influence of temperature for reducing the effect of polarization is also observed. Finally, the effect of illuminating the detector with light is also measured. Our experimental results indicate that heating a detector or turning off the bias, and then applying it during continuous irradiation can be used as satisfactory methods for recovering the CCE value close to that of a prepolarized state. In damaged regions, illumination with white light can be used as a standard method to suppress the strength of polarization induced by holes.

Effect of Substrate Pretreatment Process on the Cutting Performance of Diamond-Coated PCB Micro-Milling Tools.

Diamond coatings were deposited on PCB (printed circuit board) carbide milling tool substrates under various schemes of acid and alkali pretreatment by hot filament chemical vapor deposition (HFCVD). Scanning electron microscopy and X-ray coating analysis were used to examine the surface morphology of the milling tools and the impact of de-cobalt from the substrate surface after pretreatment. Milling experiments were carried out to study the cutting performance of diamond-coated PCB micro-milling tools under various pretreatment processes. The results show that abrasive wear, coating flaking, and cutting-edge chipping are the main failure forms of coated PCB milling tools. The substrate pretreatment process with 20 min of alkali etching followed by 20 s of acid etching allows the diamond-coated micro-milling tools to produce the best film-substrate adhesion and substrate strength. These milling tools also have the longest service lives and are suitable for the high-speed cutting processing of PCB.

CVD Nanocrystalline Diamond Film Doped with Eu.

This paper submits experimental results of a study directed towards the formation of Eu ions' luminescent centers in CVD diamond films. A new approach is based on use of diamond nanoparticles with a surface modified with Eu ions for seeding at CVD growth. Nanocrystalline diamond films (NCD) doped with Eu have been grown from the gas phase on silicon substrates by microwave plasma-assisted CVD at a frequency of 2.45 GHz. The photoluminescence spectra clearly show several electronic transitions of the Eu3+ ions, which confirm the incorporation of Eu ions into the NCD film.

Experimental Study on Fabrication of CVD Diamond Micro Milling Tool by Picosecond Pulsed Laser.

Because of the many advantages of high-precision micromachining, picosecond pulsed lasers (PSPLs) can be used to process chemical-vapor-deposited diamonds (CVD-D). With the appropriate PSPL manufacturing technique, sharp and smooth edges of CVD-D micro tools can be generated. In this study, a PSPL is used to cut CVD-D. To optimize PSPL cutting, the effects of its parameters including fluence, pulse pitch, and wavelength on the cutting results were investigated. The results showed that the wavelength had the greatest impact on the sharpness of CVD-D. With PSPL cutting, sharp cutting edges, and smooth fabricated surfaces of the CVD-D, micro tools were achieved. Finally, the fabrication of CVD-D micro milling tools and micro milling experiments were also demonstrated.

Boron Doped Diamond for Real-Time Wireless Cutting Temperature Monitoring of Diamond Coated Carbide Tools.

Among the unique opportunities and developments that are currently being triggered by the fourth industrial revolution, developments in cutting tools have been following the trend of an ever more holistic control of manufacturing processes. Sustainable manufacturing is at the forefront of tools development, encompassing environmental, economic, and technological goals. The integrated use of sensors, data processing, and smart algorithms for fast optimization or real time adjustment of cutting processes can lead to a significant impact on productivity and energy uptake, as well as less usage of cutting fluids. Diamond is the material of choice for machining of non-ferrous alloys, composites, and ultrahard materials. While the extreme hardness, thermal conductivity, and wear resistance of CVD diamond coatings are well-known, these also exhibit highly auspicious sensing properties through doping with boron and other elements. The present study focuses on the thermal response of boron-doped diamond (BDD) coatings. BDD coatings have been shown to have a negative temperature coefficient (NTC). Several approaches have been adopted for monitoring cutting temperature, including thin film thermocouples and infrared thermography. Although these are good solutions, they can be costly and become impractical for certain finishing cutting operations, tool geometries such as rotary tools, as well as during material removal in intricate spaces. In the scope of this study, diamond/WC-Co substrates were coated with BDD by hot filament chemical vapor deposition (HFCVD). Scanning electron microscopy, Raman spectroscopy, and the van der Pauw method were used for morphological, structural, and electrical characterization, respectively. The thermal response of the thin diamond thermistors was characterized in the temperature interval of 20-400 °C. Compared to state-of-the-art temperature monitoring solutions, this is a one-step approach that improves the wear properties and heat dissipation of carbide tools while providing real-time and in-situ temperature monitoring.

Fabry-Perot Pressure Sensors Based on Polycrystalline Diamond Membranes.

Pressure sensors based on diamond membranes were designed and tested for gas pressure measurement up to 6.8 MPa. The diamond film (2" diameter, 6 µm thickness)-grown by microwave plasma chemical vapor deposition on a silicon substrate-was a starting material to produce an array of membranes with different diameters in the 130-400 µm range, in order to optimize the sensor performance. Each 5 mm × 5 mm sensing element was obtained by subsequent silicon slicing. The fixed film thickness, full-scale pressure range, and sensor sensitivity were established by a proper design of the diameter of diamond membrane which represents the sensing element for differential pressure measurement. The pressure-induced deflection of the membrane was optically measured using a Fabry-Pérot interferometer formed by a single mode optical fiber front surface and the deflecting diamond film surface. The optical response of the system was numerically simulated using geometry and the elastic properties of the diamond diaphragm, and was compared with the experiments. Depending on the diamond membrane's diameter, the fabricated sensors displayed a good modulation depth of response over different full-scale ranges, from 3 to 300 bar. In view of the excellent mechanical, thermal, and chemical properties of diamond, such pressure sensors could be useful for performance in a harsh environment.

Experimental Study on High-Speed Milling of SiCf/SiC Composites with PCD and CVD Diamond Tools.

Silicon carbide fiber reinforced silicon carbide ceramic matrix composite (SiCf/SiC composite) is characterized by a high strength-to-density ratio, high hardness, and high temperature resistance. However, due to the brittleness of the matrix material and the anisotropy of the reinforcing phase, it is a huge challenge for machining of the material. The milling method has advantages of a high material removal rate and applicability to complex surface geometry. However, no published literature on milling of SiCf/SiC composite has been found up to now. In this paper, high-speed milling of SiCf/SiC composites was carried out under dry conditions and cryogenic cooling using liquid nitrogen, respectively. Polycrystalline diamond (PCD) and chemical vapor deposition (CVD) diamond cutting tools were used for the milling work. The cutting performance of the two kinds of tools in high-speed milling of SiCf/SiC composites was studied. Tool failure modes and mechanisms were analyzed. The effects of the cooling approach on tool wear and machined surface quality were also investigated. The experimental results showed that under identical cutting parameters and cooling approaches, the PCD tool yielded better cutting performance in terms of a longer tool life and better surface quality than that of the CVD diamond tool. In dry machining, the failure modes of the CVD diamond tool were a large area of spalling on the rake face, edge chipping and severe tool nose fracture, whereas for the PCD tool, only a small area of spalling around the tool nose took place. Compared to the dry machining, the wear magnitudes of both PCD and CVD diamond tools were decreased in cryogenic machining. Additionally, the surface quality also showed significant improvements. This study indicates that the PCD tool is highly suitable for machining of SiCf/SiC composite, and that the cryogenic method can improve machining efficiency and surface quality.

Multilayer Diamond Coatings Applied to Micro-End-Milling of Cemented Carbide.

Cobalt-cemented carbide micro-end mills were coated with diamond grown by chemical vapor deposition (CVD), with the purpose of micro-machining cemented carbides. The diamond coatings were designed with a multilayer architecture, alternating between sub-microcrystalline and nanocrystalline diamond layers. The structure of the coatings was studied by transmission electron microscopy. High adhesion to the chemically pre-treated WC-7Co tool substrates was observed by Rockwell C indentation, with the diamond coatings withstanding a critical load of 1250 N. The coated tools were tested for micro-end-milling of WC-15Co under air-cooling conditions, being able to cut more than 6500 m over a period of 120 min, after which a flank wear of 47.8 µm was attained. The machining performance and wear behavior of the micro-cutters was studied by scanning electron microscopy and energy-dispersive X-ray spectroscopy. Crystallographic analysis through cross-sectional selected area electron diffraction patterns, along with characterization in dark-field and HRTEM modes, provided a possible correlation between interfacial stress relaxation and wear properties of the coatings. Overall, this work demonstrates that high adhesion of diamond coatings can be achieved by proper combination of chemical attack and coating architecture. By preventing catastrophic delamination, multilayer CVD diamond coatings are central towards the enhancement of the wear properties and mechanical robustness of carbide tools used for micro-machining of ultra-hard materials.

A Diamond-Based Dose-per-Pulse X-ray Detector for Radiation Therapy.

One of the goals of modern dynamic radiotherapy treatments is to deliver high-dose values in the shortest irradiation time possible. In such a context, fast X-ray detectors and reliable front-end readout electronics for beam diagnostics are crucial to meet the necessary quality assurance requirements of care plans. This work describes a diamond-based detection system able to acquire and process the dose delivered by every single pulse sourced by a linear accelerator (LINAC) generating 6-MV X-ray beams. The proposed system is able to measure the intensity of X-ray pulses in a limited integration period around each pulse, thus reducing the inaccuracy induced by unnecessarily long acquisition times. Detector sensitivity under 6-MV X-photons in the 0.1-10 Gy dose range was measured to be 302.2 nC/Gy at a bias voltage of 10 V. Pulse-by-pulse measurements returned a charge-per-pulse value of 84.68 pC, in excellent agreement with the value estimated (but not directly measured) with a commercial electrometer operating in a continuous integration mode. Significantly, by intrinsically holding the acquired signal, the proposed system enables signal processing even in the millisecond period between two consecutive pulses, thus allowing for effective real-time dose-per-pulse monitoring.

The Hydrogenation Impact on Electronic Properties of p-Diamond/n-Si Heterojunctions.

The undoped polycrystalline diamond films (PDFs) have been deposited on n-type silicon (Si) by Hot Filament Chemical Vapor Deposition (HF CVD) technique. The reaction gases are a mixture of methane and hydrogen. The obtained PDFs were characterized by scanning electron microscopy (SEM) and Raman spectroscopy which, in addition to the diamond phase, also confirms the presence of sp2 hybridized carbon bonds. As-grown CVD diamond layers are hydrogen terminated and show p-type conductivity. The effect of the level of hydrogenation on the electrical properties of p-diamond/n-Si heterojunctions has been investigated by temperature dependent current-voltage (J-V/T) characteristics. The obtained results suggest that the energy distribution of interface states at the grain boundary (GB) subjected to hydrogenation becomes shallower, and the hole capture cross-section can be reduced. Hydrogenation can lead to a significant reduction of the GB potential barrier. These results can be interesting from the point of view of hydrogen passivation of GBs in microelectronics.

Seed Dibbling Method for the Growth of High-Quality Diamond on GaN.

The integration of diamond and GaN has been highly pursued for thermal management purposes as well as combining their exceptional complementary properties for power electronics applications and novel semiconductor heterostructures. However, the growth of diamond-on-GaN is challenging due to the high lattice and thermal expansion mismatches. The weak adhesion of diamond to GaN and high residual stresses after the deposition often result in the diamond film delamination or development of cracks, which hinder the subsequent device fabrication. Here, we present a new seed dibbling method for seeding and growing high-quality diamond films on foreign substrates, in particular on cost-effective GaN-on-Si, with significantly improved adhesion. Diamond films grown conformally on patterned GaN-on-Si presented high quality with significantly larger grains and a 95% sp3/sp2 ratio, excellent interface between diamond and GaN, and lower residual stresses (as low as 0.2 GPa) compared to conventional methods. In addition, the method provided excellent adhesion, enabling a reliable polishing of the as-grown diamond films on GaN on Si without any delamination, resulting in smooth diamond-on-GaN substrates with subnanometer root-mean-square roughness. Diamond layers deposited via seed dibbling resulted in a 2-fold improvement in the effective thermal conductivity for GaN-on-Si with only a 20 µm thick diamond layer. This method opens many new possibilities for the development of high-performance power electronic devices and integrated devices with excellent thermal management based on a diamond-on-GaN platform. In addition, this technique could be extended to other substrates to combine the outstanding properties of diamond with other kinds of devices.

Integration of GaN and Diamond Using Epitaxial Lateral Overgrowth.

Growth of single-crystalline GaN on polycrystalline diamond is reported for the first time. The structure was achieved using a combined process including selective diamond growth on GaN/Si wafers using hot filament chemical vapor deposition (CVD) and epitaxial lateral overgrowth of GaN on the window region between then above the diamond stripes via metal organic CVD. Optimization of the growth was performed by varying the ammonia to trimethylgallium mole ratio (V/III), chamber pressure, and temperature in the range of 8000-1330, 40-200 Torr, and 975-1030 °C, respectively. A lower pressure, higher V/III ratio, higher temperature, and GaN window mask openings along [11̅00] resulted in enhanced lateral growth of GaN. Complete lateral coverage and coalescence of GaN were achieved over a [11̅00]-oriented 5 µm-wide GaN window between 5 µm diamond stripes when using V/III = 7880, P = 100 Torr, and T = 1030 °C. The crystalline quality of overgrown GaN was confirmed using cross-sectional scanning electron microscopy, high-resolution X-ray diffraction, micro-Raman spectroscopy, transmission electron microscopy, and selective-area electron diffraction.