Comprehensive Magnetic Study of Nanostructured Mesoporous Manganese Oxide Materials and Implications for Catalytic Behavior

Moharreri, Ehsan; Hines, William A.; Biswas, Sourav; Perry, David M.; He, Junkai; Murray-Simmons, Dustin; Suib, Steven L.

doi:10.1021/acs.chemmater.7b05280

Title: Comprehensive Magnetic Study of Nanostructured Mesoporous Manganese Oxide Materials and Implications for Catalytic Behavior

Abstract

Magnetic behavior of nanostructured mesoporous manganese oxide materials, designated UCT-1 and UCT-18, were studied using a combination of superconducting quantum interference device (SQUID) magnetometry and ⁵⁵Mn zero-field spin–echo nuclear magnetic resonance (NMR). Curie–Weiss fits to the magnetic susceptibility for the UCT-1 and UCT-18 samples calcined at 550 °C yielded paramagnetic moment values consistent with spin-only Mn³⁺ ions in the α-Mn₂O₃ phase (S = 2, 4.90 μ_B). However, the magnetization and NMR results reported here clearly identify a small amount of the Mn₃O₄ second phase (ferrimagnetic with T_C ≈ 43 K) that does not appear in X-ray diffraction (XRD). We report the study resulted in the observation of fascinating magnetic behavior: (1) exchange bias, which occurs in cases where a ferromagnetic (or ferrimagnetic) phase forms a boundary with an antiferromagnetic phase and (2) a magnetic contribution attributed to uncompensated spins on the surfaces of the α-Mn₂O₃ nanoparticles. The presence of Mn₃O₄ and the interplay of Mn³⁺ and Mn²⁺ impact the catalytic properties.

Authors:

^[1]; Hines, William A. ^[1]; Biswas, Sourav ^[1]; Perry, David M. ^[1]; He, Junkai ^[1]; Murray-Simmons, Dustin ^[1];

^[1]

Univ. of Connecticut, Storrs, CT (United States)

Publication Date:: Mon Jan 29 00:00:00 EST 2018

Research Org.:: Univ. of Connecticut, Storrs, CT (United States)

Sponsoring Org.:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences, and Biosciences Division

OSTI Identifier:: 1597814

Grant/Contract Number:: FG02-86ER13622

Resource Type:: Accepted Manuscript

Journal Name:: Chemistry of Materials

Additional Journal Information:: Journal Volume: 30; Journal Issue: 3; Journal ID: ISSN 0897-4756

Publisher:: American Chemical Society (ACS)

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Oxides; Nanoparticles; Magnetic properties; Physical and chemical processes; Transition metals

Citation Formats


                    Moharreri, Ehsan, Hines, William A., Biswas, Sourav, Perry, David M., He, Junkai, Murray-Simmons, Dustin, and Suib, Steven L. Comprehensive Magnetic Study of Nanostructured Mesoporous Manganese Oxide Materials and Implications for Catalytic Behavior.  United States: N. p., 2018. 
Web.  doi:10.1021/acs.chemmater.7b05280.

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                    Moharreri, Ehsan, Hines, William A., Biswas, Sourav, Perry, David M., He, Junkai, Murray-Simmons, Dustin, & Suib, Steven L. Comprehensive Magnetic Study of Nanostructured Mesoporous Manganese Oxide Materials and Implications for Catalytic Behavior.  United States.  https://doi.org/10.1021/acs.chemmater.7b05280

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                    Moharreri, Ehsan, Hines, William A., Biswas, Sourav, Perry, David M., He, Junkai, Murray-Simmons, Dustin, and Suib, Steven L. Mon .  
"Comprehensive Magnetic Study of Nanostructured Mesoporous Manganese Oxide Materials and Implications for Catalytic Behavior".  United States.  https://doi.org/10.1021/acs.chemmater.7b05280.  https://www.osti.gov/servlets/purl/1597814.

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@article{osti_1597814,

  title        = {Comprehensive Magnetic Study of Nanostructured Mesoporous Manganese Oxide Materials and Implications for Catalytic Behavior},

  author       = {Moharreri, Ehsan and Hines, William A. and Biswas, Sourav and Perry, David M. and He, Junkai and Murray-Simmons, Dustin and Suib, Steven L.},

  abstractNote = {Magnetic behavior of nanostructured mesoporous manganese oxide materials, designated UCT-1 and UCT-18, were studied using a combination of superconducting quantum interference device (SQUID) magnetometry and 55Mn zero-field spin–echo nuclear magnetic resonance (NMR). Curie–Weiss fits to the magnetic susceptibility for the UCT-1 and UCT-18 samples calcined at 550 °C yielded paramagnetic moment values consistent with spin-only Mn3+ ions in the α-Mn2O3 phase (S = 2, 4.90 μB). However, the magnetization and NMR results reported here clearly identify a small amount of the Mn3O4 second phase (ferrimagnetic with TC ≈ 43 K) that does not appear in X-ray diffraction (XRD). We report the study resulted in the observation of fascinating magnetic behavior: (1) exchange bias, which occurs in cases where a ferromagnetic (or ferrimagnetic) phase forms a boundary with an antiferromagnetic phase and (2) a magnetic contribution attributed to uncompensated spins on the surfaces of the α-Mn2O3 nanoparticles. The presence of Mn3O4 and the interplay of Mn3+ and Mn2+ impact the catalytic properties.},

  doi          = {10.1021/acs.chemmater.7b05280},

  journal      = {Chemistry of Materials},

  number       = 3,

  volume       = 30,

  place        = {United States},

  year         = {Mon Jan 29 00:00:00 EST 2018},

  month        = {Mon Jan 29 00:00:00 EST 2018}

}

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Title: Comprehensive Magnetic Study of Nanostructured Mesoporous Manganese Oxide Materials and Implications for Catalytic Behavior

Abstract

Citation Formats

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Antiferromagnetic MnO nanoparticles with ferrimagnetic Mn 3 O 4 shells: Doubly inverted core-shell system journal, January 2008

Distinguishing the core from the shell in MnOx/MnOy and FeOx/MnOx core/shell nanoparticles through quantitative electron energy loss spectroscopy (EELS) analysis journal, January 2012

Magnetic and Crystallographic Transitions in the α − Mn 2 O 3 − Fe 2 O 3 System journal, November 1968

Magnetism of Mn 2 O 3 nanocrystals dispersed in a silica matrix: Size effects and phase transformations journal, September 2006

Surface anisotropy effects in NiO nanoparticles journal, October 2005

Nanorods of manganese oxalate: a single source precursor to different manganese oxide nanoparticles (MnO, Mn2O3, Mn3O4) journal, January 2004

Formation and magnetic behaviour of manganese oxide nanoparticles journal, March 2010

Advanced Materials for Next‐Generation Spacecraft journal, August 2018

Aerobic Self‐Esterification of Alcohols Assisted by Mesoporous Manganese and Cobalt Oxide journal, June 2019

Ordered mesoporous molecular sieves synthesized by a liquid-crystal template mechanism
journal, October 1992

Synthesis of Hard Magnetic Ordered Mesoporous Co ₃ O ₄ /CoFe ₂ O ₄ Nanocomposites
journal, June 2012

Highly Ordered Mesoporous Cobalt Oxide Nanostructures: Synthesis, Characterisation, Magnetic Properties, and Applications for Electrochemical Energy Devices
journal, August 2010

Controlled Synthesis of Self-Assembled Metal Oxide Hollow Spheres Via Tuning Redox Potentials: Versatile Nanostructured Cobalt Oxides
journal, March 2008

Facile Synthesis and Characterization of Novel Mesoporous and Mesorelief Oxides with Gyroidal Structures
journal, January 2004

Ion induced promotion of activity enhancement of mesoporous manganese oxides for aerobic oxidation reactions
journal, April 2015

Aerobic Oxidation of Amines to Imines by Cesium-Promoted Mesoporous Manganese Oxide
journal, June 2015

Mesoporous Mn2O3 and Mn3O4 with Crystalline Walls
journal, November 2007

Mesoporous Copper/Manganese Oxide Catalyzed Coupling of Alkynes: Evidence for Synergistic Cooperative Catalysis
journal, July 2016

Manganese Oxides with Rod-, Wire-, Tube-, and Flower-Like Morphologies: Highly Effective Catalysts for the Removal of Toluene
journal, March 2012

Heterogeneous Sodium-Manganese Oxide Catalyzed Aerobic Oxidative Cleavage of 1,2-Diols
journal, July 2017

Charge localization and successive magnetic phase transitions of mixed-valence manganese oxides $K_{1.5} {(H}_{3} {O)}_{x} {Mn}_{8} O_{16}$ $(0 < x < 0.5)$
journal, May 1999

A general approach to crystalline and monomodal pore size mesoporous materials
journal, December 2013

Studies of the Hierarchical Structure in UCT Manganese Oxides
journal, July 2017

Cross Sectional Analysis of Cation Doped Transition Metal Oxide Mesoporous Catalyst Materials
journal, July 2017

Robust Mesoporous Manganese Oxide Catalysts for Water Oxidation
journal, February 2015

Mesoporous Co ₃ O ₄ with Controlled Porosity: Inverse Micelle Synthesis and High-Performance Catalytic CO Oxidation at −60 °C
journal, July 2014

Synthesis of Mesoporous Iron Oxides by an Inverse Micelle Method and Their Application in the Degradation of Orange II under Visible Light at Neutral pH
journal, April 2015

Mesoporous Manganese Oxide Catalyzed Aerobic Oxidative Coupling of Anilines To Aromatic Azo Compounds
journal, January 2016

Cross dehydrogenative coupling of N -aryltetrahydroisoquinolines (sp ³ C–H) with indoles (sp ² C–H) using a heterogeneous mesoporous manganese oxide catalyst
journal, January 2017

Morphology-conserved transformation: synthesis of hierarchical mesoporous nanostructures of Mn2O3 and the nanostructural effects on Li-ion insertion/deinsertion properties
journal, January 2011

Mn ₅ O ₈ Nanoparticles as Efficient Water Oxidation Catalysts at Neutral pH
journal, July 2015

Structure–Property Relationship of Bifunctional MnO ₂ Nanostructures: Highly Efficient, Ultra-Stable Electrochemical Water Oxidation and Oxygen Reduction Reaction Catalysts Identified in Alkaline Media
journal, August 2014

Urchin-Shaped Manganese Oxide Nanoparticles as pH-Responsive Activatable T1 Contrast Agents for Magnetic Resonance Imaging
journal, September 2011

Manganese oxide-based materials as electrochemical supercapacitor electrodes
journal, January 2011

Nanostructured carbon–metal oxide composite electrodes for supercapacitors: a review
journal, January 2013

Nanoscale metal oxide-based heterojunctions for gas sensing: A review
journal, December 2014

Band Bending in Semiconductors: Chemical and Physical Consequences at Surfaces and Interfaces
journal, June 2012

Magnetic and Crystallographic Transitions in ${Sc}^{3 +}$ , ${Cr}^{3 +}$ , and ${Ga}^{3 +}$ Substituted ${Mn}_{2}$ $O_{3}$
journal, May 1970

Spin state of Mn $_{3}$ O $_{4}$ investigated by $^{55}$ Mn nuclear magnetic resonance
journal, November 2011

Adsorption of Gases in Multimolecular Layers
journal, February 1938

The Determination of Pore Volume and Area Distributions in Porous Substances. I. Computations from Nitrogen Isotherms
journal, January 1951

Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report)
journal, October 2015

⁵⁵ Mn nuclear magnetic resonance for antiferromagnetic α-Mn ₂ O ₃
journal, January 2011

The enhancement effect in the domain and domain wall in Fe ⁵⁷ nuclear magnetic resonance
journal, February 1997

A Magnetic Route to Measure the Average Oxidation State of Mixed-Valent Manganese in Manganese Oxide Octahedral Molecular Sieves (OMS)
journal, May 2005

Enhanced Magnetic Properties in Antiferromagnetic-Core/Ferrimagnetic-Shell Nanoparticles
journal, April 2015

Synthesis and Size-Dependent Exchange Bias in Inverted Core−Shell MnO|Mn ₃ O ₄ Nanoparticles
journal, July 2007

Exchange bias in nanostructures
journal, December 2005

Antiferromagnetic MnO nanoparticles with ferrimagnetic ${Mn}_{3} O_{4}$ shells: Doubly inverted core-shell system
journal, January 2008

Distinguishing the core from the shell in MnOx/MnOy and FeOx/MnOx core/shell nanoparticles through quantitative electron energy loss spectroscopy (EELS) analysis
journal, January 2012

Magnetic and Crystallographic Transitions in the $α - {Mn}_{2} O_{3} - {Fe}_{2} O_{3}$ System
journal, November 1968

Magnetism of ${Mn}_{2} O_{3}$ nanocrystals dispersed in a silica matrix: Size effects and phase transformations
journal, September 2006

Surface anisotropy effects in NiO nanoparticles
journal, October 2005

Nanorods of manganese oxalate: a single source precursor to different manganese oxide nanoparticles (MnO, Mn2O3, Mn3O4)
journal, January 2004

Formation and magnetic behaviour of manganese oxide nanoparticles
journal, March 2010

Advanced Materials for Next‐Generation Spacecraft
journal, August 2018

Aerobic Self‐Esterification of Alcohols Assisted by Mesoporous Manganese and Cobalt Oxide
journal, June 2019