Preparation of Nano-Crystalline Diamond Films on Poly-Crystalline Diamond Thick Films by Microwave Plasma Enhanced Chemical Vapor Deposition

Nano-crystalline diamond （NCD） films were prepared on poly-crystalline diamond （PCD） thick flims by the microwave plasma enhanced chemical vapor deposition （MPCVD） method. Free standing PCD thick film （50 mm in diameter） with a thickness of 413 μm was deposited in CHn/H2 plasma. It was then abraded for 2 hours and finally cut into pieces in a size of 10×10 mm^2 by pulse laser. NCD fihns were deposited on the thick film substrates by introducing a micro-crystalline diamond （MCD） interlayer. Results showed that a higher carbon concentration （5%） and a lower substrate temperature （650℃） were feasible to obtain a highly smooth interlayer, and the appropriate addition of oxygen （2%） into the gas mixture was conducive to obtaining a smooth nano-crystalline diamond film with a tiny grain size.

Effect of Gas Sources on the Deposition of Nano-Crystalline Diamond Films Prepared by Microwave Plasma Enhanced Chemical Vapor Deposition

Nano-crystalline diamond （NCD） films were deposited on silicon substrates by a microwave plasma enhanced chemical vapor deposition （MPCVD） reactor in C2H5OH/H2 and CH4/H2/O2 systems, respectively, with a constant ratio of carbon/hydrogen/oxygen. By means of atomic force microscopy （AFM） and X-ray diffraction （XRD）, it was shown that the NCD films deposited in the C2H5OH/H2 system possesses more uniform surface than that deposited in the CH4/H2/O2 system. Results from micro-Raman spectroscopy revealed that the quality of the NCD films was different even though the plasmas in the two systems contain exactly the same proportion of elements. In order to explain this phenomenon, the bond energy of forming OH groups, energy distraction in plasma and the deposition process of NCD films were studied. The experimental results and discussion indicate that for a same ratio of carbon/hydrogen/oxygen, the C2H5OH/H2 plasma was beneficial to deposit high quality NCD films with smaller average grain size and lower surface roughness.

Effect of nitrogen on deposition and field emission properties of boron-doped micro-and nano-crystalline diamond films

In this paper,we report the effect of nitrogen on the deposition and properties of boron doped diamond films synthesized by hot filament chemical vapor deposition.The diamond films consisting of micro-grains(nano-grains) were realized with low(high) boron source flow rate during the growth processes.The transition of micro-grains to nano-grains is speculated to be strongly(weekly) related with the boron(nitrogen) flow rate.The grain size and Raman spectral feature vary insignificantly as a function of the nitrogen introduction at a certain boron flow rate.The variation of electron field emission characteristics dependent on nitrogen is different between microcrystalline and nanocrystalline boron doped diamond samples,which are related to the combined phase composition,boron doping level and texture structure.There is an optimum nitrogen proportion to improve the field emission properties of the boron-doped films.

Preparation and characterization of nano-crystalline diamond films on glass substrate

Adherent nano diamond films were successfully deposited on glass substrate bymicrowave plasma assisted CVD method in H_2-CH_4 and Ar-CH_4 environment. Raman, AFM (Atomic ForceMicroscope), TEM (Transmission Electron Microscope), FTIR, and Nano Indentation techniques were usedfor characterization of the obtained nano diamond films. It was found that the average grain sizewas less than 100 nm with a surface roughness value as low as 2 nm. The nano diamond films werefound to have excellent transparency in visible and IR spectrum range, and were as hard as naturaldiamond. Experimental results were presented. Mechanisms for nano diamond film deposition werediscussed.

Ellipsometric analysis and optical absorption characterization of nano-crystalline diamond film

A nano-crystalline diamond (NCD) film with a smooth surface was successfully deposited on silicon by a hot filament chemical vapor deposition (HFCVD) method. Scanning electron microscopy (SEM), atomic force microscopy (AFM), RAMAN scattering spectra, as well as spectroscopic ellipsometry were employed to characterize the as-grown film. By fitting the spectroscopic ellipsometric data in the energy range of 0.75?1.50 eV with a three-layer model, Si|diamond+non-diamond|diamond+ non-diamond+void|air, the optical constants are obtained. The refractive index of the NCD film varies little from 2.361 to 2.366 and the extinction coefficient is of the order of 10?2. According to the optical transmittance and absorption coefficient in the wavelength range from 200 to 1 100 nm, the optical gap of the film is estimated to be 4.3 eV by a direct optical transition mechanics.

Deposition and Boron Doping of Nano-Crystalline Diamond Thin Films on Poly-Crystalline Diamond Thick Films

Boron-doped nano-crystalline diamond （NCD） thin films have been successfully deposited on well-polished poly-crystalline diamond （PCD） thick films in a microwave plasma enhanced chemical vapor deposition （MPCVD） reactor for the first time. Different surface pretreatment techniques are carried out under different gas conditions （CH4, H2, Ar, and CH4/H2） to eliminate the effect of grain boundaries on the growth of a smooth NCD intrinsic layer. Well doped NCD films have been fabricated in CH4/H2/B2H6 plasma by varying the atomic ratio of B/C and the substrate temperature. Atomic force microscopy （AFM） results show that pretreatment in pure CH4 plasma at 1000℃ is most effective for NCD growth, while hydrogen containing plasma is harmful to the surface smoothness of NCD thin fihns. Doping research indicates that the optimum parameters for the boron-doping of high-quality NCD thin films are B/C=300 ppm （10-6） and 800℃.

Plasma Processing of Boron-Doped Nano-Crystalline Diamond Thin Film Fabricated on Poly-Crystalline Diamond Thick Film

Plasma treatments of boron-doped nano-crystalline diamond （NCD） thin films were carried out in order to improve their electrical properties of the films. Boron-doped NCD thin films were fabricated on well polished poly-crystalline diamond （PCD） thick films in a microwave plasma enhanced chemical vapor deposition （MPCVD） reactor, then they were processed in methane, ar- gon, hydrogen and B2H~ （0.1% diluted by H~） plasmas, respectively. Scanning electron microscopy （SEM） and atomic force microscope （AFM） results show that the surface morphology changed lit- tle during the 10 min treatment. Secondary ion mass spectroscopy （SIMS） results indicate that B2H6 plasma was efficient for increasing boron concentration in NCD films, while the carrier anal- yses demonstrates that CH4 plasma processing was effective to activate the dopants and resulted in good electrical properties.

PREPARATION OF NANO-CRYSTALLINE Fe-Cu THIN FILMS AND THEIR MAGNETIC PROPERTIES

Fe-Cu thin films of 0.2 mum in thickness with different Cu contents wereprepared by using r.f. magnetron sputtering onto glass substrate. The effect of sputteringparameters, including Ar gas pressure and input rf power, on the structure and magnetic propertieswas investigated. It was found that when the power is lower than 70W, the structure of the filmsremained single bcc-Fe phase with Cu solubility of up to 50at. percent. TEM observations for thebcc-Fe phase showed that the grain size was in the nanometer range of less than 20nm. The coercivityof Fe- Cu films was largely affected by not only Ar gas pressure but also rf power, and reachedabout 2.5Oe in the pressure of 0.67-6.67Pa and in the power of less than 100W. In addition,saturation magnetization, with Cu content less than 60at. percent, was about proportional to thecontent of bcc-Fe. When Cu content was at 60at. percent, however, saturation magnetization was muchsmaller than its calculation value.

Brightness of Blue/Violet Luminescent Nano-Crystalline AZO and IZO Thin Films with Effect of Layer Number:For High Optical Performance

From different reports, it （AZO） and indium-doped including usage areas. We nanocrystalline films with is realized that there is a need to consider all sides of aluminum-doped zinc oxide zinc oxide （IZO） thin films with their optical, luminescence and surface properties establish an assessment to carry out further information to summarize AZO and IZO impact of the layer number.

Hexagonal Nano-Crystalline BCN Films Grown on Si (100) Substrate Studied by X-Ray Absorption Spectroscopy

Hexagonal nano-crystalline boron carbonitride (h-BCN) films grown on Si (100) substrate have been precisely investigated. The films were synthesized by radio frequency plasma enhanced chemical vapor deposition using tris-dimethylamino borane as a single-source molecular precursor. The deposition was performed by setting RF power at 400 - 800 W. The reaction pressure was at 2.6 Pa and the substrate temperature was recorded at 700°C - 800°C. Formation of the nano-crystalline h-BCN compound has been confirmed by X-ray diffraction analysis. The diffraction peaks at 26.3° together with a small unknown peak at 29.2° were elucidated due to the formation of an h-BCN structure. The films composed of B, C, and N atoms with different B-N, B-C, C-N chemical bonds in forming the sp2-BCN atomic configuration studied by X-ray photoelectron spectroscopy. Orientation and local structures of the h-BCN hybrid were studied by near-edge X-ray absorption fine structure (NEXAFS) measurements. The dominant presence of p* and s* resonance peaks of the sp2-hybrid orbitals in the B K-edge NEXAFS spectra revealed the formation of the sp2-BCN configuration around B atoms like-BN3 in h-BN. The orientation was suggested on the basis of the polarization dependence of B K-edge and N K-edge of the NEXAFS spectra.

Numerical Analysis of Nd:YAG Pulsed Laser Polishing CVD Self-standing Diamond Film

Chemical vapor deposited （CVD） diamond film has broad application foreground in high-tech fields. But polycrystalline CVD self-standing diamond thick film has rough surface and non-uniform thickness that adversely affect its extensive applications. Laser polishing is a useful method to smooth self-standing diamond film. At present, attentions have been focused on experimental research on laser polishing, but the revealing of theoretical model and the forecast of polishing process are vacant. The paper presents a finite element model to simulate and analyze the mechanism of laser polishing diamond based on laser thermal conduction theory. The experimental investigation is also carried out on Nd：YAG pulsed laser smoothing diamond thick film. The simulation results have good accordance with the results of experimental results. The temperature and thermal stress fields are investigated at different incidence angles and parameters of Nd：YAG pulsed laser. The pyramidal-like roughness of diamond thick film leads to the non-homogeneous temperature fields. The temperature at the peak of diamond film is much higher than that in the valley, which leads to the smoothing of diamond thick film. The effect of laser parameters on the surface roughness and thickness of graphite transition layer is also carried out. The results show that high power density laser makes the diamond surface rapid heating, evaporation and sublimation after its graphitization. It is also found that the good polish quality of diamond thick film can be obtained by a combination of large incident angle, moderate laser pulsed energy, large repetition rate and moderate laser pulse width. The results obtained here provide the theoretical basis for laser polishing diamond film with high efficiency and high quality.

AFM Study on Interface of HTHP As-grown Diamond Single Crystal and Metallic Film

The study for the interface of as-grown diamond and metallic film surrounding diamond is an attractive way for understanding diamond growth mechanism at high temperature and high pressure (HTHP), because it is that through the interface carbon atom groups from the molten film are transported to growing diamond surface. It is of great interest to perform atomic force microscopy (AFM) experiment; which provides a unique technique different from that of normal optical and electron microscopy studies, to observe the interface morphology. In the present paper, we report first that the morphologies obtained by AFM on the film are similar to those of corresponding diamond surface, and they are the remaining traces after the carbon groups moving from the film to growing diamond. The fine particles and a terrace structure with homogeneous average step height are respectively found on the diamond (100) and (111) surface. Diamond growth conditions show that its growth rates and the temperature gradients in the boundary layer of the molten film at HTHP result in the differences of surface morphologies on diamond planes, being rough on (100) plane and even on the (111) plane. The diamond growth on the (100) surface at HPHT could be considered as a process of unification of these diamond fine particles or of carbon atom groups recombination on the growing diamond crystal surface. Successive growth layer steps directly suggest the layer growth mechanism of the diamond (111) plane. The sources of the layer steps might be two-dimensional nuclei and dislocations.

Simulations of the Dependence of Gas Physical Parameters on Deposition Variables during HFCVD Diamond Films

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.

Microwave CVD Thick Diamond Film Synthesis Using CH4/H2/H2O Gas Mixtures

Thick diamond films with a thickness of up to 1.2 mm and a area of 20 cm^2 have been grown in a homemade 5 kW microwave plasma chemical vapor deposition （MPCVD） reactor using CH4/H2/H2O gas mixtures. The growth rate, radial profiles of the film thickness, diamond morphology and quality were evaluated with a range of parameters such as the substrate temperature of 700℃ to 1100℃, the fed gas composition CH4/H2 = 3.0%, H2O/H2 = 0.0%,-2.4%. They were characterized by scanning electron microscopy and Raman spectroscopy. Translucent diamond wafers have been produced without any sign of non-diamond carbon phases, Raman peak as narrow as 4.1 cm^-1. An interesting type of diamond growth instability under certain deposition conditions was observed in a form of accelerated growth of selected diamond crystallites of a very big lateral size, about 1 mm, and of a better structure compared to the rest of the film.

Fabrication and Characterization of FeNiCr Matrix-TiC Composite for Polishing CVD Diamond Film

Dynamic friction polishing （DFP） is one of the most promising methods appropriate for polishing CVD diamond film with high efficiency and low cost. By this method CVD diamond film is polished through being simply pressed against a metal disc rotating at a high speed utilizing the thermochemical reaction occurring as a result of dynamic friction between them in the atmosphere. However, the relatively soft materials such as stainless steel, cast iron and nickel alloy widely used for polishing CVD diamond film are easy to wear and adhere to diamond film surface, which may further lead to low efficiency and poor polishing quality. In this paper, FeNiCr matrix-TiC composite used as grinding wheel for polishing CVD diamond film was obtained by combination of mechanical alloying （MA） and spark plasma sintering （SPS）. The process of ball milling, composition, density, hardness, high-temperature oxidation resistance and wear resistance of the sintered piece were analyzed. The results show that TiC was introduced in MA-SPS process and had good combination with FeNiCr matrix and even distribution in the matrix. The density of composite can be improved by mechanical alloying. The FeNiCr matrix-TiC composite obtained at 1273 K was found to be superior to at 1173 K sinterin8 in hardness, high-temperature oxidation resistance and wearability. These properties are more favorable than SUS304 for the preparation of high-performance grinding wheel for polishing CVD diamond film.

A CVD diamond film detector for pulsed proton detection

A chemical vapour deposition （CVD） diamond film detector was prepared and the main characteristics for pulsed proton detection were studied at Beijing Tandem Accelerator. The result shows that the charge collection efficiency of the detector increases with increasing electric field intensity and reaches to 9.44% at 5 V/μm with the charge collection distance of 15.9 μm. The relationship between the sensitivity of the detector and proton energy is consistent with the Monte Carlo （MC） simulation result. Its plasma time for a pulse with 4.85×10^5 protons is 1l.2ns. The dose threshold for onset of damage under 9MeV proton irradiation in the detector is about 10^13 cm^-2. All of the results show that a CVD diamond detector has fast time response and high radiation hardness, and can be used in pulsed proton detection.

Microwave Plasma Chemical Vapor Deposition of Diamond Films on Silicon From Ethanol and Hydrogen

Diamond films with very smooth surface and good optical quality have been deposited onto silicon substrate using microwave plasma chemical vapor deposition (MPCVD) from a gas mixture of ethanol and hydrogen at a low substrate temperature of 450 ℃. The effects of the substrate temperature on the diamond nucleation and the morphology of the diamond film have been investigated and observed with scanning electron microscopy (SEM). The microstructure and the phase of the film have been characterized using Raman spectroscopy and X-ray diffraction (XRD). The diamond nucleation density significantly decreases with the increasing of the substrate temperature. There are only sparse nuclei when the substrate temperature is higher than 800 ℃ although the ethanol concentration in hydrogen is very high. That the characteristic diamond peak in the Raman spectrum of a diamond film prepared at a low substrate temperature of 450 ℃ extends into broadband indicates that the film is of nanophase. No graphite peak appeare

Effects of Alcohol Addition on the Deposition of Diamond Thick Films by dc Plasma Chemical Vapor Deposition Method

Diamond films have been deposited by dc plasma chemical vapor deposition method.The addition of alcohol in the resource gas largely increases the deposition rate.The effects of alcohol addition on deposition rate and film quality are analyzed by scanning electron microscopy and Raman spectrometry.The mechanism of experimental phenomena is discussed.

A MONTE CARLO SIMULATION OF THE CVD DIAMOND FILM

A Monte Carlo algorithm has been developed by the authors to simulate the chemical vapor deposition (CVD) processes of diamond films. The method considers both the diffusion and the incorporation of the growth radicals on the growing surface in simulating the evolution of the morphology and microstructure. The calculation of configuration energy is used to determine the orientation of adsorbed growth radicals. The effect of processing variables such as nucleation density and substrate temperature on the morphology and microstructure is discussed. It is found that competitive characteristic and coarsening effect exist in the simulation results, which agree with the experimental observations.

A novel approach of deposition for uniform diamond films on circular saw blades

Uniform diamond films are highly desirable for cutting industries, due to their high performance and long lifetime used on cutting tools. Nevertheless, they are difficult to obtain on cutting tools with complicated shapes, greatly limiting the applications of diamond films. In this study, a novel approach of deposition for uniform diamond films is proposed, on circular saw blades made of cemented carbide using reflectors of brass sheets. Diamond films are deposited using hot filament chemical vapor deposition（HFCVD）. A novel concave structure of brass sheets is designed and fabricated, improving the distribution of temperature field, and overcoming the disadvantages of the conventional HFCVD systems. This increases the energy efficiency of use without changing the structure and increasing the cost of HFCVD. The grains are refined and the intensities of diamond peaks are strengthened obviously, which is confirmed by scanning electron microscopy and Raman spectra respectively.