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In Situ Monitoring of Non-Thermal Plasma Cleaning of Surfactant Encapsulated Nanoparticles

Journal Article · · Nanomaterials
DOI:https://doi.org/10.3390/nano14030290· OSTI ID:2283473

Surfactants are widely used in the synthesis of nanoparticles, as they have a remarkable ability to direct their growth to obtain well-defined shapes and sizes. However, their post-synthesis removal is a challenge, and the methods used often result in morphological changes that defeat the purpose of the initial controlled growth. Moreover, after the removal of surfactants, the highly active surfaces of nanomaterials may undergo structural reconstruction by exposure to a different environment. Thus, ex situ characterization after air exposure may not reflect the effect of the cleaning methods. Here, combining X-ray photoelectron spectroscopy, in situ infrared reflection absorption spectroscopy, and environmental transmission electron microscopy measurements with CO probe experiments, we investigated different surfactant-removal methods to produce clean metallic Pt nanoparticles from surfactant-encapsulated ones. It was demonstrated that both ultraviolet-ozone (UV-ozone) treatment and room temperature O2 plasma treatment led to the formation of Pt oxides on the surface after the removal of the surfactant. On the other hand, when H2 was used for plasma treatment, both the Pt0 oxidation state and nanoparticle size distribution were preserved. In addition, H2 plasma treatment can reduce Pt oxides after O2-based treatments, resulting in metallic nanoparticles with clean surfaces. These findings provide a better understanding of the various options for surfactant removal from metal nanoparticles and point toward non-thermal plasmas as the best route if the integrity of the nanoparticle needs to be preserved.

Research Organization:
Brookhaven National Laboratory (BNL), Upton, NY (United States)
Sponsoring Organization:
USDOE; USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)
Grant/Contract Number:
SC0012704; SC0022199
OSTI ID:
2283473
Alternate ID(s):
OSTI ID: 2326922
Report Number(s):
BNL--225408-2024-JAAM; PII: nano14030290
Journal Information:
Nanomaterials, Journal Name: Nanomaterials Journal Issue: 3 Vol. 14; ISSN 2079-4991; ISSN NANOKO
Publisher:
MDPI AGCopyright Statement
Country of Publication:
Switzerland
Language:
English

References (56)

Structural and Chemical Effects of Plasma Treatment on Close-Packed Colloidal Nanoparticle Layers journal August 2008
Gold Nanorods: From Synthesis and Properties to Biological and Biomedical Applications journal July 2009
Catalytic Oxidation of CO on a Curved Pt(111) Surface: Simultaneous Ignition at All Facets through a Transient CO‐O Complex** journal August 2020
Assessing the Effect of Surface Chemistry on Gold Nanorod Uptake, Toxicity, and Gene Expression in Mammalian Cells journal January 2008
Graphene-Like MoS 2 /Graphene Composites: Cationic Surfactant-Assisted Hydrothermal Synthesis and Electrochemical Reversible Storage of Lithium journal June 2013
Influence of Surfactant Bilayers on the Refractive Index Sensitivity and Catalytic Properties of Anisotropic Gold Nanoparticles journal November 2015
Infrared spectra for co isotopes chemisorbed on Pt “111”: Evidence for strong absorbate coupling interactions journal November 1977
An infrared study of CO adsorption on Pt(111) journal July 1988
Removal efficiency of organic contaminants on Si wafer by dry cleaning using UV/O3 and ECR plasma journal February 2003
Gold nanorods: Their potential for photothermal therapeutics and drug delivery, tempered by the complexity of their biological interactions journal February 2012
Surface science approach to Pt/carbon model catalysts: XPS, STM and microreactor studies journal May 2018
Polyaniline-supported nano metal-catalyzed coupling reactions: Opportunities and challenges journal February 2023
Cold plasma reduction of surface carbon on SmCo5 nano-flakes prepared by surfactant-assisted ball-milling journal February 2019
FTIR spectroscopy study of CO and NO adsorption and co-adsorption on Pt/TiO2 journal September 2007
Nanoparticle decoration with surfactants: Molecular interactions, assembly, and applications journal February 2017
Reaction of atomic oxygen with a Pt() surface: chemical and structural determination using XPS, CAICISS and LEED journal November 2003
CO-Induced Restructuring on Stepped Pt Surfaces: A Molecular Dynamics Study journal August 2016
XPS Study of Stability and Reactivity of Oxidized Pt Nanoparticles Supported on TiO 2 journal August 2017
In Situ Tracking of Nonthermal Plasma Etching of ZIF-8 Films journal April 2022
Plasma Cleaning of Cationic Surfactants from Pd Nanoparticle Surfaces: Implications for Hydrogen Sorption journal May 2023
The Critical Impacts of Ligands on Heterogeneous Nanocatalysis: A Review journal May 2021
Manipulating the Microenvironment of Surfactant-Encapsulated Pt Nanoparticles to Promote Activity and Selectivity journal October 2022
Plasma-Enabled Ligand Removal for Improved Catalysis: Furfural Conversion on Pd/SiO2 journal October 2023
Gold Nanoparticles with Tipped Surface Structures as Substrates for Single-Particle Surface-Enhanced Raman Spectroscopy: Concave Nanocubes, Nanotrisoctahedra, and Nanostars journal September 2014
Surfactant Removal for Colloidal Nanoparticles from Solution Synthesis: The Effect on Catalytic Performance journal June 2012
Monodisperse MFe 2 O 4 (M = Fe, Co, Mn) Nanoparticles journal January 2004
Homogeneously Alloyed CdS x Se 1 - x Nanocrystals:  Synthesis, Characterization, and Composition/Size-Dependent Band Gap journal September 2006
Chemisorption of CO and Mechanism of CO Oxidation on Supported Platinum Nanoclusters journal March 2011
Selective Synthesis of Single-Crystalline Rhombic Dodecahedral, Octahedral, and Cubic Gold Nanocrystals journal January 2009
Sub-10 nm Platinum Nanocrystals with Size and Shape Control: Catalytic Study for Ethylene and Pyrrole Hydrogenation journal April 2009
Probing the Interaction of Poly(vinylpyrrolidone) with Platinum Nanocrystals by UV−Raman and FTIR journal October 2006
Vibrational Sum Frequency Generation Spectroscopy of Dodecanethiol on Metal Nanoparticles journal June 2007
Local Refractive Index Sensing Based on Edge Gold-Coated Silver Nanoprisms journal October 2013
Electrocatalytic Reduction of Oxygen by FePt Alloy Nanoparticles journal March 2008
Sum Frequency Generation and Catalytic Reaction Studies of the Removal of Organic Capping Agents from Pt Nanoparticles by UV−Ozone Treatment journal February 2009
Monodisperse Pt 3 Co Nanoparticles as a Catalyst for the Oxygen Reduction Reaction: Size-Dependent Activity journal October 2009
Multimetallic Au/FePt 3 Nanoparticles as Highly Durable Electrocatalyst journal March 2011
Selective Excitation of Individual Plasmonic Hotspots at the Tips of Single Gold Nanostars journal February 2011
Tunable Plasmonic Nanoparticles with Catalytically Active High-Index Facets journal May 2014
Synthesis and Oxygen Reduction Activity of Shape-Controlled Pt 3 Ni Nanopolyhedra journal February 2010
Emerging Device Applications for Semiconducting Two-Dimensional Transition Metal Dichalcogenides journal January 2014
Au Nanomatryoshkas as Efficient Near-Infrared Photothermal Transducers for Cancer Treatment: Benchmarking against Nanoshells journal May 2014
Quantum Dot Sensitized Solar Cells. A Tale of Two Semiconductor Nanocrystals: CdSe and CdTe journal May 2009
Nanocrystal bilayer for tandem catalysis journal April 2011
Single-layer MoS2 transistors journal January 2011
The golden age: gold nanoparticles for biomedicine journal January 2012
Controlled one-step synthesis of Pt decorated octahedral Fe 3 O 4 and its excellent catalytic performance for CO oxidation journal January 2015
Single-particle study: effects of oxygen plasma treatment on structural and spectral changes of anisotropic gold nanorods journal January 2020
Characterization and global modelling of low-pressure hydrogen-based RF plasmas suitable for surface cleaning processes journal November 2013
Ambient pressure phase transitions over Ir(1 1 1): at the onset of CO oxidation journal October 2017
A Brief Review on Atmospheric Air Plasma journal October 2021
Colloidal Nanocrystal Shape and Size Control: The Case of Cobalt journal March 2001
Shape-Controlled Synthesis of Gold and Silver Nanoparticles journal December 2002
Topotactic Interconversion of Nanoparticle Superlattices journal August 2013
Identification of active sites in CO oxidation and water-gas shift over supported Pt catalysts journal September 2015
Effects of Plasma Treated Alumina Nanoparticles on Breakdown Strength, Partial Discharge Resistance, and Thermophysical Properties of Mineral Oil-Based Nanofluids journal June 2021