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 o...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.展开更多
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 concentratio...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.展开更多
The heteroepitaxy of diamond films has received widespread attention;however,its application remains limited owing to the mismatch in properties and structure between diamond and heterogeneous substrates.In this study...The heteroepitaxy of diamond films has received widespread attention;however,its application remains limited owing to the mismatch in properties and structure between diamond and heterogeneous substrates.In this study,diamond films were successfully synthesized on high-entropy alloys(HEAs)substrates using microwave plasma chemical vapor deposition.The resulting diamond films were continuous,uniform,and adhered to the HEAs substrates.The mixed carbides were identified using X-ray diffraction,and the quality of the diamond films was examined using Raman spectroscopy.Moreover,the corrosion test revealed that the diamond/TiZrHfMo samples had excellent electrochemical stability and corrosion resistance with a corrosion potential value of-0.169 V in a 3.5wt%NaCl solution.A multiple regression model was established to evaluate the effects of the structure and growth parameters,which confirmed that the mixing entropy significantly affected the grain size and corrosion properties.展开更多
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...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.展开更多
The effects of Si doping on morphology, components and structure characteristics of CVD diamond films were studied. Si-doped CVD diamond films were deposited on Si substrate by adding tetraethoxysilane （TEOS） into a...The effects of Si doping on morphology, components and structure characteristics of CVD diamond films were studied. Si-doped CVD diamond films were deposited on Si substrate by adding tetraethoxysilane （TEOS） into acetone as source of reactant gas. The morphology and microstructure of diamond films were characterized by scanning electron microcopy （SEM）. The crystalline quality of diamond films was studied by Raman spectroscopy and X-ray diffractometry （XRD）. The surface roughness of the films was evaluated with surface profilometer. The results suggest that Si doping tends to reduce the crystallite size, enhance grain refinement and inhibit the appearance of （11 I） facets. Raman spectra indicate that Si doping can enhance the formation of sp2 phase in diamond films. Moreover, Raman signal of SiC was detected, which suggests the existence of Si in the diamond films. Smooth fine-grained diamond （SFGD） film was synthesized at Si to C ratio of 1%.展开更多
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 equilibri...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.展开更多
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 c...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.展开更多
During the growth of the hot filament chemical vapor deposition （HFCVD） diamond films, numerical simulations in a 2-D mathematical model were employed to investigate the influence of various deposition parameters on...During the growth of the hot filament chemical vapor deposition （HFCVD） diamond films, numerical simulations in a 2-D mathematical model were employed to investigate the influence of various deposition parameters on the gas physical parameters, including the temperature, velocity and volume density of gas. It was found that, even in the case of optimized deposition parameters, the space distributions of gas parameters were heterogeneous due primarily to the thermal blockage come from the hot filaments and cryogenic pump effect arisen from the cold reactor wall. The distribution of volume density agreed well with the thermal round-flow phenomenon, one of the key obstacles to obtaining high growth rate in HFCVD process. In virtue of isothermal boundary with high temperature or adiabatic boundary condition of reactor wall, however, the thermal roundflow was profoundly reduced and as a consequence, the uniformity of gas physical parameters was considerably improved, as identified by the experimental films growth.展开更多
Selective deposition of diamond film on patterned Si (100) substrates has been achieved by using microwave plasma chemical vapor deposition (MPCVD) method. The films have been characterized by scanning electron micr...Selective deposition of diamond film on patterned Si (100) substrates has been achieved by using microwave plasma chemical vapor deposition (MPCVD) method. The films have been characterized by scanning electron microscope (SEM) and Raman spectrum. The influence of substrate temperature on the nucleation behavior of diamond was discussed in detail and the optimized deposition condition has been obtained.展开更多
The etching technique using Ce is a convenient and fast method for polishing and shaping diamond films. In this study, the influence of polishing parameters such as polishing temperature and time on the surface crysta...The etching technique using Ce is a convenient and fast method for polishing and shaping diamond films. In this study, the influence of polishing parameters such as polishing temperature and time on the surface crystallinity and phase composition of diamond films was thoroughly investigated via the analysis of Raman spectra such as FWHM and ID/IG. Moreover, the issue on the graphitization of diamond after polishing with Ce was further researched through the detailed study of the depth distribution of Raman data including FWHM and ID/IG, and a result completely different from the hot-iron metal polished ones was obtained. The results showed that polished diamond films had considerably higher diamond content than those before polishing, and not a bit of graphitization was found in the polished ones, owing to a higher solubility of carbon in rare earth metal Ce than that in transition metals, and the original crystallinity of the films polished with Ce did not deteriorate.展开更多
With the advantages of high deposition rate and large deposition area, polycrystalline diamond films prepared by direct current （DC） arc jet chemical vapor deposition （CVD） are considered to be one of the most pro...With the advantages of high deposition rate and large deposition area, polycrystalline diamond films prepared by direct current （DC） arc jet chemical vapor deposition （CVD） are considered to be one of the most promising materials for high-frequency and high-power electronic devices. In this paper, high-quality self-standing polycrystalline diamond films with the diameter of 100 mm were prepared by DC arc jet CVD, and then, the p-type surface conductive layer with the sheet carrier density of 10^11-10^13 cm-2 on the H-terminated diamond film was obtained by micro-wave hydrogen plasma treatment for 40 min. Ti/Au and Au films were deposited on the H-terminated diamond surface as the ohmic contact electrode, respectively, afterwards, they were treated by rapid vacuum annealing at different temperatures. The properties of these two types of ohmic contacts were investigated by measuring the specific contact resistance using the transmission line method （TLM）. Due to the formation of Ti-related carbide at high temperature, the specific contact resistance of Ti/Au contact gradually decreases to 9.95 × 10^-5 Ω-cm2 as the temperature increases to 820℃. However, when the annealing temperature reaches 850℃, the ohmic contact for Ti/Au is degraded significantly due to the strong diffusion and reaction between Ti and Au. As for the as-deposited Au contact, it shows an ohmic contact. After annealing treatment at 550℃, low specific contact resistance was detected for Au contact, which is derived from the enhancement of interdiffusion between Au and diamond films.展开更多
Cu ion implantation and subsequent rapid annealing at 500℃ in N2 result in low surface resistivity of 1.611 ohm/sq with high mobility of 290 cm2 V-1S-1 for microcrystalline diamond （MCD） films. Its electrical field...Cu ion implantation and subsequent rapid annealing at 500℃ in N2 result in low surface resistivity of 1.611 ohm/sq with high mobility of 290 cm2 V-1S-1 for microcrystalline diamond （MCD） films. Its electrical field emission behavior can be turned on at Eo = 2.6 V/μm, attaining a current density of 19.5μA/cm2 at an applied field of 3.5 V/#m. Field emission scanning electron microscopy combined with Raman and x-ray photoelectron mi- croscopy reveal that the formation of Cu nanoparticles in MCD films can catalytically convert the less conducting disorder/a-C phases into graphitic phases and can provoke the formation of nanographite in the films, forming conduction channels for electron transportation.展开更多
Nano-diamond particles are co-deposited on Ti substrates with metal(Ti/Ni) nanoparticles(NPs) by the electrophoretic deposition(EPD) method combined with a furnace annealing at 800℃ under N_(2) atmosphere. Modificati...Nano-diamond particles are co-deposited on Ti substrates with metal(Ti/Ni) nanoparticles(NPs) by the electrophoretic deposition(EPD) method combined with a furnace annealing at 800℃ under N_(2) atmosphere. Modifications of structural and electron field emission(EFE) properties of the metal-doped films are investigated with different metal NPs concentrations. Our results show that the surface characteristics and EFE performances of the samples are first enhanced and then reduced with metal NPs concentration increasing. Both the Ti-doped and Ni-doped nano-diamond composite films exhibit optimal EFE and microstructural performances when the doping quantity is 5 mg. Remarkably enhanced EFE properties with a low turn-on field of 1.38 V/μm and a high current density of 1.32 mA/cm^(2) at an applied field of 2.94 V/μm are achieved for Ni-doped nano-diamond films, and are superior to those for Ti-doped ones. The enhancement of the EFE properties for the Ti-doped films results from the formation of the TiC-network after annealing. However, the doping of electron-rich Ni NPs and formation of high conductive graphitic phase are considered to be the factor, which results in marvelous EFE properties for these Ni-doped nano-diamond films.展开更多
In this study, diamond films were synthesized on silicon substrates by microwave plasma enhanced chemical vapor deposition（CVD） over a wide range of experimental parameters. The effects of the microwave power,CH;/H;...In this study, diamond films were synthesized on silicon substrates by microwave plasma enhanced chemical vapor deposition（CVD） over a wide range of experimental parameters. The effects of the microwave power,CH;/H;ratio and gas pressure on the morphology, growth rate, composition, and quality of diamond films were investigated by means of scanning electron microscope（SEM）, X-ray diffraction（XRD）, Raman spectroscopy and X-ray photoelectron spectroscopy（XPS）. A rise of microwave power can lead to an increasing pyrolysis of hydrogen and methane, so that the microcrystalline diamond film could be synthesized at low CH;/H;levels. Gas pressure has similar effect in changing the morphology of diamond films, and high gas pressure also results in dramatically increased grain size. However,diamond film is deteriorated at high CH;/H;ratio due to the abundant graphite content including in the films. Under an extreme condition of high microwave power of 10 kW and high CH;concentration, a hybrid film composed of diamond/graphite was successfully formed in the absence of N;or Ar,which is different from other reports. This composite structure has an excellent measured sheet resistance of 10-100 Ω/Sqr. which allows it to be utilized as field electron emitter. The diamond/graphite hybrid nanostructure displays excellent electron field emission（EFE） properties with a low turn-on field of 2.17 V/μm and β= 3160, therefore it could be a promising alternative in field emission applications.展开更多
Microcrystalline diamond(MCD)films with different grain sizes ranging from 160 nm to 2200 nm are prepared by using a hot filament chemical vapor deposition(HFCVD)system,and the influences of grain size and structural ...Microcrystalline diamond(MCD)films with different grain sizes ranging from 160 nm to 2200 nm are prepared by using a hot filament chemical vapor deposition(HFCVD)system,and the influences of grain size and structural features on optical properties are investigated.The results show that the film with grain size in a range of 160 nm–310 nm exhibits a higher refractive index in a range of(2.77–2.92).With grain size increasing to 620±300 nm,the refractive index shows a value between 2.39 and 2.47,approaching to that of natural diamond(2.37–2.55),and a lower extinction coefficient value between 0.08 and 0.77.When the grain size increases to 2200 nm,the value of refractive index increases to a value between 2.66 and 2.81,and the extinction coefficient increases to a value in a range of 0.22–1.28.Visible Raman spectroscopy measurements show that all samples have distinct diamond peaks located in a range of 1331 cm-1–1333 cm-1,the content of diamond phase increases gradually as grain size increases,and the amount of trans-polyacetylene(TPA)content decreases.Meanwhile,the sp2 carbon clusters content and its full-width-at-half-maximum(FWHM)value are significantly reduced in MCD film with a grain size of 620 nm,which is beneficial to the improvement of the optical properties of the films.展开更多
Under optimal conditions free-standing high quality diamond films were prepared by DC arc plasma jet CVD method at a growth rate of 7-10 Pm/h. Surface and cross section morphologies of the diamond films were observed ...Under optimal conditions free-standing high quality diamond films were prepared by DC arc plasma jet CVD method at a growth rate of 7-10 Pm/h. Surface and cross section morphologies of the diamond films were observed by SEM. Raman spectrometer wasused to characterize the quality of diamond films. The IR transmittivity measured by IR spectrometer is close to the theoretical value ofabout 71% in the far infrared band. The thermal conductivity measured by photothermal deflection exceeds 18 W/cm' K. <l 10> is thepreferential growth orientation of the films detected by X-ray diffractometer. As s result, the extremely high temperature of DC arc plasma jet can produce supersaturated atomic hydrogen, which played an important role in the process for the deposition of high quality diamond films.展开更多
Tribological properties of chemical vapor deposition (CVD) diamond films greatly affect its application in the mechanical field. In this paper, a novel multilayer structure is proposed, with which multilayer diamond f...Tribological properties of chemical vapor deposition (CVD) diamond films greatly affect its application in the mechanical field. In this paper, a novel multilayer structure is proposed, with which multilayer diamond films are deposited on silicon carbide by hot filament CVD (HFCVD) method. The different micrometric diamond grains are produced by adjusting deposition parameters. The as-deposited multilayer diamond films are characterized by scanning electron microscope (SEM) and white-light interferometry. The friction tests performed on a reciprocating ball-on-plate tribometer suggest that silicon carbide presents the friction coefficient of 0.400 for dry sliding against silicon nitride (Si3N4) ceramic counterface. With the water lubrication, the corresponding friction coefficients of silicon carbide and as-deposited multilayer diamond films further reduce to 0.193 and 0.051, respectively. The worn surfaces indicate that multilayer diamond films exhibit considerably high wear resistance.展开更多
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...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.展开更多
Monte Carlo simulations are adopted to study the electron motion in the mixture of H2 and CH4 during diamond synthesis via Glow Plasma-assisted Chemical Vapor Deposition (GPCVD). The non-uniform electric field is used...Monte Carlo simulations are adopted to study the electron motion in the mixture of H2 and CH4 during diamond synthesis via Glow Plasma-assisted Chemical Vapor Deposition (GPCVD). The non-uniform electric field is used and the avalanche of electrons is taken into account in this simulation. The average energy distribution of electrons and the space distribution of effective species such as CH3, CH+3, CH+ and H at various gas pressures are given in this paper, and optimum experimental conditions are inferred from these results.展开更多
Oxygen-doped diamond films are prepared by implanting various dose oxygen ions into the diamond films synthesized by hot filament chemical vapour deposition, and their electrical and structural properties are investig...Oxygen-doped diamond films are prepared by implanting various dose oxygen ions into the diamond films synthesized by hot filament chemical vapour deposition, and their electrical and structural properties are investigated. Hall effect measurements show that lower dose oxygen ion implantation is beneficial to preparing n-type diamonds. The carrier concentration increases with the dose increasing, indicating that oxygen ions supply electrons to the diamonds. The results of AES spectrum indicate that oxygen ions are doped into the diamond films, and the O-implanted depth is around 0.1μm. Raman spectrum measurements indicate that the lower dose oxygen ion implantation at 10^14 cm^-2 or 10^15 cm^-2 is favourable for producing less damaged O-doDed diamond films.展开更多
基金Project (51005154) supported by the National Natural Science Foundation of ChinaProject (12CG11) supported by the Chenguang Program of Shanghai Municipal Education Commission, ChinaProject (201104271) supported by the China Postdoctoral Science Foundation
文摘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.
基金Project(2012ZX04003-031)supported by the National Science and Technology Major Project,China
文摘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.
基金financial support from the Shanxi Scholarship Council of China(No.2024-057)the Water Conservancy Science and Technology Research and Promotion Project of Shanxi Province,China(No.2025GM13)the National Natural Science Foundation of China(No.52571048).
文摘The heteroepitaxy of diamond films has received widespread attention;however,its application remains limited owing to the mismatch in properties and structure between diamond and heterogeneous substrates.In this study,diamond films were successfully synthesized on high-entropy alloys(HEAs)substrates using microwave plasma chemical vapor deposition.The resulting diamond films were continuous,uniform,and adhered to the HEAs substrates.The mixed carbides were identified using X-ray diffraction,and the quality of the diamond films was examined using Raman spectroscopy.Moreover,the corrosion test revealed that the diamond/TiZrHfMo samples had excellent electrochemical stability and corrosion resistance with a corrosion potential value of-0.169 V in a 3.5wt%NaCl solution.A multiple regression model was established to evaluate the effects of the structure and growth parameters,which confirmed that the mixing entropy significantly affected the grain size and corrosion properties.
文摘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.
基金Project(51275302)supported by the National Natural Science Foundation of ChinaProject(BC2012124)supported by Technical Innovation Funds for the Sci-Tech Enterprise of Jiangsu Province,China
文摘The effects of Si doping on morphology, components and structure characteristics of CVD diamond films were studied. Si-doped CVD diamond films were deposited on Si substrate by adding tetraethoxysilane （TEOS） into acetone as source of reactant gas. The morphology and microstructure of diamond films were characterized by scanning electron microcopy （SEM）. The crystalline quality of diamond films was studied by Raman spectroscopy and X-ray diffractometry （XRD）. The surface roughness of the films was evaluated with surface profilometer. The results suggest that Si doping tends to reduce the crystallite size, enhance grain refinement and inhibit the appearance of （11 I） facets. Raman spectra indicate that Si doping can enhance the formation of sp2 phase in diamond films. Moreover, Raman signal of SiC was detected, which suggests the existence of Si in the diamond films. Smooth fine-grained diamond （SFGD） film was synthesized at Si to C ratio of 1%.
基金Project(20110933K) supported by the State Key Laboratory of Powder Metallurgy,ChinaProject(2012QNZT002) supported by the Freedom Explore Program of Central South University,ChinaProject(CSUZC2012024) supported by the Open-End Fund for the Valuable and Precision Instruments of Central South University,China
文摘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.
基金Projects(51275302,51005154)supported by the National Natural Science Foundation of China
文摘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.
基金This work was partially supported by the National Natural Science Foundation of China （NSFC） under Contract No. 59292800 the Science and Technology Committee of Liaoning Province.
文摘During the growth of the hot filament chemical vapor deposition （HFCVD） diamond films, numerical simulations in a 2-D mathematical model were employed to investigate the influence of various deposition parameters on the gas physical parameters, including the temperature, velocity and volume density of gas. It was found that, even in the case of optimized deposition parameters, the space distributions of gas parameters were heterogeneous due primarily to the thermal blockage come from the hot filaments and cryogenic pump effect arisen from the cold reactor wall. The distribution of volume density agreed well with the thermal round-flow phenomenon, one of the key obstacles to obtaining high growth rate in HFCVD process. In virtue of isothermal boundary with high temperature or adiabatic boundary condition of reactor wall, however, the thermal roundflow was profoundly reduced and as a consequence, the uniformity of gas physical parameters was considerably improved, as identified by the experimental films growth.
文摘Selective deposition of diamond film on patterned Si (100) substrates has been achieved by using microwave plasma chemical vapor deposition (MPCVD) method. The films have been characterized by scanning electron microscope (SEM) and Raman spectrum. The influence of substrate temperature on the nucleation behavior of diamond was discussed in detail and the optimized deposition condition has been obtained.
文摘The etching technique using Ce is a convenient and fast method for polishing and shaping diamond films. In this study, the influence of polishing parameters such as polishing temperature and time on the surface crystallinity and phase composition of diamond films was thoroughly investigated via the analysis of Raman spectra such as FWHM and ID/IG. Moreover, the issue on the graphitization of diamond after polishing with Ce was further researched through the detailed study of the depth distribution of Raman data including FWHM and ID/IG, and a result completely different from the hot-iron metal polished ones was obtained. The results showed that polished diamond films had considerably higher diamond content than those before polishing, and not a bit of graphitization was found in the polished ones, owing to a higher solubility of carbon in rare earth metal Ce than that in transition metals, and the original crystallinity of the films polished with Ce did not deteriorate.
基金financially supported by the National Natural Science Foundation of China (No. 51272024)the Ph.D. Programs Foundation of the Ministry of Education of China (No. 20110006110011)the Fundamental Research Funds for Central Universities (No. FRF-TP-13-035A)
文摘With the advantages of high deposition rate and large deposition area, polycrystalline diamond films prepared by direct current （DC） arc jet chemical vapor deposition （CVD） are considered to be one of the most promising materials for high-frequency and high-power electronic devices. In this paper, high-quality self-standing polycrystalline diamond films with the diameter of 100 mm were prepared by DC arc jet CVD, and then, the p-type surface conductive layer with the sheet carrier density of 10^11-10^13 cm-2 on the H-terminated diamond film was obtained by micro-wave hydrogen plasma treatment for 40 min. Ti/Au and Au films were deposited on the H-terminated diamond surface as the ohmic contact electrode, respectively, afterwards, they were treated by rapid vacuum annealing at different temperatures. The properties of these two types of ohmic contacts were investigated by measuring the specific contact resistance using the transmission line method （TLM）. Due to the formation of Ti-related carbide at high temperature, the specific contact resistance of Ti/Au contact gradually decreases to 9.95 × 10^-5 Ω-cm2 as the temperature increases to 820℃. However, when the annealing temperature reaches 850℃, the ohmic contact for Ti/Au is degraded significantly due to the strong diffusion and reaction between Ti and Au. As for the as-deposited Au contact, it shows an ohmic contact. After annealing treatment at 550℃, low specific contact resistance was detected for Au contact, which is derived from the enhancement of interdiffusion between Au and diamond films.
基金Supported by the National Natural Science Foundation of China under Grant No 11405114the Natural Science Foundation of Shanxi Province under Grant No 2015021065
文摘Cu ion implantation and subsequent rapid annealing at 500℃ in N2 result in low surface resistivity of 1.611 ohm/sq with high mobility of 290 cm2 V-1S-1 for microcrystalline diamond （MCD） films. Its electrical field emission behavior can be turned on at Eo = 2.6 V/μm, attaining a current density of 19.5μA/cm2 at an applied field of 3.5 V/#m. Field emission scanning electron microscopy combined with Raman and x-ray photoelectron mi- croscopy reveal that the formation of Cu nanoparticles in MCD films can catalytically convert the less conducting disorder/a-C phases into graphitic phases and can provoke the formation of nanographite in the films, forming conduction channels for electron transportation.
基金supported by the Science and Technology Major Project of Shanxi Province,China (Grant No. 20181102013)the Fund from the “1331 Project”Engineering Research Center of Shanxi Province,China (Grant No. PT201801)。
文摘Nano-diamond particles are co-deposited on Ti substrates with metal(Ti/Ni) nanoparticles(NPs) by the electrophoretic deposition(EPD) method combined with a furnace annealing at 800℃ under N_(2) atmosphere. Modifications of structural and electron field emission(EFE) properties of the metal-doped films are investigated with different metal NPs concentrations. Our results show that the surface characteristics and EFE performances of the samples are first enhanced and then reduced with metal NPs concentration increasing. Both the Ti-doped and Ni-doped nano-diamond composite films exhibit optimal EFE and microstructural performances when the doping quantity is 5 mg. Remarkably enhanced EFE properties with a low turn-on field of 1.38 V/μm and a high current density of 1.32 mA/cm^(2) at an applied field of 2.94 V/μm are achieved for Ni-doped nano-diamond films, and are superior to those for Ti-doped ones. The enhancement of the EFE properties for the Ti-doped films results from the formation of the TiC-network after annealing. However, the doping of electron-rich Ni NPs and formation of high conductive graphitic phase are considered to be the factor, which results in marvelous EFE properties for these Ni-doped nano-diamond films.
基金financial support from the Project supported by the National Natural Science Foundation of China(Grant No.51202257)Shenyang Double-Hundreds Project(Z17-7-027,Z18-0-025)
文摘In this study, diamond films were synthesized on silicon substrates by microwave plasma enhanced chemical vapor deposition（CVD） over a wide range of experimental parameters. The effects of the microwave power,CH;/H;ratio and gas pressure on the morphology, growth rate, composition, and quality of diamond films were investigated by means of scanning electron microscope（SEM）, X-ray diffraction（XRD）, Raman spectroscopy and X-ray photoelectron spectroscopy（XPS）. A rise of microwave power can lead to an increasing pyrolysis of hydrogen and methane, so that the microcrystalline diamond film could be synthesized at low CH;/H;levels. Gas pressure has similar effect in changing the morphology of diamond films, and high gas pressure also results in dramatically increased grain size. However,diamond film is deteriorated at high CH;/H;ratio due to the abundant graphite content including in the films. Under an extreme condition of high microwave power of 10 kW and high CH;concentration, a hybrid film composed of diamond/graphite was successfully formed in the absence of N;or Ar,which is different from other reports. This composite structure has an excellent measured sheet resistance of 10-100 Ω/Sqr. which allows it to be utilized as field electron emitter. The diamond/graphite hybrid nanostructure displays excellent electron field emission（EFE） properties with a low turn-on field of 2.17 V/μm and β= 3160, therefore it could be a promising alternative in field emission applications.
基金Project supported by the Key Project of the National Natural Science Foundation of China(Grant No.U1809210)the National Natural Science Foundation of China(Grant Nos.50972129 and 50602039)+4 种基金the International Science Technology Cooperation Program of China(Grant No.2014DFR51160)the National Key Research and Development Program of China(Grant No.2016YFE0133200)the European Union’s Horizon 2020 Research and Innovation Staff Exchange(RISE)Scheme(Grant No.734578)the Belt and Road International Cooperation Project from Key Research and Development Program of Zhejiang Province,China(Grant No.2018C04021)the Natural Science Foundation of Zhejiang Province,China(Grant Nos.LQ15A040004 and LY18E020013)
文摘Microcrystalline diamond(MCD)films with different grain sizes ranging from 160 nm to 2200 nm are prepared by using a hot filament chemical vapor deposition(HFCVD)system,and the influences of grain size and structural features on optical properties are investigated.The results show that the film with grain size in a range of 160 nm–310 nm exhibits a higher refractive index in a range of(2.77–2.92).With grain size increasing to 620±300 nm,the refractive index shows a value between 2.39 and 2.47,approaching to that of natural diamond(2.37–2.55),and a lower extinction coefficient value between 0.08 and 0.77.When the grain size increases to 2200 nm,the value of refractive index increases to a value between 2.66 and 2.81,and the extinction coefficient increases to a value in a range of 0.22–1.28.Visible Raman spectroscopy measurements show that all samples have distinct diamond peaks located in a range of 1331 cm-1–1333 cm-1,the content of diamond phase increases gradually as grain size increases,and the amount of trans-polyacetylene(TPA)content decreases.Meanwhile,the sp2 carbon clusters content and its full-width-at-half-maximum(FWHM)value are significantly reduced in MCD film with a grain size of 620 nm,which is beneficial to the improvement of the optical properties of the films.
文摘Under optimal conditions free-standing high quality diamond films were prepared by DC arc plasma jet CVD method at a growth rate of 7-10 Pm/h. Surface and cross section morphologies of the diamond films were observed by SEM. Raman spectrometer wasused to characterize the quality of diamond films. The IR transmittivity measured by IR spectrometer is close to the theoretical value ofabout 71% in the far infrared band. The thermal conductivity measured by photothermal deflection exceeds 18 W/cm' K. <l 10> is thepreferential growth orientation of the films detected by X-ray diffractometer. As s result, the extremely high temperature of DC arc plasma jet can produce supersaturated atomic hydrogen, which played an important role in the process for the deposition of high quality diamond films.
基金the National Natural Science Foundation of China (No. 50975177)
文摘Tribological properties of chemical vapor deposition (CVD) diamond films greatly affect its application in the mechanical field. In this paper, a novel multilayer structure is proposed, with which multilayer diamond films are deposited on silicon carbide by hot filament CVD (HFCVD) method. The different micrometric diamond grains are produced by adjusting deposition parameters. The as-deposited multilayer diamond films are characterized by scanning electron microscope (SEM) and white-light interferometry. The friction tests performed on a reciprocating ball-on-plate tribometer suggest that silicon carbide presents the friction coefficient of 0.400 for dry sliding against silicon nitride (Si3N4) ceramic counterface. With the water lubrication, the corresponding friction coefficients of silicon carbide and as-deposited multilayer diamond films further reduce to 0.193 and 0.051, respectively. The worn surfaces indicate that multilayer diamond films exhibit considerably high wear resistance.
基金Project(21271188)supported by the National Natural Science Foundation of ChinaProject(2012M521541)supported by the China Postdoctoral Science Foundation,China+2 种基金Project(2012QNZT002)supported by the Fundamental Research Funds for the Central Universities,ChinaProject(20110933K)supported by the State Key Laboratory of Powder Metallurgy,ChinaProject(CSUZC2013016)supported by the Open-End Fund for Valuable and Precision Instruments of Central South University,China
文摘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.
基金This work was supported by Doctor Foundation of Hebei Education Committee Hebei Natural Science Foundation(599091 ) of China
文摘Monte Carlo simulations are adopted to study the electron motion in the mixture of H2 and CH4 during diamond synthesis via Glow Plasma-assisted Chemical Vapor Deposition (GPCVD). The non-uniform electric field is used and the avalanche of electrons is taken into account in this simulation. The average energy distribution of electrons and the space distribution of effective species such as CH3, CH+3, CH+ and H at various gas pressures are given in this paper, and optimum experimental conditions are inferred from these results.
文摘Oxygen-doped diamond films are prepared by implanting various dose oxygen ions into the diamond films synthesized by hot filament chemical vapour deposition, and their electrical and structural properties are investigated. Hall effect measurements show that lower dose oxygen ion implantation is beneficial to preparing n-type diamonds. The carrier concentration increases with the dose increasing, indicating that oxygen ions supply electrons to the diamonds. The results of AES spectrum indicate that oxygen ions are doped into the diamond films, and the O-implanted depth is around 0.1μm. Raman spectrum measurements indicate that the lower dose oxygen ion implantation at 10^14 cm^-2 or 10^15 cm^-2 is favourable for producing less damaged O-doDed diamond films.
