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To deposited a hydrogenated nanocrystalline cubic silicon carbide (nc-3C-SiC:H) film onto silicon substrate at low temperature.
To characterize the deposited film in terms of their structure, chemical composition, surface morphology, and optical properties.
SCOPE OF THE STUDY
Scope of this study is:
Study of the nc-3C-SiC:H film and HMCVD method.
Design and construction the equipment of the hot mesh chemical vapour deposition (HM-CVD) system.
Leakage and heating testing for the HM-CVD system.
Evaluation of hydrogen atom density on a tungsten mesh surface.
Growth a hydrogenated nanocrystalline cubic silicon carbide (nc-3C-SiC:H) film onto silicon substrate at low temperature.
Characterize of the nc-3C-SiC:H film on Si Substrate.
THE IMPORTANCE OF STUDY
The importance of this study on the project is:
HM-CVD method is a simple method to growth nc-3C-SiC: H film on Si substrate compared PECVD and MBE method.
Can be developed to growth nc-3C-SiC: H film on Si substrate in the large area deposition.
Can be used to growth nc-3C-SiC: H film on Si substrate at low temperature.
Can be generated a high density hydrogen radical by catalytic reaction on the hot mesh tungsten wire surface.
Can be developed nc-3C-SiC: H film on Si substrate for high temperature and high power devices.
In recent years there has been increasing interest and research into silicon carbide (SiC) as a semiconductor for use in high temperature, high power and high operating condition under which the silicon and the III-V semiconductors. The growth of the SiC film on silicon substrate are usually prepared by the atmospheric pressure chemical vapour deposition (APCVD), low pressure CVD or plasma enhance CVD method. The problem for that method mention above is diffusion limited rather than surface controlled, there is worry of the influence of plasma damage, the high temperature are usually required for fabrication and the high density radical hydrogen cannot be easily produced. The hot mesh chemical vapour deposition (HMCVD) method was developed to overcome these problem because that technique is one of the most method for growth nc-3C-SiC: H film on Si substrate at low temperature and large area deposition of functional thin film. In this study will be design and construction of the HMCVD apparatus to growth nc-3C-SiC: H film on Si substrate.
The HMCVD method is low cost apparatus, low temperature deposition, low damage deposition and high radical hydrogen generated. Furthermore, successful outcomes of this research may open an avenue for the use of SiC films for many purposes, including the high temperature and high power devices, solar cells, hetero bipolar transistor, piezoresistive sensor and MEMS application.
Introduction of the Silicon Carbide (SiC)
Materials technology in the next future, humanities strife to further miniaturize, accelerated and expedite the virtual word grows increasingly stronger, where in the new millennium the materials supposed to become bigger, better and faster operation so the materials old will no longer suffice. Silicon carbide (SiC), a hard dense synthetically produced compound of Si and C atom, has been the focus material for the future of many industrial application. The unique properties such as large energy band gap (2.2 eV), a high saturated drift velocity (2.7 x 107 cm s-1), large breakdown field (5 x 106 V cm-1), high thermal conductivity (5 Wcm-1 K-1) and good chemical stability its possible use in high-power, high-frequency and high-temperature devices. These properties are also well suited for use some devices such as a window layer of solar cell , high current gain heterojunction bipolar transistors (HBTs)  and microelectromechanical system (MEMS) .
SiC exists as a large family of crystals known as polytypes, which the difference between the polytypes is the stacking order between succeeding double layers of carbon and silicon atoms. All polytypes have a hexagonal frame with a carbon atom situated above the centre of triangle of Si atoms and underneath a Si atom belonging to the next layer (Figure 1). They are named according to their structure (i.e. cubic, hexagonal, etc...) and the periodicity of repetition the atomic layer. For example the 3C polytype (which is the only cubic form of SiC) has a cubic structure and the same arrangement repeats every 3 layers. Table 1, shows some other common SiC polytypes. The most common cubic and hexagonal SiC lattice structures and their stacking patterns are shown in Figure 2 .
Figure 1. The tetragonal bonding of a carbon atom with nearest silicon neighbour
Table 1. Common SiC polytypes
Figure 2. The stacking sequence of the most common SiC polytypes
SiC deposited in the form of thin film is fairly recent and highly researched technology. The range of work includes crystalline SiC thin films created at high temperature and low pressures to amorphous SiC at low temperature and high pressure. Many deposition techniques exist, with the most common being chemical vapour deposition (or some form of it) and physical vapour deposition. Applications of the SiC film are mainly geared towards the microelectronic and semiconductor industries.
Much of the work done to date has used corning 1737 glass, quartz and silicon as the substrate materials. The aim of the present work is to create hydrogenated nanocrystalline cubic SiC (nc-3C-SiC: H) thin film at low temperature using hot mesh chemical vapour deposition method and to examine the material properties of such film. The SiC films were deposited onto silicon substrate with varying deposition time, filament temperature, and distance between substrate and the mesh tungsten wire. These parameters were optimized to create the best films.
CVD method for Silicon Carbide thin film
Ohno et. al.  have prepared 4H-SiC single crystal by hot wall type CVD method using Silane (SiH4) and propane (C3H8) for source gases with a H2 carrier gas. The catalytic CVD technique for preparation b-SiC thin film has been reported by Zhao et al. , where nanocrystalline b-SiC thin films were epitaxally grown on Si(100) substrate using SiH4, CH4 and H2 gas. The tungsten wire filament was fixed at 2000°C and substrate temperature was 300°C. Thereafter, the deposition time to growth the annocrystalline b-SiC thin film was controlled for 110 minutes.
Miyajima et al.  have successfully deposited µc-3C-SiC:H films from a mixture of monomethylsilane (SiH3CH3) and hydrogen (H2). The deposition was performed in a hot wire CVD (HWCVD) at low temperature and a pressure was kept constant at 100 Pa. The filament temperature is 1400°C by DC current. The flow rate gas of H2 was kept constant at 200 sccm and SiH3CH3 flow rate was 0.8 - 1.6 sccm. The study confirmed that the influence hydrogen dilution ratio on film properties. It was found that the film deposited with low hydrogen dilution ratio had a lower defect density than the film deposited with high hydrogen dilution ratio. These result suggested that high-quality µc-3C-SiC:H films can be obtained under the low hydrogen dilution condition.
Polycrystalline 3C-SiC films deposited from a mixture of silane and propane as procursors and hydrogen as carrier gas were investigated by Ricciardi et al. . The films were deposited using the ultra high vacuum cold wall vertical (LPCVD) reactor onto silicon substrate at pressure was 10 Torr and the temperature 1000°C. The H2 gas flow rate was 1200 sccm. The presence oriented structures in the SiC films were checked by Selected Area electron diffraction (SAD) patterns. It was observed that the major growth directions were in the (110) oriented planes.
Tabata et al.  conducted a study properties of nanocrystalline cubic silicon carbide thin films on corning 1737 glass substrate for use in the thin film solar cells. They used hot wire CVD (HWCVD) method with SiH4, CH4 and H2 gases. Before the deposition, the tungsten wire was heated at 2000°C in H2 atmosphere to eliminate oxygen. During deposition the filament temperature was kept at 1800°C and the substrate temperature was varied between 104 and 434°C. The XRD patterns of the nc-3C-SiC thin film was observed that the major growth direction were in the (111), (220) and (311) planes. These finding indicates that nc-3C-SiC:H grew at substrate temperature above 187°C. On the other hand, for the substrate temperature lower than 187°C (Ts = 104°C), no XRD peak attributed to nc-3C-SiC:H was observed, indicating that the amorphous.
Crystalline SiC films deposited by monomethylsilane as a source gas and hydrogen as carrier gas using hot mesh chemical vapour deposition (HMCVD) method were studied by Yasui et al.  and Narita et al. . The main focus study from that researcher was to growth the SiC thin film with low temperature deposition and developed the HMCVD to be effective method to growth SiC film. Two method of deposition were used, they are PECVD and HMCVD method with a monomethylsilane and hydrogen gases. They are reported that the HMCVD method was very effective for SiC growth on Si substrate at low temperature.
Hot Mesh Chemical Vapour Deposition Method (HMCVD)
The catalytic chemical vapor deposition (cat-CVD) or hot wire CVD (HWCVD) or hot mesh CVD (HMCVD) is included in the cold wall reactor and that is the same way to crate the radical hydrogen generated. HMCVD method is one of the promising techniques for the low temperature composition and large area deposition of functional thin film. The HMCVD apparatus consists of three parts: 1) the part for gas inlet into the low pressure deposition chamber, 2) the part for gas decomposition via catalytic cracking reaction at the surface of a heated catalyzer, and 3) the substrates for film formation using decomposed species transported from the catalyzer .
The benefit of the HMCVD method is its high gas decomposition efficiency and a simple method compared with molecular beam epitaxial and plasma enhance chemical vapour deposition method. An easy creation of hydrogen radical generation with high concentration and no ion damage during a cracking reaction process. An easily applicable to deposition on large area substrate compared with MBE method. Scaling to large areas merely requires an increase in catalytic surface along with a proportionally larger supply of source gases. Substrate can be easily be handled as they do not have a role in the decomposition process. Step coverage is excellent, and uniformity can easily be optimized as substrates can be moved during deposition.
The catalytic CVD method was developed by Weismann et. al. in 1979  to overcome the problem arising in the PCVD processes. They are reported that silicon thin films could be formed by cracking silane gas with a heated tungsten or carbon filament. However, their attempt was not successful because the photoconductivity and the photosensitivity of their a-Si films were much worse than those obtained by PCVD at that time. In 1985, Weismann and his group succeeded in obtaining an excellent quality of hydrofluorinated a-Si (a-SiF:H) by mixing intermediate species, silicon difluoride (SiF2) with atomic hydrogen generated by catalytic reaction of hydrogen gas with a heated tungsten catalyzer placed near the substrate. These successful results appeared to encourage some researcher to start similar study using that method with other materials. Conceptual on catalytic reaction or cracking reactions in W-mesh can be shown in the Figure 3.
Figure 3. A Conceptual of cracking reaction of HMCVD process.
From the Figure 3, can be seen a hydrogen molecule is dissociatively adsorbed on the surface of tungsten (W) wire at high temperature, the reaction on the surface goes on and major decomposition configuration becomes H radical (H* is hydrogen active). The precursor gas in this study was used monomethylsilane (MMS). The MMS gas was supplied directly onto the substrate surface with the temperature of the substrate was lower than mesh wire temperature. The MMS gas will be adsorb on the silicon substrate to make a SiC bond. In the process of the SiC film, they are have three type of bonding, i.e. C-H bond (strong bond), Si-C (middle bond) and Si-H (weak bond). Hydrogen on the Si-H bond will be adsorb of the Si substrate where it is heating a certain temperature. When the hydrogen was adsorb so the dangling bond will be occurred in the substrate surface. The H radical from the decomposition process on the tungsten mesh wire will be change the dangling bond.
In this case, when a MMS gas stays for a long period by making a bond with a tungsten active site, W-silicide will be stars to grow. The silicide is growing on the W mesh and finally the catalyzer is broken. However, when the W temperature is higher than a certain temperature, W-silicide not be occur. Matsumura et. al. , reported the W-silicide can be avoided when the W temperature is higher than 1600°C.
The deposition mechanism has been extensively studied and various application have been attempted to explore new field. The kind of films prepared by this technique is expanding. Amorphous silicon (a-Si) [13,14], amorphous silicon carbide (a-SiC) [15,16], amorphous carbon , silicon nitride (SiNx) , Silicon dioxide (SiO2) , Aluminum oxide (Al2O3) , gallium nitrid (GaN) [21-25], polycrystalline silicon (poly-Si) , carbon doped silicon oxide (Si-O-C) , carbon doped silicon nitride (Si-N-C) , diamond [28,29], carbon nanotube , carbon nanowall [31,32], carbon nano particle , poly-tetra-fluoro-ethylene (PTFE) and poly-glycidyl-methacrylate (PGMA) , nanocrystalline cubic silicon carbide (nc-3C-SiC:H) [34,35], Titanium oxide (TiO2) , and SiC on Insulator (SiCOI) . The example of application of cat-CVD technology, reported so far, are summarized in Table 2  and the current technologies using SiC thin films are shown in Table 3.
Table 2. Examples of application of cat-CVD technology
Features of cat -CVD
GaAs or GaN devices
Synthesis of organic compounds
Bio- and medical component
Gate side wall
Gas -barrier films
Coating of CNT TFT
TFT for LCD
Coat of glass or organic substrate
Photo receptor of copier
a-Si solar cells
a-Si for HIT solar cells
Anti reflection coating
Gas barrier for food rapping
Surface modification of fibers
Surface coating, alternative to electro deposition
Organic synthesis by selected species
Photo- resist removal by H
Good step coverage
Low H contents
High gas barrier ability
Low deposition temperature
High efficiency of gas use
High rate deposition
Low cost apparatus
Highly photo conductive a-Si
High efficiency of gas use
Low photo degradation
Low damage deposition
High gas barrier ability
Low temperature deposition
Water resistive films
Low friction films
High rate deposition
High gas barrier ability
Free from electric discharge
Low temperature deposition
Low damage deposition
Low temperature deposition
Low damage deposition
Formation of low stress films
Generation of high density H atoms and radical
Table 3. SiC thin films properties and current typical application
SiC thin film
High stiffness and high thermal stability mirrors used for ground based and space based telescopes and directed energy application
Coating for nozzles and seals etc... where a long life and low wear rate are necessary. Can be up to 3 to 6 times longer lasting than conventional sintered SiC.
High temperature MOSFET
High temperature Power Thyristor
Low kdielectric materials
Literature Review of nc-3C-SiC:H, and HMCVD system
Design reactor chamber and prepare HMCVD vacuum system
Installation of chamber reactor and vacuum system
Leakage and heating testing (ULVAC company)
Installation of a HMCVD system (Ibnu Sina Institute Laboratory)
Growth and fabrication of nc-3C-SiC:H by using HMCVD system
Characterization of the nc-3C-SiC:H film sample
Analysis and optimation parameter
Final Report (Writing)
Submitted to SPS
Design Reactor chamber and construction of HMCVD system
In this study, the HMCVD system will be designed and constructed in our laboratory (Nanostructures and Nanophysics Laboratory, IIS, UTM). The schematic of HMCVD system can be shown in Figure 4.
Figure 4. A schematic of HMCVD system
Research Material and Equipment
In this research was used some materials such as source gas, substrate, and W-mesh wire. Source gas was used in here is monomethylsilane, hydrogen and nitrogen gas. The equipment to growth of the nc-3C-SiC:H film by using HMCVD system.
The step of the pre-treatment process in this study is cutting and cleaning process. In the cutting process, the silicon (Si) wafer will be cuted using diamond scriber for obtaining 15 x 15 mm size substrate sample. Furthermore, in the cleaning process, the part of the Si wafer is an ultrasonic immersion of the methanol, acetone, and HF solution. Each of the ultrasonic immersion takes up to 5 minutes and rinsing in de-ionized water for 2 minute. The last step in the cleaning process is blow dries Si wafer with nitrogen air before insert to the chamber reactor. This process is needed to make sure the Si wafer is clean enough and free of any particles for the following process.
Deposition Process (Growth sample)
In this study, we will try to growth the nc-3C-SiC: H thin film sample on Si substrate using HMCVD method. The deposition parameter will be varied in order to find the optimum condition in which a good quality sample to nanoelectronics devices.
The flow chart of the research methodology is proposed as shown as in Figure 5.
Figure 5. Research methodology flowchart
Characterization of the hydrogenated nanocrystalline cubic silicon carbide (nc-3C-SiC:H)
Sic materials in nanometer scale have been studied over many years and many physical, chemical and thermal properties related to the nanometer size have been reported. One of the critical challenges faced currently by researcher in the nanotechnology and nanoscience field is the inability and the lack of the instruments to observe, measure, and manipulate the materials at the nanometer level by manifesting at the microscopic level. In the past, the studies have been focused mainly on the collective behaviours and properties of the large number of nanostructure materials. The properties and behaviours observed and measured are typically group characteristics .
A better fundamental understanding and various potential applications increasingly demand the ability and instrumentation to observe measure and manipulate the individual nanomaterials and nanostructures. Characterizations of individual nanostructure require extreme sensitivity, extreme accuracy, and atomic level resolution. Various microscopies will play a central role in characterization and measurements of nanostructures materials.
X-ray Diffraction (XRD)
XRD is a very important experiment technique that has long used to address all issue related to the crystal structure of solid, including lattice constans and geometry, identification of unknown materials, orientation of single crystals, preferred orientation of polycrystals, defect, stresses, etc.
The vitreous state was determined by X-ray diffraction (XRD) analysis to conform the sample is crystal or amorphous. A relatively fine powder is placed on the aluminium holder and the XRD analysis was done using Philips Analytical X-Ray Diffractometer with CuKÎ± radiation and Î» = 1.5408Çº. The 2Î¸ scan from 10° to 70°, at the step of 0.050° and time per step was 0.5s for all the samples. The non existence of any peaks would verify that the sample is in the amorphous state.
Fourier Transform Infrared (FTIR) Spectroscopy
The composition, kind of chemical bond and atomic arrangement that are present in sample can be determined using FTIR spectroscopy. Infrared spectroscopy in the system 2000R NIR FT-Raman is by using Michelson interferometer method (Perkin Elmer, 2000). The spectrometer source for these system is tungsten halogen with envelop quartz and the detector is by using InSb. The spectrum can be obtained from the interferogram with fourier transformation.
The samples were placed in the spectrometer and a scan as obtained for radiation at wave number (k = 2Ï€/Î») in the spectral range of 400 - 4000 cm-1 and were run at the resolution of 2 cm-1. The spectrum of the glass can be obtained with subtraction the infrared spectrum sample with substrate and the background spectrum (wave number = reciprocal of wavelength, usually expressed in cm-1).
Raman scattering experiments have been performed at right-angle geometry using a NIR FT-Raman Pelkin Elmer Spectrometer of an Nd:YAG laser with mW aoutput power. The NIR FT-Raman instrument used InGaAs detectors which is sensitive at the near infrared. The working range of the system at room temperature was 3600 -150 cm-1 Raman Shift.
A continuous wave (CW) laser was fired into the sample. The sample scatters the incident radiation elastically (Rayleigh scattering) and inelastically (Raman scattering) in all directions. Figure 3 shows a schematic optic diagram. In the arrangement scattered radiation is collected in a direction 180° to the incident laser beam. The scattered radiation was collected by the lens system, focused onto the J-stop, and so into the modulator of the FT-instrument.
Figure 6. A schematic optical diagram of NIR FT-Raman spectrometer
It is necessary to remove the intense Rayleigh scattering that occurs at the wavenumber of the exciting laser. This was done using a set of optical filters placed throughout the beampath before detector NIR FT-Raman spectrometer are dispersive systems that use gratings and slits and can avoid saturating the detector with Rayleigh scattered light by simply not scanning at the wavenumber of the laser.
Study of optical absorption and particularly the absorption edge is useful method to investigate optically induce transitions and to obtain information about the band structures and energy gap (Eg) of both crystalline and noncrystalline materials. The principle behind this technique is that a photon with energies greater than band gap energy will be absorbed. There are two kinds of optical transition at the fundamental absorption edge of crystalline and non-crystalline materials, namely direct and indirect transitions. Both involve interaction of an electronic wave with an electron in the valence band (VB), which is raised across the fundamental gap to the conduction band (CB). Indirect transition also involve simultaneous interactions with lattice vibrations; thus the wave vector of the electron can change in the optical transitions, with the momentum change being taken or given up by phonons. If the excitation formation or electron-hole interaction is neglected, the form of the Î± as a function of Ñ’Ï‰ depend on the type of energy bands containing the initial and final state. In many crystalline and noncrystalline semiconductors, the Î±Ï‰ depends exponentially on the Ñ’Ï‰. This exponential dependence, known as the urbach rule, can be written in the form:
Î±(Ï‰) = B exp (1)
where B is a constant and Î”Î• is the width of the band tails of the localized states known as Urbach energy. In general both direct and indirect transition can occur in crystalline material. The smallest gap leads to direct transition. The indirect transition is associated with a smaller Î±. Mott and Davis (1971)  suggested the following expression for direct transitions:
Î±(Ï‰)Ñ›Ï‰ = B (Ñ›Ï‰-Eopt)n (2)
where n = ½ or 3/2, depending on whether the transition is allowed or forbidden, B is a constant, and for indirect transitions, n = 2 for allowed transition and n = 3 for forbidden transition.
UV-Visible transmission the sample at room temperature was measured using a Shimadzu 3101 pc UV-VIS NIR spectrophotometer. This system using halogen lamp (340 < Î» < 2500 nm) for pumping source at scanning increment 0.2 nm. The absorbance signal was analyzed using double monochromatic diffraction grating system and photomultiplier R-928 detector with resolution about 0.1nm (Shimadzu,1997). For the measurement, the glass samples need to be polished and ground to a thickness range 2-5 mm.
Transmission Electron Microscopy (TEM)
The transmission electron microscopy (TEM) is used to identify imperfection in the atomic level structures of materials by analysis of microscopic surfaces. The principle of TEM can be seen in Figure 7. A very thin slice of the material to be tested is exposed to a beam of electrons. When the electrons interact with consistent material structure, a constant fraction of electrons is transmitted back from the sample to a detector. Once a structural imperfection is encountered, the fraction of transmitted electrons changes. Two common methods of TEM microstructural imaging reveal important information about the material being tested. Diffraction contrast is useful in identifying large structures and crystallographic features. Phase contrast is used for high magnification imaging of atomic columns.
A cross-sectional bright field image of the SiC thin film will be obtained using a JEM-2100 Electron microscope (JEOL). The JEM-2100 electron microscope is a having the maximum capabilities of ultra-high resolution, high image quality, easy operation and stability performance. Various optional attachments such as STEM image, an EDS, and an EELS. JEM-2100 used a single crystal LaB6 filament as the source of electron, which emitting electron when heated in the vacuum. This instrument can be operated at high voltage (up to 200kV) and gave a spatial resolution of 0.194 nm.
Figure 7. Principle of the Transmission Electron Microscopy
Design of HMCVD system
The schematic of HMCVD system is shown in Figure 8 and Appendix 1.
The output expected of this project is obtained the nc-3C-SiC: H film by using HMCVD system as result from our design and construct in our laboratory. The optimum of growth parameter such as gas flow rate, pressure, substrate temperature, W-mesh temperature, distance between substrate and W-mesh will used during nc-3C-SiC: H fabrication process. Furthermore, from the characterization process will be obtained the nc-3C-SiC: H film properties are applicable for high temperature, high power and high frequency devices.
Accordingly the research methodology as shown on flow chart, the working of the research will be continued on the assembly the HMCVD system for fabrication of nc-3C-SiC:H film, growth of self assembled nc-3C-SiC:H, characterize of the sample and analysis the data. The last work is doing writing for the paper and thesis completed.
This research project is consist of design and construct the HMCVD system for growth nc-3C-SiC:H film. The HMCVD system has been done designed. The construction of HMCVD system is in progress. HMCVD system will be used for fabrication the nc-3C-SiC:H for applied in high temperature, high power and high frequency devices.
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