CrN powder was synthesized by nitriding Cr metal in ammonia gas flow, and its chemical reaction mechanism and nitridation process were studied. Through thermodynamic calculations, the Cr-N-O predominance diagrams were...CrN powder was synthesized by nitriding Cr metal in ammonia gas flow, and its chemical reaction mechanism and nitridation process were studied. Through thermodynamic calculations, the Cr-N-O predominance diagrams were constructed for different tempera- tures. Chromium nitride formed at 700-1200℃ under relatively higher nitrogen and lower oxygen partial pressures. Phases in the products were then investigated using X-ray diffraction (XRD), and the Cr2N content varied with reaction temperature and holding time. The results indicate that the Cr metal powder nitridation process can be explained by a diffusion model. Further, Cr2N formed as an intermediate product because of an incomplete reaction, which was observed by high-resolution transmission electron microscopy (HRTEM). After nitriding at 1000℃ for 20 h, CrN powder with an average grain size of 63 nm was obtained, and the obtained sample was analyzed by using a scanning electron microscope (SEM).展开更多
Chromium nitride (Cr2N) thin films were prepared by a DC magnetron sputtering technique. The deposition temperature was raised from 50 to 300℃, and its influence on the film structure and refractive index was inves...Chromium nitride (Cr2N) thin films were prepared by a DC magnetron sputtering technique. The deposition temperature was raised from 50 to 300℃, and its influence on the film structure and refractive index was investigated. X-ray diffraction analysis shows that the crystalline strucure of the films transforms from the (101) to (002) oriented hexagonal CrzN phase as the increase of substrate tempera- ture above 50℃, and a highly texatred film grows at 100℃. An empirical relation between the crystalline orientation and infrared active modes of the films is obtained, i.e., the Fourier transform infrared (FTIR) spectrum of the film prepared at 50℃ exhibits only A1 (TO) mode. The prominent peak in the FTIR spectra of the film prepared above 50℃is assigned to the E1 (TO) mode and is correlated with the (002) or c-axis oriented hexagonal wurtzite phase of Cr2N. In the surface analysis of atomic force microscopy, a transformation from the featureless surface to columnar-type morphology is observed with the increase of substrate temperature from 50 to 100℃, exhibiting c-axis oriented crystallite growth. A further increase in substrate temperature to 200℃ causes the c-axis crystallites to merge, resulting in the formation of voids. The refractive index (n) of the deposited films is obtained using spectroscopic ellipsometry.展开更多
Low temperature composite chromizing is a process composed of a plain ion-carbonitriding or ion-nitriding at 550-580℃, followed by a low-temperature chromizing in a salt-bath of 590℃. The microstructure and properti...Low temperature composite chromizing is a process composed of a plain ion-carbonitriding or ion-nitriding at 550-580℃, followed by a low-temperature chromizing in a salt-bath of 590℃. The microstructure and properties of the low temperature composite chromized layer on H13 tool steel were investigated using metallography, X-ray diffraction, microanalysis, hardness and wear tests. It was found that this low temperature process was thermo-dynamically and kinetically possible, and the composite chromized layer on H13 steel, with a thickness of 3-6 μm, consisted of three sub-layers (bands), viz. the outer Cr-rich one, the intermediate (black) one, and the inner, original white layer. After chromizing, the former diffusion layer was thickened. The results of X-ray diffraction showed that the composite chromized layer contained such nitrides and carbides of chromium as CrN, Cr2N, (Cr, Fe)23C6, and (Cr, Fe)7C3, as well as plain α-(Fe, Cr). A high surface microhardness of 1450-1550 HV0.025, which is much higher than that obtained by the conventional ion carbonitriding and ion nitriding, was obtained. In addition, an excellent wear resistance was gained on the composite chromized layer.展开更多
CrN coated steels assisted with a nano Cr interlayer were investigated. The Cr nano-interlayers were prepared by sputter deposition with a thickness about 70-100 nm. CrN coatings were also prepared by sputter depositi...CrN coated steels assisted with a nano Cr interlayer were investigated. The Cr nano-interlayers were prepared by sputter deposition with a thickness about 70-100 nm. CrN coatings were also prepared by sputter deposition on the Cr nano-interlayers. The crystal structures, microhardness, and scratch resistance of CrN/Cr coatings were determined. Results show that the Cr nano-interlayers improve scratch resistance and the microhardness of CrN coated steels. A rapid heat treatment with infrared (IR) was performed for coated specimens in the attempt to improve bonding, With IR heat treatments, the beneficial effect of the Cr nano-interlayers was clearly observed. Without the Cr nano-interlayers, severe cracks on the surface of coatings were observed after IR heat treatment. However, with a Cr interlayer, no cracks on the surface of CrN coatings were observed after the heat treatment. The scratch resistance of coatings was also affected by the Cr nano-interlayers. The scratch track was clean and showed significantly smaller amount of scratch debris for CrN coatings with Cr interlayers than those without the Cr nano-interlayers. The microhardness of coatings with the Cr nano-interlayers is higher than those without the Cr nano-interlayers after IR heat treatment. The Cr and CrN phase have been identified with X-ray diffraction analysis, and the results show that the higher the nitrogen content in the sputtering gas, the stronger the CrN peaks observed in the diffraction patterns are.展开更多
The precipitation kinetics of secondary phases in two austeno-ferritic lean duplex stainless steels(lean DSS)were examined after aging the materials at 800 ℃.Owing to the instability of ferrite,all DSS are known to...The precipitation kinetics of secondary phases in two austeno-ferritic lean duplex stainless steels(lean DSS)were examined after aging the materials at 800 ℃.Owing to the instability of ferrite,all DSS are known to be sensitive to solid-state phase transformations in the critical temperature range 600-1,000 ℃ and different secondary phases may form,depending on composition and microstructure.The performed thermodynamic simulations revealed the proneness to the precipitation of such phases also have been done in lean DSS,but only information on the equilibrium microstructures were achieved.Therefore,the materials were aged at various times,in order to verify the simulations and determine the precipitation kinetics.The occurred structural modifications were observed and quantified by scanning electron microscope and X-ray diffraction measurements,determining phase type,composition and volumetric fraction.At 800 ℃,grade 2101 was found to be only affected by Cr_2N nitrides precipitation,whereas a significant amount of σ-phase was found to form in LDX 2404 for treatment longer than 1 h,almost totally replacing ferrite after 50 h.Up to now,the intermetallic σ-phase has been observed only in the high alloyed DSS,and the unexpected precipitation in grade 2404 highlighted that the increased content of molybdenum in this steel might be considered as determinant for the formation.展开更多
基金financially supported by the Innovation Foundation of Shanghai University (Nos. sdcx2012033 and sdcx2012062)the Special Research Foundation for Training and Selecting Outstanding Young Teachers of Universities in Shanghai (No. B.37-0407-12-008)+1 种基金the National Natural Science Foundation of China (Nos. 51072112 and 51272154)the Projects of International Cooperation and Exchanges NSFC (No. 51311130110)
文摘CrN powder was synthesized by nitriding Cr metal in ammonia gas flow, and its chemical reaction mechanism and nitridation process were studied. Through thermodynamic calculations, the Cr-N-O predominance diagrams were constructed for different tempera- tures. Chromium nitride formed at 700-1200℃ under relatively higher nitrogen and lower oxygen partial pressures. Phases in the products were then investigated using X-ray diffraction (XRD), and the Cr2N content varied with reaction temperature and holding time. The results indicate that the Cr metal powder nitridation process can be explained by a diffusion model. Further, Cr2N formed as an intermediate product because of an incomplete reaction, which was observed by high-resolution transmission electron microscopy (HRTEM). After nitriding at 1000℃ for 20 h, CrN powder with an average grain size of 63 nm was obtained, and the obtained sample was analyzed by using a scanning electron microscope (SEM).
基金financially supported by the National Institute of Laser and Optronics(NILOP)
文摘Chromium nitride (Cr2N) thin films were prepared by a DC magnetron sputtering technique. The deposition temperature was raised from 50 to 300℃, and its influence on the film structure and refractive index was investigated. X-ray diffraction analysis shows that the crystalline strucure of the films transforms from the (101) to (002) oriented hexagonal CrzN phase as the increase of substrate tempera- ture above 50℃, and a highly texatred film grows at 100℃. An empirical relation between the crystalline orientation and infrared active modes of the films is obtained, i.e., the Fourier transform infrared (FTIR) spectrum of the film prepared at 50℃ exhibits only A1 (TO) mode. The prominent peak in the FTIR spectra of the film prepared above 50℃is assigned to the E1 (TO) mode and is correlated with the (002) or c-axis oriented hexagonal wurtzite phase of Cr2N. In the surface analysis of atomic force microscopy, a transformation from the featureless surface to columnar-type morphology is observed with the increase of substrate temperature from 50 to 100℃, exhibiting c-axis oriented crystallite growth. A further increase in substrate temperature to 200℃ causes the c-axis crystallites to merge, resulting in the formation of voids. The refractive index (n) of the deposited films is obtained using spectroscopic ellipsometry.
基金This work was financially supported by the Research Fund for the Doctoral Program of High Education of China(No.20030561001)by the National Natural Science Foundation of China(Grant No.50371028).
文摘Low temperature composite chromizing is a process composed of a plain ion-carbonitriding or ion-nitriding at 550-580℃, followed by a low-temperature chromizing in a salt-bath of 590℃. The microstructure and properties of the low temperature composite chromized layer on H13 tool steel were investigated using metallography, X-ray diffraction, microanalysis, hardness and wear tests. It was found that this low temperature process was thermo-dynamically and kinetically possible, and the composite chromized layer on H13 steel, with a thickness of 3-6 μm, consisted of three sub-layers (bands), viz. the outer Cr-rich one, the intermediate (black) one, and the inner, original white layer. After chromizing, the former diffusion layer was thickened. The results of X-ray diffraction showed that the composite chromized layer contained such nitrides and carbides of chromium as CrN, Cr2N, (Cr, Fe)23C6, and (Cr, Fe)7C3, as well as plain α-(Fe, Cr). A high surface microhardness of 1450-1550 HV0.025, which is much higher than that obtained by the conventional ion carbonitriding and ion nitriding, was obtained. In addition, an excellent wear resistance was gained on the composite chromized layer.
文摘CrN coated steels assisted with a nano Cr interlayer were investigated. The Cr nano-interlayers were prepared by sputter deposition with a thickness about 70-100 nm. CrN coatings were also prepared by sputter deposition on the Cr nano-interlayers. The crystal structures, microhardness, and scratch resistance of CrN/Cr coatings were determined. Results show that the Cr nano-interlayers improve scratch resistance and the microhardness of CrN coated steels. A rapid heat treatment with infrared (IR) was performed for coated specimens in the attempt to improve bonding, With IR heat treatments, the beneficial effect of the Cr nano-interlayers was clearly observed. Without the Cr nano-interlayers, severe cracks on the surface of coatings were observed after IR heat treatment. However, with a Cr interlayer, no cracks on the surface of CrN coatings were observed after the heat treatment. The scratch resistance of coatings was also affected by the Cr nano-interlayers. The scratch track was clean and showed significantly smaller amount of scratch debris for CrN coatings with Cr interlayers than those without the Cr nano-interlayers. The microhardness of coatings with the Cr nano-interlayers is higher than those without the Cr nano-interlayers after IR heat treatment. The Cr and CrN phase have been identified with X-ray diffraction analysis, and the results show that the higher the nitrogen content in the sputtering gas, the stronger the CrN peaks observed in the diffraction patterns are.
文摘The precipitation kinetics of secondary phases in two austeno-ferritic lean duplex stainless steels(lean DSS)were examined after aging the materials at 800 ℃.Owing to the instability of ferrite,all DSS are known to be sensitive to solid-state phase transformations in the critical temperature range 600-1,000 ℃ and different secondary phases may form,depending on composition and microstructure.The performed thermodynamic simulations revealed the proneness to the precipitation of such phases also have been done in lean DSS,but only information on the equilibrium microstructures were achieved.Therefore,the materials were aged at various times,in order to verify the simulations and determine the precipitation kinetics.The occurred structural modifications were observed and quantified by scanning electron microscope and X-ray diffraction measurements,determining phase type,composition and volumetric fraction.At 800 ℃,grade 2101 was found to be only affected by Cr_2N nitrides precipitation,whereas a significant amount of σ-phase was found to form in LDX 2404 for treatment longer than 1 h,almost totally replacing ferrite after 50 h.Up to now,the intermetallic σ-phase has been observed only in the high alloyed DSS,and the unexpected precipitation in grade 2404 highlighted that the increased content of molybdenum in this steel might be considered as determinant for the formation.