DIFFERENTIAL SCANNING CALORIMETRY AND X-RAY DIFFRACTION STUDIES ON AGING BEHAVIOR OF Zn-Al ALLOYS

Decomposition processes of the quenched Zn-Al alloys were studied by differential scanning calorimetry (DSC), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the stabilities of supersaturated solid solution (SSS) of Zn-Al alloy and α' phase formed by quenching would reduce with the increase of Zn content and the precipitation of η-Zn phases even when aging at ambient temperature, so that the exothermic precipitation peak in DSC curve would disappear. The activation energy of the η-Zn precipitation and the reaction enthalpy were calculated and measured. The kinetics of α' decomposition or η-Zn formation was determined by XRD. The microstructure change during aging was observed by TEM.

Assessment of parameters for precipitation simulation of heat treatable aluminum alloys using differential scanning calorimetry

Differential scanning calorimetry （DSC） has been used extensively to study different solid state reactions. The signals measured in DSC are associated with the growth and dissolution of different precipitates during a specific heat cycle. The time-temperature dependence of heat cycles and the corresponding heat flow evolution measured in the sample by DSC provide valuable experimental information about the phase evolution and the precipitation kinetics in the material. The thermo-kinetic computer simulation was used to predict the DSC signals of samples taken from 6xxx and 2xxx alloys. In the model, the evolution of different metastable and stable phases and the role and influence of excess quenched-in vacancies in the early stage of precipitation were taken into account. Transmission electron microscopy （TEM） and high-resolution TEM were used to verify the existence of precipitates, their size and number density at specific points of the DSC curves.

Synthesis kinetics of Mg_2Sn in Mg-Sn powder mixture using non-isothermal differential scanning calorimetry

The non-isothermal heating process of Mg-Sn powder mixture was studied by differential scanning calorimetry(DSC) technique and the synthesis kinetics of Mg2Sn was evaluated by the model-free and model-fitting methods.The activation energy and conversion function of Mg2Sn synthesis reaction are calculated to be 281.7 kJ/mol and g(α)=[-ln(1-α)] 1/4,respectively.The reaction mechanism of 2Mg+Sn→Mg2Sn under non-isothermal condition is regarded as "nucleation and growth" .During the non-isothermal heating process,the phase transformation occurred in the Mg-Sn powder mixture was analyzed by XRD and the microstructure evolution of Mg2Sn was observed by optical microscopy,which is in good agreement with the reaction mechanism of 2Mg+Sn→ Mg2Sn deduced from the kinetic evaluation.

Research on thermal decomposition of 1,3,5-trinitro-1,3,5-triazinane based on differential scanning calorimetry

In order to test the thermal decomposition of 1,3,5-trinitro-1,3,5-triazinane(RDX),the linear temperature rise experiment of RDX was carried out by differential scanning calorimeter under different heating rate conditions.The kinetic calculation of RDX thermal decomposition curve was carried out by Kissinger and Ozawa methods,respectively,and the thermal analysis software was used to calculate the parameters such as self-accelerating decomposition temperature.The results show that the initial decomposition temperature range,decomposition peak temperature range,and decomposition completion temperature range of RDX are 208.4-214.2,225.7-239.3 and 234.0-252.4℃,respectively,and the average decomposition enthalpy is 362.9 J·g^-1.Kissinger method was used to calculate the DSC experimental data of RDX,the apparent activation energy obtained is 190.8 kJ·mol^-1,which is coincident with the results calculated by Ozawa method at the end of the reaction,indicating that the apparent activation energy calculated by the two methods is relatively accurate.When the packaging mass values are 1.0,2.0 and 5.0 kg,respectively,the self-accelerating decomposition temperatures are 97.0,93.0 and 87.0℃,respectively,indicating that with the increase of packaging mass,the self-accelerating decomposition temperature gradually decreases,and the risk increases accordingly.

Measurement of Crystallinity of Acrylic Copolymer by Swelling Differential Scanning Calorimetry

In this paper the measurement of crystallinity(C)ofacrylic copolymer(PAC),by Swelling Differential Scan-ning Calorimetry(SDSC)is discussed.Common DSC isonly used for measuring the crystallinity of polymers withmelting point,(T_m),below their decomposition temper-ature,(T_d).As temperature rises,polymers with swell-ing agent added become swollen and dissolved,goingthrough whole process of breaking solid structures.Thus,SDSC makes it possible to measure the crystallini-ty of polymers even with T_d below T_m.But the C mea-sured by WAXD and the total endothermal melting(swelling)heat in SDSC thermograms,(△H_l),are notlinearly correlated.It has been found that,instead of the△H_l,△H_l’obtained from the △H_l by subtracting the en-dothermal heat,△H_l,and the C measured by WAXDare linearly correlated.On the basis of this linear rela-tion,the unknown C of another PAC sample is measuredby SDSC.The result is in good accordance with thatmeasured by WAXD.

Studies of the Energy Release of Mitochondria from Sporophyte Cytoplasmic Male Sterile Rice by Differential Scanning Calorimetry

The differential scanning calorimetric (DSC)curves of the mitochondria isolated from two varieties of sporophyte cytoplasmic male sterile and their fertile lines of Yie Bai and Ma Xie type rice have been determined. The curves show that the energy is released continuously as temperature rise to 70℃. Some thermodynamic and kinetic parameters of the energy release of the mitochondria have been obtained. The presented results showed that the mitochondria from cytoplasmic male sterile rice released more heat and they had higher energy barrier, less rate, and more complicated mechanism than that of their fertile lines in the energy release process.

Comparison between Glass and Stainless-Steel Vessels in Differential Scanning Calorimetry Estimation

Differential scanning calorimetry (DSC) provides easy screening for thermal hazard evaluation. Here, we investigate the difference between using glass and stainless-steel vessels on the DSC measurement of exothermic decomposition energy (QDSC) for 41 chemical substances (containing nitro, halogen, peroxide, and sulfur groups, and hydrazine bonds). Two borosilicate glass vessels (capillary and ampule) and one stainless-steel vessel were used. All QDSC values obtained were investigated with reference to the permissible fluctuation range specified by the ASTM (American Society for Testing and Materials) international Both glass vessels produced very similar QDSC values, despite different sample scales. The QDSC values obtained with the glass vessels were generally roughly within the variation tolerance range of the stainless-steel vessel. Notable exceptions were halogen- or sulfur-containing compounds;these exhibited smaller QDSC values with glass vessels in almost all cases. We will investigate whether certain structures in compounds react with stainless steel. The vessel material choice is crucial in evaluating the true reactivity of a substance.

Application of Single Scan Differential Scanning Calorimetry Technique for Determination of Kinetic Parameters of Crystallisation in Se-Sb-Ag

A single scan has been performed in Differential Scanning Calorimetry (DSC) at a heating rate of 15oC/min under non-isothermal conditions to investigate the crystallization kinetics of glassy Se90Sb10-xAgx alloys (where x = 2, 4, 6, 8). For this purpose, Handerson’s theory based on non-isothermal method for thermal analysis of single-scan DSC data has been used. The activation energy of crystallization and order parameter has been determined and composition dependence of these parameters has been discussed.

Thermal Diffusivity and Thermal Conductivity of Epoxy-Based Nanocomposites by the Laser Flash and Differential Scanning Calorimetry Techniques

Nanocomposites were fabricated by using a commercial two part epoxy as a matrix and multiwalled carbon nanotubes, graphite fibers and boron nitride platelets as filler materials. Multiwalled carbon nanotubes (MWCNTs) that were produced by chemical vapor deposition were found to produce nanocomposites with better thermal diffusivity and thermal conductivity than the MWCNTs that were produced by the combustion method. Compared to the MWCNTs produced by both methods and graphite fibers, boron nitride produced nanocomposites with the highest thermal conductivity. Specific heat capacity was measured by using differential scanning calorimetry and thermal diffusivity was measured by using the laser flash.

Application of differential scanning calorimetry to study the interpretation on herbal medicinal drugs:a review

Background:Differential scanning calorimetry as a method of investigating and monitoring the kinetics of herbal medicinal plants.Some instrumental and experimental aspects are discussed.Methods:A brief survey is made of herbal medicinal plants and results of differential scanning calorimetry studies are reviewed and this discussion is presented the effects of the instrumental conditions like heating rate and the sample conditions like sample particle size,sample mass,sample purity,sample stability in the melting region and property of impurities.Conclusion:This study suggests that application of differential scanning calorimetry to study the interpretation on herbal medicinal drugs.

ON A DIFFERENTIAL EQUATION FOR KINETICS OF NON- ISOTHERMAL CRYSTALLIZATION

A new differential equation was derived from the modified first-order kinetic model to describe the polymer crystallization processes. The crystallization experiments were carried out by means of DSC. Poly (ethylene terephthalate) resins were selected as the samples containing different catalysts. The relationships between the parameters obtained from the known Avrami equation and from one in the present paper were discussed. A method for applying the equation to determine the kinetic parameters from a constant heating and a constant cooling curve was proposed.

基于特级初榨橄榄油两种不同特性的DSC掺假分析方法研究

该文基于油脂物理特性与氧化稳定性2种特性,利用差示扫描量热法(differential scanning calorimetry,DSC)对市面上常见的特级初榨橄榄油(extra virgin olive oil,EVOO)中大豆油掺假问题进行研究。在物理特性方面,采用DSC冷却曲线来分析EVOO掺假。随着大豆油掺假比例升高,油样在-40~-60℃结晶焓值ΔH由EVOO的29.78 J/g减小为40%掺假混合油的6.133 J/g,对EVOO质量比构建的一元回归方程Y=57.556X-28.44(R2=0.997)。在氧化稳定性方面,氧化温度160℃下,不同油样诱导氧化时间随大豆油掺假比例上升逐渐变短,由EVOO的25.8 min逐渐减小为40%掺假混合油的17.8 min,Y=-19.4X+25.64(R^(2)=0.996),掺假模型相关性较好。这2种DSC检验掺假分析方法都能有效鉴别EVOO中大豆油的掺假且各有特点,可根据实际情况选取合适的方法更好处理EVOO掺假问题。

加热氧化对山茶油热力学及流变学特性的影响

目的探究加热氧化对山茶油热力学及流变学特性的影响。方法山茶油经加热氧化处理后,运用差示扫描量热技术(differential scanning calorimetry,DSC)、旋转流变技术,研究其DSC氧化稳定性,熔融结晶特性及黏度随剪切速率、温度变化等特性。结果山茶油加热时间越长,其DSC热力学氧化稳定性越低,当加热120 min后较初始山茶油的氧化起始温度降低了8.3℃,加热氧化后它的熔融温度及熔融焓降低,主要结晶峰消失。山茶油加热氧化后流动性变差,表现为黏度升高,加热120 min的山茶油较初始山茶油黏度提高了2.8倍,山茶油氧化程度越高,其黏度随温变化的速率越快。结论加热氧化降低了山茶油的热力学稳定性及流变学稳定性,本研究为山茶油精深加工的热力学性能及流变性能提供了一定的理论支撑。

Formation mechanism of the Zn-5%Al hot-dip coating amorphous alloys(Ⅰ)--The analysis of differential scanning calorimetry

HOT-DIPPING Zn+5% Al + (0.01%-0.2%) RE alloy on steel surface by the gas reductionmethod is a new technology. Owing to its good anti-corrosive and forming properties as wellas good technical periormances, the coating attracts wide interest and has been put into indus-trial production rapidly. The authors successfully produced the coating by the electrolytic ac-tivity aid agent method and put it into industrial production. The products have been used inthe electric power and railway engineerings. Results show that the anti-corrosive

基于强流脉冲离子束的中子辐照模拟装置及评价技术

依据高能原子辐照与中子辐照的初级离位原子(PKA)能谱相似性,基于TEMP-6M型强流脉冲离子束(HIPIB)系统,研发了一种中子辐照模拟装置,该装置以磁绝缘离子二极管伴生的强流脉冲二次电子束流实现0.1 MeV以上高能离子的高效率中和,获得动能为0.1~1 MeV、脉冲宽度为120~160 ns、脉冲辐照剂量为1012~10^(15)n/cm^(2)的强流脉冲原子或混合束,原子占比为85%~100%。通过辐照缺陷原位差热分析方法,快速确定材料缺陷数量、密度及dpa损伤速率等抗中子辐照性能评价指标。以核级AISI 304奥氏体不锈钢为例,计算PKA相似性定标曲线,采用220~280 keV的C原子等效1.8~2.3 MeV中子进行辐照模拟,调节名义束流能量密度0.5~4 J/cm^(2),实测辐照剂量范围为0.46×10^(13)~8.55×10^(13)n/cm^(2),热分析确定Frenkel缺陷密度为1.99×10^(16)~2.90×10^(17)/cm^(2),外推预测奥氏体不锈钢在1021n/cm^(2)中子剂量条件下的辐照损伤为500 dpa量级,适用于核电厂结构材料60年服役寿期评价需求。

可降解生物基含酯键环氧树脂的固化动力学研究

采用非等温差示扫描量热(DSC)法研究了可降解生物基含酯键环氧树脂固化动力学,分别建立了n级反应动力学模型、自催化模型以及结合n级反应和自催化模型的分段模型,并将模型预测值与实验数据进行了对比分析。结果表明,n级反应模型与实验曲线的偏差较大,自催化模型与实验曲线变化趋势基本一致,但仍然存在一定偏差,而结合两者的分段模型与实验曲线吻合较好,表明分段模型能更准确地描述该环氧树脂体系的固化反应过程,为其树脂基复合材料固化成型工艺条件优化提供理论指导。

Review of MEMS differential scanning calorimetry for biomolecular study

Differential scanning calorimetry （DSC） is one of the few techniques that allow direct determination of enthalpy values for binding reactions and conformational transitions in biomolecules. It provides the thermody- namics information of the biomolecules which consists of Gibbs free energy, enthalpy and entropy in a straightfor- ward manner that enables deep understanding of the structure function relationship in biomolecules such as the folding/unfolding of protein and DNA, and ligand bindings. This review provides an up to date overview of the applications of DSC in biomolecular study such as the bovine serum albumin denaturation study, the relationship between the melting point of lysozyme and the scanning rate. We also introduce the recent advances of the development of micro-electro-mechanic-system （MEMS） based DSCs.

基于差示扫描量热法的费托蜡非等温结晶动力学

以滴熔点为113、104、92、83、78和73℃的6种窄馏分费托蜡为研究对象,采用差示扫描量热法(DSC)研究其在不同冷却速率下的非等温结晶过程,应用Jeziorny法和莫志深法对结晶动力学参数进行理论预测,通过Kissinger方程计算非等温结晶活化能。结果表明:不同蜡样品的非等温结晶过程相似,并且结晶过程依赖于冷却速率;所采用的动力学模型与试验数据吻合良好,Avrami指数n平均值在1~2之间,说明结晶过程为二次成核,成核后生长形成棒状或纤维状晶体;蜡样品的非等温结晶活化能越小或冷却速率越快,越容易发生结晶。

氯丁橡胶硫化反应动力学

以1,2-亚乙基硫脲为促进剂、氧化锌和氧化镁为硫化剂对氯丁橡胶进行硫化,采用差示扫描量热法研究了氯丁橡胶的非等温硫化反应动力学,通过Kissinger方程和Crane方程计算了硫化反应的动力学参数,并采用硫化仪法研究了等温硫化反应的动力学,计算了硫化反应热硫化阶段的表观活化能。结果表明,n级动力学模型可以有效描述氯丁橡胶的非等温硫化过程,硫化反应的表观活化能为92.78 kJ/mol,反应级数为0.93;氯丁橡胶的等温硫化过程可以分为焦烧阶段、热硫化阶段和平坦硫化阶段,其中热硫化阶段符合一级反应动力学特征,此时表观活化能为53.38 kJ/mol。

一种均质TPO防水卷材的成分分析和性能研究

论文选取一种匀质TPO防水卷材,分析了其正面和反面材料的成分、组成和微观结构。在 115 ℃ 条件下对匀质TPO 防水卷材进行了热老化,研究了其热老化后的力学性能变化规律。为了研究匀质TPO防水卷材在更高温度下的热老化规律,根据国外标准,在 135 ℃ 条件下对匀质TPO防水卷材进行了热老化,测量其质量损失和外观变化,同时也比较了其在 135 ℃热老化后的力学性能变化规律。