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.

Related information:

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
Type of Instrument:
Microscope
The Helium Ion Microscope promises to advance biological, geochemical, biogeochemical, and surface/interface studies using its combined surface...
The JEOL JEM-3000SFF was designed for high-resolution cryogenic transmission electron microscopy (cryo-EM) of biological samples and expands EMSL/...

Science Highlights

Posted: October 07, 2014
The Science Steam reforming is a method for converting biomass-derived light hydrocarbons and aromatics into a mixture of carbon monoxide and...
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...

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.

Related information:

Investigating the Synthesis of Ligated Metal Clusters in Solution Using a Flow Reactor and Electrospray Ionization Mass

Abstract: 

The scalable synthesis of subnanometer metal clusters containing an exact number of atoms is of interest due to the highly size-dependent catalytic, electronic and optical properties of these species. While significant research has been conducted on the batch preparation of clusters through reduction synthesis in solution, the processes of metal complex reduction as well as cluster nucleation, growth and post-reduction etching are still not well understood. Herein, we demonstrate a temperature-controlled flow reactor for studying cluster formation in solution at well-defined conditions. Employing this technique methanol solutions of a chloro(triphenylphosphine)gold precursor, 1,4-bis(diphenylphosphino)butane capping ligand and borane-tert-butylamine reducing agent were combined in a mixing tee and introduced into a heated capillary with an adjustable length. In this manner, the temperature dependence of the relative abundance of different ionic reactants, intermediates and products synthesized in real time was characterized using online mass spectrometry. A wide distribution of doubly and triply charged cationic gold clusters was observed as well as smaller singly charged metal-ligand complexes. The results demonstrate that temperature plays a crucial role in determining the relative population of cationic gold clusters and, in general, that higher temperature promotes the formation of doubly charged clusters and singly charged metal-ligand complexes while hindering the growth of triply charged clusters. Moreover, the distribution of clusters observed at elevated temperatures is found to be consistent with that obtained at longer reaction times at room temperature, thereby demonstrating that heating may be used to access cluster distributions characteristic of different stages of reduction synthesis in solution.

Citation: 
Olivares AM, J Laskin, and GE Johnson.2014."Investigating the Synthesis of Ligated Metal Clusters in Solution Using a Flow Reactor and Electrospray Ionization Mass Spectrometry."Journal of Physical Chemistry A 118(37):8464-8470. doi:10.1021/jp501809r
Authors: 
AM Olivares
J Laskin
GE Johnson
Facility: 
Volume: 
118
Issue: 
37
Pages: 
8464-8470
Publication year: 
2014

Size-dependent stability toward dissociation and ligand binding energies of phosphine-ligated gold cluster ions.

Abstract: 

The stability of sub-nanometer size gold clusters ligated with organic molecules is of paramount importance to the scalable synthesis of monodisperse size-selected metal clusters with highly tunable chemical and physical properties. For the first time, a Fourier transform ion cyclotron resonance mass spectrometer (FT-ICR-MS) equipped with surface induced dissociation (SID) has been employed to investigate the time and collision energy resolved fragmentation behavior of cationic doubly charged gold clusters containing 7-9 gold atoms and 6-7 triphenylphosphine (TPP) ligands prepared by reduction synthesis in solution. The TPP ligated gold clusters are demonstrated to fragment through three primary dissociation pathways: (1) Loss of a neutral TPP ligand from the precursor gold cluster, (2) asymmetric fission and (3) symmetric fission and charge separation of the gold core resulting in formation of complementary pairs of singly charged fragment ions. Threshold energies and activation entropies of these fragmentation pathways have been determined employing Rice-Ramsperger-Kassel-Marcus (RRKM) modeling of the experimental SID data. It is demonstrated that the doubly charged cluster ion containing eight gold atoms and six TPP ligands, (8,6)2+, exhibits exceptional stability compared to the other cationic gold clusters examined in this study due to its large ligand binding energy of 1.76 eV. Our findings demonstrate the dramatic effect of the size and extent of ligation on the gas-phase stability and preferred fragmentation pathways of small TPP-ligated gold clusters.

Citation: 
Johnson GE, TA Priest, and J Laskin.2014."Size-dependent stability toward dissociation and ligand binding energies of phosphine-ligated gold cluster ions."Chemical Science 5:3275-3286. doi:10.1039/c4sc00849a
Authors: 
GE Johnson
TA Priest
J Laskin
Facility: 
Volume: 
Issue: 
Pages: 
Publication year: 
2014

The Mechanisms of Oxygen Reduction and Evolution Reactions in Nonaqueous Lithium-Oxygen Batteries.

Abstract: 

The oxygen reduction/evolution reaction (ORR/OER) mechanisms in nonaqueous Li-O2 batteries have been investigated by using electron paramagnetic resonance spectroscopy in this work. We identified the superoxide radical anion (O2•-) as an intermediate in the ORR process using 5,5-dimethyl-pyrroline N-oxide as a spin trap, while no O2•- in OER was detected during the charge process. These findings provide insightful understanding on the fundamental oxygen reaction mechanisms in rechargeable nonaqueous Li-O2 batteries.

Citation: 
Cao R, ED Walter, W Xu, EN Nasybulin, P Bhattacharya, ME Bowden, MH Engelhard, and J Zhang.2014."The Mechanisms of Oxygen Reduction and Evolution Reactions in Nonaqueous Lithium-Oxygen Batteries."ChemSusChem 7(9):2436-2440. doi:10.1002/cssc.201402315
Authors: 
R Cao
ED Walter
W Xu
EN Nasybulin
P Bhattacharya
ME Bowden
MH Engelhard
J Zhang
Instruments: 
Volume: 
7
Issue: 
9
Pages: 
2436-2440
Publication year: 
2014

Effect of Composition and Heat Treatment on MnBi Magnetic Materials.

Abstract: 

The metallic compound MnBi is a promising rare-earth-free permanent magnet material. Compare to other rare-earth-free candidates, MnBi stands out for its high intrinsic coercivity (Hci) and its large positive temperature coefficient. Several groups have demonstrated that the Hci of MnBi compound in thin film or in powder form can exceed 12 kOe and 26 kOe at 300 K and 523 K, respectively. Such steep increase in Hci with increasing temperature is unique to MnBi. Consequently, MnBi is a highly sought-after hard phase for exchange coupling nanocomposite magnets. The reaction between Mn and Bi is peritectic, so Mn tends to precipitate out of the MnBi liquid during the solidification process. As result, the composition of the Mn-Bi alloy with the largest amount of the desired LTP (low temperature phase) MnBi and highest saturation magnetization will be over-stoichiometric and rich in Mn. The amount of additional Mn required to compensate the Mn precipitation depends on solidification rate: the faster the quench speed, the less Mn precipitates. Here we report a systematic study of the effect of composition and heat treatments on the phase contents and magnetic properties of Mn-Bi alloys. In this study, Mn-Bi alloys with 14 compositions were prepared using conventional metallurgical methods such as arc melting and vacuum heat treatment, and the obtained alloys were analyzed for compositions, crystal structures, phase content, and magnetic properties. The results show that the composition with 55 at.% Mn exhibits the highest LTP MnBi content and the highest magnetization. The sample with this composition shows >90 wt.% LTP MnBi content. Its measured saturation magnetization is 68 emu/g with 2.3 T applied field at 300 K; its coercivity is 13 kOe and its energy product is 12 MGOe at 300 K. A bulk magnet fabricated using this powder exhibits an energy product of 8.2 MGOe.

Citation: 
Cui J, JP Choi, E Polikarpov, ME Bowden, W Xie, G Li, Z Nie, N Zarkevich, MJ Kramer, and DD Johnson.2014."Effect of Composition and Heat Treatment on MnBi Magnetic Materials."Acta Materialia 79:374-381. doi:10.1016/j.actamat.2014.07.034
Authors: 
J Cui
JP Choi
E Polikarpov
ME Bowden
W Xie
G Li
Z Nie
N Zarkevich
MJ Kramer
DD Johnson
Volume: 
Issue: 
Pages: 
Publication year: 
2014

In Situ One-Step Synthesis of Hierarchical Nitrogen-Doped Porous Carbon for High Performance Supercapacitors.

Abstract: 

Electrochemical performance of the existing state-of-the art capacitors is not very high, key scientific barrier is that its charge storage mechanism wholly depends on adsorption of electrolyte on electrode. We present a novel method for the synthesis of nitrogen -doped porous carbons and address the drawback by precisely controlling composition and surface area. Nitrogen-doped porous carbon was synthesized using a self-sacrificial template technique without any additional nitrogen and carbon sources. They exhibited exceptionally high capacitance (239 Fg-1) due to additional pseudocapacitance originating from doped nitrogen. Cycling tests showed no obvious capacitance decay even after 10,000 cycles, which meets the requirement of commercial supercapacitors. Our method is simple and highly efficient for the production of large quantities of nitrogen-doped porous carbons.

Citation: 
Jeon JW, R Sharma, P Meduri, BW Arey, HT Schaef, J Lutkenhaus, JP Lemmon, PK Thallapally, MI Nandasiri, BP McGrail, and SK Nune.2014."In Situ One-Step Synthesis of Hierarchical Nitrogen-Doped Porous Carbon for High Performance Supercapacitors."ACS Applied Materials & Interfaces 6(10):7214-7222. doi:10.1021/am500339x
Authors: 
JW Jeon
R Sharma
P Meduri
BW Arey
HT Schaef
J Lutkenhaus
JP Lemmon
PK Thallapally
MI Nasiri
BP McGrail
SK Nune
Instruments: 
Volume: 
6
Issue: 
10
Pages: 
7214-7222
Publication year: 
2014

Structures and Stabilities of (MgO)n Nanoclusters.

Abstract: 

Global minima for (MgO)n structures were optimized using a tree growth−hybrid genetic algorithm in conjunction with MNDO/MNDO/d semiempirical molecular orbital calculations followed by density functional theory geometry optimizations with the B3LYP functional. New lowest energy isomers were found for a number of (MgO)n clusters. The most stable isomers for (MgO)n (n > 3) are 3-dimensional. For n < 20, hexagonal tubular (MgO)n structures are more favored in energy than the cubic structures. The cubic structures and their variations dominate after n = 20. For the cubic isomers, increasing the size of the cluster in any dimension improves the stability. The effectiveness of increasing the size of the cluster in a specific dimension to improve stability diminishes as the size in that dimension increases. For cubic structures of the same size, the most compact cubic structure is expected to be the more stable cubic structure. The average Mg−O bond distance and coordination number both increase as n increases. The calculated average Mg−O bond distance is 2.055 Å at n = 40, slightly smaller than the bulk value of 2.104 Å. The average coordination number is predicted to be 4.6 for the lowest energy (MgO)40 as compared to the bulk value of 6. As n increases, the normalized clustering energy ΔE(n) for the (MgO)n increases and the slope of the ΔE(n)vs n curve decreases. The value of ΔE(40) is predicted to be 150 kcal/mol, as compared to the bulk value ΔE(∞) = 176 kcal/mol. The electronic properties of the clusters are presented and the reactive sites are predicted to be at the corners.

Citation: 
Chen M, AR Felmy, and DA Dixon.2014."Structures and Stabilities of (MgO)n Nanoclusters."Journal of Physical Chemistry A 118(17):3136-3146. doi:10.1021/jp412820z
Authors: 
M Chen
AR Felmy
DA Dixon
Instruments: 
Volume: 
118
Issue: 
17
Pages: 
3136-3146
Publication year: 
2014

Physical Properties of Ambient and Laboratory-Generated Secondary Organic Aerosol.

Abstract: 

The size and thickness of organic aerosol particles collected by impaction in five field campaigns were compared to those of laboratory generated secondary organic aerosols (SOA). Scanning transmission x-ray microscopy (STXM) was used to measure the total carbon absorbance (TCA) by individual particles as a function of their projection areas on the substrate. Because they flatten less upon impaction, particles with higher viscosity and surface tension can be identified by a steeper slope on a plot of TCA vs. size. The slopes of the ambient data are statistically similar indicating a small range of average viscosities and surface tensions across five field campaigns. Steeper slopes were observed for the plots corresponding to ambient particles, while smaller slopes were indicative of the laboratory generated SOA. This comparison indicates that ambient organic particles have higher viscosities and surface tensions than those typically generated in laboratory SOA studies.

Citation: 
O'Brien RE, A Neu, SA Epstein, A MacMillan, B Wang, ST Kelly, S Nizkorodov, A Laskin, RC Moffet, and MK Gilles.2014."Physical Properties of Ambient and Laboratory-Generated Secondary Organic Aerosol."Geophysical Research Letters 41(2):4347-4353. doi:10.1002/2014GL060219
Authors: 
RE O'Brien
A Neu
SA Epstein
A MacMillan
B Wang
ST Kelly
S Nizkorodov
A Laskin
RC Moffet
MK Gilles
Facility: 
Volume: 
41
Issue: 
2
Pages: 
4347-4353
Publication year: 
2014

Oxidative Remobilization of Technetium Sequestered by Sulfide-Transformed Nano Zerovalent Iron.

Abstract: 

The dissolution of Tc(IV) sulfide and concurrent transformation of sulfidated ZVI during 2 oxidation were examined. Kinetic data obtained with 10 mL batch reactors showed that Tc(VII) 3 reduced by sulfidated nZVI has significantly slower reoxidation rates than Tc(VII) reduced by 4 nZVI only. In a 50 mL batch reactor, initial inhibition of Tc(IV) dissolution was apparent and 5 lasted until 120 hours at S/Fe = 0.112, presumably due to the redox buffer capacity of FeS. This 6 is evidenced by the parallel trends in oxidation-reduction potentials (ORP) and Tc dissolution 7 kinetics. Mӧssbauer spectra and micro X-ray diffraction of S/Fe = 0.112 suggested the 8 persistence of FeS after 24-h oxidation although X-ray photoelectron spectroscopy indicated 9 substantial surface oxidation. After 120-h oxidation, all characterizations showed complete 10 oxidation of FeS, which further indicates that FeS inhibits Tc oxidation. X-ray absorption 11 spectroscopy for S/Fe = 0.011 showed significantly increasing percentage of TcS2 in the solid 12 phase after 24-h oxidation, indicating TcS2 is more resistant to oxidation than TcO2. At S/Fe = 13 0.112, the XAS results revealed significant transformation of Tc speciation from TcS2 to TcO2 14 after 120-h oxidation at S/Fe = 0.112. Given that no apparent Tc dissolution occurred during this 15 period, the speciation transformation might play a secondary role in hindering Tc oxidation, 16 especially as redox buffer capacity approached depletion.

Citation: 
Fan D, R Anitori, BM Tebo, PG Tratnyek, JS Lezama Pacheco, RK Kukkadapu, L Kovarik, MH Engelhard, and ME Bowden.2014."Oxidative Remobilization of Technetium Sequestered by Sulfide-Transformed Nano Zerovalent Iron."Environmental Science & Technology 48(13):7409-7417. doi:10.1021/es501607s
Authors: 
D Fan
R Anitori
BM Tebo
PG Tratnyek
JS Lezama Pacheco
RK Kukkadapu
L Kovarik
MH Engelhard
ME Bowden
Instruments: 
Volume: 
48
Issue: 
13
Pages: 
7409-7417
Publication year: 
2014

Automated High-Pressure Titration System with In Situ Infrared Spectroscopic Detection.

Abstract: 

A fully automated titration system with infrared detection was developed for investigating interfacial chemistry at high pressures. The apparatus consists of a high-pressure fluid generation and delivery system coupled to a high-pressure cell with infrared optics. A manifold of electronically actuated valves is used to direct pressurized fluids into the cell. Precise reagent additions to the pressurized cell are made with calibrated tubing loops that are filled with reagent and placed in-line with the cell and a syringe pump. The cell’s infrared optics facilitate both transmission and attenuated total reflection (ATR) measurements to monitor bulk-fluid composition and solid-surface phenomena such as adsorption, desorption, complexation, dissolution, and precipitation. Switching between the two measurement modes is accomplished with moveable mirrors that direct radiation from a Fourier transform infrared spectrometer into the cell along transmission or ATR light paths. The versatility of the high-pressure IR titration system is demonstrated with three case studies. First, we titrated water into supercritical CO2 (scCO2) to generate an infrared calibration curve and determine the solubility of water in CO2 at 50 °C and 90 bar. Next, we characterized the partitioning of water between a montmorillonite clay and scCO2 at 50 °C and 90 bar. Transmission-mode spectra were used to quantify changes in the clay’s sorbed water concentration as a function of scCO2 hydration, and ATR measurements provided insights into competitive residency of water and CO2 on the clay surface and in the interlayer. Finally, we demonstrated how time-dependent studies can be conducted with the system by monitoring the carbonation reaction of forsterite (Mg2SiO4) in water-bearing scCO2 at 50 °C and 90 bar. Immediately after water dissolved in the scCO2, a thin film of adsorbed water formed on the mineral surface, and the film thickness increased with time as the forsterite began to dissolve. However, after approximately 2.5 hours, the trend reversed, and a carbonate precipitate began to form on the forsterite surface, exposing dramatic chemical changes in the thin-water film. Collectively, these applications illustrate how the high-pressure IR titration system can provide molecular-level information about the interactions between variably wet scCO2 and minerals relevant to underground storage of CO2 (geologic carbon sequestration). The apparatus could also be utilized to study high-pressure interfacial chemistry in other areas such as catalysis, polymerization, food processing, and oil and gas recovery.

Citation: 
Thompson CJ, PF Martin, J Chen, P Benezeth, HT Schaef, KM Rosso, AR Felmy, and JS Loring.2014."Automated High-Pressure Titration System with In Situ Infrared Spectroscopic Detection."Review of Scientific Instruments 85(4):Article No. 044102. doi:10.1063/1.4870411
Authors: 
CJ Thompson
PF Martin
J Chen
P Benezeth
HT Schaef
KM Rosso
AR Felmy
JS Loring
Instruments: 
Volume: 
Issue: 
Pages: 
Publication year: 
2014

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