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At least 1,747 records · Page 97

Quantum cascade laser based monitoring of CF{sub 2} radical concentration as a diagnostic tool of dielectric etching plasma processes

Dielectric etching plasma processes for modern interlevel dielectrics become more and more complex by the introduction of new ultra low-k dielectrics. One challenge is the minimization of sidewall damage, while etching ultra low-k porous SiCOH by fluorocarbon plasmas. The optimization of this process requires a deeper understanding of the concentration of the CF{sub 2} radical, which acts as precursor in the polymerization of the etch sample surfaces. In an industrial dielectric etching plasma reactor, the CF{sub 2} radical was measured in situ using a continuous wave quantum cascade laser (cw-QCL) around 1106.2 cm{sup −1}. We measured Doppler-resolved ro-vibrational absorption lines and determined absolute densities using transitions in the ν{sub 3} fundamental band of CF{sub 2} with the aid of an improved simulation of the line strengths. We found that the CF{sub 2} radical concentration during the etching plasma process directly correlates to the layer structure of the etched wafer. Hence, this correlation can serve as a diagnostic tool of dielectric etching plasma processes. Applying QCL based absorption spectroscopy opens up the way for advanced process monitoring and etching controlling in semiconductor manufacturing.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

A study of internal structure in components made by additive manufacturing process using 3 D X-ray tomography

Additive manufacturing methods are gaining increasing popularity for rapidly and efficiently manufacturing parts and components in the industrial context, as well as for domestic applications. However, except when used for prototyping or rapid visualization of components, industries are concerned with the load carrying capacity and strength achievable by additive manufactured parts. In this paper, the wire-arc additive manufacturing (AM) process based on gas tungsten arc welding (GTAW) has been examined for the internal structure and constitution of components generated by the process. High-resolution 3D X-ray tomography is used to gain cut-views through wedge-shaped parts created using this GTAW additive manufacturing process with titanium alloy materials. In this work, two different control conditions for the GTAW process are considered. The studies reveal clusters of porosities, located in periodic spatial intervals along the sample cross-section. Such internal defects can have a detrimental effect on the strength of the resulting AM components, as shown in destructive testing studies. Closer examination of this phenomenon shows that defect clusters are preferentially located at GTAW traversal path intervals. These results highlight the strong need for enhanced control of process parameters in ensuring components with minimal defects and higher strength.

36 MATERIALS SCIENCE↗

Thermographic process monitoring in powderbed based additive manufacturing

Selective Laser Melting is utilized to build metallic parts directly from CAD-Data by solidification of thin powder layers through application of a fast scanning laser beam. In this study layerwise monitoring of the temperature distribution is used to gather information about the process stability and the resulting part quality. The heat distribution varies with different kinds of parameters including scan vector length, laser power, layer thickness and inter-part distance in the job layout which in turn influence the resulting part quality. By integration of an off-axis mounted uncooled thermal detector the solidification as well as the layer deposition are monitored and evaluated. Errors in the generation of new powder layers usually result in a locally varying layer thickness that may cause poor part quality. For effect quantification, the locally applied layer thickness is determined by evaluating the heat-up of the newly deposited powder. During the solidification process space and time-resolved data is used to characterize the zone of elevated temperatures and to derive locally varying heat dissipation properties. Potential quality indicators are evaluated and correlated to the resulting part quality: Thermal diffusivity is derived from a simplified heat dissipation model and evaluated for every pixel and cool-down phase of a layer. This allows the quantification of expected material homogeneity properties. Maximum temperature and time above certain temperatures are measured in order to detect hot spots or delamination issues that may cause a process breakdown. Furthermore, a method for quantification of sputter activity is presented. Since high sputter activity indicates unstable melt dynamics this can be used to identify parameter drifts, improper atmospheric conditions or material binding errors. The resulting surface structure after solidification complicates temperature determination on the one hand but enables the detection of potential surface defects on the other hand. These issues and proper key figures for thermographic monitoring of the Selective Laser Melting process are discussed in the paper. Even though microbolometric temperature measurement is limited to repetition rates in the Hz-regime and sub megapixel resolution, current results show the feasibility of process surveillance by thermography for a limited section of the building platform in a commercial system.

42 ENGINEERING↗

A review on the processing accuracy of two-photon polymerization

Two-photon polymerization (TPP) is a powerful and potential technology to fabricate true three-dimensional (3D) micro/nanostructures of various materials with subdiffraction-limit resolution. And it has been applied to microoptics, electronics, communications, biomedicine, microfluidic devices, MEMS and metamaterials. These applications, such as microoptics and photon crystals, put forward rigorous requirements on the processing accuracy of TPP, including the dimensional accuracy, shape accuracy and surface roughness and the processing accuracy influences their performance, even invalidate them. In order to fabricate precise 3D micro/nanostructures, the factors influencing the processing accuracy need to be considered comprehensively and systematically. In this paper, we review the basis of TPP micro/nanofabrication, including mechanism of TPP, experimental set-up for TPP and scaling laws of resolution of TPP. Then, we discuss the factors influencing the processing accuracy. Finally, we summarize the methods reported lately to improve the processing accuracy from improving the resolution and changing spatial arrangement of voxels.

36 MATERIALS SCIENCE↗

Relativistic decay widths of autoionization processes: The relativistic FanoADC-Stieltjes method

Electronic decay processes of ionized systems are, for example, the Auger decay or the Interatomic/ Intermolecular Coulombic Decay. In both processes, an energetically low lying vacancy is filled by an electron of an energetically higher lying orbital and a secondary electron is instantaneously emitted to the continuum. Whether or not such a process occurs depends both on the energetic accessibility and the corresponding lifetime compared to the lifetime of competing decay mechanisms. We present a realization of the non-relativistically established FanoADC-Stieltjes method for the description of autoionization decay widths including relativistic effects. This procedure, being based on the Algebraic Diagrammatic Construction (ADC), was adapted to the relativistic framework and implemented into the relativistic quantum chemistry program package Dirac. It is, in contrast to other existing relativistic atomic codes, not limited to the description of autoionization lifetimes in spherically symmetric systems, but is instead also applicable to molecules and clusters. We employ this method to the Auger processes following the Kr3d{sup −1}, Xe4d{sup −1}, and Rn5d{sup −1} ionization. Based on the results, we show a pronounced influence of mainly scalar-relativistic effects on the decay widths of autoionization processes.

74 ATOMIC AND MOLECULAR PHYSICS↗

Functionalization of polymer powders for SLS-processes using an atmospheric plasma jet in a fluidized bed reactor

Recently additive manufacturing processes such as selective laser sintering (SLS) of polymers have gained more importance for industrial applications [1]. Tailor-made modification of polymers is essential in order to make these processes more efficient and to cover the industrial demands. The so far used polymer materials show weak performance regarding the mechanical stability of processed parts. To overcome this limitation, a new route to functionalize the surface of commercially available polymer particles (PA12; PE-HD; PP) using an atmospheric plasma jet in combination with a fluidized bed reactor has been investigated. Consequently, an improvement of adhesion and wettability [2] of the polymer surface without restraining the bulk properties of the powder is achieved. The atmospheric plasma jet process can provide reactive species at moderate temperatures which are suitable for polymer material. The functionalization of the polymer powders improves the quality of the devices build in a SLS-process.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

A novel process route for the production of spherical SLS polymer powders

Currently, rapid prototyping gradually is transferred to additive manufacturing opening new applications. Especially selective laser sintering (SLS) is promising. One drawback is the limited choice of polymer materials available as optimized powders. Powders produced by cryogenic grinding show poor powder flowability resulting in poor device quality. Within this account we present a novel process route for the production of spherical polymer micron-sized particles of good flowability. The feasibility of the process chain is demonstrated for polystyrene e. In a first step polymer microparticles are produced by a wet grinding method. By this approach the mean particle size and the particle size distribution can be tuned between a few microns and several 10 microns. The applicability of this method will be discussed for different polymers and the dependencies of product particle size distribution on stressing conditions and process temperature will be outlined. The comminution products consist of microparticles of irregular shape and poor powder flowability. An improvement of flowability of the ground particles is achieved by changing their shape: they are rounded using a heated downer reactor. The influence of temperature profile and residence time on the product properties will be addressed applying a viscous-flow sintering model. To further improve the flowability of the cohesive spherical polymer particles nanoparticles are adhered onto the microparticles’ surface. The improvement of flowability is remarkable: rounded and dry-coated powders exhibit a strongly reduced tensile strength as compared to the comminution product. The improved polymer powders obtained by the process route proposed open new possibilities in SLS processing including the usage of much smaller polymer beads.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Structural modification of nanocrystalline diamond films via positive/negative bias enhanced nucleation and growth processes for improving their electron field emission properties

Electron field emission (EFE) properties of nanocrystalline diamond (NCD) films synthesized by the bias-enhanced growth (beg) process under different bias voltages were investigated. The induction of the nanographitic phases is presumed to be the prime factor in enhancing the EFE properties of negative biased NCD films. Transmission electron microscopic investigations reveal that a negative bias voltage of −300 V increases the rate of growth for NCD films with the size of the grains changing from nano to ultranano size. This effect also is accompanied by the induction of nanographitic filaments in the grain boundaries of the films. The turn-on field (E{sub 0}) for the EFE process then effectively gets reduced. The EFE process of the beg-NCD{sub −300V} films can be turned on at E{sub 0} = 3.86 V/μm, and the EFE current density achieved is 1.49 mA/cm{sup 2} at an applied field of 7.85 V/μm. On the other hand, though a positive-bias beg process (+200 V) results in the reduction of grain size, it does not induce sufficient nanographitic phases to lower the E{sub 0} value of the EFE process. Moreover, the optical emission spectroscopic investigation indicates that one of the primary causes that changes the granular structure of the NCD films is the increase in the proportion of C{sub 2} and CH species induced in the growing plasma. The polarity of the bias voltage is of less importance in the microstructural evolution of the films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Direct observation of atomic-level nucleation and growth processes from an ultrathin metallic glass films

Till date, there have been no direct atomic-level experimental observations of the earliest stages of the nucleation and growth processes of nanocrystals formed by thermally induced crystallization in ultrathin metallic glasses (MGs). Here, we present a study of the crystallization process in atomically thin and highly stable MG films using double spherical aberration-corrected scanning transmission electron microscopy (Cs-TEM). Taking advantage of the stability of MG films with a slow crystallization process and the atomic-level high resolution of Cs-TEM, we observe the formation of the nucleus precursor of nanocrystals formed by atom aggregation followed by concomitant coalescence and stepwise evolution of the shape of the nanocrystals with a monodispersed and separated bimodal size distribution. Molecular dynamics simulation of the atomic motion in the glass film on a rigid amorphous substrate confirms the stepwise evolution processes of atom aggregation, cluster formation, cluster movement on the substrate, and cluster coalescence into larger crystalline particles. Our results might provide a better fundamental understanding of the nucleation and growth processes of nanocrystals in thin MG films.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Growth of α-V{sub 2}O{sub 5} nanostructured thin films as a function of deposition process

In this communication, we synthesizedvanadium pentoxide (α-V{sub 2}O{sub 5}) nanostructured thin films (NSTs) using four different methods for obtaining vanadate species namely thermal evaporation (source of vanadate species are V{sub 2}O{sub 5} powder and vanadium metal foil) and plasma assisted sublimation process (source of vanadate species are V{sub 2}O{sub 5} powder and vanadium metal foil). The effect of plasmaon morphological and structural propertieshave been systematicallystudied. XRD revealed thermal evaporation process yielded amorphous films whereassublimation process yielded highly crystalline α-V{sub 2}O{sub 5} films. HRTEM of nanobelts show, the growth is preferred in (001) crystallographic direction with interplanar distance of 0.43 nm. XPS revealed O/V ratio of ~2.4, which nearly agrees with standard V{sub 2}O{sub 5} stoichiometry. SEM revealed deposition process affect morphology of films; thermal evaporation results in smoother film while plasma assisted sublimation process reveals nanoflakes and nanobelts (NBs). All the results are inconcordance with each other.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Study on process and characterization of high-temperature resistance polyimide composite

A novel polyimide composite with upper-use temperature of 420°C was prepared by autoclave process. The thermogravimetic analysis and rheological properties of uncured polyimide resin powders were analyzed. The influences of process parameters and post-treatment process on the properties of composites were also investigated. The morphologies of polyimide composites after shear fracture were observed by scanning electron microscope (SEM). The high-temperature resistance of composite was characterized by dynamic mechanical thermal analyzer (DMTA). Results showed that the imidization reaction mainly occurred in the temperature range of 100°C~220°C, and the largest weight loss rate appearing at 145°C indicated a drastic imidization reaction occurred. The melt viscosity of polyimide resin decreased with increasing the temperature between 220°C ∼305°C, and then increased with the increase of temperature due to the molecular crosslinking reactions. The fiber volume contents and void contents could be effectively controlled by applying the pressure step by step. The fiber volume content was sensitive to the initial pressure (P{sub i}) during the imidization. The second-stage pressure (P{sub 2}) and the temperature for applying the P{sub 2} (T{sub 2}) during the imidization had a great effect on the void content of composite. Good mechanical properties and interfacial adhesion of polyimide composite could obtain by optimized process. The post-treatment process can obviously increase the high-temperature resistance of polyimide composite. The polyimide composite treated at 420°C exhibited good retention of mechanical properties at 420°C and had a glass transition temperature (Tg) of 456°C. The retentions of flexible strength, flexible modulus and short beam shear strength of polyimide composite at 420°C were 65%, 84% and 62% respectively.

36 MATERIALS SCIENCE↗

Effect of annealing on the laser induced damage of polished and CO{sub 2} laser-processed fused silica surfaces

We investigate the effect of different heat treatments on the laser-induced damage probabilities of fused silica samples. Isothermal annealing in a furnace is applied, with different temperatures in the range 700–1100 °C and 12 h annealing time, to super-polished fused silica samples. The surface flatness and laser damage probabilities at 3 ns, 351 nm are measured before and after the different annealing procedures. We have found a significant improvement of the initial laser damage probabilities of the silica surface after annealing at 1050 °C for 12 h. A similar study has been conducted on CO{sub 2} laser-processed sites on the surface of the samples. Before and after annealing, we have studied the morphology of the sites, the evolution of residual stress, and the laser-induced damage threshold measured at 351 nm, 3 ns. In this case, we observe that the laser damage resistance of the laser created craters can reach the damage level of the bare fused silica surface after the annealing process, with a complete stress relieve. The obtained results are then compared to the case of local annealing process by CO{sub 2} laser irradiation during 1 s, and we found similar improvements in both cases. The different results obtained in the study are compared to numerical simulations made with a thermo-mechanical model based on finite-element method that allows the simulation of the isothermal or the local annealing process, the evolution of stress and fictive temperature. The simulation results were found to be very consistent with experimental observations for the stresses evolution after annealing and estimation of the heat affected area during laser-processing based on the density dependence with fictive temperature. Following this work, the temperature for local annealing should reach 1330–1470 °C for an optimized reduction of damage probability and be below the threshold for material removal, whereas furnace annealing should be kept below the annealing point to avoid sample deformation.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Characterization of process-induced damage in Cu/low-k interconnect structure by microscopic infrared spectroscopy with polarized infrared light

Microscopic Fourier-transform infrared (FT-IR) spectra are measured for a Cu/low-k interconnect structure using polarized IR light for different widths of low-k spaces and Cu lines, and for different heights of Cu lines, on Si substrates. Although the widths of the Cu line and the low-k space are 70 nm each, considerably smaller than the wavelength of the IR light, the FT-IR spectra of the low-k film were obtained for the Cu/low-k interconnect structure. A suitable method was established for measuring the process-induced damage in a low-k film that was not detected by the TEM-EELS (Transmission Electron Microscope-Electron Energy-Loss Spectroscopy) using microscopic IR polarized light. Based on the IR results, it was presumed that the FT-IR spectra mainly reflect the structural changes in the sidewalls of the low-k films for Cu/low-k interconnect structures, and the mechanism of generating process-induced damage involves the generation of Si-OH groups in the low-k film when the Si-CH{sub 3} bonds break during the fabrication processes. The Si-OH groups attract moisture and the OH peak intensity increases. It was concluded that the increase in the OH groups in the low-k film is a sensitive indicator of low-k damage. We achieved the characterization of the process-induced damage that was not detected by the TEM-EELS and speculated that the proposed method is applicable to interconnects with line and space widths of 70 nm/70 nm and on shorter scales of leading edge devices. The location of process-induced damage and its mechanism for the Cu/low-k interconnect structure were revealed via the measurement method.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Recombination activity of grain boundaries in high-performance multicrystalline Si during solar cell processing

Here in this work, we applied internal quantum efficiency mapping to study the recombination activity of grain boundaries in High Performance Multicrystalline Silicon under different processing conditions. Wafers were divided into groups and underwent different thermal processing, consisting of phosphorus diffusion gettering and surface passivation with hydrogen rich layers. After these thermal treatments, wafers were processed into heterojunction with intrinsic thin layer solar cells. Light Beam Induced Current and Electron Backscatter Diffraction were applied to analyse the influence of thermal treatment during standard solar cell processing on different types of grain boundaries. The results show that after cell processing, most random-angle grain boundaries in the material are well passivated, but small-angle grain boundaries are not well passivated. Special cases of coincidence site lattice grain boundaries with high recombination activity are also found. Based on micro-X-ray fluorescence measurements, a change in the contamination level is suggested as the reason behind their increased activity. Published by AIP Publishing.

36 MATERIALS SCIENCE↗

Effect of self-bias on cylindrical capacitive discharge for processing of inner walls of tubular structures—Case of SRF cavities

Cylindrical capacitive discharge is a convenient medium for generating reactive ions to process inner walls superconductive radio-frequency (SRF) cavities. These cavities, used in particle accelerators, present a three-dimensional structure made of bulk Niobium, with axial cylindrical symmetry. Manufactured cavity walls are covered with Niobium oxides and scattered particulates, which must be removed for desired SRF performance. Cylindrical capacitive discharge in a mixture of Ar and Cl 2 is a sole and natural non-wet acid choice to purify the inner surfaces of SRF cavities by reactive ion etching. Coaxial cylindrical discharge is generated between a powered inner electrode and the grounded outer electrode, which is the cavity wall to be etched. Plasma sheath voltages were tailored to process the outer wall by providing an additional dc current to the inner electrode with the help of an external compensating dc power supply and corrugated design of the inner electrode. The dc bias potential difference is established between two electrodes to make the set-up favorable for SRF wall processing. To establish guidelines for reversing the asymmetry and establishing the optimal sheath voltage at the cavity wall, the dc self-bias potential and dc current dependence on process parameters, such as gas pressure, rf power and chlorine content in the Ar/Cl 2 gas mixture was measured. In conclusion, the process is potentially applicable to all concave metallic surfaces.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Effect of the preform fabrication process on the properties of all-silica optical fibres

In this paper, we present a detailed comparison of technical capabilities of processes for the fabrication of all-silica optical fibre preforms with the use of an atmospheric pressure radio frequency plasma (POVD process) and low-pressure microwave plasma (PCVD process) and analyse the origin of the difference in optical properties between fibres produced by these methods. It is shown that the higher temperature of the core material and the higher oxygen partial pressure in preform fabrication by the POVD process lead to an increase in optical losses in the visible and UV spectral regions in the silica fibres with low hydroxyl (OH) content and a decrease in the solarisation resistance of the fibres with high OH content, i.e. to a more rapid increase in background losses in response to UV irradiation. No such drawbacks are detected in the case of the growth of reflective layers by the PCVD process. (paper)

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Interplay of catalysis, fidelity, threading, and processivity in the exo- and endonucleolytic reactions of human exonuclease I

Human exonuclease 1 (hExo1) is a member of the RAD2/XPG structure-specific 5'-nuclease superfamily. Its dominant, processive 5'–3' exonuclease and secondary 5'-flap endonuclease activities participate in various DNA repair, recombination, and replication processes. A single active site processes both recessed ends and 5'-flap substrates. By initiating enzyme reactions in crystals, we have trapped hExo1 reaction intermediates that reveal structures of these substrates before and after their exo- and endonucleolytic cleavage, as well as structures of uncleaved, unthreaded, and partially threaded 5' flaps. Their distinctive 5' ends are accommodated by a small, mobile arch in the active site that binds recessed ends at its base and threads 5' flaps through a narrow aperture within its interior. A sequence of successive, interlocking conformational changes guides the two substrate types into a shared reaction mechanism that catalyzes their cleavage by an elaborated variant of the two-metal, in-line hydrolysis mechanism. Coupling of substrate-dependent arch motions to transition-state stabilization suppresses inappropriate or premature cleavage, enhancing processing fidelity. Furthermore, the striking reduction in flap conformational entropy is catalyzed, in part, by arch motions and transient binding interactions between the flap and unprocessed DNA strand. At the end of the observed reaction sequence, hExo1 resets without relinquishing DNA binding, suggesting a structural basis for its processivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Processing the Interspecies Quorum-sensing Signal Autoinducer-2 (AI-2)

The molecule (S)-4,5-dihydroxy-2,3-pentanedione (DPD) is produced by many different species of bacteria and is the precursor of the signal molecule autoinducer-2 (AI-2). AI-2 mediates interspecies communication and facilitates regulation of bacterial behaviors such as biofilm formation and virulence. A variety of bacterial species have the ability to sequester and process the AI-2 present in their environment, thereby interfering with the cell-cell communication of other bacteria. This process involves the AI-2-regulated lsr operon, comprised of the Lsr transport system that facilitates uptake of the signal, a kinase that phosphorylates the signal to phospho-DPD (P-DPD), and enzymes (like LsrG) that are responsible for processing the phosphorylated signal. Because P-DPD is the intracellular inducer of the lsr operon, enzymes involved in P-DPD processing impact the levels of Lsr expression. Here we show that LsrG catalyzes isomerization of P-DPD into 3,4,4-trihydroxy-2-pentanone-5-phosphate. We present the crystal structure of LsrG, identify potential catalytic residues, and determine which of these residues affects P-DPD processing in vivo and in vitro. We also show that an lsrG deletion mutant accumulates at least 10 times more P-DPD than wild type cells. Consistent with this result, we find that the lsrG mutant has increased expression of the lsr operon and an altered profile of AI-2 accumulation and removal. Understanding of the biochemical mechanisms employed by bacteria to quench signaling of other species can be of great utility in the development of therapies to control bacterial behavior.

59 BASIC BIOLOGICAL SCIENCES↗