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Keywords = polycrystalline graphite

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27 pages, 6913 KB  
Article
Stabilizing Effect of Polycrystalline Diamond on Graphite Anodes for Li Ion Batteries
by Julio Saldaña-Rivera, Enrique Quiroga-González, Daniel Villarreal, Orlando Auciello and Elida de Obaldía
Coatings 2025, 15(12), 1450; https://doi.org/10.3390/coatings15121450 - 8 Dec 2025
Viewed by 233
Abstract
Improving the interfacial stability of graphite anodes remains a major challenge for extending the lifetime of lithium-ion batteries. In this study, ultrananocrystalline diamond (UNCD) and nitrogen-incorporated UNCD (N-UNCD) coatings were employed as protective layers to enhance the electrochemical and mechanical robustness of graphite [...] Read more.
Improving the interfacial stability of graphite anodes remains a major challenge for extending the lifetime of lithium-ion batteries. In this study, ultrananocrystalline diamond (UNCD) and nitrogen-incorporated UNCD (N-UNCD) coatings were employed as protective layers to enhance the electrochemical and mechanical robustness of graphite electrodes. Half-cells were cycled for 60 charge–discharge cycles, and their behavior was examined through electrochemical impedance spectroscopy (EIS), Distribution of Relaxation Times (DRT), and Equivalent Circuit Modeling (ECM) to disentangle the characteristic relaxation processes. The potential–capacity profiles exhibited the typical LiC12–LiC6 transition plateaus without any additional features for the coated electrodes, confirming that the UNCD and N-UNCD films do not participate in lithium storage but serve as chemically inert and electrically stable interlayers. In contrast, the uncoated reference graphite anodes showed greater capacity fluctuations and increasing interfacial impedance. DRT and ECM analyses revealed four consistent relaxation processes—electronic transport (τ1), ionic transport through the electrolyte (τ2), Solid Electrolyte Interface (SEI) response (τ3), and lithium intercalation (τ4). The τ2 process remained invariant, whereas τ3 and τ4 were markedly stabilized by the UNCD and N-UNCD coatings. UNCD exhibited the lowest SEI-related resistance and the most stable charge-transfer kinetics, while N-UNCD displayed an initially higher τ3 resistance followed by progressive self-stabilization after 20 charge/discharge cycles, linked to reorganization of nitrogen-rich grain boundaries. Overall, polycrystalline diamond coatings—particularly UNCD—proved to be highly effective in suppressing SEI layer growth, minimizing impedance rise, and preserving lithium intercalation efficiency, leading to enhanced long-term electrochemical performance. These findings highlight the potential of diamond-based protective layers as a durable and scalable strategy for next-generation graphite anodes. Full article
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18 pages, 8588 KB  
Article
Study on Sintering Behavior, Heat and Wear Resistance of Refractory Metal Borides (HfB2, ZrB2) and Al-Ni Modified PDC
by Chuang Zhao, Wenhao Dai, Shaotao Xu and Baochang Liu
Materials 2025, 18(22), 5093; https://doi.org/10.3390/ma18225093 - 9 Nov 2025
Viewed by 481
Abstract
Polycrystalline Diamond Compacts (PDC) face thermal damage and insufficient wear resistance in complex strata due to the high thermal expansion coefficient of Co binder and its catalysis on diamond graphitization. Existing studies lack a systematic comparison of HfB2, ZrB2, [...] Read more.
Polycrystalline Diamond Compacts (PDC) face thermal damage and insufficient wear resistance in complex strata due to the high thermal expansion coefficient of Co binder and its catalysis on diamond graphitization. Existing studies lack a systematic comparison of HfB2, ZrB2, and Al-Ni (1.5wt.%Al + 1.5wt.%Ni) on PDC performance under a unified process, and their synergistic mechanism with the PDC matrix remains unclear. Herein, 3wt.% of these additives were incorporated into diamond micropowder to prepare PDC via unified high-temperature and high-pressure (HTHP) sintering. XRD/SEM-EDS characterized the phase/microstructure, while thermal expansion and Vertical Turret Lathe (VTL) tests evaluated their properties. Results: (1) ZrB2-modified PDC performed the best, with a thermal failure temperature of 800 °C (8.5% higher than the blank group), VTL wear cycles of 110 Pass (22.2% higher), and ZrC (confirmed by XRD) enhancing interface bonding; (2) HfB2-modified PDC reduced the wear area by 18% (vs. the blank group) via low-expansion HfC (6.5 × 10−6/°C) and maintained a continuous structure; (3) Al-Ni-modified PDC had a wear ratio of 1.945 × 104 (4.5% higher) but only 60 Pass and structural defects. This study confirms ZrB2 as the optimal additive for PDC’s comprehensive properties, supporting high-performance PDC development for complex downhole environments. Full article
(This article belongs to the Section Metals and Alloys)
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17 pages, 2210 KB  
Article
The Preparation and Properties of Polycrystalline Bi2O2Se—Pitfalls in Reproducibility and Charge-Transport Limiting Factors
by Jan Zich, Tomáš Plecháček, Antonín Sojka, Petr Levinský, Jiří Navrátil, Pavlína Ruleová, Stanislav Šlang, Karel Knížek, Jiří Hejtmánek, Vojtěch Nečina and Čestmír Drašar
Crystals 2025, 15(11), 951; https://doi.org/10.3390/cryst15110951 - 3 Nov 2025
Viewed by 492
Abstract
Thermoelectric materials enable the direct conversion of heat into electricity, but progress is often limited by challenges in reproducibility and stability. Bi2O2Se has recently attracted attention as a promising candidate; however, reported transport properties of undoped polycrystalline samples vary [...] Read more.
Thermoelectric materials enable the direct conversion of heat into electricity, but progress is often limited by challenges in reproducibility and stability. Bi2O2Se has recently attracted attention as a promising candidate; however, reported transport properties of undoped polycrystalline samples vary by several orders of magnitude, complicating its use as a baseline for doping studies. In this work, we investigate the sources of variability and identify key factors including precursor contamination, reactions with quartz ampoules and graphite dies, grain size effects, and surface oxidation. To mitigate these issues, we employed calcination of Bi2O3 precursors, synthesis with controlled temperature gradients, coarse-fraction powders, and hot pressing in Si3N4 dies. The resulting polycrystalline Bi2O2Se exhibits improved reproducibility, reduced sensitivity to thermal cycling, and characteristic transport values around σRT ≈ 500 S·m−1 and S ≈ −300 μV·K−1 at room temperature. This is a good starting point for further doping studies and a prerequisite of thermoelectric efficiency studies in the future, which can reveal the true thermoelectric potential of this material. Full article
(This article belongs to the Special Issue Research Progress on Thermoelectric Materials)
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13 pages, 4718 KB  
Article
800 kHz Femtosecond Laser Cleaning of Microwave Plasma Chemical Vapor Deposition Diamond Growth Substrate
by Xiwang Wu and Xin Chen
Crystals 2025, 15(6), 517; https://doi.org/10.3390/cryst15060517 - 28 May 2025
Viewed by 861
Abstract
Microwave Plasma Chemical Vapor Deposition (MPCVD) plays a crucial role in the growth of high-quality diamonds. However, during the MPCVD process, residues such as polycrystalline diamond, and graphite often adhere to the high-temperature growth substrate surfaces, potentially degrading diamond growth quality. To effectively [...] Read more.
Microwave Plasma Chemical Vapor Deposition (MPCVD) plays a crucial role in the growth of high-quality diamonds. However, during the MPCVD process, residues such as polycrystalline diamond, and graphite often adhere to the high-temperature growth substrate surfaces, potentially degrading diamond growth quality. To effectively remove these contaminants and improve the quality of diamond growth, this study employed an 800 kHz femtosecond laser to clean growth substrates with residual deposits. We assessed the effects of multiple cleaning cycles on residue removal from the Foundation Trench Region (FTR) and Inwall Region (IR) and on substrate quality. The results indicate that multiple scans at a laser power of 2.38 W, a repetition rate of 800 kHz, a scanning speed of 1800 mm/s, and a scan spacing of 10 μm significantly removed residues, reduced substrate surface roughness, and restored substrate cleanliness. This approach enhances the quality and efficiency of diamond growth via MPCVD. The application of high-repetition-rate femtosecond laser cleaning techniques for growth substrates significantly improves the quality of regenerated diamond films, providing crucial support for the preparation of high-quality diamond materials. Full article
(This article belongs to the Section Materials for Energy Applications)
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14 pages, 2963 KB  
Article
Synthesis, Structure, and Electrophysical and Electrochemical Properties of Novel Composite La0.9MnO3-LaFeO3
by Mukhametkali Mataev, Zamira Sarsenbaeva, Bahadir Keskin, Marzhan Nurbekova, Amangeldi Meldeshov, Zhanar Tursyn and Karima Seitbekova
Molecules 2025, 30(1), 132; https://doi.org/10.3390/molecules30010132 - 31 Dec 2024
Cited by 5 | Viewed by 1988
Abstract
This article presents the synthesis, electrophysical, and catalytic properties of a La0.9MnO3–LaFeO3 nanocomposite material. The nanocomposite was synthesized via the sol–gel (Pechini) method. X-ray diffraction (XRD) analysis revealed a polycrystalline, biphasic perovskite structure combining both hexagonal and cubic [...] Read more.
This article presents the synthesis, electrophysical, and catalytic properties of a La0.9MnO3–LaFeO3 nanocomposite material. The nanocomposite was synthesized via the sol–gel (Pechini) method. X-ray diffraction (XRD) analysis revealed a polycrystalline, biphasic perovskite structure combining both hexagonal and cubic symmetry. The microstructure and elemental composition, examined using field emission scanning electron microscopy (FESEM), indicated an average particle size of approximately 186.9 nm. The composite exhibits semiconducting behavior within the temperature ranges of 293–323 K and 343–393 K. Developing electrocatalysts free of precious metals for the hydrogen evolution reaction (HER) is increasingly important to facilitate the production of hydrogen from renewable sources. In this study, the conductive La0.9MnO3–LaFeO3 composite was deposited on graphite and, for the first time, evaluated as an electrocatalyst for HER in acidic media. The resulting composite films were tested using linear sweep voltammetry (LSV) and electrochemical impedance spectroscopy (EIS) in a glassy carbon electrode (GCE) setup, providing insights into their potential as effective, cost-efficient electrocatalysts. Full article
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22 pages, 17244 KB  
Article
Mechanisms Behind Graphitization Modification in Polycrystalline Diamond by Nanosecond Pulsed Laser
by Xinrui Cui, Chunyu Zhang, Guo Li, Chengwei Song, Wentao Qin and Tao Wang
Materials 2024, 17(24), 6200; https://doi.org/10.3390/ma17246200 - 19 Dec 2024
Cited by 6 | Viewed by 1599
Abstract
The ultraprecision machining of diamond presents certain difficulties due to its extreme hardness. However, the graphitization modification can enhance its machinability. This work presents an investigation into the characteristics of the graphitization modification in polycrystalline diamond induced by a nanosecond pulsed laser. In [...] Read more.
The ultraprecision machining of diamond presents certain difficulties due to its extreme hardness. However, the graphitization modification can enhance its machinability. This work presents an investigation into the characteristics of the graphitization modification in polycrystalline diamond induced by a nanosecond pulsed laser. In this paper, the morphology of microgrooves under laser modification was observed, material deposition and graphitization in different regions were researched, and the regularities of microgrooves at different laser powers were obtained. A molecular dynamics (MD) simulation was carried out to reveal the mechanism behind graphitization modification; when the pulse laser acts on the diamond surface and the temperature rises to the critical temperature of graphitization, the graphite crystal nuclei form and grow, resulting in the graphitization modification. It was confirmed that the existence of grain boundaries (GBs) contributed to the graphitization of polycrystalline diamond during laser modification. It was predicted that a lower laser power could cause a higher proportion of graphitization. The results of ablation thresholds and the effect of the defocusing position on the graphitization of diamond showed that for a fixed laser power, the highest graphitization ratio could be obtained when the defocusing quantity was optimized. Finally, the results of precision grinding experiments verified the feasibility of using laser graphitization pretreatment to improve the efficiency and quality of precision grinding. Full article
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10 pages, 2545 KB  
Article
Low-Temperature Annealing of Nanoscale Defects in Polycrystalline Graphite
by Gongyuan Liu, Hajin Oh, Md Hafijur Rahman, Jing Du, William Windes and Aman Haque
C 2024, 10(3), 76; https://doi.org/10.3390/c10030076 - 26 Aug 2024
Cited by 2 | Viewed by 2569
Abstract
Polycrystalline graphite contains multi-scale defects, which are difficult to anneal thermally because of the extremely high temperatures involved in the manufacturing process. In this study, we demonstrate annealing of nuclear graphite NBG-18 at temperatures below 28 °C, exploiting the electron wind force, a [...] Read more.
Polycrystalline graphite contains multi-scale defects, which are difficult to anneal thermally because of the extremely high temperatures involved in the manufacturing process. In this study, we demonstrate annealing of nuclear graphite NBG-18 at temperatures below 28 °C, exploiting the electron wind force, a non-thermal stimulus. High current density pulses were passed through the specimens with a very low-duty cycle so that the electron momentum could mobilize the defects without heating the specimen. The effectiveness of this technique is presented with a significant decrease in electrical resistivity, defect counts from X-ray computed tomography, Raman spectroscopy, and nanoindentation-based mechanical characterization. Such multi-modal evidence highlights the feasibility of nanoscale defect control at temperatures about two orders of magnitude below the graphitization temperature. Full article
(This article belongs to the Special Issue Characterization of Disorder in Carbons (2nd Edition))
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12 pages, 2680 KB  
Article
Synthesis of Wrinkled MoS2 Thin Films Using a Two-Step Method Consisting of Magnetron Sputtering and Sulfurization in a Confined Space
by Claudia Mihai, Iosif-Daniel Simandan, Florinel Sava, Angel-Theodor Buruiana, Amelia Elena Bocirnea, Teddy Tite, Mohamed Yassine Zaki and Alin Velea
Sustainability 2024, 16(9), 3819; https://doi.org/10.3390/su16093819 - 1 May 2024
Cited by 2 | Viewed by 3337
Abstract
Considering the increasing need for sustainable and economical energy storage solutions, the integration of layered materials such as MoS2 into these systems represents an important step toward enhancing energy sustainability and efficiency. Exploring environmentally responsible fabrication techniques, this study assesses wrinkled MoS [...] Read more.
Considering the increasing need for sustainable and economical energy storage solutions, the integration of layered materials such as MoS2 into these systems represents an important step toward enhancing energy sustainability and efficiency. Exploring environmentally responsible fabrication techniques, this study assesses wrinkled MoS2 thin films synthesized from distinct Mo and MoS2 targets, followed by sulfurization conducted in a graphite box. We utilized magnetron sputtering to deposit precursor Mo and MoS2 films on Si substrates, achieving thicknesses below 20 nm. This novel approach decreases sulfur by up to tenfold during sulfurization due to the confined space technique, contributing also to avoiding the formation of toxic gases such as SO2 or the necessity of using H2S, aligning with sustainable materials development. Thinner MoS2 layers were obtained post-sulfurization from the MoS2 precursors, as shown by X-ray reflectometry. Raman spectroscopy and grazing X-ray diffraction analyses confirmed the amorphous nature of the as-deposited films. Post-sulfurization, both types of films exhibited crystalline hexagonal MoS2 phases, with the sulfurized Mo showing a polycrystalline nature with a (100) orientation and sulfurized MoS2 displaying a (00L) preferred orientation. The X-ray photoelectron spectroscopy results supported a Mo:S ratio of 1:2 on the surface of the films obtained using the MoS2 precursor films, confirming the stoichiometry obtained by means of energy dispersive X-ray spectroscopy. Scanning electron microscopy and atomic force microscopy images revealed micrometer-sized clusters potentially formed during rapid cooling post-sulfurization, with an increased average roughness. These results open the way for the further exploration of wrinkled MoS2 thin films in advanced energy storage technologies. Full article
(This article belongs to the Section Sustainable Materials)
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13 pages, 9545 KB  
Article
RHEED Study of the Epitaxial Growth of Silicon and Germanium on Highly Oriented Pyrolytic Graphite
by Kirill A. Lozovoy, Vladimir V. Dirko, Olzhas I. Kukenov, Arseniy S. Sokolov, Konstantin V. Krukovskii, Mikhail S. Snegerev, Alexey V. Borisov, Yury V. Kistenev and Andrey P. Kokhanenko
C 2024, 10(2), 36; https://doi.org/10.3390/c10020036 - 10 Apr 2024
Cited by 1 | Viewed by 3364
Abstract
Two-dimensional silicon (silicene) and germanium (germanene) have attracted special attention from researchers in recent years. At the same time, highly oriented pyrolytic graphite (HOPG) and graphene are some of the promising substrates for growing silicene and germanene. However, to date, the processes occurring [...] Read more.
Two-dimensional silicon (silicene) and germanium (germanene) have attracted special attention from researchers in recent years. At the same time, highly oriented pyrolytic graphite (HOPG) and graphene are some of the promising substrates for growing silicene and germanene. However, to date, the processes occurring during the epitaxial growth of silicon and germanium on the surface of such substrates have been poorly studied. In this work, the epitaxial growth of silicon and germanium is studied directly during the process of the molecular beam epitaxy deposition of material onto the HOPG surface by reflection high-energy electron diffraction (RHEED). In addition, the obtained samples are studied by Raman spectroscopy and scanning electron microscopy. A wide range of deposition temperatures from 100 to 800 °C is considered and temperature intervals are determined for various growth modes of silicon and germanium on HOPG. Conditions for amorphous and polycrystalline growth are distinguished. Diffraction spots corresponding to the lattice constants of silicene and germanene are identified that may indicate the presence of areas of graphene-like 2D phases during epitaxial deposition of silicon and germanium onto the surface of highly oriented pyrolytic graphite. Full article
(This article belongs to the Special Issue Advances in Bilayer Graphene)
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13 pages, 2899 KB  
Article
Real-Time Observation of Nanoscale Kink Band Mediated Plasticity in Ion-Irradiated Graphite: An In Situ TEM Study
by Melonie P. Thomas, Ryan Schoell, Nahid Sultan Al-Mamun, Winson Kuo, John Watt, William Windes, Khalid Hattar and Aman Haque
Materials 2024, 17(4), 895; https://doi.org/10.3390/ma17040895 - 15 Feb 2024
Cited by 10 | Viewed by 2438
Abstract
Graphite IG-110 is a synthetic polycrystalline material used as a neutron moderator in reactors. Graphite is inherently brittle and is known to exhibit a further increase in brittleness due to radiation damage at room temperature. To understand the irradiation effects on pre-existing defects [...] Read more.
Graphite IG-110 is a synthetic polycrystalline material used as a neutron moderator in reactors. Graphite is inherently brittle and is known to exhibit a further increase in brittleness due to radiation damage at room temperature. To understand the irradiation effects on pre-existing defects and their overall influence on external load, micropillar compression tests were performed using in situ nanoindentation in the Transmission Electron Microscopy (TEM) for both pristine and ion-irradiated samples. While pristine specimens showed brittle and subsequent catastrophic failure, the 2.8 MeV Au2+ ion (fluence of 4.378 × 1014 cm−2) irradiated specimens sustained extensive plasticity at room temperature without failure. In situ TEM characterization showed nucleation of nanoscale kink band structures at numerous sites, where the localized plasticity appeared to close the defects and cracks while allowing large average strain. We propose that compressive mechanical stress due to dimensional change during ion irradiation transforms buckled basal layers in graphite into kink bands. The externally applied load during the micropillar tests proliferates the nucleation and motion of kink bands to accommodate the large plastic strain. The inherent non-uniformity of graphite microstructure promotes such strain localization, making kink bands the predominant mechanism behind unprecedented toughness in an otherwise brittle material. Full article
(This article belongs to the Special Issue Advanced Characterization Techniques on Nuclear Fuels and Materials)
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11 pages, 3201 KB  
Article
Effects of Surface Size and Shape of Evaporation Area on SiC Single-Crystal Growth Using the PVT Method
by Yu Zhang, Xin Wen, Nuofu Chen, Fang Zhang, Jikun Chen and Wenrui Hu
Crystals 2024, 14(2), 118; https://doi.org/10.3390/cryst14020118 - 25 Jan 2024
Cited by 4 | Viewed by 3810
Abstract
Silicon carbide (SiC) polycrystalline powder. As the raw material for SiC single-crystal growth through the physical vapor transport (PVT) method, its surface size and shape have a great influence on growth of crystal. The surface size and shape of the evaporation area filled [...] Read more.
Silicon carbide (SiC) polycrystalline powder. As the raw material for SiC single-crystal growth through the physical vapor transport (PVT) method, its surface size and shape have a great influence on growth of crystal. The surface size and shape of the evaporation area filled with polycrystalline powder were investigated by numerical simulation in this study. Firstly, the temperature distribution and deposition rate distribution for the PVT system were calculated by global numerical simulation, and the optimal ratio of polycrystalline powder surface diameter to seed crystal diameter was determined to be 1.6. Secondly, the surface of the evaporation area filled with polycrystalline powder was covered by a graphite ring and a graphite disc, respectively, to change its surface shape. The results show that adjusting the surface size and shape of the evaporation area filled with polycrystalline powder is an effective method to control the growth rate, growth stability, and growth surface shape of the single crystal. Finally, the result obtained by selecting appropriate covered structures for actual growth indicates that this process can act as a reference for improving the quality of single crystals. Full article
(This article belongs to the Special Issue Wide Bandgap Semiconductor: GaN and SiC Material and Device)
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11 pages, 8081 KB  
Article
Surface Nanotexturing of Boron-Doped Diamond Films by Ultrashort Laser Pulses
by Matteo Mastellone, Eleonora Bolli, Veronica Valentini, Stefano Orlando, Antonio Lettino, Riccardo Polini, Josephus Gerardus Buijnsters, Alessandro Bellucci and Daniele Maria Trucchi
Micromachines 2023, 14(2), 389; https://doi.org/10.3390/mi14020389 - 4 Feb 2023
Cited by 9 | Viewed by 2693
Abstract
Polycrystalline boron-doped diamond (BDD) films were surface nanotextured by femtosecond pulsed laser irradiation (100 fs duration, 800 nm wavelength, 1.44 J cm−2 single pulse fluence) to analyse the evolution of induced alterations on the surface morphology and structural properties. The aim was [...] Read more.
Polycrystalline boron-doped diamond (BDD) films were surface nanotextured by femtosecond pulsed laser irradiation (100 fs duration, 800 nm wavelength, 1.44 J cm−2 single pulse fluence) to analyse the evolution of induced alterations on the surface morphology and structural properties. The aim was to identify the occurrence of laser-induced periodic surface structures (LIPSS) as a function of the number of pulses released on the unit area. Micro-Raman spectroscopy pointed out an increase in the graphite surface content of the films following the laser irradiation due to the formation of ordered carbon sites with respect to the pristine sample. SEM and AFM surface morphology studies allowed the determination of two different types of surface patterning: narrow but highly irregular ripples without a definite spatial periodicity or long-range order for irradiations with relatively low accumulated fluences (<14.4 J cm−2) and coarse but highly regular LIPSS with a spatial periodicity of approximately 630 nm ± 30 nm for higher fluences up to 230.4 J cm−2. Full article
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12 pages, 2810 KB  
Article
Growth and Characterization of Ultrathin Vanadium Oxide Films on HOPG
by Yue Sun, Koen Schouteden, María Recaman Payo, Jean-Pierre Locquet and Jin Won Seo
Nanomaterials 2022, 12(18), 3134; https://doi.org/10.3390/nano12183134 - 9 Sep 2022
Cited by 5 | Viewed by 3063
Abstract
Integration of graphene into various electronic devices requires an ultrathin oxide layer on top of graphene. However, direct thin film growth of oxide on graphene is not evident because of the low surface energy of graphene promoting three-dimensional island growth. In this study, [...] Read more.
Integration of graphene into various electronic devices requires an ultrathin oxide layer on top of graphene. However, direct thin film growth of oxide on graphene is not evident because of the low surface energy of graphene promoting three-dimensional island growth. In this study, we demonstrate the growth of ultrathin vanadium oxide films on a highly oriented pyrolytic graphite (HOPG) surface, which mimics the graphene surface, using (oxygen-assisted) molecular beam epitaxy, followed by a post-annealing. The structural properties, surface morphology, and chemical composition of the films have been systematically investigated by in situ reflection high-energy electron diffraction during the growth and by ex situ techniques, such as atomic force microscopy, scanning tunneling microscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy (XPS). Crystalline monolayer vanadium oxide can be achieved on HOPG by systematically tuning the deposition time of V atoms and by subsequent annealing at 450 °C in controlled atmospheres. Increasing the partial pressure of O2 during the deposition seems to decrease the mobility of V atoms on the graphitic surface of HOPG and promote the formation of a two-dimensional (2D) vanadium oxide. The obtained oxide layers are found to be polycrystalline with an average grain size of 15 nm and to have a mixed-valence state with mainly V5+ and V4+. Moreover, XPS valence band measurements indicate that the vanadium oxide is insulating. These results demonstrate that a 2D insulating vanadium oxide can be grown directly on HOPG and suggest vanadium oxide as a promising candidate for graphene/oxide heterostructures. Full article
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15 pages, 5548 KB  
Article
High Pressure (HP) in Spark Plasma Sintering (SPS) Processes: Application to the Polycrystalline Diamond
by Jérémy Guignard, Mythili Prakasam and Alain Largeteau
Materials 2022, 15(14), 4804; https://doi.org/10.3390/ma15144804 - 9 Jul 2022
Cited by 9 | Viewed by 4256
Abstract
High-Pressure (HP) technology allows new possibilities of processing by Spark Plasma Synthesis (SPS). This process is mainly involved in the sintering process and for bonding, growing and reaction. High-Pressure tools combined with SPS is applied for processing polycrystalline diamond without binder (binderless PCD) [...] Read more.
High-Pressure (HP) technology allows new possibilities of processing by Spark Plasma Synthesis (SPS). This process is mainly involved in the sintering process and for bonding, growing and reaction. High-Pressure tools combined with SPS is applied for processing polycrystalline diamond without binder (binderless PCD) in this current work. Our described innovative Ultra High Pressure Spark Plasma Sintering (UHP-SPS) equipment shows the combination of our high-pressure apparatus (Belt-type) with conventional pulse electric current generator (Fuji). Our UHP-SPS equipment allows the processing up to 6 GPa, higher pressure than HP-SPS equipment, based on a conventional SPS equipment in which a non-graphite mold (metals, ceramics, composite and hybrid) with better mechanical properties (capable of 1 GPa) than graphite. The equipment of UHP-SPS and HP-SPS elements (pistons + die) conductivity of the non-graphite mold define a Hot-Pressing process. This study presents the results showing the ability of sintering diamond powder without additives at 4–5 GPa and 1300–1400 °C for duration between 5 and 30 min. Our described UHP-SPS innovative cell design allows the consolidation of diamond particles validated by the formation of grain boundaries on two different grain size powders, i.e., 0.75–1.25 μm and 8–12 μm. The phenomena explanation is proposed by comparison with the High Pressure High Temperature (HP-HT) (Belt, toroidal-Bridgman, multi-anvils (cubic)) process conventionally used for processing binderless polycrystalline diamond (binderless PCD). It is shown that using UHP-SPS, binderless diamond can be sintered at very unexpected P-T conditions, typically ~10 GPa and 500–1000 °C lower in typical HP-HT setups. This makes UHP-SPS a promising tool for the sintering of other high-pressure materials at non-equilibrium conditions and a potential industrial transfer with low environmental fingerprints could be considered. Full article
(This article belongs to the Special Issue Spark Plasma Synthesis under High Pressure for Advanced Materials)
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12 pages, 3140 KB  
Article
Study on the Polycrystalline Mechanism of Polycrystalline Diamond Synthesized from Graphite by Direct Detonation Method
by Shi-Yuan Shang, Yi Tong, Zhi-Chao Wang and Feng-Lei Huang
Materials 2022, 15(12), 4154; https://doi.org/10.3390/ma15124154 - 11 Jun 2022
Cited by 2 | Viewed by 2330
Abstract
In this paper, a polycrystalline diamond was synthesized by the direct detonation method using graphite as the carbon source. By comparing the numbers of the obtained diamond particles and the original graphite particles, it was found that when the graphite phase transformed into [...] Read more.
In this paper, a polycrystalline diamond was synthesized by the direct detonation method using graphite as the carbon source. By comparing the numbers of the obtained diamond particles and the original graphite particles, it was found that when the graphite phase transformed into the polycrystalline diamond during the detonation process, a single graphite particle would form multiple diamond nuclei, and the nuclei would grow simultaneously to form polycrystals. Accordingly, a validation experiment was designed, which added different ratios of inert additives while keeping the ratio of graphite to hexogen (RDX) unchanged. It was found that increasing the ratio of inert additives within a certain range could increase the grain size of a polycrystalline diamond, which is consistent with the obtained polycrystalline mechanism. Full article
(This article belongs to the Section Carbon Materials)
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