scholarly journals The Analysis of Periodic Order in Monolayers of Colloidal Superballs

2021 ◽  
Vol 11 (11) ◽  
pp. 5117
Author(s):  
Daniël N. ten Napel ◽  
Janne-Mieke Meijer ◽  
Andrei V. Petukhov

The characterization of periodic order in assemblies of colloidal particles can be complicated by the coincidence of Bragg diffraction peaks of the structure and minima in the form factor of the particles. Here, we demonstrate a general strategy to overcome this problem that is applicable to all low-dimensional structures. This approach is demonstrated in the application of small-angle X-ray scattering (SAXS) for the characterization of monolayers of colloidal silica superballs prepared using the unidirectional rubbing method. In this method, the ordering of the colloidal superballs is achieved by mechanically rubbing them onto a polydimethylsiloxane (PDMS)-coated surface. Using three differently shaped superballs, ranging from spherical to almost cubic, we show that certain Bragg peaks may not appear in the diffraction patterns due to the presence of minima in the form factor. We show that these missing Bragg peaks can be visualized by imaging the colloidal monolayers at various orientations. Moreover, we argue that the same strategy can be applied to other techniques, such as neutron scattering.

2019 ◽  
Vol 5 (1) ◽  
pp. 29-32
Author(s):  
Erika Linda Yani Nasution

Abstrak Telah dilakukan sintesis partikel pegilasi gadolinium karbonat dengan metode solvotermal menggunakan prekursor polietilen glikol (PEG-1000) dan gadolinium asetat hidrat (Gd(CH3CO3)3) pada suhu 180oC dengan waktu pemanasan selama 3 jam, 5 jam, dan 7 Jam. Partikel pegilasi gadolinium karbonat (Gd2(CO3)3@PEG tersebut selanjutnya dianalisis pola difraksi dan bentuk struktur dengan menggunakan X-Ray Diffraction (XRD). Hasil karakterisasi spektrum XRD terhadap partikel Gd2(CO3)3 menunjukkan pila difraksi dengan posisi puncak-puncak difraksi bersesuaian dengan JCPDS No. 37-0559 dengan puncak utama pada 2θ = 11.75o.  Pada waktu  pemanasan 3 jam , sampel memiliki sifat amorf, sedangkan pada sampel waktu pemanasan 5 jam dan 7 jam sampel-sampel memiliki derajat kekristalan yang baik. Pada waktu pemanasan 5 jam lebih tinggi kristalisasinya daripada 7 jam yang mengindikasikan kualitas kristal lebih baik pada lama pemanasan 5 jam.   Kata kunci : Gadolinium karbonat, metode solvotermal, PEG, XRD   Abstract   [Title: Analysis of XRD Characterization of Gadolinium Carbonate (Gd2 (CO3) 3 @ PEG Synthesis by Solvothermal Method] Synthesis of pegylated gadolinium carbonate particles by solvothermal method using polyethylene glycol (PEG-1000) and gadolinium acetate hydrate (Gd (CH3CO3) 3) precursors at 180oC with heating time for 3 hours, 5 hours and 7 hours. The gadolinium carbonate (Gd2 (CO3) 3 @ PEG particle pegylation was further analyzed by diffraction patterns and structural shapes using X-Ray Diffraction (XRD). The results of XRD spectrum characterization of Gd2 (CO3) 3 particles showed diffraction pila with diffraction peaks position. corresponds to JCPDS No. 37-0559 with the main peak at 2θ = 11.75 o At 3 hours of heating, the sample has amorphous properties, while the sample heating time is 5 hours and 7 hours the samples have a good degree of crystallization. 5 hours higher crystallization than 7 hours which indicates better crystal quality at 5 hours heating time.   Keywords: Gadolinium carbonate, solvothermal method, PEG, XRD


2011 ◽  
Vol 409 ◽  
pp. 492-496 ◽  
Author(s):  
Ayumi Hamaguchi ◽  
Masahiro Yoshizawa-Fujita ◽  
Yuko Takeoka ◽  
Masahiro Rikukawa

Layered perovskite (RNH3)2PbI4 (R = organic cation), which contained the fullerene derivatives, [ethyl-3-tert-butoxycarbonylaminopropyl (1,2-methanofullerene C60)]-61,61-di carboxylate iodide (EAF-I) and di [3-tert-butoxycarbonylaminopropyl (1,2-methanofullerene C60)]- 61,61-dicarboxylate diiodide (DAF-I2) in the organic layers were fabricated and compared with previously reported perovkite compound containing N-methyl-2-(4-aminophenyl)-fulleropyrrolidine iodide (AmPF-I). Because the solvent solubilities of EAF-I and DAF-I2 to N,N-dimethylformamide (DMF) were higher than AmPF-I, the film processability of EAF-I and DAF-I2 was improved compared with AmPF-I. The X-ray diffraction patterns proved the construction of the perovskite structure in (EAF)2PbI4 and (AmPF)2PbI4 cast films. EAF was well-organized and closer-packing than AmPF in the perovskite structure. For the diamine-type fullerene, DAF-I2, it is difficult to form layered structure by spin-coated or cast methods. New sharp X-ray diffraction peaks were observed for DAF-I2 films dipped in PbI2 solution. The intercalations and formation of perovskite structure of (DAF)PbI4 were studied.


2006 ◽  
Vol 514-516 ◽  
pp. 269-273
Author(s):  
Décio Dias ◽  
Rui Monteiro ◽  
Patrícia Almeida Carvalho ◽  
Alberto C. Ferro ◽  
Werner Lohwasser

The development of solid electrolytic tantalum capacitors with MnO2 as counter electrode has been carried out in order to decrease the equivalent series resistance (ESR). Capacitor samples produced under different pyrolysis conditions have been characterized in terms of equivalent circuit parameters. The Ta/Ta2O5/MnO2 system has also been characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). X-ray powder diffraction patterns obtained were inconclusive due to the MnO2 complex structure and to the presence of highly intense tantalum peaks that shadow interesting MnO2 diffraction peaks. Electron diffraction TEM results enabled the characterization of the microstructure and furthermore revealed the complex crystalline structure that affects the electrical properties of the semiconductor layer. A relation between the calculated circuit parameters and microstructure of MnO2 is discussed.


2008 ◽  
Vol 41 (5) ◽  
pp. 831-835 ◽  
Author(s):  
Alexei Vorobiev ◽  
Dmitry Chernyshov ◽  
Gennady Gordeev ◽  
Diana Orlova

The combination of magnetic and nonmagnetic interactions between the colloidal particles in ferrofluids results in various local inter-particle correlations that, in turn, change the macroscopic properties of the whole system. Therefore, characterization of the particle ensemble is a crucial point, allowing optimization of a ferrofluid for a particular application. Here it is shown how the crystal structure of the particles can be easily obtained in a fast synchrotron light diffraction experiment without any special treatment of the ferrofluid sample. Moreover, from the same diffraction patterns, such important parameters as particle mean size and dispersion are retrieved; these are compared with the corresponding parameters obtained from electron microscopy data. A particular problem of magnetite–maghemite transformation in nanoparticles stabilized by the surfactant shell is pointed out.


1997 ◽  
Vol 30 (5) ◽  
pp. 637-641 ◽  
Author(s):  
M. Megens ◽  
C. M. van Kats ◽  
P. Bösecke ◽  
W. L. Vos

Synchrotron small-angle X-ray scattering (SAXS) experiments have been performed at the ESRF on colloidal dispersions. The samples are optically multiply scattering and are aimed at so-called photonic applications. Scattering from dilute suspensions yields the particle form factor, which shows many oscillations. From these results, the radius, size distribution and information about the internal structure of the particles in situ can be determined, in contrast to most studies on colloids. Using the form factor, structure factors can be extracted from the diffraction patterns of the colloidal crystals. The structure factors clearly reveal sharp Bragg peaks. The crystal structure, lattice parameter and average orientations were determined as a function of height in sedimented samples. This provides important information for the interpretation of optical experiments.


2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.


1981 ◽  
Vol 46 (7) ◽  
pp. 1675-1681 ◽  
Author(s):  
Josef Baldrian ◽  
Božena N. Kolarz ◽  
Henrik Galina

Porosity variations induced by swelling agent exchange were studied in a styrene-divinylbenzene copolymer. Standard methods were used in the characterization of copolymer porosity in the dry state and the results were compared with related structural parameters derived from small angle X-ray scattering (SAXS) measurements as developed for the characterization of two-phase systems. The SAXS method was also used for porosity determination in swollen samples. The differences in the porosity of dry samples were found to be an effect of the drying process, while in the swollen state the sample swells and deswells isotropically.


2021 ◽  
Vol 92 (1) ◽  
pp. 013102
Author(s):  
Roberto Daniel Pérez ◽  
Juan José Leani ◽  
José Ignacio Robledo ◽  
Héctor Jorge Sánchez

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