Response of chemical vapor deposition diamond detectors to X-ray

The outstanding properties of diamond, such as radiation hardness, high carrier mobility, high band gap and breakdown field, distinguish it as a good candidate for radiation detectors. The detector's performance is strongly limited by the concentration of defects (grain boundaries and/or impurities) in chemical vapor deposition (CVD) diamond. We report the response of free-standing CVD diamond with a thickness of 300 μm and area of 2×2 cm², synthesized by a hot filament chemical vapor deposition (HFCVD) technique, to 5.9 keV X-ray radiation from a ⁵⁵Fe source. The linear I-V characteristics indicate that CVD diamond has good ohmic contacts. This detector also shows good results such as dark-current of 10⁻⁸ A, photocurrent of 10⁻⁶ A, energy resolution <0.4%, and a high ratio of signal to noise.     

Characterization of phosphorus-doped homoepitaxial (1 0 0) diamond films grown using high-power-density MWPCVD method with a conventional quartz-tube chamber

Phosphorus-doped n-type homoepitaxial diamond films have been successfully grown at high substrate temperatures (>1000 °C) on high-pressure/high-temperature-synthesized type-Ib single-crystalline diamond (1 0 0) substrates, by using a conventional microwave plasma chemical-vapor-deposition (CVD) system with high power densities. The deposition system employed in this work had an easily exchangeable 36 mm inner-diameter quartz-tube growth chamber. The homoepitaxial diamond films thus grown were characterized by means of Hall-effect measurements with an AC magnetic field, atomic force microscope observations and secondary ion mass spectrometry techniques. The dependences of the substrate temperature (≤1300 °C) and the P/C ratio in the source gas (≤9900 ppm) on the specimen features were investigated. The optimum substrate temperature deduced was ≈1160 °C, which was also applicable to the CVD growth of undoped homoepitaxial diamond layers. The n-type conductions with an activation energy ≈0.6 eV were observed for the specimens with amounts of the P atoms incorporated to ≈1.5 × 10¹⁸ cm⁻³ whereas the doping efficiencies changed from ≈0.06% to ≈0.92% with the growth condition. Possible origins for these results are discussed in relation to the growth mechanism.     

Optical and electrical properties of different oriented CVD diamond films

Due to different oriented diamond films having different properties, in this paper optical and electrical properties of different oriented diamond films have been investigated. The measured results indicate diamond films are of high quality and the properties of the (0 0 1)-oriented diamond film are better than those of the (1 1 1)-oriented one. Refractive index and extinction coefficient of (0 0 1)-oriented diamond film in the wavelength range of 2.5-12.5 μm is 2.391 and in the order of 10⁻⁵, respectively. And for the (1 1 1)-oriented one it is 2.375 and in the order of 10⁻⁴. The dark current of the (0 0 1)-oriented diamond film is 33.7 nA under an applied electric field of 100 kV/cm. The resistivity of the (0 0 1)-oriented diamond film obtained is about 2.33 × 10¹⁰ Ω cm. The current of (0 0 1)-oriented diamond film is almost no change with the time testing.     

Analysis of the current-transport mechanism across a CVD diamond/silicon interface

This work presents a study on the mechanism of injection and charge transport through a CVD diamond/n⁺-Si interface. The current-voltage-temperature characteristics of CVD diamond/silicon heterojunctions measured in the temperature range 119-400 K have been interpreted according to thermionic theory and thermionic field-emission theory. This junction shows deviations from the ideal thermionic theory current model, suggesting the presence of surface states, thin-layer depletion and/or non-homogeneity in the diamond/silicon interface. The T₀ anomaly has been used to explain the behaviour of the ideality factor with temperature. At very low temperatures tunnelling may occur because the E₀₀ values for these junctions are close to the value expected by thermionic field-emission theory. The usual activation-energy plot deviates from linearity at low temperatures. This deviation has been corrected supposing a ln(J_S/T²) versus 10³/nT plot. Under these conditions the Richardson constant is found to be 0.819 A cm⁻² K⁻², which is close to the theoretical value of 1.2 A cm⁻² K⁻². Field-emission device is a promising application for diamond/silicon structure.     

Surface morphology, growth rate and quality of diamond films synthesized in hot filament CVD system under various methane concentrations

Hot filament chemical vapor deposition (CVD) technique has been used to deposit diamond films on silicon substrate. In the present study, diamond films were grown at various vol.% CH₄ in H₂ from 0.5% to 3.5%, at substrate temperature and pressure of 850 °C and 80 torr, respectively. Scanning electron microscopy, X-ray diffraction and Raman spectroscopy were employed to analyze the properties of deposited films. The formation of methyl radicals as a function of vol.% CH₄ not only changes film morphology but also increase film growth rate. At low, intermediate and high vol.% CH₄, cluster, faceted cubes and pyramidal features growth, were dominant. By increasing vol.% CH₄ from 0.5% to 3.5%, as the growth rate improved from ∼0.25 μm/h to ∼2.0 μm/h. Raman studies features revealed high purity diamond films at intermediate range of vol.% CH₄ and grain density increased by increasing CH₄ concentration. The present study represents experimentally surface morphology, growth rate and quality of diamond films grown in hot filament CVD system at various CH₄ concentrations.     

An optical emission spectroscopy study of the plasma generated in the DC HF CVD nucleation of diamond

Optical emission spectroscopy (OES) was used to study the plasma generated by the activation of the gas phase CH₄ + H₂ both by hot filaments and by a plasma discharge (DC HF CVD) during the nucleation of CVD diamond. The effects of nucleation parameters, such as methane concentration and extraction potential, on the plasma chemistry near the surface were investigated. The density of the diamond nucleation and the quality of the diamond films were studied by scanning electron microscopy (SEM) and Raman scattering, respectively. The OES results showed that the methane concentration influenced strongly the intensity ratio of H_β-H_α implying an increase of electron mean energy, as well as CH, CH⁺, C₂. A correlation between the relative increase of CH⁺ and the diamond nucleation density was found, conversely the increase of C₂ contributed to the introduction of defects in the diamond nuclei.     

Characteristic energy band values and electron attenuation length of a chemical-vapor-deposition diamond (0 0 1)2 × 1 surface

The characteristic energy band values such as the Fermi-level position with respect to valence band top for a boron-doped p-type hydrogen-terminated chemical-vapor-deposition (CVD) diamond (0 0 1)2 × 1 surface and for a clean CVD diamond (0 0 1)2 × 1 surface have been determined by a new method with an accuracy of ±0.02 eV. The electron attenuation length for the clean diamond (0 0 1)2 × 1 surface for the electron kinetic energy of C 1s X-ray photoemission peak by Mg Kα excitation is experimentally determined to be 2.1-2.2 nm. These values are compared and discussed with the previously reported experimental and simulation values.     

Field emission from nitrogen-implanted CVD diamond film grown on silicon wafer

Nitrogen was implanted into chemical vapor deposition (CVD) diamond films and the electron field emission properties of the nitrogenated diamond films were investigated. Nitrogen implantation was carried out using 10 keV in the dose range from 1×10¹⁶ to 5×10¹⁷ cm^-2 at room temperature. Raman and X-ray photoelectron spectroscopy measurements revealed that nitrogen implantation damaged the structure of the diamond film and promoted the formation of sp² C–C and sp² C–N bondings. Increasing the implantation dose could lower the threshold field of the emission of the diamond film from 18 V/m to 4 V/m. The effective work function of the nitrogen-implanted CVD diamond films was estimated to be in the range of 0.01–0.1 eV. The enhancement of field emission for nitrogen-implanted CVD diamond films was attributed to the increase of the sp² C bonds fraction and the formation of defect bands within the bulk diamond band gap induced by nitrogen implantation, which could alter the work function and elevate the Fermi level. Consequently, the energy barrier for electron tunneling was reduced.     

Effect of nanostructured AlN coatings on the oxidation-resistant properties of optical diamond films

Diamond film is an ultra-durable optical material with high thermal conductivity and good transmission in near-infrared and far-IR (8-14 μm) wavebands. CVD diamond is subjected to oxidation at temperature higher than 780 °C bared in air for 3 min, while it can be protected from oxidation for extended exposure in air at temperature up to 900 °C by a coating of aluminum nitride. Highly oriented AlN coatings were prepared for infrared windows on diamond films by reactive sputtering method and the average surface roughness (R_a) of the coatings was about 10 nm. The deposited films were characterized by X-ray diffraction (XRD) and atom force microscope (AFM). XRD confirmed the preferential orientation nature and AFM showed nanostructures. Optical properties of diamond films coated AlN thin film was investigated using infrared spectrum (IR) compared with that for as-grown diamond films.     

Monte Carlo simulations of multiplexed electronic grade CVD diamond for neutron detection

A novel and evolutionary multiplexing technique is introduced in this work where electronic grade single crystal chemical vapor deposition (CVD) diamond plates are multiplexed together in both a series and parallel configuration, sending electronic signals from each diamond plate to a single electronic acquisition system. Modeling of this novel multiplexing technique consisted of MCNPX simulations and significant post processing. The model developed allowed for the characterization of charge collection efficiency corrections to the location of charge creation to determine the effect of increasing detection medium size with respect to charge collection direction on the measured pulse height spectrum. This work was conducted to show that this technique is theoretically capable of replacing a single crystal diamond plate of similar size for use in neutron detection without the immediate need of advancing CVD diamond growth technologies. Further, this work indicates the expected pulse height evolution from a singular large single crystal diamond if such a crystal is produced in the future. The results of this work indicate that a 14.1 MeV neutron induced energy pulse of 8.4 MeV (due to the ¹²C(n,α_o)⁹Be reaction) in the pulse height spectrum has its energy resolution broadened by a factor of two to a total value of 0.225 percent for a multiplexed array with a thickness from 0.05 to 1 cm and an intrinsic detection efficiency of 25.4 percent for a 1 cm thick diamond crystal. It is also qualitatively discussed that the number of secondary neutron interactions with the diamond detector array may be about 5 percent. The results of this work indicate the capability of multiplexing diamond plates together for spectroscopic neutron detection with a combined intrinsic detection efficiency and energy resolution greater than any other diamond-based neutron detection system reported to date.     

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 10⁵, and the X‐ray beam position resolution of the device was better than a micrometer for a 1 kHz sampling rate.     

Growth and field emission properties of globe-like diamond microcrystalline-aggregate

The globe-like diamond microcrystalline-aggregates were fabricated by microwave plasma chemical vapor deposition (MPCVD) method. The ceramic with a Ti mental layer was used as substrate. The fabricated diamond was evaluated by Raman scattering spectroscopy, X-ray diffraction spectrum (XRD), and scanning electron microscope (SEM). The field emission properties were tested by using a diode structure in a vacuum. A phosphor-coated indium tin oxide (ITO) anode was used for observing and characterizing the field emission. It was found that the globe-like diamond microcrystalline-aggregates exhibited good electron emission properties. The turn-on field was only 0.55 V/μm, and emission current density as high as 11 mA/cm² was obtained under an applied field of 2.9 V/μm for the first operation. The growth mechanism and field emission properties of the globe-like diamond microcrystalline-aggregates are discussed relating to microstructure and electrical conductivity.     

Characterization of soft-X-ray detectors fabricated with high-quality CVD diamond thin films

We have characterized the performance of soft-X-ray detectors fabricated with undoped and B-doped homoepitaxial diamond layers of high quality which were grown on a commercially available type Ib (1 0 0) substrate by means of a high-power microwave-plasma chemical-vapor-deposition (CVD) method. The signal currents of the diamond-based detectors with thin TiN electrodes formed vertically (along the homoepitaxial growth direction) were measured at room temperature as a function of the applied voltage, V_a, for irradiations of 500-1200 eV soft-X-ray beams ranging from ≈6 × 10⁹ to ≈1 × 10¹¹ photons/s. The deduced apparent quantum efficiencies increased with the increasing V_a and reached to 2.5 × 10³ at V_a = 60 V. As expected from the device structure, the detector performance depended only very slightly on the applied magnetic field up to 10 T. The excellently high sensitivities attained for soft-X-ray photons are discussed in relation to carrier amplification mechanisms which invested the above diamond detectors.     

Characterization of diamond films deposited on Re substrate by magnetic field-assisted hot filament chemical vapor deposition

A periodically magnetic field (PMF) was used in a hot-filament chemical vapor deposited (HFCVD) for diamond growth on the rhenium substrate. The morphology, band structures and crystalline structure of the film were analyzed by the scanning electron microscopy (SEM), Raman spectroscopy and X-ray diffractometer (XRD), respectively. The results show that the thickness of the diamond film is about 2900 nm by 4 h deposition with magnetic field-assisted. There is no interlayer between diamond film and the rhenium substrate. The result shows that the turn on voltage of the sample is enhanced from 3.3 to 2.6 V/μm with the PMF. Also the total emission current density at 6.2 V/μm increased from 6.3 to 21.5 μA/cm².     

Ion-induced self-organized ripple patterns on graphite and diamond surfaces

In order to investigate the allotropic effect on ripple pattern formation, highly oriented pyrolytic graphite (HOPG) and single crystalline diamond were irradiated with 10-200 keV Xe⁺ at an incident angle of 60° with respective to the surface normal. The irradiation fluence was 2 × 10¹⁷ cm⁻² for all irradiations. Ripple patterns were observed on both HOPG and diamond surfaces. However, large differences in ripple wavelengths, amplitudes and surface roughnesses between HOPG and diamond were recognized. The reason for these differences is discussed.     

Fabrication of a three-dimensional complex carbon nanoneedle from carbon nanowalls

A three-dimensional complex carbon nanoneedle has been fabricated from carbon nanowalls by a direct current plasma chemical vapor deposition system. Sample grown on stainless wire substrate pretreated with the mixing powders of diamond and molybdenum exhibits novel three-dimensional complex nanostructure, the center of which is a carbon nanoneedle, and many carbon nanowalls growing from the needle. The density of unique nanostructure emitters was about 5 × 10⁷/cm². The I-V characteristic addressed an emission current density of 314 mA/cm² at the electric field of 2.5 V/μm.     

Diamond deposition on siliconized stainless steel

Silicon diffusion layers in AISI 304 and AISI 316 type stainless steels were investigated as an alternative to surface barrier coatings for diamond film growth. Uniform 2 μm thick silicon rich interlayers were obtained by coating the surface of the steels with silicon and performing diffusion treatments at 800 °C. Adherent diamond films with low sp² carbon content were deposited on the diffused silicon layers by a modified hot filament assisted chemical vapor deposition (HFCVD) method. Characterization of as-siliconized layers and diamond coatings was performed by energy dispersive X-ray analysis, scanning electron microscopy, X-ray diffraction and Raman spectroscopy.     

Silane overpressure post-implant annealing of Al dopants in SiC: Cold wall CVD apparatus

We report on the successful post-implantation annealing of 4H-SiC samples that were implanted at elevated temperature with high-dose Al implants. Anneals at temperatures up to 1700 °C were conducted in a silane ambient at a process pressure of 150 Torr using a cold wall CVD reactor. A series of 30 min anneals were performed in 3% silane premixed in 97% UHP argon (Ar), which was further diluted in a 6 slm Ar carrier gas. The surface morphology of the samples was studied via plan-view secondary electron microscopy (SEM) and atomic force microscopy (AFM). The resulting surface morphology showed no evidence of step bunching or any other surface degradation. We also report the electrical characterization of Al⁺ implanted p⁺/n 4H-SiC diodes realized on samples that were annealed at 1600 °C. The current-voltage characteristics of the p⁺/n diodes and the resistivity of the implanted layer were measured at room temperature. Most of the diodes had a turn-on voltage of 1.75 V, with ideality factors of up to 1.2 and very low reverse leakage current at −100 V, corresponding to an average reverse leakage current density of (9.7 ± 0.4) × 10⁻⁹ A/cm². The breakdown voltage was near the theoretical value for an epitaxial 4H-SiC layer. However, the resistivity value of the implanted Al⁺ layer was 11 Ω cm, which was an order magnitude higher than the expected value.     

Electric field breakdown of lateral-type Schottky diodes formed on lightly doped homoepitaxial diamond

The reverse current of lateral-type Schottky diodes fabricated on p-type homoepitaxial diamond was analyzed by changing the distance between Schottky and Ohmic electrodes and the metal materials in the Schottky electrodes. The maximum electric field at breakdown was 0.56 MV cm⁻¹ for the Au Schottky contact and less than 0.26 MV cm⁻¹ for the Al Schottky contact. The breakdown voltage depended on the electrode distance when the diamond surface was revealed in vacuum, whereas the Schottky diodes sustained the applied voltage of 500 V, corresponding to 0.69 MV cm⁻¹, after covering of the diamond surface with an insulating liquid. Diamond surface protection is an indispensable technique for fabrication of high-voltage Schottky diodes based on diamond.     

Effect of nitrogen doping on the properties of AlSiO film for wide bandgap semiconductors

A gate insulator film with a wide bandgap and a high dielectric constant is required to achieve high-power field effect transistors (FET) using wide bandgap semiconductors such as SiC, GaN, and diamond. It is observed that an aluminum silicon oxide (AlSiO) film containing 11% nitrogen has a high resistivity of 5 × 10¹⁵ Ω cm, and the leakage current of a nitrogen-doped aluminum silicon oxide (AlSiON) film is also suppressed at high temperature, as compared to the AlSiO film. For example, the leakage current at 240 °C is four orders of magnitude smaller than that of the AlSiO film, suggesting that the AlSiON film is applicable to high temperature operation of wide bandgap semiconductor devices.