Crystallinity thermal treatment

The small (10 -lm) coating particles are typically aluminum oxide [1344-28-1/, Al O. These particles can have BET surface areas of 100 to 300 m /g. The thermal and physical properties of alumina crystalline phases vary according to the starting phase (aluminum hydroxide or hydrate) and thermal treatment (see ALUMINUM COMPOUNDS, ALUMINUM OXIDE). 

Thus, tantalum and niobium hydroxides are converted into oxides following a two-step thermal treatment. The first step is usually performed at relatively low temperatures in the range of 100-200°C in order to dry the wet precursors. The second thermal treatment brings about the decomposition of hydroxides, removes the rest of the water and converts the material into crystalline oxides. The second thermal treatment is usually performed at temperatures as high as 900-1000°C. 

Alumina is not widely used in modem HPLC [48]. Porous gamma alumina is prepared by dehydration and thermal treatment of crystalline bayerite [8,49]. It is available in several types with pore diameters from 6-lS nm, surface areas 70-250 m /g and pore volumes 0.2-0.3 ml/g. After conditioning with acid or base its apparent surface pH can be adjusted between pH 3-9. The alumina surface is more heterogeneous than silica containing both hydroxyl... 

Zinc hydroxy double salts are layered materials similar to layered double hydroxides which show intercrystalline reactivity and incorporate organic compounds between layers.337 Hydroxy double salts of high crystallinity can be obtained by reacting ZnO with organic metal salts in water. Zinc oxide crystals could then be prepared by thermal treatment of hydroxy zinc acetate.338... 

The thermally expanded graphite was used without any preliminary treatment the carbon was synthesized by carbonation of the raw material in an argon flow at 500°C with subsequent thermal treatment. Carbon residues strongly differing in the crystallinity degree were obtained as depends on the temperature which ranged from 500°C to 1300°C. The identity of each material was checked by X-ray spectroscopy. 

The phase transition from amorphous to crystalline can sometimes be promoted by thermal treatment (annealing) [ 1.45]. In a laboratory scale, this can be done relatively simple. In a production scale the process must be proven as reproducible and reliable by a validation process, which is time consuming. It is therefore recommended, that a search for CPAs and process conditions, which would lead to crystallization be carried out, using methods such as DTA, DSC, ER and DRS (see Section 1.1.5) also see Yarwood [1.46. If this is not successful, time and temperature for TT should be chosen in such away, that the tolerances for time and temperature are not to narrow, e. g. -24.0 °C 0.5 °C and 18 min 1 min are difficult to operate, while -30 °C 1.5 °C and 40 min 2 min might be easier to control. 

Other antibiotics still require freeze drying, e. g. Na-Cephalotin (Na-CET). Takeda [ 1.32] showed, that thermal treatment of Na-CET was not sufficient to produce pure crystalline Na-CET, as the amorphous fraction discolors during storage and must be avoided. Takeda described the production of pure crystalline Na-CET by adding microcrystals of Na-CET to a saturated solution of Na-CET. If this mixture was frozen and freeze dried, then no amorphous or quasi-crystalline were found. Koyama et al. [3.35] described, that after thermal treatment for 24 h some parts remained incompletely crystallized. After adding 5 % (w/w) isopropylalcohol, a thermal treatment of 1 h was sufficient. Furthermore, the product could be dried at a higher pressure. Thus the drying time could be reduced and 100 % of the product could be used. 

X-ray diffraction uses X-rays of known wavelengths to determine the lattice spacing in crystalline structures and therefore directly identify chemical compounds. This is in contrast to the other X-ray methods discussed in this chapter (XRF, electron microprobe analysis, PIXE) which determine concentrations of constituent elements in artifacts. Powder XRD, the simplest of the range of XRD methods, is the most widely applied method for structural identification of inorganic materials, and, in some cases, can also provide information about mechanical and thermal treatments during artifact manufacture. Cullity (1978) provides a detailed account of the method. 

Figure 5.4 The relationship between change in microfibril width and degree of crystallinity following thermal treatment in wet and dry conditions, according to the data of Bhuiyan etal. (2000).

This method requires the addition of a mixed M(II)/M(III) salt solution to an alkaline solution containing the desired interlayer anion. Preparations under conditions of high supersaturation generally give rise to less crystalline materials, because of the high number of crystallization nuclei. Because this method leads to a continuous change in solution pH, the formation of impurity M(0H)2 and/or M(OH)3 phases, and consequently an LDH product with an undesired M(II)/M(III) ratio, often results. Thermal treatment performed following coprecipitation may help increase the crystallinity of amorphous or badly crystallized materials. 

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