In subsurface imaging and oil recovery where temperatures and salinities are high, it is challenging to design polymer-coated nanoparticles with low retention (high mobility) in porous rock. Herein, the grafting of poly(2-acrylamido-2-methyl-1-propanesulfonic acid-co-acrylic acid) (poly(AMPS-co-AA)) on magnetic iron oxide nanoparticles was sufficiently uniform to achieve low adsorption on model colloidal silica and crushed Berea sandstone in highly concentrated API brine (8% NaCl and 2% CaCl2 by weight). The polymer shell was grafted via amide bonds to an aminosilica layer, which was grown on silica-coated magnetite nanoparticles. The particles were found to be stable against aggregation in American Petroleum Institute (API) brine at 90 °C for 24 h. For IO nanoparticles with ∼23% polymer content, Langmuir adsorption capacities on colloidal silica and crushed Berea Sandstone in batch experiments were extremely low at only 0.07 and 0.09 mg of IO/m2, respectively. Furthermore, upon injection of a 2.5 mg/mL IO suspension in API brine in a column packed with crushed Berea sandstone, the dynamic adsorption of IO nanoparticles was only 0.05 ± 0.01 mg/m2, which is consistent with the batch experiment results. The uniformity and high concentration of solvated poly(AMPS-co-AA) chains on the IO surfaces provided electrosteric stabilization of the nanoparticle dispersions and also weakened the interactions of the nanoparticles with negatively charged silica and sandstone surfaces despite the very large salinities.
Epitaxial barium titanate (BTO) thin films are grown on strontium titanate-buffered Si(001) using atomic layer deposition (ALD) at 225 °C. X-ray diffraction confirms compressive strain in BTO films after the low temperature growth for films as thick as 66 nm, with the BTO c-axis oriented in the out-of-plane direction. Postdeposition annealing above 650 °C leads to an in-plane c-axis orientation. Piezoresponse force microscopy was used to verify the ferroelectric switching behavior of ALD-grown films. Electrical and electro-optic measurements confirm BTO film ferroelectric behavior in out-of-plane and in-plane directions, respectively, at the micrometer scale.
Patterned, crystalline BaTiO 3 (BTO) films were formed directly on STO(001) surfaces using atomic layer deposition and restricting Ba and Ti precursor adsorption to STO(001) by passivating regions of the substrate with a polystyrene blocking layer. Patterns were prepared by spin-coating polystyrene onto STO(001), UVcrosslinking the polystyrene, and rinsing away uncrosslinked polystyrene with toluene. Amorphous 9−12 nm thick BTO films were deposited at 225 °C on polystyrene-patterned STO(001) surfaces. These films were crystallized upon annealing at elevated temperatures. Atomic force microscopy, scanning electron microscopy, and time of flight secondary ion mass spectroscopy were used after growth of BTO and removal of polystyrene resist and reveal BTO features with dimensions similar to the shadow mask. Reflection high-energy electron diffraction and X-ray diffraction show that BTO epitaxially crystallizes to the substrate, forming BTO(001), after annealing under vacuum at ≥770 °C with an oxygen partial pressure of 1 × 10 −6 Torr.
Using in situ X-ray photoelectron spectroscopy, reflection high-energy electron diffraction, and density functional theory, we analyzed the surface core level shifts and surface structure during the initial growth of ABO3 perovskites on Ge (001) by atomic layer deposition, where A = Ba, Sr and B = Ti, Hf, Zr. We find that the initial dosing of the barium- or strontium-bis(triisopropylcyclopentadienyl) precursors on a clean Ge surface produces a surface phase that has the same chemical and structural properties as the 0.5-monolayer Ba Zintl layer formed when depositing Ba by molecular beam epitaxy. Similar binding energy shifts are found for Ba, Sr, and Ge when using either chemical or elemental metal sources. The observed germanium surface core level shifts are consistent with the flattening of the initially tilted Ge surface dimers using both molecular and atomic metal sources. Similar binding energy shifts and changes in dimer tilting with alkaline earth metal adsorption are found with density functional theory calculations. High angle angular dark field scanning transmission microscopy images of BaTiO3, SrZrO3, SrHfO3, and SrHf0.55Ti0.45O3 reveal the location of the Ba (or Sr) atomic columns between the Ge dimers. The results imply that the organic ligands dissociate from the precursor after precursor adsorption on the Ge surface, producing the same Zintl template critical for perovskite growth on Group IV semiconductors during molecular beam epitaxy.
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