Simultaneous electrochemical determination of uric acid and hypoxanthine at a TiO₂/graphene quantum dot-modified electrode

• Vu Ngoc Hoang,
• Dang Thi Ngoc Hoa,
• Nguyen Quang Man,
• Le Vu Truong Son,
• Le Van Thanh Son,
• Vo Thang Nguyen,
• Le Thi Hong Phong,
• Ly Hoang Diem,
• Kieu Chan Ly,
• Ho Sy Thang and
• Dinh Quang Khieu

Beilstein J. Nanotechnol. 2024, 15, 719–732, doi:10.3762/bjnano.15.60

• , titanium alkoxides and halides are extensively used as precursors [20][21]. Because of their high reactivity, a complicate control over the reaction conditions is critical to achieve the desired crystalline structures and morphology [22]. Recently, a synthesis using stable water-soluble titanium complexes

• has been developed to overcome the disadvantages of these precursors and to easily obtain fine titania particles with a controlled shape [23]. The synthesis of TiO2/GQDs from water-soluble titanium complexes is expected to form a homogeneous suspension that is convenient for developing modified

• with 0.1 M HCl and distilled water until a supernatant with neutral pH was obtained. The solid was dried at 80 °C for 2 h. This product was then mixed with 30 mL of H2O2 (35%, d = 1.11 g·cm3) at 90 °C under magnetic stirring for 1 h to obtain a clear yellow solution of peroxo titanium complexes. The

Elastic modulus of β-Ga₂O₃ nanowires measured by resonance and three-point bending techniques

• Annamarija Trausa,
• Sven Oras,
• Sergei Vlassov,
• Mikk Antsov,
• Tauno Tiirats,
• Andreas Kyritsakis,
• Boris Polyakov and
• Edgars Butanovs

Beilstein J. Nanotechnol. 2024, 15, 704–712, doi:10.3762/bjnano.15.58

• with Au nanoparticles (NPs, 100 nm of diameter, water suspension, Alfa Aesar) were positioned in a lower-temperature region 10 cm away from the furnace centre. Au NPs served as catalysts for the vapour–liquid–solid (VLS) growth mechanism. The reactor was heated to 1010 °C (high-temperature zone) under

Gold nanomakura: nanoarchitectonics and their photothermal response in association with carrageenan hydrogels

• Nabojit Das,
• Vikas,
• Akash Kumar,
• Sanjeev Soni and
• Raja Gopal Rayavarapu

Beilstein J. Nanotechnol. 2024, 15, 678–693, doi:10.3762/bjnano.15.56

• hydrogels) is shown in Figure 8. The net temperature rise of the gold nanomakura suspension and deionized water during visible broadband irradiation ON (heating) and OFF (cooling) for 1200 seconds each, measured using a “K-type” thermocouple is shown in Figure 8. Figure 8a shows the heating and cooling of

• gold nanoparticle suspensions of CTAB-AuNM, MTAB-AuNM, and DTAB-AuNM, respectively, whereas Figure 8b shows heating and cooling of DTAB-AuNR and CTAB-AuNR, respectively. From Figure 8a, it was observed that the temperature of deionized water reached up to ≈3 °C under irradiation with a light source

• nitrate (AgNO3, Merck), ʟ-(+)-ascorbic acid (Sigma-Aldrich), and sodium borohydride (NaBH4, Sigma-Aldrich). Prior to synthesis, all the glassware was cleaned with aqua regia and further rinsed with double-distilled (DD) water. Double-distilled water was used throughout the experiments. Methodology

Functional fibrillar interfaces: Biological hair as inspiration across scales

• Guillermo J. Amador,
• Brett Klaassen van Oorschot,
• Caiying Liao,
• Jianing Wu and
• Da Wei

Beilstein J. Nanotechnol. 2024, 15, 664–677, doi:10.3762/bjnano.15.55

• providing insulation (Figure 2A), prevent the penetration of water through hierarchical superhydrophobicity (Figure 2B), or provide protection from predators or disease vectors through mechanical interactions (Figure 2C). Thermoregulation Regarding thermal regulation, mammals have evolved certain traits

• morphology, including shape and packing density, differ from terrestrial mammals in order to maintain a trapped air layer within the arrays of hair when submerged in water [30]. Hairs of aquatic animals have been found to be flatter, shorter, and packed in higher densities. Additionally, mammals that also

• preventing water from spreading; thus, they exhibit low wettability. In order to achieve superhydrophobicity, surfaces should have structural hierarchy and be composed of materials with low surface energy. The classic example of such a surface in nature is the lotus leaf [39], which possesses wax-covered

Laser synthesis of nanoparticles in organic solvents – products, reactions, and perspectives

• Theo Fromme,
• Sven Reichenberger,
• Katharine M. Tibbetts and
• Stephan Barcikowski

Beilstein J. Nanotechnol. 2024, 15, 638–663, doi:10.3762/bjnano.15.54

• 23284, USA 10.3762/bjnano.15.54 Abstract Laser synthesis and processing of colloids (LSPC) is an established method for producing functional and durable nanomaterials and catalysts in virtually any liquid of choice. While the redox reactions during laser synthesis in water are fairly well understood

• mechanisms of organic liquid decomposition and carbon shell formation are highlighted and discussed regarding current challenges and future perspectives of LSPC using organic liquids instead of water. Keywords: alloy; photochemistry; pyrolysis; radicals; surface chemistry; Introduction Since the first

• liquid. Hereby, in ideal cases that fulfill the “purity” claim, the liquid shall not be degraded into reaction products that may adsorb to the nanoparticle surface as they are difficult to remove afterward. Here, water is less critical than organic solvents, where liquid hydrocarbons and other species

Exfoliation of titanium nitride using a non-thermal plasma process

• Priscila Jussiane Zambiazi,
• Dolores Ribeiro Ricci Lazar,
• Larissa Otubo,
• Rodrigo Fernando Brambilla de Souza,
• Almir Oliveira Neto and
• Cecilia Chaves Guedes-Silva

Beilstein J. Nanotechnol. 2024, 15, 631–637, doi:10.3762/bjnano.15.53

• flow. The arc was generated between a 316 L steel electrode and another electrode composed of graphite. The process lasted 60 min. Subsequently, the resultant material was collected, rinsed in a 1:1 mixture of water and isopropanol, and decanted for 24 h. Then, the liquid phase was filtered using a

Comparative analysis of the ultrastructure and adhesive secretion pathways of different smooth attachment pads of the stick insect Medauroidea extradentata (Phasmatodea)

• Julian Thomas,
• Stanislav N. Gorb and
• Thies H. Büscher

Beilstein J. Nanotechnol. 2024, 15, 612–630, doi:10.3762/bjnano.15.52

• particles together into larger complexes for easier removal [25][26]. It can also improve attachment to surfaces with different surface chemistry by mediating between the two surfaces in contact [27][28]. The lipid-containing pad secretion protects the insect from additional water loss through the thin

• but mostly contains water-soluble and lipid-soluble substances [31][32][33][34][35] creating lipid droplets in an aqueous fluid [27][36] or hydrophilic nanodroplets embedded in an oily continuous phase [23][37]. Additionally, the tarsal secretion could be a mixture of multiple substances that are

• tarsomeres were fixed in 2.5% glutaraldehyde in (pH 7.4) phosphate-buffered saline (PBS) for 24 h, washed two times in PBS for 30 min each, fixed in 1% aqueous OsO4 for 1 h, and washed two times in double-distilled water, for 30 min each. After fixation, the samples were dehydrated using an ascending ethanol

Radiofrequency enhances drug release from responsive nanoflowers for hepatocellular carcinoma therapy

• Yanyan Wen,
• Ningning Song,
• Yueyou Peng,
• Weiwei Wu,
• Qixiong Lin,
• Minjie Cui,
• Rongrong Li,
• Qiufeng Yu,
• Sixue Wu,
• Yongkang Liang,
• Wei Tian and
• Yanfeng Meng

Beilstein J. Nanotechnol. 2024, 15, 569–579, doi:10.3762/bjnano.15.49

• , China). Ultrapure water was obtained from a Laibopate purification system (Changchun Lab Partner Technology Development Co., Ltd., Changchun, China) and used in all experiments. Human hepatocellular carcinoma cells (Huh-7 cells) and Dulbecco’s modified Eagle’s medium (DMEM, ZQ-101) were purchased from

• madded is the mass of CUR added to prepare the NPs, msupernatant is the mass of CUR in the supernatant, and mNPs is the mass of the preparation after the completion of the NPs synthesis. Synthesis of CUR-Fe@MnO2 NFs The prepared CUR-Fe NPs (9 mg) were suspended in 30 mL of deionized water and sonicated

• with KMnO4 powder (1.5 mg) for 10 min at room temperature to ensure that the NPs were well suspended. Then, MES (2.7 mg) and PEG (0.3 mg) were dispersed into 5 mL of water and added to the mixture dropwise for 5 min with ultrasonication (100 W, 40 kHz) at room temperature for 30 min [34]. The obtained

On the additive artificial intelligence-based discovery of nanoparticle neurodegenerative disease drug delivery systems

• Shan He,
• Julen Segura Abarrategi,
• Harbil Bediaga,
• Sonia Arrasate and
• Humberto González-Díaz

Beilstein J. Nanotechnol. 2024, 15, 535–555, doi:10.3762/bjnano.15.47

• = [Dd1, Dd2, Dd3] in order to define the chemical structure of the NDD compound. Specifically, we used two types of molecular descriptor for the i-th compound, namely Dd1 = logarithm of the n-octanol/water partition coefficient (LOGPi) and Dd2 = topological polar surface area (PSAi). The detailed

• of potential bioactive molecules [73]. These structural descriptors are Dd1 = logarithm of the n-octanol/water partition coefficient (LOGPi) and Dd2 = topological polar surface area (PSAi). In contrast, the cytotoxicity NP vector lists the elements as Dnk = [Dn1, Dn2, Dn3, Dn4, Dn5, Dn6, Dn7, Dn8

• octanol/water partition coefficient), Dn13 = ALOGP2coat (squared Ghose–Crippen octanol/water partition coefficient (logP^2)), Dn14 = SAtotcoat (total surface area from P_VSA-like descriptors), Dn15 = SAacccoat (surface area of acceptor atoms from P_VSA-like descriptors), Dn16 = SAdoncoat (surface area of

Cholesterol nanoarchaeosomes for alendronate targeted delivery as an anti-endothelial dysfunction agent

• Horacio Emanuel Jerez,
• Yamila Roxana Simioni,
• Kajal Ghosal,
• Maria Jose Morilla and
• Eder Lilia Romero

Beilstein J. Nanotechnol. 2024, 15, 517–534, doi:10.3762/bjnano.15.46

• plates by covering them with 10% formaldehyde in PBS for 15 min at room temperature (RT). After removing the fixing buffer carefully, cells were covered with fresh ORO working solution (6 mL of 5 mg/mL ORO in isopropanol stock solution) and 4 mL of distilled water filtered through a 3 μm pore size filter

• ) for at least 1 h at RT. Then cells were rinsed several times carefully with distilled water and allowed to air-dry. Cells were visualized under an optical microscope Olympus BX51 equipped with an Oan Olympus DP-70 camera (Olympus, Japan). The designation of a macrophage as FC required positive ORO

Aero-ZnS prepared by physical vapor transport on three-dimensional networks of sacrificial ZnO microtetrapods

• Veaceslav Ursaki,
• Tudor Braniste,
• Victor Zalamai,
• Emil Rusu,
• Vladimir Ciobanu,
• Vadim Morari,
• Daniel Podgornii,
• Pier Carlo Ricci,
• Rainer Adelung and
• Ion Tiginyanu

Beilstein J. Nanotechnol. 2024, 15, 490–499, doi:10.3762/bjnano.15.44

• pollutants from the atmosphere and from water, in other catalytic processes, including photocatalytic water splitting, in energy production and storage, in microfluidic systems, in drug delivery and other biomedical applications, in sensing, in electronic, photoelectronic, optoelectronic and nanophotonic

• properties when compressed against water was fabricated using HVPE of CdS on sacrificial ZnO microtetrapods through the simultaneous or subsequent transformation of CdS into ZnS and the removal of the sacrificial ZnO crystals [16]. Self-propelled liquid marbles have been demonstrated on the basis of this

Photocatalytic degradation of methylene blue under visible light by cobalt ferrite nanoparticles/graphene quantum dots

• Vo Chau Ngoc Anh,
• Le Thi Thanh Nhi,
• Le Thi Kim Dung,
• Dang Thi Ngoc Hoa,
• Nguyen Truong Son,
• Nguyen Thi Thao Uyen,
• Nguyen Ngoc Uyen Thu,
• Le Van Thanh Son,
• Le Trung Hieu,
• Tran Ngoc Tuyen and
• Dinh Quang Khieu

Beilstein J. Nanotechnol. 2024, 15, 475–489, doi:10.3762/bjnano.15.43

• hydrolyse the starch. Then, the mixture was transferred to a 100 mL Teflon-lined autoclave and heated at 200 °C for 24 h. After hydrolysis, the product was cooled to room temperature. The brown solid was centrifuged, washed several times with distilled water, and calcinated at 700 °C for 3 h to obtain

• ratio of 2:1:4.5:540 was dissolved in a flask and heated to 80–85 °C for 1 h to hydrolyse the starch. Then, the mixture was transferred to a 100 mL Teflon-line autoclave and heated at 140, 180, and 200 °C for 24 h. The brown solid was centrifuged, washed several times with distilled water, and dried at

• , available to react with H2O to produce •OH radicals. The electrons in the CB band directly reduce MB to its degradation products or interact with oxygen in the aqueous solution to form peroxy anion radicals (). A part of h+ oxidizes water to form hydroxyl radicals (•OH), or it can oxidize directly MB to its

Fabrication of nanocrystal forms of ᴅ-cycloserine and their application for transdermal and enteric drug delivery systems

• Hsuan-Ang Tsai,
• Tsai-Miao Shih,
• Theodore Tsai,
• Jhe-Wei Hu,
• Yi-An Lai,
• Jui-Fu Hsiao and
• Guochuan Emil Tsai

Beilstein J. Nanotechnol. 2024, 15, 465–474, doi:10.3762/bjnano.15.42

• improve the bioavailability. In this study, for the first time, DCS, a highly water-soluble compound, has formed nanocrystals and this was confirmed by scanning electronic microscopy and X-ray powder diffraction. Furthermore, DCS nanocrystals were applied to several formulations to test their stability

• , matrix, and microneedle systems [24][25][26]. In addition, enteric-coated solid dosage forms for oral administration have shown significant improvement in providing better absorption and targeted delivery [27][28]. In this study, due to high water solubility of DCS (Log P = −1.72) and difficulty to

• dissolving DCS in organic solvents to fabricate the matrix patch formulation, only reservoir patch formulations of DCS in well-suspended (DCS nanocrystals) or emulsified (DCS water solution) forms were feasible to evaluate transdermal drug delivery. Coating drugs with pharmaceutically biocompatible enteric

Sidewall angle tuning in focused electron beam-induced processing

• Sangeetha Hari,
• Willem F. van Dorp,
• Johannes J. L. Mulders,
• Piet H. F. Trompenaars,
• Pieter Kruit and
• Cornelis W. Hagen

Beilstein J. Nanotechnol. 2024, 15, 447–456, doi:10.3762/bjnano.15.40

• by etching with water and it is shown, using transmission electron microscopy imaging, that the sidewall angle can be tuned from outward to inward by controlling the etch position on the sidewall. A surprising under-etching due to the emission of secondary electrons from the deposit was observed

• , which was not indicated by a simple model based on etching. An analytical model was developed to include continued etching once the deposit has been removed at the exposed pixel. At this stage the secondary electrons from the substrate then cause the adsorbed water molecules to become effective in

• qualitative agreement with the experimental observations. As a demonstration, the proposed method is applied to a carbon FEBID structure whose sidewall is etched using FEBIE with water in an SEM, using SE signal monitoring to determine when a vertical sidewall has been achieved. Results Sidewall slope

Potential of a deep eutectic solvent in silver nanoparticle fabrication for antibiotic residue detection

• Le Hong Tho,
• Bui Xuan Khuyen,
• Ngoc Xuan Dat Mai and
• Nhu Hoa Thi Tran

Beilstein J. Nanotechnol. 2024, 15, 426–434, doi:10.3762/bjnano.15.38

• stirring, the obtained Ag NPs-DES were washed with DI water several times, and the pellets were re-dispersed in DI water for further use. The Ag NPs-DES thin film was prepared following the procedure for self-assembly monolayer construction. A clean glass substrate was treated with oxygen plasma to form

Insect attachment on waxy plant surfaces: the effect of pad contamination by different waxes

• Elena V. Gorb and
• Stanislav N. Gorb

Beilstein J. Nanotechnol. 2024, 15, 385–395, doi:10.3762/bjnano.15.35

• septempunctata (L.) (Coleoptera, Coccinellidae) on microporous substrates able to absorb both polar (water) and non-polar (oil) fluids clearly showed a strong reduction of the attachment force on these substrates compared to reference smooth solid substrates [24]. The latter result has been explained by

On the mechanism of piezoresistance in nanocrystalline graphite

• Sandeep Kumar,
• Simone Dehm and
• Ralph Krupke

Beilstein J. Nanotechnol. 2024, 15, 376–384, doi:10.3762/bjnano.15.34

• flexible glass was preferred for the Raman measurements because the spectra of NCG cannot be resolved on PET as a result of a strong Raman signal of the substrate itself. The 50 μm thick flexible glass was acquired from Schott. The glass loses its flexibility at 600 °C and also in water [23]. To keep the

• flexibility, the NCG film was grown on both sides of the glass substrate. There are three reasons for that. First, the negative thermal expansion coefficient of NCG prevents the release of stress initially present in the glass [25]. Second, the film protects the glass from any corrosion from water if the

• etching of SiO2. Using a clean glass wafer, the NCG/PMMA film was transferred from the NaOH solution to a clean water beaker and allowed to float on the top. The cleaning was repeated three times to ensure the no residues of NaOH remained on the NCG film. The film was then removed from the water using a

Controllable physicochemical properties of WO_x thin films grown under glancing angle

• Rupam Mandal,
• Aparajita Mandal,
• Alapan Dutta,
• Rengasamy Sivakumar,
• Sanjeev Kumar Srivastava and
• Tapobrata Som

Beilstein J. Nanotechnol. 2024, 15, 350–359, doi:10.3762/bjnano.15.31

• thin films were deposited on ultrasonically cleaned p-Si (100) and soda lime glass substrates of 1 × 1 cm2 dimension using a rf magnetron sputtering setup (Excel Instruments). Trichloroethylene, propanol, acetone, and DI water were used to carry out ultrasonication of the substrates for removing

Nanomedicines against Chagas disease: a critical review

• Maria Jose Morilla,
• Kajal Ghosal and
• Eder Lilia Romero

Beilstein J. Nanotechnol. 2024, 15, 333–349, doi:10.3762/bjnano.15.30

• soluble drugs are those whose solubility is below 1 mg/mL over the physiological pH range and the BNZ solubility in distilled water or simulated gastric and enteric fluids oscillates between 0.2 and 0.4 mg/mL [29][30], BNZ is considered a poorly soluble drug. Some authors classify BNZ as a class-II drug

• self-nanoemulsified drug delivery systems (SNEDDSs). SNEEDSs provide a pediatric liquid formulation of BNZ, which is only marketed as solid tablets. SNEDDSs are isotropic mixtures of oil, surfactants, and co-surfactants that form submicrometer-droplet emulsions under agitation in water or

• nanoparticulate vaccine is the anti-malarial Mosquirix™ (RTS, S/AS01), recommended by the World Health Organization in four doses for children in 2021. Mosquirix™ employs a liposome-based adjuvant, AS01 (GlaxoSmithKline) [103] that contains 3-O-desacyl-monophosphoryl lipid A and QS-21, a water-soluble triterpene

Comparative electron microscopy particle sizing of TiO₂ pigments: sample preparation and measurement

• Ralf Theissmann,
• Christopher Drury,
• Markus Rohe,
• Thomas Koch,
• Jochen Winkler and
• Petr Pikal

Beilstein J. Nanotechnol. 2024, 15, 317–332, doi:10.3762/bjnano.15.29

• application laboratory in Waldbronn, Germany, and the particle counting threshold was set at 30 nm. The samples were first intensively dispersed by ultrasonication in a polyphosphate solution in water (562 J/mL, 2.5% pigment, 2% polyphosphate) one day before measurement. The energy of 562 J/mL was chosen

• as in [11], differences in method M1 with respect to [11][21] are described below. These three methods differ substantially in all their characteristic steps, including ultrasonic bath dispersion in water, dry dispersion in a solid polymer, and the powdering onto a sticky sample stub without

• KRONOS INT. Inc., Research Services, involving the dispersion of 2.5% TiO2 in a polyphosphate solution in water (with 2% polyphosphate for stabilisation). Dispersion was performed by an ultrasonic finger (13 mm tip) for 5 min at 250 W and 60% amplitude, equivalent to 562 J/mL. It is worth noting that

Exploring the relationships between physiochemical properties of nanoparticles and cell damage to combat cancer growth using simple periodic table-based descriptors

• Joyita Roy and
• Kunal Roy

Beilstein J. Nanotechnol. 2024, 15, 297–309, doi:10.3762/bjnano.15.27

• a vital role in adhesion to the hydro–water interface and solid surfaces, providing an idea about the viability and permeability of the cell membrane under stress. As most of the cell surface carries a negative charge, metals with higher zeta potential can easily enter the cell and increase the

Determining by Raman spectroscopy the average thickness and N-layer-specific surface coverages of MoS₂ thin films with domains much smaller than the laser spot size

• Felipe Wasem Klein,
• Jean-Roch Huntzinger,
• Vincent Astié,
• Damien Voiry,
• Romain Parret,
• Houssine Makhlouf,
• Sandrine Juillaguet,
• Jean-Manuel Decams,
• Sylvie Contreras,
• Périne Landois,
• Ahmed-Azmi Zahab,
• Jean-Louis Sauvajol and
• Matthieu Paillet

Beilstein J. Nanotechnol. 2024, 15, 279–296, doi:10.3762/bjnano.15.26

Vinorelbine-loaded multifunctional magnetic nanoparticles as anticancer drug delivery systems: synthesis, characterization, and in vitro release study

• Zeynep Özcan and
• Afife Binnaz Hazar Yoruç

Beilstein J. Nanotechnol. 2024, 15, 256–269, doi:10.3762/bjnano.15.24

• three times with distilled water, and the PDA/Fe3O4 NPs were dried in a vacuum oven at 55 °C. Surface functionalization of PDA/Fe3O4 nanoparticles with SH-PEG For the surface modification process with SH-PEG, 50 mg of PDA/Fe3O4 NPs were added to 50 mL of Tris-HCl solution. Then, 100 mg of thiol

• particles were removed by washing with distilled water. The PEGylation PDA/Fe3O4 NPs were then dried in a vacuum oven at 45 °C. The PDA-coated Fe3O4 nanoparticles were modified with SH-PEG to facilitate their accumulation in tumour regions. In similar studies, the conjugation of SH-PEG onto the surface of

• was separated with the assistance of a magnet, followed by three thorough rinses with distilled water. All wash supernatants were collected to measure the VNB loading content based on UV–vis spectrophotometry. The resulting nanostructure underwent vacuum drying at 45 °C. The loading entrapment

Multiscale modelling of biomolecular corona formation on metallic surfaces

• Parinaz Mosaddeghi Amini,
• Ian Rouse,
• Julia Subbotina and
• Vladimir Lobaskin

Beilstein J. Nanotechnol. 2024, 15, 215–229, doi:10.3762/bjnano.15.21

• analogues (SCA) within the system [33][34]. The AMBER force field is a widely recognized and extensively validated force field that provides accurate descriptions of molecular systems [35]. We evaluated the short-range PMFs between 22 SCAs and an Al slab in a solvent environment comprising water and salt

• water density profiles obtained from MD simulations for the slab–water system in the context of Al surfaces revealed characteristics that were previously observed for other simulated metallic surfaces [2][28]. The profiles exhibited two distinct regions with elevated water density located approximately

• 0.15–0.18 nm and 0.42–0.48 nm away from the aluminum surface. These regions corresponded to the first and second water layers adjacent to the metal surface, respectively (as depicted in Supporting Information File 1, Figure S1). Further examination of the ion density profiles indicated the presence of

Ion beam processing of DNA origami nanostructures

• Leo Sala,
• Agnes Zerolová,
• Violaine Vizcaino,
• Alain Mery,
• Alicja Domaracka,
• Hermann Rothard,
• Philippe Boduch,
• Dominik Pinkas and
• Jaroslav Kocišek

Beilstein J. Nanotechnol. 2024, 15, 207–214, doi:10.3762/bjnano.15.20

• additional MilliQ water to reach the desired final volume (usually 100 μL for a standard synthesis). We used a higher excess of the staple strands because of the already long storage time of our staple stock solution [34]. The mixture was then annealed to 90 °C and slowly cooled down at a rate of −7 °C·min−1