Using hydrous aluminum chloride (AlCl3·6H2O) and silicon ethoxide (Si (OC2H5)4) as raw materials, a kind of nano-sized mullite powder was synthesized with the sol-gel process at the medium calcination tempe...Using hydrous aluminum chloride (AlCl3·6H2O) and silicon ethoxide (Si (OC2H5)4) as raw materials, a kind of nano-sized mullite powder was synthesized with the sol-gel process at the medium calcination temperature. The microstructures of the alumina-silica binary aerogel and calcined nano-sized materials were investigated by means of thermogravimetry-differential thermal analysis (TG-DTA), scanning electron microscopy (SEM) and X-ray diffractometer (XRD). The results show that the mullitization of Al2O3-SiO2 in gel starts from about 1 000℃ and its formation ofmullite takes place in the range of 1 100℃-1 250 ℃. The size of the nano-sized mullite powder calcined at 1 250 ℃ is measured to be about 30 nm.展开更多
Monophasic mullite (3Al2O3?2SiO2) samples doped with 0.002 M, 0.02 M, 0.1 M, 0.15 M and 0.2 M of cobalt were prepared by a sol-gel process. Prepared gels were then dried, grinded, pressed into pellets and sintered ...Monophasic mullite (3Al2O3?2SiO2) samples doped with 0.002 M, 0.02 M, 0.1 M, 0.15 M and 0.2 M of cobalt were prepared by a sol-gel process. Prepared gels were then dried, grinded, pressed into pellets and sintered at 1 000 °C and 1 300 °C for 4 h. Phase formation and densification behavior has been investigated as a function of the cobalt content and sintering temperature. Mullite densification behavior was analyzed .The density of the sintered ceramics was measured using Archimedes method. CoO and Co related compounds were detected by the analysis for G3, G4 and G5 doping levels. The mullite X-ray diffraction suggests predominant incorporation of Co in the glassy phase, whose quantity increased with the doping level.展开更多
Nanoscale mullite powder were synthesized via Sol-gel-SCFD and middle temperature treatment by using AIP( aluminum-isopropoxde) and TEOS ( tetraethyl orthosili-cate) as starting materials. Both of the binary aerogel o...Nanoscale mullite powder were synthesized via Sol-gel-SCFD and middle temperature treatment by using AIP( aluminum-isopropoxde) and TEOS ( tetraethyl orthosili-cate) as starting materials. Both of the binary aerogel of alumina-silica and calcined nanoscale materials were investigated by using TG-DSC ( thermogravimetry-differentialscanning calorimeter) , TEM( transmission electron microscope) , XRD(X-Ray diffractometer ) and specific surfacearea and porosimetry. TG-DSC indicated the removal of most of the volatiles, i.e. 15.98% up to about 700℃ ,and in the DSC curve , existence of two exothermic peak atabout 445℃ and 1015℃ may be due to the crystallizationof Si-O-Al-O in diphasic gels and mullitization and a small endothermic peak at about 805℃ indicated the decomposition of structural water molecules . On the colligation of the results of TG-DSC, XRD and TEM, the beginning temperature of mullitization in Al2O3-SiO2 aerogel system can be confirmed at about 1015℃. XRD results also showed the formation of mullite at the range 1100-1200℃. TEM and surface area and porosimetry results showed that the nanosized mullite were calcinated at 1100and 1200℃ exhibited size 30 nm and 50 nm, specific surface area 138.91 m2/g and 95.81 m2/g.展开更多
Al12Si3.75Ge0.25O26 ceramic powder was prepared by sol-gel method using Al(NO3)3,Si(OC2H5)4 and Cl3GeCH2-CH2COOH as precursors.The structural formation of Al12Si3.75Ge0.25O26 ceramic powder was analyzed by XRD.Aft...Al12Si3.75Ge0.25O26 ceramic powder was prepared by sol-gel method using Al(NO3)3,Si(OC2H5)4 and Cl3GeCH2-CH2COOH as precursors.The structural formation of Al12Si3.75Ge0.25O26 ceramic powder was analyzed by XRD.After reduction by flowing H2/Ar mixture gas,strong room temperature photoluminescence (PL) can be observed at 565 nm,613 nm,682 nm,731 nm and 777 nm,respectively.The PL intensity scarcely depends on the reduction temperature and duration,while the sample reduced at 500 ℃ for A^3 hours has the highest PL intensity.Before and after reduction at 500 ℃,the volume of unit cell of mullite solid solution decreases to 0.4699 3.Based on the analysis of XPS and Raman spectra,it can be approved that the PL phenomenon at room temperature is caused by the embedded Ge nanoparticles with the average size of about 1.95 nm.展开更多
Boehmite sol is synthesized via sol-gel process using Al 2(SO 4) 3·18H 2O and (CH 2) 6N 4 as starting materials, then adding silica sol into boehmite sol to prepare mullite precursor gels. XRD studies are ...Boehmite sol is synthesized via sol-gel process using Al 2(SO 4) 3·18H 2O and (CH 2) 6N 4 as starting materials, then adding silica sol into boehmite sol to prepare mullite precursor gels. XRD studies are performed to characterize the gels. It is found that the gel can be transformed into mullite when calcined at 1100℃ and completed at 1300℃. Corundum-mullite firebricks with different additions of the mullite precursor gel are made by mixing, semi-dry pressing and then sintering at 1520℃. Apparent porosity, bulk density, flexural strength and thermal shock resistance are measured. Results show that the mullite gel can improve densification and strength of corundum-mullite firebricks, especially enhance the thermal shock resistance. SEM micrographs show that the gel added can be formed into needlelike and elongated mullite in the matrix, whose micromorphology can enhance the strength and thermal shock resistance of the samples.展开更多
Highly crystallized mullite has been achieved at temperatures of 1100℃and 1400℃by sol-gel technique in presence of titanium and strontium ions of different concentrations:G_(0)=0 M,G_(1)=0.002 M,G_(2)=0.01 M,G_(3)=0...Highly crystallized mullite has been achieved at temperatures of 1100℃and 1400℃by sol-gel technique in presence of titanium and strontium ions of different concentrations:G_(0)=0 M,G_(1)=0.002 M,G_(2)=0.01 M,G_(3)=0.02 M,G_(4)=0.1 M,G_(5)=0.2 M and G6=0.5 M.X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FTIR),field emission scanning electron microscopy(FESEM),LCR meter characterized the samples.Mullite formation was found to depend on the concentration of the ions.The dielectric properties(dielectric constant,loss tangent and AC conductivity)of the composites have been measured,and their variation with increasing frequency and concentration of the doped metals was investigated.All the experiments were performed at room temperature.The composites showed maximum dielectric constants of 24.42 and 37.6 at 1400℃of 0.01 M concentration for titanium and strontium ions at 2 MHz,respectively.Due to the perfect nature of the doped mullite,it can be used for the fabrication of high charge storing capacitors and also as ceramic capacitors in the pico range.展开更多
The corrosion behavior of environmental barrier coatings(EBCs)directly affects the service life and stability of ceramic matrix composite(CMC)structural parts in the aero-engines.The silicon carbide(SiC)whisker toughe...The corrosion behavior of environmental barrier coatings(EBCs)directly affects the service life and stability of ceramic matrix composite(CMC)structural parts in the aero-engines.The silicon carbide(SiC)whisker toughening phase and c-AlPO_(4) bonding phase are firstly used to improve the service life of novel tri-layer Yb_(2)Si_(2)O_(7)/mullite/SiC EBCs in the burner rig test.The formation of penetrating cracks in Yb_(2)Si_(2)O_(7)/mullite/SiC coating caused the failure of coating at 1673 K.The SiC whiskers in mullite middle coating significantly inhibited the formation of penetrating cracks in Yb_(2)Si_(2)O_(7)/mullite/SiC coating,and efficiently prevented the oxidation of carbon fiber reinforced silicon carbide(C_(f)/SiC)samples for 360-min thermal cycles(24 times)with a weight loss of 6.19×10^(−3) g·cm^(−2).Although c-AlPO_(4) particles further improved the service life of SiC_(w)-mullite(SM)coating,the overflow of PO_(x) gas aggravated the formation and expansion of cracks in the Yb_(2)Si_(2)O_(7) outer coating,and caused the service life of overall Yb_(2)Si_(2)O_(7)/c-AlPO_(4)-SiC_(w)-mullite(ASM)/SiC coating to be slightly lower than that of Yb_(2)Si_(2)O_(7)/SM/SiC coating.This study guides the design of modified tri-layer EBCs with long service life in high-temperature and high-speed gas environment.展开更多
Sodium potassium niobate (KNN) (K0.5Na0.5NbO3) nanopowder with a mean particle size of about 20 - 30 nm was synthesized by wet chemical route using Nb2O5 as Nb source. A solution of K, Na and Nb cations was prepared, ...Sodium potassium niobate (KNN) (K0.5Na0.5NbO3) nanopowder with a mean particle size of about 20 - 30 nm was synthesized by wet chemical route using Nb2O5 as Nb source. A solution of K, Na and Nb cations was prepared, which resulted in a clear gel after the thermal treatment. Phase analysis, microstructure and morphology of the powder were determined by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Field Emission Scanning Electron Microscopy (FESEM). The obtained gel was first analyzed by Thermo Gravimetric Analyzer (TGA) and Differential Scanning Calorimetry (DSC), and then calcined at different temperatures of 400℃, 500℃, 600℃ and 700℃. The X-Ray Diffraction (XRD) patterns of the synthesized samples confirmed the formation of the orthorhombic crystal phase of K0.5Na0.5NbO3 at 500?C, a temperature significantly lower than that typically used in the conventional mixed oxide route. The process developed in this work is convenient to realize the mass production of KNN nanopowders at low cost and suitable for various industrial applications.展开更多
Nd/Yb-co-doped YAG transparent ceramic nano-powder was prepared by a sol-gel combustion method.The structure,morphology and properties were characterized by thermogravimetric-differential thermal analysis,X-ray diffra...Nd/Yb-co-doped YAG transparent ceramic nano-powder was prepared by a sol-gel combustion method.The structure,morphology and properties were characterized by thermogravimetric-differential thermal analysis,X-ray diffraction,transmission electron microscopy,infrared spectroscopy,absorption analysis and fluorescence spectroscopy,respectively.The results show that the mass loss of the powder calcinated at 900 ℃ for 3 h is 49.56%.A well-crystallized Nd/Yb:YAG nano-powder with the superior sintering performance and high purity is obtained,and the morphology of the particles with the average diameter in the range of 60-100 runs appears regular.The nano-powder exhibits an intense absorption at 808 nm,corresponding to the 4I/9/2-4F7/2 transition of Nd^(^(3+) ions,which is suitable to absorb the wavelength of 808 nm from a laser diode source.The emission peak at 1046 nm of the Nd/Yb:YAG powder is more intense than that of Nd^(^(3+):YAG powder.It is indicated that the energy absorbed by Yb^(^(3+) ions from the laser diode source can be transmitted to Nd^(^(3+) ions based on the cross relaxation process of[(4F3/2)Nd,(2F7/2)Yb]-[(479/2)Nd,(2F5/2)Yb].展开更多
基金National High Technology Research and Development Program of China (2004AA332060)
文摘Using hydrous aluminum chloride (AlCl3·6H2O) and silicon ethoxide (Si (OC2H5)4) as raw materials, a kind of nano-sized mullite powder was synthesized with the sol-gel process at the medium calcination temperature. The microstructures of the alumina-silica binary aerogel and calcined nano-sized materials were investigated by means of thermogravimetry-differential thermal analysis (TG-DTA), scanning electron microscopy (SEM) and X-ray diffractometer (XRD). The results show that the mullitization of Al2O3-SiO2 in gel starts from about 1 000℃ and its formation ofmullite takes place in the range of 1 100℃-1 250 ℃. The size of the nano-sized mullite powder calcined at 1 250 ℃ is measured to be about 30 nm.
文摘Monophasic mullite (3Al2O3?2SiO2) samples doped with 0.002 M, 0.02 M, 0.1 M, 0.15 M and 0.2 M of cobalt were prepared by a sol-gel process. Prepared gels were then dried, grinded, pressed into pellets and sintered at 1 000 °C and 1 300 °C for 4 h. Phase formation and densification behavior has been investigated as a function of the cobalt content and sintering temperature. Mullite densification behavior was analyzed .The density of the sintered ceramics was measured using Archimedes method. CoO and Co related compounds were detected by the analysis for G3, G4 and G5 doping levels. The mullite X-ray diffraction suggests predominant incorporation of Co in the glassy phase, whose quantity increased with the doping level.
基金This work was supported by the project of Wuhan Science & Technology(20011007088)and Hubei province project of key problem tackling(2001AA101B07)
文摘Nanoscale mullite powder were synthesized via Sol-gel-SCFD and middle temperature treatment by using AIP( aluminum-isopropoxde) and TEOS ( tetraethyl orthosili-cate) as starting materials. Both of the binary aerogel of alumina-silica and calcined nanoscale materials were investigated by using TG-DSC ( thermogravimetry-differentialscanning calorimeter) , TEM( transmission electron microscope) , XRD(X-Ray diffractometer ) and specific surfacearea and porosimetry. TG-DSC indicated the removal of most of the volatiles, i.e. 15.98% up to about 700℃ ,and in the DSC curve , existence of two exothermic peak atabout 445℃ and 1015℃ may be due to the crystallizationof Si-O-Al-O in diphasic gels and mullitization and a small endothermic peak at about 805℃ indicated the decomposition of structural water molecules . On the colligation of the results of TG-DSC, XRD and TEM, the beginning temperature of mullitization in Al2O3-SiO2 aerogel system can be confirmed at about 1015℃. XRD results also showed the formation of mullite at the range 1100-1200℃. TEM and surface area and porosimetry results showed that the nanosized mullite were calcinated at 1100and 1200℃ exhibited size 30 nm and 50 nm, specific surface area 138.91 m2/g and 95.81 m2/g.
基金Funded by the Program for New Century Excellent Talents in Univer-sity (NCET-05-0658)SRF for ROCS, SEM
文摘Al12Si3.75Ge0.25O26 ceramic powder was prepared by sol-gel method using Al(NO3)3,Si(OC2H5)4 and Cl3GeCH2-CH2COOH as precursors.The structural formation of Al12Si3.75Ge0.25O26 ceramic powder was analyzed by XRD.After reduction by flowing H2/Ar mixture gas,strong room temperature photoluminescence (PL) can be observed at 565 nm,613 nm,682 nm,731 nm and 777 nm,respectively.The PL intensity scarcely depends on the reduction temperature and duration,while the sample reduced at 500 ℃ for A^3 hours has the highest PL intensity.Before and after reduction at 500 ℃,the volume of unit cell of mullite solid solution decreases to 0.4699 3.Based on the analysis of XPS and Raman spectra,it can be approved that the PL phenomenon at room temperature is caused by the embedded Ge nanoparticles with the average size of about 1.95 nm.
文摘Boehmite sol is synthesized via sol-gel process using Al 2(SO 4) 3·18H 2O and (CH 2) 6N 4 as starting materials, then adding silica sol into boehmite sol to prepare mullite precursor gels. XRD studies are performed to characterize the gels. It is found that the gel can be transformed into mullite when calcined at 1100℃ and completed at 1300℃. Corundum-mullite firebricks with different additions of the mullite precursor gel are made by mixing, semi-dry pressing and then sintering at 1520℃. Apparent porosity, bulk density, flexural strength and thermal shock resistance are measured. Results show that the mullite gel can improve densification and strength of corundum-mullite firebricks, especially enhance the thermal shock resistance. SEM micrographs show that the gel added can be formed into needlelike and elongated mullite in the matrix, whose micromorphology can enhance the strength and thermal shock resistance of the samples.
基金We are grateful to DST and UGC(PURSE program),Government of India,for the financial assistance.
文摘Highly crystallized mullite has been achieved at temperatures of 1100℃and 1400℃by sol-gel technique in presence of titanium and strontium ions of different concentrations:G_(0)=0 M,G_(1)=0.002 M,G_(2)=0.01 M,G_(3)=0.02 M,G_(4)=0.1 M,G_(5)=0.2 M and G6=0.5 M.X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FTIR),field emission scanning electron microscopy(FESEM),LCR meter characterized the samples.Mullite formation was found to depend on the concentration of the ions.The dielectric properties(dielectric constant,loss tangent and AC conductivity)of the composites have been measured,and their variation with increasing frequency and concentration of the doped metals was investigated.All the experiments were performed at room temperature.The composites showed maximum dielectric constants of 24.42 and 37.6 at 1400℃of 0.01 M concentration for titanium and strontium ions at 2 MHz,respectively.Due to the perfect nature of the doped mullite,it can be used for the fabrication of high charge storing capacitors and also as ceramic capacitors in the pico range.
基金funded by the National Key R&D Program of China(Grant Nos.2021YFB3703800 and 2021YFB3703802)National Natural Science Foundation of China(Grant No.52102122)+1 种基金National Key Laboratory of Science and Technology on High-strength Structural Materials,Central South University(Grant No.SYSJJ2021LWS01)China Postdoctoral Science Foundation(Grant No.2022M711540).
文摘The corrosion behavior of environmental barrier coatings(EBCs)directly affects the service life and stability of ceramic matrix composite(CMC)structural parts in the aero-engines.The silicon carbide(SiC)whisker toughening phase and c-AlPO_(4) bonding phase are firstly used to improve the service life of novel tri-layer Yb_(2)Si_(2)O_(7)/mullite/SiC EBCs in the burner rig test.The formation of penetrating cracks in Yb_(2)Si_(2)O_(7)/mullite/SiC coating caused the failure of coating at 1673 K.The SiC whiskers in mullite middle coating significantly inhibited the formation of penetrating cracks in Yb_(2)Si_(2)O_(7)/mullite/SiC coating,and efficiently prevented the oxidation of carbon fiber reinforced silicon carbide(C_(f)/SiC)samples for 360-min thermal cycles(24 times)with a weight loss of 6.19×10^(−3) g·cm^(−2).Although c-AlPO_(4) particles further improved the service life of SiC_(w)-mullite(SM)coating,the overflow of PO_(x) gas aggravated the formation and expansion of cracks in the Yb_(2)Si_(2)O_(7) outer coating,and caused the service life of overall Yb_(2)Si_(2)O_(7)/c-AlPO_(4)-SiC_(w)-mullite(ASM)/SiC coating to be slightly lower than that of Yb_(2)Si_(2)O_(7)/SM/SiC coating.This study guides the design of modified tri-layer EBCs with long service life in high-temperature and high-speed gas environment.
文摘Sodium potassium niobate (KNN) (K0.5Na0.5NbO3) nanopowder with a mean particle size of about 20 - 30 nm was synthesized by wet chemical route using Nb2O5 as Nb source. A solution of K, Na and Nb cations was prepared, which resulted in a clear gel after the thermal treatment. Phase analysis, microstructure and morphology of the powder were determined by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Field Emission Scanning Electron Microscopy (FESEM). The obtained gel was first analyzed by Thermo Gravimetric Analyzer (TGA) and Differential Scanning Calorimetry (DSC), and then calcined at different temperatures of 400℃, 500℃, 600℃ and 700℃. The X-Ray Diffraction (XRD) patterns of the synthesized samples confirmed the formation of the orthorhombic crystal phase of K0.5Na0.5NbO3 at 500?C, a temperature significantly lower than that typically used in the conventional mixed oxide route. The process developed in this work is convenient to realize the mass production of KNN nanopowders at low cost and suitable for various industrial applications.
基金supported by special project of Changchun Science & Technology Office(2014228)the Development and Reform Commission of Jilin Province(2015Y69)
文摘Nd/Yb-co-doped YAG transparent ceramic nano-powder was prepared by a sol-gel combustion method.The structure,morphology and properties were characterized by thermogravimetric-differential thermal analysis,X-ray diffraction,transmission electron microscopy,infrared spectroscopy,absorption analysis and fluorescence spectroscopy,respectively.The results show that the mass loss of the powder calcinated at 900 ℃ for 3 h is 49.56%.A well-crystallized Nd/Yb:YAG nano-powder with the superior sintering performance and high purity is obtained,and the morphology of the particles with the average diameter in the range of 60-100 runs appears regular.The nano-powder exhibits an intense absorption at 808 nm,corresponding to the 4I/9/2-4F7/2 transition of Nd^(^(3+) ions,which is suitable to absorb the wavelength of 808 nm from a laser diode source.The emission peak at 1046 nm of the Nd/Yb:YAG powder is more intense than that of Nd^(^(3+):YAG powder.It is indicated that the energy absorbed by Yb^(^(3+) ions from the laser diode source can be transmitted to Nd^(^(3+) ions based on the cross relaxation process of[(4F3/2)Nd,(2F7/2)Yb]-[(479/2)Nd,(2F5/2)Yb].