Thermal analysis study of LiFeO2 formation from Li2CO3–Fe2O3 mechanically activated reagents

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Abstract

The solid-phase synthesis of LiFeO2 lithium ferrite from mechanically activated Fe2O3–Li2CO3 initial reagent mixtures was investigated by X-ray powder diffraction and thermal analysis techniques. The mechanical milling of powder mixture was carried out by AGO-2S planetary ball mill with a rotation speed of 2220 rpm for 60 min. According to the XRD data, the crystallite sizes of milled reagents decrease as a result of ball milling. From thermal analysis, it was shown that the ferrite synthesis starts with the interaction between reagents and lithium carbonate decomposition and accompanied by mass loss process due to CO2 evaporation. For non-milled mixtures, the mass loss process occurs in the temperature range 400–740 °C and comprises two steps. As for milled samples, this process shifts toward lower temperatures, where a slight mass loss process is observed from 100 °C up to 400 °C, while the main mass loss occurs in the temperature range of 400–550 °C in one stage. The results indicate that the major mechanism of solid-state reaction can be attributed to the two-step model of the reaction proceed, whose rate is diffusion controlled over the entire temperature range for non-milled mixture, but corresponds to the diffusion and n-order equation depending on conversion degree for milled mixture. Generally, a preliminary mechanical activation of Fe2O3–Li2CO3 considerably enhances the reactivity of the solid-phase system, thereby reducing the temperature of lithium ferrite thermal synthesis. Thus, LiFeO2 ferrite can be obtained from reagents mixture mechanically activated for 60 min at temperature of 600 °C for 2 h, that is, at a significantly lower synthesis time and temperature than in the case of using conventional solid-state synthesis from non-milled reagents.

Original languageEnglish
Pages (from-to)81-87
Number of pages7
JournalJournal of Thermal Analysis and Calorimetry
Volume134
Issue number1
DOIs
Publication statusPublished - 1 Oct 2018

Fingerprint

Thermoanalysis
reagents
thermal analysis
ferrites
Ferrite
synthesis
lithium
Temperature
temperature
solid phases
balls
Lithium
solid state
Lithium Carbonate
Ball mills
Ball milling
Crystallite size
Solid state reactions
carbonates
Powders

Keywords

  • Ball milling
  • LiFeO
  • Lithium ferrites
  • Mechanical activation
  • Solid-phase synthesis
  • TG/DSC
  • Thermal analysis

ASJC Scopus subject areas

  • Condensed Matter Physics
  • Physical and Theoretical Chemistry

Cite this

@article{0431fbcb49d348caaf20da8e8b201b7a,
title = "Thermal analysis study of LiFeO2 formation from Li2CO3–Fe2O3 mechanically activated reagents",
abstract = "The solid-phase synthesis of LiFeO2 lithium ferrite from mechanically activated Fe2O3–Li2CO3 initial reagent mixtures was investigated by X-ray powder diffraction and thermal analysis techniques. The mechanical milling of powder mixture was carried out by AGO-2S planetary ball mill with a rotation speed of 2220 rpm for 60 min. According to the XRD data, the crystallite sizes of milled reagents decrease as a result of ball milling. From thermal analysis, it was shown that the ferrite synthesis starts with the interaction between reagents and lithium carbonate decomposition and accompanied by mass loss process due to CO2 evaporation. For non-milled mixtures, the mass loss process occurs in the temperature range 400–740 °C and comprises two steps. As for milled samples, this process shifts toward lower temperatures, where a slight mass loss process is observed from 100 °C up to 400 °C, while the main mass loss occurs in the temperature range of 400–550 °C in one stage. The results indicate that the major mechanism of solid-state reaction can be attributed to the two-step model of the reaction proceed, whose rate is diffusion controlled over the entire temperature range for non-milled mixture, but corresponds to the diffusion and n-order equation depending on conversion degree for milled mixture. Generally, a preliminary mechanical activation of Fe2O3–Li2CO3 considerably enhances the reactivity of the solid-phase system, thereby reducing the temperature of lithium ferrite thermal synthesis. Thus, LiFeO2 ferrite can be obtained from reagents mixture mechanically activated for 60 min at temperature of 600 °C for 2 h, that is, at a significantly lower synthesis time and temperature than in the case of using conventional solid-state synthesis from non-milled reagents.",
keywords = "Ball milling, LiFeO, Lithium ferrites, Mechanical activation, Solid-phase synthesis, TG/DSC, Thermal analysis",
author = "Lysenko, {Elena N.} and Surzhikov, {Anatoly P.} and Nikolaev, {Evgeniy V.} and Vlasov, {Vitaly A.}",
year = "2018",
month = "10",
day = "1",
doi = "10.1007/s10973-018-7113-2",
language = "English",
volume = "134",
pages = "81--87",
journal = "Journal of Thermal Analysis and Calorimetry",
issn = "1388-6150",
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TY - JOUR

T1 - Thermal analysis study of LiFeO2 formation from Li2CO3–Fe2O3 mechanically activated reagents

AU - Lysenko, Elena N.

AU - Surzhikov, Anatoly P.

AU - Nikolaev, Evgeniy V.

AU - Vlasov, Vitaly A.

PY - 2018/10/1

Y1 - 2018/10/1

N2 - The solid-phase synthesis of LiFeO2 lithium ferrite from mechanically activated Fe2O3–Li2CO3 initial reagent mixtures was investigated by X-ray powder diffraction and thermal analysis techniques. The mechanical milling of powder mixture was carried out by AGO-2S planetary ball mill with a rotation speed of 2220 rpm for 60 min. According to the XRD data, the crystallite sizes of milled reagents decrease as a result of ball milling. From thermal analysis, it was shown that the ferrite synthesis starts with the interaction between reagents and lithium carbonate decomposition and accompanied by mass loss process due to CO2 evaporation. For non-milled mixtures, the mass loss process occurs in the temperature range 400–740 °C and comprises two steps. As for milled samples, this process shifts toward lower temperatures, where a slight mass loss process is observed from 100 °C up to 400 °C, while the main mass loss occurs in the temperature range of 400–550 °C in one stage. The results indicate that the major mechanism of solid-state reaction can be attributed to the two-step model of the reaction proceed, whose rate is diffusion controlled over the entire temperature range for non-milled mixture, but corresponds to the diffusion and n-order equation depending on conversion degree for milled mixture. Generally, a preliminary mechanical activation of Fe2O3–Li2CO3 considerably enhances the reactivity of the solid-phase system, thereby reducing the temperature of lithium ferrite thermal synthesis. Thus, LiFeO2 ferrite can be obtained from reagents mixture mechanically activated for 60 min at temperature of 600 °C for 2 h, that is, at a significantly lower synthesis time and temperature than in the case of using conventional solid-state synthesis from non-milled reagents.

AB - The solid-phase synthesis of LiFeO2 lithium ferrite from mechanically activated Fe2O3–Li2CO3 initial reagent mixtures was investigated by X-ray powder diffraction and thermal analysis techniques. The mechanical milling of powder mixture was carried out by AGO-2S planetary ball mill with a rotation speed of 2220 rpm for 60 min. According to the XRD data, the crystallite sizes of milled reagents decrease as a result of ball milling. From thermal analysis, it was shown that the ferrite synthesis starts with the interaction between reagents and lithium carbonate decomposition and accompanied by mass loss process due to CO2 evaporation. For non-milled mixtures, the mass loss process occurs in the temperature range 400–740 °C and comprises two steps. As for milled samples, this process shifts toward lower temperatures, where a slight mass loss process is observed from 100 °C up to 400 °C, while the main mass loss occurs in the temperature range of 400–550 °C in one stage. The results indicate that the major mechanism of solid-state reaction can be attributed to the two-step model of the reaction proceed, whose rate is diffusion controlled over the entire temperature range for non-milled mixture, but corresponds to the diffusion and n-order equation depending on conversion degree for milled mixture. Generally, a preliminary mechanical activation of Fe2O3–Li2CO3 considerably enhances the reactivity of the solid-phase system, thereby reducing the temperature of lithium ferrite thermal synthesis. Thus, LiFeO2 ferrite can be obtained from reagents mixture mechanically activated for 60 min at temperature of 600 °C for 2 h, that is, at a significantly lower synthesis time and temperature than in the case of using conventional solid-state synthesis from non-milled reagents.

KW - Ball milling

KW - LiFeO

KW - Lithium ferrites

KW - Mechanical activation

KW - Solid-phase synthesis

KW - TG/DSC

KW - Thermal analysis

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U2 - 10.1007/s10973-018-7113-2

DO - 10.1007/s10973-018-7113-2

M3 - Article

VL - 134

SP - 81

EP - 87

JO - Journal of Thermal Analysis and Calorimetry

JF - Journal of Thermal Analysis and Calorimetry

SN - 1388-6150

IS - 1

ER -