Chemical preparation

Refractory carbide and nitride powders are usually produced by chemical reaction between the elements or compounds of the eluents. These processes are moderate in cost but do not generally produce materials of the highest purity and consistency. 

Refractory Carbides. The various chemical preparation reactions for refi tory carbide powders are summarized in Table 14.2.1 1 

As shown in the table, a common method of preparing transition-metal carbide powders is to react the metal oxide (i.e., Ti02, Zr02, etc.) with carbon in the form of powders in the presence of hydrogen and in the temperature range of 1500 C to 2400 C, depending on the metal.l  

Beta-SiC powder can be produced in a microwave ovoi (2540 MHz) by simple solid-state reaction between silicon and charcoal powder at temperature lower than 1000 C.1 1 

Reaction of Ti02 with carbon at 2000°C or above in hydrogen Carburization of titanium sponge 

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In contrast to tire preparation of LB films, tliat of SAMs is fairly simple and no special equipment is required. The inorganic substrate is simply immersed into a dilute solution of tire surface active material in an organic solvent (typically in tire mM range) and removed after an extended period ( 24 h). Subsequently, tire sample is rinsed extensively witli tire solvent to remove any excess material (wet chemical preparation). 

Among the other chemicals prepared from ethylene are ethanol and acetaldehyde... 

Section 20 5 Acid anhydrides may be prepared from acyl chlorides m the laboratory but the most commonly encountered ones (acetic anhydride phthahc anhydride and maleic anhydride) are industrial chemicals prepared by specialized methods... 

In some cases it may be advantageous to deviate from the classical technology. For example, in wet-chemical preparation better chemical and morphological control may be achieved by starting from salt solutions. 

Pandya et al. have used extended X-ray ascription fine structure (EXAFS) to study both cathodically deposited -Ni(OH)2 and chemically prepared / -Ni(OH)2 [44], Measurements were done at both 77 and 297 K. The results for / -Ni(OH)2 are in agreement with the neutron diffraction data [22]. In the case of -Ni(OH)2 they found a contraction in the first Ni-Ni bond distance in the basal plane. The value was 3.13A for / -Ni(OH)2 and 3.08A for a-Ni(OH)2. The fact that a similar significant contraction of 0.05A was seen at both 77 and 297K when using two reference compounds (NiO and / -Ni(OH)2) led them to conclude that the contraction was a real effect and not an artifact due to structural disorder. They speculate that the contraction may be due to hydrogen bonding of OH groups in the brucite planes with intercalated water molecules. These ex-situ results on a - Ni(OH)2 were compared with in-situ results in I mol L"1 KOH. In the ex-situ experiments the a - Ni(OH)2 was prepared electrochemi-cally, washed with water and dried in vac-... 

Rhombohedral Se was found as a high-pressure allotrope of sulfur above 9-10 GPa by several groups [58, 137, 150, 184, 186, 188, 191]. The pressure dependence of frequencies [137, 150, 184] as well as the kinetics of the transition from p-S to Ss [186] have been investigated systematically by Raman spectroscopy. The pressure dependent frequency shifts of chemically prepared Ss and of high-pressure Ss have been found to be identical [137, 150]. 

For quantum chemical estimates of radical stability and reactivity, one often needs to know the conditions and medium in which they arise. As there are many reviews on chemical preparations of radicals, we give here only a brief description of the most important preparative methods and a note on a specific problem in chemical preparations of cation radicals. 

If an elastomer is bonded to a substrate such as steel, it is usual for the bond to have small areas of imperfection where the adhesive or the chemical preparation of the surface is defective. Such areas are known as holidays. In high-pressure gas environments, these holidays form nucleation sites for the growth of half-bubbles or domes, under conditions where gas has been dissolved in the elastomer and the pressure has subsequently been reduced. Gas collecting at the imperfection at the interface will inflate the mbber layer, and domes will show as bumps on the surface of the mbber-coating layer—just as a paint layer bubbles up in domes when the wood underneath gives off moisrnre or solvents in particular areas. 

This method is one of the dry methods in which no chemical reaction is involved. Preparation of ultrafine particles by physical vapor deposition (PVD) dose not require washing and calcination, which are indispensable for chemical preparation such as in CP and DP methods. As waste water and waste gases are not by-produced, the arc plasma (AP) method is expected to grow in popularity as one of the industrial production methods for gold catalysts and as a clean preparation method. 

Poly(2,6-dimethyl-l,4-oxyphenylene) (poly(phenylene oxide), PPG) is a material widely used as high-performance engineering plastics, thanks to its excellent chemical and physical properties, e.g., a high 7 (ca. 210°C) and mechanically tough property. PPO was first prepared from 2,6-dimethylphenol monomer using a copper/amine catalyst system. 2,6-Dimethylphenol was also polymerized via HRP catalysis to give a polymer exclusively consisting of 1,4-oxyphenylene unit, while small amounts of Mannich-base and 3,5,3, 5 -tetramethyl-4,4 -diphenoquinone units are always contained in the chemically prepared PPO. 

This was corroborated by experimental evidence. Higher conversions were found for the wet-chemically prepared catalyst. 

An example for chemical preparation that can be carried out within seconds in a beaker is this Dissolve pyrrole in dilute sulfuric acid. Add ferric chloride as an aqueous solution and watch the black polypyrrole precipitate. The oxidizing Fe ions are reduced to Fe, imparting one +-charge and donating their now excessive Cr ion as dopant ion to the polymer. 

This chapter will mainly deal with the advantages of the alkaline EG synthesis method for the chemical preparation of noble metal nanoclusters stabilized by EG and simple ions, as well as the excellent performances of the functional materials assembled using these unprotected metal nanoclusters as building blocks. 

Scheme 1. Procedure of alkaline EG method for the chemical preparation of metal nanoclusters stabilized by EG and sample ions.

In the chemical preparation of unprotected metal colloids, the metal concentration usually has a significant influence on the particle size of obtained metal nanoclusters. For example, when increasing Pd concentration from 0.1 to 1.0 mM in the preparation of Pd metal colloids by the thermal decomposition of Pd acetate in methyl isobutyl ketone, the average Pd particle size increased from 8 to 140nm [6,7]. However, in the alkaline EG synthesis method, the size of metal nanoclusters was only slightly dependent on the metal concentration of the colloidal solution. The colloidal Pt particles prepared with a metal concentration of 3.7 g/1 had an average diameter of... 

The alkaline EG S5mthesis method is a very effective technology for the chemical preparation of unprotected metal and alloy nanoclusters stabilized by EG and simple ions. This method is characterized by two steps involving the formation of metal hydroxide or oxide colloidal particles and the reduction of them by EG in a basic condition. The strategy of separating the core formation from reduction processes provides a valid route to overcome the obstacle in producing stable unprotected metal nanoclusters in colloidal solutions with high metal concentrations. Noble metal and alloy nanoclusters such as Pt, Rh, Ru, Os, Pt/Rh and Pt/Ru nanoclusters with small particle... 

Part A Chemical preparations Part B Preparations of microorganisms or viruses... 

None of the above-mentioned ICPMS techniques can rival MC-TIMS and MC-ICPMS in terms of analytical precision, but the advantage of conventional ICPMS lies in the speed and ease with which data can be acquired. Analysis times are typically less than 10 minutes, and results can be obtained on solid, liquid or gas samples directly, without chemical preparation. Direct analysis will, however, give rise to high levels of molecular... 

Skotheim et al. [286, 357, 362] have performed in situ electrochemistry and XPS measurements using a solid polymer electrolyte (based on poly (ethylene oxide) (PEO) [363]), which provides a large window of electrochemical stability and overcomes many of the problems associated with UHV electrochemistrty. The use of PEO as an electrolyte has also been investigated by Prosperi et al. [364] who found slow diffusion of the dopant at room temperature as would be expected, and Watanabe et al. have also produced polypyrrole/solid polymer electrolyte composites [365], The electrochemistry of chemically prepared polypyrrole powders has also been investigated using carbon paste electrodes [356, 366] with similar results to those found for electrochemically-prepared material. 

Konovalova, T. A., S. A. Dikanov et al. (2001a). Detection of anisotropic hyperfine components of chemically prepared carotenoid radical cations ID and 2D ESEEM and pulsed ENDOR study.. /. Phys. Chem. B 105 8361-8368. 

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