Synthesis solvothermal routes

Fig. 7 Comparison between the experimental powder XRD pattern of a material prepared by mechanochemical synthesis and the simulated powder XRD pattern of a potential candidate known structure prepared previously by a solvothermal route. Visual comparison (top part) might tend to suggest that the two materials are very similar. However, detailed comparison (bottom part) reveals important differences between the powder XRD patterns. In particular, the peak at 26 29° is present for the material prepared by mechanochemical synthesis but is absent...

Fig. 11 Crystal structure of a metal-organic framework material Zn2(fina)2(bipy) prepared by mechanochemical synthesis, with the structure determined directly from powder XRD data. The structure is viewed (a) along the c-axis and (b) along the b-axis. The two (identical) interpenetrated frameworks are indicated by yellow and purple shading. For comparison, (c) and (d) show the corresponding views of the stmcture of a DMF solvate material Zn2(fma)2(bipy)(DMF)o.5 prepared by a solvothermal route. Although there is some similarity between these structures, there are nevertheless important stmctural differences between them...

Iron particles were synthesized by a solvothermal route, to the best of our knowledge, which is seldom used in the synthesis of nanometals[20].The reaction was as the follows ... 

Other technological aspects of carbon nanotube synthesis currently under scrutiny include study of the growth mechanism [67,71], attempts to control the diameter [72-74], processes which yield very long CNTs [70,75], optimization of the catalyst composition [76], and improvements in purity [77]. A major area of focus is the production of CNTs at selected sites on a substrate (micropatterning) [78-81]. Other synthetic methods investigated have been (i) a solvothermal route, in which reactants are heated in solution in a sealed autoclave [82,83] (ii) a solid-state metathesis process [84] (iii) a hydrothermal process which produces MWNTs from amorphous carbon [85] and (iv) low-temperature processes [59]. 

Nickel sulfide nanoparticles synthesized by Guo et al. also showed efficient photocatalytic activity in the degradation of Congo Red under visible-light irradiation. The NiS nanoparticles were by a hydrothermal method. A solution of nickel salt, sodium hydroxide and thioacetamide was sealed in a Teflon lined reactor and heated in an oven for 160 °C for 24 hr. After cooling the product was filtered and washed with water and ethanol. CdS nanowires have been used as ID nanoscale substrates for the growth of NiS nanoparticles by a solution phase method.The step involves the synthesis of the CdS nanowires by a solvothermal route. The as-prepared CdS nanowires and NiCla HaO were dissolved in ethanol and loaded into a Telfon autoclave. 

Traditionally, the synthesis of MOFs follows a solvothermal route, heating a ligand (typically in protonated form) and metal salt mixture in solvents such as dimethylformamide (DMF) for hours or up to several days. However, this often produces small amounts of the desired crystals (ca. 1 g or less) and the amount of solvent required limits feasible scale-up. Other methods have been examined, such as sonochemical and microwave assisted synthesis, with both of these methods and others covered in an in-depth review by Meek. These methods are outside the scope of this report, which is limited to an electrosynthetic focus. 

Yang, G., and Fu, S.-Y. (2008) One-pot template-free synthesis of monodisperse and single-crystal magnetite hollow spheres by a simple solvothermal route. 

Srivastava P, Singh K (2012) Synthesis of CdSe nanoparticles by solvothermal route structural, optical and spectroscopic properties. Adv Mater Lett 3(4) 340-344... 

Recently, our group has reported the synthesis of CdTe nanorods using solvothermal route from two different single source molecular precursors and their subsequent characterization by XRD and SEM [271], Initially, the single source molecular precursor Cadmium complex of bis-(aminopropyl) telluride has been prepared as per the scheme shown below (Fig. 6) ... 

A.K. Tiwari, T.A. Jain, V.K. Verma, S. Choubey, P.K. Bajpai, Synthesis and Characterization of HgTe nanorods via solvothermal route. Archives of Applied Science Research 6 (2014) 37-41. 

Demazeau G. Solvothermal reactions an original route for the synthesis of novel materials. Journal of Materials Science. 2008 43(7) 2104—2114. 

In addition to the catalytic solvothermal synthesis of carbon nanotubes (Fig. 2) [7], SiC nanowires and tubular structures (Fig. 8) were prepared through a solvothermal reduction-carburization route using silicon powders and CCI4 as Si and carbon sources [20], Si3N4 nanorods were also prepared with a similar process [12]. 

Hydro(solvo)thermal synthesis chemistry focuses on the chemistry in preparation, synthesis, and assembly of special compounds or materials under hydro(solvo)thermal conditions. More importantly, hydrothermal or solvothermal synthesis routes can be used to prepare materials with special structures and properties, or phases, types, and morphologies which cannot be obtained by using solid-state reactions. In some cases, the materials can be obtained under mild conditions by using hydrothermal and solvothermal synthesis instead of under critical conditions by using a solid-phase reaction synthesis route. 

According to the reaction temperature, hydrothermal and solvothermal synthesis can be classified into subcritical and supercritical synthesis reactions. In subcritical synthesis, the temperature is in the range of 100 to 240 °C, while in supercritical synthesis, the temperature could reach 1000 °C and the pressure could reach 0.3 GPa. By using the special properties of solvent water and other reactants under supercritical high temperature and pressure, various syntheses with specific features could be conducted, resulting in the formation of numerous crystal materials with simple to very complex structures. In addition, it should be pointed out that some crystal materials cannot be obtained by using other preparation approaches except for using hydrothermal or solvothermal synthesis routes. 

Later, Yaghi et al.[32] proposed an alternative route for the synthesis of these sulfides, in which crystals were obtained from the diffusion of an aqueous solution of the 3d metal into a solution of R-Ge4S10 complex at room temperature. In 1997, Martin and Greenwood133 successfully prepared a new class of microporous metal chlorides, named CZX-n, under solvothermal conditions (160°C) in benzene solution. The framework of CZX-1 is isostructural with the aluminosilicate sodalite (SOD), while CZX-2... 

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