Protein microtubules (MTs) have been used as templates for the biomimetic synthesis of metal oxide, metal sulfide, and metallic nanomaterials. These materials were coated onto MTs via three distinct synthetic pathways: metal ion hydrolysis which yielded iron oxide or zinc oxide-coated microtubules, metal ion/sulfide co-precipitation which yielded zinc sulfide coated MTs, and metal ion reduction which yielded gold-coated MTs. The growth process of metal oxide coating involves heterogeneous nucleation on the MT surface and produces even, microcrystalline films. Metal sulfide and metal coating initially involves the formation of nanoparticle arrays that decorate the MT surface and can eventually lead to either semi- or fully continuous coatings.

IE-911 is a bound form of cystalline silicotitanate (CST) that was extensively tested for removing 137Cs from the Savannah River Site (SRS) tank wastes. In some simulant tests, column plugging incidents were observed, which led to thorough investigations to determine the causes and to develop protocols to avoid future plugging incidents. A related problem was the apparent decrease in Cs scavenging capability in some long-term tests. Our studies revealed that the interaction of IE-911 with the highly basic, high ionic strength, SRS average salt simulant could result in precipitation of; 1) poorly crystalline Nb-oxide, or 2) aluminosilicate zeolitic phases. The source for the Nb-oxide precipitate was determined to be a minor impurity phase that is a byproduct of CST manufacturing. The mechanisms of dissolution and re-precipitation of this phase in column pretreatment solution were investigated, and a protocol to rid IE-911 of this impurity was devised. The source material for the aluminosilicate zeolite precipitate was determined to be predominantly from the waste solution rather than the IE-911. Solubility experiments coupled with a thermodynamic analysis provided a protocol to predict when aluminosilicate precipitation will and will not occur. Finally, it was also established that aluminosilicate precipitation on the surfaces of the IE-911 granules could also account for an apparent decrease in equilibrium Kd and decrease in kinetics of Cs sorption.

Laser deposits fabricated from two different compositions of 304L stainless steel powder were characterized to determine the nature of the solidification and solid state transformations. One of the goals of this work was to determine to what extent novel microstructures consisting of single-phase austenite could be achieved with the thermal conditions of the LENS process. Although ferrite-free deposits were not obtained, structures with very low ferrite content were achieved. It appeared that, with slight changes in alloy composition, this goal could be met via two different solidification and transformation mechanisms.

Samples of chemically-vapor-deposited sub-micrometer-thick films of polysilicon were analyzed by transmission electron microscopy (TEM) in cross-section and by Raman spectroscopy with illumination at their surface. TEM and Raman spectroscopy both find varying amounts of polycrystalline and amorphous silicon in the wafers. Raman spectra obtained using blue, green and red excitation wavelengths to vary the Raman sampling depth are compared with TEM crosssections of these films. Some films have Raman spectra with a band near 497 cm−1, corresponding to numerous nanometer-scale faulted regions in the TEM micrographs.

Ferroelectric polycrystalline thin films are being pursued as materials for use in the next generation of radiation hardened nonvolatile semiconductor memories, optical switches and optical computers. Of particular interest are PZT films with a composition near the morphotropic phase boundary. In order to fully understand the the difference in electrical properties as a function of processing parameters it is necessary to fully characterize phase composition and crystallographic properties of these films. Since some films are produced by either spinning or dipping successive layers to obtain the desired thickness it was necessary to compare the properties of each layer.

X-ray diffraction techniques employing parallel beam optics with grazing incidence angle geometry were used to characterize the films. Experimental procedures using sealed tube xray diffraction systems to determine differences in crystallite size and microstrain as a function of depth into the films are a rather unique application of this technique. Discerning the contribution to line broadening due to phase changes, grazing incident angle geometry, crystallite size and microstrain are key to the success of this technique.

This paper discusses the experimental techniques employed and will demonstrate how we were able to successfully determine microstrain as a function of depth into the film. We use transmission electron microscopy (TEM) to aid in the characterization of the films. A brief description of the processing procedures used to produce the films is also provided.

The use of grazing incidence parallel beam x-ray diffraction (GIXRD) in the characterization of lead zirconate titanate (PZT) films is described. This tool has enabled us to depth profile the films. The transmission electron microscopy (TEM) results obtained from a cross section of one film are shown to compliment the GIXRD results. The variation in crystallographic structure versus depth in the film was the primary focus of this study.

The insults from three PZT films having Zr/Ti ratios of 25/75, 48/52, and 75/25 are given. TEM results are reported from the sample with a Zr/Ti ratio of 48/52.

Transmission electron microscopy of leached NaOċ3SiO2 and K2Oċ3SiO2 glasses showed that the hydrateg glass surface is a silica rich gel which phase separates during leaching. Phase separation is initiated when pockets of an aqueous phase nucleate and grow in the hydrated silica matrix. The aqueous pockets eventually become a network of interconnected pores with a pore diameter of ∼30 nm. In advanced stages of leaching, the remaining interconnected silica rich phase resembles an aggregation of colloidal silica particles. The observed phase separation is consistent with literature models concerning the chemistry of silica in aqueous solutions and in leached glass.

Surface layers are a common feature of leached surfaces of borosilicate waste glasses. Layers are also observed upon weathering of volcanic glasses[l] and of silicate minerals[2]. The question of whether these layers can protect the glass against further attack by decreasing the leach rate is stïll a subject of controversy[3]. Both in geochemical work[4] and in work on waste forms [5,6], surface layers are attributed a protective function, and the stability of leached, million years old volcanic glasses[1] may be due to the presence of palagonite, a thin (≤100 μm) alteration layer, which forms in a few years but does not seem to increase in thickness after this time. The present study investigates the effects of layer formation on leaching kinetics of a borosilicate waste glass containing 20 wt.% LWR-type simulated waste oxides.

The first observations of physical and chemical changes induced by lead implantation damage and leaching are reported for two proposed U.S. nuclear waste forms (PNL 76–68 borosilicate glass and Sandia titanate ceramics) for commercial wastes. To simulate the effects of recoil nucleii due to alpha decay, the materials were implanted with lead ions at equivalent doses up to approximately 1 × 1019 a decays/cm3 . In the titanate waste form, the zirconolite, perovskite, hollandite, and rutile phases all exhibited a mottled appearance in the transmission electron microscope (TEM) typical of defect clusters in radiation damaged, crystalline solids. One titanate phase containing uranium was found by TEM to be amorphous after implantation at the highest dose. No enhanced leaching (deionized water, room temperature, 24 hours) of the irradiated titanate waste form, including the amorphous phase, was detected by TEM, but Rutherford backscattering (RBS) suggested a loss of cesium and calcium after 21 hours of leaching. The RBS spectra also indicated enhanced leaching from the PNL 76–68 borosilicate glass after implantation with lead ions, in general agreement with the observations of Dran, et al. [6,7] on other irradiated materials. Elastic recoil detection spectroscopy (ERD), used to profile hydrogen after leaching, showed penetration of the hydrogen to several thousand angstroms for both the implanted and unimplanted materials. These basic studies identified techniques to follow the changes that occur on implantation and leaching of complex amorphous and crystalline waste forms. These studies were not designed to produce comparisons between waste forms of gross leach rates.

Zirconolites, CaZrTi2O7, from Sri Lanka and Pala Bora, South Africa, and a calzirtite, CaZr3 TiO9, from Jacupiranga, Brazil, were examined using the electron microprobe, x-ray diffraction (annealing study), transmission electron microscopy, scanning electron microscopy and optical microscopy. The x-ray data indicate that all three zirconolites are metamict. Both Sri Lanka zirconolites are amorphous to the limits of resolution of the electron microscope (֮10 A). The Pala Bora zirconolite is largely amorphous but contains isolated domains (50–200 A) of crystalline material which may be the result of post—metamict recrystallization and alteration. The only other significant evidence for chemical alteration was the lower Th concentration (1–2 weight percent) and slightly lower analytic totals for the rims of the Sri Lanka zirconolites. Upon annealing at 1130°C for 5 hours, all three zirconolites recrystallized as microcrystalline aggregates. Refined unit cell parameters and volumes are consistent with published data for synthetic zirconolites. Both Sri Lanka zirconolites contain microvoids, spherical in shape, and 200 Angstroms to 2 microns in size. This porosity may be the result of helium accumulation arising from the decay of U and Th. The calzirtite was highly crystalline, exhibited no porosity, and was unchanged by the annealing treatment.