Aluminum hydroxide adjuvant exhibits a poorly crystalline boehmite(PCB)structure,which demonstrates instability during prolonged storage.In the present study,we systematically investigated the quality alterations of t...Aluminum hydroxide adjuvant exhibits a poorly crystalline boehmite(PCB)structure,which demonstrates instability during prolonged storage.In the present study,we systematically investigated the quality alterations of the adjuvant stored at roo m temperature by analyzing its crystal structure,particle size distribution,electron microscopic characteristics,pH,isoelectric point(pI),and adsorption capacity.These assessments aimed to ensure the effectiveness and safety of vaccine production.Three batches of adjuvants were stored at room temperature for 15 months,and their changes were monitored using X-ray diffraction patterns,transmission electron microscopy(TEM),pH measurements,pI determination,and adsorption capacity analysis.X-ray diffraction revealed that the crystalline phases of aluminum hydroxide initially exhibited a PCB structure,which became progressively more ordered during storage.Notably,after 12 months,a new diffraction peak emerged at 18.2°2θ,with its intensity increasing over time.This corresponded to the formation of highly crystalline gibbsite and bayerite,which compromised the stability of the adjuvant.Furthermore,the pH and pI values decreased during storage,reflecting a decline in the chemical stability of the adjuvant.Comprising nanoparticles with a mean diameter of 130 nm,the adjuvant maintained a high surface area and excellent adsorption capacity.The adsorption rate at 8 mg BSA/mg Al3+consistently exceeded 97%,with no statistically significant differences observed between the adsorption capacities at 1 and 15 months(P>0.05).This indicated that the nanoparticle aluminum hydroxide adjuvant sustained high adsorption efficiency throughout the storage period,underscoring its reliability as a vaccine adsorbent.However,in the later stages of storage,the emergence of highly crystalline gibbsite and bayerite,coupled with declines in pH and pI,negatively impacted the adjuvant’s stability.Based on these findings,we recommended that aluminum hydroxide adjuvants should not be stored at room temperature for longer than 12 months to preserve their quality and efficacy.展开更多
Different structure models of a long-period ordered phase in Fe-C martenstie formed during aging have been checked by computer simulation of electron diffraction(ED) patterns based on these models.The results showed t...Different structure models of a long-period ordered phase in Fe-C martenstie formed during aging have been checked by computer simulation of electron diffraction(ED) patterns based on these models.The results showed that the simulated ED pattern of γ'-FexC(Ⅱ) model proposed by the present authors is in good agreement with experimentally observed ED pattern.It was also confirmed that the incommensurate superperiod stems from the coexistence of several γ'-Fe_xC(H) phases with different superperiods.The Fe(144)C(24)(Fe6C) model proposed by Uwakweh et al.generated ED patterns remarkably different from the experimental ones.展开更多
Transmission electron microscopy (TEM) is a very powerful technique for materials characteriza-tion, providing information relating to morphology, composition, and crystal structure. Selected area diffraction patterns...Transmission electron microscopy (TEM) is a very powerful technique for materials characteriza-tion, providing information relating to morphology, composition, and crystal structure. Selected area diffraction patterns (SADPs) are crystallographic data that can be obtained using a TEM in-strument. Conventional identification through SADP/TEM is tricky and tedious, thereby increasing the difficulty of phase identification. To establish a procedure for phase identification of known and unknown phases, in this study we examined two samples: one, a known phase, was Si with alignment;the other, unknown, was the TixOy phase at the 96.4Au-3Ni-0.6Ti interlayer/ yttria-stabilized zirconia (YSZ) interface of a steel/96.4Au-3Ni-0.6Ti interlayer/YSZ joint. The procedures for phase identification of the known and unknown phases are described herein using a series of SADPs and energy dispersive spectrometry within TEM that would be useful for general researchers.展开更多
Effects of multiple strengthening treatments （i.e. ag mechanical properties and stability of nanoscale prec in this research. Various tests such as hardness, tensi ng either at three or four consecutive temperatures...Effects of multiple strengthening treatments （i.e. ag mechanical properties and stability of nanoscale prec in this research. Various tests such as hardness, tensi ng either at three or four consecutive temperatures） on pitated phases in an AA2090 alloy have been evaluated e, electrical resistance, differential scanning calorimetric （DSC）, and transmission electron microscopy （TEM） have been performed. The results show that the ultimate tensile strength （UTS） and the yield strength of the samples aged at four consecutive temperatures （i.e. natural aging＋190℃＋150℃＋100℃） can be increased approximately to 660 and 610 MPa, respectively. It is also found that precipitation of T1 phase occurs during multiple aging process of the alloy and the higher amounts of enthalpies shown in DSC charts are linked to higher volume fraction of this precipitate. Furthermore, TEM observations reveal that T1 phase has plate shape morphology and its crystal structure is in the form of hcp with lattice parameters of a=0.467 nm and c=0.878 nm.展开更多
Sr0.6 Ba0.4 Nb2 O6 micro-rods are prepared by the molten-salt method with K2 SO4,KCl-K2 SO4,and KCl as fluxes.It reveals that the Sr0.6 Ba0.4 Nb2 O6 synthesized with KCl as a flux exhibits a single phase with tetragon...Sr0.6 Ba0.4 Nb2 O6 micro-rods are prepared by the molten-salt method with K2 SO4,KCl-K2 SO4,and KCl as fluxes.It reveals that the Sr0.6 Ba0.4 Nb2 O6 synthesized with KCl as a flux exhibits a single phase with tetragonal tungsten bronze structure.The measurement of X-ray diffraction indicates that the Sr0.6 Ba0.4 Nb2 O6 micro-rods synthesized at 1 300℃are anisotropic.The morphology of the powers is examined by transmission electron microscope.It reveals that the length-diameter ratio of Sr0.6 Ba0.4 Nb2 O6 micro-rods increases with increasing annealing temperature from 900℃to 1 300℃.At 1 300℃,the rod possesses a large length-diameter ratio of 8∶1.Moreover,the analysis of the piezoelectric properties of single micro-rods using apiezo-response force microscope indicates that the domains of the material are arranged along its radial direction.展开更多
The recrystallization behavior of 98.5% cold rolled high purity aluminum foils annealed at 300 ℃ was investigated,and the evolution of the microstructures was followed by electron back scattered diffraction(EBSD).The...The recrystallization behavior of 98.5% cold rolled high purity aluminum foils annealed at 300 ℃ was investigated,and the evolution of the microstructures was followed by electron back scattered diffraction(EBSD).The results show that the recrystallization process of the high purity aluminum foils at 300 ℃ is a mixture of discontinuous-and continuous-recrystallization.The orientations of the recrystallization nuclei include not only the cube orientation,but also other orientations such as some near deformation texture components which are the results of strong recovery process.However,such continuously recrystallized grains are usually associated with relatively high free energy,so they would be consumed by the discontinuously-recrystallized grains(cube-oriented grains)in subsequent annealing.On the other hand,the pattern quality index of recrystallized grains shows dependence on the crystal orientation which might introduce some errors into evaluating volume fraction of recrystallization by integrating pattern quality index of EBSD.展开更多
It is well known that the lattice waves in alloy can be looked upon as the superposition of a series of plane waves with different wave vectors. Because of these plane wave′s diffraction action for X photon, there ar...It is well known that the lattice waves in alloy can be looked upon as the superposition of a series of plane waves with different wave vectors. Because of these plane wave′s diffraction action for X photon, there are two satellites (sidebands) around X ray main diffraction peak. With the wavelength and asymmetric factor α y of rectangle wave of the distribution of concentration introduced, the amplitude of modulation wave appearing along some crysallographic direction can be expressed clearly in the form of a sum of several diffraction wave vectors in the reciprocal space, and the diffracted intensity can be obtained. The X ray diffraction angle of sidebands strongly depends on the distribution of the wavelength. Fig.1b gives the simulated X ray diffraction profiles. It shows that when we fix the average modulated wavelength and change the distribution of wavelength, the angle difference between the satellite and main diffraction peak varies correspondingly. The simulated diffraction profiles are in good agreement with experimental results [1] (Fig.1a). The more diffuse the distribution of wavelength is, the nearer the sidebands are to main peak, and vice versa. In addition, the intensity and position of satellite are obviously restricted by the asymmetric factor of wave shape. Any lattice wave propagating in crystal can be resolved along coordinate axes. On the basis of the principle of superposition, all compositions of the lattice wave have diffraction profiles of themselves. Add two diffraction patterns perpendicular to each other on the reciprocal plane which is normal to the projected direction, we get the simulated TEM diffraction pattern of spinodal decomposition. Fig.2a is the TEM pattern by Kubo H [2] , Fig.2b and 2c are the simulated TEM patterns by Kubo H [2] and Khachaturyan A G [3] respectively. Our simulated TEM pattern (Fig.2d) is in good agreement with Fig.2a.展开更多
文摘Aluminum hydroxide adjuvant exhibits a poorly crystalline boehmite(PCB)structure,which demonstrates instability during prolonged storage.In the present study,we systematically investigated the quality alterations of the adjuvant stored at roo m temperature by analyzing its crystal structure,particle size distribution,electron microscopic characteristics,pH,isoelectric point(pI),and adsorption capacity.These assessments aimed to ensure the effectiveness and safety of vaccine production.Three batches of adjuvants were stored at room temperature for 15 months,and their changes were monitored using X-ray diffraction patterns,transmission electron microscopy(TEM),pH measurements,pI determination,and adsorption capacity analysis.X-ray diffraction revealed that the crystalline phases of aluminum hydroxide initially exhibited a PCB structure,which became progressively more ordered during storage.Notably,after 12 months,a new diffraction peak emerged at 18.2°2θ,with its intensity increasing over time.This corresponded to the formation of highly crystalline gibbsite and bayerite,which compromised the stability of the adjuvant.Furthermore,the pH and pI values decreased during storage,reflecting a decline in the chemical stability of the adjuvant.Comprising nanoparticles with a mean diameter of 130 nm,the adjuvant maintained a high surface area and excellent adsorption capacity.The adsorption rate at 8 mg BSA/mg Al3+consistently exceeded 97%,with no statistically significant differences observed between the adsorption capacities at 1 and 15 months(P>0.05).This indicated that the nanoparticle aluminum hydroxide adjuvant sustained high adsorption efficiency throughout the storage period,underscoring its reliability as a vaccine adsorbent.However,in the later stages of storage,the emergence of highly crystalline gibbsite and bayerite,coupled with declines in pH and pI,negatively impacted the adjuvant’s stability.Based on these findings,we recommended that aluminum hydroxide adjuvants should not be stored at room temperature for longer than 12 months to preserve their quality and efficacy.
文摘Different structure models of a long-period ordered phase in Fe-C martenstie formed during aging have been checked by computer simulation of electron diffraction(ED) patterns based on these models.The results showed that the simulated ED pattern of γ'-FexC(Ⅱ) model proposed by the present authors is in good agreement with experimentally observed ED pattern.It was also confirmed that the incommensurate superperiod stems from the coexistence of several γ'-Fe_xC(H) phases with different superperiods.The Fe(144)C(24)(Fe6C) model proposed by Uwakweh et al.generated ED patterns remarkably different from the experimental ones.
文摘Transmission electron microscopy (TEM) is a very powerful technique for materials characteriza-tion, providing information relating to morphology, composition, and crystal structure. Selected area diffraction patterns (SADPs) are crystallographic data that can be obtained using a TEM in-strument. Conventional identification through SADP/TEM is tricky and tedious, thereby increasing the difficulty of phase identification. To establish a procedure for phase identification of known and unknown phases, in this study we examined two samples: one, a known phase, was Si with alignment;the other, unknown, was the TixOy phase at the 96.4Au-3Ni-0.6Ti interlayer/ yttria-stabilized zirconia (YSZ) interface of a steel/96.4Au-3Ni-0.6Ti interlayer/YSZ joint. The procedures for phase identification of the known and unknown phases are described herein using a series of SADPs and energy dispersive spectrometry within TEM that would be useful for general researchers.
文摘Effects of multiple strengthening treatments （i.e. ag mechanical properties and stability of nanoscale prec in this research. Various tests such as hardness, tensi ng either at three or four consecutive temperatures） on pitated phases in an AA2090 alloy have been evaluated e, electrical resistance, differential scanning calorimetric （DSC）, and transmission electron microscopy （TEM） have been performed. The results show that the ultimate tensile strength （UTS） and the yield strength of the samples aged at four consecutive temperatures （i.e. natural aging＋190℃＋150℃＋100℃） can be increased approximately to 660 and 610 MPa, respectively. It is also found that precipitation of T1 phase occurs during multiple aging process of the alloy and the higher amounts of enthalpies shown in DSC charts are linked to higher volume fraction of this precipitate. Furthermore, TEM observations reveal that T1 phase has plate shape morphology and its crystal structure is in the form of hcp with lattice parameters of a=0.467 nm and c=0.878 nm.
基金supported by the National Natural Science Foundation of China(No.11475086)
文摘Sr0.6 Ba0.4 Nb2 O6 micro-rods are prepared by the molten-salt method with K2 SO4,KCl-K2 SO4,and KCl as fluxes.It reveals that the Sr0.6 Ba0.4 Nb2 O6 synthesized with KCl as a flux exhibits a single phase with tetragonal tungsten bronze structure.The measurement of X-ray diffraction indicates that the Sr0.6 Ba0.4 Nb2 O6 micro-rods synthesized at 1 300℃are anisotropic.The morphology of the powers is examined by transmission electron microscope.It reveals that the length-diameter ratio of Sr0.6 Ba0.4 Nb2 O6 micro-rods increases with increasing annealing temperature from 900℃to 1 300℃.At 1 300℃,the rod possesses a large length-diameter ratio of 8∶1.Moreover,the analysis of the piezoelectric properties of single micro-rods using apiezo-response force microscope indicates that the domains of the material are arranged along its radial direction.
基金Project(2004053304) supported by the PhD Program Foundation of Education Ministry of China
文摘The recrystallization behavior of 98.5% cold rolled high purity aluminum foils annealed at 300 ℃ was investigated,and the evolution of the microstructures was followed by electron back scattered diffraction(EBSD).The results show that the recrystallization process of the high purity aluminum foils at 300 ℃ is a mixture of discontinuous-and continuous-recrystallization.The orientations of the recrystallization nuclei include not only the cube orientation,but also other orientations such as some near deformation texture components which are the results of strong recovery process.However,such continuously recrystallized grains are usually associated with relatively high free energy,so they would be consumed by the discontinuously-recrystallized grains(cube-oriented grains)in subsequent annealing.On the other hand,the pattern quality index of recrystallized grains shows dependence on the crystal orientation which might introduce some errors into evaluating volume fraction of recrystallization by integrating pattern quality index of EBSD.
文摘It is well known that the lattice waves in alloy can be looked upon as the superposition of a series of plane waves with different wave vectors. Because of these plane wave′s diffraction action for X photon, there are two satellites (sidebands) around X ray main diffraction peak. With the wavelength and asymmetric factor α y of rectangle wave of the distribution of concentration introduced, the amplitude of modulation wave appearing along some crysallographic direction can be expressed clearly in the form of a sum of several diffraction wave vectors in the reciprocal space, and the diffracted intensity can be obtained. The X ray diffraction angle of sidebands strongly depends on the distribution of the wavelength. Fig.1b gives the simulated X ray diffraction profiles. It shows that when we fix the average modulated wavelength and change the distribution of wavelength, the angle difference between the satellite and main diffraction peak varies correspondingly. The simulated diffraction profiles are in good agreement with experimental results [1] (Fig.1a). The more diffuse the distribution of wavelength is, the nearer the sidebands are to main peak, and vice versa. In addition, the intensity and position of satellite are obviously restricted by the asymmetric factor of wave shape. Any lattice wave propagating in crystal can be resolved along coordinate axes. On the basis of the principle of superposition, all compositions of the lattice wave have diffraction profiles of themselves. Add two diffraction patterns perpendicular to each other on the reciprocal plane which is normal to the projected direction, we get the simulated TEM diffraction pattern of spinodal decomposition. Fig.2a is the TEM pattern by Kubo H [2] , Fig.2b and 2c are the simulated TEM patterns by Kubo H [2] and Khachaturyan A G [3] respectively. Our simulated TEM pattern (Fig.2d) is in good agreement with Fig.2a.
