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Determining the age of the geomagnetic field is of paramount importance for understanding the evolution of the planet because the field shields the atmosphere from erosion by the solar wind. The absence or presence of the geomagnetic field also provides a unique gauge of early core conditions. Evidence for a geomagnetic field 4.2 billion-year (Gy) old, just a few hundred million years after the lunar-forming giant impact, has come from paleomagnetic analyses of zircons of the Jack Hills (Western Australia). Herein, we provide new paleomagnetic and electron microscope analyses that attest to the presence of a primary magnetic remanence carried by magnetite in these zircons and new geochemical data indicating that select Hadean zircons have escaped magnetic resetting since their formation. New paleointensity and Pb-Pb radiometric age data from additional zircons meeting robust selection criteria provide further evidence for the fidelity of the magnetic record and suggest a period of high geomagnetic field strength at 4.1 to 4.0 billion years ago (Ga) that may represent efficient convection related to chemical precipitation in Earth’s Hadean liquid iron core.

Studying the anisotropic physical properties of hexagonal closed-packed (hcp) iron is essential for understanding the properties of the Earth’s inner core related to the preferred orientation of the inner core materials suggested by seismic observations. Investigating the anisotropic physical properties of hcp iron requires (1) the synthesis of hcp iron samples that exhibit several distinctive types of strong lattice preferred orientation (LPO) and (2) the quantitative LPO analysis of the samples. Here, we report the distinctive LPO of hcp iron produced from single-crystal body-centered cubic (bcc) iron compressed along three different crystallographic orientations ([100], [110], and [111]) in a diamond anvil cell based on synchrotron multiangle X-ray diffraction measurements up to 80 GPa and 300 K. The orientation relationships between hcp iron and bcc iron are consistent with the Burgers orientation relationship with variant selection. We show that the present method is a way to synthesize hcp iron with strong and characteristic LPO, which is beneficial for experimentally evaluating the anisotropic physical properties of hcp iron.

High-pressure single-crystal X-ray diffraction patterns on five synthetic Mg-Al tourmalines with near end-member compositions [dravite NaMg3Al6Si6O18(BO3)3(OH)3OH, K-dravite KMg3Al6Si6O18(BO3)3(OH)3OH, magnesio-foitite ∎(Mg2Al)Al6Si6O18(BO3)3(OH)3OH, oxy-uvite CaMg3Al6Si6O18(BO3)3(OH)3O, and olenite NaAl3Al6Si6O18(BO3)3O3OH, where ∎ represents an X-site vacancy] were collected to 60 GPa at 300 K using a diamond-anvil cell and synchrotron radiation. No phase transitions were observed for any of the investigated compositions. The refined unit-cell parameters were used to constrain third-order Birch-Murnaghan pressure-volume equation of states with the following isothermal bulk moduli (K0 in GPa) and corresponding pressure derivatives (K'0 = δK0/δP)T: dravite K0 = 97(6), K'0 = 5.0(5); K-dravite K0 = 109(4), K'0 = 4.3(2); oxy-uvite K0 = 110(2), K'0 = 4.1(1); magnesio-foitite K0 = 116(2), K'0 = 3.5(1); olenite K0 = 116(6), K'0 = 4.7(4). Each tour-maline exhibits highly anisotropic behavior under compression, with the c axis 2.8-3.6 times more compressible than the a axis at ambient conditions. This anisotropy decreases strongly with increasing pressure and the c axis is only 14% more compressible than the a axis near 60 GPa. The octahedral Y- and Z-sites' composition exerts a primary control on tourmaline's compressibility, whereby Al content is correlated with a decrease in the c-axis compressibility and a corresponding increase in K0 and K'0. Contrary to expectations, the identity of the X-site-occupying ion (Na, K, or Ca) does not have a demonstrable effect on tourmaline's compression curve. The presence of a fully vacant X site in magnesio-foitite results in a decrease of K'0 relative to the alkali and Ca tourmalines. The decrease in K'0 for magnesio-foitite is accounted for by an increase in compressibility along the a axis at high pressure, reflecting increased compression of tourmaline's ring structure in the presence of a vacant X site. This study highlights the utility of synthetic crystals in untangling the effect of composition on tourmaline's compression behavior.

The high-pressure behavior of dravite tourmaline [Na(Mg3)Al6(Si6O18)(BO3)3(OH)3(OH)] has been studied using luminescence spectroscopy and synchrotron-based single-crystal diffraction up to ∼65 and ∼24 GPa, respectively. Two emission bands associated with Cr3+/V2+ substitution are constant in energy up to ∼9.0 GPa, and they shift to longer wavelength at higher pressures, suggesting that a change in compressional mechanism could occur at this pressure. Single-crystal diffraction data show subtle changes in ring ditrigonality occur near 9.0 GPa, which could cause the observed change in luminescence. Near 15 GPa, a splitting of one of the emission bands is observed, suggesting that a phase transition occurs at this pressure and that two unique octahedral sites are present in the high-pressure phase. Hysteresis is not observed on decompression, which indicates that this is a second-order transition, and the high-pressure structure appears to be metastable up to ∼65 GPa. Single-crystal diffraction measurements show that a phase transition from rhombohedral R3m to rhombohedral R3 occurs at pressures near 15.4 GPa. The high-pressure phase is characterized by a distorted Si6O18 ring (e.g., the Si-Si-Si angles deviate from 120°), and the Si, Al, O6, O7, and O8 sites of the low-pressure phase split, implying that the high-pressure phase of tourmaline is a higher entropy phase. The large X-site exerts the primary control on compressibility, and the substitution of larger cations into this site will likely lower the pressure at which this transition occurs. Dravite tourmaline shows anisotropic compression with the c-axis being more compressible than the a-axis. The pressure and volume data up to ∼15.4 GPa were fit with second- and third-order Birch-Murnaghan equations of state. We obtain a bulk modulus, K0 = 109.6(3.2) GPa, and a pressure derivative, K0' = 4.6(8) GPa, and with the pressure derivative set to 4, a bulk modulus of 112.0(1.0) GPa is derived. Moreover, our high-pressure results show that massive overbonding of the X and Y sites can be accommodated by the tourmaline structure. This unexpected result may explain the extraordinary structural tolerance with respect to chemical substitution on the X, Y, and Z sites.

In view of recently reported discrepancies in mineral solubility results obtained with the classical diamond trap method, an alternative approach to quantify the composition of high P–T fluids was developed. In this approach the high P–T fluids are trapped in laser-drilled holes within single-crystal diamond plates and subsequently analyzed by LA–ICP–MS using the same pit size as the one that was used to drill the holes, which allows more rigorous testing of the data reproducibility than in the case of the classical diamond trap, where the fluid resides in a large, open network. To reduce the spikiness of the LA–ICP–MS signals and minimize element fractionation, the aqueous solution within the holes was allowed to evaporate, and the solid residue was melted to a glass. Because this results in the partial loss of the internal standard elements that are usually used for quantifying the LA–ICP–MS signals we developed a new quantification procedure that works without any internal standard in the fluid but instead uses the carbon signal produced by the epoxy that was filled into the holes after melting the precipitates. The new method was first tested on holes filled with epoxy resins doped with known amounts of chemicals, then on holes filled with known amounts of minerals that were subsequently melted, and finally on real high P–T mineral solubility experiments at 1.0 GPa and 700–900 °C in the quartz–H2O and olivine–enstatite–H2O systems, for which reliable reference data exist. In all 15 experiments the measured concentrations agree within 1–21% (avg. 13%) with the reference values. In contrast, four mineral solubility experiments that were performed at identical conditions with the classical diamond trap method returned concentrations that deviated by 7–56% (avg. 28%) from the reference value. Furthermore, a strong fractionation effect that has been observed during the ablation of albite + H2O in a classical diamond trap is efficiently prevented in our single-crystal diamond trap (SCDT) approach. On the downside, we observe significant mobility of alkalies during the melting step in our approach.

The structure and isothermal equation of state of aragonite were determined to 40 GPa using synchrotron single-crystal X-ray techniques. In addition, powder diffraction techniques were used to determine thermal expansion between 298-673 K. At room temperature, aragonite has orthorhombic Pnma structure to 40 GPa, with an isothermal bulk modulus of 66.5(7) GPa and K' = 5.0(1). Between 25-30 GPa the aragonite unit cell begins to distort due to a stiffening of the c-axis compressibility, which is controlled by the orientation and distortion of the carbonate groups. The ambient pressure thermal expansion measurements yielded thermal expansion coefficients a0 = 4.9(2) × 10-5 and a1 = 3.7(5) × 10-8. The combined results allow the derivation of a thermal equation of state. The new data provide constraints on the behavior of carbonates and carbon cycling in the Earth's crust and mantle.

We report the crystal structure of dolomite-IV, a high-pressure polymorph of Fe-dolomite stabilized at 115 GPa and 2500 K. It is orthorhombic, space group Pnma, a = 10.091(3), b = 8.090(7), c = 4.533(3) A, V = 370.1(4) A3 at 115.2 GPa and ambient temperature. The structure is based on the presence of threefold C3O9 carbonate rings, with carbon in tetrahedral coordination. The starting Fe-dolomite single crystal during compression up to 115 GPa transforms into dolomite-II (at 17 GPa) and dolomite-IIIb (at 36 GPa). The dolomite-IIIb, observed in this study, is rhombohedral, space group R3, a = 11.956(3), c = 13.626(5) A, V = 1686.9(5) A3 at 39.4 GPa. It is different from a previously determined dolomite-III structure, but topologically similar. The density increase from dolomite-IIIb to dolomite IV is ca. 3%. The structure of dolomite-IV has not been predicted, but it presents similarities with the structural models proposed for the high-pressure polymorphs of magnesite, MgCO3 A ring-carbonate structure match with spectroscopic analysis of high-pressure forms of magnesite-siderite reported in the literature, and, therefore, is a likely candidate structure for a carbonate at the bottom of the Earth's mantle, at least for magnesitic and dolomitic compositions.

The single-crystal elastic moduli of minerals and related materials with cubic symmetry have been collected and evaluated. The compiled data set covers measurements made over an approximately 70 year period and consists of 206 compositions. More than 80% of the database is comprised of silicates, oxides, and halides, and approximately 90% of the entries correspond to one of six crystal structures (garnet, rocksalt, spinel, perovskite, sphalerite, and fluorite). Primary data recorded are the composition of each material, its crystal structure, density, and the three independent nonzero adiabatic elastic moduli (C11, C12, and C44). From these, a variety of additional elastic and acoustic properties are calculated and compiled, including polycrystalline aggregate elastic properties, sound velocities, and anisotropy factors. The database is used to evaluate trends in cubic mineral elasticity through consideration of normalized elastic moduli (Blackman diagrams) and the Cauchy pressure. The elastic anisotropy and auxetic behavior of these materials are also examined. Compilations of single-crystal elastic moduli provide a useful tool for investigation structure-property relationships of minerals.

Order–disorder transitions in minerals are of significance for technological applications and for the development of models that aid the understanding of the dynamics and composition of the Earth's interior. The present study investigates the effect of Fe content in ankerite, Ca(FexMg1−x)(CO3)2 (0 ≤x≥0.7, R3¯ space group), on the distribution of cations in its crystal structure as a function of temperature. This investigation was conducted using ex situ experiments in a piston cylinder apparatus performed at 2–3 GPa and variable-temperature conditions (450–1000 °C). Crystal structure refinements, using single-crystal X-ray diffraction data, indicate that the temperature of the order–disorder phase transition in ankerite, when the space group changes from R3¯ to R3¯c, is significantly influenced by the amount of Fe in the mineral's crystal structure, being full disordering conditions attained at 1000 and 800 °C in ankerites with x=0.3 and x=0.7, respectively. Prior to undergoing the order–disorder phase transition, it is shown that Fe exhibits a greater aptitude than Mg to exchange in the place of Ca (and vice versa). Mg, conversely, has a tendency to be bound at the M2 site or to exchange in smaller quantities than Fe. Furthermore, the significance of Fe as a parameter influencing the chemo-physical behavior of ankerite, as well as the temperature and character of the disordering process, is highlighted. This has the potential to significantly impact the mineral physics of ankerite under non-ambient conditions, particularly with regard to compressibility, phase stability, thermal and electric conductivity, and its role in the Earth's mantle geophysical modeling.

The first test explosion of a nuclear bomb, the Trinity test of 16 July 1945, resulted in the fusion of surrounding sand, the test tower, and copper transmission lines into a glassy material known as “trinitite.” Here, we report the discovery, in a sample of red trinitite, of a hitherto unknown composition of icosahedral quasicrystal, Si61Cu30Ca₇Fe₂. It represents the oldest extant anthropogenic quasicrystal currently known, with the distinctive property that its precise time of creation is indelibly etched in history. Like the naturally formed quasicrystals found in the Khatyrka meteorite and experimental shock syntheses of quasicrystals, the anthropogenic quasicrystals in red trinitite demonstrate that transient extreme pressure–temperature conditions are suitable for the synthesis of quasicrystals and for the discovery of new quasicrystal-forming systems.