Membrane preparation ceramic membranes

Frequently, inorganic membranes are used instead of polymeric membranes because of their outstanding chemical and thermal resistances. In addition, the pore size in these membranes can be better controlled and as a consequence the pore size distribution is generally very narrow (see also chapter IV). Various techniques can be used to prepare ceramic membranes with some important ones being ... 

Because membranes appHcable to diverse separation problems are often made by the same general techniques, classification by end use appHcation or preparation method is difficult. The first part of this section is, therefore, organized by membrane stmcture preparation methods are described for symmetrical membranes, asymmetric membranes, ceramic and metal membranes, and Hquid membranes. The production of hollow-fine fiber membranes and membrane modules is then covered. Symmetrical membranes have a uniform stmcture throughout such membranes can be either dense films or microporous. 

The sol—gel technique has been used mosdy to prepare alumina membranes. Figure 18 shows a cross section of a composite alumina membrane made by sHp coating successive sols with different particle sizes onto a porous ceramic support. SiUca or titanium membranes could also be made by the same principles. Unsupported titanium dioxide membranes with pore sizes of 5 nm or less have been made by the sol—gel process (57). 

Sol-gel techniques have been widely used to prepare ceramic or glass materials with controlled microstructures. Applications of the sol-gel method in fabrication of high-temperature fuel cells are steadily reported. Modification of electrodes, electrolytes or electrolyte/electrode interface of the fuel cell has been also performed to produce components with improved microstructures. Recently, the sol-gel method has expanded into inorganic-organic hybrid membranes for low-temperature fuel cells. This paper presents an overview concerning current applications of sol-gel techniques in fabrication of fuel cell components. 

Fig. 4. Configuration of a ceramic membrane reactor for partial oxidation of methane. The membrane tube, with an outside diameter of about 6.5 mm and a length of up to about 30 cm and a wall thickness of 0.25-1.20 mm, was prepared from an electronic/ionic conductor powder (Sr-Fe-Co-O) by a plastic extrusion technique. The quartz reactor supports the ceramic membrane tube through hot Pyrex seals. A Rh-containing reforming catalyst was located adjacent to the tube (57).

Fig. 6. Configuration of a ceramic membrane reactor for partial oxidation of methane. The membrane disk was prepared by pressing Bao.5Sro.5Coo.8Feo.2O3-s oxide powder in a stainless steel module (17 mm inside diameter) under a pressure of (1.3-1.9) X 109 Pa. The effective area of the membrane disk exposed to the feed gas (CH4) was 1.0 cm2 (72).

Larbot, A., J. A. Alary, C. Guizard, L. Cot and J. Gillot. 1987. New inorganic ultrafiltration membranes Preparation and characterization. Int. J. High Technology Ceramics 3 145-51. 

Ohya, H., Y. Tanaka, M. Niwa, R. Hongladaromp, Y. Negismi and K. Matsumoto. 1986. Preparation of composite microporous glass membrane on ceramic tubing. Maku 11 41-44. 

Terpstra, R. A., B. C. Bonekamp and H. J. Veringa. 1988. Preparation, characterization and some properties of tubular alpha alumina ceramic membranes for microfiltration and as a support for ultrafiltration and gas separation membranes. Desalination 70 395-404. 

Hollow glass microbeads Porous ceramic membranes Microbeads coated by Ti02 particles Porous ceramic Ti02 and ZnO membranes prepared by sol-gel technique... 

While considerable progress has been made in the preparation of ceramic membranes by sol-gel processing, the development of membranes from hybrid polymers is in its infancy (see also Section V). This is, nevertheless, a very promising area of development, because the possibility of forming mechanically stable membranes by inorganic polycondensation is implemented by the possibility to incorporate organic functions. 

In this chapter membrane preparation techniques are organized by membrane structure isotropic membranes, anisotropic membranes, ceramic and metal membranes, and liquid membranes. Isotropic membranes have a uniform composition and structure throughout such membranes can be porous or dense. Anisotropic (or asymmetric) membranes, on the other hand, consist of a number of layers each with different structures and permeabilities. A typical anisotropic membrane has a relatively dense, thin surface layer supported on an open, much thicker micro-porous substrate. The surface layer performs the separation and is the principal barrier to flow through the membrane. The open support layer provides mechanical strength. Ceramic and metal membranes can be either isotropic or anisotropic. 

Recently, attempts have been made to reduce the cost of palladium metal membranes by preparing composite membranes. In these membranes a thin selective palladium layer is deposited onto a microporous ceramic, polymer or base metal layer [19-21], The palladium layer is applied by electrolysis coating, vacuum sputtering or chemical vapor deposition. This work is still at the bench scale. 

During the last few years, ceramic- and zeolite-based membranes have begun to be used for a few commercial separations. These membranes are all multilayer composite structures formed by coating a thin selective ceramic or zeolite layer onto a microporous ceramic support. Ceramic membranes are prepared by the sol-gel technique described in Chapter 3 zeolite membranes are prepared by direct crystallization, in which the thin zeolite layer is crystallized at high pressure and temperature directly onto the microporous support [24,25],... 

Preparation of Pt-TiOx/Pd membranes. It was also desirable to prepare metalloceramic membranes in which the catalytic activity of the ceramic phase was enhanced through the addition of a noble metal. The very low surface area of the titania films prepared as described above made them difficult to impregnate with adequate dispersion by traditional incipient wetness techniques. Instead, finely ground titania (>200 mesh) was impregnated with platinum via the incipient wetness method with a chloroplatinic acid solution. This powder was then sprinkled onto the surface of a freshly dipped membrane, which was dried and heat treated as described. These materials were activated before use at 350°C in hydrogen for three hours. 

The in situ membrane growth technique cannot be applied using the zeolite-based ceramic porous membrane as support, under hydrothermal conditions in a solution containing sodium hydroxide. The high pH conditions will cause membrane amorphization and lead to final dissolution. Therefore, we tried to synthesize an aluminophosphate zeolite such as AlP04-5 [105] over a zeolite porous ceramic membrane. For the synthesis of the AlP04-5-zeolite-based porous membrane composite, the in situ membrane growth technique [7,13,22] was chosen. Then, the support, that is, the zeolite-based porous ceramic membrane, was placed in contact with the synthesis mixture and, subsequently, subjected to a hydrothermal synthesis process [18]. The batch preparation was as follows [106] ... 

In the preparation of multi-layered ceramic membranes, the quality of the support is of crucial importance to the integrity of the membrane layers that are applied in the subsequent preparation steps. First, the surface roughness and homogeneity of the support will determine the integrity of these membrane layers, and, second the surface roughness determines the minimal thickness of the membrane layer for complete surface coverage. 

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