Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric Acid
In this work, graphite intercalation compounds (GICs) were synthesized using three different oxidizers: (NH<sub>4</sub>)<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, K<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, and CrO<sub&...
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MDPI AG
2022-03-01
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| Series: | Crystals |
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| Online Access: | https://www.mdpi.com/2073-4352/12/3/421 |
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| author | Gintare Rimkute Mantvydas Gudaitis Jurgis Barkauskas Aleksej Zarkov Gediminas Niaura Justina Gaidukevic |
| author_facet | Gintare Rimkute Mantvydas Gudaitis Jurgis Barkauskas Aleksej Zarkov Gediminas Niaura Justina Gaidukevic |
| author_sort | Gintare Rimkute |
| collection | DOAJ |
| description | In this work, graphite intercalation compounds (GICs) were synthesized using three different oxidizers: (NH<sub>4</sub>)<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, K<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, and CrO<sub>3</sub> with and without P<sub>2</sub>O<sub>5</sub> as a water-binding agent. Furthermore, the samples obtained were heat-treated at 800 °C. Specimens were characterized by optical microscopy, Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), and scanning electron microscopy (SEM). The correlation between different characteristic parameters of the Raman analysis has shown that the use of CrO<sub>3</sub> results in a much higher structural disorder compared to the products obtained using persulfate oxidizers. Narrowing the correlation set revealed that minimal defect concentration can be reached by using K<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, while the use of (NH<sub>4</sub>)<sub>2</sub>S<sub>2</sub>O<sub>8</sub> causes a slightly higher concentration of defects. It was also established that the additional use of P<sub>2</sub>O<sub>5</sub> can help to achieve more effective intercalation and has a positive effect on the formation of the stage I GIC phase. After heat treatment, the intercalated products mostly return to a graphite-like structure; however, the samples obtained with CrO<sub>3</sub> stand out with the most significant changes in their surface morphology. Therefore, analysis suggests that GICs obtained using persulfate oxidizers and P<sub>2</sub>O<sub>5</sub> could be a candidate to produce high-quality graphene or graphene oxide. |
| first_indexed | 2024-03-09T13:46:57Z |
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| issn | 2073-4352 |
| language | English |
| last_indexed | 2024-03-09T13:46:57Z |
| publishDate | 2022-03-01 |
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| series | Crystals |
| spelling | doaj.art-323ef9b78f164f1a83c13ab46ccdc5bc2023-11-30T20:58:01ZengMDPI AGCrystals2073-43522022-03-0112342110.3390/cryst12030421Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric AcidGintare Rimkute0Mantvydas Gudaitis1Jurgis Barkauskas2Aleksej Zarkov3Gediminas Niaura4Justina Gaidukevic5Institute of Chemistry, Faculty of Chemistry and Geosciences, Vilnius University, Naugarduko Str. 24, LT-03225 Vilnius, LithuaniaDepartment of Organic Chemistry, Center for Physical Sciences and Technology (FTMC), Saulėtekio Av. 3, LT-10257 Vilnius, LithuaniaInstitute of Chemistry, Faculty of Chemistry and Geosciences, Vilnius University, Naugarduko Str. 24, LT-03225 Vilnius, LithuaniaInstitute of Chemistry, Faculty of Chemistry and Geosciences, Vilnius University, Naugarduko Str. 24, LT-03225 Vilnius, LithuaniaDepartment of Organic Chemistry, Center for Physical Sciences and Technology (FTMC), Saulėtekio Av. 3, LT-10257 Vilnius, LithuaniaInstitute of Chemistry, Faculty of Chemistry and Geosciences, Vilnius University, Naugarduko Str. 24, LT-03225 Vilnius, LithuaniaIn this work, graphite intercalation compounds (GICs) were synthesized using three different oxidizers: (NH<sub>4</sub>)<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, K<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, and CrO<sub>3</sub> with and without P<sub>2</sub>O<sub>5</sub> as a water-binding agent. Furthermore, the samples obtained were heat-treated at 800 °C. Specimens were characterized by optical microscopy, Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), and scanning electron microscopy (SEM). The correlation between different characteristic parameters of the Raman analysis has shown that the use of CrO<sub>3</sub> results in a much higher structural disorder compared to the products obtained using persulfate oxidizers. Narrowing the correlation set revealed that minimal defect concentration can be reached by using K<sub>2</sub>S<sub>2</sub>O<sub>8</sub>, while the use of (NH<sub>4</sub>)<sub>2</sub>S<sub>2</sub>O<sub>8</sub> causes a slightly higher concentration of defects. It was also established that the additional use of P<sub>2</sub>O<sub>5</sub> can help to achieve more effective intercalation and has a positive effect on the formation of the stage I GIC phase. After heat treatment, the intercalated products mostly return to a graphite-like structure; however, the samples obtained with CrO<sub>3</sub> stand out with the most significant changes in their surface morphology. Therefore, analysis suggests that GICs obtained using persulfate oxidizers and P<sub>2</sub>O<sub>5</sub> could be a candidate to produce high-quality graphene or graphene oxide.https://www.mdpi.com/2073-4352/12/3/421graphite intercalation compoundsgraphite bisulfatestaging in graphite intercalation compoundsstructural characterizationthermal treatment |
| spellingShingle | Gintare Rimkute Mantvydas Gudaitis Jurgis Barkauskas Aleksej Zarkov Gediminas Niaura Justina Gaidukevic Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric Acid Crystals graphite intercalation compounds graphite bisulfate staging in graphite intercalation compounds structural characterization thermal treatment |
| title | Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric Acid |
| title_full | Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric Acid |
| title_fullStr | Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric Acid |
| title_full_unstemmed | Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric Acid |
| title_short | Synthesis and Characterization of Graphite Intercalation Compounds with Sulfuric Acid |
| title_sort | synthesis and characterization of graphite intercalation compounds with sulfuric acid |
| topic | graphite intercalation compounds graphite bisulfate staging in graphite intercalation compounds structural characterization thermal treatment |
| url | https://www.mdpi.com/2073-4352/12/3/421 |
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