Physical Phenomena Leading to Melting of Metals

2017 ◽  
Vol 884 ◽  
pp. 3-17 ◽  
Author(s):  
Roberto Montanari ◽  
Alessandra Varone

Precursor phenomena of melting in pure metals and alloys have been investigated by means of Mechanical Spectroscopy (MS) and High Temperature X-ray Diffraction (HT-XRD). The examined materials were the pure metals In, Sn, Pb and Bi, and some alloys of the systems In-Sn and Pb-Bi with different compositions.MS tests have been carried out by means of a novel method developed by us that permits to operate in resonance conditions and employs hollow reeds of stainless steel containing the liquid metal. In all the metals a sharp drop of dynamic modulus and a Q-1 maximum were observed in a temperature range ΔT before melting that depends on the specific metal and its structure. Such anelastic behaviour is consistent with an increase of the interstitialcies concentration as predicted by the Granato’s theory.Moreover, HT-XRD evidenced that sudden grain re-orientation, shift and broadening of diffraction peaks occur just before the formation of the first liquid, therefore self-interstitials and vacancies seem to play a synergic role in melting. The increase of self-interstitials over ΔT has the effect of weakening interatomic bonds that favours the successive vacancy avalanche leading to the collapse of crystal lattice (melting).

2016 ◽  
Vol 879 ◽  
pp. 66-71 ◽  
Author(s):  
Roberto Montanari ◽  
Alessandra Varone

Precursor phenomena of melting in pure metals (In, Pb, Bi and Sn) and alloys of the systems Pb-Bi and In-Sn with different compositions have been investigated by means of Mechanical Spectroscopy (MS), i.e. dynamic modulus and damping measurements. MS tests evidenced that a sharp drop of dynamic modulus E takes place in a temperature range ΔT before the formation of the first liquid: the modulus variation ΔE and the corresponding temperature range ΔT depend on the specific metal or alloy. The modulus drop is consistent with a relevant increase of interstitial concentration (self-interstitials assuming the dumbbell configuration), as predicted by the Granato’s theory of melting. The increase of damping in the same temperature range of modulus drop supports this explanation. Owing to their dumbbell configuration self-interstitials interact with the flexural vibration of samples and the periodic re-orientation under the external applied stress leads to energy loss and damping increase. The increase of self-interstitials has the effect to weaken interatomic bonds (modulus drop) and favours the collapse of crystal lattice (melting).


2016 ◽  
Vol 879 ◽  
pp. 2026-2031 ◽  
Author(s):  
Roberto Montanari ◽  
Oriana Tassa ◽  
Alessandra Varone

Microstructure stability of the directionally solidified Ni base IN792 superalloy has been investigated by Mechanical Spectroscopy (MS), i.e. internal friction (IF) and dynamic modulus measurements. Repeated IF test runs from room temperature to 1173 K have been carried out on the same samples and a Q-1 maximum has been always observed above 700 K. Its position does not depend on the resonance frequency. After each run the values of modulus and Q-1 at room temperature change indicating that a progressive irreversible transformation occurs. Damping phenomena have been attributed to the rearrangement of dislocation structures in disordered matrix which modifies dislocation density and average distance of pinning points. The results are supported by X-ray diffraction (XRD) and transmission electron microscopy (TEM) observations.


2015 ◽  
Vol 71 (4) ◽  
pp. 361-367 ◽  
Author(s):  
Federica Fabrizi ◽  
Pamela A. Thomas ◽  
Gareth Nisbet ◽  
Stephen P. Collins

A novel method is presented for the identification of the absolute crystallographic structure in multi-domain polar materials such as ferroelectric KTiOPO4. Resonant (or `anomalous') X-ray diffraction spectra collected across the absorptionKedge of Ti (4.966 keV) on a single Bragg reflection demonstrate a huge intensity ratio above and below the edge, providing a polar domain contrast of ∼270. This allows one to map the spatial domain distribution in a periodically inverted sample, with a resolution of ∼1 µm achieved with a microfocused beam. This non-contact, non-destructive technique is well suited for samples of large dimensions (in contrast with traditional resonant X-ray methods based on diffraction from Friedel pairs), and its potential is particularly relevant in the context of physical phenomena connected with an absence of inversion symmetry, which require characterization of the underlying absolute atomic structure (such as in the case of magnetoelectric coupling and multiferroics).


2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.


2021 ◽  
Vol 19 (1) ◽  
pp. 745-754
Author(s):  
Khoirina Dwi Nugrahaningtyas ◽  
Eddy Heraldy ◽  
Rachmadani ◽  
Yuniawan Hidayat ◽  
Indriana Kartini

Abstract The properties of three types of CoMo/USY catalysts with different synthesized methods have been studied. The sequential and co-impregnation methods followed by activation using calcination and reduction process have been conducted. The properties of the catalysts were examined using Fourier-transform-infrared (FTIR) spectroscopy, X-ray diffraction (XRD) with refinement, and surface area analyzer (SAA). The FTIR spectrum study revealed the enhanced intensity of its Bronsted acid site, and the XRD diffractogram pattern verified the composition of pure metals, oxides, and alloys in the catalyst. The SAA demonstrated the mesoporous features of the catalyst. Scanning electron microscopy showed an irregular particle morphology. Additional analysis using the transmission electron microscopy indicated that the metal has successfully impregnated without damaging the USY structure.


2004 ◽  
Vol 812 ◽  
Author(s):  
Nobutoshi Fujii ◽  
Kazuhiro Yamada ◽  
Yoshiaki Oku ◽  
Nobuhiro Hata ◽  
Yutaka Seino ◽  
...  

AbstractPeriodic 2-dimensional (2-D) hexagonal and the disordered pore structure silica films have been developed using nonionic surfactants as the templates. The pore structure was controlled by the static electrical interaction between the micelle of the surfactant and the silica oligomer. No X-ray diffraction peaks were observed for the disordered mesoporous silica films, while the pore diameters of 2.0-4.0 nm could be measured by small angle X-ray scattering spectroscopy. By comparing the properties of the 2-D hexagonal and the disordered porous silica films which have the same porosity, it is found that the disordered porous silica film has advantages in terms of the dielectric constant and Young's modulus as well as the hardness. The disordered porous silica film is more suitable for the interlayer dielectrics for ULSI.


2012 ◽  
Vol 184 ◽  
pp. 434-439 ◽  
Author(s):  
Roberto Montanari ◽  
Alessandra Varone

Liquid Pb–Bi eutectic alloy has been selected as coolant and neutron spallation source for the development of MYRRHA, an accelerator driven system. The alloy has been characterized in liquid state from melting (125 °C) to 650 °C by mechanical spectroscopy. Experiments have been carried out using hollow reeds of austenitic stainless steel filled with the Pb-Bi alloy and sealed at the extremities. From 350 °C to 520 °C modulus shows a remarkable drop accompanied by a broad internal friction maximum. In the same temperature range radial distribution functions, determined from X-ray diffraction patterns, evidenced variations of the mean distance between the 1st nearest neighbour atoms. The anelastic phenomena have been attributed to a structural re-arrangement of liquid metal. For comparison, other alloys of the Pb-Bi system with hypo-eutectic composition have been investigated.


2012 ◽  
Vol 472-475 ◽  
pp. 1451-1454
Author(s):  
Xue Hui Wang ◽  
Wu Tang ◽  
Ji Jun Yang

The porous Cu film was deposited on soft PVDF substrate by magnetron sputtering at different sputtering pressure. The microstructure and electrical properties of Cu films were investigated as a function of sputtering pressure by X-ray diffraction XRD and Hall effect method. The results show that the surface morphology of Cu film is porous, and the XRD revealed that there are Cu diffraction peaks with highly textured having a Cu-(220) or a mixture of Cu-(111) and Cu-(220) at sputtering pressure 0.5 Pa. The electrical properties are also severely influenced by sputtering pressure, the resistivity of the porous Cu film is much larger than that fabricated on Si substrate. Furthermore, the resistivity increases simultaneously with the increasing of Cu film surface aperture, but the resistivity of Cu film still decreases with the increasing grain size. It can be concluded that the crystal structure is still the most important factor for the porous Cu film resistivity.


2010 ◽  
Vol 428-429 ◽  
pp. 126-131
Author(s):  
Wei Zhong Lu ◽  
Chun Wei ◽  
Qui Shan Gao

Polymethylene bis(p-hydroxybenzoates) were prepared from methyl p-hydroxybenzoate and different diols by melted transesterification reaction. Three liquid crystalline polyesters were synthesized from terephthaloyl dichloride and polymethylene bis(p-hydroxybenzoates). Its structure, morphology and properties were characterized by Ubbelohde viscometer, Fourier transform infrared spectroscopy (FT-IR), Differential scanning calorimetry (DSC), polarized optical microscopy (POM) with a hot stage, and wide-angle X-ray diffraction (WAXD). Results indicated that the intrinsic viscosities were between 0.088 and 0.210 dL/g. Optical microscopy showed that the TLCP has a highly threaded liquid crystalline texture and a high birefringent schlieren texture character of nematic phase and has wider mesophase temperature ranges for all polyesters. DSC analysis were found that the melting point (Tm), isotropic temperature (Ti) of TLCPs decreased and the temperature range of the liquid crystalline phase became wider with increased number of methylene spacers in the polyester. The WAXD results showed that TLCPs owned two strong diffraction peaks at 2θ near 19° and 23°.


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