The elegant 2D multiquantum (MQ) MAS NMR has been applied to investigate the coordination of Al atoms in SAPO-34. The results show that the effects of the template and/or water on the coordination of Al atoms are sig...The elegant 2D multiquantum (MQ) MAS NMR has been applied to investigate the coordination of Al atoms in SAPO-34. The results show that the effects of the template and/or water on the coordination of Al atoms are significant, which lead to the formation of various Al species. Up to four kinds of Al species are distinctly resolved.展开更多
The coordination structure of aluminum in magnesium aluminum hydroxide was studied by 27Al NMR. The result showed that tetrahedral aluminum (AlIV) existed in magnesium aluminum hydroxide, and the contents of AlIV inc...The coordination structure of aluminum in magnesium aluminum hydroxide was studied by 27Al NMR. The result showed that tetrahedral aluminum (AlIV) existed in magnesium aluminum hydroxide, and the contents of AlIV increased with the increase of the ratio of Al/Mg and with the peptizing temperature. AlIV originated from the so-called Al13 polymer with the structure of one Al tetrahedron surrounded by twelve Al octahedrons.展开更多
The IR spectrum and 11B and 27Al MAS NMR spectra of Al18B4O33 are presented and discussed in relation to the possible existence of boron atoms substituting for aluminum atoms. The IR spectrum shows that the strong vi...The IR spectrum and 11B and 27Al MAS NMR spectra of Al18B4O33 are presented and discussed in relation to the possible existence of boron atoms substituting for aluminum atoms. The IR spectrum shows that the strong vibrations of the BO3 groups are present in the 1 500-1 200 cm-1 region, and very weak bands of BO4 units are present in the region from 1 000 to 1 100 cm-1. 11B MAS NMR spectrum indicates that the strong signal for BO3 units appears in the region from δ+5 to δ+20, and the very weak signal for BO4 units is at about δ- 1, while 27Al MAS NMR spectrum shows five peaks at about δ+62, +42. 1, +14, -4. 7 and -6. 4, originating from AlO4, AlO4, AlO5, AlO6 and AlO6, respectively. These results reveal that there are minor BO4 units in Al18B4O33, indicating that a small amount of B atoms substitute for Al atoms in the 4-fold coordination.展开更多
In this study,the effects of low temperature on aluminum(Ⅲ)(Al)hydrolysis were examined both theoretically and experimentally by constructing a solubility diagram for amorphous aluminum hydroxide(Al(OH)_3(am))and a d...In this study,the effects of low temperature on aluminum(Ⅲ)(Al)hydrolysis were examined both theoretically and experimentally by constructing a solubility diagram for amorphous aluminum hydroxide(Al(OH)_3(am))and a distribution diagram of hydrolyzed Al species.First,thermodynamic data of Al species at 4℃were calculated from that at 25℃.A well confirmed polymeric Al species, AlO_4Al_(12)(OH)_(24)^(7+)(Al_(13)),was involved in building the diagrams and,correspondingly,the non-linear simultaneous equations wit...展开更多
The microstructural study was conducted on cement and cement-slag pastes immersed in different concentrations of Mg（NO3）2 solutions utilizing ^29Si, ^27Al NMR spectroscopy and XRD techniques. The results show that t...The microstructural study was conducted on cement and cement-slag pastes immersed in different concentrations of Mg（NO3）2 solutions utilizing ^29Si, ^27Al NMR spectroscopy and XRD techniques. The results show that the hydration of both the cement and cement-slag pastes is delayed when the pastes are cured in Mg（NO3）2 solutions as compared to the pastes cured in water. Moreover, Mg^2＋ ions also exhibit an decalcifying and dealuminizing effect on the C-A-S-H in cement and cement-slag pastes, and thereby decrease Ca/Si and Al[4]/Si ratios of the C-A-S-H. The dealuminization of C-A-S-H is mitigated for cement-slag paste as compared to pure cement paste. The depolymerized calcium and aluminum ions from C-A-S-H gel mainly enter the pore solution to maintain the pH value and form Al^[6] in TAH, respectively. On the other hand, Mg^2＋ ions exert an impact on the intra-transition between Al^[6] species, from AFm and hydrogarnet to hydrotalcite-like phase. NO3^-ions are interstratified in the layered Mg-Al structure and formed nitrated hydrotalcite-like phase（Mg1-xAlx（OH）2（NO3）x·nH2O）. Results from both ^27Al NMR and XRD data show that ettringite seems not to react with Mg^2＋ ions.展开更多
Al Ferron timed complex colorimetric method (AFM) and 27 Al NMR spectroscopy method(ANM) were discussed. For the former, the different colorimetric reagent preparation methods' results indicate that the...Al Ferron timed complex colorimetric method (AFM) and 27 Al NMR spectroscopy method(ANM) were discussed. For the former, the different colorimetric reagent preparation methods' results indicate that there are some differences beteween them, and the combined method can be used as a simplified procedure. For the latter, the small tube method is more accurate. Eventually, the Al 13 (ANM) was compared to the Al b (AFM).展开更多
A new heteropolycomplex, K 6H 3[ZnW 11 O 40 Al]·9 5H 2O was prepared and characterized by means of elemental analysis, IR, UV spectroscopy, 27 Al NMR , electrochemistry and X ray crystall...A new heteropolycomplex, K 6H 3[ZnW 11 O 40 Al]·9 5H 2O was prepared and characterized by means of elemental analysis, IR, UV spectroscopy, 27 Al NMR , electrochemistry and X ray crystallography. The crystal of K 6H 3[ZnW 11 O 40 Al]·9 5H 2O is cubic, space group Fm 3m , with lattice constants a=b=c =2 144 8(2) nm, V =9 866(2) nm 3, Mo radiation, R =0 057 8 for 497 independent data with [ I>2δ(I) ]. The anion is of α type Keggin structure with C s symmetry.展开更多
To investigate the influence of preparation process on the properties of synthesized C4AF,the powder was prepared via the self-propagating combustion reaction（SPCR）method using urea as fuel and metal nitrates as cat...To investigate the influence of preparation process on the properties of synthesized C4AF,the powder was prepared via the self-propagating combustion reaction（SPCR）method using urea as fuel and metal nitrates as cation precursors.Synthesis mechanism of the SPCR method,calculation and adjusting principles of urea dosage were detailedly introduced.Material characterization of synthesized C4AF was performed with the aid of X-ray diffractometry,Fourier transform infrared spectrometry,scanning electron microscopy,energydispersive X-ray spectroscopy,^27Al nuclear magnetic resonance and isothermal microcalorimetric technique.Remaining content of transition phase of calcium carbonate in synthesized C4AF was determined by quantitative analysis of X-ray diffractometry.It was found that there was no difference in the hydration behavior of C4AF synthesized by the SPCR method and the traditional solid-state reaction（SSR）method.C3AH6 and amorphous iron（III）hydroxide（Fe（OH）3）would be formed during the hydration of C4AF while CH not.Crystallite size of synthesized C4AF was 16.1 A and the apparent activation energy was 36.2 kJ/mol.Coordinated condition of Al in C4AF can be detected by ^27Al NMR technique,but the peaks were broadened and the intensities were relatively low,supporting the use of ^27Al NMR for the quantitative analysis of C3A in Portland cements.展开更多
基金We are grateful to the support of the National Natural Science Foundation of China and the Ministry of Science and Technology of China. We appreciate Dr. R. Fu (NHMFL Tallahassee) for his kind help regarding the MQ MAS NMR experiments.
文摘The elegant 2D multiquantum (MQ) MAS NMR has been applied to investigate the coordination of Al atoms in SAPO-34. The results show that the effects of the template and/or water on the coordination of Al atoms are significant, which lead to the formation of various Al species. Up to four kinds of Al species are distinctly resolved.
基金This research is supported by NNSFC No:20273041.
文摘The coordination structure of aluminum in magnesium aluminum hydroxide was studied by 27Al NMR. The result showed that tetrahedral aluminum (AlIV) existed in magnesium aluminum hydroxide, and the contents of AlIV increased with the increase of the ratio of Al/Mg and with the peptizing temperature. AlIV originated from the so-called Al13 polymer with the structure of one Al tetrahedron surrounded by twelve Al octahedrons.
基金Supported by the National Natural Science Foundation of China.
文摘The IR spectrum and 11B and 27Al MAS NMR spectra of Al18B4O33 are presented and discussed in relation to the possible existence of boron atoms substituting for aluminum atoms. The IR spectrum shows that the strong vibrations of the BO3 groups are present in the 1 500-1 200 cm-1 region, and very weak bands of BO4 units are present in the region from 1 000 to 1 100 cm-1. 11B MAS NMR spectrum indicates that the strong signal for BO3 units appears in the region from δ+5 to δ+20, and the very weak signal for BO4 units is at about δ- 1, while 27Al MAS NMR spectrum shows five peaks at about δ+62, +42. 1, +14, -4. 7 and -6. 4, originating from AlO4, AlO4, AlO5, AlO6 and AlO6, respectively. These results reveal that there are minor BO4 units in Al18B4O33, indicating that a small amount of B atoms substitute for Al atoms in the 4-fold coordination.
文摘In this study,the effects of low temperature on aluminum(Ⅲ)(Al)hydrolysis were examined both theoretically and experimentally by constructing a solubility diagram for amorphous aluminum hydroxide(Al(OH)_3(am))and a distribution diagram of hydrolyzed Al species.First,thermodynamic data of Al species at 4℃were calculated from that at 25℃.A well confirmed polymeric Al species, AlO_4Al_(12)(OH)_(24)^(7+)(Al_(13)),was involved in building the diagrams and,correspondingly,the non-linear simultaneous equations wit...
基金Funded by National Natural Science Foundation of China(Nos.51778513,51402003,51578004)China Ministry of Science and Technology(No.2015CB655101)
文摘The microstructural study was conducted on cement and cement-slag pastes immersed in different concentrations of Mg（NO3）2 solutions utilizing ^29Si, ^27Al NMR spectroscopy and XRD techniques. The results show that the hydration of both the cement and cement-slag pastes is delayed when the pastes are cured in Mg（NO3）2 solutions as compared to the pastes cured in water. Moreover, Mg^2＋ ions also exhibit an decalcifying and dealuminizing effect on the C-A-S-H in cement and cement-slag pastes, and thereby decrease Ca/Si and Al[4]/Si ratios of the C-A-S-H. The dealuminization of C-A-S-H is mitigated for cement-slag paste as compared to pure cement paste. The depolymerized calcium and aluminum ions from C-A-S-H gel mainly enter the pore solution to maintain the pH value and form Al^[6] in TAH, respectively. On the other hand, Mg^2＋ ions exert an impact on the intra-transition between Al^[6] species, from AFm and hydrogarnet to hydrotalcite-like phase. NO3^-ions are interstratified in the layered Mg-Al structure and formed nitrated hydrotalcite-like phase（Mg1-xAlx（OH）2（NO3）x·nH2O）. Results from both ^27Al NMR and XRD data show that ettringite seems not to react with Mg^2＋ ions.
文摘Al Ferron timed complex colorimetric method (AFM) and 27 Al NMR spectroscopy method(ANM) were discussed. For the former, the different colorimetric reagent preparation methods' results indicate that there are some differences beteween them, and the combined method can be used as a simplified procedure. For the latter, the small tube method is more accurate. Eventually, the Al 13 (ANM) was compared to the Al b (AFM).
文摘A new heteropolycomplex, K 6H 3[ZnW 11 O 40 Al]·9 5H 2O was prepared and characterized by means of elemental analysis, IR, UV spectroscopy, 27 Al NMR , electrochemistry and X ray crystallography. The crystal of K 6H 3[ZnW 11 O 40 Al]·9 5H 2O is cubic, space group Fm 3m , with lattice constants a=b=c =2 144 8(2) nm, V =9 866(2) nm 3, Mo radiation, R =0 057 8 for 497 independent data with [ I>2δ(I) ]. The anion is of α type Keggin structure with C s symmetry.
基金Funded partly by the National“973”Program of China(No.2015CB655101)National Natural Science Foundation of China(No.51379163)
文摘To investigate the influence of preparation process on the properties of synthesized C4AF,the powder was prepared via the self-propagating combustion reaction（SPCR）method using urea as fuel and metal nitrates as cation precursors.Synthesis mechanism of the SPCR method,calculation and adjusting principles of urea dosage were detailedly introduced.Material characterization of synthesized C4AF was performed with the aid of X-ray diffractometry,Fourier transform infrared spectrometry,scanning electron microscopy,energydispersive X-ray spectroscopy,^27Al nuclear magnetic resonance and isothermal microcalorimetric technique.Remaining content of transition phase of calcium carbonate in synthesized C4AF was determined by quantitative analysis of X-ray diffractometry.It was found that there was no difference in the hydration behavior of C4AF synthesized by the SPCR method and the traditional solid-state reaction（SSR）method.C3AH6 and amorphous iron（III）hydroxide（Fe（OH）3）would be formed during the hydration of C4AF while CH not.Crystallite size of synthesized C4AF was 16.1 A and the apparent activation energy was 36.2 kJ/mol.Coordinated condition of Al in C4AF can be detected by ^27Al NMR technique,but the peaks were broadened and the intensities were relatively low,supporting the use of ^27Al NMR for the quantitative analysis of C3A in Portland cements.
