scholarly journals A rapid method of cryofixation of tissues in situ for ultracryomicrotomy.

1980 ◽  
Vol 28 (1) ◽  
pp. 47-51 ◽  
Author(s):  
S H Chang ◽  
W J Mergner ◽  
R E Pendergrass ◽  
R E Bulger ◽  
I K Berezesky ◽  
...  

A device is described for the rapid freezing of tissue in situ by a punch biopsy approach using a specially designed cryogun with a highly thermal conductive specimen holder. The cryogun consists of a sampling device using a double, spring-loaded gun mechanism and a system of cryochambers. Ultrathin freeze-dried sections cut from samples obtained with this cryogun are relatively free of artifacts and have few ice crystals. Organelles are seen by natural contrast when cryosections of approximately 1000 A are observed with a transmission electron microscope or in the transmission mode of a scanning electron microscope. The construction of the cryogun is described along with a method of obtaining improved, ultrafast cryofixation of tissue specimens. The reliability of obtaining x-ray microanalysis measurements of diffusible ions where movement within cell compartments has been retained is discussed.

2014 ◽  
Vol 20 (4) ◽  
pp. 1038-1045 ◽  
Author(s):  
Christian D. Damsgaard ◽  
Henny Zandbergen ◽  
Thomas W. Hansen ◽  
Ib Chorkendorff ◽  
Jakob B. Wagner

AbstractSpecimen transfer under controlled environment conditions, such as temperature, pressure, and gas composition, is necessary to conduct successive complementary in situ characterization of materials sensitive to ambient conditions. The in situ transfer concept is introduced by linking an environmental transmission electron microscope to an in situ X-ray diffractometer through a dedicated transmission electron microscope specimen transfer holder, capable of sealing the specimen in a gaseous environment at elevated temperatures. Two catalyst material systems have been investigated; Cu/ZnO/Al2O3 catalyst for methanol synthesis and a Co/Al2O3 catalyst for Fischer–Tropsch synthesis. Both systems are sensitive to ambient atmosphere as they will oxidize after relatively short air exposure. The Cu/ZnO/Al2O3 catalyst, was reduced in the in situ X-ray diffractometer set-up, and subsequently, successfully transferred in a reactive environment to the environmental transmission electron microscope where further analysis on the local scale were conducted. The Co/Al2O3 catalyst was reduced in the environmental microscope and successfully kept reduced outside the microscope in a reactive environment. The in situ transfer holder facilitates complimentary in situ experiments of the same specimen without changing the specimen state during transfer.


2014 ◽  
Vol 20 (2) ◽  
pp. 323-329 ◽  
Author(s):  
Nestor J. Zaluzec ◽  
M. Grace Burke ◽  
Sarah J. Haigh ◽  
Matthew A. Kulzick

AbstractThe use of analytical spectroscopies during scanning/transmission electron microscope (S/TEM) investigations of micro- and nano-scale structures has become a routine technique in the arsenal of tools available to today’s materials researchers. Essential to implementation and successful application of spectroscopy to characterization is the integration of numerous technologies, which include electron optics, specimen holders, and associated detectors. While this combination has been achieved in many instrument configurations, the integration of X-ray energy-dispersive spectroscopy and in situ liquid environmental cells in the S/TEM has to date been elusive. In this work we present the successful incorporation/modifications to a system that achieves this functionality for analytical electron microscopy.


1997 ◽  
Vol 82 (3-4) ◽  
pp. 302-309 ◽  
Author(s):  
Alistair R. Lennie ◽  
Simon A. T. Redfern ◽  
Pamela E. Champness ◽  
Chris P. Stoddart ◽  
Paul F. Schofield ◽  
...  

2006 ◽  
Vol 05 (02n03) ◽  
pp. 245-251 ◽  
Author(s):  
JUNPING LI ◽  
YAO XU ◽  
DONG WU ◽  
YUHAN SUN

ZnS nanofibers with lamellar mesostructure could be built up from in situ generated ZnS precursors via hydrothermal routes using neutral n-alkylamines as structure-directing template and ethylene diamine tetraacetic acid (EDTA) as stabilizer. The morphology and structure of the obtained products were thoroughly investigated via scanning electron microscope (SEM), energy dispersive analysis of X-rays (EDX), transmission electron microscope (TEM), X-ray powder diffraction (XRD) and thermal analyses. HRTEM and XRD results revealed that the so-produced nanofibers were lamellar mesostructure and its framework was built of crystalline wurtzite ZnS . It was also found that the distance between the layers was proportional to the chain length of the alkylamine. The UV-visible absorption spectrum showed that the nanofibers exhibited strong quantum-confined effect with a blue shift in the band gap. Finally, a probable mechanism for the assembly of the nanofibers was also proposed.


Author(s):  
M.L. McDonald ◽  
J.M. Gibson

Interest in ultrahigh vacuum (UHV) specimen environments in the transmission electron microscope (TEM) has grown considerably in recent years. The possibility of in-situ studies of atomically clean surfaces has been demonstrated by Yagi et.al., Wilson & Petroff & others. Most designs have involved a side entry specimen holder with cryopumping in the pole piece and are not easily compatible with ultrahigh resolution(UHR) due to size and stability requirements. We have designed a differentially pumped UHV specimen chamber for the JEOL 200CX (UHRTEM). It is intended to allow examination of clean thin specimens at pressures below 10-9 torr with a point to point resolution of 2.5 Å. Provisions for in-situ heating, cooling & deposition have been made. A unique part of this design is the relatively large volume sample chamber held at UHV (figsl&2). This design allows characterization of the atmosphere to which the sample is exposed & cleaning & preparation of samples out of the pole piece which is believed to be necessary for UHRTEM. Another possibility with this design is the transfer of a sample into the TEM from other chambers by use of a transfer case without exposing the sample to an atmosphere above 10-9 torr. Extra ports have been provided to accommodate future experiments.


Author(s):  
C. A. Ackerley ◽  
L. E. Becker

Although a small degree of mineralization can be a common occurrence without associated pathological symptoms, certain diseases of the brain do however exhibit distinct increases in mineralization with characteristic distributions l>2. In this study, tissues from a number of these disorders were prepared for x-ray microanalysis in several ways. Where possible, material was slam frozen on a liquid nitrogen cooled polished copper block, cryosections prepared and freeze dried in the scanning transmission electron microscope (STEM) using a cold stage prior to analysis by energy dispersive x-ray spectrometry (EDS). In addition, samples were freeze substituted for several days, embedded in LR white and cut on dry knives before analysis. Where only formalin fixed paraffin embedded materials were available, .5μ.m sections were cut and mounted on carbon planchets. The specimens were then deparaffinized with xylene and viewed with the backscatter electron detector (BEI) in the scanning electron microscope (SEM) and analyzed by EDS.


Catalysts ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 952 ◽  
Author(s):  
Huiyuan Xue ◽  
Xingxing Gong ◽  
Jingjing Xu ◽  
Rongrong Hu

The in-situ hydrodeoxygenation of bio-derived phenol is an attractive routine for upgrading bio-oils. Herein, an active trimetallic Ni-Cu-Co/Al2O3 catalyst was prepared and applied in the in-situ hydrodeoxygenation of bio-derived phenol. Comparison with the monometallic Ni/Al2O3 catalyst and the bimetallic Ni-Co/Al2O3 and Ni-Cu/Al2O3 catalysts, the Ni-Cu-Co/Al2O3 catalyst exhibited the highest catalytic activity because of the formation of Ni-Cu-Co alloy on the catalyst characterized by using X-ray powder diffraction (XRD), temperature programmed reduction (TPR), N2 physisorption, scanning electron microscope (SEM), and transmission electron microscope (TEM). The phenol conversion of 100% and the cyclohexane yield of 98.3% could be achieved in the in-situ hydrodeoxygenation of phenol at 240 °C and 4 MPa N2 for 6 h. The synergistic effects of Ni with Cu and Co of the trimetallic Ni-Cu-Co/Al2O3 catalyst played a significant role in the in-situ hydrodeoxygenation process of phenol, which not only had a positive effect on the production of hydrogen but also owned an excellent hydrogenolysis activity to accelerate the conversion of cyclohexanol to cyclohexane. Furthermore, the catalyst also exhibited excellent recyclability and good potential for the upgrading of bio-oils.


Author(s):  
Roy H. Geiss ◽  
William A. Jesser

An Ortec Si(Li) energy dispersive X-ray detector designed for use on a Cambridge scanning electron microscope has been coupled to a Siemens transmission electron microscope by replacing the side tilt control on the Siemens by a brass tube as shown in figure 1. The Siemens specimen holder was modified to tilt the specimen approximately 20° from a horizontal position and to elevate it such that it is just visible to the detector through the side port. This increased specimen height requires an objective focal length of greater than 8 mm and consequently effects a lower resolution of the image, especially at low accelerating voltages. The peak/background in the X-ray spectra is best at 40kV, however, and deteriorates progressively with increasing accelerating voltage.Experiments similar to those of Fuchs, who employed a wavelength dispersive system on a Siemens TEM to measure film thickness, were repeated with the present energy dispersive system by analysing spectra from vacuum deposited gold films of various thicknesses. A linear relation between peak height and thickness was confirmed for several films up to 2000Å thick by comparing spectra from two adjacent grid squares, one covered by a single thickness of gold, the other covered by a double thickness, and noting that the peak heights were in the ratio of 1:2 to within a few percent.


MRS Bulletin ◽  
1994 ◽  
Vol 19 (6) ◽  
pp. 17-21 ◽  
Author(s):  
Frances M. Ross

This issue of the MRS Bulletin aims to highlight the innovative and exciting materials science research now being done using in situ electron microscopy. Techniques which combine real-time image acquisition with high spatial resolution have contributed to our understanding of a remarkably diverse range of physical phenomena. The articles in this issue present recent advances in materials science which have been made using the techniques of transmission electron microscopy (TEM), including holography, scanning electron microscopy (SEM), low-energy electron microscopy (LEEM), and high-voltage electron microscopy (HVEM).The idea of carrying out dynamic experiments involving real-time observation of microscopic phenomena has always had an attraction for materials scientists. Ever since the first static images were obtained in the electron microscope, materials scientists have been interested in observing processes in real time: we feel that we obtain a true understanding of a microscopic phenomenon if we can actually watch it taking place. The idea behind “materials science in the electron microscope” is therefore to use the electron microscope—with its unique ability to image subtle changes in a material at or near the atomic level—as a laboratory in which a remarkable variety of experiments can be carried out. In this issue you will read about dynamic experiments in areas such as phase transformations, thin-film growth, and electromigration, which make use of innovative designs for the specimen, the specimen holder, or the microscope itself. These articles speak for themselves in demonstrating the power of real-time analysis in the quantitative exploration of reaction mechanisms.The first transmission electron microscopes operated at low accelerating voltages, up to about 100 kV. This placed a severe limitation on the thickness of foils that could be examined: Heavy elements, for example, had to be made into foils thinner than 0.1 μm. It was felt that any phenomenon whose “mean free path” was comparable to the foil thickness would be significantly affected by the foil surfaces, and therefore would be unsuitable for study in situ. However, technology quickly generated ever higher accelerating voltages, culminating in the giant 3 MeV electron microscopes. At these voltages, electrons can penetrate materials as thick as 6–9 μm for light elements such as Si and Al, and 1 μm for very heavy ones such as Au and U.


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