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The Application of Temper-Etch Inspection to Micromilled AISI 4340 Steel SpecimenJanuary 2010 (has links)
abstract: Micromachining has seen application growth in a variety of industries requiring a miniaturization of the machining process. Machining at the micro level generates different cutter/workpiece interactions, generating more localized temperature spikes in the part/sample, as suggested by multiple studies. Temper-etch inspection is a non-destructive test used to identify `grind burns' or localized over-heating in steel components. This research investigated the application of temper-etch inspection to micromachined steel. The tests were performed on AISI 4340 steel samples. Finding, indications of localized over-heating was the primary focus of the experiment. In addition, change in condition between the original and post-machining hardness in the machined slot bottom was investigated. The results revealed that, under the conditions of the experiment, no indications of localized over-heating were present. However, there was a change in hardness at the bottom of the machined slot compared to the rest of the sample. Further research is needed to test the applicability of temper-etch inspection to micromilled steel and to identify the source of the change in hardness. / Dissertation/Thesis / M.S.Tech Technology 2010
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Swift heavy ion irradiation of polyester and polyolefin polymeric film for gas separation applicationAdeniyi, Olushola Rotimi January 2015 (has links)
Philosophiae Doctor - PhD / The combination of ion track technology and chemical etching as a tool to enhance
polymer gas properties such as permeability and selectivity is regarded as an avenue to establish technology commercialization and enhance applicability. Traditionally, permeability and selectivity of polymers have been major challenges especially for gas applications. However, it is important to understand the intrinsic polymer properties in order to be able to predict or identify their possible ion-polymer interactions thus facilitate the reorientation of existing polymer structural configurations. This in turn can enhance the gas permeability and selectivity properties of the polymers. Therefore, the choice of polymer is an important prerequisite. Polyethylene terephthalate (PET) belongs to the polyester group of polymers and has been extensively studied within the context of post-synthesis modification techniques using swift heavy ion irradiation and chemical treatment which is generally referred to as ‘track-etching’. The use of track-etched polymers in the form of symmetrical membranes structures to investigate gas permeability and selectivity properties has proved successful. However, the previous studies on track-etched polymers films have been mainly focused on the preparation of symmetrical membrane structure, especially in the case of polyesters such as PET polymer films. Also, polyolefins such as polymethyl pentene (PMP) have not been investigated using swift heavy ions and chemical etching procedures. In addition, the use of ‘shielded’ material on PET and PMP polymer films prior to swift heavy ion irradiation and chemical etching to prepare asymmetrical membrane structure have not been investigated. The gas permeability and selectivity of the asymmetrical membrane prepared from swift heavy ion irradiated etched 'shielded' PET and PMP polymer films have not been determined. These highlighted limitations will be addressed in this study. The overall objective of this study was to prepare asymmetric polymeric membranes with porous surface on dense layer from two classes of polymers; (PET and PMP) in order to improve their gas permeability and selectivity properties. The research approach in this study was to use a simple and novel method to prepare an
asymmetric PET and PMP polymer membrane with porous surface and dense layer
by mechanical attachment of ‘shielded’ material on the polymer film before swift
heavy ion irradiation. This irradiation approach allowed for the control of swift
heavy ion penetration depth into the PET and PMP polymer film during irradiation.
The procedure used in this study is briefly described. Commercial PET and PMP
polymer films were mechanically ‘shielded’ with aluminium and PET foils
respectively. The ‘shielded’ PET polymer films were then irradiated with swift
heavy ions of Xe source while ‘shielded’ PMP polymer films were irradiated with
swift heavy ions Kr. The ion energy and fluence of Xe ions was 1.3 MeV and 106
respectively while the Kr ion energy was 3.57 MeV and ion fluence of 109. After
swift heavy ion irradiation of ‘shielded’ PET and PMP polymer films, the attached
‘shielded’ materials were removed from PET and PMP polymer film and the
irradiated PET and PMP polymer films were chemically etched in sodium hydroxide (NaOH) and acidified chromium trioxide (H2SO4 + CrO3) respectively. The chemical etching conditions of swift heavy ion irradiated ‘shielded’ PET was
performed with 1 M NaOH at 80 ˚C under various etching times of 3, 6, 9 and 12
minutes. As for the swift heavy ion irradiated ‘shielded’ PMP polymer film, the
chemical etching was performed with 7 M H2SO4 + 3 M CrO3 solution, etching
temperature was varied between 40 ˚C and 80 ˚C while the etching time was
between 40 minutes to 150 minutes. The SEM (surface and cross-section micrograph) morphology results of the swift heavy ion irradiated ‘shielded’ etched PET and PMP films showed that asymmetric membranes with a single-sided porous surface and dense layer was prepared and remained unchanged even after 12 minutes of etching with 1 M NaOH solution as in the case of PET and 2 hours 30 minutes of etching with 7 M H2SO4 + 3 M CrO3 as observed for PMP polymer film. Also, the swift heavy ion irradiated ‘shielded’ etched PET polymer film showed the presence of pores on the polymer film surface within 3 minutes of etching. After 12 minutes chemical etching with 1 M NaOH solution, the dense layer of swift heavy ion irradiated ‘shielded’ etched PET polymer film experienced significant reduction in thickness of about 40 % of the original thickness of as-received PET polymer film. The surface morphology of swift heavy ion irradiated ‘shielded’ etched PET polymer film by SEM analysis revealed finely distributed pores with spherical shapes for the swift heavy ion irradiated ‘shielded’ etched PET polymer film within 6 minutes of etching with 1 M NaOH solution. Also, after 9 minutes and 12 minutes of etching with 1 M NaOH solution of the swift heavy ion irradiated ‘shielded’ etched PET polymer film, the pore walls experienced complete collapse with intense surface roughness. Interestingly, the 12 minutes etched swift heavy ion ‘shielded’ irradiated PET did not lose its asymmetrical membrane structure despite the collapse of the pore walls. In the case of swift heavy ion irradiated ‘shielded’ etched PMP polymer film, SEM morphology analysis showed that the pores retained their shape with the presence of defined pores without intense surface roughness even after extended etching with 7 M H2SO4 + 3 M CrO3 for 2 hours 30 minutes. Also, the pores of swift heavy ion irradiated ‘shielded’ etched PMP polymer films were observed to be mono dispersed and not agglomerated or overlapped. The SEM cross-section morphology of the swift heavy ion irradiated ‘shielded’ etched PMP polymer film showed radially oriented pores with increased pore diameters in the PMP polymer film which indicated that etching was radial instead of lateral, and no through pores were observed showing that the dense asymmetrical structure was retained. The SEM results revealed that the pore morphology i.e. size and shape could be accurately controlled during chemical etching of swift heavy ion ‘shielded’ irradiated PET and PMP polymer films. The XRD results of swift heavy ion irradiated ‘shielded’ etched PET revealed a single diffraction peak for various times of chemical etching in 1 M NaOH solution at 3, 6, 9 and 12 minutes. The diffraction peak of swift heavy ion irradiated ‘shielded’ etched PET was observed to reduce in intensity and marginally shifted to lower angles from 25.95˚ 2 theta to 25.89˚ 2 theta and also became broad in shape. It was considered that the continuous broadening of diffraction peaks due to an increase in etching times could be attributed to disorderliness of the ordered region within the polymer matrix and thus decreases in crystallinity of the swift heavy ion irradiated ‘shielded’ etched PET polymer film. The XRD analysis of swift heavy ion irradiated ‘shielded’ etched PMP polymer films indicated the presence of the diffraction peak at 9.75˚ 2 theta with decrease in intensity while the diffraction peaks located at 13.34˚, 16.42˚, 18.54˚ and 21.46˚ 2 theta disappeared after chemical etching in acidified chromium trioxide (H2SO4 + CrO3) after 2 hours 30 minutes. The TGA thermal profile analysis of swift heavy ion irradiated ‘shielded’ etched PET did not show the evolution of volatile species or moisture at lower temperatures even after 12 minutes of etching in 1 M NaOH solution in comparison with commercial PET polymer film. Also, it was observed that the swift heavy ion irradiated layered’ etched PET polymer film started to undergo degradation at a higher temperature than untreated PET which resulted in an approximate increase of 50 ˚C in comparison with the commercial PET polymer film. The TGA results of swift heavy ion irradiated ‘shielded’ etched PMP polymer film revealed an improvement of about 50 ˚C in thermal stability before thermal degradation even after etching in acidified chromium trioxide for 2 hours 30 minutes at 80 ˚C. Spectroscopy (IR) analysis of the swift heavy ion irradiated ‘shielded’ etched PET and PMP polymer films showed the presence of characteristic functional groups associated with either PET or PMP structures. The variations of irradiation and chemical etching conditions revealed that the swift heavy ion ‘shielded’ irradiated etched PET polymer film experienced continuous degradation of available functional groups as a function of etching time and also with complete disappearance of some functional groups such as 1105 cm-1 and 1129 cm-1 compared with the as-received PET polymer film which are both associated with the para-substituted position of benzene rings. In the case of swift heavy ion irradiated ‘shielded’ etched PMP polymer film, spectroscopic (IR) analysis showed significant variations in the susceptibility of associated functional groups within the PMP polymer film with selective attack and emergence of some specific functional groups such as at 1478 cm-1, 1810 cm-1 and 2115 cm-1 which were assigned to methylene, CH3 (asymmetry deformation), CH3 and CH2 respectively Also, the IR results for swift heavy ion irradiated ‘shielded’ etched PMP polymer showed that unsaturated olefinic groups were the dominant functional groups that were being attacked by during etching with acidified chromium trioxide (H2SO4+CrO3) which is an aggressive chemical etchant. The gas permeability analysis of swift heavy ion irradiated ‘shielded’ etched PET and PMP polymer films showed that the gas permeability was improved in comparison with the as-received PET and as-received PMP polymer films. The gas
permeability of swift heavy ion irradiated ‘shielded’ etched PET increased as a
function of etching time and was found to be highest after 12 minutes of chemical
etching in 1 M NaOH at 80 ˚C. In the case of swift heavy ion irradiated ‘shielded’
etched PMP, the gas permeability was observed to show the highest gas
permeability after 2 hours 30 minutes of etching in H2SO4 + CrO3 solution. The gas
permeability analysis for swift heavy ion irradiated ‘shielded’ PET and PMP
polymer films was tested for He, CO2 and CH4 and the permeability results showed
that helium was most permeable compared with CO2 and CH4 gases. In comparison, the selectivity analysis was performed for He/CO2 and CH4/He and the results showed that the selectivity decreased with increasing in etching time as expected. This study identified some important findings. Firstly, it was observed that the use of ‘shielded’ material on PET and PMP polymer films prior to swift heavy ion irradiation proved successful in the creation of asymmetrical polymer membrane structure. Also, it was also observed that the chemical etching of the ‘shielded’ swift heavy ion irradiated PET and PMP polymer films resulted in the presence of pores on the swift heavy ion irradiated side while the unirradiated sides of the PET and PMP polymer films were unaffected during chemical etching hence the pore depth could be controlled. In addition, the etching experiment showed that the pores geometry can be controlled as well as the gas permeability and selectivity properties of swift heavy ion ‘shielded’ irradiated etched PET and PMP polymer films. The process of polymer bulk and surface properties modification using ion-track technology i.e. swift heavy ion irradiation and subsequent chemical treatment of the irradiated polymer serves to reveal characteristic pore profiles unique to the prevailing ion-polymer interaction and ultimately results in alteration of the polymer characteristics.
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The amounts of fluorides (alkali-soluble as well as insoluble) gained on and in enamel of third molars from a high fluoride areaVan Zyl, Jacobus Francois January 1992 (has links)
Magister Chirurgiae Dentium (MChD) / A total of 25 third molar teeth (erupted [9], as well as unerupted [16]), from subjects who had lived continuously since birth in an area where the water fluoride concentration was more than 1,8 ppm, were studied. (The range was 1,8 ppm - 2,64 ppm of F-). The subjects had no systemic fluoride supplementation. Tooth brushing with a fluoride containing dentifrice and, perhaps, occasional fluoride mouth rinsing was the only additional exposure to fluoride. The acid-etch biopsy technique was used to determine the fluoride and calcium concentrations at various depths on the enamel surface. The fluoride concentration of the buffered etch solution was determined with an adapted fluoride ion-selective electrode technique, and the amount of calcium by flame atomic absorption spectrophotometry. Six consecutive etchings were done on the mesio-buccal and mesio-lingual cusps of each tooth; the teeth were then washed in an alkali and the same procedure repeated on the disto-buccal and disto-lingual cusps. The depth of etch of each biopsy was calculated assuming that human enamel contains 37% Ca and has a density of 2,95g/ml. It was previously reported, (Grobler & Joubert, 1988), that the enamel fluoride levels of the mesio-buccal and mesio-Iingual sides did not differ from that of the disto-buccal and disto-Iingual sides. The average etch depth and fluoride concentration value as calculated from the values for the two cusps per tooth were used for statistical analysis. The mean etch depths (pm) and mean enamel fluoride concentrations of alkali-washed and unwashed enamel of both erupted and unerupted teeth were tabled, together with the standard deviations and range for each etch. Contrary to the results obtained from a low F- area, no significant difference (p>O.05) could be found in the etch depth between erupted and unerupted enamel in this study. Graphs were plotted by a line fitted to the mean enamel fluoride concentration and mean etch depths values of unwashed erupted, unwashed unerupted, alkali-washed erupted and alkali-washed unerupted third molar teeth. These graphs were compared to the graphs obtained in a comparable study done by Grobler and Kotze (1990), on erupted and unerupted third molar teeth from a low fluoride area (F- < 0,10 ppm). Results indicate that the enamel fluoride concentration in the bulk of the enamel of teeth from a high fluoride area (> 1,8 ppm), is higher than that of teeth from a low fluoride area « 0,10 ppm ). In contrast to the teeth from a low fluoride area, where there was a significant increase (p<0.05) in the fluoride concentration of the outer layer (± 4 J,lm) of erupted enamel when compared to that of the unerupted enamel, no notable increase in the F- content of the enamel was observed in the present study of teeth from a high fluoride area (p>0,05). There was, in addition, no significant (p>0.05) difference between the enamel fluoride content of alkali-washed and unwashed, erupted and unerupted teeth, which showed that very little CaF 2-like material was gained by the enamel after eruption. In both studies the subjects had brushed with a fluoride dentifrice for a period of 1 - 16 years. It was expected that this topical exposure would increase the surface enamel concentration in the high fluoride area similar to the increase found in the low fluoride area. However, this was not the case, and as all the teeth from the high fluoride area exhibited some degree of fluorosis, it was concluded that posteruptive fluoride uptake by fluorotic human enamel without severe enamel loss is limited. This is in agreement with work done by Richards, Fejerskov, Baelum and Likimani (1989).
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In vitro comparison of shear bond strength and remaining adhesive using a new commercial self-etching primer, 35% and 20% prosphoric acid multi-step systemMazzarella, Jennifer 01 December 2011 (has links)
December 2011.
A thesis submitted to the College of Dental Medicine of Nova Southeastern University of the degree of Master of Science in Dentistry.
Introduction: The purpose of this study is to compare the shear bond strengths (SBSs) of two new commercial adhesive systems to a conventional multistep bonding system incorporating a 35% phosphoric acid gel. In addition, the amount of adhesive remaining on each tooth following debonding will be analyzed and compared using the adhesive remnant index (ARI). Methods: 88 human premolar teeth chosen from the Nova Southeastern tooth databank were randomly divided into four groups. Group I (control group): Transbond XT primer and adhesive (35% phosphoric acid), Group II: iBond Total Etch system with iBond 35 gel (35% phosphoric acid), Group III: iBond Total Etch system with iBond 20 gel (20% phosphoric acid). Group IV: iBond Self Etch. A scanning electron microscope (SEM) was utilized to qualitatively examine the enamel surface of one randomly selected tooth per group immediately after etching, leaving 21 teeth per group available for the debonding procedure (n=21). Following bonding of the stainless steel brackets (3M Unitek, Monrovia, CA), the teeth were stored in water at 37°C ± 2°C for forty-eight hours. A universal testing machine (Instron, Canton, MA) was then used to determine the shear bond strength of each bracket. Additionally, the amount of adhesive remaining on each tooth following debonding was recorded using 10x light microscopy. Results: A 1-way ANOVA revealed that no statistical differences in bond strength were found between the four groups. SBS values of groups I (11.7 ± 3.9), II (11.6 ± 4.6), III (10.3 ± 4.1), and IV (10.8 ± 3.9) demonstrated mean SBSs considered adequate. The iBond Total Etch (20%) and iBond Total Etch (35%) groups were more likely to have an ARI score of 2-3 than the control group (Transbond XT). No significant differences were found between iBond Self Etch and the control group. Conclusion: The SBS's of all three groups, as compared to the control group, were adequate. The iBond Total Etch system, whether used with iBond 20 gel or iBond 35 gel, had more adhesive remaining on the tooth surface after debonding. Standardization amongst shear bond strength studies is significantly needed in the near future in order to accurately compare findings.
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SURFACE ROUGHNESS AND SUPERHYDROPHOBICITY BEHAVIOR IN ELECTROCHEMICALLY-ETCHED FE- AND NI-BASED ALLOYSBenjamin P Smith (11820377) 09 December 2021 (has links)
<blockquote><div><div>Methods and techniques for tailoring the surface morphology of metallic surfaces are determined in part by the complex behavior of elemental interactions in conjunction with electrochemical reactions. In this work, we show how the surface morphology can be predicted based on experimental data resulting from polarization curves and compositional differences of Fe- and Ni-based superalloys. Electrochemical treatments utilizing NaCl as the electrolyte were adapted using parameters such as the pitting resistance equivalent (PRE) number and polarization curves to obtain both rough and smooth surfaces. Utilizing these metrics, we electrochemically etched Inconel 600, SS304, Inconel 718 and Inconel 625 obtaining average surface roughness values that ranged from 0.05 to 57.4 μm indicating the success of tailoring the technique to obtaining rough and smooth surfaces. The effect of current density, current pulsing, and temperature were varied to elucidate roughness and pitting behavior, and strong correlations to the PRE number and polarization curve properties of the alloy were observed. Heat treatments and subsequent evolution to the microstructure in the form of grain growth and precipitation altered the etching behavior. These techniques can be used in preventing corrosion failure and enhancing electrochemical machining</div></div></blockquote>
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Study of ohmic contact formation on AlGaN/GaN heterostructuresWen, Kai-Hsin January 2019 (has links)
It is challenging to achieve low-resistive ohmic contacts to III-nitride semiconductors due to their wide bandgap. A common way to reduce the contact resistance is to recess the ohmic area prior to metallization. In the minimization of the contact resistance, parameters like the recess depth, anneal temperature and design of the metal stack are commonly optimized. In this work, three other approaches have been evaluated. All experiments were performed on AlGaN/GaN heterostructures. The fabricated ohmic contacts were recess etched, metallized with a Ta/Al/Ta stack, and annealed at 550-575◦C.Firstly, it is shown that the laser writer intensity, transmittance and focus offset during optical lithography affect the contact resistance. The reason is believed to be the variation in the resist profile, which has an impact on the metal coverage. At the optimum intensity/transmittance/focus condition, which generates a relatively medium undercut, a contact resistance of 0.23 Ωmm was obtained.In the second approach, the metal layer of annealed contacts was removed by wet etching, followed by the re-deposition of a metal stack and annealing. The purpose was to increase the amount of N vacancies in the AlGaN, which are responsible for the contact formation. A minimum contact resistance of 0.41 Ωmm was achieved with this method, compared to 0.28 Ωmm with the regular method (without remetallization).In the last approach, the bottom Ta layer was sputtered, whereas evaporation was used in all other cases. The minimum contact resistance was found to be 0.6 Ωmm, which was higher than for the evaporated contacts. The reason was assumed that the thickness of sputtered Ta should be thinner than the evaporated Ta due to its higher density. Moreover, the obtained lower sheet resistance is assumed to caused by the atomic scale damage due to the high energy ions during sputtering. / En utmaning med III-nitrid-halvledare är att uppnå låg-resistivitetskontakter, på grund av deras breda bandgap. Ett konventionellt tillvägagångsätt för att reducera kontaktresistansen är att fördjupa ohmska ytan före metallisering. I strävandet av att minska den ohmska resistansen sker vanligtvis en optimering av följande parametrar, recessddjup, anlöpningstemperatur och metallagersdesign. I detta arbete så har samtliga tre parametrar evaluerats. Alla experiment utfördes på AlGaN/GaNheterostrukturer. De tillverkade ohmska kontakterna var recesssetsade, metalliserade med ett Ta/Al/Ta lager och anlöpt vid 550-575◦C.Den primära undersökningen, visar att laserritar-intensitet, -transmission och fokusförskjutning under optisk litografi inverkar på kontaktresistansen. Anledningen antas vara variation i resistprofilen, vilket påverkar metallbeläggningen. Vid optimal intensitet/transmission/fokus-förhållanden, (som genererar en underskärning), blev den resulterande kontaktresistansen 0.23 Ωmm uppmätt.I en sekundär undersökning, avlägsnas ohmska kontaktens metallager genom våtetsning, följt av en återdeponering av ett nytt metallager, samt anlöpning. Syftet var att öka mängden N-vakanser i AlGaN-lagret, som formar ohmska kontakten. Minsta kontaktresistansen uppmätt var 0.41Wmm, att jämföras med 0.28 Ωmm, som uppnåddes genom den konventionella metoden (utan återmetallisering).Den sista undersökningen jämförde sputtrade med evaporerade bottenlager av Ta, (evaporation användes som standardmetod i de tidigare undersökningarna). Med sputtrning blev den minsta kontakresistansen 0.6 Ωmm, (högre än de evaporerade kontakterna). En hypotetisk förklarning kan vara att det sputtrade Ta-lagret är tunnare än det evaporerade Ta-lagret, på grund av en dess högre densitet. Därutöver, den uppmätta lägre skiktresistansen antas bero på den skada i atomskala som sker vid de höga energi-kollisioner som joner skapar vid sputtrning.
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Plant Virus Diagnostics: Comparison of classical and membrane-based techniques for immunoassay and coat protein sequence characterization for Cucumber mosaic virus and three potyvirusesChang, Peta-Gaye Suzette 06 July 2009 (has links)
Diagnostics is important in the development and implementation of pest management strategies. The virus diagnostic capabilities of several plant pathology collaborators within the Integrated Pest Management Collaborative Research Support Program (IPM CRSP) host countries were evaluated with the aid of a survey. Very few plant disease diagnostic clinics had funds to cover daily operations despite over half of the responding clinics receiving an operational budget. Academically and government affiliated clinics within the developing host countries had little access to molecular tools and equipment, relying mostly on biological and serological methods. Clinics affiliated with private companies and within the USA relied more upon molecular assays. Ten CMV isolates identified by tissue blot immunoassay (TBIA) were collected from a garden at the Historic Smithfield Plantation on the Virginia Tech campus, and from Painter, Virginia on the Eastern Shore. Three CMV isolates from Smithfield were biologically compared to six early CMV isolates stored since the 1970s, while all isolates were compared serologically and molecularly. Sequences obtained after reverse transcription-polymerase chain reaction (RT-PCR) assigned the CMV isolates into subgroups, with eleven to subgroup 1A and three to subgroup 2. The subgroup assignments were confirmed by TBIA using CMV subgroup-specific monoclonal antibodies (Agdia Inc). At Smithfield Plantation, another virus, Turnip mosaic virus (TuMV) was identified from Dame's Rocket (Hesperis matronalis L.). This is the first report of TuMV in Virginia. In TBIA virus-infected plant samples are blotted onto nitrocellulose membranes, dried, and processed. Membranes can be stored for long periods of time and transported safely across borders without risk of introducing viruses into new environments, but virus remains immunologically active for several months. Methods were developed with CMV and three potyviruses, using the same membranes, for detecting viral RNA by RT-PCR and direct sequencing of PCR products.. Amplification by RT-PCR was possible after membrane storage for up to 15 months. The membranes also performed well with samples sent from IPM CRSP host countries and within the USA. This method should improve molecular diagnostic capabilities in developing countries, as samples can be blotted to membranes and sent to a centralized molecular laboratory for analysis. / Ph. D.
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Transport Studies In The Ferromagnetic Semiconductor (Ga,Mn)AsOpondo, Noah F. 13 August 2009 (has links)
No description available.
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Characterization and modeling of dry etch processes for titanium nitride and titanium films in Cl₂/N₂ and BCl₃ plasmasMuthukrishnan, N. Moorthy 06 June 2008 (has links)
In the past few years, the demands for high speed semiconductor integrated circuits have warranted new techniques in their fabrication process which will meet the ever-shrinking dimensions. The gaseous plasma assisted etching is one of these revolutionary processes. However, the plasma and the etch process are very complex in nature. It has been very difficult to understand various species present in the plasma and their role in the etch reaction. In addition, the submicron geometries also require interconnect materials which will satisfy the necessary properties such as thermal stability and low electrical resistance. Titanium (Ti) and titanium nitride (TiN) are widely used as barriers between aluminum (Al) and silicon (Si) to prevent the destructive intermixing of these two materials. The process of patterning of the interconnect containing Ti and TiN along with Al has been a challenge to the semiconductor process engineers. Therefore, complete characterization of the plasma etch process of Ti and TiN films and development of mathematical models to represent the responses such as the etch rate and uniformity is necessary for a good understanding of the etching process. A robust and well controlled metal etch process usually results in good die yield per wafer and hence can translate into higher profits for the semiconductor manufacturer.
The objective of this dissertation is to characterize the plasma etch processes of Ti and TiN films in chlorine containing plasmas such as BCl₃ and Cl₂/N₂ and to develop mathematical models for the etch processes using statistical experimental design and analysis technique known as Response Surface Methodology (RSM). In this work, classical experiments are conducted on the plasma etch process of Ti and TiN films by varying the process parameters, such as gas flow, radio frequency (RF) power, reaction pressure, and temperature, one parameter at a time, while maintaining the other parameters constant. The variation in the etch rate with the change in the process parameter of the film is studied and the results were explained in terms of the concepts of plasma. These experiments, while providing very good understanding of the main effects of the parameters, yield little or no information on the higher order effects or interaction between the process parameters. Therefore, modern experimental design and analysis techniques using computerized statistical methods need to be employed for developing mathematical models for these complex plasma etch processes.
The second part of this dissertation concentrates on the Design and Analysis of Experiments using Response Surface Methodology (RSM) and development of models for the etch rate and the etch uniformity of the Ti and TiN films in chlorine-containing plasmas such as Cl₂/N₂ and Cl₂/N₂/BCl₃. A complete characterization of the plasma etch process of Ti and TiN films is achieved with the RSM technique and a well fitting and statistically significant models have been developed for the process responses, such as the etch rate and the etch uniformity. These models also provide a means for quantitative comparison of main effects, which are also known as first order effects, second order effects and two factor interactions. The models, thus developed, can be effectively used for an etch process optimization, prediction of the responses without actually conducting the experiments, and the determination of process window.
This dissertation work has achieved a finite study of the plasma etch process of Ti and TiN films. There is tremendous potential and scope for further research in this area, limited only by the available resources for wafer processing. A few of the possibilities for further research is discussed in the next few sentences. The optimized process derived from the RSM technique needs to be implemented in the actual production process of the semiconductor ICs and its effects on the wafer topography, etch residue and the resulting die yield have to be studied. More research studies are needed to examine the effect of process parameters such as temperature, the size and shape of the etch chamber, the quality of the film being etched, among other parameters. It is worth emphasizing in this respect that this dissertation marks beginning of research work into the ever-increasing complexities of gas plasma. / Ph. D.
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Three-Dimensional Passivated-Electrode Insulator-Based Dielectrophoresis (3D-PiDEP)Zellner, Phillip Andrew 25 July 2013 (has links)
The focus of this research is the isolation of waterborne pathogens which are one of the grand challenges to human health, costing the lives of about 2.5 million people worldwide each year. The aim was to develop new microfluidic techniques for selectively concentrating and detecting waterborne pathogens. Detection of microbes in water can greatly help reduce deaths; however, analytical instruments cannot readily detect them due to the extreme dilution of these microbes, and hence, require significant sample concentration. Current methods are expensive and either require days to process or are not sufficiently robust for water monitoring. Microfluidic chips based on insulator-based dielectrophoresis (iDEP) provide a promising solution to these problems and have been previously used to selectively concentrate biological particle such as bacteria. The microfluidic devices in this work were created with a 3D mircofabrication technique, which we also developed as part of this project. The core process of the technique is the etching of 3D structures in silicon with a single plasma etch utilizing an effect known as reactive ion etch lag (RIE lag). Using this unique process, 3D devices are fabricated in both silicon and the polymer polydimenthylsiloxane (PDMS). Using both numerical modeling and experimental results, we show how these 3D structures enhance the performance of the dielectrophoretic devices. The main findings indicate that 3D structures can help reduce Joule heating in the devices and lower the applied voltage necessary to operate the devices. Additionally, within this work, we develop a new dielectrophoresis technique called off-chip passivated-electrode, insulator-based dielectrophoresis microchip (O"DEP). This technique combines the sensitivity of electrode-based dielectrophoresis (eDEP) with the high-throughput and inexpensive device characteristics of insulator-based dielectrophoresis. The result is a cartridge based system which is accessible, economical, high-performance, and high-throughput technologies allowing timely detection of pathogenic bacteria. / Ph. D.
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