Thermal decomposition of magnesium ammonium phosphate and adsorption properties of its pyrolysis products toward ammonia nitrogen

High-purity magnesium ammonium phosphate （MAP） was precipitated by controlling pH value of the reaction system of 9.0-9.5. The thermal decomposition behavior of MAP and the adsorption properties of its pyrolysis products toward ammonia-nitrogen were also studied by XRD, SEM, TGA-DTA and FT-IR methods. The results indicated that high-purity MAP was obtained at pH value of 9.0-9.5. Upon heating to 100-120℃ for 120 min, MAP was thermally decomposed, losing water and ammonia concomitantly with a reduction in grain size and crystallinity. The capacity of pyrolysis products for ammonia nitrogen adsorption reached 72.5 mg/g, with a removal rate of up to 95% from an 800 mg/L solution. The characteristic diffraction peaks corresponding to MAP mainly appeared in their XRD patterns after adsorption of ammonia nitrogen. The pyrolysis products of MAP at 100-120 ℃ could be recycling-used as the chemical treatment regents of ammonia nitrogen in the practical application.

Synthesis and photoluminescence properties of single-crystal ZnO hexagonal pyramids by PEG400-assisted thermal decomposition route

Large-scale synthesis of ZnO hexagonal pyramids was achieved by a simple thermal decomposition route of precursor at 240 oC in the presence of PEG400. The precursor was obtained by room-temperature solid-state grinding reaction between Zn（CH3COO）2-2H2O and Na2CO3. Crystal structure and morphology of the products were analyzed and characterized by X-ray diffraction （XRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM） and high-resolution transmission electron microscopy （HRTEM）. The results of further experiments show that PEG400 has an important role in the formation of ZnO hexagonal pyramids. Difference between the single and double hexagonal pyramid structure may come from the special thermal decomposition reaction. The photoluminescence （PL） spectra of ZnO hexagonal pyramids exhibit strong near-band-edge emission at about 386 nm and weak green emission at about 550 nm. The Raman-active vibration at about 435 cm-1 suggests that the ZnO hexagonal pyramids have high crystallinity.

Salt-Assisted Combustion Synthesis of NdCoO_3 Nanoparticles and Their Catalytic Properties in Thermal Decomposition of Ammonium Perchlorate

Highly dispersed perovskite NdCoO3 nanoparticles were prepared by a novel salt-assisted combustion process. The effects of NaCl content and calcination temperature on the characteristics of the products were characterized by X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM) and BET surface area measurement. The facile introduction of NaCl in the conventional combustion synthesis process was found to result in the formation of well-dispersed perovskite nanoparticles and increase specific surface areas of the resultants from 1.7 to 43.2 m2·g-1. The catalytic properties of the typical NdCoO3 samples for thermal decomposition of ammonia perchlorate (AP) and their correlation with the NdCoO3 microstructure were investigated by Differential Scanning Calorimetry (DSC). The DSC results indicate that the addition of the amorphous NdCoO3 nanoparticles to AP incorporates two small exothermic peaks of AP into a strong exothermic peak, decreases the temperature of the AP exothermic peak to 314.0 ℃ by reduction of 138.3 ℃ and increases the apparent decomposition heat from 515 J·g-1 to over 1441 J·g-1, showing the intense catalytic activity for thermal decomposition of AP. It is also clear that the catalytic activity of the resultant NdCoO3 is related to their microstructure. According to Kissinger′s method, the kinetics parameters of the thermal decomposition of AP catalyzed by the as-prepared NdCoO3 samples were calculated to account for the order of their catalytic activity.

Synthesis Characterization Non-isothermal Kinetics of the Thermal Decomposition and Redox Properties Derived from Copper(Ⅱ) Binuclear Coordination Compound of 1,4-Bis-(1'-Phenyl-3'-Methyl-5'-Pyrazolone-4')-1,4-Butanedione

The paper reports the synthetic procedure and character of Copper(II) binuclearcoordination compound of 1,4-bis-(1'-phenyl-3'-methyl-5'-pyrazolone Thenon-isothermal kinetics of thermal decomposition of the complex has been stUdied from the TG-DTGcurves by means of the Achar et al. and Coats-Redfern methods,the most probab1e kinetic equation canbe expressed as dofdtrAe -E / RT * l /(2Q).The corresponding kinetic compensation effect expressions arefound to be lnuA=0. 1794E+0. 1689.The non-isothermal thermal decomposition process of the complex isone-dimensional diffusion.But electrochemical studies of the complex(Cu2L'2)from cyclic voltamrnetriccurves by means of powder microelectrodes technique'',shows one two-electron irreversible process.

Synthesis of Nano-sized Yttria via a Sol-Gel Process Based on Hydrated Yttrium Nitrate and Ethylene Glycol and Its Catalytic Performance for Thermal Decomposition of NH_4ClO_4

Nano-sized yttria particles were synthesized via a non-aqueous sol-gel process based on hydrated yttrium nitrate and ethylene glycol. The effects of the molar ratio of ethylene glycol to yttrium ion and calcination temperature on crystallite size of the products were studied. The catalytic performance of the as-prepared yttria for the ammonium perchlorate （AP） decomposition was investigated by differential scanning calorimetry （DSC）. The results indicate that the nano-sized cubic yttria particles with less than 20 nm in average crystallite size can be obtained after 2 h reflux at 70℃, dried at 90 ℃, forming xerogel, and followed by annealing of xerogel for 2 h, and that the addition of the nano-sized yttria to AP incorporates two small exothermic peaks of AP in the temperature ranges of 310 - 350 ℃ and 400 - 470 ℃ into a strong exothermic peak of AP and increases the apparent decomposition heat from 515 to over 1110 J·g^- 1. It is also clear that the temperature of AP decomposition exothermic peak decreases and the apparent decomposition heat of AP increases with the increase of the amount of nano-sized yttria. The fact that the addition of the 5 % nano-sized yttria to AP decreases the temperature of AP exothermic peak to 337.7℃ by reduction of 114.6℃ and increases the apparent decomposition heat from 515 to 1240 J·g^-1, reveals that nano-sized yttria shows strong catalytic property for AP thermal decomposition.

Synthesis of Tin Oxide Through Thermal Decomposition of Sn_2(NH_4)_2(C_2O_4)_3 and Its Gas Sensing Property

Nanocrystalline tin oxide samples were prepared by using Sn2 （NH4 ）2 （C2O4）3 as the precursor. The thermal decompositions were respectively conducted at 250,450 and 650 ℃. TG-DTA, XRD, TEM, FTIR were used to characterize the samples. The indirect heating sensors by using these materials as sensitive bodies were fabricated on an alumina tube with Au electrodes and platinum wires. Sensing properties of these sensors were investigated. It was found that the tin oxide sample obtained by thermal decomposition at 450 ℃ has a higher sensitivity to C2H5OH and a higher selectivity to hexane and ammonia than those obtained via the conventional precipitate method and the working temperatures needed were greatly decreased.

Thermal kinetic and thermal safety of Shuangfang-3 gun propellant based on thermal decomposition characteristics

Differential scanning calorimetry(DSC)was used to investigate the thermal decomposition and thermal safety characteristics of Shuangfang-3(SF-3)gun propellant.The kinetic calculation of the DSC curve was carried out by Kissinger and Friedman models,and the time to the maximum rate under adiabatic conditions and the self-accelerating decomposition temperature were calculated by using the AKTS thermal analysis software in combination with the heat balance equation.The thermal history experiment was carried out to further analyze the autocatalytic properties of SF-3.The results show that the initial decomposition temperature,decomposition peak temperature,and decomposition completion temperature of SF-3 all move to the high temperature direction with the increase of heating rate,and the average decomposition heat is 1521.4 J/g.The kinetic model showcased that SF-3 has different reactions in different reaction stages,and its apparent activation energy is 168.2 kJ/mol.When the times to maximum rate under adiabatic conditions are 2.0 h,4.0 h,8.0 h,24.0 h,respectively,the corresponding temperatures are 130.7℃,124.8℃,119.2℃and 110.5℃,respectively.When the masses are 5.0 kg,15.0 kg,25.0 kg,50.0 kg,100.0 kg,respectively,the corresponding self-accelerating decomposition temperatures are 110.0℃,105.0℃,102.0℃,99.0℃and 96.0℃,respectively.As the packaging mass increases,it is more difficult to exchange the liberated heat into the surrounding environment and its safety would be further reduced.The thermal history experiment demonstrates that the thermal decomposition of SF-3 is an n-stage reaction and does not have autocatalytic properties.Therefore,the size and ventilation conditions of the sample have a certain impact on the storage stability of SF-3.In the actual production,usage,storage and transportation,sample size and ventilation conditions should be controlled,and practical and effective measures should be taken according to the actual situation.

Synthesis, Crystal Structure and Luminescent Properties of a Novel 1D Zigzag Chain Barium(Ⅱ) Coordination Polymer

A new coordination polymer {[Ba（L）（H2o）5]·H2O}n （1, H2L = 3,3＇-（（（（ethane-l,2- diylbis（oxy））-bis（2,1-phenylene））bis（methylene））bis（oxy））dibenzoic acid） has been synthesized under evaporation process and characterized by elemental analysis, IR spectra, TG analysis, fluorescence spectrum, powder X-ray diffraction analysis and single-crystal X-ray diffraction. Complex 1 crystallizes in the monoclinic system, space group P21/c, with a = 20.918（5）, b = 7.4539（2）, c = 20.168（5）A, β = 95.486（2）°, V= 3130.1（1） A.3, Z= 4, C30Ha4BaO14, Mr = 755.91, Dc = 1.604 g/cm3, F（000） = 1528,μ = 1.34 mm-1, the final R = 0.0404 and wR = 0.0676 for all data. Single-crystal X-ray structural reveals that the Ba（II） ion adopts a nine-coordinated distorted tricapped trigonal prism coordination geometry. Adjacent Ba（lI） ions are linked by one μ2-L2- anion and two （μ2-H20） water molecules to generate an infinite 1D zigzag chain structure. Then these chains are further linked into a 2D layer supramolecular architecture through O-H…-O hydrogen bonds. Luminescent property and thermal stability of complex I were investigated.

Thermal and luminescent properties of 2 μm emission in thulium-sensitized holmium-doped silicate-germanate glass

In this paper, we present the luminescent properties of Tm^(3+)∕Ho^(3+)co-doped new glass. A series of silicategermanate glass was prepared by the conventional melt-quenching method. In the Tm^(3+)∕Ho^(3+)co-doped silicategermanate glass, a strong emission of 2 μm originating from the Ho^(3+):~5I_7→~5I_8transition can be observed under conventional 808 nm pumping. The characteristic temperatures, structure, and absorption spectra have been measured. The radiative properties of Ho^(3+)in the prepared glass were calculated. The emission cross section of Ho^(3+)ions transition can reach 4.78 × 10^(-21)cm^2 around 2 μm, and the FWHM is as high as 153 nm. The energy transfer efficiency between Ho^(3+)and Tm^(3+)has a large value(52%), which indicates the Tm^(3+)∕Ho^(3+)co-doped silicategermanate glass is a suitable candidate for the 2 μm laser. Moreover, the energy transfer mechanism between Tm^(3+)and Ho^(3+)ions was investigated.

Controllable hydrothermal synthesis of star-shaped Sr3Fe2（OH）12 assemblies and their thermal decomposition and magnetic properties

Pure phase star-shaped hydrogarnet Sr3Fe2（OH）12 assemblies were synthesized by a mild hydrothermal method （210℃, 12 h）, and the effects of the preparation conditions on the phase composition of the product were investigated. It was found that the impurity phases could be decreased or eliminated by increasing the molar ratio of Sr2＋ to Fe3＋, and that high temperatures favored the formation of Sr3 Fe2（OH）12 and reduced the concentration of CO32- -containing byproducts. The thermal decomposition of the star-shaped Sr3Fe2（OH）12 assemblies was examined, and the results showed that the dehydration process at higher temperatures is accompanied by the formation of SrFeO3-δ. Above 655 ℃, a solid state reaction between the SrFeO3-δ and Sr（OH）2 or SrCO3 results in the formation of Sr4Fe3O10-δ.The mag- netic properties of the as-synthesized Sr3Fe2（OH）12 and of samples calcined at different temperatures were assessed. A sample calcined at 575 ℃ exhibited greatly enhanced ferromagnetic properties, with a remanent magnetization of 1.28 emu/g and a coercivity of 4522.1 Oe at room temperature.

A novel method to prepare metal oxide electrode:Spin-coating with thermal decomposition

In this work,we propose a new spin-coating method coupling with high thermal decomposition,to prepare the tin-antimony（Sn-Sb） oxide electrode.The character of the spin-coating electrode was compared with the dip-coating electrode through X-ray diffraction（XRD）,scanning electron microscopy（SEM）,accelerated life test,cyclic voltammetry,and electrolytic degradability. The results showed that the spin-coating electrode had a better defined crystal form,a smoother and more compact surface than that of the dip-coating electrode.Service time of the spin-coating electrode was determined to be longer than 15 h,and it was less than 2 min for the dip-coating electrode.Electrochemical characterization analysis showed that the electrolytic degradability of the spin-coating electrode is better than that of the dip-coating electrode.

Two Novel Nitrogen-rich Energetic Coordination Compounds M_2(DAT)_5(H_2O)_3(TNR)_2(M = Zn and Co):Synthesis,Characterization,Thermal Properties and Sensitivity

Two novel energetic coordination compounds Zn2（DAT）5（H2O）3（TNR）2 and Co2（DAT）5（H2O）3（TNR）2 were synthesized and their structures were characterized by elemental analysis and FT-IR spectroscopy.The crystal structures were determined by single-crystal X-ray diffraction.The results reveal that the compounds have similar molecular structures and the crystals belong to the triclinic system,space group P with a = 11.491（3）,b = 13.564（3）,c = 15.496（3） ,V = 2180.4（8） 3,C17H28 Zn2N36O19,Mr = 1203.02 g·mol-1,Dc = 1.832 g·cm-3,μ（MoKα） = 1.221 mm-1,F（000） = 1223,Z = 2,R = 0.0596 and wR = 0.1514 for 11289 observed reflections（I 〉 2σ（I）） for Zn2（DAT）5（H2O）3（TNR）2 and a = 11.5291（13）,b = 13.4894（15）,c = 15.4852（17） ,V = 2164.8（4） 3,C17H28Co2N36O19,Mr = 1190.14 g·mol-1,Dc = 1.826 g·cm-3,μ（MoKα） = 0.888 mm-1,F（000） = 1211,Z = 2,R = 0.0576 and wR = 0.1431 for 11218 observed reflections（I 〉 2σ（I）） for Co2（DAT）5（H2O）3（TNR）2,respectively.The thermal decomposition characteristics of the com-pounds were investigated using differential scanning calorimetry and thermal gravimetry-diffediffer-rential thermal gravimetry.The results of thermal decomposition processes were similar for the two compounds.Both undergo four-step decomposition after the loss of coordinated H2O molecules.The final solid residues for the two DAT complexes were the corresponding metal oxides.The kinetic parameter of the first exothermic process of the compounds was studied by applying the Kissinger and Ozawa-Doyle methods.The thermodynamic parameters of the activation could be calculated.Sensitivity tests revealed that Co2（DAT）5（H2O）3（TNR）2 was more sensitive than Zn2（DAT）5（H2O）3（TNR）2.

Facile thermal decomposition synthesis of sub-5 nm nanodots with long-lived luminescence for autofluorescence-free bioimaging

Persistent nanophosphors can remain luminescent after the removal of the excitation.Persistent nanophosphors exhibit great advantages in biomedical fields,particularly in autofluorescence-free bioimaging and in-siteexcitation-free photo-theranostics.Despite the great promise of persistent nanophosphors in biomedicine,studies on the controlled synthesis of persistent nanophosphors are limited.Herein,a metal acetylacetonate-based thermal decomposition method was developed for the synthesis of ultra-small persistent luminescence nanodots(PLNDs).The PLNDs display uniform size,good dispersibility and strong persistent luminescence.The luminescent properties of the PLNDs can be readily regulated by ion doping.The thermal decomposition method shows excellent versatility in the synthesis of PLNDs including gallate,sulfide and fluoride.Due to their ultra-small size and surface adsorbed hydrophobic ligand,the PLNDs can be easily integrated with liposomes to construct a stable and biocompatible persistent luminescent nanoplatform for biomedical applications.This work puts forwards a versatile method for the controlled synthesis of ultra-small persistent nanophosphors,and it may further contributes to the areas ranging from biosensing to cancer therapy.

Luminescence investigation of Dy2O2S and Dy2O2SO4 obtained by thermal decomposition of sulfate hydrate

The yellow emitting dysprosium oxysulfide （Dy2O2S） and dysprosium oxysulfate （Dy202SO4） compounds were prepared from the thermal decomposition of hydrated dysprosium sulphate. The materials were characterized by using thermogravimetry （TG/DTG）, X-ray powder diffraction （XRD）, Fourier transform infrared （FTIR） and Raman spectroscopies. The thermal stability temperatures at around 1151 and 1313 K were determined for the Dy202S and Dy202SO4 materials, respectively. The photolumines- cence properties of the dysprosium oxysulfide were investigated, showing narrow emission bands assigned to the 4F9/2----＊6HJ intracon- figurational transitions of the Dy3＋ ion. The yellow emission color of this phosphor suggests that the Dy202S is a promising material for applications in LEDs.

Non-isothermal Decomposition Kinetics of [Cu（en）2H2O] （FOX-7）2·H2O

The thermal behavior and non-isothermal decomposition kinetics of [Cu（en）2H2O]（FOX-7）2·H2O （en=ethylenediamine） were studied with DSC and TG-DTG methods.The kinetic equation of the exothermal process is dα/dt=（10^17.92/β）4α^3/4exp（-1.688×10^5/RT）.The self-accelerating decomposition temperature and critical temperature of the thermal explosion are 163.3 and 174.8 ℃,respectively.The specific heat capacity of [Cu（en）2H2O]（FOX-7）2·H2O was determined with a micro-DSC method,with a molar heat capacity of 661.6 J·mol^-1·K^-1 at 25 ℃.Adiabatic time-to-explosion was also estimated as 23.2 s.[Cu（en）2H2O]（FOX-7）2·H2O is less sensitive.

Hydrothermal Synthesis, Crystal Structure and Properties of One Binuclear Nickel(Ⅱ) Complex with 3-(2-Pyridiyl)-1H-1,2,4-triazole

A new binuclear nickel（Ⅱ） complex [Ni_2（C_7 N_4 H_5）_3（C_9 H_9 O_2）]n has been hydrothermally synthesized with nickel sulfate, 3-（pyridin-2-yl）-1H-1,2,4-triazole and 3,5-dimethylbenzoic acid（3,5-DMBA）. It crystallizes in the triclinic space group P1 with a = 11.5769（7）, b = 12.3115（7）, c = 12.6431（7） A, α = 81.4860（10）o, β = 64.2830（10）o, γ = 63.7130（10）o, V = 1453.45（15） A^3, D_c = 1.604 g/cm^3, Z = 2, F（000） = 720, the final GOOF = 1.048, R = 0.0285 and wR = 0.0628. The crystal structure shows that the whole molecule consists of two nickel ions bridged by three μ_2-η~1：η~0-3-（pyridin-2-yl）-1,2,4-triazole anions. The coordination environment of Ni（Ⅱ） ion is NiO_2 N_4 and NiN_5, giving a distorted octahedral geometry and square pyramidal geometry respectively. The luminescence and thermal properties of the complex were investigated.

Hydrothermal Synthesis,Crystal Structure and Properties of a 1D Chain Copper(Ⅱ) Polymer with 3-(2-Pyridiyl)-1H-1,2,4-triazole(Hpt)

A new 1D copper（Ⅱ） polymer [Cu（Hpt）（3,5-DMBA）]n has been hydrothermally synthesized with copper acetate,3-（pyridin-2-yl）-1,2,4-triazole（Hpt） and 3,5-dimethylbenzoic acid（3,5-DMBA）. It crystallizes in triclinic space group P1,with a = 8.1974（6）,b = 8.3280（6）,c = 12.5021（9） ？,α = 84.3320（10）,β = 71.8870（10）,γ= 65.4560（10）o,V = 737.44（9） ？~3,Dc = 1.612 g/cm3,Z = 2,F（000） = 366,GOOF = 1.035,R = 0.0298 and w R = 0.0855. The crystal structure is a one-dimensional（1-D） chain in which the Cu（Ⅱ） is five-coordinated with square pyramidal geometry. The crystal structure shows that the whole molecule consists of two copper ions bridged by two μ12-η：η0-3,5-dimethylbenzoic acid anions and two 3-（pyridin-2-yl）-1,2,4-triazole molecules. The coordination environment of Cu（Ⅱ） ion is CuO＋2N_3. The luminescence and thermal properties of the complex were investigated.

A 2D Lanthanide-organic Framework Based on Inorganic Lanthanum(Ⅲ) Sulfate Skeletons:Synthesis,Structure,and Luminescence and Thermal Properties

A new lanthanum coordination polymer formulated as {[La2（pyda） 2（μ4-SO4） ·5H2O]· 2H2O}n（1,H2pyda = 2,6-pyridine-dicarboxylic acid） has been synthesized from the reaction of H2pyda with lanthanide nitrate in the presence of sulfate as a counter anion. The compound was characterized by elemental analysis,IR spectroscopy and X-ray single-crystal diffraction. It crystallizes in the orthorhombic system,space group Pna21,with a = 18.8558（19） ,b = 6.5831（7） and c = 18.7543（19） . The compound is a 2D hybrid,in which the La（Ⅲ） ions were doubly connected by the carboxylic group of pyda2-ligand to form the La（Ⅲ） dimer followed by being grafted into 1D zig-zag chains which are further connected into a 2D network containing {[La（SO4） ]＋}n helical chains. The interchain hydrogen bonding and π-π stacking interactions extended the 2D networks into a 3D supramolecular edifice.

Isothermal thermo-analytical study and decomposition kinetics of non-activated and mechanically activated indium tin oxide(ITO) scrap powders treated by alkaline solution

Isothermal decomposition process of chemically transforming indium tin oxide（ITO） powders into indium（III） hydroxide powders was investigated. Two types of powders were analyzed, i.e., non-activated and mechanically activated. It has been found that in the case of activated sample, shorter induction periods appear, which permits growth of smaller crystals, while in the case of non-activated sample, long induction periods appear, characterized by the growth of larger crystals. DAEM approach has shown that decomposition processes of non-activated and mechanically activated samples can be described by contracting volume model with a linear combination of two different density distribution functions of apparent activation energies（Ea）, and with first-order model, with a single symmetrical density distribution function of Ea, respectively. It was established that specific characteristics of particles not only affect the mechanism of decomposition processes, but also have the significant impact on thermodynamic properties.

Effect of heat treatment of titanium substrates on the properties of IrO_2-Ta_2O_5 coated anodes

The Ti substrates of IrO 2 -Ta 2 O 5 coated anodes were treated by solid-solution and aging, stress relieving annealing, and recrystallization annealing, and the coatings were prepared by thermal decomposition of a mixture of H 2 IrCl 6 ·6H 2 O dissolved in hydrochloric acid and TaCl 5 dissolved in alcohol. Scanning electron microscopy （SEM）, cyclic voltammetry （CV）, electrochemical impedance spectroscopy （EIS）, and accelerated life test （ALT） were employed to study the microstructure and electrochemical properties of the anodes. Compared with the anode without heat treatment, the anodes with heat treatment are of higher electrochemical activity and longer accelerated life; especially, the anode with recrystallization annealing treatment has the best electrochemical properties and the longest accelerated life.