Pressed face powders

Finely divided preparations of amorphous silica, silica-alumina gels, and synthetic zeolites give satisfactory films by pressing the powders between polished steel faces generally at about 10,000 Ib/in. (McDonald [1958]). Separation of the sample from the surface is facilitated by introducing aluminum foil between the sample and the steel faces. The film can then be separated from the foil by the technique shown in Figure 2. These self-supporting... 

Polycrystalline yttria-stabilized zirconia (YSZ-8) disks were prepared using 8 mol % Y203-doped zirconia powder (TOSOH zirconia, TZ-8Y, TOSOH Corp.). The powder was pressed uniaxially into disks which were cold isostatically pressed at 40,000 psi and then sintered at 1450°C for 4 h. Pt paste (Engelhard 6926) was painted on both faces of the YSZ-8 disks. Pt wires (0.0025 cm diam) were connected to the YSZ by using Pt meshes (150 X 150 mesh, 0.005 cm wire diam, Unique Wire Weaving Co., Inc.). 

Powders compressed into flat-faced tablets by action of punch and die, comminuted and screened to form feed for final compression. Dry granulation, slugging, pre-compression Heavy duty tableting press... 

Before the actual sintering, the powder was pelleted in a small die. The pellets varied from 7/16 to 3/16 inch in diameter and were about 0.006 inch thick. After pelletization, the sample was placed between the faces of the anvils. A ferric oxide-coated pyrophylite ring was used to contain the sample. Pressure was increased in 10,000-atm. increments. About 2 minutes were allowed for the dissipation of the heat generated by each compression. The sample was maintained at the maximum pressure for about 10 minutes, after which pressure was reduced continuously until the press rams opened, permitting withdrawal of anvils. 

It should be noted that this discussion assumes that only one punch is actively applying the force to the powder mass while the other is stationary and passive. This is true in the case of an excentric press, but with a rotary tablet press, both punches move and hence both exert forces on the powder bed. The force distribution so obtained is thus different from that shown in Fig. 7, and results in two low density zones near the faces of the tablet and a high density zone in approximately the centre of the powder mass. 

Hot mounting uses hot-press equipment as shown in Figure 1.18. A specimen is placed in the cylinder of a press and embedded in polymeric powder. The surface to be examined faces the bottom of the cylinder. Then, the specimen and powder are heated at about 150°C under constant pressure for tens of minutes. Heat and pressure enable the powder to bond with the specimen to form a cylinder. Phenolic (bakelite) is the most widely used polymeric powder for hot mounting. Hot mounting is suitable for most metal specimens. However, if the microstructure of the material changes at the mounting temperature, cold mounting should be used. 

XRF is used for the analysis of solid and liquid samples. For quantitative analysis the surface of the sample must be as flat as possible, as will be discussed in the applications section. There are two classes of sample holders, cassettes for bulk solid samples and cells for loose powders, small drillings, and liquids. A typical cassette for a flat bulk solid such as a polished metal disk, a pressed powder disk, a glass or polymer flat is shown in Fig. 8.26(a). The cassette is a metal cylinder, with a screw top and a circular opening or aperture, where the sample will be exposed to the X-ray beam. The maximum size for a bulk sample is shown. The sample is placed in the cassette. For a system where the sample is analyzed face down, the cassette is placed with the opening down and the... 

The ATR objective has a polished face of diamond, germanium or zinc selenide (ZnSe) that is pressed into contact with the sample (Sawyer et al. 2008). Infrared reflection is attenuated by absorption within a surface layer a few micrometers deep. In this case, a good contact is required, but that is easy for most polymers, and the advantage is that no sample preparation is required. Therefore, powders, films, gels and even polymer solutions can be characterized. 

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