Silicon nitride （Si3N4） powders were prepared by the direct nitridation of silicon powders diluted with a- Si3N4 at normal pressure. Silicon powders of 2.2 μm in average diameter were used as the raw materials. The...Silicon nitride （Si3N4） powders were prepared by the direct nitridation of silicon powders diluted with a- Si3N4 at normal pressure. Silicon powders of 2.2 μm in average diameter were used as the raw materials. The nitriding temperature was from 1623 to 1823 K, and the reaction time ranged from 0 to 20 min. The phase compositions and morphologies of the products were analyzed by X-ray diffraction and scanning electron microscopy, respectively. The effects of nitriding temperature and reaction time on the conversion rate of silicon were determined. Based on the shrinking core model as well as the relationship between the conversion rate of silicon and the reaction time at different temperatures, a simple model was derived to describe the reaction between silicon and nitrogen. The model revealed an asymptotic exponential trend of the silicon conversion rate with time. Three kinetic parameters of silicon nitridation at atmospheric pressure were calculated, including the pre-exponential factor （2.27 cm.s^-1） in the Arrhenius equation, activation energy （114 kJ·mol^-1）, and effective diffusion coefficient （6.2×10-s cm2.s^-1）. A formula was also derived to calculate the reaction rate constant.展开更多
This paper reviewed the effect of powder characteristics and additives including metals,rare earth oxides,and ZrO2 on nitridation of Si powder.The decrease of particle size of Si powder increased nitridation.Most of m...This paper reviewed the effect of powder characteristics and additives including metals,rare earth oxides,and ZrO2 on nitridation of Si powder.The decrease of particle size of Si powder increased nitridation.Most of metal additives inhibited nitridation,while some metal additives such as Fe,Cu,Cr,and Ca increased nitrida—tion.Otherwise,the addition of metals might lead to the degradation of physical and mechanical properties of Si3N4.All the rare earth oxides,especially CeO2 and Eu2O3,showed nitridation enhancing effect.In addition,ZrO2 with small particle size showed a stronger enhancing effect.展开更多
Effects of particle size （A：d50 = 336. 9 μm, B：d50 =123.5μm, C： d50=19.5 μm, D： dso=2.21μm） and content （1 wt% , 3 wt% , 5 wt% , 7 wt% ） of silicon powder on cold crushing strength （CCS） , pore size dis...Effects of particle size （A：d50 = 336. 9 μm, B：d50 =123.5μm, C： d50=19.5 μm, D： dso=2.21μm） and content （1 wt% , 3 wt% , 5 wt% , 7 wt% ） of silicon powder on cold crushing strength （CCS） , pore size distribution and microstructure of Al2O3 - ZrO2 - C refractories coked at high temperature had been investigated by means of mercury porosimeter, SEM, EDS, tic. The results indicated that particle size and content of silicon powder affected the cold crushing strength of coked specimens. It increased with the addition of silicon powder and its finer particle size. However, it decreased greatly when using too fine silicon powder. The particle size and content of silicon powder also impacted the phase evolution and microstructure of coked specimens, much more β-SiC whiskers constituted network structure and well distributed in specimens with reduction of their slenderness ratios when finer silicon powder was added, corresponding to that, the specimens＇ pore size distribution range became narrower with smaller pore diameter, but β-SiC whiskers were distributed sparsely and the specific pore volume of small pores increased when much finer powder was added. It was worthly mentioned that some nitride could form in specimens with addition of appropriate particle size and content of silicon powder.展开更多
In order to reduce the hydrolysis rate of Si powder and inhibit the swelling and cracking of cast samples,Si powder was treated at different temperatures for 5 h,and then slurries and SiC-Si3N4 materials were prepared...In order to reduce the hydrolysis rate of Si powder and inhibit the swelling and cracking of cast samples,Si powder was treated at different temperatures for 5 h,and then slurries and SiC-Si3N4 materials were prepared.The effect of the preheating temperature on the composition of the Si powder,the hydrolysis rate as well as the nitridation of the SiC-Si3N4 materials was studied.The results show that with the increase of the pretreatment temperature of Si powder,the oxidation degree of Si powders increases,the viscosity of the slurry with PAAS dispersant decreases gradually,and the hydrolysis reaction of Si powder decreases gradually;the Si powder pretreated at 700℃ or lower has little effect on the nitriding process,while the Si powder pretreated at 800 t has a great effect on the nitriding process,which is not conducive to the nitriding sintering of the samples.Therefore,the Si powder pretreated at 700 t for 5 h has the best properties,which not only has lower hydrolysis rate and good slurry fluidity,but also has mild effect on the nitriding reaction.展开更多
The nanocomposite of MoSi2-SiaN4 （molybdenum disilicide-silicon nitride） was synthesized by reaction milling of the Mo and Si powder mixture. Changing the processing parameters led to the formation of different prod...The nanocomposite of MoSi2-SiaN4 （molybdenum disilicide-silicon nitride） was synthesized by reaction milling of the Mo and Si powder mixture. Changing the processing parameters led to the formation of different products such as a- and B-MoSi2, SiaN4, Mo2N, and M05Si3 at various milling times. A thermodynamic appraisal showed that the milling of Moa2Siss powder mixture was associated with highly exothermic mechanically induced self-sustaining reaction （MSR） between Mo and Si. The MSR took place around 5 h of milling led to the formation of a-MoSi2 and the reaction between Si and N2 to produce Si3N4 under a nitrogen pressure of 1 MPa. By increasing the nitrogen pressure to 5 MPa, more heat is released, resulting in the dissociation of Si3N4 and the transformation of a-MoSi2 to β-MoSi2. Heat treatment was also performed on the milled samples and led to the formation of Mo2N and the transformation of a-MoSi2 to β-MoSi2 at the milling times of 10 and 40 h, respectively.展开更多
Si3N4 powders were synthesized by a carbothermal reduction method using a SiO2 ＋ C combustion synthesis precur- sor derived from a mixed solution consisting of silicic acid （Si source）, polyacrylamide （additive）,...Si3N4 powders were synthesized by a carbothermal reduction method using a SiO2 ＋ C combustion synthesis precur- sor derived from a mixed solution consisting of silicic acid （Si source）, polyacrylamide （additive）, nitric acid （oxidizer）, urea （fuel）, and glucose （C source）. Scanning electron microscopy （SEM） micrographs showed that the obtained precursor exhibited a uniform mixture of SiO2 ＋ C composed of porous blocky particles up to -20 μm. The precursor was subsequently calcined under nitrogen at 1200-1550℃ for 2 h. X-ray diffraction （XRD） analysis revealed that the initial reduction reaction started at about 1300℃, and the complete transition of SiQ into Si3N4 was found at 1550℃. The Si3N4 powders, synthesized at 1550℃, exhibit a mixture phase of α- and -Si3N4 and consist of mainly agglomerates of fine particles of 100-300 nm, needle-like crystals and whiskers with a diameter of about 100 nm and a length up to several micrometers, and a minor amount of irregular-shaped growths.展开更多
Si3N4 powder was synthesized by carbothermal re- duction nitridation reaction using sawdust as carbon source and introducing SiO2 by silica sol immersion. Effects of SiO2 content of silica sol, molding pressure, react...Si3N4 powder was synthesized by carbothermal re- duction nitridation reaction using sawdust as carbon source and introducing SiO2 by silica sol immersion. Effects of SiO2 content of silica sol, molding pressure, reaction temperature, reaction duration, and N2 flow rate on phase compositions and microstructure of result- ants were studied. The results show that using 7. 5 mass% SiO2 containing silica sol immersed sawdust as raw materials, the prepared Si3N4 powder is featured with high α-Si3N4 content, few impurities, etc. in the conditions of 1 450 ℃ of reaction temperature, 9 h of reaction duration, 400 mL ·min- 1 of N2 flow rate and 10 MPa of molding pressure.展开更多
本文研究了用激光气相法制备的超微 Si 粉在高纯 N_2下的高温氮化过程,并将含游离 Si 较多的超微 Si_3N_4粉进行了相似的处理.实验表明,在常压气氛下,超微 Si 粉在1300℃的高温下能全部氮化生成 Si_3N_4,其颗粒大小及形状基本仍具有激...本文研究了用激光气相法制备的超微 Si 粉在高纯 N_2下的高温氮化过程,并将含游离 Si 较多的超微 Si_3N_4粉进行了相似的处理.实验表明,在常压气氛下,超微 Si 粉在1300℃的高温下能全部氮化生成 Si_3N_4,其颗粒大小及形状基本仍具有激光法的一些优点,含氮量达到39.5%.展开更多
基金supported by the Natural Science Foundation of China(No.51106008)the Major State Basic Research and Development Program of China(No.2012CB720406)
文摘Silicon nitride （Si3N4） powders were prepared by the direct nitridation of silicon powders diluted with a- Si3N4 at normal pressure. Silicon powders of 2.2 μm in average diameter were used as the raw materials. The nitriding temperature was from 1623 to 1823 K, and the reaction time ranged from 0 to 20 min. The phase compositions and morphologies of the products were analyzed by X-ray diffraction and scanning electron microscopy, respectively. The effects of nitriding temperature and reaction time on the conversion rate of silicon were determined. Based on the shrinking core model as well as the relationship between the conversion rate of silicon and the reaction time at different temperatures, a simple model was derived to describe the reaction between silicon and nitrogen. The model revealed an asymptotic exponential trend of the silicon conversion rate with time. Three kinetic parameters of silicon nitridation at atmospheric pressure were calculated, including the pre-exponential factor （2.27 cm.s^-1） in the Arrhenius equation, activation energy （114 kJ·mol^-1）, and effective diffusion coefficient （6.2×10-s cm2.s^-1）. A formula was also derived to calculate the reaction rate constant.
基金financially supported by Guangdong Innovative and Entrepreneurial Research Team Program ( No. 2013G061)the National Natural Science Foundation of China ( No. 51402055)
文摘This paper reviewed the effect of powder characteristics and additives including metals,rare earth oxides,and ZrO2 on nitridation of Si powder.The decrease of particle size of Si powder increased nitridation.Most of metal additives inhibited nitridation,while some metal additives such as Fe,Cu,Cr,and Ca increased nitrida—tion.Otherwise,the addition of metals might lead to the degradation of physical and mechanical properties of Si3N4.All the rare earth oxides,especially CeO2 and Eu2O3,showed nitridation enhancing effect.In addition,ZrO2 with small particle size showed a stronger enhancing effect.
文摘Effects of particle size （A：d50 = 336. 9 μm, B：d50 =123.5μm, C： d50=19.5 μm, D： dso=2.21μm） and content （1 wt% , 3 wt% , 5 wt% , 7 wt% ） of silicon powder on cold crushing strength （CCS） , pore size distribution and microstructure of Al2O3 - ZrO2 - C refractories coked at high temperature had been investigated by means of mercury porosimeter, SEM, EDS, tic. The results indicated that particle size and content of silicon powder affected the cold crushing strength of coked specimens. It increased with the addition of silicon powder and its finer particle size. However, it decreased greatly when using too fine silicon powder. The particle size and content of silicon powder also impacted the phase evolution and microstructure of coked specimens, much more β-SiC whiskers constituted network structure and well distributed in specimens with reduction of their slenderness ratios when finer silicon powder was added, corresponding to that, the specimens＇ pore size distribution range became narrower with smaller pore diameter, but β-SiC whiskers were distributed sparsely and the specific pore volume of small pores increased when much finer powder was added. It was worthly mentioned that some nitride could form in specimens with addition of appropriate particle size and content of silicon powder.
文摘In order to reduce the hydrolysis rate of Si powder and inhibit the swelling and cracking of cast samples,Si powder was treated at different temperatures for 5 h,and then slurries and SiC-Si3N4 materials were prepared.The effect of the preheating temperature on the composition of the Si powder,the hydrolysis rate as well as the nitridation of the SiC-Si3N4 materials was studied.The results show that with the increase of the pretreatment temperature of Si powder,the oxidation degree of Si powders increases,the viscosity of the slurry with PAAS dispersant decreases gradually,and the hydrolysis reaction of Si powder decreases gradually;the Si powder pretreated at 700℃ or lower has little effect on the nitriding process,while the Si powder pretreated at 800 t has a great effect on the nitriding process,which is not conducive to the nitriding sintering of the samples.Therefore,the Si powder pretreated at 700 t for 5 h has the best properties,which not only has lower hydrolysis rate and good slurry fluidity,but also has mild effect on the nitriding reaction.
文摘The nanocomposite of MoSi2-SiaN4 （molybdenum disilicide-silicon nitride） was synthesized by reaction milling of the Mo and Si powder mixture. Changing the processing parameters led to the formation of different products such as a- and B-MoSi2, SiaN4, Mo2N, and M05Si3 at various milling times. A thermodynamic appraisal showed that the milling of Moa2Siss powder mixture was associated with highly exothermic mechanically induced self-sustaining reaction （MSR） between Mo and Si. The MSR took place around 5 h of milling led to the formation of a-MoSi2 and the reaction between Si and N2 to produce Si3N4 under a nitrogen pressure of 1 MPa. By increasing the nitrogen pressure to 5 MPa, more heat is released, resulting in the dissociation of Si3N4 and the transformation of a-MoSi2 to β-MoSi2. Heat treatment was also performed on the milled samples and led to the formation of Mo2N and the transformation of a-MoSi2 to β-MoSi2 at the milling times of 10 and 40 h, respectively.
基金supported by the National Natural Science Foundation of China (Nos. 50802006 and 51172017)the Natural Science Foundation of Beijing (No. 2102028)+2 种基金the Fundamental Research Funds for the Central Universities (No. FRF-TP-11-004A)the Fok Ying Tung Education Foundation Fund for Young College Teachers (No. 122016)the Public Foundation of Beijing Key Lab for Advanced Powder Metallurgy and Particulate Materials (USTB)
文摘Si3N4 powders were synthesized by a carbothermal reduction method using a SiO2 ＋ C combustion synthesis precur- sor derived from a mixed solution consisting of silicic acid （Si source）, polyacrylamide （additive）, nitric acid （oxidizer）, urea （fuel）, and glucose （C source）. Scanning electron microscopy （SEM） micrographs showed that the obtained precursor exhibited a uniform mixture of SiO2 ＋ C composed of porous blocky particles up to -20 μm. The precursor was subsequently calcined under nitrogen at 1200-1550℃ for 2 h. X-ray diffraction （XRD） analysis revealed that the initial reduction reaction started at about 1300℃, and the complete transition of SiQ into Si3N4 was found at 1550℃. The Si3N4 powders, synthesized at 1550℃, exhibit a mixture phase of α- and -Si3N4 and consist of mainly agglomerates of fine particles of 100-300 nm, needle-like crystals and whiskers with a diameter of about 100 nm and a length up to several micrometers, and a minor amount of irregular-shaped growths.
文摘Si3N4 powder was synthesized by carbothermal re- duction nitridation reaction using sawdust as carbon source and introducing SiO2 by silica sol immersion. Effects of SiO2 content of silica sol, molding pressure, reaction temperature, reaction duration, and N2 flow rate on phase compositions and microstructure of result- ants were studied. The results show that using 7. 5 mass% SiO2 containing silica sol immersed sawdust as raw materials, the prepared Si3N4 powder is featured with high α-Si3N4 content, few impurities, etc. in the conditions of 1 450 ℃ of reaction temperature, 9 h of reaction duration, 400 mL ·min- 1 of N2 flow rate and 10 MPa of molding pressure.
