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Analyses of Particulate Contaminants in Semiconductor Processing Fluids

Description: Particle contamination control is a critical issue for the semiconductor industry. In the near future, this industry will be concerned with the chemical identities of contaminant particles as small as 0.01 pm in size. Therefore, analytical techniques with both high chemical sensitivity and spatial resolution are required. Transmission electron microscopy (TEM) provides excellent spatial resolution and yields structural and compositional information. It is rarely used, however, due to the difficulty of sample preparation. The goals of this research are to promote the use of TEM as an ultrafine particle analysis tool by developing new sample preparation methods, and to exploit the new TEM techniques for analysis of particles in semiconductor processing fluids. A TEM methodology for the analysis of particulate contaminants in fluids with an elemental detectability limit as low as 0.1 part per trillion (ppt), and a particle concentration detectability limit as low as 1 particle/ml for particles greater than 0.2 pm was developed and successfully applied to the analysis of particles in HF, H202, de-ionized (DI) water, and on the surface of an electronic device. HF samples from three manufacturers were examined. For HF (B), the maximum particle concentration was 8.3 x 103 particles/ml. Both a viscous material and lath-shaped particles were observed. The Sb concentration was less than 0.6 part per billion (ppb). HF (C) was the cleanest. CaF2 and TiO2 particles were identified in HF (D). For H2 02, iron and tin oxides and hydroxides were identified. The maximum particle concentration was 990 particles/ml. The Sn and Fe concentrations were less than 0.3 ppb. Spherical and dendritic particles were observed. For DI water, spherical and dendritic particles (<2 particles/ml), and particles containing Fe or Si with concentrations less than 0.1 ppt were observed. Contaminants on an electronic device surface were also analyzed. Clusters of small particles ...
Date: August 1998
Creator: Xu, Daxue

Investigation of growth kinetics of self-assembling monolayers by means of contact angle, optical ellipsometry, angle-resolved XPS and IR spectroscopy.

Description: Absorption of octadecanethiol and p-nitrobenzenethiol onto gold surfaces from ethanol solutions has been studied by means of contact angle, optical ellipsometry, angle-resolved XPS (ARXPS), and with grazing angle total reflection FTIR. Growth of the monolayers from dilute solutions has been monitored and Langmuir isotherm adsorption curves were fitted to experimental data. A saturated film is formed within approximately 5h after immersion in solutions of concentrations ranging from 0.0005mM to 0.01mM. We found, that the final density of monolayer depends on the concentration of the solution.
Date: August 2004
Creator: Jakubowicz, Agnieszka

Characterization of Methyltrimethoxysilane Sol-Gel Polymerization and the Resulting Aerogels.

Description: Methyl-functionalized porous silica is of considerable interest as a low dielectric constant film for semiconductor devices. The structural development of these materials appears to affect their gelation behaviors and impact their mechanical properties and shrinkage during processing. 29Si solution NMR was used to follow the structural evolution of MTMS (methyltrimethoxysilane) polymerization to gelation or precipitation, and thus to better understand the species that affect these properties and gelation behaviors. The effects of pH, water concentration, type of solvents, and synthesis procedures (single step acid catalysis and two-step acid/base catalysis) on MTMS polymerization were discussed. The reactivity of silicon species with different connectivity and the extent of cyclization were found to depend appreciably on the pH value of the sol. A kinetic model is presented to treat the reactivity of both silicon species involved in condensations separately based on the inductive and steric effects of these silicon species. Extensive cyclization in the presence of acid, which was attributed to the steric effects among numerous reaction pathways for the first time, prevents MTMS gelation, whereas gels were obtained from the two-step method with nearly random condensations. The experimental degree of condensation (DC) at the gel point using the two-step procedure was determined to be 0.86, which is considerably higher than that predicted by the current accepted theories. Both chemical and physical origins of this high value were suggested. Aerogels dried by supercritical CO2 extraction were characterized by FTIR, 13C and 29Si solid-state NMR and nitrogen sorption. The existence of three residual groups (Si-OH, Si-OCH3, and Si-OC2H5) was confirmed, but their concentrations are very low compared to silica aerogels. The low concentrations of the residual groups, along with the presence of Si-CH3, make MTMS aerogels permanently hydrophobic. To enhance applicability, MTMS aerogels were successfully prepared that demonstrated shrinkage less than 10% after supercritical ...
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Date: August 2003
Creator: Dong, Hanjiang

Application of Thermomechanical Characterization Techniques to Bismuth Telluride Based Thermoelectric Materials

Description: The thermoelectric properties of bismuth telluride based thermoelectric (TE) materials are well-characterized, but comparatively little has been published on the thermomechanical properties. In this paper, dynamic mechanical analysis (DMA) and differential scanning calorimetry data for bismuth telluride based TE materials is presented. The TE materials' tan delta values, indicative of viscoelastic energy dissipation modes, approached that of glassy or crystalline polymers, were greater than ten times the tan delta of structural metals, and reflected the anisotropic nature of TE materials. DMA thermal scans showed changes in mechanical properties versus temperature with clear hysteresis effects. These results showed that the application of DMA techniques are useful for evaluation of thermophysical and thermomechanical properties of these TE materials.
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Date: August 2002
Creator: White, John B.

Mechanical Properties of Polymer Modified Mortar

Description: The mechanical properties of the polymer-modified mortar are markedly improved over conventional cement mortar. We utilized recycled ABS in powder form and a polymer latex emulsion, polymer percentage ranges from 0 to 25 percent by polymer/cement ratio were investigated. The mechanical properties investigated were compression strength and adhesion strength. Compression strength effects did not have an impact on adhesion strength. Adhesion strength was calculated with pullout testing apparatus designed by the author. Results indicate that recycled ABS had a lower adhesive strength than the acrylic latex emulsion and the base mortar, but did increase in adhesive strength when mixed with maleic-anhydride. The adhesive strength was investigated for a Fiber Reinforced Polymer (FRP) made of an "E" glass fiber that is a continuous strand roving oriented and pre-tensioned longitudinally in an isopthalic polyester matrix material. The FRP rebar was compared to standard steel rebars, and found that the standard steel corrugated rebar had a higher adhesive strength, due to mechanical interlocking. This was clarified by measurements using a smooth steel rebar. Characterization of the polymer-modified mortar was conducted by pore analysis and scanning electron microscopy. Scanning Electron Microscopy was implemented to view the polymer particles, the cement fibrils formed by the hydration, and to prove Ohama's theory of network structure.
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Date: August 2002
Creator: Palos, Artemio

Fabrication of MOS capacitor and transitor structure using contact photolithography.

Description: This problem in lieu of thesis report describes a practical photolithographic method to produce micro patterns on metal-oxide-semiconductor or metal-oxide-semiconductor-metal layers for electrical measurements. The desired patterns are then transferred from the photo mask to the photoresist-coated metal film by exposure, followed by wet etching. In the procedure described in this report, it was observed that microstructures as small as 27 mm with an edge roughness of ~ 2 mm can be reproducibly generated with this process. MOS capacitors and transistors structures can be fabricated by using this technique. The method described in this report requires access to only simple facilities so that it is relatively inexpensive, and the overall time required for the whole process is short.
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Date: August 2002
Creator: Su, Danni

Influence of design and coatings on the mechanical reliability of semiconductor wafers.

Description: We investigate some of the mechanical design factors of wafers and the effect on strength. Thin, solid, pre-stressed films are proposed as a means to improve the bulk mechanical properties of a wafer. Three-point bending was used to evaluate the laser scribe density and chemical processing effect on wafer strength. Drop and strike tests were employed to investigate the edge bevel profile effect on the mechanical properties of the wafer. To characterize the effect of thin films on strength, one-micron ceramic films were deposited on wafers using PECVD. Coated samples were prepared by cleaving and were tested using four-point bending. Film adhesion was characterized by notched four-point bending. RBS and FTIR were used to obtain film chemistry, and nanoindentation was used to investigate thin film mechanical properties. A stress measurement gauge characterized residual film stress. Mechanical properties of the wafers correlated to the residual stress in the film.
Date: August 2002
Creator: Yoder, Karl J.

Materials properties of hafnium and zirconium silicates: Metal interdiffusion and dopant penetration studies.

Description: Hafnium and Zirconium based gate dielectrics are considered potential candidates to replace SiO2 or SiON as the gate dielectric in CMOS processing. Furthermore, the addition of nitrogen into this pseudo-binary alloy has been shown to improve their thermal stability, electrical properties, and reduce dopant penetration. Because CMOS processing requires high temperature anneals (up to 1050 °C), it is important to understand the diffusion properties of any metal associated with the gate dielectric in silicon at these temperatures. In addition, dopant penetration from the doped polysilicon gate into the Si channel at these temperatures must also be studied. Impurity outdiffusion (Hf, Zr) from the dielectric, or dopant (B, As, P) penetration through the dielectric into the channel region would likely result in deleterious effects upon the carrier mobility. In this dissertation extensive thermal stability studies of alternate gate dielectric candidates ZrSixOy and HfSixOy are presented. Dopant penetration studies from doped-polysilicon through HfSixOy and HfSixOyNz are also presented. Rutherford backscattering spectroscopy (RBS), heavy ion RBS (HI-RBS), x-ray photoelectron spectroscopy (XPS), high resolution transmission electron microscopy (HR-TEM), and time of flight and dynamic secondary ion mass spectroscopy (ToF-SIMS, D-SIMS) methods were used to characterize these materials. The dopant diffusivity is calculated by modeling of the dopant profiles in the Si substrate. In this disseration is reported that Hf silicate films are more stable than Zr silicate films, from the metal interdiffusion point of view. On the other hand, dopant (B, As, and P) penetration is observed for HfSixOy films. However, the addition of nitrogen to the Hf - Si - O systems improves the dopant penetration properties of the resulting HfSixOyNz films.
Date: August 2002
Creator: Quevedo-Lopez, Manuel Angel

Polymer hydrogel nanoparticles and their networks

Description: The thermally responsive hydroxypropyl cellulose (HPC) hydrogel nanoparticles have been synthesized and characterized. The HPC particles were obtained by chemically crosslinking collapsed HPC polymer chains in water-surfactant (dodecyltrimethylammonium bromide) dispersion above the lower critical solution temperature (LCST) of the HPC. The size distributions of microgel particles, measured by dynamic light scattering, have been correlated with synthesis conditions including surfactant concentration, polymer concentration, and reaction temperature. The swelling and phase transition properties of resultant HPC microgels have been analyzed using both static and dynamic light scattering techniques. By first making gel nanoparticles and then covalently bonding them together, we have engineered a new class of gels with two levels of structural hierarchy: the primary network is crosslinked polymer chains in each individual particle, while the secondary network is a system of crosslinked nanoparticles. The covalent bonding contributes to the structural stability of the nanostructured gels, while self-assembly provides them with crystal structures that diffract light, resulting in colors. By using N-isopropylacrylamide copolymer hydrogel nanoparticles, we have synthesized nanoparticle networks that display a striking iridescence like precious opal but are soft and flexible like gelatin. This is in contrast to previous colored hydrogels, which were created either by adding dyes or fluorescent, or by organic solvent or by embedding a colloidal crystal array of polymer solid spheres . Creating such periodic 3D structures in materials allows us to obtain useful functionality not only from the constituent building blocks but also from the long-range ordering that characterizes these structures. Hydroxypropyl cellulose (HPC) and poly (acrylic acid ) (PAA) complexes were studied using turbidity measurement and laser light scattering. The phase transition temperature of the complexes is found to depend on pH and molecular weights of PAA and HPC. The driving force for this phenomenon is due to the hydrogen bonding and hydrophobic interaction ...
Date: August 2002
Creator: Lu, Xihua

Polyamide-imide and Montmorillonite Nanocomposites

Description: Solvent suspensions of a high performance polymer, Polyamide-imide (PAI) are widely used in magnetic wire coatings. Here we investigate the effect that the introduction of montmorillonite (MMT) has on PAI. MMT was introduced into an uncured PAI suspension; the sample was then cured by step-wise heat treatment. Polarized optical microscopy was used to choose the best suitable MMT for PAI matrix and to study the distribution of MMT in PAI matrix. Concentration dependent dispersion effect was studied by x-ray diffraction (XRD) and was confirmed by Transmission electron microscopy (TEM). Differential scanning Calorimetry (DSC) and Thermogravimetric analysis (TGA) was used to study impact of MMT on glass transition temperature (Tg) and degradation properties of PAI respectively. Micro-hardness testing of PAI nanocomposites was also performed. A concentration dependent state of dispersion was obtained. The glass transition (Tg), degradation and mechanical properties were found to correlate to the state of dispersion.
Date: August 2001
Creator: Ranade, Ajit

Thermal, Electrical, and Structural Analysis of Graphite Foam

Description: A graphite foam was developed at Oak Ridge National Laboratory (ORNL) by Dr. James Klett and license was granted to POCO Graphite, Inc. to manufacture and market the product as PocoFoam™. Unlike many processes currently used to manufacture carbon foams, this process yields a highly graphitic structure and overcomes many limitations, such as oxidation stabilization, that are routinely encountered in the development of carbon foam materials. The structure, thermal properties, electrical resistivity, isotropy, and density uniformity of PocoFoam™ were evaluated. These properties and characteristics of PocoFoam™ are compared with natural and synthetic graphite in order to show that, albeit similar, it is unique. Thermal diffusivity and thermal conductivity were derived from Fourier's energy equation. It was determined that PocoFoam™ has the equivalent thermal conductivity of metals routinely used as heat sinks and that thermal diffusivity is as much as four times greater than pure copper and pure aluminum. SEM and XRD results indicate that PocoFoam™ has a high degree of crystalline alignment and near theoretical d spacing that is more typical of natural flake graphite than synthetic graphite. PocoFoam™ is anisotropic, indicating an isotropy factor of 0.5, and may yield higher thermal conductivity at cryogenic temperatures than is observed in polycrystalline graphite.
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Date: August 2001
Creator: Morgan, Dwayne Russell