Microwave-assisted hydrothermal synthesis of nanocrystalline lithium-ion sieve from biogenic manganese oxide, its characterization and lithium sorption studies

Qianqian Yu, Keiko Sasaki

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6 Citations (Scopus)

Abstract

Biogenic birnessite (BB) is a stable form of manganese oxide. It is widely distributed in the natural environment and originates from microbial oxidation. It has potential applications in functional material fabrication because of its unique morphology. Using a microwave-assisted hydrothermal method, nano-sized lithium-ion sieves were prepared from BB with a short reaction time. A combination of sorption experiments and structural characterization was used to compare Li uptake by nanoparticles with that by microparticles. X-ray diffraction (XRD) patterns showed that the nano- and microparticles had similar fundamental structures, but the lattice parameter of nanoparticles is smaller than microparticles. Mn K-edge X-ray absorption fine structure (XAFS) spectroscopy showed that the oxidation state of Mn increased from 3.50 to 3.69 with decreasing crystal size, and the Mn–Mn atomic distance decreased from 2.92 to 2.89 Å. Li extraction resulted in significant cleavage of the microparticle surfaces. The oxidation state of Mn increased to 4.0, and the Mn–Mn atomic distance decreased to 2.86 Å. XRD showed that dissolution of the polycrystalline phase of the nanoparticles occurred during acid washing. However, the EXAFS spectrum was similar to that of the original material before acid washing. The specific surface areas and Li-sorption capacities of the nano-sized lithium-ion sieves prepared from manganese carbonate were significantly higher than those of a similarly prepared micro-sized lithium-ion sieve. The results obtained in this work suggest that BB is a promising starting material for the energy-saving fabrication of functional materials for highly efficient Li recovery.

Original languageEnglish
Pages (from-to)118-124
Number of pages7
JournalHydrometallurgy
Volume165
DOIs
Publication statusPublished - Oct 1 2016

Fingerprint

Manganese oxide
Sieves
Hydrothermal synthesis
Lithium
Sorption
Microwaves
Ions
Nanoparticles
Functional materials
Washing
Oxidation
X ray absorption fine structure spectroscopy
Fabrication
X ray diffraction
Acids
Specific surface area
Diffraction patterns
Lattice constants
Manganese
Carbonates

All Science Journal Classification (ASJC) codes

  • Industrial and Manufacturing Engineering
  • Metals and Alloys
  • Materials Chemistry

Cite this

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title = "Microwave-assisted hydrothermal synthesis of nanocrystalline lithium-ion sieve from biogenic manganese oxide, its characterization and lithium sorption studies",
abstract = "Biogenic birnessite (BB) is a stable form of manganese oxide. It is widely distributed in the natural environment and originates from microbial oxidation. It has potential applications in functional material fabrication because of its unique morphology. Using a microwave-assisted hydrothermal method, nano-sized lithium-ion sieves were prepared from BB with a short reaction time. A combination of sorption experiments and structural characterization was used to compare Li uptake by nanoparticles with that by microparticles. X-ray diffraction (XRD) patterns showed that the nano- and microparticles had similar fundamental structures, but the lattice parameter of nanoparticles is smaller than microparticles. Mn K-edge X-ray absorption fine structure (XAFS) spectroscopy showed that the oxidation state of Mn increased from 3.50 to 3.69 with decreasing crystal size, and the Mn–Mn atomic distance decreased from 2.92 to 2.89 {\AA}. Li extraction resulted in significant cleavage of the microparticle surfaces. The oxidation state of Mn increased to 4.0, and the Mn–Mn atomic distance decreased to 2.86 {\AA}. XRD showed that dissolution of the polycrystalline phase of the nanoparticles occurred during acid washing. However, the EXAFS spectrum was similar to that of the original material before acid washing. The specific surface areas and Li-sorption capacities of the nano-sized lithium-ion sieves prepared from manganese carbonate were significantly higher than those of a similarly prepared micro-sized lithium-ion sieve. The results obtained in this work suggest that BB is a promising starting material for the energy-saving fabrication of functional materials for highly efficient Li recovery.",
author = "Qianqian Yu and Keiko Sasaki",
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N2 - Biogenic birnessite (BB) is a stable form of manganese oxide. It is widely distributed in the natural environment and originates from microbial oxidation. It has potential applications in functional material fabrication because of its unique morphology. Using a microwave-assisted hydrothermal method, nano-sized lithium-ion sieves were prepared from BB with a short reaction time. A combination of sorption experiments and structural characterization was used to compare Li uptake by nanoparticles with that by microparticles. X-ray diffraction (XRD) patterns showed that the nano- and microparticles had similar fundamental structures, but the lattice parameter of nanoparticles is smaller than microparticles. Mn K-edge X-ray absorption fine structure (XAFS) spectroscopy showed that the oxidation state of Mn increased from 3.50 to 3.69 with decreasing crystal size, and the Mn–Mn atomic distance decreased from 2.92 to 2.89 Å. Li extraction resulted in significant cleavage of the microparticle surfaces. The oxidation state of Mn increased to 4.0, and the Mn–Mn atomic distance decreased to 2.86 Å. XRD showed that dissolution of the polycrystalline phase of the nanoparticles occurred during acid washing. However, the EXAFS spectrum was similar to that of the original material before acid washing. The specific surface areas and Li-sorption capacities of the nano-sized lithium-ion sieves prepared from manganese carbonate were significantly higher than those of a similarly prepared micro-sized lithium-ion sieve. The results obtained in this work suggest that BB is a promising starting material for the energy-saving fabrication of functional materials for highly efficient Li recovery.

AB - Biogenic birnessite (BB) is a stable form of manganese oxide. It is widely distributed in the natural environment and originates from microbial oxidation. It has potential applications in functional material fabrication because of its unique morphology. Using a microwave-assisted hydrothermal method, nano-sized lithium-ion sieves were prepared from BB with a short reaction time. A combination of sorption experiments and structural characterization was used to compare Li uptake by nanoparticles with that by microparticles. X-ray diffraction (XRD) patterns showed that the nano- and microparticles had similar fundamental structures, but the lattice parameter of nanoparticles is smaller than microparticles. Mn K-edge X-ray absorption fine structure (XAFS) spectroscopy showed that the oxidation state of Mn increased from 3.50 to 3.69 with decreasing crystal size, and the Mn–Mn atomic distance decreased from 2.92 to 2.89 Å. Li extraction resulted in significant cleavage of the microparticle surfaces. The oxidation state of Mn increased to 4.0, and the Mn–Mn atomic distance decreased to 2.86 Å. XRD showed that dissolution of the polycrystalline phase of the nanoparticles occurred during acid washing. However, the EXAFS spectrum was similar to that of the original material before acid washing. The specific surface areas and Li-sorption capacities of the nano-sized lithium-ion sieves prepared from manganese carbonate were significantly higher than those of a similarly prepared micro-sized lithium-ion sieve. The results obtained in this work suggest that BB is a promising starting material for the energy-saving fabrication of functional materials for highly efficient Li recovery.

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