Articles written in Bulletin of Materials Science
Volume 6 Issue 2 May 1984 pp 129-149 Preparative And Characterization
This paper reviews four major equipment developed at the National Physical Laboratory for growth and perfection evaluation of single crystals, namely (i) a crystal puller for growth of nearly perfect crystals by the Czochralski method; (ii) a microfocus x-ray generator; (iii) an x-ray diffraction topography camera; and (iv) a triple crystal x-ray diffractometer. The crystal puller can provide smooth, uniform and variable pulling rates. The maximum length of pull is nearly 60cm. Efforts have been made to isolate vibrations. Nearly perfect single crystals of KCl, KBr and NaCl with maximum diameter of ∼ 60 mm have been grown. The crystals give diffraction curves with half width in the range of 10–30 sec of arc. In the projection topographs, dislocations can be resolved and characterized. The microfocus x-ray generator is a demountable continuously evacuated system with specially designed electron gun and anode assembly. The vacuum is continuously monitored for ease of maintenance. In the point focus mode the spot size is 40 µm on the anode. X-ray topography system is a versatile equipment used for projection and section topography. It can provide 360° rotations to the specimen disc around an axis perpendicular to it. Rotations of a few sec of arc can be given to the specimen around a vertical axis. Typical diffraction curves of a dislocation-free crystal and a crystal with boundaries are shown. Well-resolved images of dislocations are shown in a topograph as an illustration. In the triple crystal x-ray diffractometer a highly collimated and monochromated Kα1 exploring x-ray beam is obtained by combining microfocus source, a special collimator and crystal monochromators of Bonse-Hart type. With this beam very narrow diffraction curves with half width of about 5 sec of arc can be recorded. Typical results of measurement of diffuse x-ray scattering (
Volume 16 Issue 6 December 1993 pp 617-642
Real structure together with composition and elemental purity of single crystals controls their properties. This paper reviews recent work carried out at the National Physical Laboratory on application of high resolution X-ray diffractometry, topography and diffuse X-ray scattering for direct observation and characterization of real structure of single crystals of silicon, gallium arsenide, diamond and LiNbO3. A series of six multicrystal X-ray diffractometers have been designed, developed and fabricated indigenously. The most versatile of these systems is a five crystal X-ray diffractometer with state-of-the-art level resolution. These techniques and equipments have been applied in studying several interesting problems. Even in dislocation-free crystals of silicon, remarkable differences in the defect structure have been observed if the growth method was changed from float zone to Czochralski. Study of effect of externally applied electric fields and ion implantation on real structure of crystals has yielded interesting results. Images of ‘filaments’ which show nonhomogeneous distribution of electric current through semiconductors and insulators have been recorded for the first time in high resolution traverse topographs. Diffracted X-ray intensities could be modified by externally applied electric fields. It has been shown that implantation of BF2+ ions in silicon for producing shallow junctions does not produce homogeneous distribution of boron. The impurity is partially in clustered form. Biaxial stress introduced by thin depositions in substrate crystals are of considerable applied concern. The value and nature of stress have been determined in a number of systems. Typical results obtained on GaAs: multilayer metallizations are described. Also, degradation of perfection of substrates has been monitored. This work has shown that the stress is not homogeneously distributed and is quite anisotropic. A new high resolution X-ray diffraction technique has been developed for direct observation and study of forward diffracted X-ray beam and anomalous transmission of X-rays through ‘thin’ diamond crystals of varying degrees of perfection.
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