Deposition and Microfabrication

Physical structures ranging in size from miniature objects (nanomaterials) to electrical devices (thin films) with planned properties can be made using the deposition and microfabrication capability. Materials with specific surface, bulk and interfacial properties for energy and environmental applications can be designed and made using these integrated capabilities. See a complete list of Deposition and Microfabrication instruments.

Resources and Techniques

  • Functionalized surfaces – Design and manufacture surfaces optimized for specific functions related to catalysis and other areas.
  • Model systems for geochemistry/biogeochemistry – Grow model oxide and mineral films with varying structure and complexity.
  • Materials with designed properties – Film growth and ion implantation for materials with specific properties.
  • Chemical and biological sensing – Film and surface layer deposition and modification, micro and nano-lithography, and solution synthesis capabilities.
  • Microfabrication – Engineering, software development and fabrication are used to design and fabricate next-generation components.

Description

Capability Details
• Unique oxygen-plasma-assisted molecular beam epitaxy system for designing and constructing high-quality oxide thin films
• Spin coating and wet chemical synthesis to prepare thin films and nanostructures
• Focused ion beam for nanolithography and deposition and manipulation of structures at the nano scale
• Microfabrication suite for designing and etching complex patterns into varied substrates
• Hybrid physical vapor deposition system for depositing thin films of metals, oxides, nitrides and alloys with high purity and thickness control
• Pulsed laser deposition for growing complex oxides films
• Low-energy ion deposition for preparing ultra-pure films of complex molecules, including biomolecules, through a mass-selected soft-landing process
• Diverse and unrivaled expertise in advanced signal acquisition and processing instrumentation, signal analysis algorithms, laboratory automation systems and scientific data management solutions

Instruments

EMSL's molecular beam epitaxy (MBE) deposition system is used for the synthesis and characterization of novel oxide, ceramic, and mineral materials...
This instrument is newly available to EMSL users. For more information about this instrument and the science it will help enable, see the ...
Custodian(s): Ryan Kelly, Hardeep S Mehta
The FEI Helios Nanolab dual-beam focused ion beam/scanning electron microscopy (FIB/SEM) microscope combines two important high-resolution...
Custodian(s): Bruce Arey
Only available at EMSL, the Discovery Deposition System has been customized to be a fully automated multi-functional "hybrid" instrument with...
The mass-selected ion deposition system is a new instrument constructed at EMSL. The apparatus, shown in Figure 1, includes a high-transmission...
Custodian(s): Julia Laskin

Publications

Nanostructured silicon is a promising anode material for high performance lithium-ion batteries, yet scalable synthesis of such materials, and...
Transition Al2O3 derived from thermal decomposition of AlOOH Boehmite have complex structures and to a large extent remain poorly understood. Here we...
Dealuminated zeolite HY was used to support Ir(CO)2 complexes formed from Ir(CO)2(C5H7O2). Infrared and X-ray absorption spectra and atomic-...
A hybrid microchip/capillary CE system was developed to allow unbiased and lossless sample loading and high throughput repeated injections. This new...
We record sequences of Raman spectra at a plasmonic junction formed by a gold AFM tip in contact with a silver surface coated with 4,4’-...

Science Highlights

Posted: December 19, 2014
Strontium titanate and other titanium oxides hold the promise of turning sunlight into fuel. They are excellent candidates for solar hydrolysis –...
Posted: September 10, 2014
Scientists at EMSL and Pacific Northwest National Laboratory have generated a material that allows oxygen to efficiently move through it at...
Posted: August 07, 2013
Predictive models of biogeochemical interactions in soils are more accurate and scalable if they consider the reaction chemistry that occurs in...
Posted: July 29, 2013
Scientists have gained the first quantitative insights into electron transfer from minerals to microbes by studying that transfer in a nature-...
Posted: May 20, 2013
Pacific Northwest National Laboratory scientists working at EMSL wrote a review of how microfluidic devices are being used in scientific instruments...

Physical structures ranging in size from miniature objects (nanomaterials) to electrical devices (thin films) with planned properties can be made using the deposition and microfabrication capability. Materials with specific surface, bulk and interfacial properties for energy and environmental applications can be designed and made using these integrated capabilities. See a complete list of Deposition and Microfabrication instruments.

Resources and Techniques

  • Functionalized surfaces – Design and manufacture surfaces optimized for specific functions related to catalysis and other areas.
  • Model systems for geochemistry/biogeochemistry – Grow model oxide and mineral films with varying structure and complexity.
  • Materials with designed properties – Film growth and ion implantation for materials with specific properties.
  • Chemical and biological sensing – Film and surface layer deposition and modification, micro and nano-lithography, and solution synthesis capabilities.
  • Microfabrication – Engineering, software development and fabrication are used to design and fabricate next-generation components.

Pneumatic Microvalve-Based Hydrodynamic Sample Injection for High-Throughput, Quantitative Zone Electrophoresis in Capillaries.

Abstract: 

A hybrid microchip/capillary CE system was developed to allow unbiased and lossless sample loading and high throughput repeated injections. This new hybrid CE system consists of a polydimethylsiloxane (PDMS) microchip sample injector featuring a pneumatic microvalve that separates a sample introduction channel from a short sample loading channel and a fused silica capillary separation column that connects seamlessly to the sample loading channel. The sample introduction channel is pressurized such that when the pneumatic microvalve opens briefly, a variable-volume sample plug is introduced into the loading channel. A high voltage for CE separation is continuously applied across the loading channel and the fused silica capillary separation column. Analytes are rapidly separated in the fused silica capillary with high resolution. High sensitivity MS detection after CE separation is accomplished via a sheathless CE/ESI-MS interface. The performance evaluation of the complete CE/ESI-MS platform demonstrated that reproducible sample injection with well controlled sample plug volumes could be achieved by using the PDMS microchip injector. The absence of band broadening from microchip to capillary indicated a minimum dead volume at the junction. The capabilities of the new CE/ESI-MS platform in performing high throughput and quantitative sample analyses were demonstrated by the repeated sample injection without interrupting an ongoing separation and a good linear dependence of the total analyte ion abundance on the sample plug volume using a mixture of peptide standards. The separation efficiency of the new platform was also evaluated systematically at different sample injection times, flow rates and CE separation voltages.

Citation: 
Kelly RT, C Wang, SJ Rausch, CS Lee, and K Tang.2014."Pneumatic Microvalve-Based Hydrodynamic Sample Injection for High-Throughput, Quantitative Zone Electrophoresis in Capillaries."Analytical Chemistry 86(13):6723-6729. doi:10.1021/ac501910p
Authors: 
RT Kelly
C Wang
SJ Rausch
CS Lee
K Tang
Volume: 
86
Issue: 
13
Pages: 
6723-6729
Publication year: 
2014

Iridium Complexes and Clusters in Dealuminated Zeolite HY: Distribution between Crystalline and Impurity Amorphous Regions.

Abstract: 

Dealuminated zeolite HY was used to support Ir(CO)2 complexes formed from Ir(CO)2(C5H7O2). Infrared and X-ray absorption spectra and atomic-resolution electron microscopy images identify these complexes, and the images and 27Al NMR spectra identify impurity amorphous regions in the zeolite where the iridium is more susceptible to aggregation than in the crystalline regions. The results indicate a significant stability limitation of metal in amorphous impurity regions of zeolites.

Citation: 
Martinez-Macias C, P Xu, SJ Hwang, J Lu, CY Chen, ND Browning, and BC Gates.2014."Iridium Complexes and Clusters in Dealuminated Zeolite HY: Distribution between Crystalline and Impurity Amorphous Regions."ACS Catalysis 4(8):2662–2666. doi:10.1021/cs5006426
Authors: 
C Martinez-Macias
P Xu
SJ Hwang
J Lu
CY Chen
ND Browning
BC Gates
Instruments: 
Volume: 
Issue: 
Pages: 
Publication year: 
2014

Structure of δ-Alumina: Toward The Atomic Level Understanding Of Transition Alumina Phases.

Abstract: 

Transition Al2O3 derived from thermal decomposition of AlOOH Boehmite have complex structures and to a large extent remain poorly understood. Here we report a detailed atomic level analysis of ΔAl2O3 for the first time using a combination of Scanning Transmission Electron Microscopy imaging, XRD refinement, and DFT calculations. We show that the structure of ΔAl2O3 represents a complex structural intergrowth from several crystallographic variants. The two main crystallographic variants, which are identified as Δ1-Al2O3 and Δ2−Al2O3, are fully structurally described. In addition, we also derive the energy of formation for Δ1 and Δ2-Al2O3 and the other relevant transition Al2O3 phases, and show how energetic degeneracy leads to structural disorder and complex intergrowths among several transition Al2O3. The results of the work have important implications for understanding thermodynamic stability and transformation processes in transition alumina.

Citation: 
Kovarik L, ME Bowden, A Genc, J Szanyi, CHF Peden, and JH Kwak.2014."Structure of ?-Alumina: Toward The Atomic Level Understanding Of Transition Alumina Phases."Journal of Physical Chemistry C 118:18051-18058. doi:10.1021/jp500051j
Authors: 
L Kovarik
ME Bowden
A Genc
J Szanyi
CHF Peden
JH Kwak
Facility: 
Volume: 
Issue: 
Pages: 
Publication year: 
2014

Mesoporous Silicon Sponge as an Anti-Pulverization Structure for High-Performance Lithium-ion Battery Anodes.

Abstract: 

Nanostructured silicon is a promising anode material for high performance lithium-ion batteries, yet scalable synthesis of such materials, and retaining good cycling stability in high loading electrode remain significant challenges. Here, we combine in-situ transmission electron microscopy and continuum media mechanical calculations to demonstrate that large (>20 micron) mesoporous silicon sponge (MSS) prepared by the scalable anodization method can eliminate the pulverization of the conventional bulk silicon and limit particle volume expansion at full lithiation to ~30% instead of ~300% as observed in bulk silicon particles. The MSS can deliver a capacity of ~750 mAh/g based on the total electrode weight with >80% capacity retention over 1000 cycles. The first-cycle irreversible capacity loss of pre-lithiated MSS based anode is only <5%. The insight obtained from MSS also provides guidance for the design of other materials that may experience large volume variation during operations.

Citation: 
Li X, M Gu, SY Hu, R Kennard, P Yan, X Chen, CM Wang, MJ Sailor, J Zhang, and J Liu.2014."Mesoporous Silicon Sponge as an Anti-Pulverization Structure for High-Performance Lithium-ion Battery Anodes."Nature Communications 5:Article No. 4105. doi:10.1038/ncomms5105
Authors: 
Li X
M Gu
SY Hu
R Kennard
P Yan
X Chen
CM Wang
MJ Sailor
J Zhang
J Liu
Facility: 
Volume: 
Issue: 
Pages: 
Publication year: 
2014

Synechococcus elongatus UTEX 2973, a fast growing cyanobacterial chassis for biosynthesis using light and CO2.

Abstract: 

Photosynthetic microbes are of emerging interest as production organisms in biotechnology because they can grow autotrophically using sunlight, an abundant energy source, and CO2, a greenhouse gas. Important traits for such microbes are fast growth and amenability to genetic manipulation. Here we describe Synechococcus elongatus UTEX 2973, a unicellular cyanobacterium capable of rapid autotrophic growth, comparable to heterotrophic industrial hosts such as yeast. Synechococcus 2973 can be readily transformed for facile generation of desired knockout and knock-in mutations. Genome sequencing coupled with global proteomics studies revealed that Synechococcus 2973 is a close relative of the widely studied cyanobacterium Synechococcus elongatus PCC 7942, an organism that grows more than two times slower. A small number of nucleotide changes are the only significant differences between the genomes of these two cyanobacterial strains. Thus, our study has unraveled genetic determinants necessary for rapid growth of cyanobacterial strains of significant industrial potential.

Citation: 
Yu J, ML Liberton, P Cliften, R Head, JM Jacobs, RD Smith, DW Koppenaal, JJ Brand, and HB Pakrasi.2015."Synechococcus elongatus UTEX 2973, a fast growing cyanobacterial chassis for biosynthesis using light and CO2."Scientific Reports 5:8132. doi:10.1038/srep08132
Authors: 
Yu J
ML Liberton
P Cliften
R Head
JM Jacobs
RD Smith
DW Koppenaal
JJ Br
HB Pakrasi
Facility: 
Volume: 
Issue: 
Pages: 
Publication year: 
2015

Conversion of 1,2-Propylene Glycol on Rutile TiO2(110).

Abstract: 

We have studied the reactions of 1,2-propylene glycol (1,2-PG), DOCH(CH3)CH2OD, on partially reduced, hydroxylated and oxidized TiO2(110) surfaces using temperature programmed desorption. On reduced TiO2(110), propylene, propanal, and acetone are identified as primary carbon-containing products. While the propylene formation channel dominates at low 1,2-PG coverages, all of the above-mentioned products are observed at high coverages. The carbon-containing products are accompanied by the formation of D2O and D2. The observation of only deuterated products shows that the source of hydrogen (D) is from the 1,2-PG hydroxyls. The role of bridging oxygen vacancy (VO) sites was further investigated by titrating them via hydroxylation and oxidation. The results show that hydroxylation does not change the reactivity because the VO sites are regenerated at 500 K, which is a temperature lower than the 1,2-PG product formation temperature. In contrast, surface oxidation causes significant changes in the product distribution, with increased acetone and propanal formation and decreased propylene formation. Additionally D2 is completely eliminated as an observed product at the expense of D2O formation.

Citation: 
Chen L, Z Li, RS Smith, BD Kay, and Z Dohnalek.2014."Conversion of 1,2-Propylene Glycol on Rutile TiO2(110)."Journal of Physical Chemistry C 118(28):15339-15347. doi:10.1021/jp504770f
Authors: 
L Chen
Z Li
RS Smith
BD Kay
Z Dohnalek
Facility: 
Volume: 
118
Issue: 
28
Pages: 
15339-15347
Publication year: 
2014

Vibronic Raman Scattering at the Quantum Limit of Plasmons.

Abstract: 

We record sequences of Raman spectra at a plasmonic junction formed by a gold AFM tip in contact with a silver surface coated with 4,4’-dimercaptostilbene (DMS). A 2D correlation analysis of the recorded trajectories reveals that the observable vibrational states can be divided into sub-sets. The first set comprises the totally symmetric vibrations of DMS (ag) that are neither correlated with each other nor to the fluctuating background, which is assigned to the signature of charge transfer plasmons tunneling through DMS. The second set consists of bu vibrations, which are correlated both with each other and with the continuum. Our findings are rationalized on the basis of the charge-transfer theory of Raman scattering, and illustrate how the tunneling plasmons modulate the vibronic coupling term from which the intensities of the bu states are derived.

Citation: 
El-Khoury PZ, and WP Hess.2014."Vibronic Raman Scattering at the Quantum Limit of Plasmons."Nano Letters 14(7):4114-4118. doi:10.1021/nl501690u
Authors: 
PZ El-Khoury
WP Hess
Facility: 
Volume: 
14
Issue: 
7
Pages: 
4114-4118
Publication year: 
2014

Modeling Interfacial Glass-Water Reactions: Recent Advances and Current Limitations.

Abstract: 

The altered layer (i.e., amorphous hydrated surface layer and crystalline reaction products)represents a complex region, both physically and chemically, sandwiched between two distinct boundaries - pristine glass surface at the inner most interface and aqueous solution at the outer most. The physico-chemical processes that control the development of this region have a significant impact on the long-term glass-water reaction. Computational models, spanning different length and time-scales, are currently being developed to improve our understanding of this complex and dynamic process with the goal of accurately describing the pore-scale changes that occur as the system evolves. These modeling approaches include Geochemical Reaction Path simulations, Glass Reactivity in Allowance for Alteration Layer simulations, Monte Carlo simulations, and Molecular Dynamics methods. Discussed in this manuscript are the advances and limitations of each modeling approach placed in the context of the glass water reaction and how collectively these approaches provide insights into the mechanisms that control the formation and evolution of altered layers; thus providing the fundamental data needed to develop pore-scale equations that enable more accurate predictions of nuclear waste glass corrosion in a geologic repository.

Citation: 
Pierce EM, P Frugier, LJ Criscenti, KD Kwon, and SN Kerisit.2014."Modeling Interfacial Glass-Water Reactions: Recent Advances and Current Limitations."International Journal of Applied Glass Science 5(4):421-435. doi:10.1111/ijag.12077
Authors: 
EM Pierce
P Frugier
LJ Criscenti
KD Kwon
SN Kerisit
Volume: 
5
Issue: 
4
Pages: 
421-435
Publication year: 
2014

Formation of Interfacial Layer and Long-Term Cylability of Li-O-2 Batteries.

Abstract: 

Extended cycling of the Li-O2 battery under full discharge/charge conditions is achievable upon selection of appropriate electrode materials and cycling protocol. However, the decomposition of the side products also contribute to the observed good cycling behavior of high capacity Li-O2 batteries. Quantitative analyses of the discharge and charge products reveals a quick switch from the predominant formation of Li2O2 to the predominant formation of side products during the first a few cycles of the Li-O2 batteries. After the switch, cycling stabilizes with a repeatable formation of Li2O2/side products at ~1:2 ratio. CNTs/Ru composite electrodes exhibits lower charge voltage and deliver 50 full discharge-charge cycles without sharp capacity drop. Ru coated glass carbon electrode can lead to more than 500 cycles without change in its cycling profiles. The better understanding on Li-O2 reaction processes developed in this work may lead to the further improvement on the long term cycling behavior of high capacity Li-O2 batteries.

Citation: 
Nasybulin EN, W Xu, BL Mehdi, EC Thomsen, MH Engelhard, RC Masse, P Bhattacharya, M Gu, WD Bennett, Z Nie, CM Wang, ND Browning, and J Zhang.2014."Formation of Interfacial Layer and Long-Term Cylability of Li-O-2 Batteries."ACS Applied Materials & Interfaces 6(16):14141-14151. doi:10.1021/am503390q
Authors: 
EN Nasybulin
W Xu
BL Mehdi
EC Thomsen
MH Engelhard
RC Masse
P Bhattacharya
M Gu
WD Bennett
Z Nie
CM Wang
ND Browning
J Zhang
Facility: 
Instruments: 
Volume: 
6
Issue: 
16
Pages: 
14141-14151
Publication year: 
2014

Automated genome mining of ribosomal peptide natural products.

Abstract: 

Ribosomally synthesized and posttranslationally modified peptides (RiPPs), especially from microbial sources, are a large group of bioactive natural products that are a promising source of new (bio)chemistry and bioactivity (1). In light of exponentially increasing microbial genome databases and improved mass spectrometry (MS)-based metabolomic platforms, there is a need for computational tools that connect natural product genotypes predicted from microbial genome sequences with their corresponding chemotypes from metabolomic datasets. Here, we introduce RiPPquest, a tandem mass spectrometry database search tool for identification of microbial RiPPs and apply it for lanthipeptide discovery. RiPPquest uses genomics to limit search space to the vicinity of RiPP biosynthetic genes and proteomics to analyze extensive peptide modifications and compute p-values of peptide-spectrum matches (PSMs). We highlight RiPPquest by connection of multiple RiPPs from extracts of Streptomyces to their gene clusters and by the discovery of a new class III lanthipeptide, informatipeptin, from Streptomyces viridochromogenes DSM 40736 as the first natural product to be identified in an automated fashion by genome mining. The presented tool is available at cy-clo.ucsd.edu.

Citation: 
Mohimani H, R Kersten, W Liu, M Wang, SO Purvine, S Wu, HM Brewer, L Pasa-Tolic, N Bandeira, BS Moore, PA Pevzner, and PC Dorrestein.2014."Automated genome mining of ribosomal peptide natural products."ACS Chemical Biology 9(7):1545-1551. doi:10.1021/cb500199h
Authors: 
H Mohimani
R Kersten
W Liu
M Wang
SO Purvine
S Wu
HM Brewer
L Pasa-Tolic
N Beira
BS Moore
PA Pevzner
PC Dorrestein
Instruments: 
Volume: 
9
Issue: 
7
Pages: 
1545-1551
Publication year: 
2014

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