Wet Chemical Synthesis of Germanium Nanocrystals

2005 ◽  
Vol 879 ◽  
Author(s):  
Xianmao Lu ◽  
Brian A. Korgel ◽  
Keith P. Johnston

AbstractSupercritical CO2 (sc-CO2) was first time utilized to make germanium (Ge) nanocrystals by thermolysis of diphenylgermane (DPG) or tetraethylgermane (TEG) with octanol as capping ligand at 500°C and 27.6 MPa. A new approach to prepare Ge nanocrystals of high chemical yield by reduction of GeI2 with LiAlH4 in trioctylphosphine (TOP) at 300°C is also presented. In both cases, Ge nanoparticles with high crystallinity were observed with high resolution transmission electron microscopy (HRTEM), and the presence of Ge was confirmed by X-ray diffraction (XRD) pattern. Compared to the supercritical organic solvents investigated in the previous study to make Ge nanoparticles, the reaction in sc-CO2 produced much less organic contaminants and made the removal of by-products and cleaning of the nanocrystals much easier. While Ge nanoparticles were synthesized in sc-CO2 with DPG and octanol, bulk Ge instead of nanoparticles was obtained without the presence of CO2 at the same concentration of DPG and octanol. High chemical yield of up to 75% was achieved for the Ge nanoparticles made from GeI2 with TOP, and only minimal cleaning is required to obtain Ge nanocrystals with high purity.

Minerals ◽  
2021 ◽  
Vol 11 (6) ◽  
pp. 611
Author(s):  
Celia Marcos ◽  
María de Uribe-Zorita ◽  
Pedro Álvarez-Lloret ◽  
Alaa Adawy ◽  
Patricia Fernández ◽  
...  

Chert samples from different coastal and inland outcrops in the Eastern Asturias (Spain) were mineralogically investigated for the first time for archaeological purposes. X-ray diffraction, X-ray fluorescence, transmission electron microscopy, infrared and Raman spectroscopy and total organic carbon techniques were used. The low content of moganite, since its detection by X-ray diffraction is practically imperceptible, and the crystallite size (over 1000 Å) of the quartz in these cherts would be indicative of its maturity and could potentially be used for dating chert-tools recovered from archaeological sites. Also, this information can constitute essential data to differentiate the cherts and compare them with those used in archaeological tools. However, neither composition nor crystallite size would allow distinguishing between coastal and inland chert outcrops belonging to the same geological formations.


Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2623
Author(s):  
Monika Wójcik-Bania ◽  
Jakub Matusik

Polymer–clay mineral composites are an important class of materials with various applications in the industry. Despite interesting properties of polysiloxanes, such matrices were rarely used in combination with clay minerals. Thus, for the first time, a systematic study was designed to investigate the cross-linking efficiency of polysiloxane networks in the presence of 2 wt % of organo-montmorillonite. Montmorillonite (Mt) was intercalated with six quaternary ammonium salts of the cation structure [(CH3)2R’NR]+, where R = C12, C14, C16, and R’ = methyl or benzyl substituent. The intercalation efficiency was examined by X-ray diffraction, CHN elemental analysis, and Fourier transform infrared (FTIR) spectroscopy. Textural studies have shown that the application of freezing in liquid nitrogen and freeze-drying after the intercalation increases the specific surface area and the total pore volume of organo-Mt. The polymer matrix was a poly(methylhydrosiloxane) cross-linked with two linear vinylsiloxanes of different siloxane chain lengths between end functional groups. X-ray diffraction and transmission electron microscopy studies have shown that the increase in d-spacing of organo-Mt and the benzyl substituent influence the degree of nanofillers’ exfoliation in the nanocomposites. The increase in the degree of organo-Mt exfoliation reduces the efficiency of hydrosilylation reaction monitored by FTIR. This was due to physical hindrance induced by exfoliated Mt particles.


IUCrJ ◽  
2018 ◽  
Vol 5 (4) ◽  
pp. 497-509 ◽  
Author(s):  
Paul Benjamin Klar ◽  
Iñigo Etxebarria ◽  
Gotzon Madariaga

Synchrotron single-crystal X-ray diffraction has revealed diffuse scattering alongside sharp satellite reflections for different samples of mullite (Al4+2xSi2−2xO10−x). Structural models have been developed in (3+1)-dimensional superspace that account for vacancy ordering and Al/Si ordering based on harmonic modulation functions. A constraint scheme is presented which explains the crystal-chemical relationships between the split sites of the average structure. The modulation amplitudes of the refinements differ significantly by a factor of ∼3, which is explained in terms of different degrees of ordering,i.e.vacancies follow the same ordering principle in all samples but to different extents. A new approach is applied for the first time to determine Al/Si ordering by combining density functional theory with the modulated volumes of the tetrahedra. The presence of Si–Si diclusters indicates that the mineral classification of mullite needs to be reviewed. A description of the crystal structure of mullite must consider both the chemical composition and the degree of ordering. This is of particular importance for applications such as advanced ceramics, because the physical properties depend on the intrinsic structure of mullite.


2007 ◽  
Vol 7 (2) ◽  
pp. 530-534 ◽  
Author(s):  
Chunyi Zhi ◽  
Yoshio Bando ◽  
Guozhen Shen ◽  
Chengchun Tang ◽  
Dmitri Golberg

Adopting a wet chemistry method, Au and Fe3O4 nanoparticles were functionalized on boron nitride nanotubes (BNNTs) successfully for the first time. X-ray diffraction pattern and transmission electron microscopy were used to characterize the resultant products. Subsequently, a method was proposed to fabricate heterojunction structures based on the particle-functionalized BNNTs. As a demonstration, BNNT-carbon nanostructure, BNNT-ZnO and BNNT-Ga2O3 junctions were successfully fabricated using the functionalized particles as catalysts.


Nanomaterials ◽  
2019 ◽  
Vol 9 (7) ◽  
pp. 999
Author(s):  
Yi-An Chen ◽  
Kuo-Hsien Chou ◽  
Yi-Yang Kuo ◽  
Cheng-Ye Wu ◽  
Po-Wen Hsiao ◽  
...  

To the best of our knowledge, this report presents, for the first time, the schematic of the possible chemical reaction for a one-pot synthesis of Zn0.5Cd0.5Se alloy quantum dots (QDs) in the presence of low/high oleylamine (OLA) contents. For high OLA contents, high-resolution transmission electron microscopy (HRTEM) results showed that the average size of Zn0.5Cd0.5Se increases significantly from 4 to 9 nm with an increasing OLA content from 4 to 10 mL. First, [Zn(OAc)2]–OLA complex can be formed by a reaction between Zn(OAc)2 and OLA. Then, Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD) data confirmed that ZnO is formed by thermal decomposition of the [Zn(OAc)2]–OLA complex. The results indicated that ZnO grew on the Zn0.5Cd0.5Se surface, thus increasing the particle size. For low OLA contents, HRTEM images were used to estimate the average sizes of the Zn0.5Cd0.5Se alloy QDs, which were approximately 8, 6, and 4 nm with OLA loadings of 0, 2, and 4 mL, respectively. We found that Zn(OAc)2 and OLA could form a [Zn(OAc)2]–OLA complex, which inhibited the growth of the Zn0.5Cd0.5Se alloy QDs, due to the decreasing reaction between Zn(oleic acid)2 and Se2−, which led to a decrease in particle size.


2000 ◽  
Vol 638 ◽  
Author(s):  
WK Choi ◽  
V Ng ◽  
YW Ho ◽  
TB Chen ◽  
V Ho

AbstractThe high resolution transmission electron microscopy and Raman spectroscopy results of germanium nanocrystals embedded in SiO2 synthesized by rapid thermal processing (RTA) have been presented. From the results of samples with different Ge concentrations, it was concluded that there is a narrow window in the Ge concentration that can produce nanocrystals. We also showed that it is possible to vary RTA duration or temperature to produce Ge nanocrystals with varying sizes. Our results therefore suggest that it is possible to utilize (i) annealing duration and; (ii) temperature to tune crystal sizes for optoelectronic applications.


2010 ◽  
Vol 88 (12) ◽  
pp. 1256-1261 ◽  
Author(s):  
Guifang Sun ◽  
Faming Gao ◽  
Li Hou

Boron carbonitride (BCN) nanotubes have been successfully prepared using NH4Cl, KBH4, and ZnBr2 as the reactants at 480 °C for 12 h by a new benzene-thermal approach in a N2 atmosphere. As its by-product, a new form of carbon regular hexagonal nanocages are observed. The samples are characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM), transmission electron diffraction (TED), electron energy loss spectroscopy (EELS), and high-resolution transmission electron microscopy (HRTEM). The prepared nanotubes have uniform outer diameters in the range of 150 to 500 nm and a length of up to several micrometerss. The novel carbon hexagonal nanocages have a typical size ranging from 100 nm to 1.5 µm, which could be the giant fullerene cages of [Formula: see text] (N = 17∼148). So, high fullerenes are observed for the first time. The influences of reaction temperature and ZnBr2 on products and the formation mechanism of BCN nanotubes are discussed.


2014 ◽  
Vol 07 (06) ◽  
pp. 1440001 ◽  
Author(s):  
Michał Świętosławski ◽  
Marcin Molenda ◽  
Piotr Natkański ◽  
Piotr Kuśtrowski ◽  
Roman Dziembaj ◽  
...  

Polyanionic cathode materials for lithium-ion batteries start to be considered as potential alternative for layered oxide materials. Among them, Li 2 CoSiO 4, characterized by outstanding capacity and working voltage, seems to be an interesting substitute for LiFePO 4 and related systems. In this work, structural and electrical investigations of Li 2 CoSiO 4 obtained by sol–gel synthesis were presented. Thermal decomposition of gel precursor was studied using EGA (FTIR)-TGA method. Chemical composition of the obtained material was confirmed using X-ray diffraction and energy-dispersive X-ray spectroscopy. The morphology of β- Li 2 CoSiO 4 was studied using transmission electron microscopy. High temperature electrical conductivity of Li 2 CoSiO 4 was measured for the first time. Activation energies of the electrical conductivity of two Li 2 CoSiO 4 polymorphs (β and γ) were determined. The room temperature electrical conductivity of those materials was estimated as well.


2003 ◽  
Vol 789 ◽  
Author(s):  
Hyunsuk Kim ◽  
Kyoungah Cho ◽  
Byungdon Min ◽  
Jong Soo Lee ◽  
Man Young Sung ◽  
...  

ABSTRACTPhotocurrent mechanism in a hybrid system of 1-thioglycerol and HgTe quantum dots(QDs) was studied for the first time in the intra-red (IR) range. 1-thioglycerol-capped HgTe QDs were prepared using colloidal method in aqueous solution; the synthesis and size of the HgTe QDs were examined by x-ray diffraction, Raman scattering, and high-resolution transmission electron microscopy. Absorption and photoluminescence spectra of the capped HgTe QDs revealed the strong excitonic peaks in the range from 900 to 1100nm, because of their widened band gap due to the shrinkage of their sizes to about 3 nm. The wavelength dependence of the photocurrent for the hybred system of the 1-thioglycerol and HgTe QDs was very close to that of the absorption spectrum, indicating that charge carriers photoexcited in the HgTe QDs give direct contribution to the photocurrent in the medium of 1-thioglycerol. In this hybrid system, the photo-excited electrons in the HgTe QDs are strongly confined, but the photo-excited holes act as free carriers. Hence, in the photocurrent mechanism of the this hybrid system, only holes among electron-hole pairs created by incident photons in the HgTe QDs are transferred to 1-thioglycerol surrounding HgTe QDs and contribute photocurrent flowing in the medium of 1-thioglycerol.


Author(s):  
Д.А. Ложкина ◽  
Е.В. Астрова ◽  
Р.В. Соколов ◽  
Д.А. Кириленко ◽  
А.А. Левин ◽  
...  

In this work, the processes of disproportionation of solid-phase silicon monoxide, accompanied by the formation of nanocrystalline silicon precipitates in the medium of amorphous SiOx suboxide (initial composition SiO0.9), have been studied. Based on the data of X-ray diffraction analysis and transmission electron microscopy, the dynamics of changes in the amount, concentration and size of phase precipitates of silicon with an increase in the temperature of isochronous annealing from 800 °C to 1200 °C is traced. It was found that with a monotonic increase in the total mass of the precipitated silicon, the number of its crystallization centers per unit volume nonmonotonically depends on temperature. The activation energy of diffusion of silicon atoms in the SiOx matrix was determined to be Ea1= 1.64 eV, and the activation energy of their transfer from the formed precipitates to the growth medium of SiOx was Ea2 = 2.38 eV. Anisotropic deformation of silicon crystallites precipitated during the disproportionation of SiO has been revealed for the first time. This phenomenon is associated with the difference in the specific volumes of the separated phases and the anisotropy of the growth rate of silicon precipitates formed in a solid amorphous medium.


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