Control of Stress Concentration in Surface‐Mounted Multilayer Ceramic Capacitor Subjected to Bending

Failure of surface‐mounted multilayer ceramic capacitor (MLCC) results mainly from bending of the printed circuit board during handling and applications. Cracking of MLCC normally initiates at the junction of the bottom end of termination and the dielectric ceramics and it would cut through dielectric ceramics and electrodes to result in the capacitance loss and failure of MLCC. The purpose of this study was to mitigate the stress concentration and to shift the stress concentration location toward the side end of MLCC to minimize the number of electrodes cut by cracking. To achieve this, effects of the stiffness and the thickness of the solder and the size of MLCC on the location of crack initiation and the fracture load were examined. Nanoindentation was performed to obtain the mechanical properties of the constituents of the system. Finite element analyses were conducted to simulate the stress field in the surface‐mounted MLCC subjected to bending and the results were compared to the observed crack initiation locations and the fracture load. The outcome would provide guidelines in mounting and designing of MLCCs to enhance its reliability and lifetime.     

Barrier effect of flame retardant systems in poly(methyl methacrylate): Study of the efficiency of the surface treatment by octylsilane of silica nanoparticles in combination with phosphorous fire retardant additives

In this work, flame retardant systems comprising ammonium polyphosphate (AP423) and hydrophilic (A200) or hydrophobic (R805) nanometric silica were incorporated into PMMA. The following techniques were performed to detail the fire behaviour of the composites: mass loss cone calorimetry, pyrolysis‐combustion flow calorimetry, pyrolysis‐gas chromatography–mass spectrometry, thermogravimetric analysis, X‐ray diffraction analysis, Fourier transform infrared spectroscopy and microscopic observations. The best fire behaviour was obtained with the surface‐treated silica in the presence of AP423. The formation of a new crystalline phase from the interactions between AP423 and R805 silica and a strong barrier effect due to a layered residue were the main modes of action of this system. Moreover, we have shown that the difference between the AP423 + R805 and AP423 + A200 systems was due to poor dispersion of the silica into the PMMA matrix in the latter formulation. Copyright © 2011 John Wiley & Sons, Ltd.     

A new slurry-based shaping process for fabricating ceramic green part by selective laser scanning the gelled layer

This paper proposes a new slurry-based shaping process for fabricating ceramic green parts. Slurry was composed of SiO₂ powders (without polymer coating) as a structural element, silica sol and polyvinyl alcohol (PVA) as binders. The new process derived gelling effect from vaporization to generate a uniform gelled layer. By selective laser scanning, an alkali-insoluble 2D pattern was formed on the gelled layer. A green part was built by sequentially layer casting, drying, selective scanning and self-supporting removing. Because gelling occurs uniformly in the whole fresh layer, distortion is minimized. Therefore, this process not only can cast thinner layers to improve the staircase effect but also achieve a better surface by preventing surface pitting induced by laser ablation. No additional design for supports is required since overhangs and undercuts are supported by an inherent gelled support. Compared to other slurry-based processes, the process possesses time-efficiency in slurry preparation and support removal.     

Isothermal crystallization behavior of nano-alumina particles-filled poly(ether ether ketone) composites

The isothermal crystallization behavior of nano-alumina particle-filled poly(ether ether ketone) (PEEK) composites has been investigated using differential scanning calorimeter. The results show that all the neat PEEK and nano-alumina-filled PEEK composites exhibit the double-melting behavior under isothermal crystallization. The peak crystallization times (τ_p) for all the neat PEEK and PEEK/aluminum oxide (Al₂O₃) composites increase with increasing crystallization temperature. Moreover, the crystallinity of the PEEK/Al₂O₃ composite with 7.5 wt % nano-filler content reached the maximum value of 44.8% at 290°C, higher than that of the neat PEEK polymer. From the lower value in τ_p and higher value in X_c for the PEEK/Al₂O₃ composites, the inclusion of the nano-alumina into the PEEK matrix favored the occurrence of heterogeneous nucleation. The Avrami exponents n of all the neat PEEK and PEEK/Al₂O₃ composites ranged from 2 to 3, and the n values for PEEK/Al₂O₃ composites were slightly higher than that of the neat PEEK polymer, indicating that the inclusion of the nano-filler made the crystallization mechanism more complex. However, the growth rate of crystallization was lowered as the nano- filler was introduced, and the decrease in growth rate reduced the grain size of the PEEK spherulites because of the lowering of molecule mobility during isothermal crystallization. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Phase evolution and thermal behaviors of the solid-state reaction between SrCO3 and Al2O3 to form SrAl2O4 under air and CO2-air atmospheres

The solid-state reactions between SrCO₃ and Al₂O₃ forming SrAl₂O₄ under air and CO₂-air atmospheres were investigated. The solid-state reaction between SrCO₃ and Al₂O₃ under a CO₂ atmosphere can be separated into multiple reaction stages. The first stage is attributed to the formation of SrAl₂O₄ resulting from the reaction between SrCO₃ and Al₂O₃. The diffusion of Al₂O₃ through the product layer then takes place to continue the reaction. At a higher temperature, the Sr₃Al₂O₆ formation reaction occurs due to the chemical reaction between SrCO₃ and SrAl₂O₄. The SrCO₃ is thermally finally decomposed. The resulting SrO may diffuse rapidly through the product layer, producing pure SrAl₂O₄ formation via a complicated diffusion process at a much higher temperature. These reaction stages occur at very close temperatures under an air atmosphere, leading to a complex reaction between the solids in air.     

Preparation of TiO(2) Nanocrystallite Powders Coated with 9 mol% ZnO for Cosmetic Applications in Sunscreens

The preparation of TiO(2) nanocrystallite powders coated with and without 9 mol% ZnO has been studied for cosmetic applications in sunscreens by a co-precipitation process using TiCl(4) and Zn(NO(3))(2)·6H(2)O as starting materials. XRD results show that the phases of anatase TiO(2) and rutile TiO(2) coexist for precursor powders without added ZnO (T-0Z) and calcined at 523 to 973 K for 2 h. When the T-0Z precursor powders are calcined at 1273 K for 2 h, only the rutile TiO(2) appears. In addition, when the TiO(2) precursor powders contain 9 mol% ZnO (T-9Z) are calcined at 873 to 973 K for 2 h, the crystallized samples are composed of the major phase of rutile TiO(2) and the minor phases of anatase TiO(2) and Zn(2)Ti(3)O(8). The analyses of UV/VIS/NIR spectra reveal that the absorption of the T-9Z precursor powders after being calcined has a red-shift effect in the UV range with increasing calcination temperature. Therefore, the TiO(2) nanocrystallite powders coated with 9 mol% ZnO can be used as the attenuate agent in the UV-A region for cosmetic applications in sunscreens.     

Transesterification of Palm-based Methyl Palmitate into Esteramine Catalyzed by Calcium Oxide Catalyst

The technology for transesterification reactions between methyl esters and alcohols is well established by using classical homogeneous alkaline catalysts, which provide high conversion of methyl esters to specialty or nonindigenous esters. However, in certain products where the purity of the esters is of concern, the removal of homogeneous catalysts after the completion of the reaction is a challenge in terms of production cost and water footprint. Therefore, a study to investigate the potential of heterogeneous catalysts was conducted on reactions between methyl palmitate and triethanolamine. The degree of basicity and active surface area of calcium oxide (CaO), zinc oxide (ZnO), and magnesium oxide (MgO) were first characterized by using temperature-programmed desorption (TPD-CO₂) and Brunauere–Emmett–Teller (BET), respectively. Among the metal oxides investigated, the CaO catalyst showed the best catalytic activity toward the transesterification process as it gave the highest conversion of methyl palmitate and yielded fatty esteramine compositions similar to the conventional homogeneous catalyst. The optimum transesterification condition by using the CaO catalyst utilized a lower vacuum system of approximately 200 mbar, which could minimize a considerable amount of energy consumption. Furthermore, low CaO dosage of 0.1% was able to give a conversion of 94.5% methyl ester and formed esteramine at 170 °C for 2 h. Therefore, the production of esterquats from esteramine may become more economically feasible through the methyl ester route by using the CaO catalyst, which can be recycled three times.     

A GC–MSD method for analysis of dimethyl sulfate in palm oil-based esterquat

Dimethyl sulfate (DMS) is a quarternizing agent for esteramine used for the synthesis of esterquat. To date there is no reliable published method for quantification of DMS in palm-based esterquat. Esterquat is used in the formulation of personal care and textile cleaning. The process of quaternization is usually incomplete and there will be unreacted DMS. This work presents a new simple method involving solvent extraction of DMS followed by analysis with gas chromatography–mass spectrometry detector to quantify the unreacted DMS. This method was validated as per International Council for Harmonization requirements. This novel method showed good repeatability (relative standard deviation [RSD] < 5%) and inter-day with different analyst reproducibility (RSD < 5%). The limits of detection and quantification were 5 and 10 μg mL⁻¹, respectively. The accuracy of the method was evaluated by the analysis of spiked samples and it was found that good recovery was found at spiking levels of 20, 30, and 50 μg mL⁻¹ with % recovery falling within the 80%–120% acceptable limit. However, at 10 μg mL⁻¹, the percentage recovery was slightly below the recommended limit.     

Synthesis and characterization of novel copolymers with the trimethylsilyl group for deep‐UV photoresists

N‐(4‐Acetoxyphenyl) maleimide (APMI) and three kinds of comonomers bearing a trimethylsilyl group were copolymerized at 60°C in the presence of azobisisobutyronitrile (AIBN) as an initiator in 1,4‐dioxane to obtain the three IP, IIP, and IIIP copolymers. These copolymers were removed from the acetoxy group in a transesterification process into new IVP, VP, and VIP copolymers with a pendant hydroxyl group. Two modified processes were adopted to prepare photoresists using these copolymers. The first process involved mixing the dissolution inhibitor, o‐nitrobenzyl cholate, with the new copolymers. Second, o‐nitrobenzyl cholate was introduced into the copolymers using 1,8‐diazabicyclo[5.4.0]undec‐7‐ene (DBU) in dimethylformamide (DMF). The cyclic maleimide structure is responsible for the high thermal stability of these copolymers. After irradiation using deep–UV light and development with aqueous Na₂CO₃ (0.01 wt %), the developed patterns showed positive images and exhibited good adhesion to the silicon wafer without using any adhesion promoter. The resolution of these resists was at least 0.8 μm and an oxygen‐plasma etching rate was 1/5.3 to that of hard‐baked HPR‐204. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 2791–2798, 2002; DOI 10.1002/app.10255     

Standard reference materials for cements

The eight portland cements and two calcium aluminate cements in the Standard Reference Material (SRM) 1880 series are among the most popular SRMs in the catalog of the National Institute of Standards and Technology (NIST) Standard Reference Materials Program. Numerous laboratories rely on them for elemental analysis and qualification for ASTM C 114-00 Standard Test Methods for Chemical Analysis of Hydraulic Cement. NIST has collected new candidate materials from around the world and partnered with Construction Technology Laboratories (CTL) in their preparation and certification. This paper describes the procedures taken at NIST and CTL to prepare and test materials for certification including the homogeneity testing, the X-ray fluorescence methods and the statistical data analysis performed for value assignment.