Solvothermal Synthesis of CuInSe2 Nanostructured Powders: Comparing Open-Air with Applying Internal Imposed Pressure

2013 ◽  
Vol 829 ◽  
pp. 912-916 ◽  
Author(s):  
Alireza Khanaki ◽  
Hossein Abdizadeh ◽  
Mohammad Reza Golobostanfard

Nanocrystalline CuInSe2 (CIS) powders were synthesized with a simple open-air solvothermal method as well as under conditions of applying internal imposed pressure. No post-treating processes such as annealing or selenization were used in both methods. The synthesis processes involved the reaction of precursors in an autoclave for different process times. Structural, morphological, and opto-electronic properties of CIS powders were compared. X-ray diffraction patterns (XRD) confirmed the formation of chalcopyrite structure of CIS powders in both approaches at reaction temperature of 220 °C and for short process time. Field emission scanning electron microscopy (FESEM) results show that while CIS powders synthesized under the atmospheric condition are mostly agglomerated, particles have more specific shapes in samples synthesized under internal imposed pressure. Furthermore, the band gap energies of synthesized CIS powders were obtained using diffuse reflectance UV-vis spectroscopy (DRS) measurements.

2011 ◽  
Vol 236-238 ◽  
pp. 1712-1716 ◽  
Author(s):  
Hai Tao Liu ◽  
Jun Dai ◽  
Jia Jia Zhang ◽  
Wei Dong Xiang

Bismuth selenide (Bi2Se3) hexagonal nanosheet crystals with uniform size were successfully prepared via a solvothermal method at 160°C for 22 h using bismuth trichloride(BiCl3) and selenium powder(Se) as raw materials, sodium bisulfite(NaHSO3) as a reducing agent, diethylene glycol(DEG) as solvent, and ammonia as pH regulator. Various techniques such as X-ray diffraction (XRD), field-emission scanning electron microscope (FESEM), high-resolution transmission electron microscope (HRTEM), and selected area electron diffraction (SAED) were used to characterize the obtained products. Results show that the as-synthesized samples are pure Bi2Se3 hexagonal nanosheet crystals. A possible growth mechanism for Bi2Se3 hexagonal nanosheet crystals is also discussed based on the experiment.


2018 ◽  
Vol 7 (4) ◽  
pp. 372-379 ◽  
Author(s):  
Burcu Sümer Tüzün ◽  
Judit Hohmann ◽  
Bijen Kivcak

AbstractA green synthesis method of silver nanoparticles (AgNPs) usingCentaurea virgataLam. extract and the isolated compound eupatorin was investigated in this study. Ultraviolet-visible (UV-Vis) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM)/energy-dispersive X-ray (EDX) spectroscopy, thermal gravimetric analysis, X-ray diffraction analysis and zeta potential were used for characterization of AgNPs. The UV-Vis spectrum exhibited a characteristic absorption band at 420 nm for monodisperse nanoparticles. FTIR measurements also proved the formation. X-ray diffraction patterns showed peaks at (110) and (112), which are characteristic for hexagonal crystals and also showed peaks at (111), (200) and (240), which are characteristic for orthorhombic crystals. The TEM images of AgNPs show that the morphology of AgNPs was predominantly spherical. Obtained AgNPs were highly stable according to the zeta potential values. The nitric oxide scavenging activity, which is also related to anticancer activity, of AgNPs was evaluated. It can be concluded thatC. virgataLam. extract and eupatorin can be used as a reducing agent for potential antioxidant AgNP formation.


2018 ◽  
Vol 177 ◽  
pp. 01002
Author(s):  
Zhazgul Kelgenbaeva ◽  
Zhypargul Abdullaeva ◽  
Bektemir Murzubraimov

We present Au@Fe3O4 nanoparticles obtained from Fe nanoparticles and HAuCl4 using a simple solvothermal method. Trisodium citrate (C6H5Na3O7*2H2O) served as a reducing agent for Au. X-ray diffraction analysis, electronic microscopes and energy-dispersive X-ray spectroscopy revealed cubic structure, elemental composition (Au, Fe and O) and spherical shape of nanoparticles. Antibacterial activity of the sample was tested against E. coli bacteria and obtained results were discussed.


2014 ◽  
Vol 881-883 ◽  
pp. 1101-1104 ◽  
Author(s):  
Min Jie Zhou ◽  
Peng Cui

In this work, flower-like ZnIn2S4 microspheres were synthesized using a solvothermal method. The as-synthesized samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and ultraviolet-visible diffuse reflectance spectroscopy (DRS) techniques. The photocatalytic activity of the ZnIn2S4 microspheres was investigated. The ZnIn2S4 microspheres exhibit much higher photocatalytic activity than pure P25 TiO2.


2008 ◽  
Vol 8 (3) ◽  
pp. 1523-1527 ◽  
Author(s):  
Poulomi Roy ◽  
Suneel Kumar Srivastava

The present work reports the effect of reaction time on solvothermal synthesis of copper sulfides from CuCl2·2H2O and thiourea with various compositions and morphologies using ethylenediamine as solvent at 120 °C. X-ray diffraction patterns of the products at different durations shows the development of different stoichiometric composition of copper sulfides in where Cu:S ratio increases from 1.39 to 1.79 indicating transformation of Cu39S28 to Cu7S4. As inferred by EDX and XPS studies of the final products. SEM shows the growth of bundles of nanorods of length ≈1 μm and diameter in nanometer range are observed after 6 h. On increasing the reaction duration to 9 h, nanorods tends to combines with each other and growth occurs in six directions and after 12 h leads to the formation of flower-like morphology of copper sulfide. The optical properties of these products also have been studied.


2010 ◽  
Vol 03 (02) ◽  
pp. 125-129 ◽  
Author(s):  
CAIQUAN ZHANG ◽  
YALI CUI ◽  
DIDI ◽  
KUNPING YAN ◽  
CHAO CHEN ◽  
...  

Facile procedures to synthesize large quantities of uniform and well dispersed magnetite particles in water were developed through a solvothermal method. Magnetite microspheres were obtained by using FeCl 3 · 6H 2 O , urea and polyethylene glycol as the starting materials in ethylene glycol at 200°C for 8 h. The samples were characterized by using X-ray diffraction, transmission electron microscopy, scanning electron microscopy and vibrating sample magnetometry. Experimental results revealed that the particles were well dispersed with uniform particle size and diameters in the range 260 to 280 nm. The saturation magnetization value was 71.5 emu/g with negligible remanence.


Molecules ◽  
2018 ◽  
Vol 23 (12) ◽  
pp. 3150 ◽  
Author(s):  
Beñat Artetxe ◽  
Amaia Iturrospe ◽  
Pablo Vitoria ◽  
Estibaliz Ruiz-Bilbao ◽  
José S. Garitaonandia ◽  
...  

A new hybrid inorganic-organometallic salt has been obtained from the reaction of the Keggin-type silicotungstate anion with ferrocene in a water/methanol mixture as a result of the partial oxidation of ferrocene molecules to ferrocenium cations. Single-crystal X-ray diffraction analysis reveals the presence of four ferrocenium (FeIII) cations and one ferrocene (FeII) molecule per plenary Keggin anion in the crystal structure of [FeIII (Cp)2]4[SiW12O40]·[FeII(Cp)2]·2CH3OH (1). Compound 1 thus constitutes the first example in the literature in which ferrocenium and ferrocene species coexist in the structure of a polyoxometalate-based salt. The two crystallographically independent ferrocenium species in the asymmetric unit of 1 exhibit different configurations: One displays an eclipsed conformation with ideal D5h symmetry, whereas the conformation in the other one is staggered D5d. The crystal packing of 1 can be best described as an organometallic sub-lattice of ferrocenium and ferrocene species linked by a network of π-π interactions that generates rectangular cavities of about 14 × 10 Å in which strings of Keggin anions and methanol molecules are hosted, further connected to each other via weak OPOM···CMeOH-OMeOH···OPOM type hydrogen bonds. The charge-transfer nature of the salt has been studied by solid-state diffuse reflectance UV-Vis spectroscopy and the presence of magnetically isolated FeIII/FeII centres has been confirmed by Mössbauer spectroscopy. A topological study carried out on all of the pristine ferrocenyl species deposited in the Cambridge Structural Database (CSD) has allowed two main conclusions to be drawn: (1) these species tend to adopt extreme conformations (either eclipsed or staggered) with less than a 15% of examples showing intermediate states and (2) the oxidation state of the iron centres can be unequivocally assigned on the basis of a close inspection of the Fe···Cp distances, which allows ferrocene neutral molecules and ferrocenium cations to be easily distinguished.


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


2015 ◽  
Vol 70 (10) ◽  
pp. 705-709
Author(s):  
Qiu-Li Tu ◽  
Hong-Dan Wang ◽  
Sheng-Chun Chen ◽  
Ming-Yang He ◽  
Qun Chen

AbstractA coordination polymer {[Mn(BDC-Cl4)(DMF)4](H2BDC-Cl4)}n (1) (H2BDC-Cl4 = 2,3,5,6-tetrachloro-1,4-benzenedicarboxylic acid) was synthesized by a resin-assisted solvothermal method and isolated by a flotation method in carbon tetrachloride. Complex 1 shows a one-dimensional wave-like coordination structure in the solid state. It is readily dissolved in water. The complex has been characterized using elemental analysis, IR spectroscopy, molecular conductivity, thermogravimetric analysis, and single-crystal and powder X-ray diffraction techniques.


2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Shuisheng Wu ◽  
Qian Dong ◽  
Jun Wang ◽  
Qingming Jia ◽  
Yanlin Sun ◽  
...  

Novel BiOBr hierarchical microspheres have been successfully prepared via a facile microwave-assisted solvothermal route and used for visible-light photocatalytic degradation of RhB. The phase and morphology of the products were characterized by powder X-ray diffraction (XRD), thermogravimetric analysis (TG), scanning electron microscopy (SEM), BET, and UV-vis diffuse reflectance spectra. The SEM observations displayed that BiOBr flower-like nanostructure assembled from nanosheets. The BiOBr flower-like nanostructure, with a narrow band gap (2.63 eV), shows excellent photocatalytic activity in the degradation of RhB dye under visible-light, much higher than those of BiOBr nanosheet and P25 photocatalysts.


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