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L0087 - Improving the performance of lead-free solder reinforced with multi-walled carbon nanotubes

In this study, varying weight fractions of multi-walled carbon nanotubes were successfully incorporated into 95.8Sn-3.5Ag-0.7Cu solder, to synthesize novel lead-free composite solders. The composite solders were synthesized via the powder metallurgy route of: blending, compaction, sintering and extrusion. The extruded materials were then characterized for their physical, thermal and mechanical properties. With the addition of increasing weight percentage of carbon nanotubes, the composite solders experienced a corresponding decrease in density values and wetting property improved. The melting temperatures of the composite solders were found to be unchanged with the carbon nanotube additions. Thermomechanical analysis of the composites also showed that the presence of reinforcements decreased the average coefficient of thermal expansion of the solder matrix. An improvement in the mechanical properties was also recorded with the presence of increasing carbon nanotubes. An attempt was made, to correlate the increasing presence of reinforcements with the physical, thermal and mechanical properties obtained.


S.M.L. Nai, J. Wei, M. Gupta, Materials Science and Engineering A 423 (2006) 166-169

L0086 - Evidence of the formation of a new rock-salt type compound Li2MgTiO4 and of its role on the properties of the Li doped MgTiO3

This work deals with the sintering of MgTiO3 in presence of Lithium salt and more precisely with lithium halide. These last sintering agents lead to the formation of a new rock-salt type structure Li2MgTiO4. This new phase was synthesized by a classical solid-state route and their electric and dielectric properties were characterize. The formed material is a type I dielectric material with a permittivity close to 12 with dielectric losses inferiors to 0.3% in the range of -50 to 150°C. X-ray diffraction and investigation by TEM were also performed. The influences of the formation of this new phase on the properties of MgTiO3 are described here.


J. Bernard, D. Houivet, M. Hervieu, J.M. Haussonne, Solid State Sciences 8 (2006) 598-605

L0085 - Thermal expansion of near stoichiometric (U,Er)O2 solid solutions

Thermal expansions of (U,Er)O2 solid solutions were investigated between room temperature and 1673 K by using a thermo-mechanical analyzer. Lattice parameters of the (U,Er)O2 pellets are lower than that of UO2 and they decrease as the Er contents increase. The linear thermal expansion and average thermal expansion coefficients of (U,Er)O2 are higher than that of UO2. For the temperature range from room temperature to 1673 K, the average thermal expansion coefficient values for UO2 and (U0.8Er0.2)O2 are 10.94x10^(-6) and 11.42x10^(-6) K-1, respectively.


S-H. Kim, H-S. Kim, Y-W. Lee, D-S. Sohn, D-S. Suhr, Materials Letters 60 (2006) 1480-1483

L0084 - Development of a novel hybrid aluminum-based composite with enhanced properties

In the present study, a novel aluminum-based hybrid composite containing titanium particulates (discontinuous/particulates reinforcement) and iron mesh (continuous/interconnected reinforcement)was synthesized using a solidification processing route involving disintegrated melt deposition coupled with hot extrusion. Microstructural characterization studies conducted on hybrid composite revealed reduced grain size (~44%) when compared to monolithic aluminum, uniform distribution of unreacted and reacted titanium in matrix, and absence of reaction products at the iron-wire/aluminum matrix interface. Results of properties characterization revealed that the presence of hybrid reinforcement led to a reduction in coefficient of thermal expansion (~7.6%) and an increase in hardness, elastic modulus (~10%), 0.2% yield strength (20%) and ultimate tensile strength (~27%). The enhancement in properties realized in hybrid composite was found to be much higher when compared to conventional Al/SiC composite formulations containing relatively higher weight percentages of SiC particulates.


M. Gupta, M.O. Lai, C.Y.H. Lim, Journal of Materials Processing Technology 176 (2006) 191-199

L0082 - Fabrication of gapless triangular micro-lens array

This study presents a new process to fabricate gapless triangular micro-lens array (GTMA) optical film. The process includes ultraviolet (UV) lithography, photoresist reflow process, Ni-Co electroplating and hot embossing technique. After photoresist triangular column array is defined by UV lithography, reflow technique is applied to melt photoresist triangular column array into the shape of triangular micro-lens array. With this reflowed triangular micro-lens array, metal Ni-Co is deposited and covered uniformly on the triangular micro-lens array using electroplating process. The growth rate of Ni-Co is controlled at 0.4-0.6 µm/min at electroplating current density of 1 A/dm2 (ampere square decimetre, ASD). After this electroplating process, a mold of GTMA is obtained, which is served as the primary mold. Next, with passivation technique applied on this primary mold's surface, a secondary mold is obtained by applying the electroplating process again. This secondary mold is served as master for the subsequent hot embossing process to replicate the GTMA pattern onto polymeric material of polymethyl methacrylate (PMMA) sheet. The Ni-Co mold with hardness over hardness of vicker (Hv) 650 is obtained. The stiffness and hardness of the mold play important roles in GTMA hot embossing process. In addition, this PMMA-based GTMA film used as optical film offers a 100% fill factor and high optical coupling efficiency to improve luminance. The optical measurement shows that this optical film with GTMA pattern increases 15.1% of luminance for backlight module (BLM) of liquid crystal display (LCD).


C.T. Pan, C.H. Su, Sensors and Actuators A Physical 134 (2007) 631-640

L0081 - The rock salt oxide Li2MgTiO4: Type I dielectric and ionic conductor

The exploration of the Li-Ti-Mg-O system, using both sol-gel technique and solid state reaction method, allowed a new phase, Li2MgTiO4, with disordered rock salt structure (a = 4.159 Å ) to be synthesized. The latter is shown to be a good type I dielectric material, with a relative constant of 15 at high frequency and low dielectric loss (tand < 10^(-3)) over the temperature range - 60 to 160°C. It is also observed that the sintering temperature of this phase is strongly lowered by adopting the sol-gel technique compared to solid state reaction (1150°C instead of 1300°C). Finally we show that this phase exhibits cationic conductivity above 400°C (s600°C = 9 x 10^(-5) S cm-1).


M.V.V.M. Satya Kishore, S. Marinel, V. Pralong, V. Caignaert, S. D'Astorg, B. Raveau, Materials Research Bulletin 41 (2006) 1378-1384

L0080 - A novel low temperature sintering process for PMnN-PZT ceramics

Samples with the composition of 0.07Pb(Mn1/3Nb2/3)O3-0.468PbZrO3-0.462PbTiO3 was prepared in this study. A novel process was adapted to lower the sintering temperature without properties deterioration. The sintering process includes a vacuumed heating stage, a air-venting heating stage, and a final sintering at 1050°C with certain holding time without PbO compensating atmosphere. The influence of holding time at the final sintering stage on the characteristics of the ceramics was studied. The air-venting stage caused a large shrinkage (about 10%) and then slowing down the shrinking rate when the sample was heated up from 800 to 1050°C. The relationships between the crystalline characteristics and physical properties, such as microstructure, the mechanical quality factor (Qm), and electromechanical coupling factor (kp), are discussed in this paper.


C-Y. Chen, Y. Hu, H-L. Lin, Materials Chemistry and Physics 99 (2006) 26-29

L0079 - The effects of the physical states of a simulated fission product on the linear thermal expansion of (U0.924Ce0.076)O2

The linear thermal expansions of an (U0.924Ce0.076)O2 pellet, doped a simulated fission product (Nd2O3 or Ru), were measured from room temperature to 1673K in a flowing argon atmosphere using TMA. Nd2O3 and Ru represent the physical states of a fission product, a dissolved oxide and a metallic precipitate, respectively. Using the measured data, the mean coefficients of a linear thermal expansion was obtained as a function of the temperature, and the effects of the physical states of a simulated fission product on the thermal expansion were investigated. In the case of the Nd2O3 forming a dissolved oxide, the thermal expansion of the sample increased and the increment was proportional to the Nd contents, because the melting point of the Nd2O3 was lower than that of UO2 and although the metallic precipitate hardly affected the crystal structure, the linear thermal expansion also increased with an increasing Ru contents.


D-J. Kim, Y-S. Kim, J-H. Yang, S-H. Kim, Y-W. Lee, H-S. Kim, Journal of Alloys and Compounds 421 (2006) 151-155

L0078 - Development of Mg/Cu nanocomposites using microwave assisted rapid sintering

In the present study, magnesium composites containing different amounts of nano-size Cu particulates were successfully synthesized using powder metallurgy (PM) technique incorporating microwave assisted two-directional sintering. The sintered specimens were hot extruded and characterized in terms of physical, microstructural and mechanical properties. Microstructural characterization revealed minimal porosity and the presence of a continuous network of nano-size Cu particulates and Mg2Cu intermetallic phase decorating the particle boundaries of the metal matrix. Coefficient of thermal expansion (CTE) value of magnesium matrix was improved marginally with the addition of nano-size Cu particulates. Mechanical characterization revealed that the addition of nano-size Cu particulates lead to an increase in hardness, elastic modulus, 0.2% yield strength (YS), ultimate tensile strength (UTS) and work of fracture of the matrix. An attempt is made in the present study to correlate the effect of increasing amount of nano-size Cu reinforcement on the microstructure and properties of monolithic magnesium.


W.L.E. Wong, M. Gupta, Composites Science and Technology 67 (2007) 1541-1552

L0076 - Modelling of the grain growth and the densification of SnO2-based ceramics

This work consisted in the kinetic study of grain growth and densification processes for SnO2 and Sn0.94Zr0.06O2 ceramics between 1100 and 1200°C. From dilatometric experiments, it appeared that zirconia additions inhibited the final densification rate. For pure SnO2, the rate limiting step of the densification mechanism would correspond to the grain boundary or volume diffusion. From normal grain growth kinetics, the corresponding limiting step has been identified, i.e. either the surface diffusion in pores or grain boundary diffusion for ZrO2 free-SnO2 and Sn0.94Zr0.06O2, respectively. All of these results permit establishing the corresponding sintering map. For pure SnO2 ceramic, the experimental data have been well restored by modelling.


A. Maître, D. Beyssen, R. Podor, Ceramics International xxx (2007) xxx-xxx

L0075 - Effects of the sintering atmosphere on Nb-based dielectrics

The effects of a forming atmosphere on the stability, the sintering and the dielectric properties of Ba5Nb4O15, BaNb2O6, ZnNb2O6 and Zn3Nb2O8 ceramics were investigated, because of the primary importance of the sintering atmosphere in relation to copper sintering. These Nbbased materials were sintered in air and in Ar/H210%. Zn-containing samples are very sensitive to the reductive atmosphere. ZnO volatilises at 800-850°C and the resulting compound does not exhibit the expected properties. BaNb2O6 and Ba5Nb4O15 are more stable in term of relative weight loss. Nevertheless, the phase analysis reveals a modification of the BaNb2O6 phase, what induces the degradation of the dielectric property stability versus temperature. The properties of Ba5Nb4O15 are not modified by a sintering in reductive atmosphere. A relative permittivity of 38.8, a permittivity temperature coefficient of -150 ppm°C-1 and an insulating resistivity of 10^10.9 V cm were obtained for this latter.


S. d'Astorg, S. Marinel, Ceramics International xxx (2007) xxx-xxx

L0074 - Preparation and properties of dense Ce0.9Gd0.1O(2-d) ceramics for use as electrolytes in IT-SOFCs

Gd-doped ceria solid solutions have been recognized to be leading electrolytes for use in intermediate-temperature fuel cells. In this communication, it reported on the preparation, solubility and densification of Ce0.9Gd0.1O(2-d) ceramics derived from carbonate coprecipitation. The dissolution of Gd2O3 in CeO2 lattice was identified to complete during coprecipitation process by studying lattice parameter against temperature. The calcining temperature was found to have a significant influence on the densification behavior and final sintered density for the carbonatecoprecipitated powder. The samples prepared from the powder calcined at <700°C had an expansion at ~1250 to 1400°C during sintering, and thus lowered sintered density. 800°C was identified to be an optimal calcining temperature for carbonate-coprecipitated powder. The powder calcined at 800°C for 2 h had a mean crystalline size of ~25 nm with nearly spherical shape and narrow particle-size distribution, which had a maximum densification rate at ~1190°C. This temperature (of maximum densification rate) could further be reduced to ~1080°C for the carbonate-coprecipitated powder by adding 0.5 at.% FeO1.5 (atomic ratio). At 1200°C for 5 h, over 98% relative density with an average grain size of ~1.2µm was obtained for the 0.5 at.% Fe-loaded Ce0.9Gd0.1O(2-d) ceramics. Fe loading was also found to have a positive effect on grain boundary conductivity of Ce0.9Gd0.1O(2-d) ceramics. An increase in the grain boundary conduction by over two times was achieved in the present work for the 0.5 at.% Fe-loaded Ce0.9Gd0.1O(2-d) ceramics.


T.S. Zhang, J. Ma, L.H. Luo, S.H. Chan, Journal of Alloys and Compounds 422 (2006) 46-52

L0073 - Abnormal thermal expansion and thermal stability of Ti3Al(1-x)SixC2 solid solutions

Ti3Al(1-x)SixC2 solid solutions exhibited abnormal high coefficients of thermal expansion at temperatures of >940°C during heating, which was ascribed to the precipitation of Si as Ti5Si3. Ti5Si3 phase usually located at the grain boundaries of the solid solutions.


J.X. Chen, Y.C. Zhou and J. Zhang, Scripta Materialia 55 (2006) 675-678

L0072 - Indentation creep behavior of a Zr-based bulk metallic glass

The deformation behavior of a Zr44Ti11Cu10Ni10Be25 bulk metallic glass (LM-1B) was studied in the supercooled liquid region by indentation creep test. Before indentation the glass transition and the crystallization temperatures were determined by calorimeter as 625 and 725 K, respectively. The phases formed during crystallization were identified by X-ray diffraction. The indentation creep experiments were carried out at different temperatures and loads. It was found that the creep can be regarded as Newtonian flow at strain rates between 5x10^(-5) and 5x10^(-4) s-1. The values of the viscosity and the activation energy of deformation were determined in the temperature range of 667-687 K.


D. Fatay, J. Gubicza, J. Lendvai, Journal of Alloys and Compounds 434-435 (2007) 75-78

L0071 - Influence of the synthesis route on sol-gel SiO2-TiO2 (1:1) xerogels and powders

Five different sol-gel routes are used in order to synthesize mixed SiO2-TiO2 materials. Simple mixing of the Ti and Si precursors, prehydrolyzing of TEOS, modification of the Ti alkoxide with acetic acid, isoamyl alcohol and acetylacetone lead to translucent gels with different time of gelation. Different techniques such as TGA, DTA, XRD and IR spectroscopy are used to characterize each material. IR spectroscopy revealed the presence of Si-O-Ti and Si-O-Si bonds for all the xerogels letting suppose a composite microstructure of the gels. Pre-hydrolyzing of TEOS and modification of Ti alkoxide with isoamyl alcohol are the most appropriate routes to retain the anatase phase up to 1100°C.


S. Vives, C. Meunier, Ceramics International xxx (2007) xxx-xxx

L0070 - Proton conduction in ceria-doped Ba2In2O5 nanocrystalline ceramic at low temperature

Sintered pellets of Ce-doped Ba2In2O5 (BIC) were prepared from nanopowders. The electrical conductivities were measured using ac impedance spectroscopy under different atmospheres and temperatures. The electrical conductivity of sintered BIC was found sensitive to environmental humidity when the temperature was below 300°C. However, in the presence of hydrogen, the electrical conductivities were independent of water content in the range of 0-30 vol%. The electrical conductivities of BIC were significantly affected by the presence of hydrogen in a temperature range of 100-300°C. The estimated protonic transference number and the measured open circuit voltage suggested the existence of electronic conduction. The coefficient of thermal expansion of BIC is 11.2x10^(-6) K-1 from 25 to 1250°C.


R. Hui, R. Maric, C. Decès-Petit, E. Styles, W. Qu, X. Zhang, J. Roller, S. Yick, D. Ghosh, K. Sakata, M. Kenji, Journal of Power Sources 161 (2006) 40-46

L0069 - A study on sintering aids for Sm0.2Ce0.8O1.9 electrolyte

In this study, an addition of Co oxide or Cu oxide to Sm0.2Ce0.8O1.9 (SDC) was studied to improve the sinterability of SDC. It has been found that both Co and Cu oxide are very effective as sintering aids, and the SDC sintering temperature can be reduced from 1400°C without aids to below 1000°C with only 1 at.% of either Cu oxide or Co oxide. As compared to the pure SDC, a slight decrease of ionic conductivity was observed in SDC with Cu sintering aid. There is no obvious effect on electrochemical property of SDC with Co sintering aid under 2.5 at.%.


X. Zhang, C. Decès-Petit, S. Yick, M. Robertson, O. Kesler, R. Maric, D. Ghosh, Journal of Power Sources 162 (2006) 480-485

L0068 - Electrical properties of low-density polyethylene/multiwalled carbon nanotube nanocomposites

Low-density polyethylene (LDPE)/multiwalled carbon nanotube (CNT) nanocomposites were prepared via melt compounding. The electrical properties of LDPE/CNT nanocomposites as a function of CNT volume content, frequency and temperature were investigated. The results showed that dielectric constant of LDPE/CNT nanocomposites increases slightly with increasing CNT content up to 1.9 vol.%. Thereafter, the dielectric constant of the nanocomposites increases sharply. The dielectric constant of LDPE/3.6 vol.% CNT nanocomposite is more than two orders of magnitude larger than that of pure LDPE. The frequency dependence of electrical properties of LDPE/3.6 vol.% CNT nanocomposite can be well described by the percolation theory.


G.D. Liang, S.C. Tjong, Materials Chemistry and Physics 100 (2006) 132-137

L0067 - Low temperature sintering of ZnTiO3/TiO2 based dielectric with controlled temperature coefficient

Structure, microstructure and dielectric properties of ZnTiO3 and rutile TiO2 mixtures (ZnTiO3 + xTiO2 with x = 0, 0.02, 0.05, 0.1, 0.15 and 0.2) sintered using ZnO-B2O3 glass phase (5 wt.% added) as sintering aid have been investigated. For all compounds, the sintering temperature achieves 900°C. The X-ray diffraction patterns indicate for x = 0.1 that the material is composed by three phases identified as ZnTiO3 hexagonal, TiO2 rutile and ZnO. The presence of ZnO is explained by the introduction of Ti into Zn site to form the (Zn1-xTix)TiO3+x solid solution in resulting the departure of ZnO from the ZnTiO3 structure. The ZnTiO3 + 0.15TiO2 composition sintered at 900°C with glass addition exhibits attractive dielectrics properties (Er = 23, tan(delta) < 10^(-3) and a temperature coefficient of the dielectric constant near zero (t = 0 ppm/°C)) at 1 MHz. It is also shown that the introduction of TiO2 allows to tune the temperature coefficient of the permittivity. All these properties lead this system compatible to manufacture silver based electrodes multilayer dielectrics devices.


A. Chaouchi, S. Marinel, M. Aliouat, S. d'Astorg, Journal of the European Ceramic Society 27 (2007) 2561-2566

L0066 - Synthesis and sintering of a monazite-brabantite solid solution ceramic for nuclear waste storage

Various geological arguments suggest that monazite can be an interesting waste-form for actinides such as Np, Pu, Cm and Am. We set up a simple procedure for making dense pellets of monazite-brabantite solid-solution ceramics with composition Ca0.092Th0.092 Ce0.089La0.727PO4. It consists of co-milling CaCO3, ThO2, CeO2, La2O3, and NH4H2PO4, 1250°C calcination, milling, cold-pressing, and sintering at 1450°C for 4 h. X-ray investigations showed that the reaction scheme from oxides to monazite is complex and involves various P+La-based intermediate compounds. The final density of the the product is around 95% of the theoretical density. The texture is homogeneous with a typical grain of size 5-20 mm. This process is designed to be adapted to hot cells and telemanipulators.


J-M. Montel, B. Glorieux, A-M. Seydoux-Guillaume, R. Wirth, Journal of Physics and Chemistry of Solids 67 (2006) 2489-2500


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    THERMANS 2012

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    Mumbai, IndiaTHERMANS-2012DAE – BRNSEighteenth International Symposium & Workshop on Thermal AnalysisThe Symposium and Workshop is sponsored by Board of Research in Nuclear Sciences(BRNS), Department of Atomic Energy (DAE) in association with the Indian ThermalAnalysis Society (ITAS). In this Symposium, it is planned to focus on “Thermochemical and Thermophysical Investigations of Materials Relevant to Nuclear Industry and Allied Areas”.Training School HostelHomi Bhabha National Institute, Mumbai, IndiaJanuary 31-February 2, 2012 (Symposium)February 3-4, 2012 (Workshop)
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