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At least 703 records · Page 39
All sourcesNASA NTRSDOE OSTI
NASA NTRS2012

Damage Tolerance Assessment of Friction Pull Plug Welds

Friction stir welding is a solid state welding process developed and patented by The Welding Institute in Cambridge, England. Friction stir welding has been implemented in the aerospace industry in the fabrication of longitudinal welds in pressurized cryogenic propellant tanks. As the industry looks to implement friction stir welding in circumferential welds in pressurized cryogenic propellant tanks, techniques to close out the termination hole associated with retracting the pin tool are being evaluated. Friction pull plug welding is under development as a one means of closing out the termination hole. A friction pull plug weld placed in a friction stir weld results in a non-homogenous weld joint where the initial weld, plug weld, their respective heat affected zones and the base metal all interact. The welded joint is a composite, plastically deformed material system with a complex residual stress field. In order to address damage tolerance concerns associated with friction plug welds in safety critical structures, such as propellant tanks, nondestructive inspection and proof testing may be required to screen hardware for mission critical defects. The efficacy of the nondestructive evaluation or the proof test is based on an assessment of the critical flaw size in the test or service environments. Test data relating residual strength capability to flaw size in two aluminum alloy friction plug weld configurations is presented.

McGill, Preston↗
NASA NTRS2014

Manufacturing Challenges Associated with the Use of Metal Matrix Composites in Aerospace Structures

Metal Matrix Composites (MMCs) consist of a metal alloy reinforced with ceramic particles or fibers. These materials possess a very high strength to weight ratio, good resistance to impact and wear, and a number of other properties which make them attractive for use in aerospace and defense applications. MMCs have found use in the space shuttle orbiter's structural tubing, the Hubble Space Telescope's antenna mast, control surfaces and propulsion systems for aircraft, and tank armors. The size of MMC components is severely limited by difficulties encountered in joining these materials using fusion welding. Melting of the material results in formation of an undesirable phase (formed when molten Aluminum reacts with the reinforcement) which leaves a strength depleted region along the joint line. Friction Stir Welding (FSW) is a relatively nascent solid state joining technique developed at The Welding Institute (TWI) in 1991. The process was first used at NASA to weld the super lightweight external tank for the Space Shuttle. Today FSW is used to join structural components of the Delta IV, Atlas V, and Falcon IX rockets as well as NASA's Orion Crew Exploration Vehicle and Space Launch System. A current focus of FSW research is to extend the process to new materials, such as MMCs, which are difficult to weld using conventional fusion techniques. Since Friction Stir Welding occurs below the melting point of the workpiece material, this deleterious phase is absent in FSW-ed MMC joints. FSW of MMCs is, however, plagued by rapid wear of the welding tool, a consequence of the large discrepancy in hardness between the steel tool and the reinforcement material. This chapter summarizes the challenges encountered when joining MMCs to themselves or to other materials in structures. Specific attention is paid to the influence of process variables in Friction Stir Welding on the wear process characterizes the effect of process parameters (spindle speed, traverse rate, and length of joint) on the wear process. A phenomenological model of the wear process was constructed based on the rotating plug model of Friction Stir Welding. The effectiveness of harder tool materials (such as Tungsten Carbide, high speed steel, and tools with diamond coatings) to combat abrasive wear is also explored. In-process force, torque, and vibration signals are analyzed to assess the feasibility of in situ monitoring of tool shape changes as a result of wear (an advancement which would eliminate the need for off-line evaluation of tool condition during joining). Monitoring, controlling, and reducing tool wear in FSW of MMCs is essential to implementation of these materials in structures (such as launch vehicles) where they would be of maximum benefit. The work presented here is extendable to machining of MMCs, where wear of the tool is also a limiting factor.

Prater, Tracie↗
DOE OSTI2024

Computational analysis of flame initiation, quenching, and re-ignition in a prechamber natural gas engine under varying EGR-dilution levels

The on-road natural-gas (NG) fueled transportation relies on stoichiometric spark-ignition engines for the advantages of simple after-treatment system despite the efficiency penalty relative to lean-burn combustion strategies. Exhaust gas recirculation (EGR) has the potential to reduce this efficiency gap at low to moderate loads without the need for complex lean-exhaust aftertreatment systems. However, EGR dilution leads to reduced combustion stability and increased cycle-to-cycle variability. A promising technology that has the potential to achieve reliable operation under diluted conditions is the prechamber ignition (or turbulent jet ignition) which uses chemically active turbulent jets generated from combustion inside a prechamber to initiate, stabilize and accelerate combustion of the mixture inside the main chamber. The present work focusses on developing a RANS-based CFD approach to accurately reproduce in-cylinder phenomena in a stoichiometric NG prechamber-assisted heavy-duty engine without relying on complex combustion models that account for turbulence-chemistry interactions. This is necessary because reactive prechamber jets at high EGR dilution tend to extinguish while emerging into the main chamber, which is followed by a phase of re-ignition — a phenomenon that conventional G-equation or well-stirred reactor combustion models cannot reproduce. With addition of a damping multiplier to the well-stirred reactor model, the predictions are seen to show good agreement with experimental pressure evolution and combustion images acquired from a single cylinder Cummins N-14 optical diesel engine retrofitted with a prechamber ignition system. Model predictions of local heat release in the flame and temperature evolution inside the flame are used to investigate combustion dynamics in the prechamber and the main chamber. It is seen that the well-stirred reactor model with the inclusion of damping is able to reproduce the temporary reduction in heat release within the flame, which can be considered equivalent to quenching of jets, and the subsequent re-ignition of the flame inside the main chamber. The delay between quenching and re-ignition depends on the amount of dilution, as explained by an illustration of flame evolution in a Borghi diagram.

Prechamber ignition↗
DOE OSTI2023

An innovative and alternative approach toward gear fabrication

In this paper, we present the first demonstration of single-step gear manufacturing via an innovative in-situ friction stir forging approach. This novel process is a natural extension to the friction stir processing technique and relies on shear and normal stresses to form the complex shapes. Friction stir welding pin tool with shoulder is plunged at high revolutions per minute (rpm) into the sample to heat it to the desired temperature and enable plastic flow. Then, the tool is forged at high plunge rate to form the desired structurally-sound and defect free complex shapes. To better visualize the process the experiments are complemented by a 3D thermomechanically coupled, smoothed particle hydrodynamics (SPH) model to understand the material flow pattern both radially and through thickness in the gear teeth, plastic strain distribution, and temperature profile. We have demonstrated application of I-FSF to inherently poor formable AZ31 Mg, AA 7075-T6, and AA5083–10 vol% TiB 2 composite and fabricated 14-tooth spur gears from these materials with minimal farther machining. In conclusion, microstructure of the forged gears exhibited a directional material flow pattern due to the normal forging action and refinement of grains to 6–13 μm through dynamically recrystallization across the radial, through-thickness direction, which is in good agreement with the corresponding SPH simulation results.

42 ENGINEERING↗
DOE OSTI2018

One-pot fabrication and characterization of graphene/PMMA composite flexible films

Highlights: • Investigated the fabrication and characterization of conducting flexible films based on graphene/PMMA polymer composite. • Graphene/PMMA flexible films were fabricated by one-pot alternate stirring sonication (OPASS) process. • Electrical response of the fabricated flexible films were studied and exhibited an electrical conductivity of 44.92 S/m and 0.10 S/m with 50 wt% and 10 wt% concentrations, respectively. • Reinforcing polymers with graphite platelets will amend their surface toughness, modulus and barrier properties, suitable for commercial applications. - Abstract: The present work investigates fabrication and characterization of graphene/ poly (methyl methacrylate) (PMMA) composite flexible films. Graphene/PMMA flexible films were fabricated by one-pot alternate stirring sonication (OPASS) process. The method relies on the alternate high speed stirring and ultrasonication of graphite and its blending with PMMA without any sufactant assistance. A comparative study of the nanocomposite solution was carried out with the composite solution prepared by conventional (CL) method. The transformation of micro-sized graphite particles to nano-sized layers of graphite or few layer graphene was characterized by various analytical techniques. The electrical response of the fabricated flexible films were studied and exhibited an electrical conductivity of 44.92 S/m and 0.10 S/m with 50 wt% and 10 wt% concentrations, respectively. Thus, the fabricated flexible films could have excellent surface toughness, modulus and barrier properties, which make them a suitable candidate for commercial flexible electronic and wearable sensor applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2014

After runaway: The trans-Hill stage of planetesimal growth

When planetesimals begin to grow by coagulation, they first enter an epoch of runaway, during which the biggest bodies grow faster than all the others. The questions of how runaway ends and what comes next have not been answered satisfactorily. We show that runaway is followed by a new stage—the 'trans-Hill stage'—that commences when the bodies that dominate viscous stirring ('big bodies') become trans-Hill, i.e., when their Hill velocity matches the random speed of the small bodies they accrete. Subsequently, the small bodies' random speed grows in lockstep with the big bodies' sizes, such that the system remains in the trans-Hill state. Trans-Hill growth is crucial for determining the efficiency of growing big bodies, as well as their growth timescale and size spectrum. Trans-Hill growth has two sub-stages. In the earlier one, which occurs while the stirring bodies remain sufficiently small, the evolution is collisionless, i.e., collisional cooling among all bodies is irrelevant. The efficiency of forming big bodies in this collisionless sub-stage is very low, ∼10α << 1, where α ∼ 0.005(a/AU){sup –1} is the ratio between the physical size of a body and its Hill radius. Furthermore, the size spectrum is flat (equal mass per size decade, i.e., q = 4). This collisionless trans-Hill solution explains results from previous coagulation simulations for both the Kuiper Belt and the asteroid belt. The second trans-Hill sub-stage commences once the stirring bodies grow big enough (>α{sup –1} × the size of the accreted small bodies). After that time, collisional cooling among small bodies controls the evolution. The efficiency of forming big bodies rises and the size spectrum becomes more top heavy. Trans-Hill growth can terminate in one of two ways, depending on the sizes of the small bodies. First, mutual accretion of big bodies can become significant and conglomeration proceeds until half of the total mass is converted into big bodies. This mode of growth may explain the observed size distributions of small bodies in the solar system and is explored in our subsequent work. Second, if the big bodies' orbits become separated by their Hill radius, oligarchy commences. This mode likely precedes the formation of fully fledged planets.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2012

Modeling analysis for grout hopper waste tank

The Saltstone facility at Savannah River Site (SRS) has a grout hopper tank to provide agitator stirring of the Saltstone feed materials. The tank has about 300 gallon capacity to provide a larger working volume for the grout nuclear waste slurry to be held in case of a process upset, and it is equipped with a mechanical agitator, which is intended to keep the grout in motion and agitated so that it won't start to set up. The primary objective of the work was to evaluate the flow performance for mechanical agitators to keep an adequate stirring of the feed materials and to estimate an agitator speed which provides acceptable flow performance with a 45 deg. pitched four-blade agitator. In addition, the power consumption required for the agitator operation was estimated. The modeling calculations were performed by taking two steps of the Computational Fluid Dynamics (CFD) modeling approach. A series of sensitivity calculations for different designs of agitators and operating conditions have been performed to investigate the impact of key parameters on the grout hydraulic performance in a 300-gallon hopper tank. Recommended operational guidance was developed by using the basic concept that local shear rates and flow patterns can be used as a measure of hydraulic performance and spatial stirring. Flow patterns and fluid residence time were estimated by a Lagrangian integration technique along the flow paths from the material feed inlet. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

FSW of Aluminum Tailor Welded Blanks across Machine Platforms

Development and characterization of friction stir welded aluminum tailor welded blanks was successfully carried out on three separate machine platforms. Each was a commercially available, gantry style, multi-axis machine designed specifically for friction stir welding. Weld parameters were developed to support high volume production of dissimilar thickness aluminum tailor welded blanks at speeds of 3 m/min and greater. Parameters originally developed on an ultra-high stiffness servo driven machine where first transferred to a high stiffness servo-hydraulic friction stir welding machine, and subsequently transferred to a purpose built machine designed to accommodate thin sheet aluminum welding. The inherent beam stiffness, bearing compliance, and control system for each machine were distinctly unique, which posed specific challenges in transferring welding parameters across machine platforms. This work documents the challenges imposed by successfully transferring weld parameters from machine to machine, produced from different manufacturers and with unique control systems and interfaces.

aluminum↗
DOE OSTI2011

Detection of biological uranium reduction using magnetic resonance

The conversion of soluble uranyl ions (UOurn:x-wiley:00063592:media:BIT24369:tex2gif-stack-1) by bacterial reduction to sparingly soluble uraninite (UO2(s)) is being studied as a way of immobilizing subsurface uranium contamination. Under anaerobic conditions, several known types of bacteria including iron and sulfate reducing bacteria have been shown to reduce U (VI) to U (IV). Experiments using a suspension of uraninite (UO2(s)) particles produced by Shewanella putrefaciens CN32 bacteria show a dependence of both longitudinal (T1) and transverse (T2) magnetic resonance (MR) relaxation times on the oxidation state and solubility of the uranium. Gradient echo and spin echo MR images were compared to quantify the effect caused by the magnetic field fluctuations (equation image) of the uraninite particles and soluble uranyl ions. Since the precipitate studied was suspended in liquid water, the effects of concentration and particle aggregation were explored. A suspension of uraninite particles was injected into a polysaccharide gel, which simulates the precipitation environment of uraninite in the extracellular biofilm matrix. A reduction in the T2 of the gel surrounding the particles was observed. Tests done in situ using three bioreactors under different mixing conditions, continuously stirred, intermittently stirred, and not stirred, showed a quantifiable T2 magnetic relaxation effect over the extent of the reaction.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2019

A Perspective on Solid-State Additive Manufacturing of Aluminum Matrix Composites Using MELD

MELD, previously known as additive friction stir, is an emerging solid-state process that enables additive manufacturing of a broad range of metals and metal matrix composites. Here, we discuss its potential for fabricating aluminum matrix composites by showing examples of Al-SiC, Al 6061-Mo, and Al 6061-W composites. Thanks to its solid-state nature, MELD is uniquely suited for the use of high-strength aluminum alloys as matrix material, which would suffer from hot cracking problems in liquid-state processes. Using complementary characterization tools, we show that this process results in aluminum matrix composites with no observed porosity and homogeneous particle distribution. These properties stem from the extensive material flow and mixing during the deposition process. In addition to the high quality of produced composites, its ease of use, versatility of feed materials, and scalability all make MELD an attractive tool for additive manufacturing of aluminum matrix composites. We also discuss the limitations of MELD for composite fabrication, with issues related to maximum reinforcement loading, tool wear, and in-plane resolution. Finally, we compare the benefits and limitations of MELD with other composite fabrication processes such as powder bed fusion, friction stir processing, stir casting, and powder processing.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influence of Rotation Rate on Microstructure and Comprehensive Performance of FSWed Mg Alloy

Die-casting AZ31 Mg alloys were successfully friction stir welded at a constant welding speed and different rotation rates. More uniform and fine grains were obtained at the rotation rate of 1400 rpm due to more suitable temperature for dynamic recrystallization in this welding condition. In addition, the intensity of (0001) texture in stir zone increased with the increasing rotation rate. The results of mechanical property test indicated joint with rotation rate of 1400 rpm had better tensile property, which was associated with fine grains, uniform transition in the interface between thermo-mechanically affected zone and stir zone as well as more favorable Schmidt factor for basal slip and twinning. The corrosion resistance of joints increased with the increasing rotation rate, which is significantly related to the (0001) texture with basal plane parallel to the corroded surfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Crafting Multifunctional Materials with Tailored Mechanical and Magnetic Properties by Solid-State Non-equilibrium Processing

Aluminum matrix composites hold promise for creating lightweight structural components with multifunctional properties. Nonetheless, achieving desired magnetic or electrical characteristics without compromising their fundamental mechanical properties presents a significant challenge. Here, in this study, we explore mechanical stir-based extrusion as a solid-state metalworking technique to develop fine-grained microstructures and highly refined metallic composites. Our study focuses on creating a SmCo 5 -reinforced aluminum matrix composite using solid stir extrusion (SSE) and assessing its microstructure, mechanical, and magnetic properties through a comprehensive suite of characterization tools, including x-ray diffraction, electron microscopy, and magnetometry. Our findings reveal that incorporating a small amount (3.76 wt.%) of SmCo 5 phase in a non-heat-treatable, non-magnetic aluminum alloy via SSE yields a composite that exhibits good hard magnetic characteristics with a large coercivity (H ci = 13.5 kOe) and improved mechanical properties. This study underscores non-equilibrium processing via solid-state high-speed stirring as a compelling method for crafting multifunctional materials with tailored mechanical and magnetic properties.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Assessment of acute myocarditis by cardiac magnetic resonance imaging: Comparison of qualitative and quantitative analysis methods

Background: To compare cardiac magnetic resonance (CMR) qualitative and quantitative analysis methods for the noninvasive assessment of myocardial inflammation in patients with suspected acute myocarditis (AM). Methods: A total of 61 patients with suspected AM underwent coronary angiography and CMR. Qualitative analysis was performed applying Lake-Louise Criteria (LLC), followed by quantitative analysis based on the evaluation of edema ratio (ER) and global relative enhancement (RE). Diagnostic performance was assessed for each method by measuring the area under the curves (AUC) of the receiver operating characteristic analyses. The final diagnosis of AM was based on symptoms and signs suggestive of cardiac disease, evidence of myocardial injury as defined by electrocardiogram changes, elevated troponin I, exclusion of coronary artery disease by coronary angiography, and clinical and echocardiographic follow-up at 3 months after admission to the chest pain unit. Results: In all patients, coronary angiography did not show significant coronary artery stenosis. Troponin I levels and creatine kinase were higher in patients with AM compared to those without (both P < .001). There were no significant differences among LLC, T2-weighted short inversion time inversion recovery (STIR) sequences, early (EGE), and late (LGE) gadolinium-enhancement sequences for diagnosis of AM. The AUC for qualitative (T2-weighted STIR 0.92, EGE 0.87 and LGE 0.88) and quantitative (ER 0.89 and global RE 0.80) analyses were also similar. Conclusions: Qualitative and quantitative CMR analysis methods show similar diagnostic accuracy for the diagnosis of AM. These findings suggest that a simplified approach using a shortened CMR protocol including only T2-weighted STIR sequences might be useful to rule out AM in patients with acute coronary syndrome and normal coronary angiography.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2017

Influence of surface morphology and UFG on damping and mechanical properties of composite reinforced with spinel MgAl{sub 2}O{sub 4}-SiC core-shell microcomposites

Interface between ceramic particulate and matrix is known to control the response of the materials and functionality of the composite. Among numerous physical properties, grain structure of the materials has also played a significant role in defining the behaviour of metal matrix composites. Usually, silicon carbide (SiC) particles show poor interfacial wettability in aluminium melt. Herein, we were successfully synthesized magnesium oxide (MgO) and nanocrystalline magnesium aluminate (MgAl{sub 2}O{sub 4}) spinel coated silicon carbide (SiC) core-shell micro-composites through sol-gel technique to improve the wettability of dispersoids. Core-shell structures of submicron size were thoroughly investigated by various characterization techniques. Further, aluminium matrix composites incorporated with pristine SiC, MgO grafted SiC and MgAl{sub 2}O{sub 4} grafted SiC particles were fabricated by stir casting technique, respectively. Additionally, as-cast composites were processed via friction stir processing (FSP) technique to observe the influence of grain refinement on mechanical and damping properties. Electron back scattered diffraction (EBSD), Field emission scanning electron microscopy (FE-SEM) and X-ray energy dispersion spectroscopy (EDX) analysis were conducted for investigating grain size refinement, adequate dispersion, stability and de-agglomeration of encapsulated SiC particles in aluminium matrix. The mechanical as well as thermal cyclic (from − 100 to 400 °C) damping performance of the as-cast and friction stir processed composites were studied, respectively. Finally, the enhanced properties were attributable to reduced agglomeration, stabilization and proper dispersion of the tailored SiC particles Al matrix. - Highlights: •Synthesizing a novel coating layer of MgO and MgAl{sub 2}O{sub 4} spinel onto SiC particles •Significant improvement in UTS and hardness by reinforcing tailored SiC in Al •Significant grain refinements were obtained through FSP •SiC/MgAl{sub 2}O{sub 4}/Al exhibits ~ 61% higher storage modulus as compare to pure Al after FSP.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Evaluation of Zn-rich coatings for IMC reaction control in aluminum-magnesium dissimilar welds

Highlights: • Thermodynamic and diffusion simulations have estimated the Zn conc. required to change the IMC reaction in Al-Mg dissimilar welding. • The selected coating alloy was effective in changing the Al-Mg reaction path by forming τ-(Al,Zn){sub 49}Mg{sub 32} as a substitute for β-Al{sub 3}Mg{sub 2}. • Refill™ friction stir spot welds produced with the coating alloy exhibited a thinner reaction layer and an increase in lap shear strength. - Abstract: The dissimilar welding of Al to Mg is very challenging owing to the rapid formation of an intermetallic (IMC) reaction layer at the joint interface, typically comprised of the binary phases γ-Al{sub 12}Mg{sub 17} and β-Al{sub 3}Mg{sub 2}. A potential metallurgical solution has been explored that aimed to change the reaction path by using Al-Zn alloy coatings to promote alternative IMCs with a slower growth rate. To determine the optimum composition for the coating, combined CALPHAD thermodynamic calculations and diffusion simulations were used to estimate the minimum Zn concentration (20 at.%) required to suppress the formation of the faster growing Al{sub 3}Mg{sub 2} phase. This prediction was verified by both static diffusion and Refill™ friction stir spot welding (FSSW) experiments. In each case the selected coating alloy was effective in changing the Al-Mg reaction path by forming the τ-(Al,Zn){sub 49}Mg{sub 32} phase as a substitute for β-Al{sub 3}Mg{sub 2}. However, in static heat treatments there was no reduction in the IMC reaction layer thickness due to the new phase having similar growth kinetics to the β-Al{sub 3}Mg{sub 2} phase it replaced. Nevertheless, Refill™ friction stir spot welds prepared with the new AL-Zn coating alloy exhibited a thinner reaction layer and an increase in lap shear strength. This benefit was attributed to the Zn addition reducing the joint interface liquation temperature, which resulted in a lower peak weld temperature and less IMC reaction; although an increase in local eutectic melting limited the improvement observed.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Particle dynamics of nanoplastics suspended in water with soil microparticles: insights from small angle neutron scattering (SANS) and ultra-SANS

Small-angle neutron scattering (SANS) and ultra-SANS (USANS) were employed to understand the aggregation behavior and observe the size reduction for nanoplastics (NPs) formed from a biodegradable mulch film, and microparticles of vermiculite (V), an artificial soil, suspended in water in the presence of low convective shear (ex situ stirring) prior to measurements. Neutron contrast matching was employed to minimize the signal of V (by 100-fold) and thereby isolate the signal due to NPs in the neutron beam, as the contrast match point (CMP) for V (67 vol% deuteration of water) differed from that of NPs by more than 20%. The original NPs' size distribution was bimodal: <200 nm and 500–1200 nm, referred to as small and large NPs, i.e., SNPs and LNPs, respectively. In the absence of V, SNPs formed homoaggregates at higher concentrations that decreased with stirring time, while the size of LNPs remained unchanged. The presence of V at 2-fold lower concentration than NPs did not change the size of SNPs but reduced the size of LNPs by nearly 2-fold as stirring time increased. Because the size of SNPs and LNPs did not differ substantially between CMP and 100% D 2 O solvents, it is evident that SNPs and LNPs are mainly composed of NPs and not V. In conclusion, the results suggest that LNPs are susceptible to size reduction through collisions with soil microparticles via convection, yielding SNPs near soil–water interfaces within vadose zones.

Nanoplastics↗
DOE OSTI2014

Effect of the chemical treatments on the characteristics of natural cellulose

In order to characterize the morphology and size distribution of the cellulose fibers, natural cellulose from kenaf bast fibers was extracted using two chemical treatments; (1) alkali-bleaching-ultrasonic treatment and (2) alkali-bleaching-hydrolysis. Solutions of NaOH, H{sub 2}O{sub 2} and H{sub 2}SO{sub 4} were used for alkalization, bleaching and hydrolysis, respectively. The hydrolyzed fibers were centrifuged at a rotation speed of 10000 rpm for 10 min to separate the nanofibers from the microfibers. The separation was repeated in 7 steps by controlling pH of the solution in each step until neutrality was reached. Fourier transform infrared (FTIR) spectroscopy was performed on the fibers at the final step of each treatment: i.e. either ultrasonic treated- or hydrolyzed microfibers. Their FTIR spectra were compared with FTIR spectrum of a reference commercial α-cellulose. Changes in morphology and size distribution of the treated fibers were examined by scanning electron microscopy (SEM). FTIR spectra of ultrasonic treated- and hydrolyzed microfibers nearly coincided with the FTIR spectrum of commercial α-cellulose, suggesting successful extraction of cellulose. Ultrasonic treatment for 6 h resulted in a specific morphology in which cellulose nanofibers (≥100 nm) were distributed across the entire surface of cellulose microfibers (∼5 μm). Constant magnetic stirring combined with acid hydrolysis resulted in an inhomogeneous size distribution of both cellulose rods (500 nm-3 μm length, 100–200 nm diameter) and particles 100–200 nm in size. Changes in morphology of the cellulose fibers depended upon the stirring time; longer stirring time resulted in shorter fiber lengths.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

The effect of impeller type on silica sol formation in laboratory scale agitated tank

The multiphase polymerization reaction of the silica sol formation produced from silicic acid and potassium hydroxide solutions in laboratory scale agitated tank was studied. The reactor is equipped with four segmental baffle and top entering impeller. The inside diameter of reactor is 9 cm, the baffle width is 0.9 cm, and the impeller position is 3 cm from tank bottom. The diameter of standard six blades Rushton and three blades marine propeller impellers are 5 cm. The silicic acid solution was made from 0.2 volume fraction of water glass (sodium silicate) solution in which the sodium ion was exchanged by hydrogen ion from cation resin. The reactor initially filled with 286 ml silicic acid solution was operated in semi batch mode and the temperature was kept constant in 60 °C. The 3 ml/minute of 1 M potassium hydroxide solution was added into stirred tank and the solution was stirred. The impeller rotational speed was varied from 100 until 700 rpm. This titration was stopped if the solution in stirred tank had reached the pH of 10-The morphology of the silica particles in the silica sol product was analyzed by Scanning Electron Microscope (SEM). The size of silica particles in silica sol was measured based on the SEM image. The silica particle obtained in this research was amorphous particle and the shape was roughly cylinder. The flow field generated by different impeller gave significant effect on particle size and shape. The smallest geometric mean of length and diameter of particle (4.92 µm and 2.42 µm, respectively) was generated in reactor with marine propeller at 600 rpm. The reactor with Rushton impeller produced particle which the geometric mean of length and diameter of particle was 4.85 µm and 2.36 µm, respectively, at 150 rpm.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗