熔融盐电脱氧法制备锆镍合金的研究
发布时间：2018-07-20 21:49
【摘要】： ZrNi合金广泛应用于核工业、航天和海底探测设备的制造等领域,ZrNi合金还被用于分解水蒸气、甲烷来制取氢,对普及氢气应用和促进燃料电池的发展也有重要作用,它是一种优良的储氢材料,是目前重要的储氢材料之一熔融盐电脱氧法是近年来才发展起来的一种冶金新技术,它可以降低生产成本,简化工艺流程,污染较少。 本文采用FFC法(熔盐电脱氧法),在CaCl2和NaCl熔盐中,以烧结的ZrO2-NiO片为阴极,石墨碳棒为阳极,在一定的电压和温度下电解,将ZrO2-NiO片直接还原成锆镍合金。 实验通过记录电解过程中时产-电流变化曲线,利用X射线衍射仪测试阴极片电解前后的物相组成；利用扫描电子显微镜测试不同条件下阴极片的微观形貌,并通过EDS测定阴极片电解前后相关元素的含量,采用阿基米德排水法测定阴极片的孔隙率,研究了相关因素对电脱氧的影响。 研究发现随着烧结温度的升高和烧结时间的延长,阴极片强度升高,阴极片内部氧化物颗粒发生二次结晶,1100℃烧结12h时阴极片内部颗粒大小适中、孔隙率较高,脱氧效果较好；成型压力较小时,颗粒间结合不够紧密,导电性不好,不利于电脱氧进行,同时电极容易粉化；成型压力太大时,片体内部非常致密,孔隙率较低,熔盐向内渗透困难,也不利于电脱氧反应的进行；随着电解时间的延长,氧化物脱氧越来越完全,残余氧含量越低；随着电解温度的升高,促进了氧离子的扩散,加快了电脱氧反应的速率,但温度过高时脱氧反应不稳定,电流波动较大不利于反应的控制。实验发现NiO的加入有效的促进了Zr02电脱氧,脱氧效率可以提高80%以上 实验得到最佳的工艺条件为：ZrO2-NiO粉末在10MPa下压制成型、1100℃烧结12h,在800℃的CaCl2-NaCl熔盐中,3.1V的电压下电解8h,可得到锆镍合金,残余氧含量低于0.9%。
[Abstract]:ZrNi alloys are widely used in the nuclear industry, aerospace and submarine detection equipment, and are also used to decompose water vapor and methane to produce hydrogen, which also plays an important role in popularizing hydrogen applications and promoting the development of fuel cells. It is an excellent hydrogen storage material. It is one of the most important hydrogen storage materials at present. It is a new metallurgical technology developed in recent years. It can reduce the production cost, simplify the technological process and cause less pollution. In this paper, the ZrO2-NiO alloy was directly reduced by FFC method (molten salt electrodeoxidation method) in CaCl2 and NaCl molten salt, with the sintered ZrO2-NiO sheet as cathode and graphite bar as anode, and electrolyzed at a certain voltage and temperature, the ZrO2-NiO wafer was directly reduced to zirconium nickel alloy. The phase composition of cathode before and after electrolysis was measured by X-ray diffractometer, and the micromorphology of cathode sheet under different conditions was measured by scanning electron microscope (SEM). The content of relative elements before and after electrolysis was determined by EDS and the porosity of cathode sheet was measured by Archimedes drainage method. The effect of related factors on electrodeoxidation was studied. It is found that with the increase of sintering temperature and sintering time, the strength of cathode plate increases, and the particle size is moderate, the porosity is high and the deoxidization effect is better when the oxide particles in the cathode plate are sintered at 1100 鈩，
本文编号：2134895
[Abstract]:ZrNi alloys are widely used in the nuclear industry, aerospace and submarine detection equipment, and are also used to decompose water vapor and methane to produce hydrogen, which also plays an important role in popularizing hydrogen applications and promoting the development of fuel cells. It is an excellent hydrogen storage material. It is one of the most important hydrogen storage materials at present. It is a new metallurgical technology developed in recent years. It can reduce the production cost, simplify the technological process and cause less pollution. In this paper, the ZrO2-NiO alloy was directly reduced by FFC method (molten salt electrodeoxidation method) in CaCl2 and NaCl molten salt, with the sintered ZrO2-NiO sheet as cathode and graphite bar as anode, and electrolyzed at a certain voltage and temperature, the ZrO2-NiO wafer was directly reduced to zirconium nickel alloy. The phase composition of cathode before and after electrolysis was measured by X-ray diffractometer, and the micromorphology of cathode sheet under different conditions was measured by scanning electron microscope (SEM). The content of relative elements before and after electrolysis was determined by EDS and the porosity of cathode sheet was measured by Archimedes drainage method. The effect of related factors on electrodeoxidation was studied. It is found that with the increase of sintering temperature and sintering time, the strength of cathode plate increases, and the particle size is moderate, the porosity is high and the deoxidization effect is better when the oxide particles in the cathode plate are sintered at 1100 鈩，
本文编号：2134895
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