Makine Mühendisliği Bölümü Koleksiyonu
Permanent URI for this collectionhttps://hdl.handle.net/20.500.11779/1944
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Article Citation - WoS: 1Citation - Scopus: 1A Few Layers Graphene Encapsulated Fe-Based Nanoparticles Synthesized from Ferrocene Containing Precursors: CVD Optimization and Evaluation for Possible Nanocatalyst Performance towards H2 Production(Pergamon-Elsevier Science Ltd, 2026-04-01) Demirbas, Derya; Kutluay, Sinan; Agaogullari, Duygu; Suzer-Cicek, Layda; Mertdinc-Ulkuseven, Siddika; Padberg, Gero; Felderhoff, Michael; Süzer-Çiçek, İlaydaThis study focuses on optimizing the synthesis of a few-layer graphene-encapsulated iron-based nanoparticles (Fe/Fe3C@C), prepared through spray drying, chemical vapor deposition (CVD), and leaching processes using ferrocene-based precursors, and their application as nanocatalysts for hydrogen (H2) production via sodium borohydride (NaBH4) methanolysis. Ferrocene-impregnated silica powders were prepared by spray drying them from a solution containing ferrocene, fumed silica, and ethanol. Then, these prepared powders, known as precursor powders, were subsequently introduced into the CVD system. Both the reduction of ferrocene and the encapsulation of Fe-based nanoparticles by graphene layers occurred in-situ during the CVD process. CVD temperature and the flow rates of CH4 and H2 gases are critical parameters that effects of the microstructural, thermal, and magnetic properties of synthesized nanoparticles. The CVD system was performed at temperatures ranging from 850 to 1000 degrees C, with variable gas flow rates of 50 or 100 mL/min. Additionally, acid leaching with hydrofluoric (HF) and hydrochloric (HCl) acids ensured the synthesis of pure powders free from silica and uncoated Fe, confirming the chemical stability of the nanoparticles. The presence of graphene in all synthesized samples within these parameter ranges were confirmed by Raman spectroscopy. Phase identifications were carried out using X-ray diffraction (XRD) and Mo & uml;ssbauer spectroscopy, revealing the Fe and trace amount Fe3C as core phases. Transmission electron microscopy (TEM) revealed the core-shell structure of the nanoparticles with a few layers of graphene coatings. Based on the coercivity and magnetic saturation values obtained from vibrating sample magnetometry (VSM), synthesized core-shell nanoparticles exhibited soft magnetic properties (Ms = 22.4-33.5 emu/g, Hc = 82.3-278.3 Oe). Fe/Fe3C@C nanoparticles obtained under optimum conditions achieved very high H2 production rate (HPR = 54200 mLH2 gcat h- 1) values, with low activation energy (Ea = 20.08 kJ mol- 1) value, highlighting their potential as an efficient and promising candidate catalyst for industrial-scale H2 production via the NaBH4 methanolysis reaction. In addition, it was found that the Fe/Fe3C@C nanoparticles retained 48% and 71% of their initial activity after 5 consecutive cycles, as measured by the HPR and TOF values, respectively.Article Room-Temperature Synthesis of Refractory Borides: a Case Study on Mechanochemistry and Characterization of Mo-Borides and W-Borides(Elsevier Sci Ltd, 2025-06-01) Süzer, İlayda; Akbari, Amir; Kaya, Faruk; Mertdinç Ülküseven, Sıddıka; Derin, Bora; Öveçoğlu, M. Lütfi; Ağaoğulları, Duygu; Mertdinc-Ulkuseven, SiddikaMo-boride and W-boride powders were produced from native boron oxide, magnesium, and related metal oxide starting materials by mechanochemical synthesis (MCS) followed by an purification treatment. The reaction formation mechanisms and the products were predicted with the FactSageTM thermochemical simulation program. Different conditions were tested to determine the optimum synthesis parameters. MCS was conducted at stoichiometric ratios and different milling durations, using excess reactant amounts over the determined optimum time. After MCS, unwanted phases were removed by HCl acid leaching. Detailed phase analyses of the final powders were obtained by X-ray diffractometer (XRD), whereas detailed microstructure characterization was conducted by scanning electron microscope/energy dispersion spectrometer (SEM/EDS), transmission electron microscope (TEM) and particle size analyzer. Among the utilized parameters, the ideal composition chosen for Mo boride synthesis was 6 h milled and leached MoO3-100 wt% B2O3-50 wt% Mg (1.41 mu m), including alpha-MoB, beta-MoB, MoB2, Mo2B, Mo2B5, and Mo phases. For the synthesis of W boride, the proper composition was found as WO3-100 wt% B2O3-50 wt% Mg (0.37 mu m) containing W2B5, WB, beta-WB, WB4, W2B, and W phases after milling for 20 h and leaching. Besides, as a result of the oxidation resistance measurements at 700 and 800 degrees C, phases belonging to MoO2 and WO2 were found along with boride phases.Article Citation - WoS: 5Citation - Scopus: 4Powder metallurgy processing of seven/eight component multi-phase (HfTiZr-Mn/Mo/W/Cr/Ta)B<sub>2</sub> high entropy diboride ceramics(Elsevier, 2024-12-01) Suzer, Ilayda; Akbari, Amir; Ates, Semih; Bayrak, Kuebra Gurcan; Mertdinc-Ulkuseven, Siddika; Arisoy, C. Fahir; Agaogullari, Duygu; Öveçoğlu, M. LutfiThis study aims to show the possibility of synthesizing seven- and eight-component high entropy diboride (HEB) ceramics using high energy ball milling-assisted spark plasma sintering (SPS). Metal boride powders, synthesized in laboratory conditions from metal oxide-boron oxide-magnesium powder blends, were combined equimolarly as seven and eight components containing systems. Afterwards, hybridized powders were mechanically alloyed (MA) for 6 h and subjected to spark plasma sintering (SPS) at 2000 degrees C and under 30 MPa. Detailed phase analysis and physical, microstructural, and mechanical characterization of the samples were performed. in the sintered products, the main phase belongs to the HEB, and also low amounts of Hf/Zr oxides and secondary phases (W or Ti-rich) occurred. The highest hardness was observed at the (HfTiZrMoWCrTa)B-2 with 25 GPa, and the lowest hardness was seen at the (HfTiZrMnCrMoWTa)B2 with 17 GPa. Also, the highest wear resistance was calculated for the (HfTiZrMnCrMoTa)B-2 as 6.05 x 10(-7) mm(3)/Nm. Additionally, (HfTiZrMnMoWTa)B-2 and (HfTiZrMnMoCrTa)B-2 have the highest and lowest Archimedes' densities, with 7.94 g/cm(3) and 6.91 g/cm(3), respectively.