Ferric Phosphate Hydroxide Microstructures Affect Their Magnetic Properties

Uniformly sized and shape-controlled nanoparticles are important due to their applications in catalysis, electrochemistry, ion exchange, molecular adsorption, and electronics. Several ferric phosphate hydroxide (Fe₄(OH)₃(PO₄)₃) microstructures were successfully prepared under hydrothermal conditions. Using controlled variations in the reaction conditions, such as reaction time, temperature, and amount of hexadecyltrimethylammonium bromide (CTAB), the crystals can be grown as almost perfect hyperbranched microcrystals at 180 °C (without CTAB) or relatively monodisperse particles at 220 °C (with CTAB). The large hyperbranched structure of Fe₄(OH)₃(PO₄)₃ with a size of ∼19 μm forms with the “fractal growth rule” and shows many branches. More importantly, the magnetic properties of these materials are directly correlated to their size and micro/nanostructure morphology. Interestingly, the blocking temperature (T_B) shows a dependence on size and shape, and a smaller size resulted in a lower T_B. These crystals are good examples that prove that physical and chemical properties of nano/microstructured materials are related to their structures, and the precise control of the morphology of such functional materials could allow for the control of their performance.     

Synthesis of Co/MFe2O4 (M=Fe, Mn) core/shell nanocomposite particles

Monodispersed cobalt nanoparticles (NPs) with controllable size (8–14 nm) have been synthesized using thermal decomposition of dicobaltoctacarbonyl in organic solvent. The as-synthesized high magnetic moment (125 emu/g) Co NPs are dispersible in various organic solvents, and can be easily transferred into aqueous phase by surface modification using phospholipids. However, the modified hydrophilic Co NPs are not stable as they are quickly oxidized, agglomerated in buffer. Co NPs are stabilized by coating the MFe₂O₄ (M=Fe, Mn) ferrite shell. Core/shell structured bimagnetic Co/MFe₂O₄ nanocomposites are prepared with tunable shell thickness (1–5 nm). The Co/MFe₂O₄ nanocomposites retain the high magnetic moment density from the Co core, while gaining chemical and magnetic stability from the ferrite shell. Compared to Co NPs, the nanocomposites show much enhanced stability in buffer solution at elevated temperatures, making them promising for biomedical applications.     

Formulation of Quaternized Aminated Chitosan Nanoparticles for Efficient Encapsulation and Slow Release of Curcumin

An effective drug nanocarrier was developed on the basis of a quaternized aminated chitosan (Q-AmCs) derivative for the efficient encapsulation and slow release of the curcumin (Cur)-drug. A simple ionic gelation method was conducted to formulate Q-AmCs nanoparticles (NPs), using different ratios of sodium tripolyphosphate (TPP) as an ionic crosslinker. Various characterization tools were employed to investigate the structure, surface morphology, and thermal properties of the formulated nanoparticles. The formulated Q-AmCs NPs displayed a smaller particle size of 162 ± 9.10 nm, and higher surface positive charges, with a maximum potential of +48.3 mV, compared to native aminated chitosan (AmCs) NPs (231 ± 7.14 nm, +32.8 mV). The Cur-drug encapsulation efficiency was greatly improved and reached a maximum value of 94.4 ± 0.91%, compared to 75.0 ± 1.13% for AmCs NPs. Moreover, the in vitro Cur-release profile was investigated under the conditions of simulated gastric fluid [SGF; pH 1.2] and simulated colon fluid [SCF; pH 7.4]. For Q-AmCs NPs, the Cur-release rate was meaningfully decreased, and recorded a cumulative release value of 54.0% at pH 7.4, compared to 73.0% for AmCs NPs. The formulated nanoparticles exhibited acceptable biocompatibility and biodegradability. These findings emphasize that Q-AmCs NPs have an outstanding potential for the delivery and slow release of anticancer drugs.     

Facile deposition of gold nanoparticles on core–shell Fe3O4@polydopamine as recyclable nanocatalyst

A simple and green method for the controllable synthesis of core–shell Fe₃O₄ polydopamine nanoparticles (Fe₃O₄@PDA NPs) with tunable shell thickness and their application as a recyclable nanocatalyst support is presented. Magnetite Fe₃O₄ NPs formed in a one-pot process by the hydrothermal approach with a diameter of ∼240 nm were coated with a polydopamine shell layer with a tunable thickness of 15–45 nm. The facile deposition of Au NPs atop Fe₃O₄@PDA NPs was achieved by utilizing PDA as both the reducing agent and the coupling agent. The satellite nanocatalysts exhibited high catalytic performance for the reduction of p-nitrophenol. Furthermore, the recovery and reuse of the catalyst was demonstrated 8 times without detectible loss in activity. The synergistic combination of unique features of PDA and magnetic nanoparticles establishes these core–shell NPs as a versatile platform for potential applications.     

Characterization and Evaluation of Antimicrobial Potential of Trigonella incise (Linn) Mediated Biosynthesized Silver Nanoparticles

The goal of the research was to explore a new green method used to synthesize silver nanoparticles (Ag NPs) from an aqueous extract of Trigonella incise, which serves as a reducing and stabilizing agent. The obtained results showed an 85% yield of nanoparticles by using 2:5 (v/v) of 5% plant extract with a 0.5 M solution of AgNO₃. Different techniques were used to characterize the synthesized Ag NPs, including X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and UV–visible spectroscopy. The UV–visible spectra of green synthesized silver nanoparticles showed maximum absorption at a wavelength of 440 nm. The FT-IR studies revealed the stretching oscillation frequency of synthesized silver nanoparticles in the absorption band near 860 cm⁻¹. Similarly, the bending and stretching oscillation frequencies of the NH function group were assigned to the band in the 3226 cm⁻¹ and 1647 cm⁻¹ regions. The bending vibration of C-O at 1159 cm⁻¹ confirmed the carbonyl functional group that was also assigned to the small intensity band in the range of 2361 cm⁻¹. The X-ray diffraction analysis of Ag NPs revealed four distinct diffraction peaks at 2θ of 38°, 45°, 65° and 78°, corresponds to (111), (200), (220) and (311) of the face-centered cubic shape. The round shape morphology of Ag NPs with a mean diameter in the range 20–80 nm was analyzed via SEM images. Furthermore, the nanoparticles showed more significant antimicrobial activity against Salmonella typhi (S. typhi) and Staphylococcus aureus (S. aureus) with an inhibition zone of 21.5 mm and 20.5 mm at 6 μg/mL concentrations, respectively, once compared to the standard reference. At concentrations of 2 µg/mL and 4 µg/mL, all of the bacterial strains showed moderate activity, with inhibition zones ranging from 11 mm to 18.5 mm. Even at high concentrations of AgNPs, S. typhi showed maximum resistance. The best antifungal activity was observed by synthesized Ag NPs against Candida albicans (C. albicans) with 21 mm zone of inhibition, as compared to a standard drug which gives 22 mm of inhibition. Therefore, we conclude that the antibacterial and antifungal activities showed satisfactory results from the synthesized Ag NPs.     

Antibacterial,Antioxidant, Larvicidal and Anticancer Activities of Silver Nanoparticles Synthesized Using Extracts from Fruits of Lagerstroemia speciose and Flowers of Couroupita guianensis

The present study aimed to analyze the in vitro antibacterial, antioxidant, larvicidal and cytotoxicity properties of green synthesized silver nanoparticles (Ag NPs) using aqueous extracts from fruits of Lagerstroemia speciosa and flowers of Couropita guinensis. Synthesized Ag NPs were characterized using UV-DRS, FTIR, XRD, DLS, and High-Resolution SEM and TEM analyses. Absorption wavelength was observed at 386 nm by UV-DRS analysis and energy band gap was calculated as 3.24 eV. FTIR analysis showed the existence of various functional groups in the aqueous extract and in the NPs. DLS analysis showed the stability and particle size of the synthesized Ag NPs. SEM analysis revealed that Ag NPs are in a face centered cubic symmetry and spherical shape with a size of 23.9 nm. TEM analysis showed particle size as 29.90 nm. Ag NPs showed antibacterial activity against both Gram-positive and Gram-negative bacteria. DPPH scavenging trait of Ag NPs was ranging from 20.0 ± 0.2% to 62.4 ± 0.3% and observed significant larvicidal activity (LC50 at 0.742 ppm and LC90 at 6.061 ppm) against Culex quinquefasciatus. In vitro cytotoxicity activity of Ag NPs was also tested against human breast cancer (MCF-7) and fibroblast cells (L-929) and found that cells viabilities are ranging (500 to 25 µg/mL) from 52.5 ± 0.4 to 94.0 ± 0.7% and 53.6 ± 0.5 to 90.1 ± 0.8%, respectively. The synthesized Ag NPs have the potential to be used in the various biomedical applications.     

Investigations into the Antifungal,Photocatalytic, and Physicochemical Properties of Sol-Gel-Produced Tin Dioxide Nanoparticles

Transmission electron microscopy (TEM), atomic force microscopy (AFM), X-ray diffraction (XRD), energy dispersive X-ray (EDX), scanning electron microscopy (SEM), diffuse reflectance spectroscopy (DRS), and Fourier transform infrared (FTIR) spectroscopy were applied to evaluate the tin dioxide nanoparticles (SnO₂ NPs) amalgamated by the sol-gel process. XRD was used to examine the tetragonal-shaped crystallite with an average size of 26.95 (±1) nm, whereas the average particle size estimated from the TEM micrograph is 20.59 (±2) nm. A dose-dependent antifun3al activity was performed against two fungal species, and the activity was observed to be increased with an increase in the concentration of SnO₂ NPs. The photocatalytic activity of SnO₂ NPs in aqueous media was tested using Rhodamine 6G (Rh-6G) under solar light illumination. The Rh-6G was degraded at a rate of 0.96 × 10⁻² min for a total of 94.18 percent in 350 min.     

Biogenic Synthesis of NiO Nanoparticles Using Areca catechu Leaf Extract and Their Antidiabetic and Cytotoxic Effects

Nanoworld is an attractive sphere with the potential to explore novel nanomaterials with valuable applications in medicinal science. Herein, we report an efficient and ecofriendly approach for the synthesis of Nickel oxide nanoparticles (NiO NPs) via a solution combustion method using Areca catechu leaf extract. As-prepared NiO NPs were characterized using various analytical tools such as powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV-Visible spectroscopy (UV-Vis). XRD analysis illustrates that synthesized NiO NPs are hexagonal structured crystallites with an average size of 5.46 nm and a hexagonal-shaped morphology with slight agglomeration. The morphology, size, and shape of the obtained material was further confirmed using SEM and TEM analysis. In addition, as-prepared NiO NPs have shown potential antidiabetic and anticancer properties. Our results suggest that the inhibition of α-amylase enzyme with IC 50 value 268.13 µg/mL may be one of the feasible ways through which the NiO NPs exert their hypoglycemic effect. Furthermore, cytotoxic activity performed using NiO NPs exhibited against human lung cancer cell line (A549) proved that the prepared NiO NPs have significant anticancer activity with 93.349 μg/mL at 50% inhibition concentration. The biological assay results revealed that NiO NPs exhibited significant cytotoxicity against human lung cancer cell line (A549) in a dose-dependent manner from 0–100 μg/mL, showing considerable cell viability. Further, the systematic approach deliberates the NiO NPs as a function of phenolic extracts of A. catechu with vast potential for many biological and biomedical applications.     

The Catalytic Reduction of Nitroanilines Using Synthesized CuFe2O4 Nanoparticles in an Aqueous Medium

The primary objective of this research is to investigate the reduction of 4‐nitroaniline (4‐NA) and 2‐nitroaniline (2‐NA) using synthesized copper ferrite nanoparticles (NPs) via facile one‐step hydrothermal method as a heterogeneous nano‐catalyst. Nitroanilines were reduced in the presence and without the catalyst with a constant amount (100 mg) of reducing agent of sodium borohydride (NaBH₄) at room temperature in water to amino compounds. To characterize the functional groups, size, structure, and morphology of as‐prepared magnetic NPs, FTIR, XRD, SEM, and TEM were employed. The UV‐Vis spectrum was utilized to explore the catalytic effect of CuFe₂O₄. The outcomes revealed that the synthesized CuFe₂O₄ as a heterogeneous magnetic nano‐catalyst catalyzed the reduction of 4‐NA and 2‐NA significantly faster than other candidate catalysts. The outcomes demonstrated that the catalyst catalyzed 4‐nitroaniline to para‐phenylenediamine (p‐PDA) and 2‐nitroaniline to ortho‐phenylenediamine (o‐PDA) with a constant rate of 7.49×10⁻² s⁻¹ and 3.19×10⁻² s⁻¹, and conversion percentage of 96.5 and 95.6, in 40 s and 90 s, sequentially. Furthermore, the nanoparticles could be recovered by a magnetic separation method and reused for six consecutive cycles without remarkable loss of catalytic ability.     

Characterization,Antiplasmodial and Cytotoxic Activities of Green Synthesized Iron Oxide Nanoparticles Using Nephrolepis exaltata Aqueous Extract

The use of non-toxic synthesis of iron oxide nanoparticles (FeO NPs) by an aqueous plant extract has proven to be a viable and environmentally friendly method. Therefore, the present investigation is based on the FeO NPs synthesis by means of FeCl₃·6H₂O as a precursor, and the plant extract of Nephrolepis exaltata (N. exaltata) serves as a capping and reducing agent. Various techniques were used to examine the synthesized FeO NPs, such as UV-Visible Spectroscopy (UV-Vis), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and Energy Dispersive X-ray (EDX). The FT-IR studies were used to identify different photoactive biomolecules at 3285, 2928, 1415, 1170, and 600 cm⁻¹ in the wavenumber range from 4000 to 400 cm⁻¹, indicating the -OH, C-H, C-O, C-C, and M-O groups, respectively. The XRD examination exhibited crystallinity, and the average diameter of the particle was 16 nm. The spherical nature of synthesized FeO NPs was recognized by SEM images, while the elemental composition of nanoparticles was identified by an EDX spectrophotometer. The antiplasmodial activity of synthesized FeO NPs was investigated against Plasmodium parasites. The antiplasmodial property of FeO NPs was evaluated by means of parasite inhibitory concentration, which showed higher efficiency (62 ± 1.3 at 25 μg/mL) against Plasmodium parasite if compared to plant extracts and precursor. The cytotoxicity of FeO NPs was also assessed in human peripheral blood mononuclear cells (PBMCs) under in vitro conditions. The lack of toxic effects through FeO NPs keeps them more effective for use in pharmaceutical and medical applications.     

Research article green synthesis of zirconium oxide nanoparticles (ZrO2NPs) using Helianthus annuus seed and their antimicrobial effects

Monoclinic Zirconia (ZrO₂NPs) nanoparticles were successfully prepared by non-toxic and low-cost production using green synthesis analysis from the methanolic extract of Helianthus annuus (sunflower) seeds as the reducing agent. Mechanism of the chemical reaction has shown the reduction and which confirmed the formation of nanoparticles via chemical bonding in the IR spectrum at 502-498 ​cm^-1 ZrO₂ nanoparticles were characterized as sharp peak at 275 ​nm in the UV-Vis spectrum with 3.7eV in photon energy bandgap, it confirms the monoclinic crystal structure, as well as x-ray diffractometry, reveals zirconia crystallite is 40.59 ​nm. The internal morphology of crystal structure is exhibited by Scanning Electron Microscopy (SEM), and Transmission Electron Microscope (TEM). The stability of nanoparticles is represented in terms of zeta potential (-9.32 ​mV) and particle size distribution (~331 ​nm). Biosynthesized ZrO₂NPs were indicated as superior antimicrobial activity for biomedical applications.     

Magneto‐Plasmonic Janus Vesicles for Magnetic Field‐Enhanced Photoacoustic and Magnetic Resonance Imaging of Tumors

Magneto‐plasmonic Janus vesicles (JVs) integrated with gold nanoparticles (AuNPs) and magnetic NPs (MNPs) were prepared asymmetrically in the membrane for in vivo cancer imaging. The hybrid JVs were produced by coassembling a mixture of hydrophobic MNPs, free amphiphilic block copolymers (BCPs), and AuNPs tethered with amphiphilic BCPs. Depending on the size and content of NPs, the JVs acquired spherical or hemispherical shapes. Among them, hemispherical JVs containing 50 nm AuNPs and 15 nm MNPs showed a strong absorption in the near‐infrared (NIR) window and enhanced the transverse relaxation (T₂) contrast effect, as a result of the ordering and dense packing of AuNPs and MNPs in the membrane. The magneto‐plasmonic JVs were used as drug delivery vehicles, from which the release of a payload can be triggered by NIR light and the release rate can be modulated by a magnetic field. Moreover, the JVs were applied as imaging agents for in vivo bimodal photoacoustic (PA) and magnetic resonance (MR) imaging of tumors by intravenous injection. With an external magnetic field, the accumulation of the JVs in tumors was significantly increased, leading to a signal enhancement of approximately 2–3 times in the PA and MR imaging, compared with control groups without a magnetic field.     

Using reversed-phase liquid chromatography to monitor the sizes of Au/Pt core/shell nanoparticles

This paper describes the use of reversed-phase liquid chromatography (RPLC) to rapidly characterize Au/Pt core/shell nanoparticles (NPs) produced through seed-assisted synthesis. We monitored the sizes of Au/Pt core/shell NPs by using a porous silica-based RPLC column (pore size: ca. 100 nm) and 30 mM sodium dodecyl sulfate in deionized water as the mobile phase; the plot of the retention time with respect to the logarithm of the size of the Au NPs was linear (R² = 0.997) for diameters falling in the range from 5.3 to 40.1 nm; from five consecutive runs, the relative standard deviations of these retention times were less than 0.4%. We used the optimal separation conditions of the RPLC system to study the effects that the rate of addition of the reducing agent and the volumes of the seed, shell precursor metal ion, and reducing agent solutions had on the sizes of the Au/Pt core/shell NPs. A good correlation existed between the sizes of the Au/Pt core/shell NPs determined through RPLC and those determined using transmission electron microscopy. RPLC appears to be a useful technique for monitoring the sizes of NPs and nanomaterials in general.     

Building Nanocomposite Magnets by Coating a Hard Magnetic Core with a Soft Magnetic Shell

Controlling exchange coupling between hard magnetic and soft magnetic phases is the key to the fabrication of advanced magnets with tunable magnetism and high energy density. Using FePt as an example, control over the magnetism in exchange‐coupled nanocomposites of hard magnetic face‐centered tetragonal (fct) FePt and soft magnetic Co (or Ni, Fe₂C) is shown. The dispersible hard magnetic fct‐FePt nanoparticles are first prepared with their coercivity (H_c) reaching 33 kOe. Then core/shell fct‐FePt/Co (or Ni, Fe₂C) nanoparticles are synthesized by reductive thermal decomposition of the proper metal precursors in the presence of fct‐FePt nanoparticles. These core/shell nanoparticles are strongly coupled by exchange interactions and their magnetic properties can be rationally tuned by the shell thickness of the soft phase. This work provides an ideal model system for the study of exchange coupling at the nanoscale, which will be essential for building superstrong magnets for various permanent magnet applications in the future.     

Ranolazine-functionalized CuO NPs: efficient homogeneous and heterogeneous catalysts for reduction of 4-nitrophenol

In the present study copper oxide nanoparticles (CuO NPs) were synthesized using a hydrothermal method with ranolazine as a shape-directing agent. Ranolazine-functionalized CuO NPs were characterized by various analytical techniques such as scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD). The SEM pattern confirmed the morphology of ranolazine-functionalized CuO NPs with well-defined rice-like structures. FTIR spectroscopy confirmed the interaction between CuO NPs and ranolazine. The XRD analysis indicated that the structure of ranolazine-functionalized CuO NPs was monoclinic crystalline and the size ranged between 9 and 18 nm with an average particle size of 12 nm. The smaller size range of CuO NPs gave a large surface area that enhanced the efficiency of these catalysts employed for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) in the H ₂ O system. In homogeneous catalysis, results showed that 50 μL of CuO NPs was required in the presence of NaBH4 for 99% reduction of 4-NP in 240 s. On the other hand, for heterogeneous catalysis, 0.5 mg of CuO NPs was used in the presence of NaBH4 for 99% catalytic reduction of 4-NP to 4-AP in 320 s. The rate of reaction for homogeneous catalysis and heterogeneous catalysis was determined from the plots of In(Ct /C0) of 4-NP versus time (s), which showed good linearity with values of 1.3 × 10 ^-2 and 8.8 × 10 ^-3 s ^-1 . respectively. The high-quality catalytic efficiency, good reusability, nontoxic nature, and low cost are favorable properties of the synthesized CuO NPs for use as efficient catalysts for reduction of 4-AP to 4-NP in both homogeneous and heterogeneous media.     

Rare‐Earth Nanoparticles with Enhanced Upconversion Emission and Suppressed Rare‐Earth‐Ion Leakage

Upconversion emissions from rare‐earth nanoparticles have attracted much interest as potential biolabels, for which small particle size and high emission intensity are both desired. Herein we report a facile way to achieve NaYF₄:Yb,Er@CaF₂ nanoparticles (NPs) with a small size (10–13 nm) and highly enhanced (ca. 300 times) upconversion emission compared with the pristine NPs. The CaF₂ shell protects the rare‐earth ions from leaking, when the nanoparticles are exposed to buffer solution, and ensures biological safety for the potential bioprobe applications. With the upconversion emission from NaYF₄:Yb,Er@CaF₂ NPs, HeLa cells were imaged with low background interference.     

磁性荧光双功能复合纳米粒子Fe3O4@SiO2@ZrO2:Tb3+的合成和表征

通过原位反应合成法成功合成了一种新型水溶性的磁性荧光复合纳米粒子Fe₃O₄@SiO₂@ZrO₂:Tb³⁺,并通过扫描电子显微镜(SEM)、X射线粉末衍射仪(XRD)、红外光谱仪(FT-IR)、磁性测试仪和荧光(PL)光谱对其形貌、尺寸、相组成、磁性和荧光性能进行了表征。 结果表明,核(Fe₃O₄@SiO₂)壳(ZrO₂:Tb³⁺)结构组成的磁性荧光复合纳米粒子具有超顺磁性,其饱和磁化强度达到36 emu/g,并且在494 nm(⁵D₄→⁷F₆)、549 nm(⁵D₄→⁷F₅)、587 nm(⁵D₄→⁷F₄)和625 nm(⁵D₄→⁷F₃)处具有4个Tb³⁺特有的荧光发射光谱带峰值。 磁性荧光双功能的复合纳米粒子在生物医学领域具有潜在的应用价值。     

pH-Responsive Drug Delivery and Imaging Study of Hybrid Mesoporous Silica Nanoparticles

A system of pH-responsive and imaging nanocarriers was developed using mesoporous silica nanoparticles (MSNs), in which gadolinium (Gd) was doped through in situ doping (Gd₂O₃@MSN). Sodium alginate (SA) was attached to the surfaces of the amino groups of MSNs (NH₂-Gd₂O₃@MSN) through the electrostatic adsorption between the amino groups and the carboxyl groups with the formation of hybrid SA-Gd₂O₃@MSN nanoparticles (NPs). The SA-coated NPs were spherical or near-spherical in shape with an average size of nearly 83.2 ± 8.7 nm. The in vitro drug release experiments of a model rhodamine B (RhB) cargo were performed at different pH values. The result confirmed the pH-responsiveness of the nanocarriers. The results of the cytotoxicity studies indicated that the SA-Gd₂O₃@MSN NPs were not cytotoxic by themselves. The results of the in vivo safety evaluation and the hemolysis assay confirmed that the system is highly biocompatible. It is noteworthy that the T1 contrast of the system was significantly enhanced by the Gd, as indicated by the result of the MR imaging. This study confirms that the synthesized hybrid nanosystem is promising for pH-responsive drug delivery and MR imaging for cancer diagnosis and treatment.     

Study on the Synthesis of ZnO Nanoparticles Using Azadirachta indica Extracts for the Fabrication of a Gas Sensor

This paper compared the effects of A. indica plant proteins over chemical methods in the morphology of zinc oxide nanoparticles (ZnO NPs) prepared by a co-precipitation method, and ethanol sensing performance of prepared thin films deposited over a fluorene-doped tin oxide (FTO) bind glass substrate using spray pyrolysis technique. The average crystallite sizes and diameters of the grain-sized cluster ZnO NPs were 25 and (701.79 ± 176.21) nm for an undoped sample and 20 and (489.99 ± 112.96) nm for A. india dye-doped sample. The fourier transform infrared spectroscopy (FTIR) analysis confirmed the formation of the Zn–O bond at 450 cm⁻¹, and also showed the presence of plant proteins due to A. indica dye extracts. ZnO NPs films exhibited good response (up to 51 and 72% for without and with A. indica dye-doped extracts, respectively) toward ethanol vapors with quick response-recovery characteristics at a temperature of 250 °C for undoped and 225 °C for A. indica dye-doped ZnO thin films. The interaction of A. indica dye extracts helps to decrease the operating temperature and increased the response and recovery rates of the sensor, which may be due to an increase in the specific surface area, resulting in adsorption of more oxygen and hence high response results.     

SAXS studies of the thermally-induced fusion of diblock copolymer spheres: formation of hybrid nanoparticles of intermediate size and shape

Dilute dispersions of poly(lauryl methacrylate)–poly(benzyl methacrylate) (PLMA–PBzMA) diblock copolymer spheres (a.k.a. micelles) of differing mean particle diameter were mixed and thermally annealed at 150 °C to produce spherical nanoparticles of intermediate size. The two initial dispersions were prepared via reversible addition–fragmentation chain transfer (RAFT) dispersion polymerization of benzyl methacrylate in n-dodecane at 90 °C. Systematic variation of the mean degree of polymerization of the core-forming PBzMA block enabled control over the mean particle diameter: small-angle X-ray scattering (SAXS) analysis indicated that PLMA₃₉–PBzMA₉₇ and PLMA₃₉–PBzMA₂₉₄ formed well-defined, non-interacting spheres at 25 °C with core diameters of 21 ± 2 nm and 48 ± 5 nm, respectively. When heated separately, both types of nanoparticles regained their original dimensions during a 25–150–25 °C thermal cycle. However, the cores of the smaller nanoparticles became appreciably solvated when annealed at 150 °C, whereas the larger nanoparticles remained virtually non-solvated at this temperature. Moreover, heating caused a significant reduction in mean aggregation number for the PLMA₃₉–PBzMA₉₇ nanoparticles, suggesting their partial dissociation at 150 °C. Binary mixtures of PLMA₃₉–PBzMA₉₇ and PLMA₃₉–PBzMA₂₉₄ nanoparticles were then studied over a wide range of compositions. For example, annealing a 1.0% w/w equivolume binary mixture led to the formation of a single population of spheres of intermediate mean diameter (36 ± 4 nm). Thus we hypothesize that the individual PLMA₃₉–PBzMA₉₇ chains interact with the larger PLMA₃₉–PBzMA₂₉₄ nanoparticles to form the hybrid nanoparticles. Time-resolved SAXS studies confirm that the evolution in copolymer morphology occurs on relatively short time scales (within 20 min at 150 °C) and involves weakly anisotropic intermediate species. Moreover, weakly anisotropic nanoparticles can be obtained as a final copolymer morphology over a restricted range of compositions (e.g. for PLMA₃₉–PBzMA₉₇ volume fractions of 0.20–0.35) when heating dilute dispersions of such binary nanoparticle mixtures up to 150 °C. A mechanism involving both chain expulsion/insertion and micelle fusion/fission is proposed to account for these unexpected observations.

Dilute dispersions of poly(lauryl methacrylate)-poly(benzyl methacrylate) diblock copolymer spheres of differing mean diameter are mixed and thermally annealed at 150 °C to produce either spherical or non-spherical nanoparticles of intermediate size.