scholarly journals Multi-Scale Investigation of Body-Glaze Interface in Ancient Ceramics

Heritage ◽  
2019 ◽  
Vol 2 (3) ◽  
pp. 2480-2494 ◽  
Author(s):  
Marie Godet ◽  
Gauthier Roisine ◽  
Emmie Beauvoit ◽  
Daniel Caurant ◽  
Odile Majérus ◽  
...  

Bernard Palissy is a French Renaissance ceramist renowned for his masterpieces called Rustiques Figulines on which dozens of glazes of different chemistries (and thus firing behaviors) coexist harmoniously. This study aims at gathering information on the master procedure -never revealed- by investigating the body-glaze interface region (focusing on iron-colored honey transparent glaze-white body system). Optical and electron microscopies including transmission electron microscopy (TEM) are used to characterize the micro and nanostructure of both archaeological and replicas interfaces elaborated in controlled conditions (firing time, cooling rate, addition of Al in the glazing mixture). Both types of interfaces are comparable: a modified paste area from which are growing a relatively continuous layer of interfacial crystals identified as lead feldspars (K,Ca)PbAl2Si2O8 micro-sized single-crystals incorporating mullite 3Al2O3.2SiO2 nano-sized single-crystals. Modification of the firing parameters and removal of Al from the glazing mixture change essentially the interface extension and the micro-crystals morphology. By comparing archaeological and replica interfaces and considering previous studies, we can now state that Palissy was very likely adding clay (Al) in his frit. Moreover, he was probably working with a firing time of more than 1 h followed by slow cooling in the oven.

2009 ◽  
Vol 15 (5) ◽  
pp. 435-440 ◽  
Author(s):  
Andreja Benčan ◽  
Elena Tchernychova ◽  
Matjaž Godec ◽  
John Fisher ◽  
Marija Kosec

AbstractIn this work we investigated the chemical composition and structure of (K0.5Na0.5)NbO3 (KNN) single crystals grown by the solid state crystal growth method. The optical, scanning, and transmission electron microscopies were employed for the analysis of the chemical homogeneity and domain structure of the KNN crystal. No compositional inhomogeneities within experimental error were encountered in the KNN single crystals. The domain structure of the KNN single crystal, with a monoclinic unit cell, is composed of large 90° domains of up to 100 μm width, which further consist of smaller 180° domains with widths from 50 to 300 nm.


Author(s):  
C.D. Fermin ◽  
M. Igarashi

Otoconia are microscopic geometric structures that cover the sensory epithelia of the utricle and saccule (gravitational receptors) of mammals, and the lagena macula of birds. The importance of otoconia for maintanance of the body balance is evidenced by the abnormal behavior of species with genetic defects of otolith. Although a few reports have dealt with otoconia formation, some basic questions remain unanswered. The chick embryo is desirable for studying otoconial formation because its inner ear structures are easily accessible, and its gestational period is short (21 days of incubation).The results described here are part of an intensive study intended to examine the morphogenesis of the otoconia in the chick embryo (Gallus- domesticus) inner ear. We used chick embryos from the 4th day of incubation until hatching, and examined the specimens with light (LM) and transmission electron microscopy (TEM). The embryos were decapitated, and fixed by immersion with 3% cold glutaraldehyde. The ears and their parts were dissected out under the microscope; no decalcification was used. For LM, the ears were embedded in JB-4 plastic, cut serially at 5 micra and stained with 0.2% toluidine blue and 0.1% basic fuchsin in 25% alcohol.


Author(s):  
R.A. Ploc

Samples of low-nickel Zircaloy-2 (material MLI-788-see(1)), when anodically polarized in neutral 5 wt% NaCl solutions, were found to be susceptible to pitting and stress corrosion cracking. The SEM revealed that pitting of stressed samples was occurring below a 2000Å thick surface film which behaved differently from normal zirconium dioxide in that it did not display interference colours. Since the initial film thickness was approximately 65Å, attempts were made to examine the product film by transmission electron microscopy to deduce composition and how the corrosion environment could penetrate the continuous layer.


Author(s):  
A. Garg ◽  
R. D. Noebe ◽  
R. Darolia

Small additions of Hf to NiAl produce a significant increase in the high-temperature strength of single crystals. Hf has a very limited solubility in NiAl and in the presence of Si, results in a high density of G-phase (Ni16Hf6Si7) cuboidal precipitates and some G-platelets in a NiAl matrix. These precipitates have a F.C.C structure and nucleate on {100}NiAl planes with almost perfect coherency and a cube-on-cube orientation-relationship (O.R.). However, G-phase is metastable and after prolonged aging at high temperature dissolves at the expense of a more stable Heusler (β'-Ni2AlHf) phase. In addition to these two phases, a third phase was shown to be present in a NiAl-0.3at. % Hf alloy, but was not previously identified (Fig. 4 of ref. 2 ). In this work, we report the morphology, crystal-structure, O.R., and stability of this unknown phase, which were determined using conventional and analytical transmission electron microscopy (TEM).Single crystals of NiAl containing 0.5at. % Hf were grown by a Bridgman technique. Chemical analysis indicated that these crystals also contained Si, which was not an intentional alloying addition but was picked up from the shell mold during directional solidification.


Author(s):  
J.G. Wen ◽  
K.K. Fung

Bi-based superconducting phases have been found to be members of a structural series represented by Bi2Sr2Can−1Cun−1On+4, n=1,2,3, and are referred to as 2201, 2212, 2223 phases. All these phases are incommensurate modulated structures. The super space groups are P2/b, NBbmb 2201, 2212 phases respectively. Pb-doped ceramic samples and single crystals and Y-doped single crystals have been studied by transmission electron microscopy.Modulated structures of all Bi-based superconducting phases are in b-c plane, therefore, it is the best way to determine modulated structure and c parameter in diffraction pattern. FIG. 1,2,3 show diffraction patterns of three kinds of modulations in Pb-doped ceramic samples. Energy dispersive X-ray analysis (EDAX) confirms the presence of Pb in the three modulated structures. Parameters c are 3 0.06, 38.29, 30.24Å, ie 2212, 2223, 2212 phases for FIG. 1,2,3 respectively. Their average space groups are all Bbmb.


Author(s):  
P. Fraundorf ◽  
J. Tentschert

Since the discovery of their etchability in the early 1960‘s, nuclear particle tracks in insulators have had a diverse and exciting history of application to problems ranging from the selective filtration of cancer cells from blood to the detection of 244Pu in the early solar system. Their usefulness stems from the fact that they are comprised of a very thin (e.g. 20-40Å) damage core which etches more rapidly than does the bulk material. In fact, because in many insulators tracks are subject to radiolysis damage (beam annealing) in the transmission electron microscope, the body of knowledge concerning etched tracks far outweighs that associated with latent (unetched) tracks in the transmission electron microscope.With the development of scanned probe microscopies with lateral resolutions on the near atomic scale, a closer look at the structure of unetched nuclear particle tracks, particularly at their point of interface with solid surfaces, is now warranted and we think possible. The ion explosion spike model of track formation, described loosely, suggests that a burst of ionization along the path of a charged particle in an insulator creates an electrostatically unstable array of adjacent ions which eject one another by Coulomb repulsion from substitutional into interstitial sites. Regardless of the mechanism, the ejection process which acts to displace atoms along the track core seems likely to operate at track entry and exit surfaces, with the added feature of mass loss at those surfaces as well. In other words, we predict pits whose size is comparable to the track core width.


Author(s):  
H.J. Ryu ◽  
A.B. Shah ◽  
Y. Wang ◽  
W.-H. Chuang ◽  
T. Tong

Abstract When failure analysis is performed on a circuit composed of FinFETs, the degree of defect isolation, in some cases, requires isolation to the fin level inside the problematic FinFET for complete understanding of root cause. This work shows successful application of electron beam alteration of current flow combined with nanoprobing for precise isolation of a defect down to fin level. To understand the mechanism of the leakage, transmission electron microscopy (TEM) slice was made along the leaky drain contact (perpendicular to fin direction) by focused ion beam thinning and lift-out. TEM image shows contact and fin. Stacking fault was found in the body of the silicon fin highlighted by the technique described in this paper.


2020 ◽  
Vol 10 (3) ◽  
pp. 206-212
Author(s):  
Vijeesh Padmanabhan ◽  
Maneesha P. Madhu ◽  
Supriya M. Hariharan

Aim: To study the temperature stability of TGS doped with ZnSO4, CdCl2, BaCl2, and compare it with that of pure TGS. Objectives: Synthesizing pure and doped TGS and studying their temperature dependence using TGA, DTA, and DSC analysis. Methods: Slow cooling solution growth was used to grow single crystals of pure and doped TGS. The TGA, DTA and DSC analysis was conducted for determining the temperature stability. Results: The thermal analysis of pure and doped TGS shows that the doped samples show a similar dependence on temperature as pure TGS. The temperature of decomposition of pure and doped samples (BTGS, ZTGS, CdTGS) was 226.60°C, 228.38°C, 229.13°C, and 239.13°C respectively. The melting onset of these samples was 214.51°C, 216.04°C, 217.69°C and 216.04°C respectively. Conclusion: The study shows that doping TGS with the above three described materials did not alter their temperature stability considerably. It is a good result as doping TGS, for varying its characteristics like absorbance, reflectance, bandgap energy, etc., which did not alter its temperature stability. Therefore, TGS doped with the above three dopants can be used at the same temperature ranges as of pure TGS but with much-improved efficiency.


Author(s):  
Eric O'Quinn ◽  
Cameron Tracy ◽  
William F. Cureton ◽  
Ritesh Sachan ◽  
Joerg C. Neuefeind ◽  
...  

Er2Sn2O7 pyrochlore was irradiated with swift heavy Au ions (2.2 GeV), and the induced structural modifications were systematically examined using complementary characterization techniques including transmission electron microscopy (TEM), X-ray diffraction...


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