The Small Angle Cleavage Technique for XTEM Sample Preparation

1998 ◽  
Vol 4 (S2) ◽  
pp. 866-867
Author(s):  
S. D. Walck ◽  
J. P. McCaffrey

The Small Angle Cleavage Technique (SACT) is a relatively simple and inexpensive method of producing superior cross sectional TEM specimens. For speed of preparation, it is unsurpassed; for example, ten samples can easily be prepared in about an hour from a typical material. It is particularly well suited for rapidly examining coatings and thin films very soon after they have been deposited. A major limitation of the technique is that it does require the substrate material to cleave or fracture. For this reason, it has been applied almost exclusively to semiconductor materials, but the technique has been extended quite successfully to other substrates such as glass, silicon carbide, quartz, sapphire, and other hard materials. Several procedures have been added or modified to the original technique developed by McCaffrey that makes it much easier to get started in using the technique. A detailed pictorial outline of the technique has been described elsewhere by the authors.

1997 ◽  
Vol 480 ◽  
Author(s):  
Scott D. Walck ◽  
John P. McCaffrey

AbstractThe Small Angle Cleavage Technique is a relatively simple and inexpensive method of producing superior cross sectional TEM specimens. For speed of preparation, it is unsurpassed. One limitation is that the technique does require the substrate material to cleave or fracture. For this reason, it has been applied almost exclusively to semiconductor materials. Recently, the technique has been extended to other substrates such as glass, silicon carbide, quartz, sapphire, and other hard materials. It is particularly well suited for rapidly examining coatings and thin films very soon after they are deposited. Several procedures have been added or modified to the original technique developed by McCaffrey to simplify the technique. The steps are presented in a detailed pictorial outline form. A method for mounting the cleaved samples utilizing a commercially available grid is presented. In addition, the advantages that the special geometry of the prepared samples have when mounted properly in a double-tilt holder are discussed with respect to the angular range of tilting experiments that are now possible in the TEM.


Author(s):  
Pamela F. Lloyd ◽  
Scott D. Walck

Pulsed laser deposition (PLD) is a novel technique for the deposition of tribological thin films. MoS2 is the archetypical solid lubricant material for aerospace applications. It provides a low coefficient of friction from cryogenic temperatures to about 350°C and can be used in ultra high vacuum environments. The TEM is ideally suited for studying the microstructural and tribo-chemical changes that occur during wear. The normal cross sectional TEM sample preparation method does not work well because the material’s lubricity causes the sandwich to separate. Walck et al. deposited MoS2 through a mesh mask which gave suitable results for as-deposited films, but the discontinuous nature of the film is unsuitable for wear-testing. To investigate wear-tested, room temperature (RT) PLD MoS2 films, the sample preparation technique of Heuer and Howitt was adapted.Two 300 run thick films were deposited on single crystal NaCl substrates. One was wear-tested on a ball-on-disk tribometer using a 30 gm load at 150 rpm for one minute, and subsequently coated with a heavy layer of evaporated gold.


2004 ◽  
Vol 810 ◽  
Author(s):  
W. Skorupa ◽  
D. Panknin ◽  
M. Voelskow ◽  
W. Anwand ◽  
T. Gebel ◽  
...  

ABSTRACTThe use of flash lamp annealing for processing semiconductor materials is outlined. Specific applications include ultra-shallow junction formation and heteroepitaxial growth of improved quality thin films of cubic silicon carbide. It is demonstrated that flash lamp annealing holds great promise as a technique for fabricating novel devices.


1997 ◽  
Vol 12 (8) ◽  
pp. 1935-1938 ◽  
Author(s):  
J. R. LaGraff ◽  
J. M. Murduck

A new essentially nondestructive cross-sectional method is described for measuring the individual thicknesses of multilayer YBa2Cu3O7 (YBCO) and SrTiO3 (STO) thin films using off-axis ion milling and the atomic force microscope (AFM). Since the ion-milling is done during routine patterning of a thin-film device and the AFM requires only a small area for imaging, no additional sample preparation is required. This is a significant improvement over traditional cross-sectional techniques which often require lengthy and destructive sample preparation. Also, there is no a priori reason that this technique would not be amenable to other multilayer thin-film systems.


1985 ◽  
Vol 46 ◽  
Author(s):  
C.H. Carter ◽  
J.A. Edmond ◽  
J.W. Palmour ◽  
J. Ryu ◽  
H.J. Kim ◽  
...  

AbstractTechniques have been developed at NCSU for fabricating cross-sectional transmission electron microscopy (XTEM) foils from monocrystalline beta silicon carbide thin films grown by chemical vapor deposition. The results of the TEM observations are utilized to discern the efficacy of the various processing parameters in terms of film quality and defect structure as well as oxidation, ion implantation and annealing procedures.


Author(s):  
Kim Ostreicher ◽  
Changmo Sung

Hard materials such as tungsten carbides which contain ceramic protective coatings (from 30 nm to several microns in thickness) present unique electron-transparent sample preparation challenges for TEM observations. A cross-sectional sample would allow one to observe the coating, matrix and related interface between the two. Variations in the hardness as well as differences in the compositions of the coating and substrate make this preparation more difficult. Discs of the material cannot simply be core drilled out and mechanically or ion beam prepared since it is the surface or edge of the material containing the coating which must be retained. Ion milling also causes preferential removal of one phase in relation to others leaving a sample which is not uniformly thin or truly representative of the microstructure. A preparation technique used for many semiconductor materials involves gluing together pieces with surface layers or coatings thus forming a stack which can be further processed to yield thin, electron transparent specimens.


1997 ◽  
Vol 480 ◽  
Author(s):  
Suli Suder ◽  
C. A. Faunce ◽  
S. E. Donnelly

AbstractVarious small-angle wedge two-view samples have been prepared by a small-angle cleavage technique using hand tools and examined by transmission electron microscopy. Cleaved wedges from the same material are mounted both as plan-view and cross-sectional samples on the same TEM specimen grid allowing convenient examination in both views. Samples of Si3N4, Zr, Co and TiN/CN/TiN films deposited on Si, and He ion implanted Si prepared by this technique are shown to be suitable for analysis in the TEM.


1990 ◽  
Vol 183 ◽  
Author(s):  
T. E. Mitchell ◽  
S. N. Basu ◽  
M. Nastasi ◽  
T. Roy

AbstractThin films of YBa2Cu3O7 have been prepared by evaporation of Cu, Y and BaF2 onto (001) SrTiO3, LaGaO3. and LaAlO3 and subsequent annealing. Their microstructures have been examined by HREM of cross-sectional specimens. Epitaxial (001) grains of YBa2Cu3O7 form near the substrate interface in thin films but (001) and (010) grains tend to nucleate as the film thickens. 90° grain boundaries are therefore common, as well as other defects such as small-angle boundaries, dislocations and stacking faults. HREM of the substrate/superconductor interface indicates regions of perfect epitaxy, highly distorted areas, amorphous regions and areas showing evidence of interdiffusion. The relationship of these microstructural features to critical current density is discussed.


Author(s):  
Karren L. More

Beta-SiC is an ideal candidate material for use in semiconductor device applications. Currently, monocrystalline β-SiC thin films are epitaxially grown on {100} Si substrates by chemical vapor deposition (CVD). These films, however, contain a high density of defects such as stacking faults, microtwins, and antiphase boundaries (APBs) as a result of the 20% lattice mismatch across the growth interface and an 8% difference in thermal expansion coefficients between Si and SiC. An ideal substrate material for the growth of β-SiC is α-SiC. Unfortunately, high purity, bulk α-SiC single crystals are very difficult to grow. The major source of SiC suitable for use as a substrate material is the random growth of {0001} 6H α-SiC crystals in an Acheson furnace used to make SiC grit for abrasive applications. To prepare clean, atomically smooth surfaces, the substrates are oxidized at 1473 K in flowing 02 for 1.5 h which removes ∽50 nm of the as-grown surface. The natural {0001} surface can terminate as either a Si (0001) layer or as a C (0001) layer.


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