Single crystal samples

Most fiindamental surface science investigations employ single-crystal samples cut along a low-index plane. The single-crystal surface is prepared to be nearly atomically flat. The surface may also be modified in vacuum. For example, it may be exposed to a gas that adsorbs (sticks) to the surface, or a film can be grown onto a sample by evaporation of material. In addition to single-crystal surfaces, many researchers have investigated vicinal, i.e. stepped, surfaces as well as the surfaces of polycrystalline and disordered materials. 

Figure Bl.24.10. Random and aligned (chaimelled) backscattering spectrum from a single crystal sample of silicon. The aligned spectrum has a peak at the high energy end of the Si signal. This peak represents helium...

The total cerium content in the single crystal samples on the basis of rare-earth elements is determined by photometry after Ce(III) oxidation by ammonium persulfate. The Ce(III) content is calculated from the difference. Comparison of the determination results of the total cerium content obtained by photometric and atomic emission methods for Li GdlBO ljiCe demonstrated the elaborated procedure precision and systematic error absence. 

Single-crystal samples of conductors best other solid samples are suitable, including polycrystalline metals, polymeric materials, semiconductors, and insulators, ultrahigh vacuum compatible typically > 5 mm diameter, 1-3 mm thick... 

In the following discussion, heavy emphasis is made of examples from studies of adsorbed layers on metal single-crystal samples. These illustrate the power of the HREELS technique and represent the main use of HREELS historically. Certainly HREELS has been used outside of the single-crystal world, and mention is made concerning its use on practical materials. This latter use of HREELS represents a true frontier. 

In addition to elemental compositional information, RBS also can be used to study the structure of single-crystal samples. When a sample is channeled, the rows of atoms in the lattice are aligned parallel to the incident He ion beam. The bombard-... 

The studies of ammonia synthesis over Fe and Re and the hydrodesulfurization of thiophene over Mo, described above, illustrate the importance and success of our approach of studying catalysis over single crystal samples at high pressures. The use of surfaces having a variety of orientations allows the study of reactions that are surface structure sensitive 6Uid provides insight into the nature of the catalytic site. Here we have shown that the ammonia synthesis... 

Faiz et al. (1996) have applied micro-PIXE analysis to study solute distributions in a single crystal sample of YiBa2Cu307 5 high temperature superconductor (YBCO) of dimensions 1.3 mm x 1.5 mm x 75 pm. It contained a small secondary crystal overgrowth of dimensions 340 x 340 x 100 pm3. The interface region between the smaller crystal and the base crystal was covered with a material which appeared to be residual flux. The instrument employed a 2.5 MeV focused proton beam of about 4 pm resolution, which could scan an area of 500 x 500 pm2 on the sample surface. The microbeam current was kept low (typically about 30 pA) to avoid any damage to the sample. 

Figure 18 (A) (top) A single-scan H NMR spectrum in a single crystal sample of...

Figure 19 (A) A H magic-sandwich echo spectrum of a single crystal sample of 98.3%-...

Finally, we note that, to the best of our knowledge, only one report exists about EPR spectra of non-Kramers lanthanide ions in molecular magnets. In 2012, Hill and coworkers [51] performed a multifrequency study on powder and single crystal samples of NagHofWgOj H20, in both the pure form and when doped into the isostructural Y3+ derivative. While crystallizing in a triclinic unit cell, the symmetry of the lanthanide ion in this family is very close to Did. For this reason, susceptibility data had been previously fitted by a purely axial Hamiltonian [50]. 

Over 97% of the ions in a beam can be channeled in a crystal. This figure can be achieved for a well-collimated beam of MeV light ions, for which dmin is of order 0.1 A, directed along a low-index direction onto a single crystal sample. Typically, the sample is mounted on a goniometer which allows different low-index directions to be brought parallel to the beam during an experiment. The 2 or 3% of nonchanneled ions are those that hit the ends of the atomic rows at the surface or are scattered from surface disorder. 

In systems from which only a polycrystalline or an amorphous sample can be obtained, NMR becomes the method of choice since the diffraction technique requires single crystal samples. 

As with neutron powder methods, both monochromatic and time-of-flight (Laue) techniques have been used for single-crystal neutron studies. Such studies are much less numerous, however, as a result of the difficulty of compressing suitably sized (>1 mm ) single-crystal sample to the required pressure while maintaining the crystal quality. The piston cylinder cell design of Me Whan and others [128] has been used at the ILL reactor source for a number of neutron structural studies to... 

X-ray Diffraction Structural characterization of single crystal samples can reveal both the atomic arrangement and the composition of a sample. The unit cell size and symmetry alone can quickly establish whether a crystal is a known material or a new phase. A detailed discussion of X-ray diffraction studies of the known superconductors is the topic of another chapter in this book. 

---