Layer recrystallizations

Figure 10.12 (a) HRTEM images of YBa2Cu307 6, viewed down the [110] direction. The initial image showing a thin layer of disordered coating, and the image recorded from the same area after electron beam irradiation for 3h. The disordered layer recrystallized into a clean crystalline surface. 

Figure 4.11 Schematic of S-layer stabilized solid supported lipid membranes, (a) S-layer directly recrystallized on gold, with a lipid bilayer on top. (b) Same as (a), with an additional S-layer recrystallized on top of the lipid bilayer, (c) Thiolated SCWPs directly bound to gold and interacting with an S-layer, with a lipid bilayer on top. (d) Same as (c).

Fig. 10.10. Growth rate versus depth for an a—Si layer recrystallized at 350°C by 600 Kr ions (after Priolo et al. 1989)...

Fig. 10.12. Ion-induced growth rate versus reciprocal temperature for a—Si layers recrystallized by irradiation with a 600 keV Kr beam (Olson and Roth 1988)...

Figure Bl.24.11. The backscattering yield from an Si sample that has been implanted with Si atoms to form an amorphous layer. Upon annealing this amorphous layer recrystallizes epitaxially leading to a shift in the amorphous/single-crystal interface towards the surface. The aligned spectra have a step between the amorphous and crystal substrate which shifts towards the surface as the amorphous layer epitaxially recrystallizes on the Si. 

AFM micrographs show (a) the S-layer recrystallized in vitro at pH = 3 in the presence of an APTES-Si substrate, (b) height profile based on (a), (c) zoomed image for lattice symmetry estimation, (d) FFT analysis based on high-quality image (b) showing the p4 symmetry (see black arrows). 

The solid phase epitaxy of amorphous on crystalline silicon systems has been studied by molecular dynamics simulations. First a simulation scheme is consolidated in the case of an amorphous layer recrystallization where the a/c velocity is well known from experiments. An atomic model of the a/c interface is constmcted and annealed by MD using one suitable interatomic potential for Si-Si interactions. The motion of the amorphous/crystalline interface is extracted and compared to the experimental law by Olson and Roth. Although none of the potentials is in agreement with the experiments, two stand out Tersoff for SPE but accounting for a shift to higher temperatures compared to the real ones, and StiUinger-Weber, for LPE. 

Surface oxide layer Recrystallized grain layer ... 

Once the reaction mix has cooled after reflux, 500mL of room temperature dHsO can be added and the whole solution extracted with DCM. The DCM layer is separated and the solvent removed by distillation to give the li-nitropropene as an oil of all things. This oil can then be recrystallized in hot methanol just like the crystalline form was [38]. 

A stirred solution of o-methylpivalanilide (50 mmol) in dry THE (100 ml) was maintained at 15°C under a nitrogen atmosphere. A 1.5 M solution of n-butyllithium in hexane (3 equiv.) was added dropwise. The solution was then maintained at room temperature for 16h. The solution was cooled in an ice-bath and treated with 2 N HCl (60 ml). The organic layer was separated and the aqueous layer was further extracted with benzene. The combined layers were dried (MgS04). The product was obtained in 87% yield and recrystallized from ether-cyclohexane. 

Phenyl-3-oxopropanoic acid (25 mmol) and EtjN (87.5 mmol) were dissolved in THF (150 ml) and cooled to —40°C. Ethyl chloroformate (27.5 mmol) was added dropwise to this solution and then the reaction mixture was stirred for 30 min at —20°C. Di-n-hexylamine (27.5 mmol) was added to the suspension and it was stirred at room temperature for an additional hour. The reaction mixture was diluted with water (100 ml) and extracted with ether (400 ml). The extract was washed with aq. 5% HCl (100 ml) and brine (2 X 100 ml) and dried over NajSO. The crude amide was obtained by removal of the solvent in vacuo and phenylhydrazine (25 mmol) was added. The mixture was heated to 100°C for 30 min. The residue was held in vacuo to remove the water formed and then powdered ZnCl2 (125 mmol) was added. The mixture was heated at 170"C with manual stirring for 5 min. The cooled residue was dissolved in acetone (100 ml) and diluted with ether (500 ml). Water (100 ml) was added. The organic layer was separated and washed successively with 5% aq. HCl (100 ml) and brine (2 x 100 ml) and dried over NajSO. The solvent was removed in vacuo, and the residue was recrystallized from EtOAc-hexane. The yield was 79%. 

A solution of 2,3-dibromo-5-methoxyaniline (32 g, 0.17 mol) in CHjClj (300 ml) was stirred and cooled in an icc bath. Boron trichloride (1 M in CH2CI2, 180 ml, 0.18 mol), chloroacetonitrile (14.3 g, 0.19 mol) and TiC (1 M in CH CIj, 190ml, 0.19 mol) were added. The resulting mixture was refluxed for 1.5 h. The solution was cooled to room temperature and poured carefully on to a mixture of icc and 20% aq. HCl (700 ml). The organic layer was separated and the CH Clj removed by distillation. The residue was heated to 90°C on a water bath for 30 min. The solution was cooled and the solid collected by filtration. It was partitioned between ether (1.41) and 1 N NaOH (500 ml). The ether layer was washed with brine, dried over Na2S04 and evaporated. The residue was recrystallized from ethanol to give 2-amino-3,4-dibromo-6-methoxy-a-chloroacetophenone (55 g) in 90% yield. 

Phenylmagnesium bromide (2.8 mol) was prepared in anhydrous ether (21) from bromobenzene (440 g, 2.9 mol) and magnesium turnings (68.0 g 2.8 g-atom). To this solution was added dropwise a solution of indole (328 g, 2.8 mol) in benzene (8(X)ml). The resulting solution was stirred for 10 min and then a solution of cyclopentanoyl chloride (322 g, 2.4 mol) in benzene (800 ml) was added dropwise. The solution was stirred for 1 h and then water (11) was added carefully. The precipitate which formed was collected by filtration and dried to give 169 g of crude product. Additional product (97 g) was obtained by evaporation of the organic layer of the filtrate. The combined products were recrystallized from toluene to give 250 g (49% yield) of pure product. 

A solution of 6-bromoindole (O.lOmol) in toluene (200 ml) was treated with Pd(PPh3)4 (5mol%) and stirred for 30 min. A solution of 4-fluorophenyl-boronic acid (0.25 M, 0.15 mol) in abs. EtOH was added, followed immediately by sal aq. NaHCOj (10 eq.). The biphasic mixture was refluxed for several hours and then cooled to room temperature. The reaction mixture was poured into sat. aq. NaCl (200 ml) and the layers separated. The aq. layer was extracted with additional EtOAc (200 ml) and the combined organic layers dried (Na2S04), filtered and concentrated in vacuo. The solution was filtered through silica gel using hexane-CHjCl -hexanc for elution and evaporated. Final purification by recrystallization gave the product (19 g, 90%). 

North American Chemical Co. produces borax pentahydrate and decahydrate from Seades Lake brines in both Trona and West End, California (see Chemicals frombrines). The 88 km dry lake consists of two brine layers, the analyses of which are given in Table 11. Two distinct procedures are used for the processing of upper and lower lake brines. Borax is produced in Trona from upper lake brines by an evaporative procedure involving the crystallization of potash and several other salts prior to borax crystallization as the pentahydrate (104). A carbonation process is used in West End, California to derive borate values from lower lake brines (105). Raw lower stmcture brine is carbonated to produce sodium bicarbonate, which is calcined and recrystallized as sodium carbonate monohydrate. The borate-rich filtrate is neutralized with lake brine and refrigerated to crystallize borax. 

Ethyl 4,5-Dlbenzamldopent-4-enoate (2) Ethyl 3-lmidazol-4(5)-ylpropanoale 1 (9.2 g, 54 mmol) In ElOAc (140 mL) was treated with benzoyl chloride (15 7 g, 112 mmol) In ElOAc (40 mL) and 1M NaHCOa (380 mL) added simultaneously In 1 h under Ice-cooling. The reaction mixture was stirred for 1 h, then a further portion of benzoyl chloride (IS 7 g, 112 mmol) in ElOAc) and iM NaHCOa (280 mL) was added m the same manner, followed by an additional portion o( 1M NaHCOa (200 mL) The reaction mixture was stirred for 24 h, then the organic layer was separated, concentrated, and the residue dissolved in THF (300 mL) The THF solution was stirred with 10% NaHCOa (600 mL) for 24 h to decompose any N-lormyl intermediate and to remove benzoic acxl Extraction with EtOAc, drying (Na2S04), solvent evaporation and recrystallization of the residue from EtOAc hexane afforded 16 24 g of 2 (84%), mp 128-129°C... 

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