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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1993

Vickers indentation hardness of stoichiometric and reduced single crystal TiO2 (rutile) from 25 to 800 C

The indentation microhardness of stoichiometric and reduced single crystal rutile (TiO2) from 25 to 800 C is presented in this paper. The results serve two main purposes. One is to assess the effect of rutile's stoichiometry on its hardness. The other is to test recently suggested theory on solid lubrication with sub Stoichiometric rutile in an effort to better understand shear controlled phenomenon. Microhardness was measured using a Vickers diamond indentor on both vacuum and hydrogen reduced single crystal rutile from 25 to 800 C. The results indicate that stoichiometry and temperature have a pronounced effect on rutile's hardness. The measured effects lend support to theory on solid lubrication by enhanced crystallographic slip and suggest that solid lubricant materials may be produced by careful atomic level tailoring (stoichiometry control).

Dellacorte, Christopher↗
NASA NTRS1972

Niobian rutile in an Apollo 14 KREEP fragment.

Niobian rutile was found in a KREEP lithic fragment of basaltic texture. The niobian rutile contains 85.3% TiO2, 7.1% Nb2O5, 2.65% Cr2O3, 0.70% ZrO2, 0.61% SiO2, 0.82% Al2O3 0.61% FeO, 0.52% CaO, 0.22% V2O3 in addition to minor amounts of MnO, MgO, and CeO2. Rare-earth elements were not detected, in contrast with lunar niobian rutile of Marvin (1971). Coexisting minerals in the KREEP fragment are major amounts of plagioclase and orthopyroxene, and minor amounts of olivine, ilmenite, augite, barian K-feldspar, whitlockite, troilite, Ni-Fe, zirkelite, and chromite.

Hlava, P. F.↗
NASA NTRS1994

Mossbauer and spectral (visible and near-IR) data for Fe(3+)-substituted rutile

Titanohematite and rutile containing some Fe(3+) are possible highly oxidized weathering products of ilmenite and titanomagnetities. We report here Moessbauer and reflectivity data (visible and near-IR) for Fe(3+)-substituted rutile as a part of our continuing studies of ferric-substituted minerals that might have bearing on the interpretation of Martian spectral data.

Lauer, H. V., Jr.↗
NASA NTRS1966

Meteoritic rutile.

Rutile in meteorites, noting presence of titanium oxide as result of electron microprobe studies

RUTILE↗
NASA NTRS1972

The determination and optimization of (rutile) pigment particle size distributions

A light scattering particle size test which can be used with materials having a broad particle size distribution is described. This test is useful for pigments. The relation between the particle size distribution of a rutile pigment and its optical performance in a gray tint test at low pigment concentration is calculated and compared with experimental data.

Richards, L. W.↗
NASA NTRS1973

Moessbauer spectroscopic studies of iron-doped rutile.

Moessbauer spectra were obtained of single crystal and powdered samples of rutile (TiO2) doped to about one percent by weight in isotopically enriched iron. It is shown that the oxidation state may be reversibly altered in situ. After reduction, the oxygen neighbors of the dopant ion are apparently shifted to accomodate the larger ferrous ion. The agreement of calculated quadrupole splittings with experimental results suggests that impurities and oxygen vacancies are uniformly distributed in powdered samples, giving the dopant ions an 'ideal lattice' local environment. The differences between the single crystal and powder sample hyperfine parameters are attributed to variations in stoichiometry, charge compensation mechanisms, or other diffusion related parameters.

Stampfl, P. P.↗
NASA NTRS2002

Stability of Pseudobrookite-Type Titanium Oxides

Orthorhombic, (Bbmm), (Al, Fe, Cr, Ti)(sub 2) TiO5-(Mg, Fe)Ti2O5 solid solutions (pseudobrookites, s.l.) are found either as an oxidation product of ilmenite and/or spinel or a primary crystallizing phase in igneous and metamorphic rocks on Earth (e.g., basalt flows, crustal and mantle xenoliths, hornfels), and basaltic rocks on the Moon. Moreover, orthorhombic oxides are often part of the crystalline matrix in glass/ceramics with useful applications, and play a major role in the industrial production of TiO2. To fully exploit the potential of these compounds as petrogenetic indicators and/or useful materials we need to quantitatively understand the factors controlling their properties and stability, and thus, to extrapolate beyond the calibrating experiments. For that purpose, we need to combine thermochemistry, phase equilibrium, and in situ P-V-T-cation disorder experimental data that presently either are incomplete or lacking. Perhaps, the most complete data set is that for MgTi2O5 (karrooite) which allows the calibration of models for the Gibbs free energy of the MgTi2O5 as a function of pressure, temperature, and the Mg2+-Ti4+ distribution between the two nonequivalent octahedral sites. Consequently, the effect of cation disorder on MgTi2O5 stability, and the phase relations among MgTi2O5, other titanium oxides, and silicate minerals can be examined. Calculated phase relations in the Mg-Ti-Si-O system and phase equilibrium experiments in Fe-bearing compositions suggest that pseudobrookite-type oxides may be a more common in rocks than previously realized. However, homogeneous and heterogeneous equilibria, and crystallization paths likely affect their stability. For example, isobaric increases in temperature favor disordering and thus entropy-stabilization, in contrast, isothermal increases in pressure have the opposite effect. Although, currently, the potential effect of composition to cation disorder cannot be fully explored, it appears that enrichment in trivalent cations probably enhances entropy-stabilization and thus may increase the stability of (Al, Fe, Cr, Ti)-rich pseudobrookites relative to that of (Mg, Fe)-rich ones. In addition, high-temperature, nearly isothermal, decompression paths of olivine+orthopyroxene+oxide assemblages may favor pseudobrookites (s.l.) over rutile and/or ilmenite, in contrast, cooling at low pressures seems to favor ilmenite and/or rutile. In the case of crustal and mantle xenoliths, the presence or absence of orthorhombic oxides is probably controlled by reactions with olivine, orthopyroxene, ilmenite, and rutile. In oceanic mantle xenoliths such reactions may also involve a TiO2-enriched but not SiO2-enriched melt/fluid, because pseudobrookites (s.l.) would react with the SiO2-enriched melt/fluid to form orthopyroxene and rutile. Parenthetically, experiments and model calculations in the Mg-Ti-Si-O system suggest that low degree partial melting of low-TiO2 bulk compositions may produce Ti-enriched liquids in equilibrium with olivine, orthopyroxen ad=nd MgTi2O5, rutile or ilmenite.

Xirouchakis, Dimistrios↗
NASA NTRSDate not supplied

Mineralogical Analysis of Calcium-Aluminum-Rich Inclusions Provides Insight Into Post-Formation Processes

Introduction: Calcium-aluminum inclusions (CAIs) are cm- to mm-sized intergrowths of refractory phases found in chondritic meteorites [1]. Their mineral compositions closely match the compositions of the solids thought to condense from an extremely hot (>1500K) gas with a bulk solar composition [2-4], suggesting that CAIs were the earliest solids within the Solar System [2-4]. These inclusions provide invaluable insights into the conditions and dynamics of the early Solar System. CAIs must be transported from their formation region near the protosun to the chondrite parent-body accretion region. The nature of their journey could affect how, when, and where the secondary processes recorded in these CAIs occurred [4]. Did these secondary processes occur in the solar nebula or during accretion with the parent body, or both? How were the CAIs affected by varying thermochemical processes? To better answer these questions, we have undertaken an in-depth, textural study of the secondary alteration of select CAI samples. Methods: We chose three CAIs that experienced a range of post-formation processing to gain better understanding of secondary alteration based on previous preliminary examination [5]. Representative CAIs were chosen from NWA 5508 (CV3), NWA 12772 (CV3), and Coolidge (CL4) carbonaceous chondrites. We used scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) techniques for detailed chemical, mineralogical, and textural analysis of the CAIs. Backscattered electron (BSE) images and X-ray elemental maps were taken of Coolidge and NWA 5508 using the Lunar and Planetary Institute (LPI) Phenom SEM. The JEOL 7900F SEM at NASA Johnson Space Center (JSC) was used to obtain energy dispersive spectroscopy (EDS) chemical maps of all samples. High resolution EBSD analysis identified the mineral phases and textures, providing key information on their nature. Based on the SEM and EBSD data, minerals of interest were selected for quantitative chemical electron probe micro-analysis (EPMA) using the JEOL JXA-8530F at NASA JSC. Results and Discussion: The EDS maps show that the NWA 5508 and NWA 12772 CAIs designated “Saguaro” and “Hoopoe” respectively [5] are enriched in calcium while the Coolidge CAI designated “Cottonwood” is aluminum and magnesium rich. Saguaro. A ~1.5cm diameter igneous Type B CAI with a rounded shape. The dominant phases are melilite, spinel, and Al-Ti pyroxene with minor anorthite. Spinel is subhedral and occurs in clusters. Some of these clusters have a circular geometry which encloses other minerals, known as a palisade structure [6] (Fig. 1). Some palisades form near perfect circles while others are more irregular in shape. Melilite in Saguaro ranges in size from coarse (>250m) to fine-grained (5-7m) and forms intergrown laths. A third of the melilite grains exhibit simple twinning about their <001> axis. The spinel palisades and twinned melilite in Saguaro suggest an igneous history, and the lack of secondary minerals suggests minimal aqueous alteration. At some point in time after the initial condensation of the minerals and formation of the inclusion, the sample was remelted and quickly solidified. The formation of the palisades is still heavily debated. One hypothesis is that the palisades are the rims of smaller CAIs that accreted early on, essentially acting as xenoliths within the larger CAIs [7]. Another hypothesis suggests an igneous origin for palisade structures [6-8] wherein the melt traps gas bubbles, and the spinel nucleates on the surface of this bubble. Based on the WDS spot analyses of 41 melilite grains using EPMA, the data suggest that the composition inside and outside the palisades is nearly identical. This finding indicates that these palisades are likely not exogenous but rather formed from melt-vapor reactions. Our results are consistent with studies by Simon and Grossman,1997 [6] and Zhang et al. (2019) [8]. Hoopoe. A ~0.5cm compact Type A CAI with an irregular shape. The dominant mineral phases are melilite, spinel, and hibonite with minor amounts of anorthite, augite, and perovskite. The melilite ranges in size from ~500 to 50µm. The larger melilite grains have simple twinning along the <001> axis like melilite in Saguaro. Melilite in Hoopoe exhibits crystal-plastic strain with misorientation dominantly about the <010> and <110> axes. Spinel shows subhedral to euhedral morphology and appears in clusters. Hibonite grains are similar to spinel in habit and size but show more plastic strain. The two minerals are often found together with one appearing to replace the other. Perovskite appears in fine grained recrystallized regions alongside fine augite and spinel. The abundant strain and deformation features in the melilite and hibonite suggest that Hoopoe experienced shock. This shock could have occurred in the nebula [9] or from an impact of another body on the parent body asteroid. The appearance of fine-grained (<10m) areas of augite, perovskite, and spinel in the dominantly coarse-grained inclusion suggest recrystallization, possibly due to the sudden increase in pressure and temperature. Cottonwood. This ~0.5cm CAI exhibits distinct mineralogy and textures suggesting a high degree of alteration. It is irregular in shape. The dominant mineral phases are spinel and anorthite with minor amounts of augite and rutile. The two main texture types can be seen in Fig. 2. The first type consists of coarse euhedral to subhedral spinel and anorthite. The second includes fine grained spinel, anorthite, rutile, and iron sulfides. Within these fine-grained regions, the anorthite grains are clustered into domains exhibiting the same crystallographic orientation. Rutile exclusively occurs with fine anorthite indicating a potential relationship between the two. Cottonwood has a clear and unbroken Wark-Lovering [10] rim (Fig. 2) on one side that consists of a sequence of spinel followed by anorthite and an outer layer of augite. The abundance of the fine-grained regions containing iron oxides and iron sulfides, secondary phases such as rutile, and oriented anorthite grains is evidence for recrystallization associated with a high degree of thermal metamorphism. The EPMA analyses on both coarse- and fine-grained spinel show that the fine spinel grains are more enriched in Cr (1-2 wt. %) than their coarse counterparts (0.1-0.5 wt. %). The data suggest thermal metamorphism drove chemical exchange of the previously refractory inclusion, introducing chromium and iron as well as sulfur, which is moderately volatile. Conclusions: The three CAIs analyzed record distinct secondary nebular and parent body processes. Saguaro melted in the nebula as seen by the twinned melilite and spinel palisades. Hoopoe experienced intense shock which deformed its melilite and recrystallized perovskite, augite, and spinel in fine-grained regions. Cottonwood shows evidence of recrystallization and chemical changes consistent with thermal metamorphism occurring after accretion into the parent-body.

V E Burnette↗
NASA NTRS1972

TiO2 film properties as a function of processing temperature, volume 3

Thin film TiO2 was produced at 150 C by chemical vapor deposition using hydrolysis of tetraisopropyl titanate. Films were amorphous as grown, but annealing in air caused crystallization, with anatase formed beginning at 350 C and rutile at 700 C. Density and index of refraction increased substantially with increasing anneal temperature, while etch susceptibility in HF and H2SO4 decreased. Comparison with literature data showed two groups of processes. One group yields films having properties that gradually approach those of rutile with increasing process temperature. The other group gives rutile directly at moderate temperatures. Deposition of amorphous film followed by etching and annealing is suggested as a means for pattern definition.

Fitzgibbons, E. T.↗
NASA NTRS1973

Armalcolite and genetically associated opaque minerals in the lunar samples

A comprehensive electron microprobe study of armalcolite in samples from five Apollo sites (11-16), together with analytical data previously reported from Apollo 17 and Luna 20 show that three distinct compositional types of armacolite are present in the lunar samples. These types are classified as armalcolite, Cr-Zr-Ca-armalcolite and Zr-armalcolite. The Zr-free armalcolites are typical of high-Ti mare basalts whereas the Zr-rich armalcolites are typical of non-mare high alumina basalts. The latter armalcolites are in complete oxide intergrowths (baddeleyite, zirconolite, rutile, ilmenite, and chromite) and are in contrast to the Zr-free armalcolites which are commonly only associated with ilmenite. Subsolidus decomposition of armalcolite to an iron and Mg-rich rutile + ilmenite-geikielite, and the solid state formation of armalcolite from magnesium-ilmenite + niobian-rutile are described for the first time in the lunar samples.

Haggerty, S. E.↗
NASA NTRS1971

Mechanism of the oxidation of titanium disilicide.

Study of the oxidation of TiSi2 at temperatures of 300 to 1300 C. Wafers prepared using the techniques of powder metallurgy had densities of 95 to 98% of the theoretical value. On oxidation at temperatures up to 600 C, the polished wafers formed a protective, titania-silica glass. The rate data indicate a complex surface and diffusion-limited mechanism. Above 600 deg C, the oxide consisted of an amorphous SiO2 film with crystalline islands of TiO2 (rutile). From 1000 to 1300 C, parabolic kinetics with an activation energy of 21.3 kcal/mole were observed. These data are consistent with a model in which the rate-determining step is the diffusion of oxygen through the silica film with the simultaneous diffusion of titanium from the substrate to the islands of rutile growing on top of the amorphous silica.

Schwettmann, F. N.↗