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Title: Application of Black Silicon for Nanostructure-Initiator Mass Spectrometry

Journal Article · · Analytical Chemistry
 [1];  [1];  [1];  [2];  [1]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Life Sciences Division; USDOE Joint Genome Institute (JGI), Walnut Creek, CA (United States)
  2. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Foundry

Nanostructure-initiator mass spectrometry (NIMS) is a matrix-free desorption/ionization technique with high sensitivity for small molecules. Surface preparation has relied on hydrofluoric acid (HF) electrochemical etching which is undesirable given the significant safety controls required in this specialized process. Here in this study, we examine a conventional and widely used process for producing black silicon based on sulfur hexafluoride/oxygen (SF6/O2) inductively coupled plasma (ICP) etching at cryogenic temperatures and we find it to be suitable for NIMS. A systematic study varying parameters in the plasma etching process was performed to understand the relationship of black silicon morphology and its sensitivity as a NIMS substrate. The results suggest that a combination of higher silicon temperature and oxygen flow rate gives rise to the formation of black silicon with fine pillar structures, whose aspect ratio are ~8.7 and depth are <1 μm resulting in higher NIMS sensitivity which is attributed to surface restructuring caused by their low melting point upon laser irradiation. Interestingly, we find selectivity of these black silicon substrates to different analytes depending on the etching parameters. Though, the sensitivity of the dry etching process is lower than the traditional "wet" electrochemical etching process, it is suitable for many applications and is prepared using conventional equipment without the use of HF.

Research Organization:
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC02-05CH11231
OSTI ID:
1474922
Journal Information:
Analytical Chemistry, Vol. 88, Issue 3; ISSN 0003-2700
Publisher:
American Chemical Society (ACS)Copyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 27 works
Citation information provided by
Web of Science

References (41)

Matrix-assisted laser desorption ionization time-of-flight mass spectrometry, a revolution in clinical microbial identification journal November 2010
Matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry applied to virus identification journal October 2014
Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry in clinical chemistry journal November 2003
Analysis of carbohydrates and glycoconjugates by matrix-assisted laser desorption/ionization mass spectrometry: An update for 2009-2010: ANALYSIS OF CARBOHYDRATES AND GLYCOCONJUGATES journal May 2014
A novel strategy for MALDI-TOF MS analysis of small molecules journal January 2010
MALDI-TOF mass spectrometry of a combinatorial peptide library: effect of matrix composition on signal suppression journal January 2005
Quantitative matrix-assisted laser desorption/ionization mass spectrometry journal June 2008
Matrix-free methods for laser desorption/ionization mass spectrometry journal January 2006
Matrix-free and material-enhanced laser desorption/ionization mass spectrometry for the analysis of low molecular weight compounds journal September 2010
Desorption–ionization mass spectrometry on porous silicon journal May 1999
Matrix-Free Laser Desorption/Ionization Mass Spectrometry on Silicon Nanowire Arrays Prepared by Chemical Etching of Crystalline Silicon journal January 2010
Desorption/Ionization on Silicon Nanowires journal March 2005
Surface-Assisted Laser Desorption/Ionization Mass Spectrometry on Titania Nanotube Arrays journal July 2008
Diamond Nanowires: A Novel Platform for Electrochemistry and Matrix-Free Mass Spectrometry journal May 2015
Tailored Silicon Nanopost Arrays for Resonant Nanophotonic Ion Production journal February 2010
Top-down synthesized TiO2 nanowires as a solid matrix for surface-assisted laser desorption/ionization time-of-flight (SALDI-TOF) mass spectrometry journal July 2014
Functionalized Nanoparticles and Nanostructured Surfaces for Surface-Assisted Laser Desorption/Ionization Mass Spectrometry journal January 2010
Matrix-Free Laser Desorption/Ionization-Mass Spectrometry Using Self-Assembled Germanium Nanodots journal July 2007
Surface-Assisted Laser Desorption/Ionization Mass Spectrometric Detection of Biomolecules by Using Functional Single-Walled Carbon Nanohorns as the Matrix journal December 2012
Clathrate nanostructures for mass spectrometry journal October 2007
Nanostructure Initiator Mass Spectrometry: Tissue Imaging and Direct Biofluid Analysis journal April 2009
Nanostructure Initiator Mass Spectrometry for tissue imaging in metabolomics: Future prospects and perspectives journal August 2012
“Replica-Extraction-Transfer” Nanostructure-Initiator Mass Spectrometry Imaging of Acoustically Printed Bacteria journal October 2013
Nanostructure-Initiator Mass Spectrometry (NIMS) for Molecular Mapping of Animal Tissues book October 2014
Nanostructure-initiator mass spectrometry: a protocol for preparing and applying NIMS surfaces for high-sensitivity mass analysis journal July 2008
Metabolic Imaging Using Nanostructure-Initiator Mass Spectrometry (NIMS) book January 2014
The black silicon method: a universal method for determining the parameter setting of a fluorine-based reactive ion etcher in deep silicon trench etching with profile control journal June 1995
An ultra-black silicon absorber: An ultra-black silicon absorber journal January 2014
Fabrication and characteristics of black silicon for solar cell applications: An overview journal September 2014
Sub-50-nm self-assembled nanotextures for enhanced broadband antireflection in silicon solar cells journal January 2015
Black silicon—new functionalities in microsystems journal May 2006
Black silicon method: X. A review on high speed and selective plasma etching of silicon with profile control: an in-depth comparison between Bosch and cryostat DRIE processes as a roadmap to next generation equipment journal February 2009
Characterization of low-temperature bulk micromachining of silicon using an SF 6 /O 2 inductively coupled plasma journal July 2012
The structural and optical properties of black silicon by inductively coupled plasma reactive ion etching journal November 2014
On the optical and morphological properties of microstructured Black Silicon obtained by cryogenic-enhanced plasma reactive ion etching journal May 2013
Passivation mechanisms in cryogenic SF 6 /O 2 etching process journal October 2003
Black silicon layer formation for application in solar cells journal November 2006
Guidelines for etching silicon MEMS structures using fluorine high-density plasmas at cryogenic temperatures journal August 2002
OpenMSI: A High-Performance Web-Based Platform for Mass Spectrometry Imaging journal October 2013
Nanowire-assisted laser desorption and ionization mass spectrometry for quantitative analysis of small molecules journal January 2005
High surface area of porous silicon drives desorption of intact molecules journal November 2007

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Ecosystem Fabrication (EcoFAB) Protocols for The Construction of Laboratory Ecosystems Designed to Study Plant-microbe Interactions journal January 2018