Quiet Wing

EMSL’s Quiet Wing supports a wide range of research areas, including climate, biological, environmental and energy systems, of importance to the Department of Energy. It is among the most advanced quiet laboratories in the world for high-resolution imaging capabilities.

The Quiet Wing is a unique research environment housing a suite of ultrasensitive microscopy and scanning instruments. It was designed to help accelerate critical science by allowing state-of-the-art ultrasensitive microscopy equipment to operate at optimal resolution. A temperature-controlled facility, the wing’s design eliminates or reduces to a minimum the vibrations, acoustics and electromagnetic noise that can interfere with the resolution of ultrasensitive scientific instrumentation.

The 9,500-square-foot facility features eight quiet laboratory cells and a sample preparation area. The wing currently houses seven microscopy instruments and has room for one more. These microscopes are just a few of the extensive suite of microscopy instruments at EMSL available for scientific inquiry.

EMSL's microscopy capabilities, including those in the Quiet Wing, are available to the scientific community at typically no cost for openly published research. Scientists gain access to instruments and collaborate with onsite microscopy experts through a peer-reviewed proposal process. Learn more about becoming an EMSL user.

Learn more about each instrument and the science it advances on EMSL's YouTube channel and watch the video below on the Quiet Wing.

Read the brochure.

Instruments

EMSL's ultra-high vacuum, low-temperature scanning probe microscope instrument, or UHV LT SPM, is the preeminent system dedicated to surface...
Custodian(s): Igor Lyubinetsky
Type of Instrument:
Microscope
EMSL's ultra-high vacuum, variable-temperature scanning probe microscope system, or UHV VT SPM, is a state-of-the-art surface science tool...
Custodian(s): Igor Lyubinetsky
EMSL's environmental transmission electron microscope (ETEM) is a state-of-the-art, Cs-corrected field emission gun (FEG) scanning transmission...
Custodian(s): Libor Kovarik
Helium ion microscope The Helium Ion Microscope promises to advance biological, geochemical, biogeochemical, and surface/interface studies using its...
The JEOL JEM-3000SFF was designed for high-resolution cryogenic transmission electron microscopy (cryo-EM) of biological samples and expands EMSL/...

Science Highlights

Posted: August 03, 2014
The Science Nanocatalysts consisting of two metals can offer superior performance compared with those made up of only one metal, so they are widely...
Posted: April 15, 2014
Scientists at EMSL and Pacific Northwest National Laboratory are studying energy storage devices to make them last longer and be able to be...
Posted: March 12, 2014
The Science Lithium-sulfur batteries are promising options for electric vehicles and for storing renewable energy because they can store a lot of...
Posted: March 05, 2014
Lithium-ion batteries fade because the materials lose their structure in response to charging and discharging. This fading relates to electron-rich...
Posted: December 26, 2013
Researchers have developed a way to microscopically view battery electrodes while they are bathed in wet electrolytes, mimicking realistic...

EMSL’s Quiet Wing supports a wide range of research areas, including climate, biological, environmental and energy systems, of importance to the Department of Energy. It is among the most advanced quiet laboratories in the world for high-resolution imaging capabilities.

The Quiet Wing is a unique research environment housing a suite of ultrasensitive microscopy and scanning instruments. It was designed to help accelerate critical science by allowing state-of-the-art ultrasensitive microscopy equipment to operate at optimal resolution. A temperature-controlled facility, the wing’s design eliminates or reduces to a minimum the vibrations, acoustics and electromagnetic noise that can interfere with the resolution of ultrasensitive scientific instrumentation.

The 9,500-square-foot facility features eight quiet laboratory cells and a sample preparation area. The wing currently houses seven microscopy instruments and has room for one more. These microscopes are just a few of the extensive suite of microscopy instruments at EMSL available for scientific inquiry.

EMSL's microscopy capabilities, including those in the Quiet Wing, are available to the scientific community at typically no cost for openly published research. Scientists gain access to instruments and collaborate with onsite microscopy experts through a peer-reviewed proposal process. Learn more about becoming an EMSL user.

Learn more about each instrument and the science it advances on EMSL's YouTube channel and watch the video below on the Quiet Wing.

Read the brochure.

Quantitatively Probing the Al Distribution in Zeolites.

Abstract: 

The degree of substitution of Si4+ by Al3+ in the oxygen-terminated tetrahedra (Al T-sites) of zeolites determines the concentration of ion-exchange and Brønsted acid sites. As the location of the tetrahedra and the associated subtle variations in bond angles influence the acid strength, quantitative information about Al T-sites in the framework is critical to rationalize catalytic properties and to design new catalysts. A quantitative analysis is reported that uses a combination of extended X-ray absorption fine structure (EXAFS) analysis and 27Al MAS NMR spectroscopy supported by DFT-based molecular dynamics simulations. To discriminate individual Al atoms, sets of ab initio EXAFS spectra for various T-sites are generated from DFT-based molecular dynamics simulations allowing quantitative treatment of the EXAFS single- and multiple-photoelectron scattering processes out to 3-4 atom shells surrounding the Al absorption center. It is observed that identical zeolite types show dramatically different Al-distributions. A preference of Al for T-sites that are part of one or more 4-member rings in the framework over those T-sites that are part of only 5- and 6-member rings in the HBEA150 sample has been determined from a combination of these methods. This work was supported by the U. S. Department of Energy (DOE), Office of Basic Energy Sciences, Division of Chemical Sciences, Geosciences & Biosciences.

Citation: 
Vjunov A, JL Fulton, T Huthwelker, S Pin, D Mei, GK Schenter, N Govind, DM Camaioni, JZ Hu, and JA Lercher.2014."Quantitatively Probing the Al Distribution in Zeolites."Journal of the American Chemical Society 136(23):8296-8306. doi:10.1021/ja501361v
Authors: 
A Vjunov
JL Fulton
T Huthwelker
S Pin
D Mei
GK Schenter
N Govind
DM Camaioni
JZ Hu
JA Lercher
Instruments: 
Volume: 
136
Issue: 
23
Pages: 
8296-8306
Publication year: 
2014

Molecular Structure and Stability of Dissolved Lithium Polysulfide Species.

Abstract: 

Ability to predict the solubility and stability of lithium polysulfide is vital in realizing longer lasting lithium-sulfur batteries. Herein we report a combined computational and experimental spectroscopic analysis to understand the dissolution mechanism of lithium polysulfide species in an aprotic solvent medium. Multinuclear NMR and sulfur K-edge X-ray absorption (XAS) analysis reveals that the lithium exchange between polysulfide species and solvent molecule constitutes the first step in the dissolution process. Lithium exchange leads to de-lithiated polysulfide ions which subsequently forms highly reactive free radicals through disproportion reaction. The energy required for the disproportion and possible dimer formation reactions of the polysulfide species are analyzed using density functional theory (DFT) calculations. We validate our calculations with variable temperature electron spin resonance (ESR) measurements. Based on these findings, we discuss approaches to optimize the electrolyte in order to control the polysulfide solubility. The energy required for the disproportion and possible dimer formation reactions of the polysulfide species are analyzed using density functional theory (DFT) calculations. We validate our calculations with variable temperature electron spin resonance (ESR) measurements. Based on these findings, we discuss approaches to optimize the electrolyte in order to control the polysulfide solubility.

Citation: 
Vijayakumar M, N Govind, ED Walter, SD Burton, AK Shukla, A Devaraj, J Xiao, J Liu, CM Wang, AM Karim, and S Thevuthasan.2014."Molecular Structure and Stability of Dissolved Lithium Polysulfide Species."Physical Chemistry Chemical Physics. PCCP 16(22):10923-10932. doi:10.1039/c4cp00889H
Authors: 
M Vijayakumar
N Govind
ED Walter
SD Burton
AK Shukla
A Devaraj
J Xiao
J Liu
CM Wang
AM Karim
S Thevuthasan
Instruments: 
Volume: 
16
Issue: 
22
Pages: 
10923-10932
Publication year: 
2014

Electrochemically Stable Cathode Current Collectors for Rechargeable Magnesium Batteries .

Abstract: 

Rechargeable Mg batteries are attractive energy storage systems and could bring cost-effective energy solutions. Currently, however, no practical cathode current collectors that can withstand high voltages in Mg2+ electrolytes has been identified and therefore cathode research is greatly hindered. Here we identified that two metals, Mo and W, are electrochemically stable through formation of surface passive layers. The presented results could have significant impacts on the developments of high voltage Mg batteries.

Citation: 
Cheng Y, TL Liu, Y Shao, MH Engelhard, J Liu, and G Li.2014."Electrochemically Stable Cathode Current Collectors for Rechargeable Magnesium Batteries ."Journal of Materials Chemistry A 2(8):2473 - 2477. doi:10.1039/C3TA15113A
Authors: 
Y Cheng
TL Liu
Y Shao
MH Engelhard
J Liu
G Li
Facility: 
Instruments: 
Volume: 
Issue: 
Pages: 
Publication year: 
2014

Highly Active and Stable MgAl2O4 Supported Rh and Ir Catalysts for Methane Steam Reforming: A Combined Experimental and

Abstract: 

In this work we present a combined experimental and theoretical investigation of stable MgAl2O4 spinel-supported Rh and Ir catalysts for the steam methane reforming (SMR) reaction. Firstly, catalytic performance for a series of noble metal catalysts supported on MgAl2O4 spinel was evaluated for SMR at 600-850°C. Turnover rate at 850°C follows the order: Pd > Pt > Ir > Rh > Ru > Ni. However, Rh and Ir were found to have the best combination of activity and stability for methane steam reforming in the presence of simulated biomass-derived syngas. It was found that highly dispersed ~2 nm Rh and ~1 nm Ir clusters were formed on the MgAl2O4 spinel support. Scanning Transition Electron Microscopy (STEM) images show that excellent dispersion was maintained even under challenging high temperature conditions (e.g. at 850°C in the presence of steam) while Ir and Rh catalysts supported on Al2O3 were observed to sinter at increased rates under the same conditions. These observations were further confirmed by ab initio molecular dynamics (AIMD) simulations which find that ~1 nm Rh and Ir particles (50-atom cluster) bind strongly to the MgAl2O4 surfaces via a redox process leading to a strong metal-support interaction, thus helping anchor the metal clusters and reduce the tendency to sinter. Density functional theory (DFT) calculations suggest that these supported smaller Rh and Ir particles have a lower work function than larger more bulk-like ones, which enables them to activate both water and methane more effectively than larger particles, yet have a minimal influence on the relative stability of coke precursors. In addition, theoretical mechanistic studies were used to probe the relationship between structure and reactivity. Consistent with the experimental observations, our theoretical modeling results also suggest that the small spinel-supported Ir particle catalyst is more active than the counterpart of Rh catalyst for SMR. This work was financially supported by the United States Department of Energy (DOE)’s Bioenergy Technologies Office (BETO) and performed at the Pacific Northwest National Laboratory (PNNL). PNNL is a multi-program national laboratory operated for DOE by Battelle Memorial Institute. Computing time was granted by a user proposal at the Molecular Science Computing Facility in the William R. Wiley Environmental Molecular Sciences Laboratory (EMSL) located at PNNL. Part of the computational time was provided by the National Energy Research Scientific Computing Center (NERSC).

Citation: 
Mei D, VA Glezakou, VMC Lebarbier, L Kovarik, H Wan, KO Albrecht, MA Gerber, RJ Rousseau, and RA Dagle.2014."Highly Active and Stable MgAl2O4 Supported Rh and Ir Catalysts for Methane Steam Reforming: A Combined Experimental and Theoretical Study."Journal of Catalysis 316:11-23. doi:10.1016/j.jcat.2014.04.021
Authors: 
D Mei
VA Glezakou
VMC Lebarbier
L Kovarik
H Wan
KO Albrecht
MA Gerber
RJ Rousseau
RA Dagle
Facility: 
Instruments: 
Volume: 
Issue: 
Pages: 
Publication year: 
2014

Mineralization of Basalts in the CO2-H2O-SO2-O2 System.

Abstract: 

Sequestering carbon dioxide (CO2) containing minor amounts of co-contaminants in geologic formations was investigated in the laboratory through the use of high pressure static experiments. Five different basalt samples were immersed in water equilibrated with supercritical CO2 containing 1wt% sulfur dioxide (SO2) and 1wt% oxygen (O2) at reservoir conditions (~100 bar, 90°C) for 49 and 98 days. Gypsum (CaSO4) was a common precipitate, occurred early as elongated blades with striations, and served as substrates for other mineral products. Bimodal pulses of water released during dehydroxylation were key indicators along with X-ray diffraction for verifying the presences of jarosite-alunite group minerals. Well-developed pseudocubic jarosite crystals formed surface coatings, and in some instances mixtures of natrojarosite and natroalunite aggregated into spherically shaped structures measuring 100 μm in diameter. Reaction products were also characterized using infrared spectroscopy, which indicated OH and Fe-O stretching modes. The presences of jarosite-alunite group minerals were found in the lower wavenumber region from 700–400 cm-1. A strong preferential incorporation of Fe(III) into natrojarosite was attributed to the oxidation potential of O2. Evidence of CO2 was detected during thermal decomposition of precipitates, suggesting the onset of mineral carbonation.

Citation: 
Schaef HT, JA Horner, AT Owen, CJ Thompson, JS Loring, and BP McGrail.2014."Mineralization of Basalts in the CO2-H2O-SO2-O2 System."Environmental Science & Technology 48(9):5298-5305. doi:10.1021/es404964j
Authors: 
HT Schaef
JA Horner
AT Owen
CJ Thompson
JS Loring
BP McGrail
Volume: 
48
Issue: 
9
Pages: 
5298-5305
Publication year: 
2014

Basophile: Accurate Fragment Charge State Prediction Improves Peptide Identification Rates.

Abstract: 

In shotgun proteomics, database search algorithms rely on fragmentation models to predict fragment ions that should be observed for a given peptide sequence. The most widely used strategy (Naive model) is oversimplified, cleaving all peptide bonds with equal probability to produce fragments of all charges below that of the precursor ion. More accurate models, based on fragmentation simulation, are too computationally intensive for on-the-fly use in database search algorithms. We have created an ordinal-regression-based model called Basophile that takes fragment size and basic residue distribution into account when determining the charge retention during CID/higher-energy collision induced dissociation (HCD) of charged peptides. This model improves the accuracy of predictions by reducing the number of unnecessary fragments that are routinely predicted for highly-charged precursors. Basophile increased the identification rates by 26% (on average) over the Naive model, when analyzing triply-charged precursors from ion trap data. Basophile achieves simplicity and speed by solving the prediction problem with an ordinal regression equation, which can be incorporated into any database search software for shotgun proteomic identification.

Citation: 
Wang D, S Dasari, MC Chambers, JD Holman, K Chen, D Liebler, DJ Orton, SO Purvine, ME Monroe, CY Chung, KL Rose, and DL Tabb.2013."Basophile: Accurate Fragment Charge State Prediction Improves Peptide Identification Rates."Genomics, Proteomics & Bioinformatics 11(2):86-95. doi:10.1016/j.gpb.2012.11.004
Authors: 
D Wang
S Dasari
MC Chambers
JD Holman
K Chen
D Liebler
DJ Orton
SO Purvine
ME Monroe
CY Chung
KL Rose
DL Tabb
Facility: 
Instruments: 
Volume: 
11
Issue: 
2
Pages: 
86-95
Publication year: 
2013

Enzyme-Directed Assembly of Nanoparticles in Tumors Monitored by In Vivo Whole Animal and Ex Vivo Super-Resolution Fluorescence

Abstract: 

Matrix metalloproteinase enzymes, overexpressed in HT-1080 human fibrocarcinoma tumors, were used to guide the accumulation and retention of an enzyme-responsive nanoparticle in a xenograft mouse model. The nanoparticles were prepared as micelles from amphiphilic block copolymers bearing a simple hydrophobic block, and a hydrophilic peptide brush. The polymers were end-labeled with Alexa Fluor 647 dyes leading to the formation of labeled micelles upon dialysis of the polymers from DMSO to aqueous buffer. This dye-labeling strategy allowed the presence of the retained material to be visualized via whole animal imaging in vivo, and in ex vivo organ analysis following intratumoral injection into HT-1080 xenograft tumors. We propose that the material is retained by virtue of an enzyme-induced accumulation process whereby particles change morphology from 20 nm spherical micelles to micron-scale aggregates, kinetically trapping them within the tumor. This hypothesis is tested here via an unprecedented super resolution fluorescence analysis of ex vivo tissue slices confirming a particle size increase occurs concomitantly with extended retention of responsive particles compared to unresponsive controls.

Citation: 
Chien MP, AS Carlini, D Hu, CV Barback, AM Rush, DJ Hall, G Orr, and NC Gianneschi.2013."Enzyme-Directed Assembly of Nanoparticles in Tumors Monitored by In Vivo Whole Animal and Ex Vivo Super-Resolution Fluorescence Imaging."Journal of the American Chemical Society 135(50):18710-18713. doi:10.1021/ja408182p
Authors: 
MP Chien
AS Carlini
D Hu
CV Barback
AM Rush
DJ Hall
G Orr
NC Gianneschi
Facility: 
Instruments: 
Volume: 
135
Issue: 
50
Pages: 
18710-18713
Publication year: 
2013

A Facile Approach Using MgCl2 to Formulate High Performance Mg2+ Electrolytes for Rechargeable Mg Batteries.

Abstract: 

Rechargeable Mg batteries have been regarded as a viable battery technology for grid scale energy storage and transportation applications. However, the limited performance of Mg2+ electrolytes has been a primary technical hurdle to develop high energy density rechargeable Mg batteries. In this study, MgCl2 is demonstrated as a non-nucleophilic and cheap Mg2+ source in combining with Al Lewis acids (AlCl3, AlPh3 and AlEtCl2) to formulate a series of Mg2+ electrolytes characteristic of high oxidation stability (up to 3.4 V vs Mg), sulfur compatibility and electrochemical reversibility (up to 100% coulombic efficiency). Three electrolyte systems (MgCl2-AlCl3, MgCl2-AlPh3, and MgCl2-AlEtCl2) were prepared free of purification and fully characterized by multinuclear NMR (27Al{1H} and 25Mg{1H}) spectroscopies, single crystal X-ray diffraction, and electrochemical analysis. The reaction mechanism of MgCl2 and the Al Lewis acids in THF is discussed to highlight the formation of the electrochemically active [(µ-Cl)3Mg2(THF)6]+ monocation in these electrolytes. We are grateful for the financial support from the Pacific Northwest National Laboratory (PNNL)-Laboratory Directed Research and Development (LDRD) program for developing magnesium battery technology. The XRD and SEM data were collected at the Environmental Molecular Sciences Laboratory, a national scientific user facility sponsored by the DOE’s Office of Biological and Environmental Research and located at PNNL. PNNL is a multiprogram laboratory operated by Battelle Memorial Institute for the Department of Energy under Contract DE-AC05-76RL01830.

Citation: 
Liu TL, Y Shao, G Li, M Gu, JZ Hu, S Xu, Z Nie, X Chen, CM Wang, and J Liu.2014."A Facile Approach Using MgCl2 to Formulate High Performance Mg2+ Electrolytes for Rechargeable Mg Batteries."Journal of Materials Chemistry A 2(10):3430 - 3438. doi:10.1039/c3ta14825d
Authors: 
TL Liu
Y Shao
G Li
M Gu
JZ Hu
S Xu
Z Nie
X Chen
CM Wang
J Liu
Volume: 
Issue: 
Pages: 
Publication year: 
2014

Metal-Insulator Photocathode Heterojunction for Directed Electron Emission.

Abstract: 

New photocathode materials capable of producing intense and directed electron pulses are needed for development of next generation light sources and dynamic transmission electron microscopy. Ideal photocathodes should have high photoemission quantum efficiency (QE) and be capable of delivering collimated and well-shaped pulses of consistent charge under high-field operating conditions. High-brightness and low-intrinsic emittance electron pulses have been predicted for hybrid metal-insulator photocathode designs constructed from three to four monolayer MgO films on atomically flat silver. Here we use angle-resolved photoelectron spectroscopy to confirm directional photoemission and a large increase in QE under ultraviolet laser excitation of an ultrathin MgO film on Ag(001). We observe new low-binding energy photoemission, not seen for Ag(001), and greater electron emission in the normal direction. Under 4.66 eV laser excitation, the photoemission quantum efficiency of the MgO/Ag(001) hybrid photocathode is a factor of seven greater than that for clean Ag(001).

Citation: 
Droubay TC, SA Chambers, AG Joly, WP Hess, K Nemeth, KC Harkay, and L Spentzouris.2014."Metal-Insulator Photocathode Heterojunction for Directed Electron Emission."Physical Review Letters 112(6):067601(5). doi:10.1103/PhysRevLett.112.067601
Authors: 
TC Droubay
SA Chambers
AG Joly
WP Hess
K Nemeth
KC Harkay
L Spentzouris
Facility: 
Volume: 
Issue: 
Pages: 
Publication year: 
2014

Signatures for Mass Spectrometry Data Quality.

Abstract: 

Ensuring data quality and proper instrument functionality is a prerequisite for scientific investigation. Manual validation for quality assurance is time consuming, expensive and subjective. Metrics for describing various features of LC-MS data have been developed to assist operators in discriminating poor (out of control) and good (in control) datasets. However, the wide variety of instrument specifications and LC-MS configurations precludes applying a simple range of acceptable values or cutoffs for such metrics. We explored a variety of statistical modeling approaches to predict the quality of LC-MS data. Using 1164 manually classified quality control (QC) LC-MS datasets, we fit logistic regression classification models to the QC data to predict whether a dataset is in or out of control. Model parameters were optimized by minimizing a loss function that accounts for the tradeoff between false positive and false negative errors. The optimal logistic regression classifier models detected bad data sets with high sensitivity (i.e. low false negative rate) while maintaining high specificity (i.e. controlling the false positive rate). As an example, predictions for Velos-Orbitrap instrumentation data had a sensitivity of 93.7% in detecting out of control datasets with a false positive rate of 8.3%. In comparison, we investigated the performance of several single metrics in predicting dataset quality. While maintaining a sensitivity of 93.7%, the corresponding false positive rates for these single-metric models unacceptably ranged from 32% to 97.7%. Finally, we evaluated the performance of the

Citation: 
Amidan BG, DJ Orton, BL Lamarche, ME Monroe, RJ Moore, AM Venzin, RD Smith, LH Sego, MF Tardiff, and SH Payne.2014."Signatures for Mass Spectrometry Data Quality."Journal of Proteome Research 13(4):2215-2222. doi:10.1021/pr401143e
Authors: 
BG Amidan
DJ Orton
BL Lamarche
ME Monroe
RJ Moore
AM Venzin
RD Smith
LH Sego
MF Tardiff
SH Payne
Facility: 
Instruments: 
Volume: 
13
Issue: 
4
Pages: 
2215-2222
Publication year: 
2014

Pages