01625nas a2200241 4500008004100000022001400041245009800055210006900153260006900222300001000291490000700301520079500308653002301103653002501126653001401151653001801165100001901183700001901202700001301221700001501234700001801249856011601267 2005 eng d a0254-058400aSynthesis of fine PbE (E = S, Se) powder from direct in situ reduction of sulphur or selenium0 aSynthesis of fine PbE E S Se powder from direct in situ reductio aPO BOX 564, 1001 LAUSANNE, SWITZERLANDbELSEVIER SCIENCE SAcSEP a91-940 v933 a

Lead sulphide and lead selenide have been prepared for the first time, by in situ reduction of elemental S or Se by using aqueous DMF or aqueous SFS as reducing agents and their reaction with lead acetate. The grayish-black powder has been characterized by powder XRD measurement, XPS and SEM/EDAX analysis. Powder X-ray diffraction pattern revealed that cubic PbE (E = S, Se) is formed with a little impurities of lead in case of PbSe. Slightly broader peaks in XRD measurement suggest small particles diameter in the powder. The particle size by using Scheffer's formula is found to be about 100 nm. Peaks due to free lead particles are observed in XPS and EDS (in case of PbSe) analysis and SEM analysis indicates agglomerated particles. (c) 2005 Elsevier B.V All rights reserved.

10aChemical synthesis10aelectronic materials10areduction10aSemiconductor1 aKhanna, P., K.1 aSubbarao, VVVS1 aWagh, M.1 aJadhav, P.1 aPatil, K., R. uhttps://library.ncl.res.in/content/synthesis-fine-pbe-e-s-se-powder-direct-situ-reduction-sulphur-or-selenium-001958nas a2200229 4500008004100000022001400041245011700055210006900172260009200241300001400333490000600347520110700353653002301460653002001483653001601503653000801519100002001527700002001547700001901567700001801586856012401604 2006 eng d a1533-488000aDirect synthesis of nanocrystalline silver from the reaction between silver carboxylates and n-trioctylphosphine0 aDirect synthesis of nanocrystalline silver from the reaction bet a26650 THE OLD RD, STE 208, VALENCIA, CA 91381-0751 USAbAMER SCIENTIFIC PUBLISHERScJUL a2095-21020 v63 a

Neat n-Trioctylphosphine (TOP) has been used for the first ever time for reduction of silver nitrate and silver carboxylates (citrate, oleate, and myristate) under mild thermal reaction conditions. UV-visible absorption measurements of re-dispersible silver particles that were obtained by reduction of silver myristrate (product-IV) and silver nitrate (product-I) showed surface plasmon resonance absorption peak at 400 nm. The powder XRD pattern of fcc zero-valent silver resulted in diameters in the range of about 25-30 nm. TEM analysis showed particle diameter similar to that was observed by the XRD. FTIR spectroscopy revealed that the organics from the carboxylate group are retained by the nano-particles in case of product-IV however, presence of TOP is observed in product-I. It is found that when silver nitrate is reduced by TOP, spherical silver nano-particles with poor redispersity are formed but extended heating results in formation of long silver rods of micrometer size however, the re-dispersible nano-particles are easily formed when silver carboxylates are reduced by TOP.

10aChemical synthesis10aNanocrystalline10anoble metal10aXRD1 aCharan, Shobhit1 aSingh, Narendra1 aKhanna, P., K.1 aPatil, K., R. uhttps://library.ncl.res.in/content/direct-synthesis-nanocrystalline-silver-reaction-between-silver-carboxylates-and-n-001952nas a2200229 4500008004100000022001400041245014000055210006900195260007300264300001400337490000700351520108200358653002301440653001601463653003001479653001801509100001901527700001401546700002001560700001801580856012401598 2006 eng d a0167-577X00aSynthesis of beta-Ag2Se from organo-selenium precursor and silver nitrate in DMF via simultaneous reduction of selenium and silver salt0 aSynthesis of betaAg2Se from organoselenium precursor and silver  aPO BOX 211, 1000 AE AMSTERDAM, NETHERLANDSbELSEVIER SCIENCE BVcAUG a2080-20850 v603 a

Reaction of selenium powder and silver nitrate in aqueous N,N'-dimethylformamide (aq. DMF) leads to formation of silver selenide. Similar reaction with cycloalkeno-1,2,3-selenadiazole an organic compound of selenium upon thermolysis, also produces silver selenide. It is believed that DMF activates selenium and reduces silver salt via in-situ generated hydrogen ion simultaneously. Slightly broadened X-ray diffraction pattern for pure beta silver selenide (beta-Ag2Se) was observed. Scanning electron microscopy (SEM) indicated that the agglomerated particles could be in the range of about 100 to 200 nm in dimension. EDAX analysis showed non-stoichiometric elemental ratio between silver and selenium. It is found that the weight percent of Ag is slightly higher than Se. However, free amorphous selenium is also detected by XPS analysis when the product is made by use of elemental selenium. Thermal analysis (TGA) revealed a small (4%) weight loss due to the presence of organics or the solvent from the reaction medium. (c) 2005 Elsevier B.V. All rights reserved.

10aChemical synthesis10anano powder10anoble metal chalcogenides10aSemiconductor1 aKhanna, P., K.1 aSingh, N.1 aCharan, Shobhit1 aPatil, K., R. uhttps://library.ncl.res.in/content/synthesis-beta-ag2se-organo-selenium-precursor-and-silver-nitrate-dmf-simultaneous-002131nas a2200241 4500008004100000022001400041245010800055210006900163260007300232300001400305490000700319520127900326653002301605653001801628653001801646653000801664100002001672700002001692700001801712700002201730700001901752856011801771 2006 eng d a0167-577X00aUnusual formation of nano-particles of CdO and Cd(OH)(2) from the reaction of dimethyl cadmium with DMF0 aUnusual formation of nanoparticles of CdO and CdOH2 from the rea aPO BOX 211, 1000 AE AMSTERDAM, NETHERLANDSbELSEVIER SCIENCE BVcDEC a3492-34980 v603 a

This paper presents generation of CdO and Cd(OH)(2) nano-particles from Dimethyl Cadmium in DMF. The CdO nano-particles were obtained instead of CdSe, even when the reaction was done in presence of 1,2,3-selenadiazole (the source of selenium) with Me2Cd in DMF (product-I). The direct reaction of Me2Cd in DMF also leads to formation of CdO (product-II). However, Cd(OH)(2) nano-particles were obtained when Me2Cd was refluxed in DMF for a few hours followed by reaction of H2S gas (product-III). The formation of Cd(OH)(2) was also established via decomposition Of Me2Cd:Et2O adduct (product-IV). Nano-particles of CdO and Cd(OH)(2) (product-I to product-IV) were characterized by X-ray powder diffraction (XRD), TEM and SEM/EDS measurements, FTIR, thermal analysis (TGA) and XPS analysis. The particle size of all the products as calculated by XRD patterns were in the range of about 20 nm. TEM images showed that the products are agglomerated clusters with the particles in the nano-meter regime. The synthesis however, is understood to be unusual as the reactions with selenium source and sulfur source should have generated the CdSe and CdS however, the end products were always found to be the product-I to product-IV (c) 2006 Elsevier B.V. All rights reserved.

10aChemical synthesis10aNanoparticles10aSemiconductor10aXRD1 aSingh, Narendra1 aCharan, Shobhit1 aPatil, K., R.1 aViswanath, A., K.1 aKhanna, P., K. uhttps://library.ncl.res.in/content/unusual-formation-nano-particles-cdo-and-cdoh2-reaction-dimethyl-cadmium-dmf-002051nas a2200277 4500008004100000022001400041245009600055210006900151260008600220300001200306490000700318520111200325653001001437653002301447653001601470653001601486653002101502100001901523700001401542700001701556700001801573700002001591700001801611700001701629856012701646 2007 eng d a1553-317400aOne-step preparation of nanosized Ag-PdCo-powder and its alloy formation at low temperature0 aOnestep preparation of nanosized AgPdCopowder and its alloy form a325 CHESTNUT ST, SUITE 800, PHILADELPHIA, PA 19106 USAbTAYLOR & FRANCIS INCcSEP a531-5390 v373 a

Nano-sized silver-palladium co-powder has been synthesized from silver nitrate-palladium chloride by wet chemical method. The present experimental conditions are applied for the first time for Ag-Pd co-powders wherein sodium formaldehyde sulfoxylate (SFS) has been used as an external reducing agent to simultaneously reduce respective metal salts. SFS reduces the metal salts at room temperature thus prevents formation of bigger particles of the respective metals in co-powder. Powder X-ray diffraction measurements ( XRD) and Transmission electron microscopy ( TEM) suggest the formation of nano-sized Ag-Pd co-powder with particle diameter in the range of about 25 nm. SEM shows that the powder morphology changes with temperature. Heat treatment of 90: 10 (Ag:Pd) composition showed shift in XRD peaks indicating alloy formation of Ag/Pd at lower temperature. Thick-films generated by use of the co-powder resulted in Ag/Pd alloy at about 500 degrees C as confirmed by the XRD. Thermal analysis showed that Ag/Pd co-powders initially gain the weight due to oxidation followed by the weight loss.

10aalloy10aChemical synthesis10anano-powder10anoble metal10aTransition Metal1 aKhanna, P., K.1 aSingh, N.1 aKulkarni, D.1 aMarimuthu, R.1 aCharan, Shobhit1 aPatil, K., R.1 aJain, G., H. uhttps://library.ncl.res.in/content/one-step-preparation-nanosized-ag-pdco-powder-and-its-alloy-formation-low-temperature-002040nas a2200241 4500008004100000022001400041245009700055210006900152260007400221300001200295490000700307520118300314653002301497653002201520653001901542653002001561100001901581700001901600700001801619700001801637700001801655856012501673 2010 eng d a1388-076400aOne-pot synthesis of oleic acid-capped cadmium chalcogenides (CdE: E = Se, Te) nano-crystals0 aOnepot synthesis of oleic acidcapped cadmium chalcogenides CdE E aVAN GODEWIJCKSTRAAT 30, 3311 GZ DORDRECHT, NETHERLANDSbSPRINGERcJAN a101-1090 v123 a

Surface-capped CdSe and CdTe nano-crystals (NCs) have been synthesized using cadmium acetate, oleic acid and respective tri-octylphosphine chalcogenide (TOPE; E = Se/Te) in diphenyl ether (DPE). Well-dispersed CdSe particles showed two absorption bands at the region of 431-34 and 458-60 nm in optical absorption study. A band-edge emission resulted at 515 nm with an excitation energy of 400 nm, in its photoluminescence (PL) spectrum. Similarly, UV-visible absorption study of CdTe revealed an absorption band at < 700 nm. The broadened X-ray diffraction (XRD) pattern showed that at higher reaction temperature cubic CdSe but hexagonal CdTe can be obtained with crystallite size of < 10 nm. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed that agglomerated particles are of spherical nature. The inter-planar spacing in CdTe was measured to be 0.406 nm, a characteristic of (100) lattice plane in hexagonal CdTe. X-ray photoelectron spectroscopy (XPS) showed that CdSe NCs have better air stability stable than CdTe. Presence of organic moiety around the semiconductor particles was confirmed by infrared (IR) spectroscopy.

10aChemical synthesis10aphotoluminescence10aSemiconductors10aSurface capping1 aKhanna, P., K.1 aRao, Srinivasa1 aPatil, K., R.1 aSingh, V., N.1 aMehta, B., R. uhttps://library.ncl.res.in/content/one-pot-synthesis-oleic-acid-capped-cadmium-chalcogenides-cde-e-se-te-nano-crystals-002296nas a2200289 4500008004100000022001400041245011600055210006900171260006900240300001200309490000800321520129400329653001301623653002301636653001101659653001401670100001901684700001901703700002801722700001801750700002501768700001901793700002101812700002301833700001901856856013101875 2010 eng d a0254-058400aSimple chemical co-precipitation/calcination route for the synthesis of simulated synroc-B and synroc-C powders0 aSimple chemical coprecipitationcalcination route for the synthes aPO BOX 564, 1001 LAUSANNE, SWITZERLANDbELSEVIER SCIENCE SAcOCT a695-6990 v1233 a

A simple chemical co-precipitation/calcination route was developed for the synthesis of simulated synroc-B and synroc-C powders using mostly nitrate salts as starting chemicals and 20% ammonia solution as precipitant. In this route, a mixed solution containing Al-nitrate, Ca-nitrate, Ba-nitrate, zirconyl nitrate and titanyl nitrate in the molar proportion required for synroc-B is added to dilute ammonia solution to precipitate these cations in the form of their hydroxides at room temperature by maintaining pH approximate to 10.5 during precipitation. Formation of a major fluorite phase with minor amounts of anatase, rutile and hollandite phases is observed in the powder obtained after calcination in air at 750 degrees C. Multiphase crystalline synroc-B matrix containing hollandite, perovskite, zirconolite, and rutile phases is obtained after sintering the heat treated powder in the form of pellets at 1230 degrees C for 4h in air. Similarly, pure synroc-C phases with 14 and 20% simulated waste loadings were synthesized following the same synthesis protocol. These pre-treated powders with a high surface area of similar to 25 m(2) g(-1) gave sintered ceramics having density of similar to 90% for 14 and 20% waste loadings. (C) 2010 Elsevier B.V. All rights reserved.

10aCeramics10aChemical synthesis10aOxides10aSintering1 aPotdar, H., S.1 aVijayanand, S.1 aMohaideen, Kamal, Khaja1 aPatil, K., R.1 aJoy, Pattayil, Alias1 aMadhavan, Raja1 aKutty, K., V. G.1 aAmbashta, Ritu, D.1 aWattal, P., K. uhttps://library.ncl.res.in/content/simple-chemical-co-precipitationcalcination-route-synthesis-simulated-synroc-b-and-synroc-002013nas a2200229 4500008004100000022001400041245011800055210006900173260010600242300001400348490000700362520110200369653002301471653003101494653001101525653003101536100002401567700001801591700001801609700002601627856013001653 2012 eng d a0025-540800aNovel microwave assisted sol-gel synthesis (MW-SGS) and electrochromic performance of petal like h-WO3 thin films0 aNovel microwave assisted solgel synthesis MWSGS and electrochrom aTHE BOULEVARD, LANGFORD LANE, KIDLINGTON, OXFORD OX5 1GB, ENGLANDbPERGAMON-ELSEVIER SCIENCE LTDcJUL a1787-17930 v473 a

Use of domestic microwave oven is first time employed for chemical deposition of nanocrystalline hexagonal WO3 (h-WO3) thin films. Low cost precursors like sodium tungstate, hydrochloric acid, oxalic acid and potassium sulfate signifies cost effectiveness of this thin film fabrication route. Scanning electron microscopy images reveal formation of petal like nanodisks. A number of analytical techniques were used to characterize the WO3 petal like nanodisks, including X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX). X-ray photoelectron spectroscopy, FT-IR spectroscopy, Raman scattering spectroscopy, UV-visible spectrophotometry and cyclic voltammetry (CV). The X-ray photoelectron spectroscopic studies revealed 2.89 O/W atomic ratio. The electrical transport studies on WO3 thin films show semiconducting behavior with n-type semiconductivity. The value of determined coloration efficiency is 57.90 cm(2)/C. The mechanism of Li+ intercalation and deinercalation in h-WO3 matrix is proposed for enhanced electrochromism. (C) 2012 Elsevier Ltd. All rights reserved.

10aChemical synthesis10aElectrochemical properties10aOxides10aphotoelectron spectroscopy1 aKharade, Rohini, R.1 aPatil, K., R.1 aPatil, P., S.1 aBhosale, Popatrao, N. uhttps://library.ncl.res.in/content/novel-microwave-assisted-sol-gel-synthesis-mw-sgs-and-electrochromic-performance-petal-h-0