Minimally Invasive (ENERGY) Dispersive Analytical Spectroscopy (MIDAS). The Golden Touch for In-Situ X-Ray Microanalysis of Bulk Bio-Organic Samples

1999 ◽  
Vol 5 (S2) ◽  
pp. 574-575
Author(s):  
Patrick Echlin

The matrix of bio-organic samples is composed primarily of carbon, hydrogen, oxygen and nitrogen. Dispersed within this matrix there is a wide spectrum of other elements whose local concentration can be measured in situ by x-ray spectroscopy. The analysis continues to present a challenge because most samples are highly hydrated, beam sensitive and of low density. In light of these restrictions there is only one sensible approach to the use of an analytical procedure which depends on the intereaction of high energy beam electrons with a labile specimen. Samples must be prepared by the least invasive preparative procedure and irradiated with the minimum amount of energy in order to obtain the maximun amount of chemical information. Low temperature sample preparation and low voltage electron beam instruments are central to these processes. By way of example, a brief description will be given of an on-going biological investigation which makes full use of these processes.

2021 ◽  
Vol 52 (5) ◽  
pp. 1812-1825
Author(s):  
Sen Lin ◽  
Ulrika Borggren ◽  
Andreas Stark ◽  
Annika Borgenstam ◽  
Wangzhong Mu ◽  
...  

AbstractIn-situ high-energy X-ray diffraction experiments with high temporal resolution during rapid cooling (280 °C s−1) and isothermal heat treatments (at 450 °C, 500 °C, and 550 °C for 30 minutes) were performed to study austenite decomposition in two commercial high-strength low-alloy steels. The rapid phase transformations occurring in these types of steels are investigated for the first time in-situ, aiding a detailed analysis of the austenite decomposition kinetics. For the low hardenability steel with main composition Fe-0.08C-1.7Mn-0.403Si-0.303Cr in weight percent, austenite decomposition to polygonal ferrite and bainite occurs already during the initial cooling. However, for the high hardenability steel with main composition Fe-0.08C-1.79Mn-0.182Si-0.757Cr-0.094Mo in weight percent, the austenite decomposition kinetics is retarded, chiefly by the Mo addition, and therefore mainly bainitic transformation occurs during isothermal holding; the bainitic transformation rate at the isothermal holding is clearly enhanced by lowered temperature from 550 °C to 500 °C and 450 °C. During prolonged isothermal holding, carbide formation leads to decreased austenite carbon content and promotes continued bainitic ferrite formation. Moreover, at prolonged isothermal holding at higher temperatures some degenerate pearlite form.


2021 ◽  
Vol 800 ◽  
pp. 140249
Author(s):  
Juan Macchi ◽  
Steve Gaudez ◽  
Guillaume Geandier ◽  
Julien Teixeira ◽  
Sabine Denis ◽  
...  

2010 ◽  
Vol 504 ◽  
pp. S155-S158 ◽  
Author(s):  
J. Bednarcik ◽  
C. Curfs ◽  
M. Sikorski ◽  
H. Franz ◽  
J.Z. Jiang

2011 ◽  
Vol 21 (15) ◽  
pp. 5604 ◽  
Author(s):  
Zonghai Chen ◽  
Yang Ren ◽  
Yan Qin ◽  
Huiming Wu ◽  
Shengqian Ma ◽  
...  

2000 ◽  
Vol 639 ◽  
Author(s):  
Ryuhei Kimura ◽  
Kiyoshi Takahashi ◽  
H. T. Grahn

ABSTRACTAn investigation of the growth mechanism for RF-plasma assisted molecular beam epitaxy of cubic GaN films using a nitrided AlGaAs buffer layer was carried out by in-situ reflection high energy electron diffraction (RHEED) and high resolution X-ray diffraction (HRXRD). It was found that hexagonal GaN nuclei grow on (1, 1, 1) facets during nitridation of the AlGaAs buffer layer, but a highly pure, cubic-phase GaN epilayer was grown on the nitrided AlGaAs buffer layer.


2007 ◽  
Vol 29-30 ◽  
pp. 143-146 ◽  
Author(s):  
Aamir Mukhtar ◽  
De Liang Zhang ◽  
C. Kong ◽  
P. R. Munroe

Cu-(2.5 or 5.0vol.%)Al2O3 nanocomposite balls and granules and Cu-(2.5vol.% or 5.0vol.%)Pb alloy powder were prepared by high energy mechanical milling (HEMM) of mixtures of Cu and either Al2O3 or Pb powders. It was observed that with the increase of the content of Al2O3 nanoparticles from 2.5vol.% to 5vol.% in the powder mixture, the product of HEMM changed from hollow balls into granules and the average grain size and microhardness changed from approximately 130nm and 185HV to 100nm and 224HV, respectively. On the other hand, HEMM of Cu–(2.5 or 5.0vol.%) Pb powder mixtures under the same milling conditions failed to consolidate the powder in-situ. Instead, it led to formation of nanostructured fine powders with an average grain size of less than 50nm. Energy dispersive X-ray mapping showed homogenous distribution of Pb in the powder particles in Cu–5vol.%Pb alloy powder produced after 12 hours of milling. With the increase of the Pb content from 2.5 to 5.0 vol.%, the average microhardness of the Cu-Pb alloy powder particles increases from 270 to 285 HV. The mechanisms of the effects are briefly discussed.


2015 ◽  
Vol 112 (52) ◽  
pp. 15803-15808 ◽  
Author(s):  
Ofer Hirsch ◽  
Kristina O. Kvashnina ◽  
Li Luo ◽  
Martin J. Süess ◽  
Pieter Glatzel ◽  
...  

The lanthanum-based materials, due to their layered structure and f-electron configuration, are relevant for electrochemical application. Particularly, La2O2CO3 shows a prominent chemoresistive response to CO2. However, surprisingly less is known about its atomic and electronic structure and electrochemically significant sites and therefore, its structure–functions relationships have yet to be established. Here we determine the position of the different constituents within the unit cell of monoclinic La2O2CO3 and use this information to interpret in situ high-energy resolution fluorescence-detected (HERFD) X-ray absorption near-edge structure (XANES) and valence-to-core X-ray emission spectroscopy (vtc XES). Compared with La(OH)3 or previously known hexagonal La2O2CO3 structures, La in the monoclinic unit cell has a much lower number of neighboring oxygen atoms, which is manifested in the whiteline broadening in XANES spectra. Such a superior sensitivity to subtle changes is given by HERFD method, which is essential for in situ studying of the interaction with CO2. Here, we study La2O2CO3-based sensors in real operando conditions at 250 °C in the presence of oxygen and water vapors. We identify that the distribution of unoccupied La d-states and occupied O p- and La d-states changes during CO2 chemoresistive sensing of La2O2CO3. The correlation between these spectroscopic findings with electrical resistance measurements leads to a more comprehensive understanding of the selective adsorption at La site and may enable the design of new materials for CO2 electrochemical applications.


2021 ◽  
Vol 118 (13) ◽  
pp. 132903
Author(s):  
Mao-Hua Zhang ◽  
Changhao Zhao ◽  
Lovro Fulanović ◽  
Jürgen Rödel ◽  
Nikola Novak ◽  
...  

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