Varshni Singh

Intensified plasma-assisted nitriding of AISI 316L stainless steel

Abstract In the present study, processing of AISI 316L stainless steel (316ss) has been conducted by intensified plasma-assisted processing (IPAP). The processing parameters (bias voltage, current density, chamber pressure and substrate temperature) of IPAP have been varied in an effort to determine which conditions lead to the formation of a single-phase structure, ‘m’ phase, and evaluate the properties of this phase. The structural characteristics of the nitrided layers produced by IPAP have been investigated by X-ray diffraction analysis. Nanoindentation experiments have been performed over cross-section to determine hardness and elastic modulus profiles. Dry sliding wear and potentiodynamic aqueous corrosion experiments have been conducted to characterize 316ss nitrided by IPAP. IPAP has been successful in producing single-phase m with high hardness and in shorter processing time compared to diode plasma nitriding. The IPAP produced single-phase nitrided layer was found to possess higher hardness (fourfold increase over the unprocessed alloy), excellent wear and corrosion resistance.

Millifluidics for Time-resolved Mapping of the Growth of Gold Nanostructures

Innovative in situ characterization tools are essential for understanding the reaction mechanisms leading to the growth of nanoscale materials. Though techniques, such as in situ transmission X-ray microscopy, fast single-particle spectroscopy, small-angle X-ray scattering, etc., are currently being developed, these tools are complex, not easily accessible, and do not necessarily provide the temporal resolution required to follow the formation of nanomaterials in real time. Here, we demonstrate for the first time the utility of a simple millifluidic chip for an in situ real time analysis of morphology and dimension-controlled growth of gold nano- and microstructures with a time resolution of 5 ms. The structures formed were characterized using synchrotron radiation-based in situ X-ray absorption spectroscopy, 3-D X-ray tomography, and high-resolution electron microscopy. These gold nanostructures were found to be catalytically active for conversion of 4-nitrophenol into 4-aminophenol, providing an example of the potential opportunities for time-resolved analysis of catalytic reactions. While the investigations reported here are focused on gold nanostructures, the technique can be applied to analyze the time-resolved growth of other types of nanostructured metals and metal oxides. With the ability to probe at least a 10-fold higher concentrations, in comparison with traditional microfluidics, the tool has potential to revolutionize a broad range of fields from catalysis, molecular analysis, biodefense, and molecular biology.

SU-8-based deep x-ray lithography/LIGA

Poly-methylmethacrylate (PMMA), a positive resist, is the most commonly used resist for deep X-ray lithography (DXRL)/LIGA technology. Although PMMA offers superior quality with respect to accuracy and sidewall roughness but it is also extremely insensitive. In this paper, we present our research results on SU-8 as negative resist for deep X-ray lithography. The results show that SU-8 is over two order of magnitude more sensitive to X-ray radiation than PMMA and the accuracy of the SU-8 microstructures fabricated by deep X-ray lithography is superior to UV-lithography and comparable to PMMA structures. The good pattern quality together with the high sensitivity offers rapid prototyping and direct LIGA capability. Moreover, the combinational use of UV and X-ray lithography as well as the use of positive and negative resists made it possible to fabricate complex multi-level 3D microstructures. The new process can be used to fabricate complex multi-level 3D structures for MEMS, MOEMS, Bio-MEMS or other micro-devices.

Magnetism of Cr-doped diamond-like carbon

Chromium-doped hydrogenated diamond-like carbon (Cr-DLC) and chromium carbide hydrogenated DLC alloys were synthesized by plasma-assisted vapor deposition and investigated by x-ray absorption near edge structure spectroscopy, extended x-ray absorption fine structure, and superconducting quantum interference device (SQUID) magnetometry. Structural and magnetic properties of the doped and alloy materials were investigated as a function of the Cr concentration (0.1–20 at. %). Toward the upper end of the concentration range, Cr precipitates in the form of chromium carbide (Cr3C2) nanoclusters. For low Cr concentrations, the systems are ferromagnetic at very low temperatures, whereas the chromium carbide clusters appear to be antiferromagnetic with uncompensated spins at the surface. Cr-DLC films and alloys with various Cr concentrations are used to make heterojunctions on silicon, and the produced diodes are investigated by I-V measurements. The heterojunctions exhibit negative magnetoresistance that saturate...

LiGA Research and Service at CAMD

Since 1995 CAMD has been offering exposure services, so called print shop for a variety of users interested in making precision High-Aspect-Ratio Microstructures (HARMST) for various application. Services have been expanded beyond only the print shop service in recent years and now include x-ray mask fabrication, substrate preparation for PMMA and SU- 8 resists, electroplating, finishing and molding. Metallic and polymeric parts are now routinely fabricated for precision engineering, micro-fluidic and micro-optic applications. This paper presents a brief overview of the actual status of LiGA services provided at CAMD including ongoing research efforts and examples of LiGA components for different applications.

Human Microvascular Endothelial Cell Seeding on Cr-DLC Thin Films for Heart Valve Applications

In this investigation, Cr-modified diamond-like carbon (Cr-DLC) films were studied for potential applications in mechanical heart valves. Three Cr-DLC samples were prepared using a magnetron sputtering technique employing an intensified plasma-assisted processing (IPAP) system. The three samples consisted of the following Cr contents: 1, 5, and 10 at.%. The biological response of human microvascular endothelial cells (HMV-EC), seeded on Cr-DLC films, was evaluated in terms of initial cell attachment and growth. The Cr-DLC films were characterized using Raman spectroscopy, x-ray diffraction, scanning electron microscopy, secondary ion mass spectroscopy, and by the contact angle technique. Endothelial cell adhesion and growth were found to be affected by changing the Cr content of Cr-DLC films.

Characterization of activated cyclic olefin copolymer: effects of ethylene/norbornene content on the physiochemical properties

The ethylene/norbornene content within cyclic olefin copolymer (COC) is well known to affect the chemical and physical properties of the copolymer, such as the glass transition temperature (Tg) and transparency. However, no work has been reported evaluating the effects of the ethylene/norbornene content on the surface properties of COC following UV/O3 or O2 plasma activation. Activation with either O2 plasma or UV/O3 is often used to assist in thermal assembly of fluidic devices, increasing the wettability of the surfaces, or generating functional scaffolds for the attachment of biological elements. Thus, we investigated differences in the physiochemical surface properties of various ethylene/norbornene compositions of COC following activation using analytical techniques such as water contact angle (WCA), ATR-FTIR, XPS, TOF-SIMS, UV-VIS, AFM and a colorimetric assay utilizing Toluidine Blue O (TBO). Results showed that increased norbornene content led to the generation of more oxygen containing functionalities such as alcohols, ketones, aldehydes and carboxyl groups when activated with either UV/O3 or O2 plasma. Specifically, COC with ∼60% norbornene content showed a significantly higher -COOH functional group density when compared to COC with a 50% norbornene content and COC with a 35% norbornene content following UV/O3 or O2 plasma activation. Furthermore, COC with large norbornene contents showed a smaller average RMS roughness (0.65 nm) when compared to COC containing low norbornene contents (0.95 nm) following activation making this substrate especially suited for nanofluidic applications, which require smooth surfaces to minimize effects arising from dielectrophoretic trapping or non-specific adsorption. Although all COC substrates showed >90% transparency at wavelengths >475 nm, COC possessing high norbornene contents showed significantly less transparency at wavelengths below 475 nm following activation, making optical detection in this region difficult. Our data showed distinct physiochemical differences in activated COC that was dependent upon the ethylene/norbornene content of the thermoplastic and thus, careful selection of the particular COC grade must be considered for micro- and nanofluidics.

Control of Internal Stress for High Quality Nickel Large Area Mold Inserts

Metallic large area mold inserts (LAMIs) are essential for the replication of polymer microfluidic devices. Successful molding of micro- or nanoscale features over large areas is dependent on improving the dimensional control of the mold inserts, particularly those fabricated by electrodeposition using the LIGA or UV-LIGA processes. A systematic approach to controlling the internal stress of the nickel deposits, which was essential for predicting the final flatness of the LAMIs prior to electroplating, was carried out. The internal stress of the nickel deposits from a nickel sulfamate solution was estimated using a bent strip stress measurement method after maintaining electroplating chemicals and conditions and reducing contamination. Over-electroplating of the nickel LAMIs was performed on SU-8 electroplating molds on 150 mm diameter Si wafers. Detailed characterization of the nickel LAMIs to determine the relationship between the overall flatness of the LAMIs and the internal stress identified a suitable process window in terms of the current densities (10–20 mA/cm2 ) and the internal stress (−8.3 ∼ −3.0 MPa) for the high quality nickel LAMIs with an overall flatness of 100 μm.© 2009 ASME

Microstructure and Tribological Behavior of Cr-DLC Nanocomposite Films

Cr-diamondlike carbon (Cr-DLC) nanocomposite films with the Cr content varying up to 27 at. % were synthesized by reactive magnetron sputtering. Their microstructure and tribological properties were studied using transmission electron microscopy (TEM) and pin-on-disc experiments, respectively. Electron diffraction and high- resolution TEM studies show that the films, with ∼ 9 at. % Cr, deposited using low (−200 V) and high (−1000 V) specimen bias during processing are composed of nanocrystalline metallic Cr and face-centered cubic chromium carbide, respectively surrounded by an amorphous matrix. The Cr-DLC film deposited at high bias exhibited enhanced adhesion to Si substrate and wear resistance compared to those deposited at low bias with the same Cr content. Wear rate of the films deposited at high bias is relatively independent of Cr content up to about 10 at. % (of the order of 10 −7 mm 3 /N-m) and then increases with increasing Cr content. The coefficient of friction for the films with a Cr content less than 19 at. % is low and remains between 0.1-0.16.

Electrokinetic Transport Properties of Deoxynucleotide Monophosphates (dNMPs) through Thermoplastic Nanochannels

The electrokinetic behavior of molecules in nanochannels (<100 nm in length) have generated interest due to the unique transport properties observed that are not seen in microscale channels. These nanoscale dependent transport properties include transverse electromigration arising from partial electrical double layer overlap, enhanced solute/wall interactions due to the small channel diameter, and field-dependent intermittent motion produced by surface roughness. In this study, the electrokinetic transport properties of deoxynucleotide monophosphates (dNMPs) were investigated, including the effects of electric field strength, surface effects, and composition of the carrier electrolyte (ionic concentration and pH). The dNMPs were labeled with a fluorescent reporter (ATTO 532) to allow tracking of the electrokinetic transport of the dNMPs through a thermoplastic nanochannel fabricated via nanoimprinting (110 nm × 110 nm, width × depth, and 100 μm in length). We discovered that the transport properties in plastic nanochannels of the dye-labeled dNMPs produced differences in their apparent mobilities that were not seen using microscale columns. We built histograms for each dNMP from their apparent mobilities under different operating conditions and fit the histograms to Gaussian functions from which the separation resolution could be deduced as a metric to gage the ability to identify the molecule based on their apparent mobility. We found that the resolution ranged from 0.73 to 2.13 at pH = 8.3. Changing the carrier electrolyte pH > 10 significantly improved separation resolution (0.80-4.84) and reduced the standard deviation in the Gaussian fit to the apparent mobilities. At low buffer concentrations, decreases in separation resolution and increased standard deviations in Gaussian fits to the apparent mobilities of dNMPs were observed due to the increased thickness of the electric double layer leading to a partial parabolic flow profile. The results secured for the dNMPs in thermoplastic nanochannels revealed a high identification efficiency (>99%) in most cases for the dNMPs due to differences in their apparent mobilities when using nanochannels, which could not be achieved using microscale columns.