3C-SiC Films Research Articles

TEM investigation of the interface formation during transfer of 3C-SiC(001) layer onto 6H-SiC(0001) wafer

At present, intensive research is underway in the field of vacuum-sublimation growth of 3C-SiC. Transfer of a thin (001)3C-SiC layer onto a 6H-SiC wafer is a promising way to fabricate a 3C-SiC/6H-SiC substrate for growing device-quality homoepitaxial films of low defect density. The article presents the results of the structural characterization of an interface formed during the transfer of a 3C-SiC layer onto a 6H-SiC(0001) wafer, performed with transmission electron microscopy (TEM). A 3C-SiC film with a thickness of about 10 μm, grown by chemical vapor deposition (CVD) on a Si(001) substrate, was utilized in the study. Silicon acted as a bonding material in the transfer process. The morphology and microstructure of the interface between a 6H-SiC substrate and a 3C-SiC (001)-oriented layer are under consideration. TEM investigation reveals an effect of “self”-orientation of the layer with respect to the wafer during the transfer process: an interaction between the molten silicon layer and silicon carbide throughout crystallization results in the generation of defined orientation relationships with respect to substrate axes. An analysis of selected area electron diffraction patterns taken from interfaces showed the relationships to be 3C-SiC{001}‖ 6H-SiC(0001) and 3C-SiC⟨11¯0⟩∼‖ 6H-SiC⟨112¯0⟩.

Impact of alternating precursor supply and gas flow on the LPCVD growth behavior of polycrystalline 3C-SiC thin films on Si

In this paper, we will provide information on the growth mechanism of 3C-SiC using alternating supply deposition (ASD). SiH4 and C3H8 were introduced successively in a low-pressure chemical vapor deposition (LPCVD) system at 1000 °C, forming a stoichiometric polycrystalline 3C-SiC thin film on Si substrates. We demonstrate the influence of different gas flow rates on thin film properties. In detail, altering the flow rates of the precursors and the carrier gas resulted in changes of the growth rate, the surface roughness, the crystal growth mechanisms as well as the crystal quality. Hydrogen inhibition and passivation are proposed to be the main effects influencing the growth behavior of ASD thin films. Applying ASD to grow 3C-SiC thin films with precursors from low to high flow rates resulted in a transition of different growth mechanisms influencing the surface roughness and grain size. Furthermore, we could prove that ASD is a cyclic step-by-step carbon-assisted redistribution of a prior deposited silicon film. This is shown by contact angle measurements of three differently terminated surfaces during the specific phases of one ASD cycle. High resolution transmission electron microscopy (HRTEM) analysis showed a continuous and homogenous thin film and confirmed the absence of silicon- or carbon-rich layers. ASD enables 3C-SiC thin films with customized properties for tailored micro electromechanical system (MEMS) applications.

Probe beam deflection technique with liquid immersion for fast mapping of thermal conductance

Frequency-domain probe beam deflection (FD-PBD) is an experimental technique for measuring thermal properties that combines heating by a modulated pump laser and measurement of the temperature field via thermoelastic displacement of the sample surface. In the conventional implementation of FD-PBD, the data are mostly sensitive to the in-plane thermal diffusivity. We describe an extension of FD-PBD that introduces sensitivity to through-plane thermal conductance by immersing the sample in a dielectric liquid and measuring the beam deflection created by the temperature field of the liquid. We demonstrate the accuracy of the method by measuring (1) the thermal conductivity of a 310 nm thick thermally grown oxide on Si, (2) the thermal boundary conductance of bonded interface between a 3C-SiC film and a single crystal diamond substrate, and (3) the thermal conductivities of several bulk materials. We map the thermal boundary conductance of a 3C-SiC/diamond interface with a precision of 1% using a lock-in time constant of 3 ms and dwell time of 15 ms. The spatial resolution and maximum probing depth are proportional to the radius of the focused laser beams and can be varied over the range of 1–20 μm and 4–80 μm, respectively, by varying the 1/e2 intensity radius of the focused laser beams from 2 to 40 μm. FD-PBD with liquid immersion thus enables fast mapping of spatial variations in thermal boundary conductance of deeply buried interfaces.

Advanced approach of bulk (111) 3C-SiC epitaxial growth

3C-SiC films grown on (111) Si substrates exhibit poor crystal quality and experience wafer cracks and bowing preventing access to bulk growth. This work reports innovative Chemical Vapor Deposition (CVD) growth methodology on 4 in. Si substrates which allowed the growth of 230 mm thick layer of (111) 3C-SiC through the melting of the Si substrate in the CVD chamber and the adoption of the resulting free standing 3C-SiC for the growth of bulk (111) 3C-SiC layer under high N fluxes. From the molten KOH etching and subsequent SEM investigation it has been ascertained that with a N2 flux of 1600 sccm there is a significant reduction in the concentration of stacking faults (SFs) from (7.16 ± 0.04) × 103 cm−1 to (0.4 ± 0.3) × 103 cm−1. This reduction is consistent with the cross section m-PL response displaying steep and uniform increase in the intensity of the band-edge signal a factor 10 higher on the surface with respect to the equal (100) 3C-SiC grown thickness. Furthermore, the emission attributed to point defects is considerably lower in (111) 3C-SiC. From Scanning Transmission Electron Microscopy (STEM) investigation it appears evident how the typical mechanism valid in (100) growths consisting in the mutual closure of SFs coming from opposing {111} planes that give rise to Lomer and l-shaped dislocations is replaced by a different panorama of evolution. Indeed, it is shown how the SFs shred but do not interrupt each other during growth. Furthermore, dropping in the number of atomic planes composing SFs layers appears to be a key phenomenon leading to both the shrinkage of the number of SF atomic layers as well as to the SF self-closure. High Angle Annular Dark Field-Scanning Transmission Electron Microscopy (HAADF-STEM) attested how the crystal tends to smooth out the lattice mismatch until the SF is suppressed. Because of the foregoing, the mechanisms of evolution of the defects in (111) 3C-SiC revealed in this study, demonstrates how the growth parameters must be matched with the kinetics of the defects in order to endorse (111) 3C-SiC adoption in high performing devices.

Optical spectroscopy study of damage in ion-irradiated 3C-SiC epilayers on a silicon substrate

Epitaxial cubic (100) 3C-SiC films on a (100) silicon wafer were irradiated at room temperature with 2.3-MeV Si+ or 3.0-MeV Kr+ ions up to a fluence of 1 × 1016 cm−2. The evolutions of the epilayer and the substrate were followed as a function of ion fluence by using micro-Raman spectroscopy, optical absorption, and diffuse reflectance spectroscopy in the UV-visible and near infrared range. Raman spectra evidence the amorphization of SiC films at an estimated dose of about 0.1 displacement per atom (dpa) for both ion irradiations. The narrow peaks of the Raman-allowed TO and LO modes of SiC and Si are recorded in the virgin sample, together with few peaks assigned to zone-edge modes of SiC arising from the intrinsic disorder in the strained films. Those crystal phonon peaks broaden or disappear with increasing fluence. The spectra finally exhibit broad extra peaks assigned to the formation of Si–Si and C–C wrong homonuclear bonds in the local order of the amorphous phase. The optical transmission and diffuse reflectance spectra feature interference fringe patterns in the SiC film that are smoothened out with irradiation due to the matching of refractive indices of the amorphous SiC film and Si substrate. The evolution of the refractive index of SiC and optical gap of Si are deduced from those spectra. The respective roles of ballistic effects and electronic excitations in the radiation damage of both SiC and Si are discussed for those two ions with about the same electronic stopping power and about one order-of-magnitude difference in nuclear stopping power. The damage is dominated by the nuclear collision processes and rather well correlated with the estimated irradiation dose in dpa. Optical spectra show that electronic excitations induce damage recovery of the amorphized substrate below the SiC/Si interface. Raman spectra and optical absorption/reflection spectra yield complementary pictures of the radiation damage.

Impact of Doping on Cross-Sectional Stress Assessment of 3C-SiC/Si Heteroepitaxy.

In this paper, we used micro-Raman spectroscopy in cross-section to investigate the effect of different doping on the distribution of stress in the silicon substrate and the grown 3C-SiC film. The 3C-SiC films with a thickness up to 10 μm were grown on Si (100) substrates in a horizontal hot-wall chemical vapor deposition (CVD) reactor. To quantify the influence of doping on the stress distribution, samples were non-intentionally doped (NID, dopant incorporation below 1016 cm-3), strongly n-type doped ([N] > 1019 cm-3), or strongly p-type doped ([Al] > 1019 cm-3). Sample NID was also grown on Si (111). In silicon (100), we observed that the stress at the interface is always compressive. In 3C-SiC, instead, we observed that the stress at the interface is always tensile and remains so in the first 4 µm. In the remaining 6 µm, the type of stress varies according to the doping. In particular, for 10 μm thick samples, the presence of an n-doped layer at the interface maximizes the stress in the silicon (~700 MPa) and in the 3C-SiC film (~250 MPa). In the presence of films grown on Si(111), 3C-SiC shows a compressive stress at the interface and then immediately becomes tensile following an oscillating trend with an average value of 412 MPa.

Investigation on Strain Sensitivity and Temperature Behaviour of Nitrogen Doped 3C-SiC Thin Films

Electrical resistance-strain behaviour of nitrogen doped 3C-SiC thin films was investigated to determine whether they could be used as strain gauges. Using a hot wall vertical low pressure chemical vapour deposition (LPCVD) reactor, these films were deposited on thermally oxidised Si (100) and alumina substrates at 2.5 mbar pressure and 1040°C temperature from methyltrichlorosilane (MTS) precursor. The nitrogen doping gas utilised was ammonia (NH3). Using four-point bending method, the gauge factor (GF) was determined for all thin films (0, 9, 17, and 30 atomic % nitrogen doped). Systematic annealing of films in a vacuum atmosphere was used to determine the TCR of nitrogen doped 3C-SiC (111). Film sheet resistance was evaluated using a four-probe approach, and it was observed to decrease as the temperature rises from 40 to 550°C. The resistivity, average TCR, and strain sensitivity of film doped with 17 atomic % nitrogen concentration were 0.14 cm, -103 ppm/°C, and -9.6, respectively, indicating that it can be employed as a strain gauge material in high temperature applications. However, film doped with 30 atomic % of nitrogen concentration showed an increase in the resistivity, TCR and strain sensitivity.

CVD Elaboration of 3C-SiC on AlN/Si Heterostructures: Structural Trends and Evolution during Growth

(111)-oriented cubic polytypes of silicon carbide (3C-SiC) films were grown by chemical vapor deposition on 2H-AlN(0001)/Si(111) and 2H-AlN(0001)/Si(110) templates. The structural and electrical properties of the films were investigated. For film thicknesses below 300 nm, the 3C-SiC material deposited on 2H-AlN/Si presented a better structural quality than the 3C-SiC films grown directly on Si(111) using the well-established two-step carbonization–epitaxy process. The good lattice match of 3C-SiC with AlN may open a reliable route towards high-quality thin heteroepitaxial 3C-SiC films on a silicon wafer. Nevertheless, the 3C-SiC was featured by the presence of twinned domains and small inclusions of 6H-SiC. The formation of a thin AlSiN film at the AlN/Si interface is also reported. This is the first time such AlSiN layers are described within an AlN/Si heterostructure. Furthermore, noticeable modifications were observed in the AlN film. First, the growth process of SiC on AlN induced a reduction of the dislocation density in the AlN, attesting to the structural healing of AlN with thermal treatment, as already observed for other AlN-based heterostructures with higher-temperature processes. The growth of SiC on AlN also induced a dramatic reduction in the insulating character of the AlN, which could be related to a noticeable cross-doping between the materials.

Elastoplastic deformation analysis of 3C-SiC film on 6H-SiC surface based on molecular dynamics nano-indentation simulation

Elastoplastic deformation analysis of 3C-SiC film on 6H-SiC surface based on molecular dynamics nano-indentation simulation

Tuning 3C-SiC(100)/Si(100) Heterostructure Interface Quality

We report a systematic spectroscopic and structural investigation of 3C-silicon carbide (3C-SiC) films grown on Si(100)-(2 × 1) by codeposition of C60 molecules and Si atoms in ultrahigh-vacuum conditions. This work focuses on reducing the macroscopic defects formed at the interface in Si-SiC heterojunctions. A wide range of parameters influence the growth process, including the substrate deposition temperature, the relative effusion fluxes of C60 and Si, and the clean Si(100) surface order. By adjusting the Si and C60 deposition rates, it is possible to reduce the Si atom diffusion from the substrate and control both the surface morphology and the specific formation of the C-rich c(2 × 2) or Si-rich 3 × 2 ordered surfaces. Our results show that the growth of 3C-SiC on flat and good quality Si substrates is a crucial and necessary starting point to obtaining good quality 3C-SiC/Si interfaces with a minimum number of defects.

Synthesis of ultrathin heteroepitaxial 3C-SiC films by pyrolysis of molecular layer deposition polyamide films on Si

Polyamide films were grown on Si(111) using a molecular layer deposition (MLD) process with 1,2-ethylenediamine and trimesoyl chloride precursors at 120 °C. Synthesized polyamide films on Si(111) were then pyrolyzed in vacuum (10−7 Torr) to yield crystalline SiC thin films. High-resolution transmission electron microscope images of heat-treated samples showed the heteroepitaxial nature of the synthesized 3C-SiC (β-SiC) with respect to the Si(111) substrate. Raman, x-ray photoelectron spectroscopy, and x-ray diffraction analysis confirmed the formation of single-crystal SiC films. Samples pyrolyzed at 1300 °C showed defects attributed to Si sublimation. Formation of highly conformal SiC film after pyrolysis was demonstrated using Bosch-processed Si trenches. The thicknesses of 3C-SiC films obtained after pyrolysis were linearly dependent on the number of MLD cycles used to deposit polyamide films.

Chemical Vapor Deposition of 3C-SiC on [100] Oriented Silicon at Low Temperature < 1200°C for Photonic Applications

3C-SiC films have been grown on [100] n-doped Si substrates in a horizontal cold wall CVD reactor. Without the use of plasma enhancement, the precursors silane and propane are used to deposit silicon carbide films at T < 1200°C. The structure of the grown films has been investigated via FESEM, XRD and Raman spectroscopy. It has been found that the growth rates are between 200 and 300 nm/h. Additionally, structural analysis give evidence of polycrystalline phases. Reasons for that could be insufficient cracking of the precursors and homogenous nucleation of Si species in the gas phase.

Precise Control of Al Incorporation during CVD Growth of SiC Epilayers by Using Hydrogen Chloride

Experimental results presented in this contribution demonstrate that adding HCl to the SiC CVD process is not only an efficient way to suppress the Aluminum memory effect but may also be considered as a powerful tool for fine tuning of intentional Al incorporation in 3C-SiC and 4H-SiC thin films. The approach is easy to implement and seems more reliable than changing TMA bubbling/dilution parameters during the growth. An ad-hoc phenomenological model is proposed to explain the correlation between the HCl supply and Al incorporation.

The Development of Monolithic Silicon Carbide Intracortical Neural Interfaces for Long-Term Human Implantation

Silicon Carbide (SiC) has been demonstrated as both a bio- and neuro-compatible wide-band-gap semiconductor with a high thermal conductivity and magnetic susceptibility and may be potentially compatible with human brain tissue. Two single-crystal, solid-state forms of SiC have been used to create monolithic intracortical neural implants (INI) without using physiologically exposed metals or polymers, thus eliminating many known reliability challenges in-vivo through a single, homogenous material. Amorphous SiC (a-SiC) was used to insulate 16-channel functional INI and the electrochemical and MRI compatibility (7T) performance were measured. 4H-SiC interfaces were fabricated using homoepitaxy,alternating epitaxial films of n-type and p-type forming an isolating PN junction which prevents substrate leakage current between the 16 adjacent electrodes and traces fabricated which were formed using deep-reactive ion etching (DRIE). 3C-SiC interfaces were fabricated in a similar fashion, but the epitaial conductive layers were grown on on both bulk crystalline (100) silicon and SOI wafers. In both cases a conformal coating of a-SiC was used as the top-side insulator and windows opened using RIE to allow electrochemical interaction. Electrochemical charaterization achieved through electrochemcial impedance spectroscopy (EIS) and cyclic voltammetry (CV) indicates performance on par, or exceeding, that of Pt reference electrodes with the same form fit. While magnetic resonance imaging (MRI) is an essential, non-contact method used to investigate issues with the nervous system, the high field MRI (e.g., 3 T and higher) necessary for proper diagnosis can be a safety issue for patients with INI due to inductive coupling between the powerful electromagnetic fields and the implanted device. This results in having to use lower electromagnetic field power (less than 1.5T), and therefore lower resolution, which hinders diagnostic prognosis for these patients. In this work the MRI compliance of epitaxial, monolithic SiC INI was studied. The specific absorption rate (SAR), induced heating, and image artifacts caused by the portion of the implant within a brain tissue phantom located in a 7 T small animal MRI machine were estimated and measured via finite element method (FEM) and Fourier-based simulations. Both the simulation and experimental results revealed that free-standing 3C-SiC films had no observable image artifacts compared to silicon and platinum reference materials inside the MRI at 7 T while FEM simulations predicted an ~30% SAR reduction for 3C-SiC compared to Pt. These initial simulations and experiments indicate a SiC monolithic INI may effectively reduce MRI induced heating and image artifacts in high field MRI.

Исследование сильно легированных эпитаксиальных пленок n-3C-SiC, выращенных методом сублимации на основе полуизолирующих подложек 6H-SiC

Heavily doped 3C-SiC films based on semi-insulating 6H-SiC substrates were obtained by sublimation epitaxy. The structural perfection of the obtained samples was monitored by X-ray diffractometry. The measurements of the photoluminescence and Hall effect spectra have confirmed the rather high perfection of the obtained epitaxial layers.

Study of heavily doped n-3C-SiC epitaxial films grown on 6H-SiC semi-insulating substraes by sublimation method

Heavily doped 3C-SiC films based on semi-insulating 6H-SiC substrates were obtained by sublimation epitaxy. The structural perfection of the obtained samples was monitored by X-ray diffractometry. The measurements of the photoluminescence and Hall effect spectra have confirmed the rather high perfection of the obtained epitaxial layers. Keywords: SiC, heteroepitaxy, cubic silicon carbide, X-ray diffractometry, Hall effect, photoluminescence.

Optical and surface properties of 3C–SiC thin epitaxial films grown at different temperatures on 4H–SiC substrates

A series of 3C–SiC films were grown on 4H–SiC substrates with different growth conditions using high-temperature chemical vapor deposition (HT-CVD). The influences of growth temperature (Tg) on the morphology, optical and material properties of films were assessed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and Raman scattering spectroscopy (RSS). Significant effects of Tg on the film crystalline quality were observed from analyzing XRD and RSS results. XPS characterized the surface states of Si, C, O elements, and variations with Tg. The 3C–SiC Raman TO mode was found to shift to lower frequency with the increase of Tg in 1530–1580 °C. Temperature dependent Raman studies indicated the anharmonic coupling and variation of phonon lifetimes. The optimized Tg is obtained. • XRD/XPS/Raman: 3C/4H-SiC films. • Quantified defects- depth variation. • Optimized growth temperature. • HT phonon coupling.

Piezoresistive Effect with a Gauge Factor of 18 000 in a Semiconductor Heterojunction Modulated by Bonded Light-Emitting Diodes.

Giant piezoresistive effect enables the development of ultrasensitive sensing devices to address the increasing demands from hi-tech applications such as space exploration and self-driving cars. The discovery of the giant piezoresistive effect by optoelectronic coupling leads to a new strategy for enhancing the sensitivity of mechanical sensors, particularly with light from light-emitting diodes (LEDs). This paper reports on the piezoresistive effect in a 3C-SiC/Si heterostructure with a bonded LED that can reach a gauge factor (GF) as high as 18 000. This value represents an approximately 1000 times improvement compared to the configuration without a bonded LED. This GF is one of the highest GFs reported to date for the piezoresistive effect in semiconductors. The generation of carrier concentration gradient in the top thin 3C-SiC film under illumination from the LED coupling with the tuning current contributes to the modulation of the piezoresistive effect in a 3C-SiC/Si heterojunction. In addition, the feasibility of using different types of LEDs as the tools for modulating the piezoresistive effect is investigated by evaluating lateral photovoltage and photocurrent under LED's illumination. The generated lateral photovoltage and photocurrent are as high as 14 mV and 47.2 μA, respectively. Recent technologies for direct bonding of micro-LEDs on a Si-based device and the discovery reported here may have a significant impact on mechanical sensors.

Growth of thick [1 1 1]-oriented 3C-SiC films on T-shaped Si micropillars

In this paper we report the morphology and the microstructural properties of thick [1 1 1]-oriented 3C-SiC films epitaxially grown on T-shaped Si micropillars. This compliant substrate was designed to release the stress developed in 3C-SiC grown on Si, due to the lattice mismatch and the different thermal expansion coefficients between 3C-SiC and Si. In this way it was possible to have 3C-SiC films as thick as 10 and 16 μm, with small bowing and no cracks. Our study relies on the use of an Electron Microscopy approach and elucidates the structure of the crystallographic defects across the 3C-SiC film, such as stacking faults (SFs), nano-twins and grain boundaries (GBs). After examination of the morphological and structural characteristics of the Si micropillar array, we analyzed the crystallographic properties of the thin 3C-SiC deposit on the Si micropillar sidewalls, since it may have an impact on the upper film. To assess the crystal quality of the 3C-SiC film, we quantified the SF density at the 3C-SiC surface, even estimating semi-quantitatively the depletion of SFs at much larger thickness. Hence, we analyzed the regions where 3C-SiC microcrystals grown on neighboring Si micropillars coalesce and form a continuous layer. We found that the coalescence between adjacent 3C-SiC microcrystals produces twinned regions, which terminate with the formation of GBs. We noticed that SFs may annihilate at the GBs, leading to the SF reduction across the 3C-SiC film. Finally, we observed the closure of the GBs inside the 3C-SiC film, thus improving the crystal quality of its surface. This work endorses the use of Si micropillars as compliant substrate to grow thick [1 1 1]-oriented 3C-SiC films with good crystal quality and is preliminary to the exploitation of 3C-SiC for high performing microelectronic devices.

Epitaxial growth of 3C-SiC film by microwave plasma chemical vapor deposition in H2-CH4-SiH4 mixtures: Optical emission spectroscopy study

Microwave (MW) plasma in silane-hydrogen and silane-hydrogen-methane mixtures is used effectively for chemical vapor deposition of Si, SiC, diamond, and SiC-diamond composite films; however, the properties of such plasma at pressures of the order of 100 Torr remain largely unexplored. Here we characterize the MW plasma (2.45 GHz) in SiH4 + H2 and SiH4 + СH4 + H2 mixtures (72 Torr) with silane content ranging from 0% to 5% in the process gas using high-resolution optical emission (OE) spectroscopy. Besides the OE lines of C2 dimer, Balmer series of excited atomic hydrogen (Hα, Hβ, Hγ, Hδ, and Hε), and CH radical, we observed atomic Si lines at 263, 288, and 391 nm and a relatively weak SiH emission. Gas temperature Tg of ≈3160 K is assessed from the rotational structure of the C2 dimer (Δν = 0, λ = 516.5 nm) emission band, and the absorbed microwave power density (MWPD) in the plasma fluctuates in the narrow range between 36 and 43 W/cm3 with a slight tendency to decrease with silane addition. The MWPD, intensity ratio Hα/Hβ of hydrogen Balmer series lines (related to excitation temperature Texc), and Si lines’ intensities in OE spectra as functions of SiH4 concentration in H2 and H2 + CH4 mixtures all show an extremum or a kink in slope near a special point at ≈0.5% SiH4. Finally, we produced a silicon carbide film of cubic polytype 3C-SiC on a (111) oriented Si substrate, which was characterized with Raman spectroscopy and x-ray diffraction, and its monocrystalline structure was confirmed.