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
The preparation of high-entropy(HE)ceramics with designed composition is essential for verifying the formability models and evaluating the properties of the ceramics.However,inevitable oxygen contamination in non-oxid...The preparation of high-entropy(HE)ceramics with designed composition is essential for verifying the formability models and evaluating the properties of the ceramics.However,inevitable oxygen contamination in non-oxide ceramics will result in the formation of metal oxide impurity phases remaining in the specimen or even escaping from the specimen during the sintering process,making the elemental compositions of the HE phase deviated from the designed ones.In this work,the preparation and thermodynamic analysis during the processing of equiatomic 9-cation HE carbide(HEC9)ceramics of the IVB,VB,and VIB groups were studied focusing on the removing of the inevitable oxygen impurity existed in the starting carbide powders and the oxygen contamination during the powder mixing processing.The results demonstrate that densification by spark plasma sintering(SPS)by directly using the mixed powders of the corresponding single-component carbides will inhibit the oxygen-removing carbothermal reduction reactions,and most of the oxide impurities will remain in the sample as(Zr,Hf)O_(2)phase.Pretreatment of the mixed powders at high temperatures in vacuum will remove most part of the oxygen impurity but result in a remarkable escape of gaseous Cr owing to the oxygen-removing reaction between Cr_(3)C_(2)and various oxide impurities.It is found that graphite addition enhances the oxygen-removing effect and simultaneously prevents the escape of gaseous Cr.On the other hand,although WC,VC,and Mo2C can also act as oxygen-removing agents,there is no metal-containing gaseous substance formation in the temperature range of this study.By using the heat-treated powders with added graphite,equiatomic HEC9 ceramics were successfully prepared by SPS.展开更多
Owing to its excellent high-temperature resistance and high conductivity,zirconium diboride(ZrB_(2)) has been applied as an infrared suppression coating.However,ZrB_(2)is susceptible to hydrolysis under high-moisture ...Owing to its excellent high-temperature resistance and high conductivity,zirconium diboride(ZrB_(2)) has been applied as an infrared suppression coating.However,ZrB_(2)is susceptible to hydrolysis under high-moisture conditions and even under mild working temperatures.The improvement in the hydrophobicity of the ZrB_(2)surface effectively reduces wetting by water and suppresses hydrolysis reaction,particularly under high-temperature and high-moisture conditions.Herein,we report a novel,easy,and highly reproducible method for producing a fully coated ZrB_(2)surface by developing a nanoscale hydrophobic layer of glassy LaF_(3)on the surface of ZrB_(2)powder particles in situ(i.e.,during the carbothermal synthesis of ZrB_(2)).Through the tests carried out at 200 ℃for 100-300 h in a hydrothermal reactor,the produced powders displayed remarkably high long-term hydrolysis resistance and pronounced chemical stability.Compared with treated ZrB_(2),ZrB_(2)@LaF_(3)remained lower infrared emissivity when continuously intensifying hydrolyzation process.The results suggest that a nanoscale surface modification strategy can be applied to stabilize the infrared emissivity of ZrB_(2)in a water-oxygen coupling environment.展开更多
In slag tapping furnaces, char particles undergo a series of complex structural evolution before and after being captured by the liquid slag layer. The evolution results affect the carbon conversion rate and are affec...In slag tapping furnaces, char particles undergo a series of complex structural evolution before and after being captured by the liquid slag layer. The evolution results affect the carbon conversion rate and are affected by temperature fluctuations, especially in the ash melting temperature zone. Experimental study on structure evolution of bituminous char prepared at around ash melting temperature was carried out on a fixed bed. The morphology, specific surface area and mineral chemical composition were measured at different temperatures. Experimental results show that the number density and the size of ash droplets exuded on the char surface increased significantly with the increasing temperature. The ash specific surface area from gasification was slightly greater than that from combustion. The residual content of chloride in the char become 1% and the contents of Fe, K, Mg and Na decrease significantly during the pyrolysis process across the ash melting temperature zone. The diffraction intensity of oldhamite increase which indicates the reaction of carbon substrate with minerals during the evolution;the diffraction intensity of quartz dramatically decreases for the reason of anorthite generation. The ignition and burnout temperatures of char were found to increase and the combustion stability decreased with the increasing pyrolysis temperature.展开更多
Biomass-derived N-doped carbon(BNC)is an important environmental material and widely used in the fields of water purification and soil remediation.However,the toxicant in the commonly used synthesis process of BNC mat...Biomass-derived N-doped carbon(BNC)is an important environmental material and widely used in the fields of water purification and soil remediation.However,the toxicant in the commonly used synthesis process of BNC materials have been largely ignored.Herein,we firstly report the presence of a highly toxic by-product(KCN)in the activation process of BNC materials consequential of the carbothermal reduction reaction.Because this carbothermal reduction reaction also regulates the N-doping and pore development of BNC materials,the KCN content directly relates with the properties of BNC material properties.Accordingly,a high KCN content(-611 mg)can occur in the production process of per g BNC material with high specific surface area(-3600 m^2/g).Because the application performance of BNC material is determined by the surface area and available N doping,therefore,production of a BNC material with high performance entails high risk.Undoubtedly,this study proves a completely new risk recognition on a familiar synthesis process of biomass-based material.And,strict protective device should be taken in fabrication process of biomass-derived carbon material.展开更多
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.
基金This work was financially supported by the National Natural Science Foundation of China(Nos.52032001 and 51872045).
文摘The preparation of high-entropy(HE)ceramics with designed composition is essential for verifying the formability models and evaluating the properties of the ceramics.However,inevitable oxygen contamination in non-oxide ceramics will result in the formation of metal oxide impurity phases remaining in the specimen or even escaping from the specimen during the sintering process,making the elemental compositions of the HE phase deviated from the designed ones.In this work,the preparation and thermodynamic analysis during the processing of equiatomic 9-cation HE carbide(HEC9)ceramics of the IVB,VB,and VIB groups were studied focusing on the removing of the inevitable oxygen impurity existed in the starting carbide powders and the oxygen contamination during the powder mixing processing.The results demonstrate that densification by spark plasma sintering(SPS)by directly using the mixed powders of the corresponding single-component carbides will inhibit the oxygen-removing carbothermal reduction reactions,and most of the oxide impurities will remain in the sample as(Zr,Hf)O_(2)phase.Pretreatment of the mixed powders at high temperatures in vacuum will remove most part of the oxygen impurity but result in a remarkable escape of gaseous Cr owing to the oxygen-removing reaction between Cr_(3)C_(2)and various oxide impurities.It is found that graphite addition enhances the oxygen-removing effect and simultaneously prevents the escape of gaseous Cr.On the other hand,although WC,VC,and Mo2C can also act as oxygen-removing agents,there is no metal-containing gaseous substance formation in the temperature range of this study.By using the heat-treated powders with added graphite,equiatomic HEC9 ceramics were successfully prepared by SPS.
基金financially supported by the National Natural Science Foundation of China(Nos.51802037 and 51972046)Sichuan Science and Technology Program(No.2020JDRC0045)
文摘Owing to its excellent high-temperature resistance and high conductivity,zirconium diboride(ZrB_(2)) has been applied as an infrared suppression coating.However,ZrB_(2)is susceptible to hydrolysis under high-moisture conditions and even under mild working temperatures.The improvement in the hydrophobicity of the ZrB_(2)surface effectively reduces wetting by water and suppresses hydrolysis reaction,particularly under high-temperature and high-moisture conditions.Herein,we report a novel,easy,and highly reproducible method for producing a fully coated ZrB_(2)surface by developing a nanoscale hydrophobic layer of glassy LaF_(3)on the surface of ZrB_(2)powder particles in situ(i.e.,during the carbothermal synthesis of ZrB_(2)).Through the tests carried out at 200 ℃for 100-300 h in a hydrothermal reactor,the produced powders displayed remarkably high long-term hydrolysis resistance and pronounced chemical stability.Compared with treated ZrB_(2),ZrB_(2)@LaF_(3)remained lower infrared emissivity when continuously intensifying hydrolyzation process.The results suggest that a nanoscale surface modification strategy can be applied to stabilize the infrared emissivity of ZrB_(2)in a water-oxygen coupling environment.
基金financial support from the Natural Science Fund of China(51576158)the support of the Instrument Analysis Center of Xi’an Jiaotong University。
文摘In slag tapping furnaces, char particles undergo a series of complex structural evolution before and after being captured by the liquid slag layer. The evolution results affect the carbon conversion rate and are affected by temperature fluctuations, especially in the ash melting temperature zone. Experimental study on structure evolution of bituminous char prepared at around ash melting temperature was carried out on a fixed bed. The morphology, specific surface area and mineral chemical composition were measured at different temperatures. Experimental results show that the number density and the size of ash droplets exuded on the char surface increased significantly with the increasing temperature. The ash specific surface area from gasification was slightly greater than that from combustion. The residual content of chloride in the char become 1% and the contents of Fe, K, Mg and Na decrease significantly during the pyrolysis process across the ash melting temperature zone. The diffraction intensity of oldhamite increase which indicates the reaction of carbon substrate with minerals during the evolution;the diffraction intensity of quartz dramatically decreases for the reason of anorthite generation. The ignition and burnout temperatures of char were found to increase and the combustion stability decreased with the increasing pyrolysis temperature.
基金the National Natural Science Foundation of China(No.21876030)。
文摘Biomass-derived N-doped carbon(BNC)is an important environmental material and widely used in the fields of water purification and soil remediation.However,the toxicant in the commonly used synthesis process of BNC materials have been largely ignored.Herein,we firstly report the presence of a highly toxic by-product(KCN)in the activation process of BNC materials consequential of the carbothermal reduction reaction.Because this carbothermal reduction reaction also regulates the N-doping and pore development of BNC materials,the KCN content directly relates with the properties of BNC material properties.Accordingly,a high KCN content(-611 mg)can occur in the production process of per g BNC material with high specific surface area(-3600 m^2/g).Because the application performance of BNC material is determined by the surface area and available N doping,therefore,production of a BNC material with high performance entails high risk.Undoubtedly,this study proves a completely new risk recognition on a familiar synthesis process of biomass-based material.And,strict protective device should be taken in fabrication process of biomass-derived carbon material.