Environmental Molecular Sciences Laboratory

A DOE Office of Science User Facility

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Epitaxial Thin Film XRD

Systems Configuration and Operational Overview

All work involving the following systems and any experiments conducted in EMSL laboratories must be performed in compliance with EMSL practices and permits.

The four-circle X-ray diffractometer is a PANalytical X'Pert MRD PRO system with a horizontal, high-resolution Ω-2Θ goniometer (320 mm radius). An open Eulerian cradle provides two additional axes of rotation (-90° < ψ < 90°, and -360° < Φ < +360°). The X-ray source is a long-fine-focus, ceramic X-ray tube with Cu anode. Normal operating power is 45 kV, 40 mA (1.8 kW). The sample stage supports diverse monolithic specimens in various shapes and sizes.

The incident-beam optic is a line-focus Hybrid monochromator. The Hybrid combines a Göbel mirror with a 4-bounce Ge(220) monochromator to provide an intense, highly collimated beam (ΔΘ ~ 25 arc seconds). The typical receiving optic is an open Xe proportional counter detector with a receiving slit (high-resolution or double-crystal X-ray diffraction). Alternatively, the detector can be placed behind the triple-axis Ge(220) analyzing crystal (Δ2Θ ~ 12 arc seconds). The principal application of this setup is structure analysis of epitaxial thin films (rocking curve measurements, etc.).

Analysis Software

The principal XRD data analysis program is JADE (Materials Data Inc., Livermore, California). JADE supports comprehensive analysis of XRD patterns, including phase identification, peak profile fitting, indexing, unit cell refinement, Rietveld analysis, etc. Available software for thin film applications includes the Bede programs RADS and REFS, as well as the PANalytical programs: X'Pert TextureX'Pert Epitaxy, andWINGIXA.

Reference Database

The principal reference database is the Powder Diffraction File (International Centre for Diffraction Data, Newtown Square, Pennsylvania).

Instrument ID:
1058
Availability: 10 hours a day, 5 days a week

Custodians

Tamas Varga (509) 371-6042 Tamas.Varga@pnnl.gov
Mark Bowden (509) 371-7816 Mark.Bowden@pnnl.gov

Publications

Synthesis of CoFe2O4 NPs surface modified with gold (Au) by a chemical method is presented. Induction heating properties of MNPs are investigated and...
Ferroelectrically induced weak ferromagnetism had been predicted earlier in compounds MTiO3 (M = Fe, Mn, Ni) with the LiNbO3-type structure. In order...
A significant body of current research is aimed at developing methods for numerical simulation of flow and transport in porous media that explicitly...
The adsorption and reaction of formaldehyde (CH2O) on the oxidized rutile TiO2(110) surface were studied by temperature programmed desorption (TPD),...
We report on the preparation and detailed characterization of ferromagnetic Zn1-xCrxO thin films deposited on Si substrates using reactive co-...
Understanding the relationship between non-stoichiometry and physical properties of ultra-thin oxides is of great importance from both scientific and...
Do liquid mixtures, cooled to temperatures below their freezing point, behave as normal liquids? We address this question using nanoscale films of...
Etched silicon microfluidic pore network models (micromodels) with controlled chemical and redox gradients, mineralogy, and microbiology under...
Polarization-induced weak ferromagnetism has been predicted a few years back in perovskite MTiO3 (M = Fe, Mn, Ni) [Fennie, Phys. Rev. Lett. 100,...
We report the development of room-temperature ferromagnetism in chemically synthesized powder samples of Sn1-xFexO2 *0.005*x*0.05* and paramagnetic...
Oxygen adsorption on reduced TiO2(110) is investigated using temperature programmed desorption and electron-stimulated desorption. At low...
We describe in detail a diffusion model used to simulate inert gas transport through supercooled liquid overlayers. In recent work, the transport of...
We investigate the mobility of supercooled liquid toluene, ethylbenzene, and benzene near their respective glass transition temperatures (Tg). The...
GaN template layer strain effects on the growth of InGaN/GaN light emitting diodes (LED) devices were investigated. Seven-period InGaN/GaN multiple...
We report the results of a detailed investigation of sol-gel synthesized nanoscale Zn1-xCoxO powders processed at 350 °C with 0 @ x @ 0.12 to...
The reactions of molecular oxygen with bridging hydroxyl groups, OHb, formed by H2O dissociation on bridging oxygen vacancies of TiO2 (110) are...
Experimental measurements of the properties supercooled liquids at temperatures near theirrespective glass transition temperatures, Tg, are requisite...
The chemistry of benzoquinone (BQ) on TiO2(110) was examined using temperature programmed desorption (TPD), electron energy loss spectroscopy (EELS)...
This work reports the discovery of room-temperature ferromagnetism in 5 - 9 nm sized Ce1-xNixO2 nanoparticles (0.01 = x = 0.10) prepared using a sol-...
We report on synthesis and functional properties of ultra-thin oxide layers synthesized on metal surfaces by room temperature photon irradiation. We...
Molecular beams were used to grow amorphous and crystalline H2O films and to dose HCl on their surface. The adsorption state of HCl on the films was...
Many species of bacteria can couple anaerobic growth to the respiratory reduction of insoluble minerals containing Fe(III) or Mn(III/IV). It has been...
We report the development of room-temperature ferromagnetism (FM), with coercivity Hc = 2850 Oe and saturation magnetization Ms ~ 0.01 emu/g, in...
Recent studies have reported room-temperature ferromagnetism (FM) in Fe doped SnO2. The FM in semiconductors due to transition metal doping has been...
The modification of the Mn charge-state, chemical composition and electronic structure of La0.8Sr0.2MnO3 (LSMO) cathodes for solid oxide fuel cell (...
Electron transporting multiheme cytochromes are essential to the metabolism of microbes that inhabit soils and carry out important biogeochemical...
The reaction of NO with hydroxylated rutile TiO2(110)-1×1 surface (h-TiO2) was investigated as a function of NO coverage using temperature-...
We have used high-energy-resolution x-ray photoelectron spectroscopy to measure valence band offsets at the epitaxial anatase TiO2(002)/n-SrTiO3(001...
Desorption of carbon tetrachloride from beneath an amorphous solid water (ASW) overlayer is explored utilizing a combination of temperature...
This paper presents the results of a comprehensive model-based analysis of a uranium tracer test conducted at the U.S Department of Energy Hanford...
Detailed knowledge of the forces between nanocrystals is very crucial for understanding many generic (e.g., random aggregation/assembly and rheology...
We report on a method to prepare clean and smooth surfaces of InAs (100) along with in-situ high-resolution studies of the nanoscale oxidation of the...
Temperature-programmed desorption (TPD) and reflection absorption infrared spectroscopy (RAIRS) are used to investigate the crystallization kinetics...
We study the diffusivity of three-methyl pentane (3MP) using the permeation of inert gases (Ar,Kr, Xe) through the supercooled created when initially...
Using temperature programmed desorption (TPD) and photon stimulated desorption (PSD), we show that coadsorbates of varying binding energies on the...
Single crystal 6H-SiC wafers were fully amorphized at room temperature or 200 K using 1.0 or 2.0 MeV Au+ ion irradiation. The thickness of the...
Oxide synthesis with controlled functional properties is desirable for a plethora of applications but is elusive due to oxide growth kinetics. Here,...
Titanomagnetite (Fe3-xTixO4) nanoparticles were synthesized by room temperature aqueous precipitation, in which Ti(IV) replaces Fe(III) and is charge...
Polarization-induced weak ferromagnetism has been predicted a few years back in perovskite MTiO3 (M = Fe, Mn, Ni) [Fennie, Phys. Rev. Lett. 100,...
We report high temperature ferromagnetism in Mn (3 - 4 at.%) doped optically transparent indium tin oxide (ITO) films prepared by a sol-gel based...
Quantitative analysis of the 16-mercaptohexadecanoic acid self-assembled monolayer (C16 COOH-SAM) layer thickness on gold nanoparticles (AuNPs) was...
Reduction of hexavalent uranium (UVI) to less soluble tetravalent uranium (UIV) through enzymatic or abiotic redox reactions has the potential to...
Polarization-induced weak ferromagnetism has been predicted recently in LiNbO3-type MTiO3 (M = Fe, Mn, Ni). While coexisting ferroelectric...
Ethylene hydrogenation is a prototypical reaction for catalytic hydrogenation of unsaturated hydrocarbons and as such it has been studied on a number...
Surfaces of titanium dioxide in both rutile and anatase polymorphs have attracted significant attention in catalysis and photochemistry. The (110)...
The free energy profile for electron flow through the bacterial deca-heme cytochrome MtrF has been computed using thermodynamic integration and...
Systematic temperature-programmed desorption (TPD) studies of NO adsorption and reactions on rutile TiO2(110)-1×1 surface reveal several distinct...
High resolution transmission electron microscopy (HRTEM) and density functional calculations are used to study the effect of interface polarity on...
Preparation of clean and smooth surfaces of InAs(100) by hydrogen molecular cleaning (HMC) along with in-situ studies of the nanoscale oxidation of...
Patterned cathodes of calcium-doped lanthanum manganite (LCM) were fabricated on polycrystalline yttria-stabilized zirconia (YSZ) substrates by RF...
RuO2 has proven to be indispensable as a co-catalyst in numerous systems designed for photocatalytic water splitting. In this study we have carried...
Natural 12CaO·7Al2O3 (C12A7) is a wide band gap insulator, but conductivity can be realized by introducing oxygen deficiency. Currently, there are...
Trimethyl acetic acid (TMAA) adsorption evolution on the rutile TiO2(110) surface from submonolayer to saturation coverages was examined at the...
This paper provides an updated overview, intended to be of practical value to analysts, of methods that can be applied to minimize or control the...
Technetium contamination remains a major environmental problem at nuclear reprocessing sites, such as at the Hanford nuclear reservation, Washington...
Ion-induced damage in strontium titanate (SrTiO3) has been investigated using 1.0 MeV Au ions at 150 K and room temperatures. Rutherford...
XPS spectra of HS(CH_2)_15 COOH terminated a self assembled monolayer (SAM)sample was collected over a period of 242 minutes to determine specimen...
Amorphous solid water (ASW) is a metastable form of water created by vapor deposition onto a cold substrate (typically less than 130 K). Since this...
The ability to form reliable, low-resistance Ohmic contacts is of critical importance to the ongoing development of oxide electronics. Most metals...
The influence of reactant coverage on photochemical activity was explored using scanning tunneling microscopy (STM) and ultraviolet photoelectron...
In this paper, we present the results of a detailed investigation of the structural, optical and magnetic properties of chemically synthesized pure...
Three distinctly different characteristic responses of a nickel/yttria-stabilized zirconia (Ni/YSZ) cermet anode to the presence of hydrogen selenide...
Experimental measurements and ab initio modeling of the optical transitions in strained G-type antiferromagnetic LaCrO3 resolve two decades of debate...
We fabricated large area (>1?×?1 cm2), epitaxial Fe nanowire arrays on MgO(001) substrates by nanoimprint lithography with a direct metallization...
Electronic energy loss is the fundamental mechanism accountable for the response of materials to ions. Helium particles are a product from alpha...
Minute changes in oxygen concentration in complex oxides even of the order of ~0.001% can significantly influence functional properties ranging from...
Redox-active transition metal (TM) oxides, hydroxide and oxyhydroxides semiconductors typically posses wide p-d charge-transfer band gaps and exhibit...
Fe-bearing clay minerals serve as an important source and sink for electrons in redox reactions in various subsurface geochemical environments, and...
Dissolution of dense non-aqueous phase liquid (DNAPL) contaminants like tetrachloroethene (PCE) can be “bioenhanced” via biodegradation, which...
The combined experimental and theoretical study of intrinsic hydrogen diffusion on bridge-bonded oxygen (BBO) rows of TiO2(110) is presented. The...
We systematically investigated the possible magnetization reversal behavior in well-characterized, epitaxial, Fe/IrMn exchange-biased bilayers as a...
Flavins are secreted by the dissimilatory iron-reducing bacterium Shewanella and can function as endogenous electron transfer mediators (ETM). In...
Despite the importance of RuO2 in photocatalytic water splitting and catalysis in general, the interactions of water with even its most stable (110)...
The authors report on a magnetic gas sensing methodology to detect hydrogen using the ferromagnetic properties of a nanoscale dilute magnetic...
We present an experimental technique to measure the diffusivity of supercooled liquids at temperatures near their Tg. The approach uses the...
The thermodynamics of mixing and its dependence on cation distribution in the Fe3O4– 14 Fe2TiO4 (magnetite-ulvöspinel) spinel solid solution were...
We provide a detailed theoretical analysis of the character of optical transitions and band gap reduction in (Fe1-xCrx)2O3 solid solutions using...
In a recent work, we have shown that chemically synthesized Sn1-xCoxO2 nanoscale powders with x = 0.01 are ferromagnetic at room-temperature when...
Hydrogen sensing is a critical component of safety to address wide spread public perceptions of the hazards of production, storage, transportation...
We describe in detail a diffusion model used to simulate inert gas transport through supercooled liquid overlayers. In recent work, the transport of...
The photon-stimulated reactions in oxygen adsorbed on reduced TiO2(110) at low temperatures (< 100 K) are studied. The amount of O2 desorbed by UV...
We fabricated large area (>1&thinsp;&times;&thinsp;1 cm2), epitaxial Fe nanowire arrays on MgO(001) substrates by nanoimprint...
We systematically investigated the possible magnetization reversal behavior in well-characterized, epitaxial, Fe/IrMn exchange-biased bilayers as a...
We present an experimental technique to measure the diffusivity of supercooled liquids at temperatures near their Tg. The approach uses the...
Nanostructured materials of various types and forms are formulated in a variety of novel ways and increasingly subject to many types of chemical and...
GaN template layer strain effects on the growth of InGaN/GaN light emitting diodes (LED) devices were investigated. Seven-period InGaN/GaN multiple...
Oxygen adsorption on reduced TiO2(110) is investigated using temperature programmed desorption and electron-stimulated desorption. At low...
Hydrogen bonding, H/D exchange and diffusion in water films (&#61603; 2 monolayers) on TiO2(110) have been studied using water electron-...
Electron-stimulated reactions in thin (< 3 monolayer, ML) water films adsorbed on TiO2(110) are investigated. For electron fluences less than ~1...
Ethylene hydrogenation is a prototypical reaction for catalytic hydrogenation of unsaturated hydrocarbons and as such it has been studied on a number...

Quick Specs

    • Principal application for analysis of epitaxial thin film
    • Normal operating power of 45 kV, 40 mA
    • Supports monolithic specimens of various shapes and sizes

Science Highlights

Posted: Tuesday, December 4, 2018 - 16:12
From Pacific Northwest National Laboratory's Physical Sciences Division Rechargeable lithium (Li) batteries are the most widely used energy storage...
Posted: Monday, August 17, 2015 - 10:15
The performance of solar cells, flat panel displays and other electronics are limited by today's materials. Scientists at Pacific Northwest National...

Projects

This EMSL user proposal requests a continuation of EMSL access for a BER funded Environmental Molecular Sciences Institute (EMSI) project led by Dr....
This activity involves extended that state of the art in surface analysis by expanding the understanding of equipment capability, testing new...
Oxide interfaces, superlattices and solid solutions provide opportunities for generating materials with novel properties, providing the atomic...
This EMSL user proposal aims to elucidate atomistic mechanisms of radiation interaction at the nanoscale in order to achieve a scientific...
Traditional models of mineral formation through monomer-by-monomer addition have been challenged by recent evidence for crystallization through the...