Hydrothermal deposition method

Some work has been reported on deposition of hydroxyapatite under hydrothermal conditions, that is much above 100 °C. This includes a study by Liu, Savino and Yates (2011) who coated hydroxyapatite on titanium, stainless steel, aluminium and copper substrates by a seeded hydrothermal deposition method. The deposition strategy included an electrochemical reaction to form quickly a thin layer of HAp seed crystals. Subsequent hydrothermal crystal growth from the seed layer resulted in dense and durable HAp films. In a typical hydrothermal synthesis, a solution of Na2EDTA (0.20 M) and Ca(NOs)2 (0.20 M) was prepared in 15 ml water and a solution of (NH4)2HP04 (0.12 M) in 15 ml water was prepared in a second container. The two source solutions were mixed together after the pH of each solution was raised to 10.0 with ammonium hydroxide. The resulting combined solution was stirred at room temperature for about 20 min and then transferred to a Teflon-lined stainless steel pressure vessel of 40 ml internal volume. 

Zeolite-supported Re catalysts have been synthesized by chemical vapor deposition (CVD) ofMTO (CH3Re03) (3) on various zeolites such as HZSM-5, H-Beta, H-USY and H-Mordenite. HZSM-5 samples with different A1 contents were prepared by a hydrothermal synthesis method. For comparison, conventional impregnated catalysts were also prepared by an impregnation method using an aqueous solution of NH4Re04. All catalysts were pretreated at 673 K in a flow of He before use as catalyst. 

As discussed in Chapters 5 and 7, the use of lime to precipitate calcium arsenates is a common method for removing inorganic As(V) from water or flue gases. Calcium arsenates were also once extensively used in pesticides (Chapter 5). The compositions of some calcium arsenates, such as johnbaumite (Ca5(As04)3(0H) Table 2.5), resemble the very common phosphate mineral, apatite (Ca5(P04)3(F,Cl,0H)), where arsenate replaces phosphate. Some lead arsenates, such as mimetite (Pb5(As04)3Cl Table 2.5), also have crystalline structures that are related to apatite. Mimetite may occur in oxidized lead-rich hydrothermal deposits. 

The basic approach to classify powder production methods is based on whether a method is top-down or bottom-up. In a top-down method, micro- and nano-particles are produced due to the stracture and size refinement through the breakdown of the larger particles in a bottom-up method, the mechanism of particle formation is usually by means of nucleatimi, growth and aggregation of atoms and molecules. In a more practical approach, one may divide the powder synthesis methods as follows (1) wet chemistry, such as the chemical precipitation, sol-gel, microemulsion, sonochemistry, and hydrothermal synthesis methods (2) mechanical attrition, grinding and milling (3) gas phase methods, such as the chemical and physical vapor deposition (4) liquid phase spray methods, such as the molten metal spray atomization, spray pyrolysis, and spray drying, and (5) liquid/gas phase methods. 

Liang, C. H., and C. S. Hwang. 2010. Effects of temperatures and cations of electrolyte on the capacitive characteristics of the manganese oxide deposited by hydrothermal electrochemical method. Journal of Alloys and Compounds 500 102-107. 

Kashima T, Matsuda Y, Fujiyama H (1991) Development of the quadrupole plasma chemical vapour deposition method for low temperature, high speed coating on an optical fibre. Mater Sci Eng A 139 79-84 Kaya C, He JY, Gu X, Butler EG (2002) Nanostructured ceramic powders by hydrothermal synthesis and their applications. Microporous Mesoporous Mater 54 37-49... 

In recent years titania has been used as photocatalysts mostly in the form of thin films. If titania thick films are prepared in a simple process, the application field is expected to expand. Electrophoretic sol-gel deposition method has been applied to preparation of titania thick films. In preparation of titaina particles, the particles tend to aggregate in the heat treatment process and the re-dispersion of the particles is difficult. However, hydrothermal treatment has been found to prevent the titania particles from aggregating and titania thick films can be prepared by the electrophoretic sol-gel deposition using these hydrothermally treated particles (Sakamoto, 1998). 

Polyaniline (PANI) nanocomposite membranes are also prepared by a sol-gel process, embedding silica in the hydrophilic clusters (Nafion) followed by its deposition by redox polymerization [51]. PANI modified the membrane structure and reduced the methanol crossover, while silica Incorporation improved the conductivity and stability. Zeolite has been incorporated as potential filler for PEMs, either by blending or by infiltration in swelled membrane, to reduce the methanol permeability and enhance the thermal stabihty [52,53]. Although the fuel cell performance of these membranes was Inferior compared with pristine Nafion membrane, incorporation of semipermeable particles is an effective method to engineer the transport properties of composite membranes. Chen et al [54] reported nanocomposite membranes by in situ hydrothermal crystallization method, with similar proton conductivity, but low methanol permeability (40% less) in comparison with Nafion membrane. These membranes showed higher OCV (3%) and power density (21%) than Nafion. 

Recently, it is reported that Xi02 particles with metal deposition on the surface is more active than pure Ti02 for photocatalytic reactions in aqueous solution because the deposited metal provides reduction sites which in turn increase the efficiency of the transport of photogenerated electrons (e ) in the conduction band to the external sjistem, and decrease the recombination with positive hole (h ) in the balance band of Xi02, i.e., less defects acting as the recombination center[l,2,3]. Xhe catalytic converter contains precious metals, mainly platinum less than 1 wt%, partially, Pd, Re, Rh, etc. on cordierite supporter. Xhus, in this study, solutions leached out from wasted catalytic converter of automobile were used for precious metallization source of the catalyst. Xhe XiOa were prepared with two different methods i.e., hydrothermal method and a sol-gel method. Xhe prepared titanium oxide and commercial P-25 catalyst (Deagussa) were metallized with leached solution from wasted catalytic converter or pure H2PtCl6 solution for modification of photocatalysts. Xhey were characterized by UV-DRS, BEX surface area analyzer, and XRD[4]. 

Over the past few years, a large number of experimental approaches have been successfully used as routes to synthesize nanorods or nanowires based on titania, such as combining sol-gel processing with electrophoretic deposition,152 spin-on process,153 sol-gel template method,154-157 metalorganic chemical vapor deposition,158-159 anodic oxidative hydrolysis,160 sonochemical synthesis,161 inverse microemulsion method,162 molten salt-assisted and pyrolysis routes163 and hydrothermal synthesis.163-171 We will discuss more in detail the latter preparation, because the advantage of this technique is that nanorods can be obtained in relatively large amounts. 

The 11 nm-sized Ti02 were crystallized using either hydrothermal or thermal methods from 100 nm, amorphous gel spheres. The Ti02 crystal and agglomerate sizes were determined by X-ray diffraction (Philip 1080) and transmission electron microscopy (JEOL JEM 2010), respectively. The surface area and chemistry of the nanostructured Ti02 were analyzed by nitrogen physisorption (Coulter SA 3100) and Fourier transform infrared spectroscopy (FTIR, Perkin-Elmer GX 2000). Metal catalyst was deposited by incipient... 

Membranes with extremely small pores ( < 2.5 nm diameter) can be made by pyrolysis of polymeric precursors or by modification methods listed above. Molecular sieve carbon or silica membranes with pore diameters of 1 nm have been made by controlled pyrolysis of certain thermoset polymers (e.g. Koresh, Jacob and Soffer 1983) or silicone rubbers (Lee and Khang 1986), respectively. There is, however, very little information in the published literature. Molecular sieve dimensions can also be obtained by modifying the pore system of an already formed membrane structure. It has been claimed that zeolitic membranes can be prepared by reaction of alumina membranes with silica and alkali followed by hydrothermal treatment (Suzuki 1987). Very small pores are also obtained by hydrolysis of organometallic silicium compounds in alumina membranes followed by heat treatment (Uhlhom, Keizer and Burggraaf 1989). Finally, oxides or metals can be precipitated or adsorbed from solutions or by gas phase deposition within the pores of an already formed membrane to modify the chemical nature of the membrane or to decrease the effective pore size. In the last case a high concentration of the precipitated material in the pore system is necessary. The above-mentioned methods have been reported very recently (1987-1989) and the results are not yet substantiated very well. 

Despite the intense hydrothermal alteration of the volcanic rocks that host the Restigouche VMS deposit, immobility of Ti02, Zr, Nb, Y, Nd, and Th is demonstrated using the Isocon method of Grant (1986). 

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