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.

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.

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.

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.

Investigation of Crystallization Kinetics in Glassy Se and Binary Se₉₈M₂(M=Ag, Cd, Zn) Alloys Using DSC Technique in Non-Isothermal Mode

The crystallization kinetics of glassy Se and binary Se98M2 (M=Ag, Cd, Zn) alloys have been studied at different heating rates (5, 10, 15, 20 Kmin-1) using Differential Scanning Calorimetric (DSC) technique. The crystallization temperature (Tc) is determined from exothermic peak obtained in DSC scans of present samples. The variation in peak crystallization temperature (Tc) with the heating rate (β) has been used to investigate the growth kinetics using Kissinger, Augis-Bennet and Matusita-Sakka models. The activation energy of crystallization (Ec) has been found to increase with Ag additive and to decrease with Zn and Cd additive. The value of various kinetic parameters such as rate constant (Kp), Avrami index (n), thermal stability (S) and Hruby number (Hr) have been calculated under non-isothermal mode. The maximum change in different kinetic parameters has been found after the incorporation of Ag additive.

Crystallization kinetics of bulk Cu_(58.1)Zr_(35.9)Al_6 alloy

The crystallization kinetics of the bulk amorphous Cu58.1Zr35.9Al6 alloy was examined by differential scanning calorimetry under continuous heating and isothermal annealing.During continuous heating,the activation energy of crystallization was determined to be 383 kJ/mol by Kissinger method.However,on the isothermal annealing,the activation energy was determined to be 459.2 kJ/mol by the Arrhenius method,which was much larger than that obtained from the Kissinger method.The different temperatures at which crystallization occurs are responsible for the discrepancy in the activation energy.The average Avrami exponent of about 3.5 implies that the crystallization process of the bulk amorphous Cu58.1Zr35.9Al6 alloy is diffusion-controlled with a nucleation rate decreasing with time.

Crystallization behavior of amorphous Zr_(70)Cu_(20)Ni_(10) alloy annealed at 380 ℃

Crystallization behavior of amorphous Zr 70 Cu 20 Ni 10 alloy isothermally annealed at 380 ℃ was first investigated by employing the differential scanning calorimetry (DSC) and transmission electron microscopy (TEM). It has been found that an exothermic peak appears in the DSC trace when the annealing time is about 17～18 min, indicating a certain phase transformation occurs in the matrix of amorphous Zr 70 Cu 20 Ni 10 alloy. Meanwhile, isothermal annealing experiments for amorphous Zr 70 Cu 20 Ni 10 alloy ranging from 360 ℃ to 400 ℃ with a temperature interval of 10 ℃ were also carried out, from which no exothermic reaction can be observed except for the case of 380 ℃. This behavior indicates that the phase transformation during isothermal annealing of amorphous Zr 70 Cu 20 Ni 10 alloy is strongly temperature and time dependent. Further investigations are required to reveal the nature of such phenomenon.

KINETICS OF NON-ISOTHERMAL CRYSTALLIZATION OF POLY (ETHYLENE TEREPHTHALATE) MODIFIED BY POLY (ETHYLENE GLYCOL)

The non-isothermal crystallization kinetics of poly(ethylene terephthalate) (PET) modified by poly (ethlene glycol) (PEG) were determined by DSC. The dual linear regression method was used to evaluate the relationship between the reciprocal of t 1/2 ( the half life of crystallization) and the appropriate temperature variable. The parameters such as the activation energy (Ed) for transport, the equilibrium melting temperature (T_m^0),the nucleation parameter (ψ),themaximum crystallization temperature (T_(e, max)), and the kinetic crystallizability (G) for the copolyesters were obtained. The influence of the PEG content in PET chains on the parameters characterizing crystallization kinetics and crystallization thermodynamics was discussed.

Isothermal and nonisothermal crystallization kinetics of bio-sourced nylon 69

Bio-sourced nylon 69,one of promising engineering plastics,has a great potential in developing sustainable technology and various commercial applications.Isothermal and nonisothermal crystallization kinetics of nylon 69 is a base to optimize the process conditions and establish the structure–property correlations for nylon 69,and it is also highly bene ficial for successful applications of nylon products in industry.Isothermal and nonisothermal crystallization kinetics has been investigated by differential scanning calorimetry for nylon 69,bio-sourced even–odd nylon.The isothermal crystallization kinetics has been analyzed by the Avrami equation,the calculated Avrami exponent at various crystallization temperatures falls into the range of 2.28 and 2.86.In addition,the Avrami equation modi fied by Jeziorny and the equation suggested by Mo have been adopted to study the nonisothermal crystallization.The activation energies for isothermal and nonisothermal crystallization have also been determined.The study demonstrates that the crystallization model of nylon 69 might be a twodimensional(circular)growth at both isothermal and nonisothermal crystallization conditions.Furthermore,the value of the crystallization rate parameter(K)decreases signi ficantly but the crystallization half-time(t1/2)increases with the increase of the isothermal crystallization temperature.To nonisothermal crystallization,the crystallization rate increases as the cooling rate increases according to the analysis of Jeziorny's theory.The results of Mo's theory suggest that a faster cooling rate is required to reach a higher relative degree of crystallinity in a unit of time,and crystallization rate decreases when the relative degree of crystallinity increases at nonisothermal crystallization conditions.

NUCLEATION AND CRYSTALLIZATION OF H-SHAPED(PS)_2PEG(PS)_2 BLOCK COPOLYMERS

A series of H-shaped （PS）2PEG（PS）2 block copolymers with different PS chain lengths were prepared. The influence of different confinements active on the crystallization and self-nucleation （SN） behavior of the PEG blocks was investigated by differential scanning calorimetry （DSC）. When the content of the crystalline block was high, a classical SN behavior was obtained. The block copolymer with PEG content of 49% （by weight） showed a classical SN behavior with a narrow self-nucleation domain and had bimodal crystallization exotherms. When the PEG dispersed as separated microdomains in the block copolymer, the self-nucleation domain disappeared and only annealing was observed.

CRYSTALLIZATION AND MELTING OF NYLON 610

Differential scanning calorimetry was used to study the crystallization and melting of nylon 610. For nylon 610 crystallized from the melt state (260 degrees C), the overall rate of bulk crystallization can be described by a simple Avrami equation with Avrami exponent n approximate to 2, independent of crystallization temperature. With the experimentally obtained T-m(0) (235 degrees C similar to 255 degrees C) of nylon 610, the fold surface free energy a, was determined to be 35 similar to 38 erg/cm(2). The effects of annealing temperature and time on the melting of quenched nylon 610 were also investigated. For nylon 610 quenched at room temperature there is only one DSC endotherm peak DSC scans on annealed samples exhibited an endotherm peak at approximately 10 degrees C above the annealing temperature. The size and position of the endothermic peak is strongly related to annealing temperature and time. An additional third melting was observed when quenched nylon 610 was annealed at high temperature for a sufficiently long residence time. The existence of the third melting peak suggests that more than one kind of distribution of lamella thickness may occur when quenched nylon 610 is annealed. The implications of these results in terms of crystal thickening mechanism were discussed.

A STUDY ON THE CRYSTALLIZATION KINETICS OF NYLON 1010

The kinetic behavior of isothermal and nonisothermal crystallization of nylon-1010 has been studied by means of dilatometry and differential scanning calorimetry, respectively. The isothermal and nonisothermal process can be described by Avrami equation and Ozawa equation, respectively. From the experimental results the kinetic parameters of crystallization and crystalline mechanism for isothermal and nonisothermal measurements are discussed.

Impact of Zn(Ⅱ)Ions on Crystallization and Thermal Properties of Poly(lactic acid)

The issues of low crystallinity and slow crystallization rate of poly(lactic acid)(PLA)have been widely addressed.In this work,we find that doping PLA with Zn(Ⅱ)ions can speed up the process of crystallization of PLA.Three kinds of Zn(Ⅱ)salts(ZnCl2,ZnSt and ZnOAc)were tested in comparison with some other ions such as Mg(Ⅱ)and Ca(Ⅱ).The increased crystallinity and crystallization rate of PLA doping with Zn(Ⅱ)are reflected in FT-IR and variable temperature Raman spectroscopy.The crystallinity is further confirmed or measured with differential scanning calorimetry and X-ray diffraction.The crystallinity rate of the PLA/ZnSt-0.4 wt%material can reach 22.46% and the crystallinity rate of the PLA/ZnOAc-0.4 wt%material can reach 24.83%,as measured with differential scanning calorimetry.

Kinetic Study of Non-Isothermal Crystallization in Se_90-xZn₁₀Sb_x(x = 0, 2, 4, 6) Chalcogenide Glasses

Crystallization and glass transition kinetics of Se90-xZn10Sbx (x = 0, 2, 4, 6) chalcogenide glasses prepared by conventional melt-quenching technique were studied under non-isothermal condition using a differential scanning Calorimeter (DSC) measurement at different heating rates 5, 7, 10 and 12°C/min. The glass transition temperatures Tg, the crystallization temperatures Tc and the peak temperatures of crystallization Tp were found to be dependent on the compositions and the heating rates. From the dependence on the heating rates of Tg and Tp, the activation energy for glass transition, Eg, and the activation energy for crystallization, Ec, are calculated and their composition dependence is discussed. The activation energy of glass transition Eg, Avrami index n, dimensionality of growth m and activation energy of crystallization Ec have been determined from different models.

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

Precipitation kinetics of 2519A aluminum alloy based on aging curves and DSC analysis

The precipitation kinetics of 2519 A aluminum alloy after different cold rolling reductions before aging was investigated by hardness test and differential scanning calorimetry（DSC）. The activation energy was calculated according to DSC curves using single heating rate method. The microstructures of as-rolled and peak-aged alloys were observed by transmission electron microscopy（TEM）. The result shows that the age hardenability reduces and the activation energy rises with increasing the reduction from 7% to 40%. Nonuniform dislocations are found in as-rolled alloy and inhomogeneous distribution of θ′ phase is revealed in peak-aged alloy when the reduction is 15%. The inhomogeneous distribution of θ′ phase may be related to the age hardenability reducing and activation energy rising.

Continuous cooling precipitation diagram of high alloyed Al-Zn-Mg-Cu 7049A alloy

The precipitation behaviour during cooling from solution annealing of high alloyed 7049A aluminium alloy was investigated, covering the complete cooling-rate-range of technical interest. This ranges from slow cooling rates close to equilibrium up to rates above complete supersaturation and is covering seven orders of magnitude in cooling rate （0.0005 to 5000 K/s）. The continuous cooling precipitation behaviour of 7049A alloy was recorded by combining different differential scanning calorimetry （DSC） techniques and microstructure analysis by SEM and Vickers hardness testing. The high alloyed, high strength and quench sensitive wrought aluminium alloy 7049A was investigated during quenching from solution annealing by conventional DSC in the cooling rate range of 0.0005 to 4 K/s. In this range at least two exothermal precipitation reactions were observed： a high temperature reaction in a narrow temperature interval of 450-430℃, and a low temperature reaction in a broad temperature interval down to about 200 ℃. Intensities of both reactions decreased with increasing cooling rate. Quenching from solution annealing with rates up to 1000 K/s was investigated by differential fast scanning calorimetry （DFSC） and the differential reheating method （DRM）. A critical quenching rate to suppress all precipitation reactions of 100-300 K/s was been determined.

Effects of beryllium and iron additions on iron-bearing phase in A357 aluminum alloys

Iron is the most deleterious impurity in the Al-Si-Mg casting alloys and can easily form inter-metallic compounds that can significantly affect the subsequent behavior of material properties.Using differential scanning calorimetry (DSC) and microstructural analysis, how the Be and Fe additions affect the iron-bearing phase in A357 alloys was investigated.The results show that the iron-bearing phase in A357 alloy comprises mainly the plate-like β-Al5FeSi and a small quantity of the script-type π-Al8FeMg3Si6; and that the plate-like β-Al5FeSi proportion increases with increasing iron content in the alloy.The iron-bearing phase is mostly transformed from the plate-like β-Al5FeSi to the script-type π-Al8FeMg3Si6 with the addition of Be in the alloy.The hardness of alloy samples was also tested.The results show that both the increasing iron content and Be content can increase the hardness of the alloy.This may be contributed to the change of morphology and distribution of the iron-bearing phase in A357 alloy with the addition of iron or Be to the alloy.

Microstructure and properties of an Al–Ti–Cu–Si brazing alloy for SiC–metal joining

An Al–Ti–Cu–Si solid–liquid dual-phase alloy that exhibits good wettability and appropriate interfacial reaction with SiC at 500–600°C was designed for SiC–metal joining. The microstructure, phases, differential thermal curves, and high-temperature wetting behavior of the alloy were analyzed using scanning electron microscopy, X-ray diffraction analysis, differential scanning calorimetry, and the sessile drop method. The experimental results show that the 76.5Al–8.5Ti–5Cu–10Si alloy is mainly composed of Al–Al2Cu and Al–Si hypoeutectic low-melting-point microstructures (493–586°C) and the high-melting-point intermetallic compound AlTiSi (840°C). The contact angle, determined by high-temperature wetting experiments, is approximately 54°. Furthermore, the wetting interface is smooth and contains no obvious defects. Metallurgical bonding at the interface is attributable to the reaction between Al and Si in the alloy and ceramic, respectively. The formation of the brittle Al4C3phase at the interface is suppressed by the addition of 10wt% Si to the alloy. © 2017, University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg.