Thermal Behavior and Non-isothermal Kinetics of the Polyoxometalate of Ciprofloxacin with Tungstophosphoric Acid

The polyoxometalate(CPFX·HCl)3 H3 PW12 O40 ·8H2 O was prepared and characterized by elemental analysis,IR spectra and TG-DTA-DTG.The thermal decomposition mechanism and non-isothermal kinetic parameters of the polyoxometalate were obtained from the analysis of TG-DTG data using the Achar equation,Coats-Redfern equation(CR),Madhusudanan-Krishnan-Ninan equation(MKN)and Horowitz-Metzger equation(HM).And their mathematical expressions of the kinetic compensation effect were also calculated.     

Effects of citric acid on hydration process and mechanical properties of thermal decomposed magnesium oxychloride cement

In order to make full use of salt lake magnesium resources and improve the strength of the thermal decomposed magnesium oxychloride cement(TDMOC), the effects of citric acid on the hydration process and mechanical properties of TDMOC was studied. The hydration heat release at initial 24 h and strengths at 3, 7, and 28 days of TDMOC specimens were conducted. The hydration products and paste microstructure were analyzed by XRD, FT-IR and SEM, respectively. The results showed that citric acid can not only reduce the 24 h hydration heat release and delay the occurring time of second peak of TDMOC, but also produce more 5Mg(OH)2·MgCl 2·8H2O and less Mg(OH)2 in hydration process of TDMOC. More perfect and slender crystals were observed in the microstructure of the TDMOC pastes with citric acid. The results demonstrated that citric acid as an additive of TDMOC can decrease the hydration heat release and increase the compressive strength and flexural strength of TDMOC. The possible mechanism for the strength enhancement was discussed.     

Thermal Decomposition of Leightonite,K2Ca2Cu（SO4）4·2H2O

The thermal decomposition of Leightonite, K2Ca2Cu（SO4）4·2H2O, was studied by thermal gravimetric analysis（TGA）, differential thermal analysis（DTA）, X-ray diffraction（XRD）, etc. The results show that the Leightonite is dehydrated around 170 ℃ to 390 ℃ and transformed to be new intermediate （K-Cu-SO4） sulphate salt with bright-green color. Moreover, the chemical structure changes during the thernal decomposition process was describled in detail. And the as-resulting phases are demonstrated to be K2Ca2（SO4）3, K2SO4, CaSO4 ,and Cu2O.     

The Thermal Decomposition Kinetics of Polysiloxane/Polymethylacrylate IPNs Materials

1Introduction Recently,anincreasingattentionhasbeenpaidtopolysiloxanebecausepolysiloxaneisthermallyresistantpolymerinhightemperaturewiththermalenduranceinoxidativeatmosphereupto300℃andmoreininertat mosphere.Thermoanalyticaltechniques,suchasthermo gravimetric(TG),differentialthermolgravimetric(DTG),anddifferentialscanningcalorimetry(DSC)havewidelybeenusedtocharacterizepolymericmaterials.Qingzeng Zhu[1]investigatedthethermaldecompositionofsilazanepolymerswiththermogravimetrymethodandindicat…     

Fabrication of Ni-, Co- and NiCo-coated graphite microspheres by heterogeneous precipitation

The precursors with NiCO₃·2Ni(OH)₂·2H₂O, Co₂(OH)₂CO₃, or both NiCO₃·2Ni(OH)₂·2H₂O and Co₂(OH)₂CO₃ coated graphite microspheres were prepared respectively by the aqueous heterogeneous precipitation using nickel sulfate, cobalt nitrate, sodium carbonate, ammonium bicarbonate and graphite microspheres as the main starting materials. Subsequently, Ni-, Co- and NiCo-coated graphite microspheres were successfully obtained by thermal reduction of the as-prepared precursors at 500 °C for 2 h, respectively. These metal-coated graphite microspheres were characterized with a smooth, cohesive surface consisting of fine metallic particles. Optimized precipitation processing parameters of the concentration of graphite microspheres (10 g/L), the rate of adding reactants (3 mL/min) and pH value (8.0) were determined by a trial and error method. The thermal analysis of the precursors was investigated by TG. Powders of the precursors and the resultant metal-(Ni, Co and NiCo alloy) coated graphite microspheres were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). Funded by the Post-graduate Innovation foundation of Jiangsu Province of China (No. CX07B_085z)     

Influence of sugar filter mud on formation of portland cement clinker

To explore the mechanisms of filter mud (FM) in the portland cement clinker formation, and to make effective use of FM in the cement production as lime-based raw materials, the influences of FM on the apparent activation energy of calcium carbonate decomposition, liquid phase amount, crystalline phase and tricalcium silicate polymorphism were investigated by TA, SEM and XRD. The experimental results show that FM can reduce apparent activation energy of calcium carbonate decomposition, and increase liquid phase amount. Appropriate FM replacement ratios are useful to promoting the C₃S formation and heightening the C₃S content. New phases of α-C₂S and C₂S·0.5Ca₃ (PO₄)₂ can be found in the clinkers while the ratios are above 15%. In addition, impurities in FM can induce the C₃S polymorph to transform.     

Preparation and reaction mechanism of red mud based ceramic simple bricks

In order to utilize solid wastes,ceramic simple bricks with high performances were made from industrial solid wastes such as red mud,fly ash and poor clay shale as main raw materials in this paper.The phase compositions and microstructures were tested by XRD,SEM and EPMA.The experimental results show that the water absorption is 45.64%,the porosity is 58.91%,bulk density is 1.29 g·cm-3,compressive strength is 54.91 MPa,bending strength is 29.52 MPa,freeze-thaw resistance is 29.28 MPa,specific heat capacity at constant pressure is 1.31 J·g-1·K-1,thermal diffusivity is 5.89×10-3 cm2·s-1,and thermal conductivity is 1.15×10-2 W·cm-1·K-1.These effects of additives and preparation process to the properties and microstructures were discussed in detail.The reaction mechanism was also discussed.The results of the reaction mechanism show that there has wollastonite and feldspar generated during the process of firing while Ca gathered around the feldspar,and then Ca would displace K and generated cacoclasite.     

Influencing mechanism and interaction of muscovite on thermal decomposition of ammonium polyphosphate

The interaction mechanism and phase evolution of ammonium polyphosphate(APP)mixed with muscovite(APP/muscovite)were studied by TG,XRD and SEM,respectively,during heating.When the temperature is not higher than 300 ℃,muscovite has no effect on the thermaldecomposition of APP,and the initialdecomposition temperature of APP/muscovite at 283 ℃ is basically the same as the APP at 295 ℃,and the main thermaldecomposition products are polyphosphoric acid and NH_4H_2PO_4 at 300 ℃.The polyphosphoric acid,the decomposition products of APP,can enable K and Siout of muscovite and interact with muscovite chemically to generate Al_2O_3·2SiO_2,α-SiO_2 and phosphates(AlPO_4 and K_5P_3O_(10))compounds during 400 ℃-800 ℃,which own obvious adhesive phenomenon and porous structure with the apparent porosity of 58.4%.Further reactions between phosphates other than reactions among Al_2O_3·2SiO_2 and α-SiO_2 can generate KAlP_2O_7 at 1 000 ℃ and the density of residualproduct is improved by low melting point phosphate filling pore to form relatively dense structure and decrease the apparent porosity to 44.4%.The flame resistant and self-supported ceramic materials are expected to enhance the fire-retarding synergistic effect between APP and muscovite.     

Thermal Behavior Study of Carbonate Inorganic Materials

The thermal decomposition processes of(MgCO_3)_4·Mg(OH)_2·5H_2O(MCH),5ZnO·2CO_3·4H_2O(ZCH),NiCO_3·2Ni(OH)_2·4H_2O(NCH),PbCO_3(LC)and [Cr(OH)_5]_2·CO_3·8H_2O(CC)were studied via TG-DSC.The results of research imply that MCH has the largest capacity of heat absorption and ZCH is second to MCH among the studied materials.The non-isothermal kinetic parameters of MCH and ZCH were calculated by Kissinger and Ozawa methods.Furthermore,thermal decomposition mechanisms of MCH and ZCH were investigated by Coats-Redfern method.Due to the large specific heat capacity,MCH and ZCH are promising to be used as a coolant in extinguishant formulations.     

晶型控制剂对碳酸钙晶须合成的影响

分别以氢氧化镁和氯化镁作为晶型控制剂,采用碳酸化法制备碳酸钙晶须,利用扫描电镜和X射线衍射对产物的形貌、结构及矿物组成进行表征,从而得出晶型控制剂对合成碳酸钙晶须的影响。结果表明:当镁钙比小于1,反应温度为80℃,搅拌速度在100~130 r/min和二氧化碳通气量为70~100 mL/min时,氢氧化镁较之氯化镁更容易促进碳酸钙晶须的生成,所得的碳酸钙晶须多呈树枝状分布。     

Co-precipitation/hydrothermal synthesis of BiFeO<Subscript>3</Subscript> powder

A coprecipitation/hydrothermal route was utilized to fabricate pure phase BiFeO3 powders using FeCl3·6H2O and Bi（NO3）3·5H2O as starting materials, ammonia as precipitant and NaOH as mineralizer. The synthesized powders were characterized by XRD, SEM and DSC-TG analysis. In the process, single-phase BiFeO3 powders could be obtained at a hydrothermal reaction temperature of 180 ℃, with NaOH of 0.15 mol/L, in contrast to 200 ℃ and 4 mol/L for conventional hydrothermal route. Meanwhile, the micro-morphology of synthesized BiFeO3 powders changed with different reaction temperatures and concentrations of NaOH. The N6el temperature, Curie temperature and decomposition temperature of the synthesized BiFeO3 powders were detected to be 301 ℃, 828 ℃ and 964 ℃, respectively. The hydrothermal reactions mechanism to fabricate BiFeO3 powders were discussed based on the in-situ transformation process.     

Preparation of Bauxite Ceramic Microsphere

Ceramic microspheres were prepared by using Chinese bauxite as raw materials through the centrifugal spray drying method. The control technology of microsphere size, degree of sphericity was researched. The ceramic microspheres were sintered by a double sintering process. The microstructure and composition of ceramic microsphere were investigated by X-ray diffraction （XRD）, scanning electron microscopy （SEM） and X-ray energy spectroscopy. The results show that the degree of sphericity of the ceramic microsphere was good and the particle size was 10-100 μm. The XRD analysis reveals that the main crystalline phase of the ceramic microsphere was a-Al2O3 and mullite （3Al2O3·2SiO2）. The product can be used as reinforced material for composite material, especially for antiskid and hard wearing aluminum alloy coating.     

In-Situ Preparation and thermal shock resistance of mullite-cordierite heat tube material for solar thermal power

In order to improve the thermal shock resistance of solar thermal heat transfer tube material, the mullite-cordierite composite ceramic as solar thermal heat transfer tube material were fabricated by pressureless sintering using α-Al2O3 , Suzhou kaolin, talc, and feldspar as starting materials. The important parameter for solar thermal transfer tube such as water absorption (Wa ), bulk density (Db ), and the mechanical properties were investigated. The phase composition and microstructure of the composite ceramics were analyzed by XRD and SEM. The experimental results show that the B3 sintered at 1 300 ℃ and holding for 3 h has an optimum thermal shock resistance. The bending strength loss rate of B3 is only 2% at 1 100℃ by air quenching-strength test and the sample can endure 30 times thermal shock cycling, and the water absorption, the bulk density and the bending strength are 0.32%, 2.58 g·cm-3 , and 125.59 MPa respectively. The XRD analysis indicated that the phase compositions of the sample were mullite, cordierite, corundum, and spinel. The SEM images illustrate that the cordierite is prismatic grain and the mullite is nano rod, showing a good thermal shock resistance for composite ceramics as potential solar thermal power material.     

Effect of MnO<Subscript>2</Subscript> on properties of SiC-mullite composite ceramics for solar sensible thermal storage

For improving the properties of SiC-mullite composite ceramics used for solar sensible thermal storage, MnO₂ was introduced as sintering additive when preparing. The composite ceramics were synthesized by using SiC, andalusite, α-Al₂O₃ as the starting materials with non-contact graphite-buried sintering method. Phase composition and microstructure of the composites were investigated by XRD and SEM, and the effect of MnO₂ on the properties of SiC composites was studied. Results indicated that samples SM1 with 0.2 wt% MnO₂ addition achieved the optimum properties: bending strength of 70.96 MPa, heat capacity of 1.02 J·(g·K)^-1, thermal conductivity of 9.05 W·(m·K)^-1. Proper addition of MnO₂ was found to weaken the volume effect of the composites and improve the thermal shock resistance with an increased rate of 27.84% for bending strength after 30 cycles of thermal shock (air cooling from 1 100 °C to RT).     

Synthesis and characterization of high-voltage cathode material LiNi0.5Mn1.5O4 by one-step solid-state reaction

LiNi_0.5Mn_1.5O₄ was prepared under various conditions by one-step solid-state reaction in air and its properties were investigated by X-ray diffractormetry (XRD), scanning electron microscopy (SEM) and electrochemical measurement. XRD patterns show that LiNi_0.5Mn_1.5O₄ synthesized under various conditions has cubic spinel structure. SEM images exhibit that the particle size increases with increasing calcination temperature and time. Electrochemical test shows that the LiNi_0.5Mn_1.5O₄ calcined at 700 °C for 24 h delivers up to 143 mA · h/g, and the capacity retains 132 mA · h/g after 30 cycles. Foundation item: Project (76600) supported by Postdoctoral Science Foundation of Central South University     

Influence of La-dopant on the material characteristics and supercapacitive performance of MnO<Subscript>2</Subscript> electrodes

Manganese dioxide was synthesized by electrodeposition method with Mn (CH3COO)2?4H2O as a raw material. La(NO3)3?6H2O was doped in electroyte during the preparing process to improve the performance of MnO2 electrodes. The micrographs, crystal structure and element content of electrodes were analyzed by SEM, XRD and atomic absorption spectroscopy, respectively. It is found that the La content ratio in the dioxide can be easily controlled by adjusting the composition of the plating solution. Appropriate amoun...     

Effect of tin on the reaction synthesis of ternary carbide Ti3AlC2

The effect of tin on synthesis of Ti₃AlC₂ by spark plasma sintering (SPS) from TiC/Ti/Al powders was investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used for phase identification and microstructure evaluation. The experimental results show that addition of tin can considerably accelerate the synthesis reaction of Ti₃AlC₂ and fully dense, essentially single-phase polycrystalline Ti₃AlC₂ could be successfully obtained by sintering 2TiC/1Ti/1Al/0.2Sn powders at 1200–1250 °C under a pressure of 30 MPa. SEM images show that Ti₃AlC₂ samples in about 2–5 μm thick and 10–25 μm long platelets can be obtained. The fracture toughness and flexural strength of Ti₃AlC₂ were 6.5±0.2 MPa·m^1/2 and 560±10 MPa, respectively. Funded by the National Natural Science Foundation of China (No.20771088, No.50572080) and Doctoral Foundation of Wuhan University of Technology (No.471-38650142)     

Synthesis and characterization of triclinic structural LiVPO4F as possible 4.2 V cathode materials for lithium ion batteries

A potential 4.2 V cathode material LiVPO4F for lithium batteries was prepared by two-step reaction method based on a carbon-thermal reduction （CTR） process. Firstly, V2O5, NH4H2PO4 and acetylene black are reacted under an Ar atmosphere to yield VPO4. The transition-metal reduction is facilitated by the CTR based on C→CO transition. These CTR conditions favor stabilization of the vanadium as V^3＋ as well as leaving residual carbon, which is useful in the subsequent electrode processing. Secondly, VPO4 reacts with ElF to yield LiVPO4F product. The property of the LiVPO4F was investigated by X-ray diffractometry （XRD）, scanning electron microscopy （SEM） and electrochemical measurement. XRD studies show that LiVPO4F synthesized has triclinic structure（space group p I ）, isostructural with the naturally occurring mineral tavorite, EiFePO4-OH. SEM image exhibits that the particle size is about 2μm together with homogenous distribution. Electrochemical test shows that the initial discharge capacity of LiVPO4F powder is 119 mA·h/g at the rate of 0.2C with an average discharge voltage of 4.2V （vs Ei/Li^＋）, and the capacity retains 89 mA·h/g after 30 cycles.     

水热辅助溶胶凝胶法制备纳米钛酸锌及其光催化性能

采用水热辅助的溶胶凝胶法制备纳米钛酸锌（ZnTiO₃）光催化剂,以罗丹明B为目标降解物,运用动力学模型分析罗丹明B（RhB）初始浓度对降解效果的影响。通过SEM、XRD、XPS、UV-Vis DRS对ZnTiO₃进行表征,并使用自由基捕获试验分析其降解机理。结果表明,ZnTiO₃为纯六方相,形貌为类球形,粒径50 nm左右。在催化剂用量为1 g/L、RhB初始浓度为5 mg/L、pH值为3的条件下,光催化反应150 min后,RhB降解率为93.2%。其动力学方程为k=0.132C₀^-1.253。ZnTiO₃光催化剂降解过程中,·OH、h⁺、·O₂^-均起到催化作用,产生·OH、h⁺的量相近且多于·O₂^-,说明·OH、h⁺在催化反应中起主要作用。     

Phase transformation of nano-grained W(Co, C) composite powder and its phase constitute

1 INTRODUCTION Nano-grained WC-Co cemented carbides with high toughness and high hardness have drawn extensive attention of hard metal industry[1?2]. There are two key processes for the fabrication of this high performance alloy[3?4]. One is the preparation of nanometer WC-Co composite powders, the other is the effective control of grain growth during sintering. At present, great technical breakthrough has been achieved in the preparation of nanometer powders. The typical methods of na…