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1.  Simulating Magnetic Nanoparticle Behavior in Low-field MRI under Transverse Rotating Fields and Imposed Fluid Flow 
In the presence of alternating-sinusoidal or rotating magnetic fields, magnetic nanoparticles will act to realign their magnetic moment with the applied magnetic field. The realignment is characterized by the nanoparticle’s time constant, τ. As the magnetic field frequency is increased, the nanoparticle’s magnetic moment lags the applied magnetic field at a constant angle for a given frequency, Ω, in rad/s. Associated with this misalignment is a power dissipation that increases the bulk magnetic fluid’s temperature which has been utilized as a method of magnetic nanoparticle hyperthermia, particularly suited for cancer in low-perfusion tissue (e.g., breast) where temperature increases of between 4°C and 7°C above the ambient in vivo temperature cause tumor hyperthermia. This work examines the rise in the magnetic fluid’s temperature in the MRI environment which is characterized by a large DC field, B0. Theoretical analysis and simulation is used to predict the effect of both alternating-sinusoidal and rotating magnetic fields transverse to B0. Results are presented for the expected temperature increase in small tumors (~1 cm radius) over an appropriate range of magnetic fluid concentrations (0.002 to 0.01 solid volume fraction) and nanoparticle radii (1 to 10 nm). The results indicate that significant heating can take place, even in low-field MRI systems where magnetic fluid saturation is not significant, with careful The goal of this work is to examine, by means of analysis and simulation, the concept of interactive fluid magnetization using the dynamic behavior of superparamagnetic iron oxide nanoparticle suspensions in the MRI environment. In addition to the usual magnetic fields associated with MRI, a rotating magnetic field is applied transverse to the main B0 field of the MRI. Additional or modified magnetic fields have been previously proposed for hyperthermia and targeted drug delivery within MRI. Analytical predictions and numerical simulations of the transverse rotating magnetic field in the presence of B0 are investigated to demonstrate the effect of Ω, the rotating field frequency, and the magnetic field amplitude on the fluid suspension magnetization. The transverse magnetization due to the rotating transverse field shows strong dependence on the characteristic time constant of the fluid suspension, τ. The analysis shows that as the rotating field frequency increases so that Ωτ approaches unity, the transverse fluid magnetization vector is significantly non-aligned with the applied rotating field and the magnetization’s magnitude is a strong function of the field frequency. In this frequency range, the fluid’s transverse magnetization is controlled by the applied field which is determined by the operator. The phenomenon, which is due to the physical rotation of the magnetic nanoparticles in the suspension, is demonstrated analytically when the nanoparticles are present in high concentrations (1 to 3% solid volume fractions) more typical of hyperthermia rather than in clinical imaging applications, and in low MRI field strengths (such as open MRI systems), where the magnetic nanoparticles are not magnetically saturated. The effect of imposed Poiseuille flow in a planar channel geometry and changing nanoparticle concentration is examined. The work represents the first known attempt to analyze the dynamic behavior of magnetic nanoparticles in the MRI environment including the effects of the magnetic nanoparticle spin-velocity. It is shown that the magnitude of the transverse magnetization is a strong function of the rotating transverse field frequency. Interactive fluid magnetization effects are predicted due to non-uniform fluid magnetization in planar Poiseuille flow with high nanoparticle concentrations.
doi:10.1016/j.jmmm.2010.03.029
PMCID: PMC2901184  PMID: 20625540
Magnetic nanoparticles; MRI; rotating magnetic field; interactive magnetization; magnetic particle imaging
2.  Preparation of Soft Magnetic Fe-Ni-Pb-B Alloy Nanoparticles by Room Temperature Solid-Solid Reaction 
The Scientific World Journal  2013;2013:946897.
The Fe-Ni-Pb-B alloy nanoparticles was prepared by a solid-solid chemical reaction of ferric trichloride, nickel chloride, lead acetate, and potassium borohydride powders at room temperature. The research results of the ICP and thermal analysis indicate that the resultants are composed of iron, nickel, lead, boron, and PVP, and the component of the alloy is connected with the mole ratio of potassium borohydride and the metal salts. The TEM images show that the resultants are ultrafine and spherical particles, and the particle size is about a diameter of 25 nm. The largest saturation magnetization value of the 21.18 emu g−1 is obtained in the Fe-Ni-Pb-B alloy. The mechanism of the preparation reaction for the Fe-Ni-Pb-B multicomponent alloys is discussed.
doi:10.1155/2013/946897
PMCID: PMC3856161  PMID: 24348196
3.  Novel bioactive Co-based alloy/FA nanocomposite for dental applications 
Dental Research Journal  2012;9(2):173-179.
Background:
Dental cobalt base alloys are biocompatible dental materials and have been widely used in dentistry. However, metals are bioinert and may not present bioactivity in human body. Bioactivity is the especial ability to interact with human body and make a bonding to soft and hard tissues. The aim of the present research was fabrication and bioactivity evaluation of novel cobalt alloy/Fluorapatite nanocomposite (CoA/FaNC) with different amounts of Fluorapatite (FA) nanopowder.
Materials and Methods:
Co-Cr-Mo alloy (ASTM F75) powder was prepared and mixed in a planetary ball mill with different amounts of FA nanopowders (10, 15, 20% wt). Prepared composite powders were cold pressed and sintered at 1100°C for 4 h. X-ray diffraction (XRD), scanning electron microscopy and transition electron microscopy techniques were used for phase analysis, crystallite size determination of FA and also for phase analysis and evaluation of particle distribution of composites. Bioactivity behavior of prepared nanocomposites was evaluated in simulated body fluid (SBF) for 1 up to 28 days.
Materials and Methods:
Co-Cr-Mo alloy (ASTM F75) powder was prepared and mixed in a planetary ball mill with different amounts of FA nanopowders (10, 15, 20% wt). Prepared composite powders were cold pressed and sintered at 1100°C for 4 h. X-ray diffraction (XRD), scanning electron microscopy and transition electron microscopy techniques were used for phase analysis, crystallite size determination of FA and also for phase analysis and evaluation of particle distribution of composites. Bioactivity behavior of prepared nanocomposites was evaluated in simulated body fluid (SBF) for 1 up to 28 days.
Results:
Results showed that nucleus of apatite were formed on the surface of the prepared CoA/FaNC during 1 up to 28 days immersion in the SBF solution. On the other hand, CoA/FaNC unlike Co-base alloy possessed bone-like apatite-formation ability.
Conclusion:
It was concluded that bioinert Co-Cr-Mo alloy could be successfully converted into bioactive nanocomposite by adding 10, 15, 20 wt% of FA nano particles.
PMCID: PMC3353694  PMID: 22623934
Bioactivity; Co-Cr-Mo alloy; FA nanopowder; nanocomposite
4.  Formulation of a dry powder influenza vaccine for nasal delivery 
AAPS PharmSciTech  2006;7(1):E131-E137.
The purpose of this research was to prepare a dry powder vaccine formulation containing whole inactivated influenza virus (VIIV) and a mucoadhesive compound suitable for nasal delivery. Powders containing WIIV and either lactose or trehalose were produced by lyophilization. A micro-ball mill was used to reduce the lyophilized cake to sizes suitable for nasal delivery. Chitosan flakes were reduced in size using a cryo-milling technique. Milled powders were sieved between 45 and 125 μm aggregate sizes and characterized for particle size and distribution, morphology, and flow properties. Powders were blended in the micro-ball mill without the ball. Lyophilization followed by milling produced irregularly shaped, polydisperse particles with a median primary particle diameter of ≈21 μm and a yield of ≈37% of particles in the 45 to 125 μm particle size range. Flow properties of lactose and trehalose powders after lyophilization followed by milling and sieving were similar. Cryo-milling produced a small yield of particles in the desired size range (<10%). Lyophilization followed by milling and sieving produced particles suitable for nasal delivery with different physicochemical properties as a function of processing conditions and components of the formulation. Further optimization of particle size and morphology is required for these powders to be suitable for clinical evaluation.
doi:10.1208/pt070119
PMCID: PMC2750726
Intranasal delivery; dry powder; influenza vaccine; mucoadhesive; lyophilization
5.  Iron oxide-based nanomagnets in nanomedicine: fabrication and applications 
Nano Reviews  2010;1:10.3402/nano.v1i0.4883.
Iron oxide-based nanomagnets have attracted a great deal of attention in nanomedicine over the past decade. Down to the nanoscale, superparamagnetic iron oxide nanoparticles can only be magnetized in the presence of an external magnetic field, which makes them capable of forming stable colloids in a physio-biological medium. Their superparamagnetic property, together with other intrinsic properties, such as low cytotoxicity, colloidal stability, and bioactive molecule conjugation capability, makes such nanomagnets ideal in both in-vitro and in-vivo biomedical applications. In this review, a chemical, physical, and biological synthetic approach to prepare iron oxide-based nanomagnets with different physicochemical properties was illustrated and compared. The growing interest in iron oxide-based nanomagnets with multifunctionalities was explored in cancer diagnostics and treatment, focusing on their combined roles in a magnetic resonance contrast agent, hyperthermia, and magnetic force assisted drug delivery. Iron oxides as magnetic carriers in gene therapy were reviewed with a focus on the sophisticated design and construction of magnetic vectors. Finally, the iron oxide-based nanomagnet also represents a very promising tool in particle/cell interfacing in controlling cellular functionalities, such as adhesion, proliferation, differentiation, and cell patterning, in stem cell therapy and tissue engineering applications.
doi:10.3402/nano.v1i0.4883
PMCID: PMC3215210  PMID: 22110854
iron oxide; coprecipitation; thermal decomposition; microemulsion; magnetosome; lithography; cancer targeting; stem cell; gene delivery; tissue engineering; cell actuation
6.  Biomedical Nanomagnetics: A Spin Through Possibilities in Imaging, Diagnostics, and Therapy 
IEEE transactions on magnetics  2010;46(7):2523-2558.
Biomedical nanomagnetics is a multidisciplinary area of research in science, engineering and medicine with broad applications in imaging, diagnostics and therapy. Recent developments offer exciting possibilities in personalized medicine provided a truly integrated approach, combining chemistry, materials science, physics, engineering, biology and medicine, is implemented. Emphasizing this perspective, here we address important issues for the rapid development of the field, i.e., magnetic behavior at the nanoscale with emphasis on the relaxation dynamics, synthesis and surface functionalization of nanoparticles and core-shell structures, biocompatibility and toxicity studies, biological constraints and opportunities, and in vivo and in vitro applications. Specifically, we discuss targeted drug delivery and triggered release, novel contrast agents for magnetic resonance imaging, cancer therapy using magnetic fluid hyperthermia, in vitro diagnostics and the emerging magnetic particle imaging technique, that is quantitative and sensitive enough to compete with established imaging methods. In addition, the physics of self-assembly, which is fundamental to both biology and the future development of nanoscience, is illustrated with magnetic nanoparticles. It is shown that various competing energies associated with self-assembly converge on the nanometer length scale and different assemblies can be tailored by varying particle size and size distribution. Throughout this paper, while we discuss our recent research in the broad context of the multidisciplinary literature, we hope to bridge the gap between related work in physics/chemistry/engineering and biology/medicine and, at the same time, present the essential concepts in the individual disciplines. This approach is essential as biomedical nanomagnetics moves into the next phase of innovative translational research with emphasis on development of quantitative in vivo imaging, targeted and triggered drug release, and image guided therapy including validation of delivery and therapy response.
doi:10.1109/TMAG.2010.2046907
PMCID: PMC2949969  PMID: 20930943
Biomedical engineering; diagnostics; imaging; magnetic relaxation; nanotechnology; small particles; superparamagnetism; therapy
7.  Accelerated sintering in phase-separating nanostructured alloys 
Nature Communications  2015;6:6858.
Sintering of powders is a common means of producing bulk materials when melt casting is impossible or does not achieve a desired microstructure, and has long been pursued for nanocrystalline materials in particular. Acceleration of sintering is desirable to lower processing temperatures and times, and thus to limit undesirable microstructure evolution. Here we show that markedly enhanced sintering is possible in some nanocrystalline alloys. In a nanostructured W–Cr alloy, sintering sets on at a very low temperature that is commensurate with phase separation to form a Cr-rich phase with a nanoscale arrangement that supports rapid diffusional transport. The method permits bulk full density specimens with nanoscale grains, produced during a sintering cycle involving no applied stress. We further show that such accelerated sintering can be evoked by design in other nanocrystalline alloys, opening the door to a variety of nanostructured bulk materials processed in arbitrary shapes from powder inputs.
In sintering, powders of small grains are packed together to form shapes or grain structures that cannot be achieved by melt casting. Here, the authors demonstrate the fast sintering of a nanostructured alloy at low temperatures, preserving its nanoscale grain structure.
doi:10.1038/ncomms7858
PMCID: PMC4423263  PMID: 25901420
8.  Nanoscale potassium niobate crystal structure and phase transition 
Nanoscale Research Letters  2011;6(1):530.
Nanoscale potassium niobate (KNbO3) powders of orthorhombic structure were synthesized using the sol-gel method. The heat-treatment temperature of the gels had a pronounced effect on KNbO3 particle size and morphology. Field emission scanning electron microscopy and transmission electron microscopy were used to determine particle size and morphology. The average KNbO3 grain size was estimated to be less than 100 nm, and transmission electron microscopy images indicated that KNbO3 particles had a brick-like morphology. Synchrotron X-ray diffraction was used to identify the room-temperature structures using Rietveld refinement. The ferroelectric orthorhombic phase was retained even for particles smaller than 50 nm. The orthorhombic to tetragonal and tetragonal to cubic phase transitions of nanocrystalline KNbO3 were investigated using temperature-dependent powder X-ray diffraction. Differential scanning calorimetry was used to examine the temperature dependence of KNbO3 phase transition. The Curie temperature and phase transition were independent of particle size, and Rietveld analyses showed increasing distortions with decreasing particle size.
doi:10.1186/1556-276X-6-530
PMCID: PMC3212068  PMID: 21943345
potassium niobate; crystal structure; phase transition; nanoscale powder.
9.  Effects of Processing Parameters on the Synthesis of (K0.5Na0.5)NbO3 Nanopowders by Reactive High-Energy Ball Milling Method 
The Scientific World Journal  2014;2014:203047.
The effects of ball milling parameters, namely, the ball-to-powder mass ratio and milling speed, on the synthesis of (K0.5Na0.5)NbO3 nanopowders by high-energy ball milling method from a stoichiometric mixture containing Na2CO3, K2CO3, and Nb2O5 were investigated in this paper. The results indicated that the single crystalline phase of (K0.5Na0.5)NbO3 was received in as-milled samples synthesized using optimized ball-to-powder mass ratio of 35 : 1 and at a milling speed of 600 rpm for 5 h. In the optimized as-milled samples, no remaining alkali carbonates that can provide the volatilizable potassium-containing species were found and (K0.5Na0.5)NbO3 nanopowders were readily obtained via the formation of an intermediate carbonato complex. This complex was mostly transformed into (K0.5Na0.5)NbO3 at temperature as low as 350°C and its existence was no longer detected at spectroscopic level when calcination temperature crossed over 700°C.
doi:10.1155/2014/203047
PMCID: PMC3925596  PMID: 24592146
10.  Properties of experimental copper-aluminium-nickel alloys for dental post-and-core applications 
PURPOSE
This study aimed to develop a copper-aluminium-nickel alloy which has properties comparable to that of dental alloys used for dental post and core applications with the reasonable cost.
MATERIALS AND METHODS
Sixteen groups of experimental copper alloys with variants of 3, 6, 9, 12 wt% Al and 0, 2, 4, 6 wt% Ni were prepared and casted. Their properties were tested and evaluated. The data of thermal, physical, and mechanical properties were analyzed using the two-way ANOVA and Tukey's test (α=0.05). The alloy toxicity was evaluated according to the ISO standard.
RESULTS
The solidus and liquidus points of experimental alloys ranged from 1023℃ to 1113℃ and increased as the nickel content increased. The highest ultimate tensile strength (595.9 ± 14.2 MPa) was shown in the Cu-12Al-4Ni alloy. The tensile strength was increased as the both elements increased. Alloys with 3-6 wt% Al exhibited a small amount of 0.2% proof strength. Accordingly, the Cu-9Al-2Ni and Cu-9Al-4Ni alloys not only demonstrated an appropriate modulus of elasticity (113.9 ± 8.0 and 122.8 ± 11.3 GPa, respectively), but also had a value of 0.2% proof strength (190.8 ± 4.8 and 198.2 ± 3.4 MPa, respectively), which complied with the ISO standard requirement (>180 MPa). Alloys with the highest contents of nickel (6 wt% Ni) revealed a widespread decolourisation zone (5.0-5.9 mm), which correspondingly produced the largest cell response, equating positive control.
CONCLUSION
The copper alloys fused with 9 wt% Al and 2-4 wt% Ni can be considered for a potential use as dental post and core applications.
doi:10.4047/jap.2014.6.3.215
PMCID: PMC4085246  PMID: 25006386
Cu-Al-Ni alloy; Copper alloy; Dental alloy; Post and core
11.  Simple and Rapid Synthesis of Magnetite/Hydroxyapatite Composites for Hyperthermia Treatments via a Mechanochemical Route 
This paper presents a simple method for the rapid synthesis of magnetite/hydroxyapatite composite particles. In this method, superparamagnetic magnetite nanoparticles are first synthesized by coprecipitation using ferrous chloride and ferric chloride. Immediately following the synthesis, carbonate-substituted (B-type) hydroxyapatite particles are mechanochemically synthesized by wet milling dicalcium phosphate dihydrate and calcium carbonate in a dispersed suspension of magnetite nanoparticles, during which the magnetite nanoparticles are incorporated into the hydroxyapatite matrix. We observed that the resultant magnetite/hydroxyapatite composites possessed a homogeneous dispersion of magnetite nanoparticles, characterized by an absence of large aggregates. When this material was subjected to an alternating magnetic field, the heat generated increased with increasing magnetite concentration. For a magnetite concentration of 30 mass%, a temperature increase greater than 20 K was achieved in less than 50 s. These results suggest that our composites exhibit good hyperthermia properties and are promising candidates for hyperthermia treatments.
doi:10.3390/ijms14059365
PMCID: PMC3676787  PMID: 23629669
magnetite; carbonate hydroxyapatite; mechanochemical effect; hyperthermia
12.  In situ Growth of NixCu1-x Alloy Nanocatalysts on Redox-reversible Rutile (Nb,Ti)O4 Towards High-Temperature Carbon Dioxide Electrolysis 
Scientific Reports  2014;4:5156.
In this paper, we report the in situ growth of NixCu1-x (x = 0, 0.25, 0.50, 0.75 and 1.0) alloy catalysts to anchor and decorate a redox-reversible Nb1.33Ti0.67O4 ceramic substrate with the aim of tailoring the electrocatalytic activity of the composite materials through direct exsolution of metal particles from the crystal lattice of a ceramic oxide in a reducing atmosphere at high temperatures. Combined analysis using XRD, SEM, EDS, TGA, TEM and XPS confirmed the completely reversible exsolution/dissolution of the NixCu1-x alloy particles during the redox cycling treatments. TEM results revealed that the alloy particles were exsolved to anchor onto the surface of highly electronically conducting Nb1.33Ti0.67O4 in the form of heterojunctions. The electrical properties of the nanosized NixCu1-x/Nb1.33Ti0.67O4 were systematically investigated and correlated to the electrochemical performance of the composite electrodes. A strong dependence of the improved electrode activity on the alloy compositions was observed in reducing atmospheres at high temperatures. Direct electrolysis of CO2 at the NixCu1-x/Nb1.33Ti0.67O4 composite cathodes was investigated in solid-oxide electrolysers. The CO2 splitting rates were observed to be positively correlated with the Ni composition; however, the Ni0.75Cu0.25 combined the advantages of metallic nickel and copper and therefore maximised the current efficiencies.
doi:10.1038/srep05156
PMCID: PMC4042123  PMID: 24889679
13.  The Effects of Adding Elements of Zinc and Magnesium on Ag-Cu Eutectic Alloy for Warming Acupuncture 
The warming acupuncture for hyperthermia therapy is made of STS304. However, its needle point cannot be reached to a desirable temperature due to heat loss caused by low thermal conductivity, and the quantification of stimulation condition and the effective standard establishment of warming acupuncture are required as a heat source. Accordingly, in this study, after Ag-Cu alloys with different composition ratios were casted and then mixed with additives to improve their physical and mechanical properties, the thermal conductivity and biocompatibility of the alloy specimens were evaluated for selecting suitable material. Ag-Cu binary alloys and ternary alloys added 5 wt% Zn or 2 wt% Mg were casted and then cold drawn to manufacture needles for acupuncture, and their physical properties, thermal conductivity, and biocompatibility were evaluated for their potential use in warming acupuncture. The results of this study showed that the physical and mechanical properties of the Ag-Cu alloys were improved by additives and that the thermal conductivity, machinability, and biocompatibility of the Ag-Cu alloys were improved by Mg addition.
doi:10.1155/2013/532735
PMCID: PMC3771487  PMID: 24078827
14.  Intratumoral Iron Oxide Nanoparticle Hyperthermia and Radiation Cancer Treatment 
The potential synergism and benefit of combined hyperthermia and radiation for cancer treatment is well established, but has yet to be optimized clinically. Specifically, the delivery of heat via external arrays /applicators or interstitial antennas has not demonstrated the spatial precision or specificity necessary to achieve appropriate a highly positive therapeutic ratio. Recently, antibody directed and possibly even non-antibody directed iron oxide nanoparticle hyperthermia has shown significant promise as a tumor treatment modality. Our studies are designed to determine the effects (safety and efficacy) of iron oxide nanoparticle hyperthermia and external beam radiation in a murine breast cancer model.
Methods
MTG-B murine breast cancer cells (1 × 106) were implanted subcutaneous in 7 week-old female C3H/HeJ mice and grown to a treatment size of 150 mm3 +/− 50 mm3. Tumors were then injected locally with iron oxide nanoparticles and heated via an alternating magnetic field (AMF) generator operated at approximately 160 kHz and 400 - 550 Oe. Tumor growth was monitored daily using standard 3-D caliper measurement technique and formula. specific Mouse tumors were heated using a cooled, 36 mm diameter square copper tube induction coil which provided optimal heating in a 1 cm wide region in the center of the coil. Double dextran coated 80 nm iron oxide nanoparticles (Triton Biosystems) were used in all studies. Intra-tumor, peri-tumor and rectal (core body) temperatures were continually measured throughout the treatment period.
Results
Preliminary in vivo nanoparticle-AMF hyperthermia (167 KHz and 400 or 550 Oe) studies demonstrated dose responsive cytotoxicity which enhanced the effects of external beam radiation. AMF associated eddy currents resulted in nonspecific temperature increases in exposed tissues which did not contain nanoparticles, however these effects were minor and not injurious to the mice. These studies also suggest that iron oxide nanoparticle hyperthermia is more effective than nonnanoparticle tumor heating techniques when similar thermal doses are applied. Initial electron and light microscopy studies of iron oxide nanoparticle and AMF exposed tumor cells show a rapid uptake of particles and acute cytotoxicity following AMF exposure.
doi:10.1117/12.706302
PMCID: PMC4187389  PMID: 25301985
15.  Investigation of phase composition and nanoscale microstructure of high-energy ball-milled MgCu sample 
Nanoscale Research Letters  2012;7(1):390.
The ball milling technique has been successfully applied to the synthesis of various materials such as equilibrium intermetallic phases, amorphous compounds, nanocrystalline materials, or metastable crystalline phases. However, how the phase composition and nanoscale microstructure evolute during ball milling in various materials is still controversial due to the complex mechanism of ball milling, especially in the field of solid-state amorphization caused by ball milling. In the present work, the phase evolution during the high-energy ball milling process of the Mg and Cu (atomic ratio is 1:1) mixed powder was investigated. It was found that Mg firstly reacts with Cu, forming the Mg2Cu alloy in the primary stage of ball milling. As the milling time increases, the diffracted peaks of Mg2Cu and Cu gradually disappear, and only a broad halo peak can be observed in the X-ray diffraction pattern of the final 18-h milled sample. As for this halo peak, lots of previous studies suggested that it originated from the amorphous phase formed during the ball milling. Here, a different opinion that this halo peak results from the very small size of crystals is proposed: As the ball milling time increases, the sizes of Mg2Cu and Cu crystals become smaller and smaller, so the diffracted peaks of Mg2Cu and Cu become broader and broader and result in their overlap between 39° and 45°, at last forming the amorphous-like halo peak. In order to determine the origin of this halo peak, microstructure observation and annealing experiment on the milled sample were carried out. In the transmission electron microscopy dark-field image of the milled sample, lots of very small nanocrystals (below 20 nm) identified as Mg2Cu and Cu were found. Moreover, in the differential scanning calorimetry curve of the milled sample during the annealing process, no obvious exothermic peak corresponding to the crystallization of amorphous phase is observed. All the above results confirm that the broad halo diffracted peak in the milled MgCu sample is attributed to the overlap of the broadened peaks of the very small Mg2Cu and Cu nanocrystalline phase, not the MgCu amorphous phase. The whole milling process of MgCu can be described as follows: Mg+Cu→Mg2Cu+Cu→Mg2Cunanocrystal+Cunanocrystal.
doi:10.1186/1556-276X-7-390
PMCID: PMC3462153  PMID: 22793264
16.  Hyperthermic potentiation of cisplatin by magnetic nanoparticle heaters is correlated with an increase in cell membrane fluidity 
Magnetic fluid hyperthermia as a cancer treatment method is an attractive alternative to other forms of hyperthermia. It is based on the heat released by magnetic nanoparticles subjected to an alternating magnetic field. Recent studies have shown that magnetic fluid hyperthermia-treated cells respond significantly better to chemotherapeutic treatment compared with cells treated with hot water hyperthermia under the same temperature conditions. We hypothesized that this synergistic effect is due to an additional stress on the cellular membrane, independent of the thermal heat dose effect that is induced by nanoparticles exposed to an alternating magnetic field. This would result in an increase in Cis-diammine-dichloroplatinum (II) (cDDP, cisplatin) uptake via passive transport. To test this hypothesis, we exposed cDDP-treated cells to extracellular copper in order to hinder the human cell copper transporter (hCTR1)-mediated active transport of cDDP. This, in turn, can increase the passive transport of the drug through the cell membrane. Our results did not show statistically significant differences in surviving fractions for cells treated concomitantly with magnetic fluid hyperthermia and cDDP, in the presence or absence of copper. Nonetheless, significant copper-dependent variations in cell survival were observed for samples treated with combined cDDP and hot water hyperthermia. These results correlated with platinum uptake studies, which showed that cells treated with magnetic fluid hyperthermia had higher platinum uptake than cells treated with hot water hyperthermia. Changes in membrane fluidity were tested through fluorescence anisotropy measurements using trimethylamine-diphenylhexatriene. Additional uptake studies were conducted with acridine orange and measured by flow cytometry. These studies indicated that magnetic fluid hyperthermia significantly increases cell membrane fluidity relative to hot water hyperthermia and untreated cells, and hence this could be a factor contributing to the increase of cDDP uptake in magnetic fluid hyperthermia-treated cells. Overall, our data provide convincing evidence that cell membrane permeability induced by magnetic fluid hyperthermia is significantly greater than that induced by hot water hyperthermia under similar temperature conditions, and is at least one of the mechanisms responsible for potentiation of cDDP by magnetic fluid hyperthermia in Caco-2 cells.
doi:10.2147/IJN.S38842
PMCID: PMC3593770  PMID: 23493492
magnetic nanoparticles; synergistic effect; hot water hyperthermia; surviving fraction; viability ratio
17.  Ferromagnetism of Fe3Sn and Alloys 
Scientific Reports  2014;4:7024.
Hexagonal Fe3Sn has many of the desirable properties for a new permanent magnet phase with a Curie temperature of 725 K, a saturation moment of 1.18 MA/m. and anisotropy energy, K1 of 1.8 MJ/m3. However, contrary to earlier experimental reports, we found both experimentally and theoretically that the easy magnetic axis lies in the hexagonal plane, which is undesirable for a permanent magnet material. One possibility for changing the easy axis direction is through alloying. We used first principles calculations to investigate the effect of elemental substitutions. The calculations showed that substitution on the Sn site has the potential to switch the easy axis direction. However, transition metal substitutions with Co or Mn do not have this effect. We attempted synthesis of a number of these alloys and found results in accord with the theoretical predictions for those that were formed. However, the alloys that could be readily made all showed an in-plane easy axis. The electronic structure of Fe3Sn is reported, as are some are magnetic and structural properties for the Fe3Sn2, and Fe5Sn3 compounds, which could be prepared as mm-sized single crystals.
doi:10.1038/srep07024
PMCID: PMC4228330  PMID: 25387850
18.  Preparation and magnetic properties of nano size nickel ferrite particles using hydrothermal method 
Background
Nickel ferrite, a kind of soft magnetic materials is one of the most attracting class of materials due to its interesting and important properties and has many technical applications, such as in catalysis, sensors and so on. In this paper the synthesis of NiFe2O4 nanoparticles by the hydrothermal method is reported and the inhibition of surfactant (Glycerol or Sodium dodecyl sulfate) on the particles growth is investigated.
Methods
For investigation of the inhibition effect of surfactant on NiFe2O4 particles growth, the samples were prepared in presence of Glycerol and Sodium dodecyl sulfate. The X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM) and inductively coupled plasma atomic emission spectrometer (ICP-AES) techniques were used to characterize the samples.
Results
The results of XRD and ICP-AES show that the products were pure NiFe2O4 and also nanoparticles grow with increasing the temperature, while surfactant prevents the particle growth under the same condition. The average particle size was determined from the Scherrer's equation and TEM micrographs and found to be in the range of 50-60 nm that decreased up to 10-15 nm in presence of surfactant. The FT-IR results show two absorption bands near to 603 and 490 cm-1 for the tetrahedral and octahedral sites respectively. Furthermore, the saturated magnetization and coercivity of NiFe2O4 nanoparticles were in the range of 39.60 emu/g and 15.67 Qe that decreased for samples prepared in presence of surfactant. As well as, the nanoparticles exhibited a superparamagnetic behavior at room temperature.
Conclusions
Nanosized nickel ferrite particles were synthesized with and without surfactant assisted hydrothermal methods. The results show that with increasing of temperature, the crystallinity of nanoparticles is increased. In the presence of surfactants, the crystallinity of NiFe2O4 nanoparticles decreased in comparison with surfactant- free prepared samples. All of the nickel ferrite nanoparticles were superparamagnetic at room temperature.
Graphical abstract
doi:10.1186/1752-153X-6-23
PMCID: PMC3348867  PMID: 22462726
Oxides; Magnetic properties; Surfactants; Nanostructures
19.  Self-Consolidation Mechanism of Nanostructured Ti5Si3 Compact Induced by Electrical Discharge 
The Scientific World Journal  2015;2015:815084.
Electrical discharge using a capacitance of 450 μF at 7.0 and 8.0 kJ input energies was applied to mechanical alloyed Ti5Si3 powder without applying any external pressure. A solid bulk of nanostructured Ti5Si3 with no compositional deviation was obtained in times as short as 159 μsec by the discharge. During an electrical discharge, the heat generated is the required parameter possibly to melt the Ti5Si3 particles and the pinch force can pressurize the melted powder without allowing the formation of pores. Followed rapid cooling preserved the nanostructure of consolidated Ti5Si3 compact. Three stepped processes during an electrical discharge for the formation of nanostructured Ti5Si3 compact are proposed: (a) a physical breakdown of the surface oxide of Ti5Si3 powder particles, (b) melting and condensation of Ti5Si3 powder by the heat and pinch pressure, respectively, and (c) rapid cooling for the preservation of nanostructure. Complete conversion yielding a single phase Ti5Si3 is primarily dominated by the solid-liquid mechanism.
doi:10.1155/2015/815084
PMCID: PMC4389978  PMID: 25884039
20.  Nanostructured Hypoeutectic Fe-B Alloy Prepared by a Self-propagating High Temperature Synthesis Combining a Rapid Cooling Technique 
Nanoscale Research Letters  2008;4(1):11-16.
We have successfully synthesized bulk nanostructured Fe94.3B5.7 alloy using the one-step approach of a self-propagating high temperature synthesis (SHS) combining a rapid cooling technique. This method is convenient, low in cost, and capable of being scaled up for processing the bulk nanostructured materials. The solidification microstructure is composed of a relatively coarse, uniformly distributed dendriteto a nanostructured eutectic matrix with α-Fe(B) and t-Fe2B phases. The fine eutectic structure is disorganized, and the precipitation Fe2B is found in the α-Fe(B) phase of the eutectic. The dendrite phase has the t-Fe2B structure rather than α-Fe(B) in the Fe94.3B5.7 alloy, because the growth velocity of t-Fe2B is faster than that of the α-Fe with the deeply super-cooling degree. The coercivity (Hc) and saturation magnetization (Ms) values of the Fe94.3B5.7 alloy are 11 A/m and 1.74T, respectively. Moreover, the Fe94.3B5.7 alloy yields at 1430 MPa and fractures at 1710 MPa with a large ductility of 19.8% at compressive test.
doi:10.1007/s11671-008-9195-4
PMCID: PMC2893940  PMID: 20596402
Nanostructured eutectic; Fe94.3B5.7 alloy; Self-propagating high temperature synthesis (SHS); Soft magnetic performance; Mechanical behavior
21.  Nanostructured Hypoeutectic Fe-B Alloy Prepared by a Self-propagating High Temperature Synthesis Combining a Rapid Cooling Technique 
Nanoscale Research Letters  2008;4(1):11-16.
We have successfully synthesized bulk nanostructured Fe94.3B5.7 alloy using the one-step approach of a self-propagating high temperature synthesis (SHS) combining a rapid cooling technique. This method is convenient, low in cost, and capable of being scaled up for processing the bulk nanostructured materials. The solidification microstructure is composed of a relatively coarse, uniformly distributed dendriteto a nanostructured eutectic matrix with α-Fe(B) and t-Fe2B phases. The fine eutectic structure is disorganized, and the precipitation Fe2B is found in the α-Fe(B) phase of the eutectic. The dendrite phase has the t-Fe2B structure rather than α-Fe(B) in the Fe94.3B5.7 alloy, because the growth velocity of t-Fe2B is faster than that of the α-Fe with the deeply super-cooling degree. The coercivity (Hc) and saturation magnetization (Ms) values of the Fe94.3B5.7 alloy are 11 A/m and 1.74T, respectively. Moreover, the Fe94.3B5.7 alloy yields at 1430 MPa and fractures at 1710 MPa with a large ductility of 19.8% at compressive test.
doi:10.1007/s11671-008-9195-4
PMCID: PMC2893940  PMID: 20596402
Nanostructured eutectic; Fe94.3B5.7alloy; Self-propagating high temperature synthesis (SHS); Soft magnetic performance; Mechanical behavior
22.  Magnetic fluid hyperthermia induced by radiofrequency capacitive field for the treatment of transplanted subcutaneous tumors in rats 
Magnetic fluid hyperthermia (MFH) induced by a magnetic field has become a new heating technology for the treatment of malignant tumors due to its ability to heat the tumor tissue precisely and properly, and due to its significant therapeutic effects. In this study, MFH induced by radiofrequency capacitive field (RCF) for the treatment of transplanted subcutaneous tumors in rats, was investigated. A total of 50 rats bearing subcutaneous tumors were randomly divided into five groups, including i) a pseudo-treatment (PT) control group, ii) magnetic fluid (MF) group, iii) pure hyperthermia (PH) group, iv) magnetic fluid hyperthermia 1 (MFH1) group, and v) magnetic fluid hyperthermia 2 (MFH2) group. Tumors were irradiated for 30 min in the MFH1 group 24 h following injection of MF. Tumors were irradiated for 30 min in the MFH2 group 24 h following injection of MF, and irradiation was repeated for 30 min 72 h following injection of MF. Tumor volumes, tumor volume inhibition ratios and survival times in the rat model were examined. Temperatures of tumor cores and rims both rapidly reached the desired temperature (∼50°C) for tumor treatment within 5 to 10 min in the MFH1 and MFH2 groups, and we maintained this temperature level by manually adjusting the output power (70–130 W). Tumor volumes of the MFH1 and MFH2 groups were reduced compared to those of the PT, MF and PH groups. The inhibitory effect on tumor growth in the MFH2 group (91.57%) was higher compared to that in the MFH1 group (85.21%) and the other groups. The survival time of the MFH2 group (51.62±2.28 days) and MFH1 group (43.10±1.57 days) was increased compared to that of the PH, MF and PT groups. The results obtained show that MFH induced by RCF may serve as a potential and promising method for the treatment of tumors.
doi:10.3892/etm.2011.397
PMCID: PMC3438723  PMID: 22969882
magnetic fluid hyperthermia; radiofrequency capacitive field; transplanted subcutaneous tumor; rat
23.  Electrochemical properties of the TiO2(B) powders ball mill treated for lithium-ion battery application 
Background
Belt or wire shaped TiO2(B) particles were synthesized for lithium ion battery application by a hydrothermal and heat treatment process. In order to facilitate TiO2(B)/C composites fabrication, the synthesized TiO2(B) particles were crushed into smaller sizes by ball milling.
Results
Ball mill treated TiO2(B) particles of less than 1.0 μm with a fraction of anatase phase, compared to as-synthesized TiO2(B) particles with about 24 μm in average particle size, showed a significant improvement in the electrochemical properties. They showed a much improved stability in the charge–discharge cycles and irreversibility. They maintained about 98% of the initial capacity during 50 cycles while as-synthesized sample before ball mill treatment showed a gradual decrease in the capacity with the cycles. The irreversibility of 12.4% of as-synthesized sample was also greatly improved to 7% after ball milling treatment.
Conclusions
Our results indicate ball mill treatment can be an economical way to improve electrochemical properties of TiO2(B) anode materials for lithium ion battery application.
doi:10.1186/1752-153X-7-174
PMCID: PMC4177134  PMID: 24196343
TiO2(B); Anode materials; Ball-milling; Lithium-ion battery; Hydrothermal method
24.  The Influence of Milling on the Dissolution Performance of Simvastatin 
Pharmaceutics  2010;2(4):419-431.
Particle size reduction is a simple means to enhance the dissolution rate of poorly water soluble BCS-class II and IV drugs. However, the major drawback of this process is the possible introduction of process induced disorder. Drugs with different molecular arrangements may exhibit altered properties such as solubility and dissolution rate and, therefore, process induced solid state modifications need to be monitored. The aim of this study was two-fold: firstly, to investigate the dissolution rates of milled and unmilled simvastatin; and secondly, to screen for the main milling factors, as well as factor interactions in a dry ball milling process using simvastatin as model drug, and to optimize the milling procedure with regard to the opposing responses particle size and process induced disorder by application of a central composite face centered design. Particle size was assessed by scanning electron microscopy (SEM) and image analysis. Process induced disorder was determined by partial least squares (PLS) regression modeling of respective X-ray powder diffractograms (XRPD) and Raman spectra. Valid and significant quadratic models were built. The investigated milling factors were milling frequency, milling time and ball quantity at a set drug load, out of which milling frequency was found to be the most important factor for particle size as well as process induced disorder. Milling frequency and milling time exhibited an interaction effect on the responses. The optimum milling settings using the maximum number of milling balls (60 balls with 4 mm diameter) was determined to be at a milling frequency of 21 Hz and a milling time of 36 min with a resulting primary particle size of 1.4 μm and a process induced disorder of 6.1% (assessed by Raman spectroscopy) and 8.4% (assessed by XRPD), at a set optimization limit of < 2 μm for particle size and < 10% for process induced disorder. This optimum was tested experimentally and the process induced disorder was determined to be 6.9% (± 2.2) by Raman spectroscopy and 7.8% (± 2.3) by XRPD. Subsequent intrinsic dissolution testing revealed that the process induced disorder was negligible with regard to the dissolution rate. The predicted primary particle size of 1.4 μm could be confirmed experimentally, but due to agglomeration of the primary particles a dissolution rate advantage was not shown, highlighting the importance of dissolution testing at an early stage of drug development.
doi:10.3390/pharmaceutics2040419
PMCID: PMC3967146
dissolution rate; ball milling; process induced disorder; response surface modeling; simvastatin
25.  Bioaccessibility, bioavailability and toxicity of commercially relevant iron- and chromium-based particles: in vitro studies with an inhalation perspective 
Background
Production of ferrochromium alloys (FeCr), master alloys for stainless steel manufacture, involves casting and crushing processes where particles inevitably become airborne and potentially inhaled. The aim of this study was to assess potential health hazards induced by inhalation of different well-characterized iron- and chromium-based particles, i.e. ferrochromium (FeCr), ferrosiliconchromium (FeSiCr), stainless steel (316L), iron (Fe), chromium (Cr), and chromium(III)oxide (Cr2O3), in different size fractions using in vitro methods. This was done by assessing the extent and speciation of released metals in synthetic biological medium and by analyzing particle reactivity and toxicity towards cultured human lung cells (A549).
Results
The amount of released metals normalized to the particle surface area increased with decreasing particle size for all alloy particles, whereas the opposite situation was valid for particles of the pure metals. These effects were evident in artificial lysosomal fluid (ALF) of pH 4.5 containing complexing agents, but not in neutral or weakly alkaline biological media. Chromium, iron and nickel were released to very low extent from all alloy particles, and from particles of Cr due to the presence of a Cr(III)-rich protective surface oxide. Released elements were neither proportional to the bulk nor to the surface composition after the investigated 168 hours of exposure. Due to a surface oxide with less protective properties, significantly more iron was released from pure iron particles compared with the alloys. Cr was predominantly released as Cr(III) from all particles investigated and was strongly complexed by organic species of ALF. Cr2O3 particles showed hemolytic activity, but none of the alloy particles did. Fine-sized particles of stainless steel caused however DNA damage, measured with the comet assay after 4 h exposure. None of the particles revealed any significant cytotoxicity in terms of cell death after 24 h exposure.
Conclusion
It is evident that particle and alloy characteristics such as particle size and surface composition are important aspects to consider when assessing particle toxicity and metal release from alloy particles compared to pure metal particles. Generated results clearly elucidate that neither the low released concentrations of metals primarily as a result of protective and poorly soluble surface oxides, nor non-bioavailable chromium complexes, nor the particles themselves of occupational relevance induced significant acute toxic response, with exception of DNA damage from stainless steel.
doi:10.1186/1743-8977-7-23
PMCID: PMC2941740  PMID: 20815895

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