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Title: Electrospray deposition tool: Creating compositionally gradient libraries of nanomaterials

Abstract

Electrospray deposition (ESD) enables the growth of solution deposited thin films in a precise and continuous manner by the delivery of submicron droplets of dilute solutions to a heated substrate. By combining ESD with programmable motor control and gradient solution pumping in a first-of-its-kind user tool at the Center for Functional Nanomaterials at Brookhaven National Laboratory, we show the ability to create one or two dimensional compositional gradient nanoscale films via ESD. These capabilities make it possible to construct thin film multicomponent “libraries” on a single substrate to rapidly and systematically characterize composition-dependent properties in a variety of material systems such as thin films involving homopolymer and block copolymer blends. Herein, we report the design, construction, and validation of a gradient ESD tool that allows users to carefully control the jet stability, flow composition, spray position, and substrate temperature. Calibrated thin films range in thickness from tens to hundreds of nanometers. We demonstrate gradient thin films using a ternary dye triangle as well as a gradual blending of polystyrene homopolymer with poly(styrene-block-methyl methacrylate) on a single substrate. Paired with the rapid measurement capabilities of synchrotron small angle X-ray scattering, this tool forms an integral part of a new platform formore » high-throughput, autonomous characterization and design of nanomaterial thin films and soft materials more generally.« less

Authors:
ORCiD logo [1]; ORCiD logo [2]; ORCiD logo [3]; ORCiD logo [3]
  1. Yale Univ., New Haven, CT (United States)
  2. Univ. of Pennsylvania, Philadelphia, PA (United States)
  3. Brookhaven National Lab. (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
Publication Date:
Research Org.:
Brookhaven National Lab. (BNL), Upton, NY (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Scientific User Facilities Division; National Science Foundation (NSF)
OSTI Identifier:
1599292
Alternate Identifier(s):
OSTI ID: 1580793
Report Number(s):
[BNL-213621-2020-JAAM]
[Journal ID: ISSN 0034-6748]
Grant/Contract Number:  
[SC0012704; DGE-1122492; CBET-1703494; DMR-1410568]
Resource Type:
Accepted Manuscript
Journal Name:
Review of Scientific Instruments
Additional Journal Information:
[ Journal Volume: 91; Journal Issue: 1]; Journal ID: ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
77 NANOSCIENCE AND NANOTECHNOLOGY

Citation Formats

Toth, Kristof, Osuji, Chinedum O., Yager, Kevin G., and Doerk, Gregory S. Electrospray deposition tool: Creating compositionally gradient libraries of nanomaterials. United States: N. p., 2020. Web. doi:10.1063/1.5129625.
Toth, Kristof, Osuji, Chinedum O., Yager, Kevin G., & Doerk, Gregory S. Electrospray deposition tool: Creating compositionally gradient libraries of nanomaterials. United States. doi:10.1063/1.5129625.
Toth, Kristof, Osuji, Chinedum O., Yager, Kevin G., and Doerk, Gregory S. Thu . "Electrospray deposition tool: Creating compositionally gradient libraries of nanomaterials". United States. doi:10.1063/1.5129625.
@article{osti_1599292,
title = {Electrospray deposition tool: Creating compositionally gradient libraries of nanomaterials},
author = {Toth, Kristof and Osuji, Chinedum O. and Yager, Kevin G. and Doerk, Gregory S.},
abstractNote = {Electrospray deposition (ESD) enables the growth of solution deposited thin films in a precise and continuous manner by the delivery of submicron droplets of dilute solutions to a heated substrate. By combining ESD with programmable motor control and gradient solution pumping in a first-of-its-kind user tool at the Center for Functional Nanomaterials at Brookhaven National Laboratory, we show the ability to create one or two dimensional compositional gradient nanoscale films via ESD. These capabilities make it possible to construct thin film multicomponent “libraries” on a single substrate to rapidly and systematically characterize composition-dependent properties in a variety of material systems such as thin films involving homopolymer and block copolymer blends. Herein, we report the design, construction, and validation of a gradient ESD tool that allows users to carefully control the jet stability, flow composition, spray position, and substrate temperature. Calibrated thin films range in thickness from tens to hundreds of nanometers. We demonstrate gradient thin films using a ternary dye triangle as well as a gradual blending of polystyrene homopolymer with poly(styrene-block-methyl methacrylate) on a single substrate. Paired with the rapid measurement capabilities of synchrotron small angle X-ray scattering, this tool forms an integral part of a new platform for high-throughput, autonomous characterization and design of nanomaterial thin films and soft materials more generally.},
doi = {10.1063/1.5129625},
journal = {Review of Scientific Instruments},
number = [1],
volume = [91],
place = {United States},
year = {2020},
month = {1}
}

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Works referenced in this record:

Physical Continuity and Vertical Alignment of Block Copolymer Domains by Kinetically Controlled Electrospray Deposition
journal, May 2015

  • Hu, Hanqiong; Choo, Youngwoo; Feng, Xunda
  • Macromolecular Rapid Communications, Vol. 36, Issue 13
  • DOI: 10.1002/marc.201500099

Thin organic films by atmospheric-pressure ion deposition
journal, April 2004

  • Saf, Robert; Goriup, Marian; Steindl, Thomas
  • Nature Materials, Vol. 3, Issue 5
  • DOI: 10.1038/nmat1117

Surface-Bound Soft Matter Gradients
journal, March 2008


Automated orthogonal control system for electrospray ionization
journal, August 2004

  • Valaskovic, Gary A.; Murphy, James P.; Lee, Mike S.
  • Journal of the American Society for Mass Spectrometry, Vol. 15, Issue 8
  • DOI: 10.1016/j.jasms.2004.04.033

Sequential deposition of block copolymer thin films and formation of lamellar heterolattices by electrospray deposition
journal, September 2015

  • Choo, Youngwoo; Hu, Hanqiong; Toth, Kristof
  • Journal of Polymer Science Part B: Polymer Physics, Vol. 54, Issue 2
  • DOI: 10.1002/polb.23913

Electrospraying route to nanotechnology: An overview
journal, March 2008


Rapid Ordering in “Wet Brush” Block Copolymer/Homopolymer Ternary Blends
journal, October 2016


A Kriging-Based Approach to Autonomous Experimentation with Applications to X-Ray Scattering
journal, August 2019


CO‐SPUTTERED Au‐SiO 2 CERMET FILMS
journal, February 1967

  • Miller, N. Carl; Shirn, George A.
  • Applied Physics Letters, Vol. 10, Issue 3
  • DOI: 10.1063/1.1754863

High-Throughput Measurement of Polymer Blend Phase Behavior
journal, August 2000

  • Meredith, J. Carson; Karim, Alamgir; Amis, Eric J.
  • Macromolecules, Vol. 33, Issue 16
  • DOI: 10.1021/ma0004662

High-speed and drop-on-demand printing with a pulsed electrohydrodynamic jet
journal, August 2010


Alternating Current Electrospraying
journal, November 2009

  • Maheshwari, Siddharth; Chetwani, Nishant; Chang, Hsueh-Chia
  • Industrial & Engineering Chemistry Research, Vol. 48, Issue 21
  • DOI: 10.1021/ie801841r

Disintegration of Water Drops in an Electric Field
journal, July 1964

  • Taylor, G.
  • Proceedings of the Royal Society A: Mathematical, Physical and Engineering Sciences, Vol. 280, Issue 1382, p. 383-397
  • DOI: 10.1098/rspa.1964.0151

Formation and properties of multivariant assemblies of surface-tethered diblock and triblock copolymers
journal, October 2008


Rapid Method for Determining Ternary‐Alloy Phase Diagrams
journal, December 1965

  • Kennedy, Kurt; Stefansky, Tibor; Davy, Gordon
  • Journal of Applied Physics, Vol. 36, Issue 12
  • DOI: 10.1063/1.1713952

Generating thickness gradients of thin polymer films via flow coating
journal, February 2006

  • Stafford, Christopher M.; Roskov, Kristen E.; Epps, Thomas H.
  • Review of Scientific Instruments, Vol. 77, Issue 2
  • DOI: 10.1063/1.2173072

Continuous and patterned deposition of functional block copolymer thin films using electrospray
journal, June 2015

  • Hu, Hanqiong; Toth, Kristof; Kim, Myungwoong
  • MRS Communications, Vol. 5, Issue 2
  • DOI: 10.1557/mrc.2015.37

Continuous Equilibrated Growth of Ordered Block Copolymer Thin Films by Electrospray Deposition
journal, March 2013

  • Hu, Hanqiong; Rangou, Sofia; Kim, Myungwoong
  • ACS Nano, Vol. 7, Issue 4
  • DOI: 10.1021/nn400279a

Electrospray cone-jet breakup and droplet production for electrolyte solutions
journal, September 2012


Electrohydrodynamic spraying functioning modes: a critical review
journal, September 1994


Morphology Development in Thin Films of a Lamellar Block Copolymer Deposited by Electrospray
journal, August 2014

  • Hu, Hanqiong; Singer, Jonathan P.; Osuji, Chinedum O.
  • Macromolecules, Vol. 47, Issue 16
  • DOI: 10.1021/ma500376n

Current and droplet size in the electrospraying of liquids. Scaling laws
journal, March 1997


Universal Cone Angle of ac Electrosprays Due to Net Charge Entrainment
journal, November 2008


Instability of Electrified Liquid Surfaces
journal, July 1917


Formation of surface-grafted copolymer brushes with continuous composition gradients
journal, January 2003

  • Tomlinson, Michael R.; Genzer, Jan
  • Chemical Communications, Issue 12
  • DOI: 10.1039/b303823h

Organic/inorganic hybrid nano-microstructured coatings on insulated substrates by electrospray deposition
journal, June 2005

  • Matsumoto, Hidetoshi; Mizukoshi, Tomoya; Nitta, Kazuya
  • Journal of Colloid and Interface Science, Vol. 286, Issue 1
  • DOI: 10.1016/j.jcis.2005.01.014

Charge and fission of droplets in electrostatic sprays
journal, January 1994

  • Gomez, Alessandro; Tang, Keqi
  • Physics of Fluids, Vol. 6, Issue 1
  • DOI: 10.1063/1.868037

Instrumentation for In situ/Operando X-ray Scattering Studies of Polymer Additive Manufacturing Processes
journal, March 2019


Control and improvement of jet stability by monitoring liquid meniscus in electrospray and electrohydrodynamic jet
journal, May 2014


Electrospray droplet sources for thin film deposition
journal, November 2006