Glasses in the ternary system Cr2O3-PbO-P2O5 were prepared by direct melting of the mixture with stoichiometric proportions of the reagents Cr2O3, PbO and (NH4)2HPO4 at 1080℃. The glasses obtained are transparent in ...Glasses in the ternary system Cr2O3-PbO-P2O5 were prepared by direct melting of the mixture with stoichiometric proportions of the reagents Cr2O3, PbO and (NH4)2HPO4 at 1080℃. The glasses obtained are transparent in colour and have a non-hygroscopic appearance. The study of the dissolution rate was carried out on ternary glasses xCr2O3-(45-x)PbO-55P2O5 with (1 ≤ x ≤ 4;mol%), immersed in distilled water at 90℃ for 24 days, indicating a maximum of chemical durability when the level of chromium oxide passed through 2 mol%. Both, IR spectra and X-ray diffraction have indicated the predominance of metaphosphate or cyclic metaphosphate groups with some traces of isolated orthophosphate groups when the Cr2O3 content is equal to x = 2. Analysis of the density values also, has showed a maximum density for x = 2 mol%. The covalent radius values of oxygen have indicated that the minimum value rcal (O2–) is observed for x = 2 mol% and therefore a relatively high reinforcement of the metal-oxygen-phosphorus (Cr-O-P) bonds. SEM Micrographs have exhibited two phases, a vitreous phase and a crystalline phase. The radical change in the structure from ultraphosphate Q3 groups to ring metaphosphate Q2 and orthophosphate groups Q0 seems to be the cause of the formation of crystallites. Beyond 2 mol% of Cr2O3, the structure of the glass changed relatively and the orthophosphate phases increased to the detriment of the metaphosphate phases. We observed a decrease in chemical durability. However, it was confirmed that the dissolution rate (DR) of the S2 analysed compound is comparable to the values of borosilicate glasses which are used as alternative materials for the immobilisation of nuclear waste substances.展开更多
Chromium iron phosphate glass was investigated for use as waste form because of its improved chemical durability. The introduction of chromium in sodium-iron-phosphate glass is used to compare its effect with iron in ...Chromium iron phosphate glass was investigated for use as waste form because of its improved chemical durability. The introduction of chromium in sodium-iron-phosphate glass is used to compare its effect with iron in inhibition of corrosion. The sodium-chromium-iron phosphate glass of composition 10Na2O-30Fe2O3-5Cr2O3-55P2O5 (mol%) was produced by melting batches of (99, 98% pure) Cr2O3, Fe2O3, Na2CO3, and (NH4)2HPO4 at 1080°C for one hour and pouring the liquid into steel mold. The sample was annealed at 680°C for 48 h. We have performed the measurement of X-Ray Diffraction (XRD), Scanning Electronic Microscopy (SEM), Infra-Red spectroscopy (IR), and the chemical durability. The IR of the glass studied, contains two dominant bands, which were characteristic of pyrophosphate groups, (P-O) stretching mode of P-O non bridging oxygen at 1055 cm-1 and sym stretching mode of bridging oxygen at444 cm-1 respectively. There is also a band at603 cm-1 attributed to isolated tetrahedral units (PO4)3-. The chemical durability of the glass was investigated by measuring the weight loss in distilled water at 90°C for 22 days.展开更多
Various characterization techniques were used to study the composition of the glass series xAl2O3-(40 - x)CaO-10Na2O-50P2O5 (with 0 ≤ x ≤ 10) in terms of chemical durability, X-ray diffraction, IR spectroscopy and s...Various characterization techniques were used to study the composition of the glass series xAl2O3-(40 - x)CaO-10Na2O-50P2O5 (with 0 ≤ x ≤ 10) in terms of chemical durability, X-ray diffraction, IR spectroscopy and scanning electron microscopy (SEM). The improved chemical durability was attributed to the replacement of easily hydrated P-O-P bonds by covalent and resistant Ca-O-P and Al-O-P bonds. However, the change in the dissolution rate (DR) versus time showed a marked decrease in chemical durability with increasing the Al2O3 content to the detriment of the CaO content. The X-ray diffraction analysis of glasses annealed at 550°C and 660°C for 48 hours indicated the presence of pyrophosphate phases and predominant metaphosphates or cyclic metaphosphate phases when the Al2O3 content was ≤7.5 mol%. Nevertheless, both, X-ray diffraction and IR spectroscopy confirmed the structural tendency change from metaphosphate (Q2) and pyrophosphate structural units (Q1). Toward short isolated orthophosphate units (Q0) when the Al2O3 content above 7.5 mol%. SEM micrographs illustrated that the number of crystallites increased in the glass network when the Al2O3 content increased at the expense of the CaO content. An increase in the Al2O3 content to 10 mol% led to the formation of a larger number of crystallites of different sizes, dominated by small crystallite sizes assigned to short isolated orthophosphate groups. This phenomenon led to a decrease in chemical durability and seems to be a favorable factor for the formation of the apatite layers which enclose the glass, in a SBF solution test, able of regenerating bone tissue in biomedical application.展开更多
The regular melting-quenching method allowed isolating very large vitreous domains within the ternary system Li2O-P2O5-Fe2O3 at 1100. The vitrification and crystallization effects are discussed in terms of phosphorus ...The regular melting-quenching method allowed isolating very large vitreous domains within the ternary system Li2O-P2O5-Fe2O3 at 1100. The vitrification and crystallization effects are discussed in terms of phosphorus pentaoxide concentration (mol%). In the course of the present study, we analyzed chemical durability along the glass domain and many sample glasses were isolated. We noticed that our compounds demonstrated very high chemical resistance to attack, even with very highly concentrated mineral acid solutions. This behavior can be assigned to the presence of poorly crystalline phases in these glasses, which tended to increase as the Fe2O3 content increased. This property is a prerequisite for many interesting industrial applications. XRD, IR spectroscopy and SEM micrographs allowed an efficient investigation of the structural changes versus composition within ternary diagrams. The results were found to be consistent with the regular structural changes of phosphate glasses.展开更多
Melt quenched “SnO2(50-x)PbO:50V2O5” glass system containing x = 5, 10, 15 in molar ratio has been investigated. Effects of heating rate, glass transition, crystallization, melting temperature and infrared spectra o...Melt quenched “SnO2(50-x)PbO:50V2O5” glass system containing x = 5, 10, 15 in molar ratio has been investigated. Effects of heating rate, glass transition, crystallization, melting temperature and infrared spectra of SnO2 substituted PbO-V2O5 glass system are reported. XRD results show that perfect vitrification has been achieved for all the glass samples after annealing at 150°C. DSC results have indicated that eutectic composition of the lead metavanadate has been maintained for all the glass systems up to 15 mole% of substitution. IR spectra for a SnO2 substitution of 5 mole% V=O stretching frequency occur at 966 cm-1 without appearance of any additional peak. But for 10 mole% and 15 mole% SnO2 substituted samples, additional peaks appear at 1023 and 1005 cm-1 indicating the effect of SnO2 in the vanadate crystalline matrix such that there is an elongation of V=O bond. Since the crystalline matrix is affected, we can expect similar effect in the glass matrix also.展开更多
The spherical CaCO3 composite was synthesized in the presence of the amphiphilic block copolymer, i.e. polystyrene-b-poly(acrylic acid). It was revealed by XRD analysis that the grains in the composite was calcite wit...The spherical CaCO3 composite was synthesized in the presence of the amphiphilic block copolymer, i.e. polystyrene-b-poly(acrylic acid). It was revealed by XRD analysis that the grains in the composite was calcite with great distortion. Infared and Raman analysis showed that the composite was composed of PS-b-PAA calcium salt and calcite, and the calcite was nano-scaled.展开更多
文摘Glasses in the ternary system Cr2O3-PbO-P2O5 were prepared by direct melting of the mixture with stoichiometric proportions of the reagents Cr2O3, PbO and (NH4)2HPO4 at 1080℃. The glasses obtained are transparent in colour and have a non-hygroscopic appearance. The study of the dissolution rate was carried out on ternary glasses xCr2O3-(45-x)PbO-55P2O5 with (1 ≤ x ≤ 4;mol%), immersed in distilled water at 90℃ for 24 days, indicating a maximum of chemical durability when the level of chromium oxide passed through 2 mol%. Both, IR spectra and X-ray diffraction have indicated the predominance of metaphosphate or cyclic metaphosphate groups with some traces of isolated orthophosphate groups when the Cr2O3 content is equal to x = 2. Analysis of the density values also, has showed a maximum density for x = 2 mol%. The covalent radius values of oxygen have indicated that the minimum value rcal (O2–) is observed for x = 2 mol% and therefore a relatively high reinforcement of the metal-oxygen-phosphorus (Cr-O-P) bonds. SEM Micrographs have exhibited two phases, a vitreous phase and a crystalline phase. The radical change in the structure from ultraphosphate Q3 groups to ring metaphosphate Q2 and orthophosphate groups Q0 seems to be the cause of the formation of crystallites. Beyond 2 mol% of Cr2O3, the structure of the glass changed relatively and the orthophosphate phases increased to the detriment of the metaphosphate phases. We observed a decrease in chemical durability. However, it was confirmed that the dissolution rate (DR) of the S2 analysed compound is comparable to the values of borosilicate glasses which are used as alternative materials for the immobilisation of nuclear waste substances.
文摘Chromium iron phosphate glass was investigated for use as waste form because of its improved chemical durability. The introduction of chromium in sodium-iron-phosphate glass is used to compare its effect with iron in inhibition of corrosion. The sodium-chromium-iron phosphate glass of composition 10Na2O-30Fe2O3-5Cr2O3-55P2O5 (mol%) was produced by melting batches of (99, 98% pure) Cr2O3, Fe2O3, Na2CO3, and (NH4)2HPO4 at 1080°C for one hour and pouring the liquid into steel mold. The sample was annealed at 680°C for 48 h. We have performed the measurement of X-Ray Diffraction (XRD), Scanning Electronic Microscopy (SEM), Infra-Red spectroscopy (IR), and the chemical durability. The IR of the glass studied, contains two dominant bands, which were characteristic of pyrophosphate groups, (P-O) stretching mode of P-O non bridging oxygen at 1055 cm-1 and sym stretching mode of bridging oxygen at444 cm-1 respectively. There is also a band at603 cm-1 attributed to isolated tetrahedral units (PO4)3-. The chemical durability of the glass was investigated by measuring the weight loss in distilled water at 90°C for 22 days.
文摘Various characterization techniques were used to study the composition of the glass series xAl2O3-(40 - x)CaO-10Na2O-50P2O5 (with 0 ≤ x ≤ 10) in terms of chemical durability, X-ray diffraction, IR spectroscopy and scanning electron microscopy (SEM). The improved chemical durability was attributed to the replacement of easily hydrated P-O-P bonds by covalent and resistant Ca-O-P and Al-O-P bonds. However, the change in the dissolution rate (DR) versus time showed a marked decrease in chemical durability with increasing the Al2O3 content to the detriment of the CaO content. The X-ray diffraction analysis of glasses annealed at 550°C and 660°C for 48 hours indicated the presence of pyrophosphate phases and predominant metaphosphates or cyclic metaphosphate phases when the Al2O3 content was ≤7.5 mol%. Nevertheless, both, X-ray diffraction and IR spectroscopy confirmed the structural tendency change from metaphosphate (Q2) and pyrophosphate structural units (Q1). Toward short isolated orthophosphate units (Q0) when the Al2O3 content above 7.5 mol%. SEM micrographs illustrated that the number of crystallites increased in the glass network when the Al2O3 content increased at the expense of the CaO content. An increase in the Al2O3 content to 10 mol% led to the formation of a larger number of crystallites of different sizes, dominated by small crystallite sizes assigned to short isolated orthophosphate groups. This phenomenon led to a decrease in chemical durability and seems to be a favorable factor for the formation of the apatite layers which enclose the glass, in a SBF solution test, able of regenerating bone tissue in biomedical application.
文摘The regular melting-quenching method allowed isolating very large vitreous domains within the ternary system Li2O-P2O5-Fe2O3 at 1100. The vitrification and crystallization effects are discussed in terms of phosphorus pentaoxide concentration (mol%). In the course of the present study, we analyzed chemical durability along the glass domain and many sample glasses were isolated. We noticed that our compounds demonstrated very high chemical resistance to attack, even with very highly concentrated mineral acid solutions. This behavior can be assigned to the presence of poorly crystalline phases in these glasses, which tended to increase as the Fe2O3 content increased. This property is a prerequisite for many interesting industrial applications. XRD, IR spectroscopy and SEM micrographs allowed an efficient investigation of the structural changes versus composition within ternary diagrams. The results were found to be consistent with the regular structural changes of phosphate glasses.
文摘Melt quenched “SnO2(50-x)PbO:50V2O5” glass system containing x = 5, 10, 15 in molar ratio has been investigated. Effects of heating rate, glass transition, crystallization, melting temperature and infrared spectra of SnO2 substituted PbO-V2O5 glass system are reported. XRD results show that perfect vitrification has been achieved for all the glass samples after annealing at 150°C. DSC results have indicated that eutectic composition of the lead metavanadate has been maintained for all the glass systems up to 15 mole% of substitution. IR spectra for a SnO2 substitution of 5 mole% V=O stretching frequency occur at 966 cm-1 without appearance of any additional peak. But for 10 mole% and 15 mole% SnO2 substituted samples, additional peaks appear at 1023 and 1005 cm-1 indicating the effect of SnO2 in the vanadate crystalline matrix such that there is an elongation of V=O bond. Since the crystalline matrix is affected, we can expect similar effect in the glass matrix also.
文摘The spherical CaCO3 composite was synthesized in the presence of the amphiphilic block copolymer, i.e. polystyrene-b-poly(acrylic acid). It was revealed by XRD analysis that the grains in the composite was calcite with great distortion. Infared and Raman analysis showed that the composite was composed of PS-b-PAA calcium salt and calcite, and the calcite was nano-scaled.
