Christopher L. Frewin

Electrical performance of Al2O3 gate dielectric films deposited by atomic layer deposition on 4H-SiC

Stoichiometric and pure Al2O3 gate dielectric films were grown on n-type 4H-SiC by a thermal atomic layer deposition process. The electrical properties of both amorphous and epitaxial Al2O3 films were studied by capacitance-voltage and current-voltage measurements of metal-oxide-semiconductor capacitors. A dielectric constant of 9 and a flatband voltage shift of +1.3V were determined. A leakage current density of 10−3A∕cm2 at 8MV∕cm was obtained for the amorphous Al2O3 films, lower than that of any high-κ gate oxide on 4H-SiC reported to date. A Fowler-Nordheim tunneling mechanism was used to determine an Al2O3∕4H-SiC barrier height of 1.58eV. Higher leakage current was obtained for the epitaxial γ-Al2O3 films, likely due to grain boundary conduction.

Atomic force microscopy analysis of central nervous system cell morphology on silicon carbide and diamond substrates.

Brain machine interface (BMI) devices offer a platform that can be used to assist people with extreme disabilities, such as amyotrophic lateral sclerosis (ALS) and Parkinsons disease. Silicon (Si) has been the material of choice used for the manufacture of BMI devices due to its mechanical strength, its electrical properties and multiple fabrication techniques; however, chronically implanted BMI devices have usually failed within months of implantation due to biocompatibility issues and the fact that Si does not withstand the harsh environment of the body. Single crystal cubic silicon carbide (3C‐SiC) and nanocrystalline diamond (NCD) are semiconductor materials that have previously shown good biocompatibility with skin and bone cells. Like Si, these materials have excellent physical characteristics, good electrical properties, but unlike Si, they are chemically inert. We have performed a study to evaluate the general biocompatibility levels of all of these materials through the use of in vitro techniques. H4 human neuroglioma and PC12 rat pheochromocytoma cell lines were used for the study, and polystyrene (PSt) and amorphous glass were used as controls or for morphological comparison. MTT [3‐(4,5‐Dimethylthiazol‐2‐Yl)‐2,5‐Diphenyltetrazolium Bromide] assays were performed to determine general cell viability with each substrate and atomic force microscopy (AFM) was used to quantify the general cell morphology on the substrate surface along with the substrate permissiveness to lamellipodia extension. 3C‐SiC was the only substrate tested to have good viability and superior lamellipodia permissiveness with both cell lines, while NCD showed a good level of viability with the neural H4 line but a poor viability with the PC12 line and lower permissiveness than 3C‐SiC. Explanations pertaining to the performance of each substrate with both cell lines are presented and discussed along with future work that must be performed to further evaluate specific cell reactions on these substrates. Copyright

A Comprehensive Study of Hydrogen Etching on the Major SiC Polytypes and Crystal Orientations

A comprehensive study on the hydrogen etching of numerous SiC polytype surfaces and orientations has been performed in a hot wall CVD reactor under both atmospheric and low pressure conditions. The polytypes studied were 4H and 6H-SiC as well as 3C-SiC grown on Si substrates. For the hexagonal polytypes the wafer surface orientation was both on- and off-axis, i.e. C and Si face. The investigation includes the influence of the prior surface polishing method on the required etching process parameters. 3C-SiC was also studied grown in both the (100) and (111) orientations. After etching, the samples were analyzed via atomic force microscopy (AFM) to determine the surface morphology and the height of the steps formed. For all cases the process conditions necessary to realize a well-ordered surface consisting of unit cell and sub-unit cell height steps were determined. The results of these experiments are summarized and samples of the corresponding AFM analysis presented.

Single-Crystal Silicon Carbide: A Biocompatible and Hemocompatible Semiconductor for Advanced Biomedical Applications

Crystalline silicon carbide (SiC) and silicon (Si) biocompatibility was evaluated in vitro by directly culturing three skin and connective tissue cell lines, two immortalized neural cell lines, and platelet-rich plasma (PRP) on these semiconducting substrates. The in vivo biocompatibility was then evaluated via implantation of 3C-SiC and Si shanks into a C57/BL6 wild type mouse. The in vivo results, while preliminary, were outstanding with Si being almost completely enveloped with activated microglia and astrocytes, indicating a severe immune system response, while the 3C-SiC film was virtually untouched. The in vitro experiments were performed specifically for the three adopted SiC polytypes, namely 3C-, 4H- and 6H-SiC, and the results were compared to those obtained for Si crystals. Cell proliferation and adhesion quality were studied using MTT [3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide] assays and fluorescent microscopy. The neural cells were studied via atomic force microscopy (AFM) which was used to quantify filopodia and lamellipodia extensions on the surface of the tested materials. Fluorescent microscopy was used to assess platelet adhesion to the semiconductor surfaces where significantly lower values of platelet adhesion to 3C-SiC was observed compared to Si. The reported results show good indicators that SiC is indeed a more biocompatible substrate than Si. While there were some differences among the degree of biocompatibility of the various SiC polytypes tested, SiC appears to be a highly biocompatible material in vitro that is also somewhat hemocompatible. This extremely intriguing result appears to put SiC into a unique class of materials that is both bio- and hemo-compatible and is, to the best of our knowledge, the only semiconductor with this property.

Surface studies of hydrogen etched 3C-SiC(001) on Si(001)

The morphology and structure of 3C-SiC(001) surfaces, grown on Si(001) and prepared via hydrogen etching, are studied using atomic force microscopy (AFM), low-energy electron diffraction (LEED), and Auger electron spectroscopy (AES). On the etched samples, flat surfaces with large terraces and atomic steps are revealed by AFM. In ultrahigh vacuum a sharp LEED pattern with an approximate (5×1) periodicity is observed. AES studies reveal a “bulklike” composition up to the near surface region and indicate that an overlayer consisting of a weakly bound silicon oxide monolayer is present.

Use of cortical neuronal networks for in vitro material biocompatibility testing

Neural interfaces aim to restore neurological function lost during disease or injury. Novel implantable neural interfaces increasingly capitalize on novel materials to achieve microscale coupling with the nervous system. Like any biomedical device, neural interfaces should consist of materials that exhibit biocompatibility in accordance with the international standard ISO10993-5, which describes in vitro testing involving fibroblasts where cytotoxicity serves as the main endpoint. In the present study, we examine the utility of living neuronal networks as functional assays for in vitro material biocompatibility, particularly for materials that comprise implantable neural interfaces. Embryonic mouse cortical tissue was cultured to form functional networks where spontaneous action potentials, or spikes, can be monitored non-invasively using a substrate-integrated microelectrode array. Taking advantage of such a platform, we exposed established positive and negative control materials to the neuronal networks in a consistent method with ISO 10993-5 guidance. Exposure to the negative controls, gold and polyethylene, did not significantly change the neuronal activity whereas the positive controls, copper and polyvinyl chloride (PVC), resulted in reduction of network spike rate. We also compared the functional assay with an established cytotoxicity measure using L929 fibroblast cells. Our findings indicate that neuronal networks exhibit enhanced sensitivity to positive control materials. In addition, we assessed functional neurotoxicity of tungsten, a common microelectrode material, and two conducting polymer formulations that have been used to modify microelectrode properties for in vivo recording and stimulation. These data suggest that cultured neuronal networks are a useful platform for evaluating the functional toxicity of materials intended for implantation in the nervous system.

Single-crystal cubic silicon carbide: An in vivo biocompatible semiconductor for brain machine interface devices

Single crystal silicon carbide (SiC) is a wide band-gap semiconductor which has shown both bio- and hemo-compatibility [1–5]. Although single crystalline SiC has appealing bio-sensing potential, the material has not been extensively characterized. Cubic silicon carbide (3C-SiC) has superior in vitro biocompatibility compared to its hexagonal counterparts [3, 5]. Brain machine interface (BMI) systems using implantable neuronal prosthetics offer the possibility of bi-directional signaling, which allow sensory feedback and closed loop control. Existing implantable neural interfaces have limited long-term reliability, and 3C-SiC may be a material that may improve that reliability. In the present study, we investigated in vivo 3C-SiC biocompatibility in the CNS of C56BL/6 mice. 3C-SiC was compared against the known immunoreactive response of silicon (Si) at 5, 10, and 35 days. The material was examined to detect CD45, a protein tyrosine phosphatase (PTP) expressed by activated microglia and macrophages. The 3C-SiC surface revealed limited immunoresponse and significantly reduced microglia compared to Si substrate.

3C-SiC Films on Si for MEMS Applications: Mechanical Properties

Single crystal 3C-SiC films were grown on (100) and (111) Si substrate orientations in order to study the resulting mechanical properties of this material. In addition, poly-crystalline 3C-SiC was also grown on (100)Si so that a comparison with monocrystaline 3C-SiC, also grown on (100)Si, could be made. The mechanical properties of single crystal and polycrystalline 3C-SiC films grown on Si substrates were measured by means of nanoindentation using a Berkovich diamond tip. These results indicate that polycrystalline SiC thin films are attractive for MEMS applications when compared with the single crystal 3C-SiC, which is promising since growing single crystal 3C-SiC films is more challenging. MEMS cantilevers and membranes fabricated from a 2 µm thick single crystal 3C-SiC grown on (100)Si under similar conditions resulted in a small degree of bow with only 9 µm of deflection for a cantilever of 700 µm length with an estimated tensile film stress of 300 MPa. Single crystal 3C-SiC films on (111)Si substrates have the highest elastic and plastic properties, although due to high residual stress they tend to crack and delaminate.

Organic functionalization of 3C-SiC surfaces.

We demonstrate the functionalization of n-type (100) and (111) 3C-SiC surfaces with organosilanes. Self-assembled monolayers (SAMs) of amino-propyldiethoxymethylsilane (APDEMS) and octadecyltrimethoxysilane (ODTMS) are formed via wet chemical processing techniques. Their structural, chemical, and electrical properties are investigated using static water contact angle measurements, atomic force microscopy, and X-ray photoelectron spectroscopy, revealing that the organic layers are smooth and densely packed. Furthermore, combined contact potential difference and surface photovoltage measurements demonstrate that the heterostructure functionality and surface potential can be tuned by utilizing different organosilane precursor molecules. Molecular dipoles are observed to significantly affect the work functions of the modified surfaces. Furthermore, the magnitude of the surface band bending is reduced following reaction of the hydroxylated surfaces with organosilanes, indicating that partial passivation of electrically active surface states is achieved. Micropatterning of organic layers is demonstrated by lithographically defined oxidation of organosilane-derived monolayers in an oxygen plasma, followed by visualization of resulting changes of the local wettability, as well as fluorescence microscopy following immobilization of fluorescently labeled BSA protein.

Electronic Passivation of 3C-SiC(001) Via Hydrogen Treatment

Electronic passivation of single-crystal, atomically flat (001) surfaces of cubic silicon carbide (3C-SiC) was attempted via hydrogen annealing and HF exposure and investigated by monitoring the surface potentials of the treated samples. It was found that HF treatment causes a negative charging of the surface and that only hydrogen annealing is effective in producing well-passivated 3C-SiC. The degree and stability of the surface electronic passivation was dependent on the final hydrogen cooling temperature of the annealing process. Surface charge densities of the hydrogen-treated surfaces were calculated from the measured surface potentials and were found to be in the 1010 cm -2 range.