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.     

The approach to diamond growth on levitating seed particles

We demonstrate the approach of diamond growth on levitating seed particles in a rf plasma. We introduce a hot filament chemical vapor deposition (CVD) technique into the rf plasma chamber in order to obtain improved crystal growth. Firstly, we confirmed diamond nucleation on seed particles placed on a Si substrate using the hot filament CVD. The deposition conditions, namely the total pressure and the rf power, were chosen so that they correspond to particles levitation conditions. We observe that a hydrogen pre-treatment on the seed particles improves the nucleation. Secondly, we confirm the levitation of particles at high temperatures. Fine particles levitated in a plasma are particularly sensitive to thermophoretic effects due to inhomogeneities in the gas heating. Therefore, proper heating procedures are required for successful particles levitation.     

Real-time monitoring of diamond nucleation and growth using field-enhanced thermionic emission current

Diamond nucleation and growth in the combustion-flame method were monitored in real time using thermionic emission current from the deposited diamond films. It was observed that the emission current evolved over three periods, the incubation, the fast increase, and the saturation periods. Ball-shaped diamond particles, faceted diamond crystals, and diamond films with well-faceted crystals were formed in the three periods. The current from a diamond-seeded substrate started to increase immediately without an incubation period, confirming that the current is from the diamond. Therefore, the current could be used for real-time monitoring of the diamond nucleation and growth.     

Ultra‐thin nanocrystalline diamond films (<100 nm) with high electrical resistivity

Thick diamond films are known to exhibit remarkably high electrical resistivity and thermal conductivity. However, on thin films, difficulties are often observed to achieve such performances. In this study, the synthesis of ultra‐thin diamond films was optimized towards the possibility to maintain high dielectric performances on layers compatible with today requirements for Silicon‐On‐Diamond technology, and namely aiming at films with thicknesses equal or below 150 nm. The nucleation of diamond nanocrystals is crucial to obtain films with thickness lower than 100 nm. A Bias Enhanced Nucleation step (BEN) was improved to achieve nucleation densities above 10¹¹ cm^–2 although the process was also tuned to limit the size of the nanocrystals during this step. The control of the carbonization of the silicon substrate is also essential to reach such a density with a high reproducibility. The BEN is followed by a growth step with optimized conditions. The films were characterized by SEM and Spectroscopic Ellipsometry. Electrical conductivity measurements were conducted on thin diamond films and values obtained on layers below 100 nm were as high as 5 × 10¹³ Ω cm; a value significantly higher than the state of the art for such thin films. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Hydrogen incorporation in ultrananocrystalline diamond/amorphous carbon films

The incorporation of hydrogen within ultrananocrystalline diamond/amorphous carbon composite films has been investigated by nuclear reaction analysis (NRA) and Fourier transform infrared spectroscopy (FTIR). The film bulk contains ca. 7.5–8% H (for a deposition temperature of 600 °C), while the H concentration in the surface region is considerably higher. FTIR measurements show that the hydrogen‐rich surface is formed right at the beginning of the deposition process and grows outward as the film thickness increases. It can thus be concluded that surface hydrogen species play an active role in the formation of ultrananocrystalline diamond/amorphous carbon films. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Low-temperature chemical vapor deposition of highly doped n-type epitaxial Si at high growth rate

We investigated the growth of in-situ n-type doped epitaxial Si layers with arsenic and phosphorus by means of low-temperature chemical vapor deposition using trisilane as Si-precursor. Indeed, in order to prevent the alteration of the characteristics of the devices which are already present on the wafer, an epitaxy process at low temperature is highly desired for applications such as BiCMOS. In this work, the varying parameters are the deposition temperature, the Si-precursor mass flow and the dopant gas flow. As a result, a process for the deposition of heavily doped epilayers was demonstrated at 600 °C with high deposition rate, which is important for maintaining high throughput and low process cost. We showed that using trisilane as a Si-precursor resulted in a much more linear n-type doping behavior than using dichlorosilane. Therefore it allowed an easier process control and a wider dynamic doping range. Our process is an interesting route for the epitaxy of a low-resistance emitter layer for bipolar transistor application.     

Diamond coating deposition by synergy of thermal and laser methods—A problem revisited

Diamond coatings were deposited by synergy of the hot filament CVD method and the pulse TEA CO₂ laser, in spectroactive and spectroinactive diamond precursor atmospheres. Resulting diamond coatings are interpreted relying on evidence of scanning electron microscopy as well as microRaman spectroscopy. Thermal synergy component (hot filament) possesses an activating agent for diamond deposition, and contributes significantly to quality and extent of diamond deposition. Laser synergy component comprises a solid surface modification as well as the spectroactive gaseous atmosphere modification. Surface modification consists in changes of the diamond coating being deposited and, at the same time, in changes of the substrate surface structure. Laser modification of the spectroactive diamond precursor atmosphere means specific consumption of the precursor, which enables to skip the deposition on a defined substrate location. The resulting process of diamond coating elimination from certain, desired locations using the CO₂ laser might contribute to tailoring diamond coatings for particular applications. Additionally, the substrate laser modification could be optimized by choice of a proper spectroactive precursor concentration, or by a laser radiation multiple pass through an absorbing medium.     

Enhanced diamond nucleation on copper substrates by graphite seeding and CO2 laser irradiation

Diamond nucleation on copper (Cu) substrates was investigated by graphite seeding and CO₂ laser irradiation at initial stages of the combustion-flame deposition. A graphite aerosol spray was used to generate a thin layer of graphite powders (less than 1 μm) on Cu substrates. The graphite-seeded Cu substrates were then heated by a continuous CO₂ laser to about 750 °C within 1 min. It was found that diamond nucleation density after this treatment was more than three times as much as that on the virgin Cu substrates. As a consequence, diamond films up to 4 μm were obtained in 5 min. The enhancement of diamond nucleation on the graphite-seeded Cu substrates was attributed to the formation of defects and edges during the etching of the seeding graphite layers by the OH radicals in the flame. The defects and edges served as nucleation sites for diamond formation. The function of the CO₂ laser was to rapidly heat the deposition areas to create a favorable temperature for diamond nucleation and growth.     

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.     

Field emitters with low turn on electric field based on carbon fibers

Field emitters of vertical carbon fibers on a silicon substrate are fabricated by catalytic chemical vapor deposition. After an ageing process of 150 min, field emission measurement of the fibers is carried out in a vacuum chamber with a base pressure of 5.0 × 10⁻⁴ Pa. The experimental results display that field emission performance of the carbon fibers depends strongly on the vacuum level during the experiments. After the field emission measurement, damage to the carbon fiber field emitters is observed from the scanning electron microscopic images.     

High-Rate Growth and Nitrogen Distribution in Homoepitaxial Chemical Vapour Deposited Single-crystal Diamond

High rate （〉 50 μm/h） growth of homoepitaxial single-crystal diamond （SCD） is carried out by microwave plasma chemical vapour deposition （MPCVD） with added nitrogen in the reactant gases of methane and hydrogen, using a polyerystalline-CVD-diamond-film-made seed holder. Photolumineseenee results indicate that the nitrogen concentration is spatially inhomogeneous in a large scale, either on the top surface or in the bulk of those as-grown SCDs. The presence of N-distribution is attributed to the facts： （i） a difference in N-incorporation efficiency and （ii） N-diffusion, resulting from the local growth temperatures changed during the high-rate deposition process. In addition, the formed nitrogen-vacancy eentres play a crucial role in N-diffusion through the growing crystal. Based on the N-distribution observed in the as-grown crystals, we propose a simple method to distinguish natural diamonds and man-made CVD SCDs. Finally, the disappearance of void defect on the top surface of SCDs is discussed to be related to a filling-in mechanism.     

Micropatterned vertically aligned carbon-nanotube growth on a Si surface or inside trenches

The good field-emission properties of carbon nanotubes coupled with their high mechanical strength, chemical stability, and high aspect ratio, make them ideal candidates for the construction of efficient and inexpensive field-emission electronic devices. The fabrication process reported here has considerable potential for use in the development of integrated radio-frequency amplifiers or field-emission-controllable cold-electron guns for field-emission displays. This fabrication process is compatible with currently used semiconductor-processing technologies. Micropatterned vertically aligned carbon nanotubes were grown on a planar Si surface or inside trenches, using chemical vapor deposition, photolithography, pulsed-laser deposition, reactive ion etching, and the lift-off method. This carbon-nanotube fabrication process can be widely applied for the development of electronic devices using carbon-nanotube field emitters as cold cathodes and could revolutionize the area of field-emitting electronic devices. Received: 30 August 2001 / Accepted: 3 September 2001 / Published online: 20 December 2001     

Rectifying properties and photoresponse of CVD diamond p(i)n‐junctions

The current–voltage characteristics and photoresponse of mesa structured {111}‐oriented homoepitaxial CVD diamond p(i)n‐junctions with different intrinsic layer thickness are investigated. When a sufficiently thick intrinsic layer is present, a rectification ratio of 10⁸ at ±10 V could be obtained. Good rectifying diodes show a high photoresponse ratio between 210 nm (above bandgap) and 500 nm (below bandgap), making them suitable for UV detection purposes. The results are compared with similar measurements carried out on polycrystalline CVD diamond pn‐junctions.

     

Microstructure and tribological performance of self-lubricating diamond/tetrahedral amorphous carbon composite film

In order to smooth the rough surface and further improve the wear-resistance of coarse chemical vapor deposition diamond films, diamond/tetrahedral amorphous carbon composite films were synthesized by a two-step preparation technique including hot-filament chemical vapor deposition for polycrystalline diamond (PCD) and subsequent filtered cathodic vacuum arc growth for tetrahedral amorphous carbon (ta-C). The microstructure and tribological performance of the composite films were investigated by means of various characterization techniques. The results indicated that the composite films consisted of a thick well-grained diamond base layer with a thickness up to 150 μm and a thin covering ta-C layer with a thickness of about 0.3 μm, and sp³-C fraction up to 73.93%. Deposition of a smooth ta-C film on coarse polycrystalline diamond films was proved to be an effective tool to lower the surface roughness of the polycrystalline diamond film. The wear-resistance of the diamond film was also enhanced by the self-lubricating effect of the covering ta-C film due to graphitic phase transformation. Under dry pin-on-disk wear test against Si₃N₄ ball, the friction coefficients of the composite films were much lower than that of the single PCD film. An extremely low friction coefficient (∼0.05) was achieved for the PCD/ta-C composite film. Moreover, the addition of Ti interlayer between the ta-C and the PCD layers can further reduce the surface roughness of the composite film. The main wear mechanism of the composite films was abrasive wear.     

Characterization of vacancy-related defects introduced into silicon during heat treatment by deep-level transient spectroscopy and gamma-ray diffraction techniques

Vacancy-related defects introduced into n-Si during annealing or aluminium diffusion at high temperature (1000–1250°C) have been studied. Different ambients (argon, nitrogen, vacuum and chlorine-containing atmosphere) were used to create a vacancy supersaturation during heat treatments. Three deep-level centers whose formation is governed by the presence of vacancies have been identified. They were characterized by the following temperature dependences of the thermal emission rate:e3 = 7.92 × 10⁷ T ² × exp(– 0.455/kT),e ₅ = 2.64 × 10⁶ T ² × exp( – 0.266/kT),e ₇ = 7.26 × 10⁶ T ² × exp (– 0.192/kT). The influence of different factors, such as heat-treatment conditions, concentration of oxygen and doping level in initial crystals, on center formation was studied. An asymmetric diffuse-ray scattering was observed near the surface of a crystal irradiated by thermal neutrons and annealed in a chlorine-containing atmosphere. This scattering is related to the formation of structural defects of the vacancy type. In the same region of the crystal, the concentration of the E7 center was one order of magnitude higher than that of other deep-level centers. Comparison of the-ray diffraction and deeplevel transient spectroscopy (DLTS) data suggests that the formation of the center occurs under the conditions of Si supersaturation with vacancies.     

Single Crystal Si Layers on Glass Fabricated by Hydrophilic Fusion Bonding and Smart-Cut Technology

A single crystal Si thin film on a glass substrate has been obtained successfully by hydrophilic fusion bonding and the smart-cut technology. Tensile strength testing shows that the bonded interface has strong adhesion and the bonding strength is about 8.7MPa. Crystallinity and microstructure of the samples have been characterized by transmission electron microscopy (TEM). Electrical properties have also been investigated by Hall measurements and four-point probe. The mobility of the transferred Si layer on glass is about 122cm^2//V.s. The results show that the single-crystal silicon layer transferred onto glass by direct bonding keeps good quality for the applications of integrated circuits, transducers, and fiat panel display.     

Use of chlorinated carbon and silicon precursors for epitaxial growth of 4H‐SiC at very high growth rates

A possibility to apply the advantages of chlorinated carbon precursors, which had been previously used in low‐temperature epitaxial growth of 4H‐SiC, to achieve very high growth rates at higher growth temperatures was investigated. Silicon tetrachloride was used as the silicon precursor to suppress gas‐phase homogeneous nucleation. The temperature increase from 1300 °C (which is the temperature of the previously reported low‐temperature halo‐carbon epitaxial growth) to 1600 °C enabled an increase of the precursor flow rates and consequently of the growth rate from 5 to more than 100 μm/h without morphology degradation. High quality of the epilayers was confirmed by low‐temperature photoluminescence spectroscopy and time‐resolved luminescence. No evidences of homogeneous nucleation were detected, however, liquid Si droplet formation on the epilayer surface seems to remain a bottleneck at very high growth rate. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structure and gas-barrier properties of amorphous hydrogenated carbon films deposited on inner walls of cylindrical polyethylene terephthalate by plasma-enhanced chemical vapor deposition

The influence of radio-frequency (RF) power on the structure and gas permeation through amorphous hydrogenated carbon films deposited on cylindrical polyethylene terephthalate (PET) samples is investigated. The results show that a higher radio-frequency power leads to a smaller sp³/sp² value but produces fewer defects with smaller size. The permeability of PET samples decreases significantly after a-C:H deposition and the RF only exerts a small influence. However, the coating uniformity, color, and wettability of the surface are affected by the RF power. A higher RF power results in to better uniformity and it may be attributed to the combination of the high-density plasma and sample heating.     

Effect of Post-Annealing on Microstructural and Electrical Properties of N^＋Ion-Implanted into ZnO：In Films

We fabricate p-type conductive ZnO thin films on quartz glass substrates by codoping of In-N using radio frequency magnetron sputtering technique together with the direct implantation of acceptor dopants （nitrogen）. The effects of thermal annealing on the structure and electrical properties of the ZnO films are investigated by an x-ray diffractometer （XRD） and a Hall measurement system. It is found that the best p-type ZnO film subjected to annealed exhibits excellent electrical properties with a hole concentration of 1.22 × 10^18 cm^-3, a Hall mobility of 2.19 cm^2 V^-1 s^- 1, and a low resistivity of about 2.33 Ωcm, indicating that the presence of In may facilitates the incorporation of N into ZnO thin films.     

Deposition of large-area, high-quality cubic boron nitride films by ECR-enhanced microwave-plasma CVD

Large-area, 1-μm-thick cubic boron nitride (cBN) films were deposited on (001) silicon substrates by electron-cyclotron-resonance-enhanced microwave-plasma chemical vapor deposition (ECR-MP CVD) in a mixture of He-Ar-N₂-BF₃-H₂ gases. With the assistance of fluorine chemistry in the gas phase and substrate reactions, the phase purity of the sp³-configuration was improved to over 85% at a reduced substrate bias voltage of -40 V. The grown films show clear Raman transversal optical (TO) and longitudinal optical (LO) phonon vibration modes, characteristic of cBN. Such Raman spectral characteristics are the first ever observed in cBN films prepared under ECR-MP CVD conditions. Received: 3 May 2002 / Accepted: 7 May 2002 / Published online: 22 November 2002 RID="*" ID="*"Corresponding author. Fax: +852-2788/7830, E-mail: apwjzh@cityu.edu.hk