{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,3,18]],"date-time":"2026-03-18T00:58:40Z","timestamp":1773795520453,"version":"3.50.1"},"reference-count":46,"publisher":"MDPI AG","issue":"11","license":[{"start":{"date-parts":[[2025,5,28]],"date-time":"2025-05-28T00:00:00Z","timestamp":1748390400000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"name":"Science Committee of the Ministry of Science and Higher Education of the Republic of Kazakhstan","award":["AP19677333"],"award-info":[{"award-number":["AP19677333"]}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Nanomaterials"],"abstract":"<jats:p>In this study, we report the synthesis of few-layer graphene via ultrasonic treatment of a graphite-benzene solution at room temperature. Raman spectroscopy revealed a significant reduction in the intensity ratio of the G and 2D peaks for samples subjected to 20 min of treatment, indicating a decrease in defect density and oxidation. Prolonged treatment times led to fragmentation of the graphene sheets, which facilitated restacking, as evidenced by Raman spectroscopy and microscopy. FTIR analysis confirmed the complete removal of the solvent from the extracted and dried graphene. Additionally, electron paramagnetic resonance (EPR) measurements indicated the presence of carbon-based magnetism in the synthesized samples, suggesting potential applications in spintronic devices. Our findings highlight the effectiveness of ultrasonic treatment for producing high-quality few-layer graphene with desirable structural and magnetic properties.<\/jats:p>","DOI":"10.3390\/nano15110817","type":"journal-article","created":{"date-parts":[[2025,5,29]],"date-time":"2025-05-29T04:46:38Z","timestamp":1748493998000},"page":"817","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["An Approach to the Improvement of Graphene Production by Ultrasonic-Bath Treatment"],"prefix":"10.3390","volume":"15","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-3728-2430","authenticated-orcid":false,"given":"Bagila A.","family":"Baitimbetova","sequence":"first","affiliation":[{"name":"Department of Materials Science, Nanotechnology and Engineering Physics, Satbayev University, Satbayeva Str. 22, Almaty 050013, Kazakhstan"},{"name":"Center for Two-Dimensional and Layered Materials, Pennsylvania State University, University Park, PA 16802, USA"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2286-3443","authenticated-orcid":false,"given":"Danil W.","family":"Boukhvalov","sequence":"additional","affiliation":[{"name":"Institute of Physics and Technology LLP, Satbayev University, Ibragimova Str. 11, Almaty 050032, Kazakhstan"},{"name":"College of Science, Institute of Materials Physics and Chemistry, Nanjing Forestry University, Nanjing 210037, China"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Kostya A.","family":"Mit\u2019","sequence":"additional","affiliation":[{"name":"Institute of Physics and Technology LLP, Satbayev University, Ibragimova Str. 11, Almaty 050032, Kazakhstan"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8929-5519","authenticated-orcid":false,"given":"Tleuzhan S.","family":"Turmagambetov","sequence":"additional","affiliation":[{"name":"Center Consulting, Tlendieva Str. 258b, Almaty 050060, Kazakhstan"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Perizat","family":"Baitimbetova","sequence":"additional","affiliation":[{"name":"Science and Innovation Park Abai Lab, Abai Kazakh National Pedagogical University, Dostyk Ave. 13, Almaty 050010, Kazakhstan"}],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"Abay S.","family":"Serikkanov","sequence":"additional","affiliation":[{"name":"Institute of Physics and Technology LLP, Satbayev University, Ibragimova Str. 11, Almaty 050032, Kazakhstan"},{"name":"National Academy of Sciences of the Republic of Kazakhstan under the President of the Republic of Kazakhstan, Shevchenko Str. 28, Almaty 050010, Kazakhstan"}],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"1968","published-online":{"date-parts":[[2025,5,28]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"1803784","DOI":"10.1002\/adma.201803784","article-title":"The Worldwide Graphene Flake Production","volume":"30","author":"Kauling","year":"2018","journal-title":"Adv. Mater."},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"502","DOI":"10.1038\/d41586-018-06939-4","article-title":"The war on fake graphene","volume":"562","year":"2018","journal-title":"Nature"},{"key":"ref_3","doi-asserted-by":"crossref","first-page":"381","DOI":"10.1039\/C3CS60217F","article-title":"Graphene via sonication assisted liquid-phase exfoliation","volume":"43","author":"Ciesielski","year":"2014","journal-title":"Chem. Soc. Rev."},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"282","DOI":"10.1038\/nature04969","article-title":"Graphene-based composite materials","volume":"442","author":"Stankovich","year":"2006","journal-title":"Nature"},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"155","DOI":"10.1039\/B512799H","article-title":"Stable aqueous dispersions of graphitic nanoplatelets via the reduction of exfoliated graphite oxide in the presence of poly(sodium 4-styrenesulfonate)","volume":"16","author":"Stankovich","year":"2006","journal-title":"J. Mater. Chem."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"864","DOI":"10.1002\/smll.200902066","article-title":"High-Concentration Solvent Exfoliation of Graphene","volume":"6","author":"Khan","year":"2010","journal-title":"Small"},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"105989","DOI":"10.1016\/j.ultras.2019.105989","article-title":"Optimizing graphene production in ultrasonic devices. Optimizing graphene production in ultrasonic devices","volume":"100","author":"Silva","year":"2020","journal-title":"Ultrasonics"},{"key":"ref_8","doi-asserted-by":"crossref","unstructured":"Han, J.T., Jang, J.I., Kim, H., Hwang, J.Y., Yoo, H.K., Woo, J.S., Choi, S., Kim, H.Y., Jeong, H.J., and Jeong, S.Y. (2014). Extremely Efficient Liquid Exfoliation and Dispersion of Layered Materials by Unusual Acoustic Cavitation. Sci. Rep., 4.","DOI":"10.1038\/srep05133"},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"563","DOI":"10.1038\/nnano.2008.215","article-title":"High-yield production of graphene by liquid-phase exfoliation of graphite","volume":"3","author":"Hernandez","year":"2008","journal-title":"Nat. Nanotechnol."},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"478","DOI":"10.1016\/j.ultsonch.2017.05.019","article-title":"State of the art and recent advances in the ultrasound-assisted synthesis, exfoliation and functionalization of graphene derivatives","volume":"39","author":"Muthoosamy","year":"2017","journal-title":"Ultrason. Sonochem."},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"20","DOI":"10.1016\/j.msea.2017.04.009","article-title":"Strengthening mechanism in graphene nanoplatelets reinforced aluminum composite fabricated through spark plasma sintering","volume":"695","author":"Bisht","year":"2017","journal-title":"Mater. Sci. Eng. A"},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"415","DOI":"10.1007\/s12666-015-0780-9","article-title":"Fatigue and Wear Behavior of Al6061\u2013Graphene Composites Synthesized by Powder Metallurgy","volume":"69","author":"Kumar","year":"2016","journal-title":"Trans. Indian Inst. Met."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"133","DOI":"10.1016\/j.ultsonch.2018.03.007","article-title":"Investigation of tip sonication effects on structural quality of graphene nanoplatelets (GNPs) for superior solvent dispersion","volume":"45","author":"Baig","year":"2018","journal-title":"Ultrason. Sonochem."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"104630","DOI":"10.1016\/j.ultsonch.2019.104630","article-title":"Method of ultrasound-assisted liquid-phase exfoliation to prepare graphene","volume":"58","author":"Gu","year":"2019","journal-title":"Ultrason. Sonochem."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"217","DOI":"10.1038\/nnano.2009.58","article-title":"Chemical methods for the production of graphenes","volume":"4","author":"Park","year":"2009","journal-title":"Nat. Nanotechnol."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"24992","DOI":"10.1039\/c2jm34517j","article-title":"Methods of graphite exfoliation","volume":"22","author":"Cai","year":"2012","journal-title":"J. Mater. Chem."},{"key":"ref_17","doi-asserted-by":"crossref","first-page":"624","DOI":"10.1038\/nmat3944","article-title":"Scalable production of large quantities of defect-free few-layer graphene by shear exfoliation in liquids","volume":"13","author":"Paton","year":"2014","journal-title":"Nat. Mater."},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"545546","DOI":"10.1038\/nmat3961","article-title":"Layered materials: Scaling up exfoliation","volume":"13","author":"Tour","year":"2014","journal-title":"Nat. Mater."},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"737","DOI":"10.1016\/j.carbon.2020.06.029","article-title":"Ultrasonic exfoliation of graphene in water: A key parameter study","volume":"168","author":"Tyurnina","year":"2020","journal-title":"Carbon"},{"key":"ref_20","doi-asserted-by":"crossref","unstructured":"Polverino, S., Castillo, A.E.D.R., Brencich, A., Marasco, L., Bonaccorso, F., and Morbiducci, R. (2022). Few-Layers Graphene-Based Cement Mortars: Production Process and Mechanical Properties. Sustainability, 14.","DOI":"10.3390\/su14020784"},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"42","DOI":"10.1016\/j.compositesa.2015.08.001","article-title":"Deformation behavior of aluminum alloy matrix composites reinforced with few-layer graphene","volume":"78","author":"Shin","year":"2015","journal-title":"Comp. Part A"},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"9","DOI":"10.1080\/00387010701799589","article-title":"The study by spectroscopy method of carbon nanostructure in carbonized ferrochromic spinel","volume":"41","author":"Baitimbetova","year":"2008","journal-title":"Spectrosc. Lett."},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"81266","DOI":"10.1039\/C5RA15607F","article-title":"Few- and multi-layer graphene on carbon fibers: Synthesis and application","volume":"5","author":"Ghaemi","year":"2015","journal-title":"RSC Adv."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"655","DOI":"10.1016\/j.carbon.2021.06.041","article-title":"Lightweight, few-layer graphene composites with improved electro-thermal properties as efficient heating devices for de-icing applications","volume":"182","author":"Ba","year":"2021","journal-title":"Carbon"},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"942","DOI":"10.3390\/nano8110942","article-title":"Liquid-phase exfoliation of graphene: An overview on exfoliation media, techniques, and challenges","volume":"8","author":"Xu","year":"2018","journal-title":"Nanomaterials"},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"4031","DOI":"10.1021\/nl902200b","article-title":"Solution Phase Production of Graphene with Controlled Thickness via Density Differentiation","volume":"9","author":"Green","year":"2009","journal-title":"Nano Lett."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"4428","DOI":"10.1039\/c3cp43205j","article-title":"Critical parameters in exfoliating graphite into graphene","volume":"15","author":"Buzaglo","year":"2013","journal-title":"Phys. Chem. Chem. Phys."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"127","DOI":"10.31489\/2022ph2\/127-132","article-title":"The study of carbon nanomaterials by IR-Fourier spectroscopy, obtained by the action of an ultrasonic field on graphite","volume":"2","author":"Baitimbetova","year":"2022","journal-title":"Bull. Karaganda Univ. Phys. Ser."},{"key":"ref_29","doi-asserted-by":"crossref","unstructured":"Baitimbetova, B.A., Ryabikin, Y.A., Rakymetov, B.A., Murzalinov, D.O., Kantarbaeva, D.O., Duamet, B., Dmitriyeva, E.A., Serikkanov, A.S., and Yelemessov, K. (2023). Paramagnetic Properties of Carbon Films. Coatings, 13.","DOI":"10.20944\/preprints202306.1957.v1"},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"209","DOI":"10.1007\/s11182-021-02318-1","article-title":"Study of paramagnetic properties of graphene structures obtained from pure graphite in organic reagents exposed to ultrasound","volume":"64","author":"Baytimbetova","year":"2021","journal-title":"Russ Phys. J."},{"key":"ref_31","doi-asserted-by":"crossref","unstructured":"Di Berardino, C., B\u00e9lteky, P., Schmitz, F., Lamberti, F., Menna, E., Kukovecz, A., and Gatti, T. (2020). Controlled Size Reduction of Liquid Exfoliated Graphene Micro-Sheets via Tip Sonication. Crystals, 10.","DOI":"10.3390\/cryst10111049"},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"51","DOI":"10.1016\/j.physrep.2009.02.003","article-title":"Raman spectroscopy in graphene","volume":"473","author":"Malard","year":"2009","journal-title":"Phys. Rep."},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"47","DOI":"10.1016\/j.ssc.2007.03.052","article-title":"Raman spectroscopy of graphene and graphite: Disorder, electron-phonon coupling, doping and nonadiabatic effects","volume":"143","author":"Ferrari","year":"2007","journal-title":"Solid State Comm."},{"key":"ref_34","doi-asserted-by":"crossref","unstructured":"Scardaci, V., and Compagnini, G. (2021). Raman Spectroscopy Investigation of Graphene Oxide Reduction by Laser Scribing. C, 7.","DOI":"10.3390\/c7020048"},{"key":"ref_35","first-page":"01610","article-title":"Effect of He ion irradiation on microstructure and electrical properties of graphene","volume":"69","author":"Zhang","year":"2020","journal-title":"Acta Phys. Sin."},{"key":"ref_36","unstructured":"Di Bartolo, B. (1968). Optical Interactions in Solids, Wiley."},{"key":"ref_37","doi-asserted-by":"crossref","unstructured":"Aliyev, E., Filiz, V., Khan, M.M., Lee, Y.J., Abetz, C., and Abetz, V. (2019). Structural Characterization of Graphene Oxide: Surface Functional Groups and Fractionated Oxidative Debris. Nanomaterial, 9.","DOI":"10.3390\/nano9081180"},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"6033","DOI":"10.1038\/s41467-021-26157-3","article-title":"Biomimetic CO oxidation below \u2212100 \u00b0C by a nitrate-containing metal-free microporous system","volume":"12","author":"Khivantsev","year":"2021","journal-title":"Nat. Commun."},{"key":"ref_39","doi-asserted-by":"crossref","first-page":"692","DOI":"10.1016\/j.snb.2013.12.017","article-title":"A practical carbon dioxide gas sensor using room-temperature hydrogen plasma reduced graphene oxide","volume":"193","author":"Hafiz","year":"2014","journal-title":"Sens. Actuators B Chem."},{"key":"ref_40","doi-asserted-by":"crossref","first-page":"11966","DOI":"10.1039\/C4RA14511A","article-title":"Mechanism of a green graphene oxide reduction with reusable potassium carbonate","volume":"5","author":"He","year":"2015","journal-title":"RSC Adv."},{"key":"ref_41","doi-asserted-by":"crossref","first-page":"225","DOI":"10.1016\/j.carbon.2013.07.055","article-title":"An improved Hummers method for eco-friendly synthesis of graphene oxide","volume":"64","author":"Chen","year":"2013","journal-title":"Carbon"},{"key":"ref_42","doi-asserted-by":"crossref","first-page":"047209","DOI":"10.1103\/PhysRevLett.100.047209","article-title":"Magnetic Correlations at Graphene Edges: Basis for Novel Spintronics Devices","volume":"100","author":"Yazyev","year":"2008","journal-title":"Phys. Rev. Lett."},{"key":"ref_43","doi-asserted-by":"crossref","first-page":"800","DOI":"10.1016\/j.carbon.2016.06.020","article-title":"Charge transfer and weak bonding between molecular oxygen and graphene zigzag edges at low temperatures","volume":"107","author":"Boukhvalov","year":"2016","journal-title":"Carbon"},{"key":"ref_44","doi-asserted-by":"crossref","first-page":"1225","DOI":"10.1016\/j.carbon.2005.10.047","article-title":"Magnetic and high resolution TEM studies of nanographite derived from nanodiamond","volume":"44","author":"Osipov","year":"2006","journal-title":"Carbon"},{"key":"ref_45","doi-asserted-by":"crossref","first-page":"11209","DOI":"10.1103\/PhysRevB.62.11209","article-title":"Structure and electronic properties of graphite nanoparticles","volume":"62","author":"Prasad","year":"1998","journal-title":"Phys. Rev. B"},{"key":"ref_46","first-page":"3283","article-title":"Spectroscopic investigation of thermal treatment of doped polypyrrole","volume":"14","author":"Altchuler","year":"2000","journal-title":"Phys. Chem."}],"container-title":["Nanomaterials"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/2079-4991\/15\/11\/817\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,9]],"date-time":"2025-10-09T17:42:29Z","timestamp":1760031749000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/2079-4991\/15\/11\/817"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2025,5,28]]},"references-count":46,"journal-issue":{"issue":"11","published-online":{"date-parts":[[2025,6]]}},"alternative-id":["nano15110817"],"URL":"https:\/\/doi.org\/10.3390\/nano15110817","relation":{},"ISSN":["2079-4991"],"issn-type":[{"value":"2079-4991","type":"electronic"}],"subject":[],"published":{"date-parts":[[2025,5,28]]}}}