Structural Studies of Potassium Hexatitanates Prepared under Hydrothermal and Solid State Conditions

2006 ◽  
Vol 517 ◽  
pp. 222-226 ◽  
Author(s):  
Rosiyah Yahya ◽  
A. Hassan ◽  
Z. Aiyub

The structural studies of potassium hexatitanates prepared under both hydrothermal and solid state conditions were carried out. Fourier Transform Infra-red spectroscopy (FTIR) results revealed that potassium hexatitanate structure consisted of TiO6 octahedral units irrespective of the preparative conditions and particle size. X-ray diffraction (XRD) results showed that the only potassium hexatitanate phase was detectable and the structure is of the Wadsley-type consisting of chains of Ti-O octahedral sharing edges with tunnels in which the potassium ions are located. From scanning electron microscopy (SEM) results, the different preparative conditions resulted in different particle sizes and morphologies of the potassium hexatitanate formed.

Author(s):  
M. Shah ◽  
D. Patel

Oxcarbazepine has low solubility and low oral bioavailability, so it’s a challenge to formulate suitable dosage form. In this present investigation, to improve the dissolution rate and solubility, skimmed milk is used as a carrier. Physical mixers were prepared using various drugs to carrier ratio and spray drying technology was used to develop solid dispersion with the carrier. Various techniques were used to characterize the solid dispersion immediately after they were made which includes differential scanning calorimetry, scanning electron microscopy, fourier transform infra- red spectroscopy, X-ray diffraction and in-vitro dissolution profiles. The differential scanning calorimetry thermograms of raw drug indicated of its anhydrous crystalline nature. In thermograms of solid dispersion, the characteristic peak was absent suggesting the change from crystalline nature to amorphous form. X-ray diffraction confirmed those results. X-ray diffraction results of raw drug showed highly intense peak characteristic of its crystalline nature where solid dispersion showed less intense, more diffused peak indicating the change in crystalline form. Fourier transforms infra-red spectroscopy studies showed there was no interaction between drug and carrier. Scanning electron microscopy support the amorphous nature of mixer. The whole formulation showed distinct enhancement in the drug release behavior and solubility. The optimum oxcarbazepine to skimmed milk ratio 1:3 enhances the in-vitro drug release by 3.5 fold and also show distinct increase in solubility. It was concluded that for improvement of solubility of poorly water soluble oxcarbazepine, skimmed milk powder as a carrier can be utilize very well.


1998 ◽  
Vol 13 (9) ◽  
pp. 2588-2596 ◽  
Author(s):  
K. H. Ryu ◽  
J-M. Yang

The low temperature pressureless sintering of a nanosized Si3N4 powder with doped sintering additives was investigated. The microstructural evolution during sintering at different temperatures was analyzed using x-ray diffraction and scanning electron microscopy. The effect of using nanosized Si3N4 powder as a catalyst to accelerate the α→β–Si3N4 transformation of a commercial Si3N4 powder with larger particle sizes was also investigated. Finally, two stage sintering was used to study the feasibility of controlling the microstructure and the mechanical properties of the nanosized silicon nitride.


2004 ◽  
Vol 836 ◽  
Author(s):  
S. L. Wang ◽  
S. H. Lee ◽  
A. Gupta ◽  
A. D. Compaan

ABSTRACTCd1-xMnxTe alloy films with band gaps of 1.6 ∼ 1.8 eV have been deposited by RF magnetron sputtering for solar-cell applications. The films have been treated by chloride vapors to improve the photovoltaic performance. These as-deposited and chloride-treated CdMnTe films have been investigated by Raman spectroscopy, x-ray diffraction (XRD) and scanning electron microscopy (SEM). Raman results indicate that Te and/or TeO2 exists in the annealed samples depending on anneal conditions.


2008 ◽  
Vol 55-57 ◽  
pp. 873-876 ◽  
Author(s):  
N. Chaiyo ◽  
R. Muanghlua ◽  
A. Ruangphanit ◽  
Wanwilai C. Vittayakorn ◽  
Naratip Vittayakorn

A corundum-type structure of cobalt niobate (Co4Nb2O9) has been synthesized by a solid-state reaction. The formation of the Co4Nb2O9 phase in the calcined powders was investigated as a function of calcination conditions by differential thermal analysis (DTA) and X-ray diffraction (XRD) techniques. Morphology and particle size have been determined by scanning electron microscopy (SEM). It was found that the minor phases of unreacted Co3O4 tend to form together with the columbite CoNb2O6 phase at a low calcination temperature and short dwell time. It seems that the single-phase of Co4Nb2O9 in a corundum phase can be obtained successfully at the calcination conditions of 900°C for 60 min, with heating/cooling rates of 20°C /min.


1994 ◽  
Vol 339 ◽  
Author(s):  
M. Tuominen ◽  
R. Yakimova ◽  
R. C. Glass ◽  
T. Tuomi ◽  
E. Janzén

ABSTRACTFor high-power device applications SiC has better physical and electronic properties than the traditional semiconductor materials Si and GaAs. In this work, structural defects of 4H SiC wafers have been studied and partly compared with results from a previous study of 6H material. Optical microscopy, scanning electron microscopy, high-resolution X-ray diffraction and synchrotron X-ray topography were used for structural studies of 4H SiC.Optical micrographs show micropipes and larger specific defects - tubes and cracks. X-ray rocking curve peaks are broad and split revealing the mosaicity of the material. Synchrotron X-ray topographs show areas having a large number of defects, images of cracks and micropipes, and misorientated regions close to the micropipes.


2014 ◽  
Vol 215 ◽  
pp. 158-162
Author(s):  
Liudmila E. Bykova ◽  
V.G. Myagkov ◽  
I.A. Tambasov ◽  
O.A. Bayukov ◽  
Victor S. Zhigalov ◽  
...  

A simple method for obtaining ZnO-Fe3O4 nanocomposites using solid-state reaction Zn + 3Fe2O3 ZnO + 2Fe3O4 is suggested. An analysis of the characteristics and properties of ZnO-Fe3O4 nanocomposites was carried out by a combination of structural and physical methods (X-ray diffraction, scanning electron microscopy, photoelectron spectroscopy, Mössbauer measurements, X-ray fluorescent analysis, and magnetic measurements). The magnetization of the hybrid ZnO-Fe3O4 films is equal to 440 emu/cm3. The resulting Fe3O4 nanoparticles are surrounded by a ZnO shell and have sizes ranging between 20 and 40 nm.


2016 ◽  
Vol 1 (2) ◽  
Author(s):  
Veni Dayu Putri

<p><strong>ABSTRAK</strong></p><p><strong> </strong></p><p>Pembuatan lapisan tipis kalsium fosfat dari kalsium nitrat tetrahidrad (Ca(NO<sub>3</sub>)<sub>2</sub>.4H<sub>2</sub>O) sebagai prekursor kalsium dan asam fosfat (H<sub>3</sub>PO<sub>4</sub>) sebagai <em>prekursor</em> fosfat dengan variasi perbandingan mol Ca/P 1.50 , 1.60 , 1.67 , 1.70 dan 1.80 melalui metode sol-gel telah dilakukan. Sol yang didapat dibakar pada suhu 1000<sup>o</sup>C sehingga terbentuk powder kalsium fosfat berwarna putih. Powder yang didapat dianalisis menggunakan Fourier Transform Infra Red Spectroscopy (FTIR), X-Ray Diffraction (XRD) dan Scanning Electron Microscopy (SEM). Analisis FTIR menunjukkan adanya serapan gugus PO<sub>4</sub><sup>3-</sup>, O-H, H<sub>2</sub>O, CO<sub>2</sub>, dan P<sub>2</sub>O<sub>7</sub><sup>4-</sup>. Difraksi sinar-X dari powder yang terbentuk memberikan puncak pada sudut 2θ yang berbeda yaitu <em>Calsium Pyrophospate</em> (Ca<sub>2</sub>P<sub>2</sub>O<sub>7</sub>) dan <em>Hydroxyapatite</em> HAP (Ca<sub>10</sub>(PO<sub>4</sub>)<sub>6</sub>(OH)<sub>2 </sub>pada perbandingan molar Ca/P 1.80 . Analisis SEM menghasilkan <em>Hydroxyapatite </em>dan <em>Calsium Pyrophospate </em>dengan distribusi partikel yang tidak merata dan berbentuk <em>spheric</em>. Proses pelapisan dilakukan pada plat kaca yaitu pada perbandingan mol Ca/P 1.80 menggunakan metode dip-coating dan kemudian dipanaskan pada suhu 400<sup>o</sup>C. Hasil analisa XRD pada lapisan kalsium fosfat memperlihatkan bahwa senyawa yang terbentuk berbentuk amorf. Sedangkan analisis menggunakan SEM memperlihatkan bahwa lapisan tipis kalsium fosfat memiliki morfologi permukaan yang halus, rapat, homogen dan berbentuk <em>speric</em>.</p><p> </p><p>         <strong><em>Kata kunci</em></strong> : kalsium fosfat, <em>hydroxyapatite</em>, <em>dip-coating</em>, metode sol-gel</p><p> </p><p><strong>ABSTRACT</strong></p><p align="center"><strong> </strong></p><p><em>Preparation a thin layer of calcium phosphate using tetrahidrad calcium nitrate (Ca(NO<sub>3</sub>)<sub>2</sub>.4H<sub>2</sub>O) as a precursor of calcium and phosphoric acid (H<sub>3</sub>PO<sub>4</sub>) as a precursor of phosphate with a variation of the mole ratio Ca/P 1.50; 1.60, 1.67, 1.70 and 1.80 through the sol-gel method have been done. Sol obtained burned at a temperature of 1000<sup>o</sup>C to form white powder of calcium phosphate. Powder obtained were analyzed using Fourier Transform Infra Red Spectroscopy (FTIR), X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). FTIR analysis showed absorption PO<sub>4</sub><sup>3-</sup> group,  O-H, H<sub>2</sub>O, CO<sub>2</sub>, and P<sub>2</sub>O<sub>7</sub><sup>4-</sup>. X-ray diffraction from powder formed providing a peak at an angle 2θ different namely Calcium Pyrophospate (Ca<sub>2</sub>P<sub>2</sub>O<sub>7</sub>) and Hydroxyapatite HAP (Ca<sub>10</sub>(PO<sub>4</sub>)<sub>6</sub>(OH)<sub>2</sub>) at a molar ratio of Ca/P 1.80. Analysis of SEM produces Hydroxyapatite and Calcium Pyrophospate with particle distribution is uneven and shaped spheric. The coating process performed on glass plates with mole ratio of Ca/P 1.80 using a dip-coating and then heated at a temperature of 400<sup>o</sup>C. XRD analysis on a layer of calcium phosphate showed that the compound formed shaped amorphous. While using SEM analysis showed the morphology of thin layer of calcium phosphate are smooth, dense, homogeneous and shaped speric.</em></p><p><em> </em></p><p><em>         <strong>Keywords :</strong> calcium phosphate, hydroxyapatite, dip-coating, sol-gel method</em></p>


2011 ◽  
Vol 239-242 ◽  
pp. 924-929 ◽  
Author(s):  
Shu Ai Chen ◽  
Jing Kun Xu ◽  
Bao Yang Lu ◽  
Xue Min Duan ◽  
Fang Fang Kong

Conducting polymers poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(3,4-ethylenedithiathiophene) (PEDTT) have been synthesized by solid-state polymerization of 2,5-dibromo-3,4-ethylenedioxythiophene (DBEDOT) and 2,5-dibromo-3,4-ethylenedithiathiophene (DBEDTT) respectively in air and under vacuum. Both polymers were completely insoluble in common organic solvents and retained partial crystal structure of monomers as indicated by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses. Thermoelectric tests showed that PEDTT exhibited Seebeck coefficient about 120 µV K−1at 170 K, which is higher than PEDOT, while the later exhibited higher electrical conductivity (0.1S cm-1at 298 K) and better thermal stability indicated by the thermal analyses. These results showed that replacement of oxygen by sulfur in the monomer structure played an important role on the properties of polymers.


Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2557
Author(s):  
Chloé Cherpin ◽  
Derek Lister ◽  
Frédéric Dacquait ◽  
Lihui Liu

Spinel ferrite compounds continue to receive a lot of attention due to their unique properties. Among the numerous synthesis routes existing, the solid-state method was applied for the production of nickel ferrite, by introducing the use of a quartz vial. A mixture of nickel oxide (NiO) and hematite (Fe2O3) was ground and vacuum-sealed in the vial and different thermal treatment programs were tested. The resulting particles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectroscopy. For temperatures, below 1000 °C, the solid-state reaction is not complete as nickel oxide (NiO) and hematite (Fe2O3) are still present. The reaction time is a decisive parameter for the morphology of the particles obtained. If, for different reaction times, the particle size distribution is always between 0.3 and 1.7 µm, a longer reaction time leads to the formation of dense, interconnected clusters of particles. Optimal parameters to synthesize a pure phase of spherical nickel ferrite were sought and found to be a reaction temperature of 1000 °C for 72 h.


2020 ◽  
Vol 16 (2) ◽  
pp. 171
Author(s):  
Wahyuni Wahyuni ◽  
Subaer Subaer ◽  
Nurhayati Nurhayati

Telah dilakukan penelitian tentang geopolimer berbasis fly ash dengan penambahan abu sekam padi. Penelitian ini bertujuan untuk mengetahui struktur dan sifat mekanik geopolimer berbasis fly ash dengan penambahan abu sekam padi. Geopolimer berbasis fly ash dibuat dengan penambahan abu sekam padi 0%, 20% dan 40% menggunakan metode aktivasi alkali dan dipanaskan pada suhu 70℃ selama 2 jam. Struktur mikro dari sampel  diketahui dengan menggunakan teknik X-Ray Diffraction (XRD) dan menggunakan Scanning Electron Microscopy (SEM). Gugus fungsi dari sampel diperoleh berdasarkan pengujian Fourier Transform Infra Red (FTIR). Sifat mekanik seperti Kuat tekan dari sampel diuji menggunakan Testing Mechine. Massa jenis, porositas dan kuat lentur dilakukan pengukuran terhadap sampel. Hasil penelitian menunjukkan diperoleh fase trydimate yang tertinggi pada sampel Geo FA+ASP (60+40)%. Hasil karakterisasi Scanning Elektron Microscopy (SEM) menunjukkan material penyusun sampel telah berikatan dengan baik walaupun sebagian kecil pertikel fly ash dan abu sekam padi masih terlihat dengan jelas. Gugus fungsi pembentuk geopolimer diperoleh pada stretching Si-O-Si dengan nilai gelombang antara 478-461cm-1 dan 791-781cm-1. Massa jenis tertinggi diperoleh pada sampel dengan penambahan 40% abu sekam padi dan porositas tertinggi diperoleh pada sampel tanpa penambahan abu sekam padi. Kuat tekan yang terbesar diperoleh dari sampel geopolimer berbasis fly ash tanpa penambahan abu sekam padi sedangkan kuat lentur tertingi diperoleh dari sampel geopolimer berbasis fly ash dengan  penambahan abu sekam padi sebesar 40%.


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