熔融鹽電脫氧法制備鋯鎳合金的研究
發(fā)布時(shí)間:2018-07-20 21:49
【摘要】: ZrNi合金廣泛應(yīng)用于核工業(yè)、航天和海底探測(cè)設(shè)備的制造等領(lǐng)域,ZrNi合金還被用于分解水蒸氣、甲烷來(lái)制取氫,對(duì)普及氫氣應(yīng)用和促進(jìn)燃料電池的發(fā)展也有重要作用,它是一種優(yōu)良的儲(chǔ)氫材料,是目前重要的儲(chǔ)氫材料之一熔融鹽電脫氧法是近年來(lái)才發(fā)展起來(lái)的一種冶金新技術(shù),它可以降低生產(chǎn)成本,簡(jiǎn)化工藝流程,污染較少。 本文采用FFC法(熔鹽電脫氧法),在CaCl2和NaCl熔鹽中,以燒結(jié)的ZrO2-NiO片為陰極,石墨碳棒為陽(yáng)極,在一定的電壓和溫度下電解,將ZrO2-NiO片直接還原成鋯鎳合金。 實(shí)驗(yàn)通過(guò)記錄電解過(guò)程中時(shí)產(chǎn)-電流變化曲線,利用X射線衍射儀測(cè)試陰極片電解前后的物相組成;利用掃描電子顯微鏡測(cè)試不同條件下陰極片的微觀形貌,并通過(guò)EDS測(cè)定陰極片電解前后相關(guān)元素的含量,采用阿基米德排水法測(cè)定陰極片的孔隙率,研究了相關(guān)因素對(duì)電脫氧的影響。 研究發(fā)現(xiàn)隨著燒結(jié)溫度的升高和燒結(jié)時(shí)間的延長(zhǎng),陰極片強(qiáng)度升高,陰極片內(nèi)部氧化物顆粒發(fā)生二次結(jié)晶,1100℃燒結(jié)12h時(shí)陰極片內(nèi)部顆粒大小適中、孔隙率較高,脫氧效果較好;成型壓力較小時(shí),顆粒間結(jié)合不夠緊密,導(dǎo)電性不好,不利于電脫氧進(jìn)行,同時(shí)電極容易粉化;成型壓力太大時(shí),片體內(nèi)部非常致密,孔隙率較低,熔鹽向內(nèi)滲透困難,也不利于電脫氧反應(yīng)的進(jìn)行;隨著電解時(shí)間的延長(zhǎng),氧化物脫氧越來(lái)越完全,殘余氧含量越低;隨著電解溫度的升高,促進(jìn)了氧離子的擴(kuò)散,加快了電脫氧反應(yīng)的速率,但溫度過(guò)高時(shí)脫氧反應(yīng)不穩(wěn)定,電流波動(dòng)較大不利于反應(yīng)的控制。實(shí)驗(yàn)發(fā)現(xiàn)NiO的加入有效的促進(jìn)了Zr02電脫氧,脫氧效率可以提高80%以上 實(shí)驗(yàn)得到最佳的工藝條件為:ZrO2-NiO粉末在10MPa下壓制成型、1100℃燒結(jié)12h,在800℃的CaCl2-NaCl熔鹽中,3.1V的電壓下電解8h,可得到鋯鎳合金,殘余氧含量低于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,
本文編號(hào):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,
本文編號(hào):2134895
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