Investigation of Surfactant Effect on Size Distribution of FePt-based Nanoparticles by Synchrotron SAXS and TEM

Chokprasombat, Komkrich; Koyvanich, Krit; Sirisathitkul, Chitnarong; Harding, Phimphaka; Rugmai, Supagorn

doi:10.1007/s12666-015-0545-5

Cited by 6 publications

(7 citation statements)

References 15 publications

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“…SR-SAXS curves are plotted as the intensity of X-ray scattering I ( q ) versus scattering vector q . The scattering vector is defined by following equation , where θ is half the scattering angle and λ is a wavelength of X-ray. According to Bragg formula The long period can be calculated by the following equation The gap value can be calculated by the following equation The long period is defined as the statistically average distance between the particles.…”

Section: Results and Discussionmentioning

confidence: 99%

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Optimal Hotspots of Dynamic Surfaced-Enhanced Raman Spectroscopy for Drugs Quantitative Detection

Yan

Zhou

et al. 2017

Anal. Chem.

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Surface-enhanced Raman spectroscopy (SERS) as a powerful qualitative analysis method has been widely applied in many fields. However, SERS for quantitative analysis still suffers from several challenges partially because of the absence of stable and credible analytical strategy. Here, we demonstrate that the optimal hotspots created from dynamic surfaced-enhanced Raman spectroscopy (D-SERS) can be used for quantitative SERS measurements. In situ small-angle X-ray scattering was carried out to in situ real-time monitor the formation of the optimal hotspots, where the optimal hotspots with the most efficient hotspots were generated during the monodisperse Au-sol evaporating process. Importantly, the natural evaporation of Au-sol avoids the nanoparticles instability of salt-induced, and formation of ordered three-dimensional hotspots allows SERS detection with excellent reproducibility. Considering SERS signal variability in the D-SERS process, 4-mercaptopyridine (4-mpy) acted as internal standard to validly correct and improve stability as well as reduce fluctuation of signals. The strongest SERS spectra at the optimal hotspots of D-SERS have been extracted to statistics analysis. By using the SERS signal of 4-mpy as a stable internal calibration standard, the relative SERS intensity of target molecules demonstrated a linear response versus the negative logarithm of concentrations at the point of strongest SERS signals, which illustrates the great potential for quantitative analysis. The public drugs 3,4-methylenedioxymethamphetamine and α-methyltryptamine hydrochloride obtained precise analysis with internal standard D-SERS strategy. As a consequence, one has reason to believe our approach is promising to challenge quantitative problems in conventional SERS analysis.

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Section: Results and Discussionmentioning

confidence: 99%

“…SR-SAXS curves are plotted as the intensity of X-ray scattering I(q) versus scattering vector q. The scattering vector is defined by following equation 30,31 π θ λ = q 4 (sin )/ (1) where θ is half the scattering angle and λ is a wavelength of Xray. According to Bragg formula…”

Section: ■ Results and Discussionmentioning

confidence: 99%

Optimal Hotspots of Dynamic Surfaced-Enhanced Raman Spectroscopy for Drugs Quantitative Detection

Yan

Zhou

et al. 2017

Anal. Chem.

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“…In the SAXS measurement, the scattering vector is set as q :

q = \frac{4 π}{l} \sin θ

where 2 θ is the scattering angle, and l is the wavelength. The scattering intensity is expressed by I ( q ), which is calculated as :

I ((), q) = I_{e} {(Δ ρ)}^{2} V \int_{0}^{\infty} γ ((), r) \frac{\sin ((), qr)}{qr} 4 π r^{2} italic핕 r

where I e is the scattering intensity of an electron, ( Δρ ) 2 is the mean square of the fluctuation of the electron density between the scatterer and the surrounding media, r is the scatter spacing, V is the volume of the scatterer irradiated by X‐rays, and γ ( r ) is the spatial correlation function of electron density fluctuations.…”

Section: Saxs Test Methodsmentioning

confidence: 99%

Study on the Structure Characteristics of Diesel Engine Particulates Based on Small‐Angle X‐Ray Scattering

Zhong

Liu

2019

Env Prog and Sustain Energy

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In this article, the particulates formed by the combustion of diesel, 20% and 50% biodiesel blended in diesel (denoted as B20 and B50, respectively), and biodiesel were collected. The micromorphologies of the particulates were observed by scanning electron microscopy. Furthermore, the small‐angle X‐ray scattering technique was used to analyze the gyration radius, size distribution, interfacial characteristics, and fractal characteristics of the particulates. The results show that the size of the particulates formed by combustion of the fuels was concentrated between 10 and 35 nm and obeyed a Gaussian distribution. Moreover, the addition of biodiesel to diesel led to smaller particulate sizes for the biodiesel/diesel blend: the mean radii of the particulates for diesel, B20, B50, and biodiesel were 11.5 nm, 10.8 nm, 10.2 nm, and 9.7 nm, respectively. In addition, an interfacial layer was observed between the particulates, and the average interfacial thickness of the particulates was between 1.54 and 1.89 nm. The mass fractal dimension of the particulates was between 0.2 and 2.5, and the surface fractal dimension of the particulates was between 2.1 and 2.9. The addition of biodiesel to diesel resulted in a more compact particulate structure and the rougher surface. © 2019 American Institute of Chemical Engineers Environ Prog, 38:e13146, 2019

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“…Its advantages are the accurate determination of nanoparticle size distributions and the discrimination between polydisperse single particle and polydisperse particle in aggregates. SAXS has been successfully used to complement TEM in probing the size distribution of several nanoparticles including Au [13], CoPt 3 [14] and FePt [15]. Furthermore, Fe 3 O 4 and CuO nanoparticles were comparatively characterized using X-ray diffractometry (XRD), TEM, DLS and SAXS [16].…”

mentioning

confidence: 99%

FePt3 nanosuspension synthesized from different precursors – a morphological comparison by SAXS, DLS and TEM

Sarmphim¹,

Soontaranon²,

Sirisathitkul³

et al. 2017

Bulletin of the Polish Academy of Sciences Technical Sciences

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Abstract. Annealed iron-platinum (FePt) is ferromagnetic in a nanoscale regime which is necessary for energy and data storage, whereas the as-synthesized form of FePt-based nanoparticles exhibits superparamagnetism useful for biomedical applications. In this study, as-synthesized nanosuspensions from the reaction of Pt(acac) 2 with Fe(acac) 3 and Fe(hfac) 3 are compared. X-ray diffraction (XRD) peaks for both samples are assigned to the FePt 3 phase. As shown by transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS), nanoparticles synthesized by using Fe(acac) 3 have a smaller average diameter, but larger polydispersity index and particle agglomerations. On the other hand, the nanoparticles synthesized by using Fe(hfac) 3 can self-assemble into a longer range of patterned monolayer. Dynamic light scattering (DLS), measuring the size of cluster of nanoparticles as well as oleic acid and oleylamine at their surface, confirms that larger agglomerations in the sample were synthesized by using Fe(acac) 3 . In addition to the size distribution, magnetic properties were influenced by the composition of these nanoparticles. Another non-destructive technique to determine the size distribution is small angle X-ray scattering (SAXS) [12]. Its advantages are the accurate determination of nanoparticle size distributions and the discrimination between polydisperse single particle and polydisperse particle in aggregates. SAXS has been successfully used to complement TEM in probing the size distribution of several nanoparticles including Au [13], CoPt 3 [14] and FePt [15]. Furthermore, Fe 3 O 4 and CuO nanoparticles were comparatively characterized using X-ray diffractometry (XRD), TEM, DLS and SAXS [16].In this study, the morphology of FePt-based nanoparticles synthesized from two alternative precursors is compared by using TEM, DLS and SAXS. Iron(III) acetylacetonate (Fe(acac) 3 ) and iron(III) hexafluoroacetylacetone (Fe(hfac) 3 ) have been investigated as a replacement for highly toxic Fe(CO) 5 . The synthetic procedure, adapted from the published method [17], replaces a N 2 glove box with an Ar Schlenk line. The heating rate in the terminal process and revolution of purified centrifugation are also reduced.

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Investigation of Surfactant Effect on Size Distribution of FePt-based Nanoparticles by Synchrotron SAXS and TEM

Cited by 6 publications

References 15 publications

Optimal Hotspots of Dynamic Surfaced-Enhanced Raman Spectroscopy for Drugs Quantitative Detection

Optimal Hotspots of Dynamic Surfaced-Enhanced Raman Spectroscopy for Drugs Quantitative Detection

Study on the Structure Characteristics of Diesel Engine Particulates Based on Small‐Angle X‐Ray Scattering

FePt3 nanosuspension synthesized from different precursors – a morphological comparison by SAXS, DLS and TEM

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