Preparation and Characterization of Large Area Li-NASICON Electrolyte Thick Films

The preparation of solid electrolyte ceramic membranes is the object of intense study for its fundamental parts in the development of all solid-state batteries and improved battery separators. In this work, the procurement of large area solid electrolyte ceramic thick film membranes of the Li-NASICO...

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Main Authors: Ricardo Jiménez, Isabel Sobrados, Sandra Martínez-Chaparro, Angel Adolfo del Campo, M. Lourdes Calzada, Jesús Sanz, Shu Yi Tsai, Ming Rui Lin, Kuan Zong Fung, Edvardas Kazakevicius, Algimantas Kežionis
Format: Article
Language:English
Published: MDPI AG 2019-08-01
Series:Inorganics
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Online Access:https://www.mdpi.com/2304-6740/7/9/107
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author Ricardo Jiménez
Isabel Sobrados
Sandra Martínez-Chaparro
Angel Adolfo del Campo
M. Lourdes Calzada
Jesús Sanz
Shu Yi Tsai
Ming Rui Lin
Kuan Zong Fung
Edvardas Kazakevicius
Algimantas Kežionis
author_facet Ricardo Jiménez
Isabel Sobrados
Sandra Martínez-Chaparro
Angel Adolfo del Campo
M. Lourdes Calzada
Jesús Sanz
Shu Yi Tsai
Ming Rui Lin
Kuan Zong Fung
Edvardas Kazakevicius
Algimantas Kežionis
author_sort Ricardo Jiménez
collection DOAJ
description The preparation of solid electrolyte ceramic membranes is the object of intense study for its fundamental parts in the development of all solid-state batteries and improved battery separators. In this work, the procurement of large area solid electrolyte ceramic thick film membranes of the Li-NASICON Li<sub>1.3</sub>Al<sub>0.3</sub>Ti<sub>1.7</sub>(PO<sub>4</sub>)<sub>3</sub> (LATP) composition is attempted. Through the use of LATP powders from a sol&#8722;gel reaction, a slurry is formulated and tape casted. The green tapes are sintered using two sintering times. In both cases, ceramic thick films of a 5.5 &#215; 5.5 cm<sup>2</sup> area and &#8776;250 &#181;m average thickness were obtained. The characterization indicated almost pure phase samples with a bi-modal microstructure composed of large and smaller grains, being larger for longer sintering time. The samples are porous and brittle, presenting very high &#8220;bulk&#8221; conductivity but lower total direct current (DC) one, as compared with the commercial Li-NASICON (OHARA) thick films with a similar area. The larger the grains, the poorer the total conductivity and the mechanical properties of the thick-films. The formation of poorly adhering grain boundaries as the grain size grows is responsible for the worsened properties. A better control of the microstructure is mandatory.
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spelling doaj.art-9eb75d9b0deb468080e26a5027f95e9f2022-12-22T01:08:34ZengMDPI AGInorganics2304-67402019-08-017910710.3390/inorganics7090107inorganics7090107Preparation and Characterization of Large Area Li-NASICON Electrolyte Thick FilmsRicardo Jiménez0Isabel Sobrados1Sandra Martínez-Chaparro2Angel Adolfo del Campo3M. Lourdes Calzada4Jesús Sanz5Shu Yi Tsai6Ming Rui Lin7Kuan Zong Fung8Edvardas Kazakevicius9Algimantas Kežionis10Instituto de Ciencia de Materiales de Madrid, ICMM-CSIC. C/Sor Juana Inés de la Cruz 3, Cantoblanco, 28049 Madrid, SpainInstituto de Ciencia de Materiales de Madrid, ICMM-CSIC. C/Sor Juana Inés de la Cruz 3, Cantoblanco, 28049 Madrid, SpainInstituto de Ciencia de Materiales de Madrid, ICMM-CSIC. C/Sor Juana Inés de la Cruz 3, Cantoblanco, 28049 Madrid, SpainInstituto de Cerámica y Vidrio, ICV-CSIC. C/Kelsen 5, Cantoblanco, 28049 Madrid, SpainInstituto de Ciencia de Materiales de Madrid, ICMM-CSIC. C/Sor Juana Inés de la Cruz 3, Cantoblanco, 28049 Madrid, SpainInstituto de Ciencia de Materiales de Madrid, ICMM-CSIC. C/Sor Juana Inés de la Cruz 3, Cantoblanco, 28049 Madrid, SpainDepartment of Materials Science and Engineering, National Cheng Kung University, No. 1, University Road, Tainan City 70101, TaiwanDepartment of Materials Science and Engineering, National Cheng Kung University, No. 1, University Road, Tainan City 70101, TaiwanDepartment of Materials Science and Engineering, National Cheng Kung University, No. 1, University Road, Tainan City 70101, TaiwanInstitute of Applied Electrodynamics and Telecommunications, Faculty of Physics, Vilnius University, Saulėtekio av. 9, LT-10222 Vilnius, LithuaniaInstitute of Applied Electrodynamics and Telecommunications, Faculty of Physics, Vilnius University, Saulėtekio av. 9, LT-10222 Vilnius, LithuaniaThe preparation of solid electrolyte ceramic membranes is the object of intense study for its fundamental parts in the development of all solid-state batteries and improved battery separators. In this work, the procurement of large area solid electrolyte ceramic thick film membranes of the Li-NASICON Li<sub>1.3</sub>Al<sub>0.3</sub>Ti<sub>1.7</sub>(PO<sub>4</sub>)<sub>3</sub> (LATP) composition is attempted. Through the use of LATP powders from a sol&#8722;gel reaction, a slurry is formulated and tape casted. The green tapes are sintered using two sintering times. In both cases, ceramic thick films of a 5.5 &#215; 5.5 cm<sup>2</sup> area and &#8776;250 &#181;m average thickness were obtained. The characterization indicated almost pure phase samples with a bi-modal microstructure composed of large and smaller grains, being larger for longer sintering time. The samples are porous and brittle, presenting very high &#8220;bulk&#8221; conductivity but lower total direct current (DC) one, as compared with the commercial Li-NASICON (OHARA) thick films with a similar area. The larger the grains, the poorer the total conductivity and the mechanical properties of the thick-films. The formation of poorly adhering grain boundaries as the grain size grows is responsible for the worsened properties. A better control of the microstructure is mandatory.https://www.mdpi.com/2304-6740/7/9/107Li-NASICONceramicthick-filmslarge areamicrostructureconfocal RamanMAS NMRbroad band impedanceionic conductivityYoung’s modulus
spellingShingle Ricardo Jiménez
Isabel Sobrados
Sandra Martínez-Chaparro
Angel Adolfo del Campo
M. Lourdes Calzada
Jesús Sanz
Shu Yi Tsai
Ming Rui Lin
Kuan Zong Fung
Edvardas Kazakevicius
Algimantas Kežionis
Preparation and Characterization of Large Area Li-NASICON Electrolyte Thick Films
Inorganics
Li-NASICON
ceramic
thick-films
large area
microstructure
confocal Raman
MAS NMR
broad band impedance
ionic conductivity
Young’s modulus
title Preparation and Characterization of Large Area Li-NASICON Electrolyte Thick Films
title_full Preparation and Characterization of Large Area Li-NASICON Electrolyte Thick Films
title_fullStr Preparation and Characterization of Large Area Li-NASICON Electrolyte Thick Films
title_full_unstemmed Preparation and Characterization of Large Area Li-NASICON Electrolyte Thick Films
title_short Preparation and Characterization of Large Area Li-NASICON Electrolyte Thick Films
title_sort preparation and characterization of large area li nasicon electrolyte thick films
topic Li-NASICON
ceramic
thick-films
large area
microstructure
confocal Raman
MAS NMR
broad band impedance
ionic conductivity
Young’s modulus
url https://www.mdpi.com/2304-6740/7/9/107
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