Individualized Pixel Synthesis and Characterization of Combinatorial Materials Chips

Conventionally, an experimentally determined phase diagram requires studies of phase formation at a range of temperatures for each composition, which takes years of effort from multiple research groups. Combinatorial materials chip technology, featuring high-throughput synthesis and characterization, is able to determine the phase diagram of an entire composition spread of a binary or ternary system at a single temperature on one materials library, which, though significantly increasing efficiency, still requires many libraries processed at a series of temperatures in order to complete a phase diagram. In this paper, we propose a "one-chip method" to construct a complete phase diagram by individually synthesizing each pixel step by step with a progressive pulse of energy to heat at different temperatures while monitoring the phase evolution on the pixel in situ in real time. Repeating this process pixel by pixel throughout the whole chip allows the entire binary or ternary phase diagram to be mapped on one chip in a single experiment. The feasibility of this methodology is demonstrated in a study of a Ge-Sb-Te ternary alloy system, on which the amorphouscrystalline phase boundary is determined.

Identification, synthesis and characterization of process related impurities of benidipine hydrochloride, stress-testing/stability studies and HPLC/UPLC method validations

Benidipine hydrochloride, used as an antihypertensive agent and long-acting calcium antagonist, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studies of benidipine, process related impurities were detected. These impurities were identified, synthesized and characterized and mechanisms of their formation were discussed in detail. After all standardization procedures, they were used as reference standards for analytical studies. In addition, a separate HPLC method was developed and validated for detection of residual 1-benzylpi- peridin-3-ol （Ben-2）, which is used during benidipine synthesis and controlled as a potential process related impurity. As complementary of this work, stress-testing studies of benidipine were carried out under specified conditions and a stability-indicating UPLC assay method was developed, validated and used during stability studies of benidipine.

Solvothermal Synthesis and Characterization of [TM(1,2-dap)3]HgSb2Se5(TM = Co,Fe)with a Chain Structure

One organic-decorated quanternaery [TM（1,2-dap）3]Hg Sb2Se5（1,2-dap = 1,2-dianinopropane, TM = Co（1）, Fe（2）） compound has been solvothermally synthesized. The compounds crystallize in triclinic space group P 1, with a = 11.248（6）, b = 11.542（7）, c = 12.180（12） A, V =1268.7（16） A^3, Z = 2, F（000） = 1010 for 1 and a = 11.311（5）, b = 11.558（5）, c = 12.180（9） A, V =1276.5（12） A^3, Z = 2, F（000） = 1008 for 2. The crystal structure consists of one-dimensional anionics chains composed of Hg Se4 tetrahedra and SbSe3 trigonal pyramids sharing corners and[TM（dap）3]^2＋ cations. The [HgSb2Se＋5^2-]∞ anionic chains run along the [001] direction, and are surrounded by the [TM（dap）3]^2＋ cations. Meanwhile, 8-ring [Hg2Sb2Se4] and 6-ring [HgSb2Se2] are alternately found. The compounds were structurally characterized by elemental analysis,thermogravimetric analysis, infrared spectroscopy and UV-Vis diffuse reflectance spectroscopy.

Low-Temperature Solid State Synthesis and Characterization of Superconducting Vanadium Nitride

Superconducting vanadium nitride （VN） is successfully synthesized by a solid-state reaction of vanadium pentox- ide, sodium amide and sulfur in an autoclave at a relatively low temperature （240-400℃）. The obtained samples are characterized by x-ray diffraction, x-ray photoelectron spectroscopy and transmission electron microscopy. The result of the magnetization of the obtained VN product as a function of temperature indicates that the onset superconducting transition temperature is about 8.4K. Furthermore, the possible reaction mechanism is also discussed.

New Zincophosphite with Infinite One-dimensional [Zn(HPO_3)(H_2PO_3)]~– Chains: Synthesis, Characterizations and Spectral Properties

With dimethylamine as a template, a new one-dimensional zincophosphite （C2H8N）·[Zn（HPO3）（H2PO3）] was prepared under hydrothermal conditions and characterized by single-crystal X-ray diffraction, FTIR spectrametry, elemental analysis, powder X-ray diffraction, and thermogravimetric analysis. The compound crystallized in the Monoclinic space group P2（1）/c, with cell parameters, a=0.78410（9） nm, b=1.54744（2） nm, c=0.81418（1） nm, β=105.8150（1）°, V=0.95049（2） nm3 and Z=4. The connectivity of the ZnO4 tetrahedron and HPO3 pseudo pyramid resulted in inifinite corner-sharing 4-membered ring chains, which were further linked by the protonated amine molecules to form a 3D structure via hydrogen bonds. To the best of our knowledge, this is the first existence of a zincophosphite with the anionic framework composition of [Zn（HPO3）（H2PO3）]-. The compound exhibits intense photoluminescence at room temperature.

THE SYNTHESIS AND CHARACTERIZATION OF ASYMMETRIC TRIPYRRANE-CONTAINING MACROCYCLES

An improved procedure was used to prepare the asymmetric tripyrrane-containing macrocycles, The yield was over 85% These maerocycles could be oxidized to the methine bridled 23 (?)-electron aromatic cadmium(Ⅱ)complexes by reating with cadmium chloride in the presence of air and their atructures were characterized.

THE SYNTHESIS AND CHARACTERIZATION OF Ba-CROSSLINKED POLYMER ANTI-RADIATION MATERIALS

Crosslinked poly(methyl methacrylate) and polystyrene with barium dimethacrylate [Ba(MA)_2] as crosslinking agent have been synthesized. The relationship between X-ray absorbability and the content of Ba(MA)_2 in polymers was investigated. TGA and DSC results indicated that the crosslinked polymers containing barium dimethacrylate have a much better heat stability than pure PMMA or PS. The mechanical properties of the polymers containing barium are improved in comparison with the pure PMMA.

THE SYNTHESIS AND CHARACTERIZATION OF ANSYMMETRIC PENTAAZADENTATE PORPHYRIN-LIKE METAL COMPLEXES

This paper presents the synthesis and structural characterization of asymmetric tripyrrane-containing macrocycle.This macrocycle could be oxidized to the methine bridged,22 π-electron aromatic macrocyclic complexes containing cadmium(Ⅱ),samarium (Ⅲ),europium(Ⅲ)and gadolinium(Ⅲ)by treating with corresponding metal chloride in the presence of air Their structures were characterized by spectral methods.

THE SYNTHESIS AND CHARACTERIZATION OF THE COORDINATION COMPOUNDS OF Pt(Ⅱ)AND Ir(Ⅲ)WITH 2-MERCAPTOPYRIDINE-1-OXIDE AND ITS METHYL DERIVATIVES

Six coordination compounds of Pt(Ⅱ)L_2 and Ir(Ⅲ)L_3 type(where L is PT^-, 3Me-PT^-or 4Me-PT^-)are reported here.Four coordination compounds of the latter two ligands have never been reported before,while PT^-'s were synthesized with H_2PtCl_6 and(NH_4)_3IrCl_6 respectively,which were different from the methods of Davidson et al.~1 and Sterinbrech^2.They were characterized by elemental analysis, UV,IR,~1HNMR and molar conductance.Their structural formulas have been determined,and the mechanism of synthetic reaction has been discussed.

PRELIMINARY STUDIES ON THE SYNTHESIS AND CHARACTERIZATION OF OXY-AND THIO-DIACETIC ACID HYDRAZITION AND THEIR FIRST-ROW TRANSITION METAL COMPLEXES

It has been made certain that thio-and oxy-diacetic acid hydrazides are potential anticancer compounds.However,their ability to form complexes with transition metals and the properties of the complexes thus formed have not been studied.Employing a new potential anticancer ligand 1,2-bis(thioacetic acid hydrazide)ethane prepared in our lab,along with ligands oxydiacetic hydrazide and 1,2-bis(oxyacetic acid hydrazide) ethane,a series of 11 new first-row transition metal(M=Zn^(2+),Cu^(2+),Co^(2+), Ni^(2+))complexes with each of the above three ligands have been synthesized and characterized by means of elemental analyses,IR,TG and X-ray powder diffraction.

Microwave-induced synthesis and characterization of nanometer Ce_(0.5)Zr_(0.5)O_2 solid solution for the acidic catalytic reaction

Ce0.5Zr0.5O2 solid solution was successfully synthesized using cerium nitrate, zirconium nitrate, and urea as raw materials by the microwave irradiation method and characterized by X-ray diffraction, fluorescence spectrum, transmission electron microscopy, and infrared spectrum. Its acid catalytic activity was evaluated in the esterification reaction of acetic acid and n-butyl alcohol. The results show that Ce0.5Zr0.5O2 solid solution has cubic fluorite structure, and its particle diameter is in the nanometer scale. As a sort of solid acid, it possesses a higher acid catalytic activity and can be easily separated from reaction liquids. It can be used for several times, and basically, its activity keeps constant. The proton acid sites and Lewis acid sites exist in the structure of Ce0.5Zr0.5O2 solid solution.

Preparation and characterization of calcium aluminate by chemical synthesis

Saturated Ca（OH）2 and AlCl3 solutions were used to synthesize calcium aluminate hydrate precipitates at room temperature; high purity calcium aluminate powders with stable phases were made by calcination of the precursors at a temperature as low as 1100℃. PSD and BET analysis revealed the particles with sizes ranging from submicrometer to several micrometers and with a specific area of 13 m^2/g. The measurement of hydraulic exotherm revealed that the exothennal rate is in peak for about 2 h. The exothermal quantities are 449.24 J/g at 12 h and 488.38 J/g at 24 h. Its strength development is quick and the 1 day curing strength is almost equal to 100% of the 3 days curing strength in the mortar test.

One-pot synthesis and structural characterization of urea-isobutyraldehyde-formaldehyde resin

Urea-isobutyraldehyde-formaldehyde (UIF) resin was synthesized from urea, isobutyraldehyde, and formaldehyde using sulfuric acid as a catalyst by one pot method. The effects of molar ratios of isobutyraldehyde to formaldehyde (n(I)/n(F)) and aldehyde to urea (n(A)/n(U)) on the yield, hydroxyl value (vs KOH) and softening point of the resin were investigated. The structure of the resin was characterized by FT-IR, 1H-NMR and 13C-NMR. The results show that when the molar ratio of urea to isobutyraldehyde to formaldehyde (n(U)/n(I)/n(F)) is 1.0/3.0/3.0, the yield UIF resin is 67.1%, and the softening point and hydroxyl value are 88 ℃ and 37 mg/g, respectively. The FT-IR, 1H-NMR and 13C-NMR results show that the lactam is formed by aminomethylation from urea, isobutyraldehyde, and formaldehyde.

Electrochemical synthesis, characterization and thermal properties of niobium ethoxide

Niobium(V) ethoxide(Nb(OEt)5) was synthesized by electrochemical reaction of ethanol with niobium plate as the sacrificial anode,stainless steel as the cathode and tetraethylammonium chloride(TEAC) as the conductive additive.The condensates were isolated by vacuum distillation under 5 kPa.The product was characterized by Fourier transform infrared(FT-IR) spectra,Raman spectra and nuclear magnetic resonance(NMR) spectra.The results indicate that the product is niobium ethoxide.Thermal properties of niobium ethoxide were analysed by TG/DTG.Vapour pressure was calculated from the Langmuir equation and the enthalpy of vaporization was calculated from the vapour pressure-temperature data using the Clausius-Clapeyron equation.The concentrations of impurity metallic elements in the sample were detected by ICP-MS.It is shown that the purity can reach 99.997%.The volatility and purity of the niobium ethoxide ensure that it could be a good precursor for chemical vapor deposition and atomic layer deposition of niobium oxide layers.

Thermal Hydrolysis Synthesis and Characterization of Monoclinic Metahewettite CaV_6O_(16)·3H_2O

Monoclinic metabewettite CaV6O16·3H2O has been fabricated via thermal hydrolysis of calcium vanadate （Ca10V6O25）. High purity calcium vanadate precipitate, featuring colnmn structure with surface area of 8.61 m2/g, can be obtained by reacting sodium 0rthovanadate （Na3VO4） with calcium oxide at 90 ℃ for 2 h. By acidification of calcium vanadate in hot water at pH of 1.0-3.0, the monoclinic metabewettite crystals with uniform particle distribution, layered structure and nonporous structure can be fabricated. With the well crystallized layered structure, CaV6O16·3H2O may be a potential cathode material for secondary batteries as well as super capacitor materials.

Ope Pot Synthesis and Characterization of Safener R-28725

The title compound was synthesized by a one pot synthesis method with ethanolamine ,ketone and dichloroacetyl chloride. The product was characterization by IR, 1 HNMR,UV, and elementary analysis.

A NOVEL THIOPHENE-DERIVED N_2O_2 MACROCYCLE AND ITS Ag(I) COMPLEX: SYNTHESIS AND CHARACTERIZATION

A novel macrocycle containing thiophene （L） was prepared first by the interaction of 2,5-bis-（chloromethyl）-thiophene （A） and salicylaldehyde to give 2, 5-bis-（2-formylphenoxymethyl）-thiophene （B）, and then by the nontemplate cyclocondensation of 1,3-diaminopropane with （B） followed by a "onepot" reduction without isolation of the diimine intermediate. The corresponding silver complex, AgLClO;, was also prepared. The macrocycle was characterized by IR, elemental analysis, MS and;HNMR.

Preliminary Synthesis and Characterization of Mesoporous Nanocrystalline Zirconia

A novel method to prepare mesoporous nano-zirconia was developed. Thesynthesis was carried out in the presence of PEO surfactants via a solid-state reaction. Thematerials exhibit a strong diffraction peak at low 2θ angle and their nitrogenadsorption/desorption isotherms are typical of type IV with H1 hysteresis loops. The pore structureimaged by TEM can be described as wormhole domains. The tetragonal zirconia nanocrystals are uniformin size (around 1.5 nm) and their mesopores focus on around 4.6 nm. The zirconia nanocrystal growthis tentatively postulated to be the result of an aggregation mechanism. This study also revealsthat the PEO surfactants can interact with the Zr-O-Zr framework to reinforce the thermal stabilityof zirconia. The ratio of NaOH to ZrOCl_2, crystallization and calcination temperature play animportant role in the synthesis of mesoporous nano-zirconia.

The Synthesis and Characterization of High Molecular Weight Poly(phenylene sulfide/ether)

Poly（phenylene sulfide/ether） （PPSE） was synthesized from 4,4＇-dihydroxydiphenyl sulfide and 4,4＇-dichlorodiphenyl sulfide in solution by nucleophilic substitution reaction. The resulting polymer was characterized by viscosity measurement, elemental analysis, FT-IR, ^1H NMR, X-ray diffraction and thermal analysis. The results showed that the viscosities of the resulting polymer were above 0.68 dL/g, and the linear chain structure of product was confirmed. PPSE had the same reflex indices as poly（p-phenylene sulfide）, an orthorhombic crystalline with unit cell a=0.853, b=0.562, c=1.026nm. The melting temperature, glass transition temperature and initial decomposition temperature were found to be 228℃, 85℃ and 325℃, respectively. The product was soluble in common organic solvents such as NMP, N, N＇-dimethylformamide, N, N＇-dimethylacetamide and 1,2-dichloroethane.

Scale-up synthesis and characterization of 2,6-diamino-3,5-dinitropyrazine-1-oxide

2,6-diamino-3,5-dinitropyrazine-1-oxide(ANPZO), as an insensitive high explosive, with a high yield and excellent purity has been prepared at pilot plant scale by an improved method. The synthesized ANPZO is characterized by IR, laser granularity measurement, SEM and HPLC.The particle analysis revealed that the improved method could offer desired product with average particle size of 40 mm and high purity(>98.45%). The experimental parameters exhibited that the detonation velocity of the formulation based on ANPZO was higher than that of the corresponding TATB formulation. The DSC curve showed that the exothermic decomposition of the product occurred at the temperature between300.5 C and 360.4 C. Furthermore, the sensitivity test suggests its safe nature towards mechanical stimulus.