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graphitization of tincone via molecular layer deposition: investigating sulfur's role and structural impacts

DALTON TRANSACTIONS 2025年第17期54卷 7095-7104页

作者： Jung, Hyolim Yang, Hae Lin Park, Gi-Beom Kim, Ji-Min Park, Jin-Seong Hanyang Univ Div Mat Sci & Engn 222 Wangsimni Ro Seoul 04763 South Korea Hanyang Univ Dept Informat Display Engn 222 Wangsimni Ro Seoul 04763 South Korea

This study investigated the synthesis of sp2 carbons using molecular layer deposition (MLD) with tincone, which utilized tetrakis(dimethylamido)tin (TDMASn) as the metal precursor and 4-mercaptophenol (4MP) as the organic linker. Tincone films were deposited at 100 degrees C without impurities and then subjected to vacuum post-annealing in a tube furnace to induce graphitization. Compositional and structural analyses revealed significant changes as the annealing temperature increased, including the breakdown of the bonds between Sn, O, S, and C. This process led to the reduction of Sn, O, and S and the formation of sp2 carbons. At 400 degrees C, the film thickness was reduced by 57.5%, and the refractive index increased from 1.8 to 1.97, as confirmed by the emergence of G-band and 2D-band peaks in the Raman spectra. X-ray photoelectron spectroscopy analysis indicated that the residual Sn content decreased to 0.75% at 600 degrees C. Interestingly, at temperatures above 400 degrees C, unique behavior was observed: increased C-S bonding disrupted the graphite structure due to the thiol (-SH) groups in 4MP. This disruption led to a reduction in C-C bonding and a decrease in the G-band peak in the Raman spectra. This study provides the first detailed investigation of the role of S in the graphitization of tincone, highlighting its impact on sp2 carbon formation and emphasizing the importance of the careful selection of precursors and linkers in MLD processes.

关键词： graphitization

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Structural analysis and elucidation of the formation process of specific carbon lamellae formed during the carbonization and graphitization of pitch

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CARBON 2025年 238卷

作者： Oshida, Kyoichi Takeuchi, Kenji Bonnamy, Sylvie Nakazawa, Tatsuo Endo, Morinobu Shinshu Univ 4-17-1 Wakasato Nagano 3808553 Japan Orleans Univ CNRS ICMN 1b Rue FerollerieCS 40059 F-45071 Orleans 2 France

A specific carbon lamella structure formed during the carbonization treatment of naphthalene-based anisotropic pitch and anisotropic coal tar pitch was investigated. Under transmission electron microscopy (TEM), the lamellae, despite being several tens of microns in size, were so thin that the TEM microgrid beneath the sample was visible through them, making them quite different from other common carbon particles. However, the detailed structure of the lamellae was not yet known. The purpose of this study was to analyze the detailed structure, formation process, properties, and surface conditions of carbon lamellae exhibiting unusual shapes. By tracing the formation process of the carbon lamellae, using various microscopy techniques, it was found that the structure of the lamella consisted of thick stacks of extremely thin hexagonal carbon layers. The edges of these layers were oriented perpendicular to the lamellar surfaces (edge-on). The lamellae were created on the surface of the thinner pores during foaming of the sample. The specific carbon lamellae were found to be graphitized in the same way as other normal carbons. Atomic force microscopy confirmed that these edge-on carbon layers could be clearly imaged. Until now, little attention has been paid to the existence of this specific carbon lamellae and their applications. However, since the edge sites of hexagonal carbon layers are much more reactive than those of basal planes, active utilization of hexagonal carbon layers is expected to lead to a variety of unprecedented applications. Further investigation of these edge sites is anticipated to open new scientific fields.

关键词： Anisotropic pitch Carbonization graphitization Optical microscopy Transmission electron microscopy Atomic force microscopy

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Catalytic graphitization of porous graphitic carbon derived from needle coke as anode materials for lithium-ion batteries

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MATERIALS RESEARCH EXPRESS 2025年第4期12卷 045502-045502页

作者： Zhang, Xiaoyu Guo, Shaoqiang Ye, Huifang Wei, Fangfang Hebei Univ Engn Sch Mat Sci & Engn Handan 056038 Peoples R China

In this work, potassium perferite (K2FeO4) is used as a catalyst in a straightforward and effective process of simultaneous activation and graphitization to create porous graphitized carbon (PGC), with coal-based green needle coke acting as starting material. The impacts of heating temperatures and K2FeO4 solution concentrations on the microstructure, morphology, and electrochemical lithium storage ability were thoroughly investigated. The as-synthesised PGC materials have a high specific surface area of 260.55 m2 g-1 and a good three-dimensional porous structure. Optimized PGC material synthesized at a temperature of 900 degrees C and concentrations of K2FeO4 solutions show excellent rate performance and cycling stability, making it a promising anode material for lithium-ion batteries (LIBs). At a current density of 100 mAg-1, it has a comparatively high specific discharge capacity of 386.05 mAh g-1 together with strong cycling stability (90.79% retention rate after 400 cycles). It maintains a discharge capacity of 325 mAh g-1 in the multiplicity test at a high current density of 1600 mA g-1. It takes less time, energy, and is much more efficient to complete the synchronous carbonization and graphitization of needle coke when potassium perferite is used as a catalyst, as opposed to traditional high-temperature graphitized technology and conventional two-step activation and graphitization strategy. The green needle coke-derived PGC materials include many active sites and defects, a high electrical conductivity, a shortened ion diffusion pathway, and a unique micro-mesoporous structure that makes them suitable electrode materials for lithium-ion batteries.

关键词： needle coke (NC) lithium storage performance potassium ferrate graphitization catalysis

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Effect of graphitization and activation on vegetable oil-derived carbon soot nanostructures for Zinc Ion hybrid capacitors

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CARBON 2025年 238卷

作者： Pandey, Antima Maurya, Prince Kumar Mishra, Ashish Kumar Banaras Hindu Univ Indian Inst Technol Sch Mat Sci & Technol Varanasi India

Hybrid Capacitors can provide solutions for fast and efficient energy supply. Here, we demonstrate oil-derived porous carbon soot nanostructures (pristine, activated, and graphitized) used as novel cathode materials for Zinc-ion hybrid capacitors (ZIHCs) with aqueous and solid electrolytes. The graphitized carbon soot (GCS) based aqueous ZIHC shows maximum discharge capacitances 255 F g-1 at 0.2 A g-1 with a maximum energy density of 90.8 W h kg-1 at power density of 160.23 W kg-1 and maximum power density of 8338.2 W kg-1 at energy density of 32 W h kg-1 within the voltage range of 0.2-1.8 V. The GCS-based aqueous ZIHC provides exceptional stability with a high-capacity retention of 95 % and nearly 100 % of coulombic efficiency up to 10,000 cycles. Moreover, solid-state zinc ion hybrid capacitors (SZIHCs) are developed by utilizing a durable polyvinyl alcohol (PVA) hydrogel with zinc sulphate as the solid-state electrolyte, achieving a high discharge capacitance of 480 F g-1 (Specific capacity = 219.7 mA h g-1) at a current density of 1 A g-1. The GCS- based SZIHC demonstrates an impressive energy density of 173.7 W h kg-1 at 799.8 W kg-1 power density coupled with a notably higher power density of 16000 W kg-1 at energy density of 21.6 W h kg-1, while maintaining outstanding nearly 98 % capacitance retention and 100 % coulombic efficiency over 10,000 cycles.

关键词： Zinc ion hybrid capacitors Carbon soot Activation graphitization Polyvinyl alcohol Zinc sulphate electrolyte

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Micropore-modulated graphitization for the construction of high-capacity hard carbon anode for sodium-ion batteries

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JOURNAL OF ENERGY STORAGE 2025年 114卷

作者： Duan, Zhihua Ye, Xiaoji Chen, Jingxun Chen, Jieqi Li, Jiakun Li, Zhenghui Guangdong Univ Technol Sch Mat & Energy Guangzhou 510006 Peoples R China Guangdong Acad Sci Inst Anal China Natl Analyt Ctr Guangzhou 510070 Peoples R China Natl Qual Inspect & Testing Ctr Green Mat & Prod Guangzhou 510070 Peoples R China Wuzhou Tongchuang New Energy Mat Co Ltd Wuzhou 543000 Peoples R China

The defects adsorption and closed pore filling contribute most of the specific capacity of hard carbon anode for sodium-ion batteries. Therefore, constructing a carbon framework with rich defects and closed pores is a promising method to achieve large Na+ storage capacity. However, this is difficult to realize because moderate graphitization facilitates the creation of closed pores but causes the elimination of structural defects. In the current work, we find that micropores can effectively hinder the ordered arrangement of carbon layers, thereby raising the graphitization temperature by approximate to 500 degrees C. Based on this, with appreciable carbonization temperature, a novel hard carbon incorporating rich defects and well-developed closed pores is developed. This hard carbon displays both large slope and plateau capacities, thus delivering a very high Na+ storage capacity of 365 mAh g-1, significantly exceeding the conventional hard carbon (253 mAh g-1). This work provides an innovative and reliable strategy for constructing high-performance hard carbon anode, which may shed light on promoting sodium-ion battery cells.

关键词： Hard carbons Micropores graphitization Sodium-ion batteries Anodes

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Evaluation of 14 C/ 12 C ratio measurements using accelerator mass spectrometry with standard materials under different graphitization conditions

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APPLIED RADIATION AND ISOTOPES 2025年 215卷 111589页

作者： Park, Sae-Hoon Lee, Seung-Won Kim, Yu-Seok Dongguk Univ Dept Energy & Elect Engn 123 Dongdae Ro Gyeongju si 38066 South Korea

In this study, an evaluation of carbon-beam tuning and 14 C/ 12 C ratio measurements is performed to validate the graphitization process in the pre-processing procedure employed at the accelerator mass spectrometry (AMS) facility of Dongguk University in Korea. The AMS isotopic ratio data are analyzed for samples subjected to three different graphitization conditions: (1) the entire process including Fe catalyst pre-heating with a high vacuum, (2) a high vacuum without pre-heating, and (3) a low vacuum without pre-heating. High-quality isotopic ratio measurements are achieved under these conditions. The measured mean isotopic ratio values for the background samples are almost equivalent to the different graphitization condition samples, with a difference in the order of 10_16. Therefore, conducting measurements with or without Fe catalyst pre-heating or high vacuum conditions is equally viable. Furthermore, the simplification of the graphitization process steps reduces the processing time required to produce five samples from 8 to 4 h, thereby enhancing the daily sample throughput by a factor of two, without compromising data quality.

关键词： Accelerator mass spectrometer Isotopic ratio Radiocarbon graphitization Sample preparation Carbon-beam tuning Fraction modern

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Low-temperature graphitization of nickel-containing carbon xerogels facilitated by the presence of citric acid and ethylene glycol in the resorcinol-formaldehyde precursor

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JOURNAL OF NON-CRYSTALLINE SOLIDS 2025年 657卷

作者： Veselov, Grigory B. Shubin, Yury V. Vedyagin, Aleksey A. Boreskov Inst Catalysis Novosibirsk Russia Nikolaev Inst Inorgan Chem Novosibirsk Russia

Carbon xerogels containing various metals are in demand for multiple applications, including electrocatalysis and energy storage systems. Nickel-containing organic xerogels were prepared via a one-pot approach based on sol-gel technology with the addition of citric acid and ethylene glycol during the polycondensation stage. The samples were characterized by several methods, including low-temperature nitrogen adsorption, X-ray diffraction analysis, Raman spectroscopy, and transmission electron microscopy. The pyrolysis of organic xerogels was studied by temperature-programmed carbonization. As found, the pyrolysis procedure performed at temperatures of 800 degrees C and above resulted in the appearance of partially graphitized carbon xerogels. Partial graphitization of nickel-doped carbon xerogels at Ni content of 2.5 % and such a low temperature as 800 degrees C is reported for the first time. The specific surface area of the prepared materials exceeded 560 m2/g. Nickel species of 10-100 nm in size were found to be evenly distributed within the carbon matrix.

关键词： Sol-gel synthesis Carbon xerogels Nickel Temperature-programmed carbonization graphitization

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Transformative Catalytic Carbon Conversion Enabling Superior graphitization and Nanopore Engineering in Hard Carbon Anodes for Sodium-Ion Batteries

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CARBON ENERGY 2025年第0期

作者： Zhang, Guilai Gao, Hong Zhang, Dingyi Xiao, Jun Sun, Limeng Li, Jiayi Li, Congcong Sun, Yiwen Yuan, Xinyao Huang, Peng Xu, Yi Guo, Xin Zhao, Yufei Wang, Yong Xiao, Yao Wang, Guoxiu Liu, Hao Shanghai Univ Sch Environm & Chem Engn Joint Int Lab Environm & Energy Frontier Mat Shanghai Peoples R China Shanghai Univ State Key Lab Adv Special Steel Shanghai Key Lab Adv Ferromet Shanghai Peoples R China Jiangsu Normal Univ Sch Chem & Mat Sci Xuzhou Jiangsu Peoples R China Shenzhen Univ Adv Technol Fac Mat Sci & Energy Engn Shenzhen Guangdong Peoples R China Univ Technol Sydney Ctr Clean Energy Technol Sydney NSW Australia Wenzhou Univ Coll Chem & Mat Engn Wenzhou Peoples R China

Hard carbons are promising anode materials for sodium-ion batteries (SIBs), but they face challenges in balancing rate capability, specific capacity, and initial Coulombic efficiency (ICE). Direct pyrolysis of the precursor often fails to create a suitable structure for sodium-ion storage. Molecular-level control of graphitization with open channels for Na+ ions is crucial for high-performance hard carbon, whereas closed pores play a key role in improving the low-voltage (< 0.1 V) plateau capacity of hard carbon anodes for SIBs. However, creation of these closed pores presents significant challenges. This work proposes a zinc gluconate-assisted catalytic carbonization strategy to regulate graphitization and create numerous nanopores simultaneously. As the temperature increases, trace amounts of zinc remain as single atoms in the hard carbon, featuring a uniform coordination structure. This mitigates the risk of electrochemically irreversible sites and enhances sodium-ion transport rates. The resulting hard carbon shows an excellent reversible capacity of 348.5 mAh g(-1) at 30 mA g(-1) and a high ICE of 92.84%. Furthermore, a sodium storage mechanism involving "adsorption-intercalation-pore filling" is elucidated, providing insights into the pore structure and dynamic pore-filling process.

关键词： catalytic carbonization graphitization hard carbon nanopores sodium-ion batteries

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Molten salt Mg²⁺/Mg bifunctional system for enhancing graphitization of low-temperature biomass-derived carbon

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IONICS 2025年第5期31卷 4421-4430页

作者： Wang, Fan Wang, Yuxin Guan, Ziheng Wei, Junjie He, Shengliang Zhong, Zhen Chen, Hao Feng, Peizhong China Univ Min & Technol Sch Mat Sci & Phys Xuzhou 221116 Jiangsu Peoples R China Zhejiang Jiahe Bamboo Technol Co Ltd Lishui 323000 Zhejiang Peoples R China Zhejiang Univ Sci & Technol Sch Biol & Chem Engn Hangzhou 310023 Peoples R China Zhejiang A&F Univ Coll Chem & Mat Engn Hangzhou 311300 Peoples R China

The development of low-temperature graphitization methods for biomass-derived carbon is critical for sustainable lithium-ion battery anodes. Herein, we propose a MgCl2-NaCl-KCl molten salt system exploiting the bifunctional role of Mg2+/Mg to achieve graphitization at 750 degrees C. The strong oxygen affinity of Mg2+ synergizes with electrochemical polarization to rapidly deoxygenate carbon surfaces, while Mg deposition catalyzes the conversion of SiO2 impurities to conductive SiC (via SiO2 + 2 Mg -> Si + 2MgO;Si + C -> SiC) and promotes carbon rearrangement. The resulting graphite/SiC composite exhibits enhanced crystallinity (27% graphitization degree) and electrochemical performance, delivering a capacity of 198 mAh g(-1) at 0.1 A g(-1) and retaining 70.2% capacity after 6000 cycles. In summary, this study fully exploited the strong bonding capability of Mg2+ with oxygen and the reduction and catalytic properties of deposited Mg. This dual-functional role not only significantly reduced the required temperature for the reaction process (750 degrees C) but also maintained the graphitization process of biomass-derived carbon at high temperatures (> 750 degrees C). This method provides a low-cost, low-energy-consumption pathway for the high-value-added application of biomass-derived hard carbon materials in lithium-ion battery graphite anodes.

关键词： Molten salt electrolysis Mg2+/Mg bifunctional Silicon-containing biomass-derived carbon graphitization C(graphite)/SiC anode

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C-C bond rupture initiated graphitization achieves highly efficient diamond polishing

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INTERNATIONAL JOURNAL OF MECHANICAL SCIENCES 2025年 287卷

作者： Liu, Nian Lei, Ling Lu, Hao Jiang, Huilong Zhang, Yongjie Xiao, Junfeng Zhang, Jianguo Chen, Xiao Xu, Jianfeng Huazhong Univ Sci & Technol Sch Mech Sci & Engn State Key Lab Intelligent Mfg Equipment & Technol Luoyu Rd 1037 Wuhan 430074 Hubei Peoples R China Minist Educ Key Lab Adv Mfg Technol High Performance Parts Beijing Peoples R China Southern Univ Sci & Technol Dept Mech & Energy Engn Shenzhen 518055 Guangdong Peoples R China Hubei Univ Technol Sch Mech & Engn Wuhan 430074 Hubei Peoples R China

Diamond is the ultimate semiconductor for power devices that operate at high-power, high-temperature, and high-frequency conditions. However, diamond polishing is challenging owing to its extreme hardness and brittleness. In this study, a novel material removal mechanism of C-C bond rupture initiated graphitization for highly efficient diamond polishing was proposed. Linear reciprocating sliding experiments demonstrated that the diamond material was removed in the form of graphite rather than chipped off as diamond fragments, and a high wear rate was achieved under low gas pressure and ultraviolet (UV) irradiation conditions. Based on this, a novel low-gas-pressure UV-assisted polishing method was proposed as a highly efficient approach for polishing diamond. A high material removal rate of 15.8 mu m/h was achieved, and the high efficiency was verified by the rapid surface roughness improvement from 465.5 to 3.7 nm within 70 min. Subsequently, a ReaxFF molecular dynamics simulation was conducted to clarify the atomic removal mechanism. Atomic attrition was accompanied by the rupture of C-C bonds, and the reconstruction of diamond into graphite was activated by large amounts of C-C bond ruptures. We propose that the reconstruction of diamond into graphite activated by a large number of C-C bond ruptures is essential for achieving a high material removal rate.

关键词： Ultraviolet assisted polishing Ultra-precision subtractive manufacturing Polishing efficiency Diamond graphitization Material removal mechanism

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