添加镁锆砂及环保沥青对低碳镁碳砖性能影响的研究
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摘要
随着炉外精炼工艺的发展,低碳镁碳耐火材料成为镁碳耐火材料的研究热点。本论文综述了低碳镁碳耐火材料的发展概况及目前存在的主要问题,根据其所必须具备的强度、抗氧化性、抗侵蚀性、抗热震性等性能要求,在实验室条件下研究了镁砂临界粒度、镁砂颗粒级配、镁锆砂粒度及加入量、环保沥青加入量对低碳镁碳耐火材料结构与性能的影响。测定了不同温度处理后试样的体积密度、耐压强度等物理性能,以及试样的热膨胀率、抗氧化性能、抗热震性能、抗渣侵蚀性。通过X-射线衍射分析了试样的物相组成,用扫描电镜观察了试样的显微结构。得出的结论如下:
1)在低碳镁碳耐火材料中,镁砂临界颗粒变小,试样的气孔率下降,气孔孔径变小,产生的热应力小,成型后试样体积密度、耐压强度增大,热膨胀率减小。此外,气孔孔径变小,氧气扩散速度降低,制品的抗氧化性也得到提高。
2)在石墨含量不变的条件下,适当减少镁砂细粉含量,增大粗、中颗粒含量,可减少镁砂颗粒总的比表面积,使得基质中石墨分布集中,具有缓解热应力的作用,且细粉量少,可降低MgO与石墨反应的速度,提高制品的抗氧化性、抗侵蚀性。
3)用颗粒及细粉两种粒度的镁锆砂替代镁砂添加到低碳镁碳耐火材料中,由于镁锆砂本身体积密度大、抗侵蚀性能好及氧化锆相变增韧的作用,可以明显增大制品体积密度,降低热膨胀率,提高抗热震性能及抗侵蚀性能。与未加镁锆砂的试样相比,当镁锆砂加入量为15%时,侵蚀层厚度降低38%,热膨胀率降低12.6%。
4)添加环保沥青后,在试样烧成过程中,由于沥青高温流动性好,促进了金属Al氧化后的产物Al_2O_3与MgO的反应及AlON固溶体的形成,制品中有大量纳米级AlON、MgAl_2O_4的生成,提高了试样的致密度、常温耐压强度。试样热震实验后,未加沥青试样抗折强度保持率为67%,而加沥青试样抗折强度保持率最高达78%,抗热震性得到提高。此外,沥青高温炭化后与树脂碳形成镶嵌结构,提高了残碳率,也有利于试样抗侵蚀性及抗热震性的提高。
With the developing of external refining technology,, low carbon magnesia-carbon refractories became a research hotspot of the magnesia-carbon refractories. This work overviewed the development and the drawbacks of low carbon magnesia-carbon material, it requires champion strength, antioxidation, corrodibility resistance and thermal shock resistance and so on. According to the requirements above, this paper studied the effect of MgO particle size, MgO granularity, magnesia-zirconia powder size and content, pitch content on structure and conventional properties of low carbon magnesia-carbon refractories.
After sintered for different experimental intentions, the bulk density, apparent porosity, cold crushing strength and high temperature bending strength of the specimens were determined, respectively. Besides properties above, antioxidation resistance, thermal expansion, thermal shock resistance and corrodibility resistance also determined, the phase composition and microstructure were observed by X-ray diffraction instrument, scanning electronic microscope, respectively. Then, conclusions are obtained as follows:
1) MgO particle size plays an important role in improving the properties of low carbon MgO-C refractories. Reducing MgO granule size, the apparent porosity, pore size of sample and thermal stress became smaller, the bulk density, compressive strength improved, and the thermal expansion of specimens reduced. Besides, the pore size diminished, the speed of O2 diffusion slowed, and that can improve the oxidation resistance.
2) Reduce magnesia power content and increase magnesia particle content, it can cause the low carbon magnesia-carbon refractories to have the graphite relative centralism phenomenon, and this can release thermal stress, and is propitious to enhance the materials’oxidation resistance and corrosion resistance.
3) The influence of particle size and quantity of magnesia-zirconia powder on properties of low carbon magnesia-carbon refractories has been investigated. The results indicated that, because of the nature characters of magnesia-zirconia powder, such as, big bulk density, good corrosion resistance and phase transformation toughening of zirconia, both particle and powder can improve the physical properties, oxidation resistance, corrosion resistance and thermal shock resistance of low carbon magnesia-carbon materials. Compared with blank sample, when the magnesia-zirconia powder content is 15%, the thickness of corrosion layer reduced 38%, and the thermal expansion ratio reduced 12.6%.
4) Pitch additive can promote the formation of spinel in specimens when sintered, this caused by the fine liquidity of pitch at high temperature. Because of the formation of AlON and MgAl_2O_4, the density, cold crushing strength and thermal shock resistance of specimens improved, after thermal shock test, the conservation rate of bend strength of blank sample remains 67%, but when pitch added, the number raise to 78%. Moreover, mosaic structure can formed when pitch and resin charred, and this will increase the carbon residue of composite, and it benefit to enhance the corrosion resistance and thermal shock resistance of specimens.
1)在低碳镁碳耐火材料中,镁砂临界颗粒变小,试样的气孔率下降,气孔孔径变小,产生的热应力小,成型后试样体积密度、耐压强度增大,热膨胀率减小。此外,气孔孔径变小,氧气扩散速度降低,制品的抗氧化性也得到提高。
2)在石墨含量不变的条件下,适当减少镁砂细粉含量,增大粗、中颗粒含量,可减少镁砂颗粒总的比表面积,使得基质中石墨分布集中,具有缓解热应力的作用,且细粉量少,可降低MgO与石墨反应的速度,提高制品的抗氧化性、抗侵蚀性。
3)用颗粒及细粉两种粒度的镁锆砂替代镁砂添加到低碳镁碳耐火材料中,由于镁锆砂本身体积密度大、抗侵蚀性能好及氧化锆相变增韧的作用,可以明显增大制品体积密度,降低热膨胀率,提高抗热震性能及抗侵蚀性能。与未加镁锆砂的试样相比,当镁锆砂加入量为15%时,侵蚀层厚度降低38%,热膨胀率降低12.6%。
4)添加环保沥青后,在试样烧成过程中,由于沥青高温流动性好,促进了金属Al氧化后的产物Al_2O_3与MgO的反应及AlON固溶体的形成,制品中有大量纳米级AlON、MgAl_2O_4的生成,提高了试样的致密度、常温耐压强度。试样热震实验后,未加沥青试样抗折强度保持率为67%,而加沥青试样抗折强度保持率最高达78%,抗热震性得到提高。此外,沥青高温炭化后与树脂碳形成镶嵌结构,提高了残碳率,也有利于试样抗侵蚀性及抗热震性的提高。
With the developing of external refining technology,, low carbon magnesia-carbon refractories became a research hotspot of the magnesia-carbon refractories. This work overviewed the development and the drawbacks of low carbon magnesia-carbon material, it requires champion strength, antioxidation, corrodibility resistance and thermal shock resistance and so on. According to the requirements above, this paper studied the effect of MgO particle size, MgO granularity, magnesia-zirconia powder size and content, pitch content on structure and conventional properties of low carbon magnesia-carbon refractories.
After sintered for different experimental intentions, the bulk density, apparent porosity, cold crushing strength and high temperature bending strength of the specimens were determined, respectively. Besides properties above, antioxidation resistance, thermal expansion, thermal shock resistance and corrodibility resistance also determined, the phase composition and microstructure were observed by X-ray diffraction instrument, scanning electronic microscope, respectively. Then, conclusions are obtained as follows:
1) MgO particle size plays an important role in improving the properties of low carbon MgO-C refractories. Reducing MgO granule size, the apparent porosity, pore size of sample and thermal stress became smaller, the bulk density, compressive strength improved, and the thermal expansion of specimens reduced. Besides, the pore size diminished, the speed of O2 diffusion slowed, and that can improve the oxidation resistance.
2) Reduce magnesia power content and increase magnesia particle content, it can cause the low carbon magnesia-carbon refractories to have the graphite relative centralism phenomenon, and this can release thermal stress, and is propitious to enhance the materials’oxidation resistance and corrosion resistance.
3) The influence of particle size and quantity of magnesia-zirconia powder on properties of low carbon magnesia-carbon refractories has been investigated. The results indicated that, because of the nature characters of magnesia-zirconia powder, such as, big bulk density, good corrosion resistance and phase transformation toughening of zirconia, both particle and powder can improve the physical properties, oxidation resistance, corrosion resistance and thermal shock resistance of low carbon magnesia-carbon materials. Compared with blank sample, when the magnesia-zirconia powder content is 15%, the thickness of corrosion layer reduced 38%, and the thermal expansion ratio reduced 12.6%.
4) Pitch additive can promote the formation of spinel in specimens when sintered, this caused by the fine liquidity of pitch at high temperature. Because of the formation of AlON and MgAl_2O_4, the density, cold crushing strength and thermal shock resistance of specimens improved, after thermal shock test, the conservation rate of bend strength of blank sample remains 67%, but when pitch added, the number raise to 78%. Moreover, mosaic structure can formed when pitch and resin charred, and this will increase the carbon residue of composite, and it benefit to enhance the corrosion resistance and thermal shock resistance of specimens.
引文
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