Browsing by Subject "Ball milling"

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Mechanochemical synthesis of antihistamine active pharmaceutical ingredient cinnarizine
(2025-02) Uzunlar, Rana
Mechanochemical methods are recognized as an appealing, greener methods for producing various molecular compounds. It has gained significance across multiple disciplines, such as chemistry and material science, due to its eco-conscious nature, allowing it to be performed without solvents or with only minimal amounts of solvent. Mechanochemical approaches also stand out as a prominent synthetic approach, enabling efficient and rapid processes compared to conventional synthesis approaches. Their synthetic capabilities through a range of solid-state transformations, yielding diverse compounds including inorganic, organic, polymeric, metal-organic-framework, and organometallic materials, have been proved over the decades. Yet another captivating illustration of mechanochemical reactions is seen in the effective pharmaceutical drugs and medicine preparations. This upward trajectory is evident in the increasing adoption of solid-state methodologies within pharmaceutical material science. These mechanochemical attempts are branched under a recently emerging field, namely “medicinal mechanochemistry,” and have been quite efficient in the synthesis of active pharmaceutical ingredients (APIs) and drugs such as paracetamol. They are also employed for the alteration of APIs through processes like the formation of salts or cocrystals. However, a synthetic pathway of many APIs in which mechanochemistry is used as a bimolecular solid-state reaction initiator, is not available yet. Here, we show that utilizing ball milling of the reactants through a simple SN2 reaction a first generation H1 antihistaminic API, cinnarizine, can be synthesized in moderate yields (25-50%). The milling and reaction parameters are explored in terms of product yields and a comparison with a conventional synthetic route is also provided. Milling produces cinnarizine in 1-60 minutes, compared to conventional organic synthesis, 4-24 hours. This route brings an innovative perspective to synthesizing widely used APIs in medicinal mechanochemistry and its potential applications in industry.
Open Access
Phase transformation during mechano-synthesis of nanocrystalline/amorphous Fe–32Mn–6Si alloys
(Elsevier, 2013) Amini, R.; Shamsipoor, A.; Ghaffari, M.; Alizadeh, M.; Okyay, Ali Kemal
Mechano-synthesis of Fe-32Mn-6Si alloy by mechanical alloying of the elemental powder mixtures was evaluated by running the ball milling process under an inert argon gas atmosphere. In order to characterize the as-milled powders, powder sampling was performed at predetermined intervals from 0.5 to 192 h. X-ray florescence analyzer, X-ray diffraction, scanning electron microscope, and high resolution transmission electron microscope were utilized to investigate the chemical composition, structural evolution, morphological changes, and microstructure of the as-milled powders, respectively. According to the results, the nanocrystalline Fe-Mn-Si alloys were completely synthesized after 48 h of milling. Moreover, the formation of a considerable amount of amorphous phase during the milling process was indicated by quantitative X-ray diffraction analysis as well as high resolution transmission electron microscopy image and its selected area diffraction pattern. It was found that the α-to-γ and subsequently the amorphous-to-crystalline (especially martensite) phase transformation occurred by milling development.
Open Access
Quantitative phase evolution during mechano-synthesis of Ti-Ni-Cu shape memory alloys
(Elsevier, 2012-05-29) Amini, R.; Alijani, F.; Ghaffari, M.; Alizadeh, M.; Okyay, Ali Kemal
Ti-41Ni-9Cu shape memory alloy was synthesized by mechanical alloying of pure elemental Ti, Ni, and Cu powders using high-energy ball milling. The qualitative and quantitative phase analyses of the as-milled powders were done by X-ray diffraction (XRD) using Rietveld refinement and the alloys microstructure was studied by scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). Concerning the results, by milling evolution, the dissolution of the primary materials occurred at different rates and a considerable amount of the amorphous phase as well as B19′-martensite and B2-austenite was created. The formation of Ni solid solution was also evidenced prior to its dissolution. It was found that at sufficient milling time, the mechano-crystallization of the amorphous phase occurred and at the end of milling, the B19′-martensite is the dominant phase of the structure.
Open Access
Tuning the nonlinear optical properties of Cu2SnS3 nanoparticles using alkali tomes doping
(Springer New York LLC, 2024-02-02) Gundogdu, Yasemin; Houimi, Amina; Gezgin, Serap Yigit; Kilic, Hamdi Sukur
In this study, rubidium (Rb), cesium (Cs), and sodium (Na) alkali materials doped into CTS (Cu2SnS3), which is frequently used in semiconductor technology, were prepared to synthesize via ball milling method. CTS and Rb-, Cs, and Na-doped target crystal structures were recorded via XRD, and the surface images were monitored by SEM. Used raw solid powder materials were purchased and prepared to form targets in a laboratory environment, and the generated targets were placed in glass vessel to produce nanoparticles in ethanol using femtosecond laser ablation technique. In the SEM images of CTS, it was seen that the average nanoparticle size in the liquid was around 57 nm. The produced nanoparticles in liquid were analyzed with linear optical properties by UV-Vis absorption spectroscopy and nonlinear optical properties with z-scan technique. Numerical values of nonlinear absorption coefficients, refractive index, and third-order susceptibility were calculated and given to be in the order of 10(-16) W/cm(2), 10(-10) W/cm, and 10(-13) esu ratios, respectively. The study also includes important results on the use of the results obtained in nonlinear photonic technology.