Comparison of α particle detectors based on single-crystal diamond films grown in two types of gas atmospheres by microwave plasma-assisted chemical vapor deposition

Chemical vapor deposition(CVD)-grown diamond films have been developed as irradiation-resistant materials to replace or upgrade current detectors for use in extreme radiation environments. However, their sensitivity in practical applications has been inhibited by space charge stability issues caused by defects and impurities in pure diamond crystal materials. In this study, two high-quality CVD-grown single-crystal diamond(SCD) detectors with low content of nitrogen impurities were fabricated and characterized. The intrinsic properties of the SCD samples were characterized using Raman spectroscopy, stereomicroscopy, and X-ray diffraction with the rocking curve mode, cathode luminescence(CL), and infrared and ultraviolet-visible-near infrared spectroscopies. After packaging the detectors, the dark current and energy resolution under α particle irradiation were investigated. Dark currents of less than 5 pA at 100 V were obtained after annealing the electrodes, which is comparable with the optimal value previously reported. The detector that uses a diamond film with higher nitrogen content showed poor energy resolution, whereas the detector with more dislocations showed poor charge collection efficiency(CCE). This demonstrates that the nitrogen content in diamond has a significant effect on the energy resolution of detectors, while the dislocations in diamond largely contribute to the poor CCE of detectors.

Edge effect during microwave plasma chemical vapor deposition diamond-film:Multiphysics simulation and experimental verification

This study focused on the investigation of the edge effect of diamond films deposited by microwave plasma chemical vapor de-position.Substrate bulge height△h is a factor that affects the edge effect,and it was used to simulate plasma and guide the diamond-film deposition experiments.Finite-element software COMSOL Multiphysics was used to construct a multiphysics(electromagnetic,plasma,and fluid heat transfer fields)coupling model based on electron collision reaction.Raman spectroscopy and scanning electron microscopy were performed to characterize the experimental growth and validate the model.The simulation results reflected the experimental trends observed.Plasma discharge at the edge of the substrate accelerated due to the increase in△h(△h=0-3 mm),and the values of electron density(n_(c)),molar concentration of H(C_(H)),and molar concentration of CH_(3)(C_(CH_(3)))doubled at the edge(for the special concave sample with△h=−1 mm,the active chemical groups exhibited a decreased molar concentration at the edge of the substrate).At=0-3 mm,a high diamond growth rate and a large diamond grain size were observed at the edge of the substrate,and their values increased with.The uniformity of film thickness decreased with.The Raman spectra of all samples revealed the first-order characteristic peak of dia-mond near 1332 cm^(−1).When△h=−1 mm,tensile stress occurred in all regions of the film.When△h=1-3 mm,all areas in the film ex-hibited compressive stress.

Fabrication of a single-crystal diamond neutron detector and its application in 14.1 MeV neutron detection in deuterium-tritium fusion experiments

A single-crystal diamond detector is fabricated to diagnose 14.1 MeV deuterium-tritium(D-T)fusion neutrons.The size of its diamond film is 4.5 mm×4.5 mm×500μm.This film is sandwiched by a flat,strip-patterned gold electrode.The dark current of this detector is experimentally measured to be lower than 0.1 nA under an electric field of 30 kV cm^(-1).This diamond detector is used to measure D-T fusion neutrons with a flux of about 7.5×10^(5) s^(-1)cm^(-2).The pronounced peak with a central energy of 8.28 MeV characterizing the^(12)C(n,α)~9Be reaction in the neutron energy spectrum is experimentally diagnosed,and the energy resolution is better than 1.69%,which is the best result reported so far using a diamond detector.A clear peak with a central energy of 6.52 MeV characterizing the^(12)C(n,n')3αreaction is also identified with an energy resolution of better than 7.67%.

Laser patterning of large-scale perovskite single-crystal-based arrays for single-mode laser displays

Lead halide perovskites have attracted considerable attention as potential candidates for high-performance nano/microlasers,owing to their outstanding optical properties.However,the further development of perovskite microlaser arrays(especially based on polycrystalline thin films)produced by the conventional processing techniques is hindered by the chemical instability and surface roughness of the perovskite structures.Herein,we demonstrate a laser patterning of large-scale,highly crystalline perovskite single-crystal films to fabricate reproducible perovskite single-crystal-based microlaser arrays.Perovskite thin films were directly ablated by femtosecond-laser in multiple low-power cycles at a minimum machining line width of approximately 300 nm to realize high-precision,chemically clean,and repeatable fabrication of microdisk arrays.The surface impurities generated during the process can be washed away to avoid external optical loss due to the robustness of the single-crystal film.Moreover,the high-quality,large-sized perovskite single-crystal films can significantly improve the quality of microcavities,thereby realizing a perovskite microdisk laser with narrow linewidth(0.09 nm)and low threshold(5.1µJ/cm2).Benefiting from the novel laser patterning method and the large-sized perovskite single-crystal films,a high power and high color purity laser display with single-mode microlasers as pixels was successfully fabricated.Thus,this study may offer a potential platform for mass-scale and reproducible fabrication of microlaser arrays,and further facilitate the development of highly integrated applications based on perovskite materials.

Epitaxial growth of CsPbBr_(3)/PbS single-crystal film heterostructures for photodetection

Epitaxial high-crystallization film semiconductor heterostructures has been proved to be an effective method to prepare single-crystal films for different functional devices in modern microelectronics,electro-optics,and optoelectronics.With superior semiconducting properties,halide perovskite materials are rising as building blocks for heterostructures.Here,the conformal vapor phase epitaxy of CsPbBr3 on PbS single-crystal films is realized to form the CsPbBr3/PbS heterostructures via a two-step vapor deposition process.The structural characterization reveals that PbS substrates and the epilayer CsPbBr3 have clear relationships:CsPbBr3(110)//PbS(100),CsPbBr3[001]//PbS[001]and CsPbBr3[001]//PbS[010].The absorption and photoluminescence(PL)characteristics of CsPbBr3/PbS heterostructures show the broadband light absorption and efficient photogenerated carrier transfer.Photodetectors based on the heterostructures show superior photoresponsivity of 15 A/W,high detectivity of 2.65×10^(11) Jones,fast response speed of 96 ms and obvious rectification behavior.Our study offers a convenient method for establishing the high-quality CsPbBr3/PbS single-crystal film heterostructures and providing an effective way for their application in optoelectronic devices.

Relationship between the spatial position of the seed and growth mode for single-crystal diamond grown with an enclosed-type holder

The relationship between the spatial position of the diamond seed and growth mode is investigated with an enclosedtype holder for single-crystal diamond growth using the microwave plasma chemical vapor deposition epitaxial method.The results demonstrate that there are three main regions by varying the spatial position of the seed.Due to the plasma concentration occurring at the seed edge,a larger depth is beneficial to transfer the plasma to the holder surface and suppress the polycrystalline diamond rim around the seed edge.However,the plasma density at the edge decreases drastically when the depth is too large,resulting in the growth of a vicinal grain plane and the reduction of surface area.By adopting an appropriate spatial location,the size of single-crystal diamond can be increased from 7 mm×7 mm×0.35 mm to8.6 mm×8.6 mm×2.8 mm without the polycrystalline diamond rim.

Ohmic and Schottky contacts of hydrogenated and oxygenated boron-doped single-crystal diamond with hill-like polycrystalline grains

Hill-like polycrystalline diamond grains(HPDGs)randomly emerged on a heavy boron-doped p+single-crystal diamond(SCD)film by prolonging the growth duration of the chemical vapor deposition process.The Raman spectral results confirm that a relatively higher boron concentration(~1.1×10^(21) cm^(-3))is detected on the HPDG with respect to the SCD region(~5.4×10^(20) cm^(-3)).It demonstrates that the Au/SCD interface can be modulated from ohmic to Schottky contact by varying the surface from hydrogen to oxygen termination.The current-voltage curve between two HPDGs is nearly linear with either oxygen or hydrogen termination,which means that the HPDGs provide a leakage path to form an ohmic contact.There are obvious rectification characteristics between oxygen-terminated HPDGs and SCD based on the difference in boron doping levels in those regions.The results reveal that the highly boron-doped HPDGs grown in SCD can be adopted as ohmic electrodes for Hall measurement and electronic devices.

Evaluation on residual stresses of silicon-doped CVD diamond films using X-ray diffraction and Raman spectroscopy

The effect of silicon doping on the residual stress of CVD diamond films is examined using both X-ray diffraction (XRD) analysis and Raman spectroscopy measurements. The examined Si-doped diamond films are deposited on WC-Co substrates in a home-made bias-enhanced HFCVD apparatus. Ethyl silicate (Si(OC2H5)4) is dissolved in acetone to obtain various Si/C mole ratio ranging from 0.1% to 1.4% in the reaction gas. Characterizations with SEM and XRD indicate increasing silicon concentration may result in grain size decreasing and diamond [110] texture becoming dominant. The residual stress values of as-deposited Si-doped diamond films are evaluated by both sin2ψ method, which measures the (220) diamond Bragg diffraction peaks using XRD, with ψ-values ranging from 0° to 45°, and Raman spectroscopy, which detects the diamond Raman peak shift from the natural diamond line at 1332 cm-1. The residual stress evolution on the silicon doping level estimated from the above two methods presents rather good agreements, exhibiting that all deposited Si-doped diamond films present compressive stress and the sample with Si/C mole ratio of 0.1% possesses the largest residual stress of ~1.75 GPa (Raman) or ~2.3 GPa (XRD). As the silicon doping level is up further, the residual stress reduces to a relative stable value around 1.3 GPa.

Effect of deposition parameters on micro-and nano-crystalline diamond films growth on WC-Co substrates by HFCVD

The characteristics of hot filament chemical vapor deposition（HFCVD） diamond films are significantly influenced by the deposition parameters, such as the substrate temperature, total pressure and carbon concentration. Orthogonal experiments were introduced to study the comprehensive effects of such three parameters on diamond films deposited on WC-Co substrates. Field emission scanning electron microscopy, atomic force microscopy and Raman spectrum were employed to analyze the morphology, growth rate and composition of as-deposited diamond films. The morphology varies from pyramidal to cluster features with temperature decreasing. It is found that the low total pressure is suitable for nano-crystalline diamond films growth. Moreover, the substrate temperature and total pressure have combined influence on the growth rate of the diamond films.

Enhancement of nucleation of diamond films deposited on copper substrate by nickel modification layer

A Ni layer with a thickness of about 100 nm was sputtered on Cu substrates,followed by an ultrasonic seeding with nanodiamond suspension.High-quality diamond film with its crystalline grains close to thermal equilibrium shape was deposited on Cu substrates by hot-filament chemical vapor deposition（HF-CVD）,and the sp2 carbon content was less than 5.56%.The nucleation and growth of diamond film were investigated by micro-Raman spectroscopy,scanning electron microscopy,and X-ray diffraction.The results show that the nucleation density of diamond on the Ni-modified Cu substrates is 10 times higher than that on blank Cu substrates.The enhancement mechanism of the nucleation kinetics by Ni modification layer results from two effects：namely,the nanometer rough Ni-modified surface shows an improved absorption of nanodiamond particles that act as starting points for the diamond nucleation during HF-CVD process;the strong catalytic effect of the Ni-modified surface causes the formation of graphite layer that acts as an intermediate to facilitate diamond nucleation quickly.

Effects of deposition parameters on HFCVD diamond films growth on inner hole surfaces of WC-Co substrates

Deposition parameters that have great influences on hot filament chemical vapor deposition (HFCVD) diamond films growth on inner hole surfaces of WC?Co substrates mainly include the substrate temperature (t), carbon content (φ), total pressure (p) and total mass flow (F). Taguchi method was used for the experimental design in order to study the combined effects of the four parameters on the properties of as-deposited diamond films. A new figure-of-merit (FOM) was defined to assess their comprehensive performance. It is clarified thatt,φandp all have significant and complicated effects on the performance of the diamond film and the FOM, which also present some differences as compared with the previous studies on CVD diamond films growth on plane or external surfaces. Aiming to deposit HFCVD diamond films with the best comprehensive performance, the key deposition parameters were finally optimized as:t=830 °C,φ=4.5%,p=4000 Pa,F=800 mL/min.

Application of ultra-smooth composite diamond film coated WC-Co drawing dies under water-lubricating conditions

A specific revised HFCVD apparatus and a novel process combining HFCVD and polishing technique were presented to deposit the micro-and nano-crystalline multilayered ultra-smooth diamond（USCD） film on the interior-hole surface of WC-Co drawing dies with aperture ranging from d1.0 mm to 60 mm.Characterization results indicate that the surface roughness values（Ra） in the entry zone,drawing zone and bearing zone of as-fabricated USCD coated drawing die were measured as low as 25.7,23.3 and 25.5 nm,respectively.Furthermore,the friction properties of USCD films were examined in both dry sliding and water-lubricating conditions,and the results show that the USCD film presents much superior friction properties.Its friction coefficients against ball-bearing steel,copper and silicon nitride balls（d4 mm）,is always lower than that of microcrystalline diamond（MCD） or WC-Co sample,regardless of the lubricating condition.Meanwhile,it still presents competitive wear resistance with the MCD films.Finally,the working lifetime and performance of as-fabricated USCD coated drawing dies were examined under producing low-carbon steel pipes in dry-sliding and water-lubricating conditions.Under the water-lubricating drawing condition,its production significantly increases by about 20 times compared with the conventional WC-Co drawing dies.

Preparation and characterization of diamond film on Cu substrate using Cu-diamond composite interlayer

Large area diamond films were fabricated on copper substrates by a multi-step process comprised of electroplating Cu-diamond composite layer on Cu substrate, plating a Cu layer to fix the protruding diamond particles, and depositing continuous diamond film on composite interlayer by hot-filament chemical vapor deposition （HFCVD）. The interface characteristics, internal stress and adhesion strength were investigated by scanning electron microscopy, Raman analysis and indentation test. The results show that the continuous film without cracks is successfully obtained. The microstructure of the film is a mixture of large cubo-octahedron grains grown from homo-epitaxial growth and small grains with （111） apparent facets grown from lateral second nuclei. The improved adhesion between diamond film and substrate results from the deep anchoring of the diamond particles in the Cu matrix and the low residual stress in the film.

Two Steps B Ion-Implantation of Diamond Film Grown on an n-Type Si Substrate and Its p-n Junction Effects

Polycrystalline diamond thin films are deposited on an n-type Si substrates by hot filament chemical vapor deposition,and then are implanted with boron ions in a 200keV ion implanter.In order to achieve a better distribution of the implanted element,boron ions are implanted by two steps:implanting boron ions with the energy of 70keV first,and then with the energy of 100keV.The homogeneous distribution of the B ion is gained.The current-voltage characteristics of the samples are studied.It is found that the p-n heterojunction effect is achieved in these samples.

DIAMOND FILMS DEPOSITED AT LOW TEMPERATURES MICROWAVE PLASMA-ASSISTED CVD METHOD

Low-temperature deposition of diamond thin films in the range of 280￣445℃ has been successfully carried out by microwave plasma-assisted CVD method.At lower deposition temperatures (280￣445℃),the large increase in the nucleation density and great improvement in the average surfae roughness of the diamond were observed. Results of low temperature deposition and characterization of diamond thin films obtained are presented.

Preparation, characterization and electrochemical properties of boron-doped diamond films on Nb substrates

A series of boron-doped polycrystalline diamond films were prepared by hot filament （HF） chemical vapor deposition on Nb substrates. The effects of B/C ratio of reaction gas on film morphology, growth rate, chemical bonding states, phase composition and electrochemical properties of each deposited sample were studied by scanning electron microscopy, Raman spectra, X-ray diffraction, microhardness indentation, and electrochemical analysis. Results show that the average grain size of diamond and the growth rate decrease with increasing the B/C ratio. The diamond films exhibit excellent adhesion under Vickers microhardness testing （9.8 N load）. The sample with 2% B/C ratio has a wider potential window and a lower background current as well as a faster redox reaction rate in H2SO4 solution and KFe（CN）6 redox system compared with other doping level electrodes.

Study on the Dielectric Properties of Chemical Vapor Deposited Diamond Film

Aim To study the dielectric properties of diamond film. Methods Dielectric properties (the frequency dependenCe of conductance, permittivity, and loss factor) of diamond film preped by DC are plasma jet chemical vapor deposition (CVD) were studied. Resuls Dielectric properties of CVD diamond fAn depend mainly on its polycrystalline nature, and the presence of non-diamond disordered graphitic regions and impurities between diamond grains of the film. Annealing at 500℃ leads to the removal of greater part of disordered graphitic regions, but am not remove all disordered graphitic regions and impurities. Conclusion Much work nab to be done tO prepare or post-treat diamond films before using CVD diamond as a substrate for electronic devices.

EFFECT OF GRID BIAS ON DEPOSITION OF NANOCRYSTALLINE DIAMOND FILMS

A positive grid bias and a negative substrate bias voltages are applied to the self-made hot filament chemical vapor deposited （HFCVD） system. The high quality nanocrystalline diamond （NCD） film is successfully deposited by double bias voltage nucleation and grid bias voltage growth. The Micro-Raman XRD SEM and AFM are used to investigate the diamond grain size, microstructure, surface morphology, and nucleation density. Results show that the obtained NCD has grain size of about 20 nm. The effect of grid bias voltage on the nucleation and the diamond growth is studied. Experimental results and theoretical analysis show that the positive grid bias increases the plasma density near the hot filaments, enhances the diamond nucleation, keeps the nanometer size of the diamond grains, and improves the quality of diamond film.

STUDY ON DIAMOND LIKE CARBON THIN FILM BY FILTERED VACUUM ARC DEPOSITION

Diamond like carbon thin film is successfully deposited on silicon, titanium and stainless steel substrate at low temperature in a filtered vacuum arc deposition system. Arc discharges are established on a graphite cathode in the system with a toroidal macroparticle filter. A cathode activating magnetic field and a filtered magnetic field to collimate the plasma beam are applied. Ion current convected by the plasma beam is measured with a negatively biased probe. It is shown that the magnetic field of the coils located on the plasma duct has a strong influence on cathode spot behavior. Orthogonally the designed experiments are carried out to optimize the deposition parameters of arc stability. Finally, the diamond like carbon thin films are studied by scanning electron microscope (SEM) and Raman spectrum.

Amorphous SiO_2 interlayers for deposition of adherent diamond films onto WC-Co inserts

Amorphous Si O2（a-Si O2） films were synthesized on WC-Co substrates with H2 and tetraethoxysilane（TEOS） via pyrolysis of molecular precursor.X-ray diffraction（XRD） pattern shows that silicon-cobalt compounds form at the interface between a-Si O2 films and WC-Co substrates.Moreover,it is observed by transmission electron microscope（TEM） that the a-Si O2 films are composed of hollow mirco-spheroid a-Si O2 particles.Subsequently,the a-Si O2 films are used as intermediate films and chemical vapor deposition（CVD） diamond films are deposited on them.Indentation tests were performed to evaluate the adhesion of bi-layer（a-Si O2 ＋ diamond） films on cemented carbide substrates.And the cutting performance of bi-layer（a-Si O2 ＋ diamond） coated inserts was evaluated by machining the glass fiber reinforced plastic（GFRP）.The results show that a-Si O2 interlayers can greatly improve the adhesive strength of diamond films on cemented carbide inserts;furthermore,thickness of the a-Si O2 interlayers plays a significant role in their effectiveness on adhesion enhancement of diamond films.