scholarly journals One-step preparation of metal-free phthalocyanine with controllable crystal form

2021 ◽  
Vol 10 (1) ◽  
pp. 95-100
Author(s):  
Xiaolong Li ◽  
Yuxi Feng ◽  
Chenyang Li ◽  
Huahui Han ◽  
Xueqing Hu ◽  
...  
Keyword(s):  
Ball Milling ◽  
Crystal Form ◽  
Milling Process ◽  
X Ray Diffraction ◽  
Step Method ◽  
Metal Free ◽  
Crystal Stability ◽  
Organic Optoelectronics ◽  
Different Temperatures ◽  
One Step

Abstract Metal-free phthalocyanine (H2Pc) has been widely used as photosensitive semiconductors in the organic optoelectronics field because of its unique planar molecular structure and high photocarriers’ generation efficiency. Herein, this paper related to a new facile and efficient one-step method for preparing specific crystal form of H2Pc with high crystallinity through ball-milling process, in which α-H2Pc can be prepared directly by dry ball-milling, and β-H2Pc and X-H2Pc can be simply obtained through wet ball-milling in butanone solvent at different temperatures. X-ray diffraction (XRD) was used to characterize the crystal stability of α-H2Pc, β-H2Pc, and X-H2Pc, which revealed that all the three crystalline H2Pc prepared had excellent crystal stability under different mechanical conditions.

Structural Evaluation of Ti-22.2Si-11.1B Powders Milled with PCA Addition

2008 ◽  
Vol 591-593 ◽  
pp. 147-153
Author(s):  
Gilbert Silva ◽  
Erika Coaglia Trindade Ramos ◽  
N.S. da Silva ◽  
Alfeu Saraiva Ramos
Keyword(s):  
Electron Microscopy ◽  
Ball Milling ◽  
Ball Mill ◽  
Milling Process ◽  
Argon Atmosphere ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structural Evaluation ◽  
Equilibrium Structures ◽  
Scanning Electron

A large amount of the Ti6Si2B compound can be formed by mechanical alloying and subsequent heat treatment from the elemental Ti-22.2at%Si-11.1at%B powder mixture, but the yield powder after ball milling is reduced due to an excessive agglomeration of ductile particles on the balls and vial surfaces. This work reports on the structural evaluation of Ti-22.2at%Si-11.1at%B powders milled with PCA addition, varying its amount between 1 and 2 wt-%. The milling process was carried out in a planetary ball mill under argon atmosphere, and the milled powders were then heated at 1200oC for 1h under Ar atmosphere in order to obtain equilibrium structures. Samples were characterized by X-ray diffraction, scanning electron microscopy, and thermal analysis. Results revealed that the PCA addition reduced the excessive agglomeration during the ball milling of Ti-22.2at-%Si-11.1at-%B powders. After heating at 1200oC for 1h, the Ti5Si3, Ti3O and/or Ti2C phases were preferentially formed in Ti-22.2at%Si-11.1at%B powders milled with PCA addition, and the Ti6Si2B formation was inhibited.

High-Energy Ball Milling and Sintering of Ti-2Ta-22Si-11B and Ti-6Ta-22Si-11B Powders Mixtures

2014 ◽  
Vol 802 ◽  
pp. 20-24 ◽  
Author(s):  
Lucas Moreira Ferreira ◽  
Luciano Braga Alkmin ◽  
Érika C.T. Ramos ◽  
Carlos Angelo Nunes ◽  
Alfeu Saraiva Ramos
Keyword(s):  
Ball Milling ◽  
Weight Ratio ◽  
High Energy ◽  
Milling Process ◽  
Wet Milling ◽  
X Ray Diffraction ◽  
Heat Treated ◽  
Equilibrium Structures ◽  
Rotary Speed ◽  
Steel Balls

The milling process of elemental Ti-2Ta-22Si-11B and Ti-6Ta-22Si-11B (at-%) powder mixtures were performed in a planetary Fritsch P-5 ball mill using stainless steel vials (225 mL) and hardened steel balls (19 mm diameter). Ball-to-powder weight ratio of 10:1 and a rotary speed of 300 rpm were adopted, varying the milling time. Wet milling (isopropyl alcohol) for 20 more minutes was used to increase the yield powder in to the vial. Following the Ti-Ta-Si-B powders milled for 600 min were heat-treated at 1100°C for 1 h in order to obtain the equilibrium structures. The milled powders and heat-treated samples were characterized by X-ray diffraction, scanning electron microscopy, and energy dispersive spectrometry. Supersaturated Ti solid solutions were formed during ball milling of Ti-Ta-Si-B powders while that the Ti5Si3 phase was formed after milling for 620 min of the Ta-richer powder mixture only. The particles sizes were initially increased during the initial milling times, and the wet milling provided the yield powder into the vials. A large amount of pores was found in both the sintered samples which presented the formation of the TiSS,(ss-solid solution) Ti6Si2B and TiB.

Microstructure and Oxidation Resistance of Mechanically Alloyed and Sintered Ni-Nb and Ni-Nb-Ta Alloys

2017 ◽  
Vol 899 ◽  
pp. 19-24
Author(s):  
Lucas Moreira Ferreira ◽  
Stephania Capellari Rezende ◽  
Antonio Augusto Araújo Pinto da Silva ◽  
Gael Yves Poirier ◽  
Gilberto Carvalho Coelho ◽  
...  
Keyword(s):  
Ball Milling ◽  
Oxidation Resistance ◽  
Energy Dispersive Spectrometry ◽  
High Energy ◽  
Milling Process ◽  
Ternary Alloys ◽  
X Ray Diffraction ◽  
Mechanically Alloyed ◽  
Static Oxidation ◽  
Energy Ball

The present work reports on the microstructure and oxidation resistance of Ni-25Nb, Ni-20Nb-5Ta and Ni-15Nb-10Ta alloys produced by high-energy ball milling and subsequent sintering. The sintered samples were characterized by optical microscopy, scanning electron microscopy, X-ray diffraction, energy dispersive spectrometry, and static oxidation tests. Homogeneous microstructures of the binary and ternary alloys indicated the major presence of the β-Ni3Nb compound as matrix, which dissolved large amounts of tantalum. Consequently, the β-Ni3Nb peaks moved toward the direction of smaller diffraction angles. Iron contamination lower than 6.7 at.-% was detected by EDS analysis, which were picked-up during the previous ball milling process. After the static oxidation tests (1100°C for 4 h) the sintered Ni-25Nb, Ni-20Nb-5Ta and Ni-15Nb-10Ta alloys presented mass gains of 31.5%, 30.5% and 28.8%, respectively. Despite the higher densification of the Ni-15Nb-10Ta alloy, the results suggested that the tantalum addition contributed to improve the oxidation resistance of the β-Ni3Nb compound.

Processing of Nano Hydroxyapatite from Eggshell and Seashell

2010 ◽  
Vol 659 ◽  
pp. 159-164 ◽  
Author(s):  
Gréta Gergely ◽  
Ferenc Wéber ◽  
Mihály Tóth ◽  
Attila Lajos Tóth ◽  
Zsolt E. Horváth ◽  
...  
Keyword(s):  
Heat Treatment ◽  
Grain Size ◽  
Ball Milling ◽  
Milling Process ◽  
Effect Of Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Attrition Milling ◽  
Milling Method ◽  
Scanning Electron

Hydroxyapatite (HAp) was successfully produced from recycled eggshell, seashell and phosphoric acid by using two different type of milling method (attrition milling and ball milling). According to the analysis, the attrition milling resulted nanosize HAp even after milling, while the ball milling process provided HAp only after a 400oC, 2 h long heat treatment. The grain size in both cases were approximately preserved during the heat treatment. The effect of temperature on stoichiometry, morphology and crystallinity of HAp powders were investigated. The structures of the HAp were characterized by X-ray diffraction and Scanning Electron Microsopy.

An Investigation on the Application of Cryogenic Ball Milling to Ibuprofen Particle and Its Characteristics

2006 ◽  
Vol 505-507 ◽  
pp. 355-360 ◽  
Author(s):  
Kyong Yop Rhee ◽  
Hyun Kab Cho ◽  
Jai Sung Hong
Keyword(s):  
Particle Size ◽  
Ball Milling ◽  
Weight Ratio ◽  
Milling Process ◽  
X Ray Diffraction ◽  
Chemical Changes ◽  
Ball Milling Process ◽  
Particle Size Analyzer ◽  
Before And After ◽  
Size Of Particles

For a present study, a cryogenic ball milling process was applied to reduce the Ibuprofen particles to submicron in order to enlarge their dissolution rate. The cryogenic ball milling was performed using 6 mm zirconia balls at a temperature of -180 °C or lower. The effects of milling time, the weight ratio of ball to Ibuprofen, and milling speed on the particle size were investigated. SEM and particle size analyzer were used to analyze the shape and size of particles before and after ball milling. The chemical changes before and after the cryogenic ball milling process were examined through XRD (x-ray diffraction) analysis. The results show that the size of Ibuprofen particles was reduced to about 1/20 of its initial size and the particle size showed negligible change after six hours of ball milling. The effect of weight ratio and the milling speed on the particle size was almost negligible. The results also show that cryogenic ball milling yielded no chemical changes in the particle.

The Modulus Formalism Used in the Dielectric Analysis with Optical Characterization of Hydroxyapatite and CaTi4P6O24 Ceramic Formers by Dry Ball Milling

2006 ◽  
Vol 514-516 ◽  
pp. 1087-1093 ◽  
Author(s):  
Cléber C. Silva ◽  
Manuel A. Valente ◽  
Manuel P.F. Graça ◽  
António S. B. Sombra
Keyword(s):  
Ball Milling ◽  
Relaxation Times ◽  
Milling Process ◽  
Dielectric Study ◽  
X Ray Diffraction ◽  
Raman Scattering Spectroscopy ◽  
Muscle Tissues ◽  
Phosphate Phase ◽  
Mineral Constituent

The bioceramic hydroxiapatite [Ca10(PO4)6 (OH)2 – HAP] is the main mineral constituent of teeth and bones with excellent biocompatibility with hard and muscle tissues. These materials exhibit several problems of handling and fabrication, which can be overcome by mixing them with a suitable binder. The dry milling process of fabrication of HAP presents the advantage that melting is not necessary and the powder obtained is nanocrystalline. The HAP has been obtained from three different experimental procedures (HAPA: Ca(H2PO4)2 + Ca(OH)2; HAPB: Ca(H2PO4)2 + CaCO3; and HAPC: CaHPO4 + CaCO3). In the reactions HAPA and HAPB the hydroxiapatite phase was obtained after 5, 10 and 15 hours of milling and after 15 hours in the reaction HAPC. In order to improve the mechanical properties of HAP, calcium phosphate ceramics with titanium (CaP-Ti) has been prepared by dry ball milling (Ca(H2PO4)2 + TiO2). The calcium titanium phosphate phase, CaTi4P6O24, was obtained. The dielectric study in function of frequency, at constant temperature of the ceramics, was made using the Modulus (M*) formalism and a distribution of relaxation times was observed. The values of the dielectric constant of the ceramics measured at room temperature are between 5.04 (CaP-Ti_5H) and 13.70 (HAPA_10H). The structure of the samples was studied by X-Ray diffraction, infrared and Raman scattering spectroscopy.

Effect of Annealing Temperatures on the Microstructure of CuInS2 Thin Film by One-Step Electrodeposition

2010 ◽  
Vol 150-151 ◽  
pp. 530-533 ◽  
Author(s):  
Lin Lu ◽  
Yan Jie Wang ◽  
Xiao Gang Li
Keyword(s):  
Thin Film ◽  
Nir Spectroscopy ◽  
Chalcopyrite Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Annealing Temperatures ◽  
Photovoltaic Applications ◽  
Different Temperatures ◽  
One Step ◽  
Cuins2 Film

CuInS2 thin film used for photovoltaic applications was prepared by one-step electrodeposition. The films were annealed at different temperatures of 350, 400, 500 °C. Effects of annealing temperatures on the properties of the film were investigated by the way of X-ray diffraction (XRD), scanning electron microscopy (SEM) and UV-Vis-NIR Spectroscopy. The result shows that CuInS2 film with chalcopyrite structure can be successfully prepared by one-step electrodeposition. Annealing is effective in improving the crystallinity of the thin film. The temperature of 400°C is favorable to the grain growth of the film without the generation of impurity.

Effect of Ball Milling Process on Electrochemical Properties of Copper Hexacyanoferrate Active Material for Calcium-Ion Batteries

2019 ◽  
Vol 803 ◽  
pp. 109-114
Author(s):  
Ha Jin Lee ◽  
Du Yeol Kim ◽  
Soon Ki Jeong
Keyword(s):  
Electrochemical Properties ◽  
Ball Milling ◽  
Calcium Ion ◽  
Crystal Surface ◽  
Active Material ◽  
Milling Process ◽  
X Ray Diffraction ◽  
Copper Hexacyanoferrate ◽  
Sem Images ◽  
Ball Milling Process

This study investigates the electrochemical properties of ball-milled copper hexacyanoferrate (CuHCF), a Prussian blue analogue, as a cathode material in aqueous calcium-ion batteries (CIBs). X-ray diffraction analysis confirmed that the ball milling process did not destroy the crystal structure of the CuHCF active material. The general grain size and crystal surface of the synthesized CuHCF active materials were confirmed from the scanning electron microscopy (SEM) images. The electrochemical test results revealed that prolonged ball milling improved the charge/discharge capacity in the initial cycle. After 200 cycles, structural collapse of the CuHCF electrode occurred, as observed by SEM.

Structural Evaluation of Mechanically Alloyed Ti-Nb Powders

2008 ◽  
Vol 591-593 ◽  
pp. 141-146 ◽  
Author(s):  
Y.A. Giffoni ◽  
Erika Coaglia Trindade Ramos ◽  
Hugo Ricardo Zschommler Sandim ◽  
M.T.T. Pacheco ◽  
Gilbert Silva ◽  
...  
Keyword(s):  
Ball Milling ◽  
Energy Dispersive Spectrometry ◽  
Structural Heterogeneity ◽  
Milling Process ◽  
X Ray Diffraction ◽  
Mechanically Alloyed ◽  
Structural Evaluation ◽  
Crystallite Sizes ◽  
Homogeneous Structures ◽  
Final Amount

This work discusses on the structural evaluation of mechanically alloyed Ti-Nb powders. The Nb amount was varied between 20 and 50 wt-%. The milling process was carried out in a planetary Fritsch P-5 ball mill under Ar atmosphere. The structural evaluation was conducted by scanning electron microscopy, X-ray diffraction, and energy dispersive spectrometry. During ball milling it was noted an excessive agglomeration of ductile Ti-Nb powders on the balls and vial surfaces, and the final amount of remaining powders was then drastically reduced into the vials. This fact was more pronounced with the increased Nb amount in starting powders. Typical lamella structures were formed during ball milling, which were refined for the longest milling times, and fine and homogeneous structures were formed in Ti-Nb (Nb=20-50wt-%) powders. XRD results indicated that the full width at half maximum values of Ti peaks were continuously increased while that the crystallite sizes were reduced for longer milling times due to the severe plastic deformation provided during ball milling of Ti-Nb powders. However, the EDS analysis revealed the presence of Nb-rich regions in Ti-Nb powders after ball milling. The critical ball milling behavior of ductile Ti- Nb powders contributed for reducing the yield powder and increasing the structural heterogeneity.

Polymorph control of 5-fluorouracil during ball milling process

CrystEngComm ◽  
2021 ◽  
Author(s):  
Fenghua Chen ◽  
Jie Fan ◽  
Xiuzhi Chen ◽  
Yanping Li ◽  
Chengfeng Liang ◽  
...  
Keyword(s):  
Ball Milling ◽  
Milling Process ◽  
Ball Milling Process ◽  
One Step

Polymorph control of 5-fluorouracil (5-FU) was achieved by ball milling. Form II was synthesized through one-step neat grinding of raw 5-FU (RFU), and Form III (a new polymorph) was obtained...

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