No Cover Image

E-Thesis 457 views 272 downloads

Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries / REBECCA GRIFFIN

Swansea University Author: REBECCA GRIFFIN

DOI (Published version): 10.23889/SUThesis.69884

Abstract

This thesis aims to synthesise the sodium super ionic conductor (NASICON) solid-state electrolyte for sodium-ion battery applications using two methodologies: solid-state and sol synthesis. The objective is to develop NASICON with enhanced chemical properties and minimised secondary phases by employ...

Full description

Published: Swansea University, Wales, UK 2025
Institution: Swansea University
Degree level: Doctoral
Degree name: Ph.D
Supervisor: Baker, J.
URI: https://cronfa.swan.ac.uk/Record/cronfa69884
first_indexed 2025-07-03T13:37:53Z
last_indexed 2025-07-04T06:42:55Z
id cronfa69884
recordtype RisThesis
fullrecord <?xml version="1.0"?><rfc1807><datestamp>2025-07-03T14:45:33.9578579</datestamp><bib-version>v2</bib-version><id>69884</id><entry>2025-07-03</entry><title>Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries</title><swanseaauthors><author><sid>d53a2269bf0c8beec668ccb9c3499f73</sid><firstname>REBECCA</firstname><surname>GRIFFIN</surname><name>REBECCA GRIFFIN</name><active>true</active><ethesisStudent>false</ethesisStudent></author></swanseaauthors><date>2025-07-03</date><abstract>This thesis aims to synthesise the sodium super ionic conductor (NASICON) solid-state electrolyte for sodium-ion battery applications using two methodologies: solid-state and sol synthesis. The objective is to develop NASICON with enhanced chemical properties and minimised secondary phases by employing less energy-intensive techniques. This involves transitioning from conventional oven heating to near-infrared (NIR) radiation sintering, achieved through the fabrication of NASICON as a thin film. All samples were characterised by x-ray diffraction (XRD) and scanning electron microscopy (SEM).NASICON was successfully synthesised using the solid-state technique, forming dense pellets (density: 2.80 g/cm3) that are 15 mm in diameter and 2 mm thick (&#xB1;0.05 mm). The final sintering step was conducted in a tube furnace in an inert environment (argon) at 1180 &#xBA;C for 16 hours, with the total oven time for the process being 70 hours and only 1.5% weight fraction secondary phase of ZrO2. Alumina crucibles and a powder bed were used to prevent the pellet fusing to the crucible (Al3+ diffusion) and reduce sodium volatilisation.The sol method also successfully formed a NASICON powder with a low secondary phase content of &lt;2%, aligned with literature values. The powder was prepared in a conventional oven (in air) with reduced sintering times of 3 hours and temperatures of 1000 &#xBA;C. Additionally, NASICON was synthesised as a dense 10 &#xB5;m thin film on a quartz substrate, utilising a sol spray coating technique. The same sintering times were employed as the powder (3 hours) but at lower a lower temperature of 950 &#xBA;C. The spray coating technique allowed the film to dry on a hot plate reducing the overall oven heating time from 16 hours (powder) to 3 hours (thin film).NIR radiation was successfully employed to synthesise NASICON as a thin film, a novel technique that has not previously been used in this field. This significantly reduced sintering times to 60 seconds, and overall oven/NIR heating times to 2 hours 2 minutes.</abstract><type>E-Thesis</type><journal/><volume/><journalNumber/><paginationStart/><paginationEnd/><publisher/><placeOfPublication>Swansea University, Wales, UK</placeOfPublication><isbnPrint/><isbnElectronic/><issnPrint/><issnElectronic/><keywords>Energy Storage, Sodium-ion, Battery, Solid-state, Electrolyte</keywords><publishedDay>21</publishedDay><publishedMonth>5</publishedMonth><publishedYear>2025</publishedYear><publishedDate>2025-05-21</publishedDate><doi>10.23889/SUThesis.69884</doi><url/><notes>A selection of content is redacted or is partially redacted from this thesis to protect sensitive and personal information.</notes><college>COLLEGE NANME</college><CollegeCode>COLLEGE CODE</CollegeCode><institution>Swansea University</institution><supervisor>Baker, J.</supervisor><degreelevel>Doctoral</degreelevel><degreename>Ph.D</degreename><degreesponsorsfunders>M2A</degreesponsorsfunders><apcterm/><funders>M2A</funders><projectreference/><lastEdited>2025-07-03T14:45:33.9578579</lastEdited><Created>2025-07-03T14:13:48.9718141</Created><path><level id="1">Faculty of Science and Engineering</level><level id="2">School of Engineering and Applied Sciences - Materials Science and Engineering</level></path><authors><author><firstname>REBECCA</firstname><surname>GRIFFIN</surname><order>1</order></author></authors><documents><document><filename>69884__34667__6ef79a7df56c4bd9af6641789bc2a3de.pdf</filename><originalFilename>2024_Griffin_R.final.69884.pdf</originalFilename><uploaded>2025-07-03T14:37:02.8101152</uploaded><type>Output</type><contentLength>12195089</contentLength><contentType>application/pdf</contentType><version>E-Thesis &#x2013; open access</version><cronfaStatus>true</cronfaStatus><documentNotes>Copyright: The author, Rebecca Griffin, 2024</documentNotes><copyrightCorrect>true</copyrightCorrect><language>eng</language></document></documents><OutputDurs/></rfc1807>
spelling 2025-07-03T14:45:33.9578579 v2 69884 2025-07-03 Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries d53a2269bf0c8beec668ccb9c3499f73 REBECCA GRIFFIN REBECCA GRIFFIN true false 2025-07-03 This thesis aims to synthesise the sodium super ionic conductor (NASICON) solid-state electrolyte for sodium-ion battery applications using two methodologies: solid-state and sol synthesis. The objective is to develop NASICON with enhanced chemical properties and minimised secondary phases by employing less energy-intensive techniques. This involves transitioning from conventional oven heating to near-infrared (NIR) radiation sintering, achieved through the fabrication of NASICON as a thin film. All samples were characterised by x-ray diffraction (XRD) and scanning electron microscopy (SEM).NASICON was successfully synthesised using the solid-state technique, forming dense pellets (density: 2.80 g/cm3) that are 15 mm in diameter and 2 mm thick (±0.05 mm). The final sintering step was conducted in a tube furnace in an inert environment (argon) at 1180 ºC for 16 hours, with the total oven time for the process being 70 hours and only 1.5% weight fraction secondary phase of ZrO2. Alumina crucibles and a powder bed were used to prevent the pellet fusing to the crucible (Al3+ diffusion) and reduce sodium volatilisation.The sol method also successfully formed a NASICON powder with a low secondary phase content of <2%, aligned with literature values. The powder was prepared in a conventional oven (in air) with reduced sintering times of 3 hours and temperatures of 1000 ºC. Additionally, NASICON was synthesised as a dense 10 µm thin film on a quartz substrate, utilising a sol spray coating technique. The same sintering times were employed as the powder (3 hours) but at lower a lower temperature of 950 ºC. The spray coating technique allowed the film to dry on a hot plate reducing the overall oven heating time from 16 hours (powder) to 3 hours (thin film).NIR radiation was successfully employed to synthesise NASICON as a thin film, a novel technique that has not previously been used in this field. This significantly reduced sintering times to 60 seconds, and overall oven/NIR heating times to 2 hours 2 minutes. E-Thesis Swansea University, Wales, UK Energy Storage, Sodium-ion, Battery, Solid-state, Electrolyte 21 5 2025 2025-05-21 10.23889/SUThesis.69884 A selection of content is redacted or is partially redacted from this thesis to protect sensitive and personal information. COLLEGE NANME COLLEGE CODE Swansea University Baker, J. Doctoral Ph.D M2A M2A 2025-07-03T14:45:33.9578579 2025-07-03T14:13:48.9718141 Faculty of Science and Engineering School of Engineering and Applied Sciences - Materials Science and Engineering REBECCA GRIFFIN 1 69884__34667__6ef79a7df56c4bd9af6641789bc2a3de.pdf 2024_Griffin_R.final.69884.pdf 2025-07-03T14:37:02.8101152 Output 12195089 application/pdf E-Thesis – open access true Copyright: The author, Rebecca Griffin, 2024 true eng
title Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries
spellingShingle Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries
REBECCA GRIFFIN
title_short Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries
title_full Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries
title_fullStr Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries
title_full_unstemmed Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries
title_sort Synthesis of Solid-state NASICON Electrolytes for Sodium-ion Batteries
author_id_str_mv d53a2269bf0c8beec668ccb9c3499f73
author_id_fullname_str_mv d53a2269bf0c8beec668ccb9c3499f73_***_REBECCA GRIFFIN
author REBECCA GRIFFIN
author2 REBECCA GRIFFIN
format E-Thesis
publishDate 2025
institution Swansea University
doi_str_mv 10.23889/SUThesis.69884
college_str Faculty of Science and Engineering
hierarchytype
hierarchy_top_id facultyofscienceandengineering
hierarchy_top_title Faculty of Science and Engineering
hierarchy_parent_id facultyofscienceandengineering
hierarchy_parent_title Faculty of Science and Engineering
department_str School of Engineering and Applied Sciences - Materials Science and Engineering{{{_:::_}}}Faculty of Science and Engineering{{{_:::_}}}School of Engineering and Applied Sciences - Materials Science and Engineering
document_store_str 1
active_str 0
description This thesis aims to synthesise the sodium super ionic conductor (NASICON) solid-state electrolyte for sodium-ion battery applications using two methodologies: solid-state and sol synthesis. The objective is to develop NASICON with enhanced chemical properties and minimised secondary phases by employing less energy-intensive techniques. This involves transitioning from conventional oven heating to near-infrared (NIR) radiation sintering, achieved through the fabrication of NASICON as a thin film. All samples were characterised by x-ray diffraction (XRD) and scanning electron microscopy (SEM).NASICON was successfully synthesised using the solid-state technique, forming dense pellets (density: 2.80 g/cm3) that are 15 mm in diameter and 2 mm thick (±0.05 mm). The final sintering step was conducted in a tube furnace in an inert environment (argon) at 1180 ºC for 16 hours, with the total oven time for the process being 70 hours and only 1.5% weight fraction secondary phase of ZrO2. Alumina crucibles and a powder bed were used to prevent the pellet fusing to the crucible (Al3+ diffusion) and reduce sodium volatilisation.The sol method also successfully formed a NASICON powder with a low secondary phase content of <2%, aligned with literature values. The powder was prepared in a conventional oven (in air) with reduced sintering times of 3 hours and temperatures of 1000 ºC. Additionally, NASICON was synthesised as a dense 10 µm thin film on a quartz substrate, utilising a sol spray coating technique. The same sintering times were employed as the powder (3 hours) but at lower a lower temperature of 950 ºC. The spray coating technique allowed the film to dry on a hot plate reducing the overall oven heating time from 16 hours (powder) to 3 hours (thin film).NIR radiation was successfully employed to synthesise NASICON as a thin film, a novel technique that has not previously been used in this field. This significantly reduced sintering times to 60 seconds, and overall oven/NIR heating times to 2 hours 2 minutes.
published_date 2025-05-21T05:28:09Z
_version_ 1851369653888090112
score 11.089572

Similar Items