利用锆英石制备ZrO_2-SiC、ZrN-Si_3N_4复合粉体及ZrN-Sialon结合刚玉复合材料
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摘要
本文首次以锆英石为原料,对其材料化利用进行了研究,为实现矿产的综合利用开辟一条新途径。在热力学分析的基础上,采用碳热还原(氮化)法制备出ZrO2-SiC和ZrN-Si3N4复合粉体,探讨了其合成机理；将ZrO2-SiC复合粉体应用于Al2O3-C质耐火材料中,研究了其添加量对耐火材料性能的影响；通过原位反应制备了Al2O3-ZrO2-SiC-C系复合耐火材料,探讨了在刚玉质和Al2O3-C质耐火材料中原位生成ZrO2-SiC材料的可行性。还以锆英石、碳黑、氧化铝微粉和电熔刚玉为原料,成功制备出ZrN-Sialon结合刚玉复合材料,并对其性能进行了研究。主要结论如下：
(1)分析了CO(g)、SiO(g)、ZrO(g)、N2(g)和02(g)等气相分压对Si-C-O、Zr-C-O、Zr-Si-C-0及Si-C-N-0等体系相稳定性的影响。
(2)研究了加热温度和添加La203对ZrO2-SiC复合粉体合成过程的影响,并探讨了其合成机理和La2O3的催化作用机理。结果表明,在本实验条件下,提高加热温度和添加La2O3有利于ZrSiO4的分解及SiC的生成；不添加La2O3时,适宜的合成温度为1600℃；当添加2%质量分数的La2O3时,其合成温度降低为1530℃。
(3)以电熔刚玉、天然石墨和酚醛树脂为原料,自合成ZrO2-SiC和工业SiC粉体为添加剂制成Al2O3-C质耐火材料,研究了添加剂加入量对耐火材料性能的影响,并分析了添加剂的抗氧化及抗热震机理。结果表明,添加ZrO2-SiC及工业SiC粉体均有利于降低Al2O3-C质耐火材料的显气孔率,提高其体积密度和常温耐压强度,改善其抗氧化性及抗热震性。在本实验条件下,添加6%质量分数的ZrO2-SiC复合粉体及工业SiC粉后,耐火材料的抗氧化和抗热震性能最佳。
(4)以电熔刚玉、天然石墨、锆英石及碳黑为原料,利用碳热还原反应在刚玉质和Al2O3-C质耐火材料中原位合成ZrO2-SiC材料。研究了原料组成、成型压力及加热温度等因素对材料制备及性能的影响。结果表明,以电熔刚玉、锆英石和碳黑为原料,在氩气气氛中于1530℃保温4h可以合成出Al2O3-ZrO2-SiC复合耐火材料;当加入20%(质量分数)锆英石和碳黑时,Al2O3-ZrO2-SiC材料的体积密度为2.58g／cm3。将适量的锆英石添加到Al2O3-C耐火材料中,于1500℃下保温4h可以原位合成Al2O3-ZrO2-SiC-C复合耐火材料；在200MPa压力下成型于该温度下合成材料的体积密度为2.73g／cm3,质量损失率为7.69%。
(5)研究了原料组成、加热温度和保温时间等工艺因素对ZrN-Si3N4复合粉体合成过程的影响,并探讨了其合成机理。结果表明,配料组成中碳黑的含量越大,碳热还原反应进行得越完全,但配C量存在一个最佳值；提高加热温度和延长保温时间均有利于ZrSiO4的分解及Si3N4和ZrN的生成。综合考虑,锆英石与碳黑的质量配比为100/40、1500℃保温12h是较理想的合成条件。
(6)根据有关反应的热力学数据绘制了Al2O3-ZrO2-SiO2-C-N2体系优势区图,分析了CO气相分压和温度对体系相稳定性的影响。研究了原料组成和加热温度等工艺因素对ZrN-Sialon结合刚玉复合材料制备及性能的影响,并探讨了其合成机理。结果表明,提高加热温度和增加锆英石和碳黑加入量均有利于ZrSiO4的分解及Sialon和ZrN的生成；在本实验条件下,制备ZrN-Sialon结合刚玉复合材料的适宜温度为1500℃。
In this paper, the utilization of zircon by means of materials synthesis was studied using zircon as the main starting materials, which developed a new route for the comprehensive application of mineral resources. Based on the thermodynamic analysis, ZrO2-SiC and ZrN-Si3N4 composite powders were prepared by carbothermal reduction (nitridation) reaction, and the synthesis mechanisms of them were discussed. Furthermore, the ZrO2-SiC composite powder was applied into Al2O3-C refractories to study the effect of its addition on properties of the refractories. In addition, the Al2O3-ZrO2-SiC-C refractories were prepared by in-situ reaction, and the feasibility of in-situ synthesis of ZrO2-SiC composite in corundum and Al2O3-C refractories was discussed. Moreover, zircon, carbon black, alumina micropowder and fused corundum were used as the starting materials for the preparation of ZrN-Sialon bonded corundum composite to study the properties of the material. The following conclusions were obtained.
(1) The effects of partial pressures of CO, SiO, ZrO, N2 and O2 gases on the phase stability in Si-C-O, Zr-C-O, Zr-Si-C-O and Si-C-N-O systems.
(2) The effects of heating temperature and La2O3 addition on the synthesis process of ZrO2-SiC composite powder were studied, and the synthesis mechanism and the catalysis action of La2O3 were discussed. The results show increasing the heating temperature and the addition of La2O3 were favorable for the decomposition of zircon and the formation of SiC in this experimental condition. The proper temperature to synthesize ZrO2-SiC composite powder was 1600℃while the sample without La2O3 addition, and the temperature was decreased to 1530℃when the sample added with 2% La2O3.
(3) The Al2O3-C refractories were prepared by using fused corundum, natural graphite and phenolic resin as the starting materials and the synthesized ZrO2-SiC composite powder and industrial SiC powder as the additives to investigate the effects of their additions on properties of the refractories, and the mechanisms of oxidation resistance and thermal shock resistance of the additives were discussed. The results show that the bulk density, cold crushing strength, oxidation resistance and thermal shock resistance of the refractories could be improved by the additions of ZrO2-SiC composite powder and industrial SiC powder, however, the apparent porosity was decreased. In this experimental condition, the refractories added with 6% ZrO2-SiC composite powder or industrial SiC powder had the best oxidation resistance and thermal shock resistance.
(4) Fused corundum, natural graphite, zircon and carbon black were used as the starting materials for in-situ synthesis of the ZrO2-SiC composite in corundum and Al2O3-C refractories by carbothermal reduction reaction, and the effects of composition of the starting materials, forming pressure and heating temperature on the preparation and properties of the composite were studied. The results show that the Al2O3-ZrO2-SiC composite could be synthesized at 1530℃for 4h in argon gas by using fused corundum, zircon and carbon black as the starting materials. The bulk density of the Al2O3-ZrO2-SiC composite by the addition of 20% zircon and carbon black reached 2.58g/cm3. Moreover, when adding moderate zircon into the Al2O3-C refractories, the Al2O3-ZrO2-SiC-C composite could be synthesized at 1500℃for 4h by in-situ reaction. The bulk density and the mass loss ratio of the synthesized composite reached 2.73g/cm3 and 7.69%, respectively.
(5) The effects of composition of the starting materials, heating temperature and holding time on the synthesis process of ZrN-Si3N4 composite powder were studied, and the synthesis mechanism was discussed. The results show that the carbothermal reduction reaction was more sufficient with the increasing of the carbon black content in sample, however, it had an optical value. Increasing the heating temperature and holding time could promote the decomposition of zircon and the formation of Si3N4 and ZrN, and the optimum synthesis condition was mass ratio of zircon and carbon black of 100/40, synthesizing temperature of 1500℃and holding time of 12h.
(6) The predominant region diagram of Al2O3-ZrO2-SiO2-C-N2 system was plotted through the thermodynamic data of some reactions to analyze the effects of partial pressure of CO gas and temperature on the stability of phases. In addition, the effects of composition of the starting materials and heating temperature on the preparation process and properties of the ZrN-Sialon bonded corundum composite were studied, and the synthesis mechanism was discussed. The results show that increasing the heating temperature as well as zircon and carbon black content were in favor of the decomposition of zircon and the formation of Sialon and ZrN. In this experimental condition, the proper temperature to synthesize ZrN-Sialon bonded corundum composite was 1500℃.
(1)分析了CO(g)、SiO(g)、ZrO(g)、N2(g)和02(g)等气相分压对Si-C-O、Zr-C-O、Zr-Si-C-0及Si-C-N-0等体系相稳定性的影响。
(2)研究了加热温度和添加La203对ZrO2-SiC复合粉体合成过程的影响,并探讨了其合成机理和La2O3的催化作用机理。结果表明,在本实验条件下,提高加热温度和添加La2O3有利于ZrSiO4的分解及SiC的生成；不添加La2O3时,适宜的合成温度为1600℃；当添加2%质量分数的La2O3时,其合成温度降低为1530℃。
(3)以电熔刚玉、天然石墨和酚醛树脂为原料,自合成ZrO2-SiC和工业SiC粉体为添加剂制成Al2O3-C质耐火材料,研究了添加剂加入量对耐火材料性能的影响,并分析了添加剂的抗氧化及抗热震机理。结果表明,添加ZrO2-SiC及工业SiC粉体均有利于降低Al2O3-C质耐火材料的显气孔率,提高其体积密度和常温耐压强度,改善其抗氧化性及抗热震性。在本实验条件下,添加6%质量分数的ZrO2-SiC复合粉体及工业SiC粉后,耐火材料的抗氧化和抗热震性能最佳。
(4)以电熔刚玉、天然石墨、锆英石及碳黑为原料,利用碳热还原反应在刚玉质和Al2O3-C质耐火材料中原位合成ZrO2-SiC材料。研究了原料组成、成型压力及加热温度等因素对材料制备及性能的影响。结果表明,以电熔刚玉、锆英石和碳黑为原料,在氩气气氛中于1530℃保温4h可以合成出Al2O3-ZrO2-SiC复合耐火材料;当加入20%(质量分数)锆英石和碳黑时,Al2O3-ZrO2-SiC材料的体积密度为2.58g／cm3。将适量的锆英石添加到Al2O3-C耐火材料中,于1500℃下保温4h可以原位合成Al2O3-ZrO2-SiC-C复合耐火材料；在200MPa压力下成型于该温度下合成材料的体积密度为2.73g／cm3,质量损失率为7.69%。
(5)研究了原料组成、加热温度和保温时间等工艺因素对ZrN-Si3N4复合粉体合成过程的影响,并探讨了其合成机理。结果表明,配料组成中碳黑的含量越大,碳热还原反应进行得越完全,但配C量存在一个最佳值；提高加热温度和延长保温时间均有利于ZrSiO4的分解及Si3N4和ZrN的生成。综合考虑,锆英石与碳黑的质量配比为100/40、1500℃保温12h是较理想的合成条件。
(6)根据有关反应的热力学数据绘制了Al2O3-ZrO2-SiO2-C-N2体系优势区图,分析了CO气相分压和温度对体系相稳定性的影响。研究了原料组成和加热温度等工艺因素对ZrN-Sialon结合刚玉复合材料制备及性能的影响,并探讨了其合成机理。结果表明,提高加热温度和增加锆英石和碳黑加入量均有利于ZrSiO4的分解及Sialon和ZrN的生成；在本实验条件下,制备ZrN-Sialon结合刚玉复合材料的适宜温度为1500℃。
In this paper, the utilization of zircon by means of materials synthesis was studied using zircon as the main starting materials, which developed a new route for the comprehensive application of mineral resources. Based on the thermodynamic analysis, ZrO2-SiC and ZrN-Si3N4 composite powders were prepared by carbothermal reduction (nitridation) reaction, and the synthesis mechanisms of them were discussed. Furthermore, the ZrO2-SiC composite powder was applied into Al2O3-C refractories to study the effect of its addition on properties of the refractories. In addition, the Al2O3-ZrO2-SiC-C refractories were prepared by in-situ reaction, and the feasibility of in-situ synthesis of ZrO2-SiC composite in corundum and Al2O3-C refractories was discussed. Moreover, zircon, carbon black, alumina micropowder and fused corundum were used as the starting materials for the preparation of ZrN-Sialon bonded corundum composite to study the properties of the material. The following conclusions were obtained.
(1) The effects of partial pressures of CO, SiO, ZrO, N2 and O2 gases on the phase stability in Si-C-O, Zr-C-O, Zr-Si-C-O and Si-C-N-O systems.
(2) The effects of heating temperature and La2O3 addition on the synthesis process of ZrO2-SiC composite powder were studied, and the synthesis mechanism and the catalysis action of La2O3 were discussed. The results show increasing the heating temperature and the addition of La2O3 were favorable for the decomposition of zircon and the formation of SiC in this experimental condition. The proper temperature to synthesize ZrO2-SiC composite powder was 1600℃while the sample without La2O3 addition, and the temperature was decreased to 1530℃when the sample added with 2% La2O3.
(3) The Al2O3-C refractories were prepared by using fused corundum, natural graphite and phenolic resin as the starting materials and the synthesized ZrO2-SiC composite powder and industrial SiC powder as the additives to investigate the effects of their additions on properties of the refractories, and the mechanisms of oxidation resistance and thermal shock resistance of the additives were discussed. The results show that the bulk density, cold crushing strength, oxidation resistance and thermal shock resistance of the refractories could be improved by the additions of ZrO2-SiC composite powder and industrial SiC powder, however, the apparent porosity was decreased. In this experimental condition, the refractories added with 6% ZrO2-SiC composite powder or industrial SiC powder had the best oxidation resistance and thermal shock resistance.
(4) Fused corundum, natural graphite, zircon and carbon black were used as the starting materials for in-situ synthesis of the ZrO2-SiC composite in corundum and Al2O3-C refractories by carbothermal reduction reaction, and the effects of composition of the starting materials, forming pressure and heating temperature on the preparation and properties of the composite were studied. The results show that the Al2O3-ZrO2-SiC composite could be synthesized at 1530℃for 4h in argon gas by using fused corundum, zircon and carbon black as the starting materials. The bulk density of the Al2O3-ZrO2-SiC composite by the addition of 20% zircon and carbon black reached 2.58g/cm3. Moreover, when adding moderate zircon into the Al2O3-C refractories, the Al2O3-ZrO2-SiC-C composite could be synthesized at 1500℃for 4h by in-situ reaction. The bulk density and the mass loss ratio of the synthesized composite reached 2.73g/cm3 and 7.69%, respectively.
(5) The effects of composition of the starting materials, heating temperature and holding time on the synthesis process of ZrN-Si3N4 composite powder were studied, and the synthesis mechanism was discussed. The results show that the carbothermal reduction reaction was more sufficient with the increasing of the carbon black content in sample, however, it had an optical value. Increasing the heating temperature and holding time could promote the decomposition of zircon and the formation of Si3N4 and ZrN, and the optimum synthesis condition was mass ratio of zircon and carbon black of 100/40, synthesizing temperature of 1500℃and holding time of 12h.
(6) The predominant region diagram of Al2O3-ZrO2-SiO2-C-N2 system was plotted through the thermodynamic data of some reactions to analyze the effects of partial pressure of CO gas and temperature on the stability of phases. In addition, the effects of composition of the starting materials and heating temperature on the preparation process and properties of the ZrN-Sialon bonded corundum composite were studied, and the synthesis mechanism was discussed. The results show that increasing the heating temperature as well as zircon and carbon black content were in favor of the decomposition of zircon and the formation of Sialon and ZrN. In this experimental condition, the proper temperature to synthesize ZrN-Sialon bonded corundum composite was 1500℃.
引文
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