作为电解质的 LiBOB 材料的合成与表征

Agus Purwanto, Annisa Salsabila Ghina Muthi, Ardian Febrianto, Muhammad Nur Ikhsanuddin
{"title":"作为电解质的 LiBOB 材料的合成与表征","authors":"Agus Purwanto, Annisa Salsabila Ghina Muthi, Ardian Febrianto, Muhammad Nur Ikhsanuddin","doi":"10.20961/esta.v3i1.73900","DOIUrl":null,"url":null,"abstract":"<span lang=\"EN-US\">Inside battery, the electrolyte becomes a very important electrochemical device. The electrolyte functions as a transfer medium for Li ions in the battery. One of the salts that can cover the deficiency of LiPF<sub>6</sub> as an electrolyte material that is currently widely used is LiBOB ( Lithium BisBorate ) salt material. Lithium bis (oxalato) borate material is a new lithium salt which was first introduced in 1999 by Xu et al </span><!--[if supportFields]><span lang=EN-US \nstyle='font-size:11.0pt;font-family:\"Arial\",sans-serif;mso-fareast-font-family: \nArial;color:black;mso-ansi-language:EN-US;mso-fareast-language:JA;mso-bidi-language: \nAR-SA'><span style='mso-element:field-begin;mso-field-lock:yes'></span>ADDIN \nCSL_CITATION \n{\"citationItems\":[{\"id\":\"ITEM-1\",\"itemData\":{\"DOI\":\"10.1149/1.1347858\",\"ISSN\":\"10990062\",\"author\":[{\"dropping-particle\":\"\",\"family\":\"Xu\",\"given\":\"W.\",\"non-dropping-particle\":\"\",\"parse-names\":false,\"suffix\":\"\"},{\"dropping-particle\":\"\",\"family\":\"Angell\",\"given\":\"C. \nA.\",\"non-dropping-particle\":\"\",\"parse-names\":false,\"suffix\":\"\"}],\"container-title\":\"Electrochemical \nand Solid-State \nLetters\",\"id\":\"ITEM-1\",\"issue\":\"3\",\"issued\":{\"date-parts\":[[\"2001\"]]},\"page\":\"6-7\",\"title\":\"Erratum: \nLiBOB and its derivatives weakly coordinating anions, and the exceptional \nconductivity of their nonaqueous solutions (Electrochem. Solid-State Lett. \n(2001) 4 (E1))\",\"type\":\"article-journal\",\"volume\":\"4\"},\"uris\":[\"http://www.mendeley.com/documents/?uuid=cf5811f8-a169-4d4b-9f92-102e6172a35a\"]}],\"mendeley\":{\"formattedCitation\":\"[4]\",\"plainTextFormattedCitation\":\"[4]\",\"previouslyFormattedCitation\":\"[4]\"},\"properties\":{\"noteIndex\":0},\"schema\":\"https://github.com/citation-style-language/schema/raw/master/csl-citation.json\"}<span \nstyle='mso-element:field-separator'></span></span><![endif]--><span lang=\"EN-US\">[4]</span><!--[if supportFields]><span \nlang=EN-US style='font-size:11.0pt;font-family:\"Arial\",sans-serif;mso-fareast-font-family: \nArial;color:black;mso-ansi-language:EN-US;mso-fareast-language:JA;mso-bidi-language: \nAR-SA'><span style='mso-element:field-end'></span></span><![endif]--><span lang=\"EN-US\">, which is currently being developed as a replacement electrolyte for lithium ion batteries. LiBOB is a promising electrolyte material regarding battery safety since judging from the potential for excess salt supported by previous research, LiBOB can be the answer to the problem of using electrolytes that are not environmentally friendly. The synthesis of LiBOB refers to Wigayati (2018) </span><!--[if supportFields]><span lang=EN-US \nstyle='font-size:11.0pt;font-family:\"Arial\",sans-serif;mso-fareast-font-family: \nArial;color:black;mso-ansi-language:EN-US;mso-fareast-language:JA;mso-bidi-language: \nAR-SA'><span style='mso-element:field-begin;mso-field-lock:yes'></span>ADDIN \nCSL_CITATION {\"citationItems\":[{\"id\":\"ITEM-1\",\"itemData\":{\"DOI\":\"10.22146/ijc.21191\",\"ISBN\":\"6221756057\",\"ISSN\":\"24601578\",\"abstract\":\"Lithium \nbis (oxalate) borate or LiBOB is an active material used as the electrolyte for \nlithium battery application. LiBOB (LiB(C2O4)2) powder was prepared from LiOH, \nH2C2O4 and H3BO3. The employed method was solid state reaction. LiBOB powder \nproduced from the reaction was then observed using SEM and TEM. Surface area \nwas analyzed using Quantachrome Nova 4200e. From the analysis analyzed using \nXRD to identify the resulting phases, crystal structure, and crystallite size. \nThe functional groups were analyzed using FT-IR. The particle morphology was \nresult, it was seen that the resulted phases were C4LiBO8 and LiB(C2O4)2.H2O, \nthe crystal structure was orthorhombic with space group Pbca and Pnma. From the \nparticle morphology observation it was shown that micro pores were created \nirregularly. When the observation was deepened, nanopores with elongated round \nshape were seen within the micropores. The pore size was approximately 50–100 \nnm. The surface area, total pore volume, and average pore diameter of LiBOB \npowder was 88.556 m2/g, 0.4252 cm3/g, and 19.2 nm \nrespectively.\",\"author\":[{\"dropping-particle\":\"\",\"family\":\"Wigayati\",\"given\":\"Etty \nMarti\",\"non-dropping-particle\":\"\",\"parse-names\":false,\"suffix\":\"\"},{\"dropping-particle\":\"\",\"family\":\"Ratri\",\"given\":\"Christin \nRina\",\"non-dropping-particle\":\"\",\"parse-names\":false,\"suffix\":\"\"},{\"dropping-particle\":\"\",\"family\":\"Purawiardi\",\"given\":\"Ibrahim\",\"non-dropping-particle\":\"\",\"parse-names\":false,\"suffix\":\"\"},{\"dropping-particle\":\"\",\"family\":\"Rohman\",\"given\":\"Fadli\",\"non-dropping-particle\":\"\",\"parse-names\":false,\"suffix\":\"\"},{\"dropping-particle\":\"\",\"family\":\"Lestariningsih\",\"given\":\"Titik\",\"non-dropping-particle\":\"\",\"parse-names\":false,\"suffix\":\"\"}],\"container-title\":\"Indonesian \nJournal of \nChemistry\",\"id\":\"ITEM-1\",\"issue\":\"3\",\"issued\":{\"date-parts\":[[\"2015\"]]},\"page\":\"242-247\",\"title\":\"Microstructure \nanalysis of synthesized \nlibob\",\"type\":\"article-journal\",\"volume\":\"15\"},\"uris\":[\"http://www.mendeley.com/documents/?uuid=defc294a-2d90-4d35-b556-2832326dcd4e\"]}],\"mendeley\":{\"formattedCitation\":\"[2]\",\"plainTextFormattedCitation\":\"[2]\",\"previouslyFormattedCitation\":\"[2]\"},\"properties\":{\"noteIndex\":0},\"schema\":\"https://github.com/citation-style-language/schema/raw/master/csl-citation.json\"}<span \nstyle='mso-element:field-separator'></span></span><![endif]--><span lang=\"EN-US\">[2]</span><!--[if supportFields]><span \nlang=EN-US style='font-size:11.0pt;font-family:\"Arial\",sans-serif;mso-fareast-font-family: \nArial;color:black;mso-ansi-language:EN-US;mso-fareast-language:JA;mso-bidi-language: \nAR-SA'><span style='mso-element:field-end'></span></span><![endif]--><span lang=\"EN-US\"> which was modified by replacing the LiOH material with Li<sub>2</sub>CO<sub>3</sub>. The ingredients lithium carbonate, boric acid and oxalic acid were prepared first with weigh and mix based on molar ratio 1 : 2 : 5. The synthesis was carried out by the solid state reaction method. Crystals were characterized by FTIR, SEM-EDX, XRD and AAS. From the results of the SEM test, it was found that the LiBOB particles had spherical and cylindrical shapes, and there were Na impurities due to the raw material H<sub>3</sub>BO<sub>3</sub>. In the XRD test it was found that the LiBOB hydrate phase matched at 2-theta 23.7641°, 20.1454° and 19.438°. As well as the LiBOB phase matched at 2-theta 19.438°, 23.4669° and 27.1796°. The FTIR test results found the same wave as the Wigayati reference chart. In the AAS test, it was found that Na and Li metals were contained in the synthesis sample.</span>","PeriodicalId":11676,"journal":{"name":"Energy Storage Technology and Applications","volume":"48 8","pages":""},"PeriodicalIF":0.0000,"publicationDate":"2024-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Synthesis and Characterization of LiBOB Material as An Electrolyte\",\"authors\":\"Agus Purwanto, Annisa Salsabila Ghina Muthi, Ardian Febrianto, Muhammad Nur Ikhsanuddin\",\"doi\":\"10.20961/esta.v3i1.73900\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<span lang=\\\"EN-US\\\">Inside battery, the electrolyte becomes a very important electrochemical device. The electrolyte functions as a transfer medium for Li ions in the battery. 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Solid-State Lett. \\n(2001) 4 (E1))\\\",\\\"type\\\":\\\"article-journal\\\",\\\"volume\\\":\\\"4\\\"},\\\"uris\\\":[\\\"http://www.mendeley.com/documents/?uuid=cf5811f8-a169-4d4b-9f92-102e6172a35a\\\"]}],\\\"mendeley\\\":{\\\"formattedCitation\\\":\\\"[4]\\\",\\\"plainTextFormattedCitation\\\":\\\"[4]\\\",\\\"previouslyFormattedCitation\\\":\\\"[4]\\\"},\\\"properties\\\":{\\\"noteIndex\\\":0},\\\"schema\\\":\\\"https://github.com/citation-style-language/schema/raw/master/csl-citation.json\\\"}<span \\nstyle='mso-element:field-separator'></span></span><![endif]--><span lang=\\\"EN-US\\\">[4]</span><!--[if supportFields]><span \\nlang=EN-US style='font-size:11.0pt;font-family:\\\"Arial\\\",sans-serif;mso-fareast-font-family: \\nArial;color:black;mso-ansi-language:EN-US;mso-fareast-language:JA;mso-bidi-language: \\nAR-SA'><span style='mso-element:field-end'></span></span><![endif]--><span lang=\\\"EN-US\\\">, which is currently being developed as a replacement electrolyte for lithium ion batteries. LiBOB is a promising electrolyte material regarding battery safety since judging from the potential for excess salt supported by previous research, LiBOB can be the answer to the problem of using electrolytes that are not environmentally friendly. The synthesis of LiBOB refers to Wigayati (2018) </span><!--[if supportFields]><span lang=EN-US \\nstyle='font-size:11.0pt;font-family:\\\"Arial\\\",sans-serif;mso-fareast-font-family: \\nArial;color:black;mso-ansi-language:EN-US;mso-fareast-language:JA;mso-bidi-language: \\nAR-SA'><span style='mso-element:field-begin;mso-field-lock:yes'></span>ADDIN \\nCSL_CITATION {\\\"citationItems\\\":[{\\\"id\\\":\\\"ITEM-1\\\",\\\"itemData\\\":{\\\"DOI\\\":\\\"10.22146/ijc.21191\\\",\\\"ISBN\\\":\\\"6221756057\\\",\\\"ISSN\\\":\\\"24601578\\\",\\\"abstract\\\":\\\"Lithium \\nbis (oxalate) borate or LiBOB is an active material used as the electrolyte for \\nlithium battery application. LiBOB (LiB(C2O4)2) powder was prepared from LiOH, \\nH2C2O4 and H3BO3. The employed method was solid state reaction. LiBOB powder \\nproduced from the reaction was then observed using SEM and TEM. Surface area \\nwas analyzed using Quantachrome Nova 4200e. From the analysis analyzed using \\nXRD to identify the resulting phases, crystal structure, and crystallite size. \\nThe functional groups were analyzed using FT-IR. The particle morphology was \\nresult, it was seen that the resulted phases were C4LiBO8 and LiB(C2O4)2.H2O, \\nthe crystal structure was orthorhombic with space group Pbca and Pnma. From the \\nparticle morphology observation it was shown that micro pores were created \\nirregularly. When the observation was deepened, nanopores with elongated round \\nshape were seen within the micropores. The pore size was approximately 50–100 \\nnm. The surface area, total pore volume, and average pore diameter of LiBOB \\npowder was 88.556 m2/g, 0.4252 cm3/g, and 19.2 nm \\nrespectively.\\\",\\\"author\\\":[{\\\"dropping-particle\\\":\\\"\\\",\\\"family\\\":\\\"Wigayati\\\",\\\"given\\\":\\\"Etty \\nMarti\\\",\\\"non-dropping-particle\\\":\\\"\\\",\\\"parse-names\\\":false,\\\"suffix\\\":\\\"\\\"},{\\\"dropping-particle\\\":\\\"\\\",\\\"family\\\":\\\"Ratri\\\",\\\"given\\\":\\\"Christin \\nRina\\\",\\\"non-dropping-particle\\\":\\\"\\\",\\\"parse-names\\\":false,\\\"suffix\\\":\\\"\\\"},{\\\"dropping-particle\\\":\\\"\\\",\\\"family\\\":\\\"Purawiardi\\\",\\\"given\\\":\\\"Ibrahim\\\",\\\"non-dropping-particle\\\":\\\"\\\",\\\"parse-names\\\":false,\\\"suffix\\\":\\\"\\\"},{\\\"dropping-particle\\\":\\\"\\\",\\\"family\\\":\\\"Rohman\\\",\\\"given\\\":\\\"Fadli\\\",\\\"non-dropping-particle\\\":\\\"\\\",\\\"parse-names\\\":false,\\\"suffix\\\":\\\"\\\"},{\\\"dropping-particle\\\":\\\"\\\",\\\"family\\\":\\\"Lestariningsih\\\",\\\"given\\\":\\\"Titik\\\",\\\"non-dropping-particle\\\":\\\"\\\",\\\"parse-names\\\":false,\\\"suffix\\\":\\\"\\\"}],\\\"container-title\\\":\\\"Indonesian \\nJournal of \\nChemistry\\\",\\\"id\\\":\\\"ITEM-1\\\",\\\"issue\\\":\\\"3\\\",\\\"issued\\\":{\\\"date-parts\\\":[[\\\"2015\\\"]]},\\\"page\\\":\\\"242-247\\\",\\\"title\\\":\\\"Microstructure \\nanalysis of synthesized \\nlibob\\\",\\\"type\\\":\\\"article-journal\\\",\\\"volume\\\":\\\"15\\\"},\\\"uris\\\":[\\\"http://www.mendeley.com/documents/?uuid=defc294a-2d90-4d35-b556-2832326dcd4e\\\"]}],\\\"mendeley\\\":{\\\"formattedCitation\\\":\\\"[2]\\\",\\\"plainTextFormattedCitation\\\":\\\"[2]\\\",\\\"previouslyFormattedCitation\\\":\\\"[2]\\\"},\\\"properties\\\":{\\\"noteIndex\\\":0},\\\"schema\\\":\\\"https://github.com/citation-style-language/schema/raw/master/csl-citation.json\\\"}<span \\nstyle='mso-element:field-separator'></span></span><![endif]--><span lang=\\\"EN-US\\\">[2]</span><!--[if supportFields]><span \\nlang=EN-US style='font-size:11.0pt;font-family:\\\"Arial\\\",sans-serif;mso-fareast-font-family: \\nArial;color:black;mso-ansi-language:EN-US;mso-fareast-language:JA;mso-bidi-language: \\nAR-SA'><span style='mso-element:field-end'></span></span><![endif]--><span lang=\\\"EN-US\\\"> which was modified by replacing the LiOH material with Li<sub>2</sub>CO<sub>3</sub>. 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引用次数: 0

摘要

在 AAS 测试中发现,合成样品中含有 Na 和 Li 金属。
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Synthesis and Characterization of LiBOB Material as An Electrolyte
Inside battery, the electrolyte becomes a very important electrochemical device. The electrolyte functions as a transfer medium for Li ions in the battery. One of the salts that can cover the deficiency of LiPF6 as an electrolyte material that is currently widely used is LiBOB ( Lithium BisBorate ) salt material. Lithium bis (oxalato) borate material is a new lithium salt which was first introduced in 1999 by Xu et al [4], which is currently being developed as a replacement electrolyte for lithium ion batteries. LiBOB is a promising electrolyte material regarding battery safety since judging from the potential for excess salt supported by previous research, LiBOB can be the answer to the problem of using electrolytes that are not environmentally friendly. The synthesis of LiBOB refers to Wigayati (2018) [2] which was modified by replacing the LiOH material with Li2CO3. The ingredients lithium carbonate, boric acid and oxalic acid were prepared first with weigh and mix based on molar ratio 1 : 2 : 5. The synthesis was carried out by the solid state reaction method. Crystals were characterized by FTIR, SEM-EDX, XRD and AAS. From the results of the SEM test, it was found that the LiBOB particles had spherical and cylindrical shapes, and there were Na impurities due to the raw material H3BO3. In the XRD test it was found that the LiBOB hydrate phase matched at 2-theta 23.7641°, 20.1454° and 19.438°. As well as the LiBOB phase matched at 2-theta 19.438°, 23.4669° and 27.1796°. The FTIR test results found the same wave as the Wigayati reference chart. In the AAS test, it was found that Na and Li metals were contained in the synthesis sample.
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