冷等离子体氢还原金属氧化物的基础研究
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摘要
氢代替碳还原金属氧化物的主要优点在于其反应产物H_2O不对环境产生任何负面影响,是一种符合人类社会可持续发展战略的绿色冶金过程。但是,要使氢还原真正成为传统碳还原过程强有力的挑战者,除了解决廉价的氢源、氢的安全储运等技术问题之外,还必须寻找出一种低温高效强化还原反应的新方法和新技术。本文研究了施加外场条件下的冷等离子体氢强化氧化物还原的效果和机理,从热力学上比较了等离子体氢和分子氢还原氧化物的差别,揭示了冷等离子体在还原过程中的作用,并分析了冷等离子体氢还原动力学,为将来的应用提供了理论和实践指导依据。
本文在综述了相关的研究进展情况和分析了低温等离子体及其化学特性基础上,选择具有不同还原难易程度的CuO、Fe_2O_3和TiO_2进行了实验,利用直流脉冲电场产生辉光冷等离子体氢对金属氧化物进行还原。
冷等离子体氢还原Fe_2O_3实验研究发现,在分子氢不能还原的条件下(1500Pa,490℃),利用冷等离子氢实现了Fe_2O_3的低温还原。冷等离子体氢还原Fe_2O_3符合逐级还原规律:Fe_2O_3→Fe_3O_4→Fe。随着还原时间的增长,还原过程出现一个加速阶段,这可能是由于试样表面等离子体鞘层的变化导致更多高能量、具有更强还原势的离子氢参加还原过程引起的。进一步的实验结果验证了这一推断。这表明等离子体相中带正电的离子氢和中性的原子氢一样都参加了还原反应,过程中氧化物在反应系统中的电位变化会影响还原的进程,这个结论对工业装置和工艺过程的设计具指导意义。在390℃～530℃范围内,温度变化对还原层厚度影响不大。在680℃的较高温条件下,利用分子氢还原Fe_2O_3仅得到少量的金属Fe和部分FeO,而利用等离子体氢(气体压力为1850Pa,等离子体的输入电压为500V、放电电流为0.3A,还原时间为15min)还原后的试样表面检测全部为金属铁相,这表明等离子体氢的还原能力比单纯的分子氢大得多。随着放电电压、气压、脉冲占空比的增加,还原层的厚度增大,增大的趋势与等离子体中产生的活性氢粒子浓度的大小密切相关。实验证明,把试样放置在活性氢粒子浓度较大的阴极区才能实现氧化物的有效还原。
容易还原的CuO可以在更低的放电气压和电压下得到还原。在体系压力为450Pa、温度为200℃下,与分子态的氢不同,等离子体氢可以还原CuO为Cu,还原过程按CuO→Cu_2O→Cu的规律逐级进行。与Fe_2O_3还原相似,随着还原时间
Reduction of oxides with hydrogen in place of carbon is considered as a green process, which is in accord with the continuable development policy. If hydrogen is applied as a reductant in metallurgical process, besides a solution to low-cast hydrogen source and its safe storage, it's necessary to find out a novel way to enhance the reduction of oxides with hydrogen at low temperature. In this paper, the reduction of oxides with hydrogen cold plasma was investigated. In terms of thermodynamics, the comparative research on reduction with plasma hydrogen and molecular one had been carried out. The effects of cold plasma on the reduction with hydrogen were explored. All done in this work are directive for the application of hydrogen reduction.On the basis of brief review of previous research work and the analysis of the chemical characteristics of cold plasma, a wide range of oxides with different reducibility, CuO, Fe_2O_3 and TiO_2, were used to be reduced in this study. The cold plasma hydrogen was generated by a DC pulsed electric field.The reduction of metal oxide Fe_2O_3 to metal Fe with cold hydrogen plasma was realized under 1500Pa ,490℃, but this reduction did not happen for using molecular hydrogen. The reaction path was as follows: Fe_2O_3→Fe_3O_4→Fe. As the reduction proceeded, the reaction started to accelerate. The reason might be that more active hydrogen species, which are of better reducing potential, participated in the reduction with the modification of the plasma sheath on the sample surface. The results of an additional experiment with a sample placed on a small insulting flake confirmed the above explanation. From this, it could be assumed that ionic and atomic hydrogen species were all involved in reduction and the sample potential was important. This provides a base for the design of the industrial equipments and technologic process. Between 390℃ and 530℃, the reaction temperature had no obvious influence on the reduction. At a high temperature of 680℃,a pressure of 1850Pa and the treatment time of 15min, Fe_2O_3 to Fe with hydrogen cold plasma(the discharge conditions are voltage-500V and current-0.3A.) was realized and only a few of Fe and FeO were detected when using molecular hydrogen. The plasma hydrogen is obviously more reactive than molecular one. With the increase of discharge voltage, gas pressure and the ratio of pulse duty, the thickness of reduced layer also increased. This
had a close relation to the density of active plasma hydrogen species. Only could oxides placed on the cathode be reduced with cold plasma hydrogen generated by DC glow discharge.The reduction of CuO to metallic Cu with cold hydrogen plasma produced by a DC pulsed glow discharge was investigated under a pressure of 450Pa and a reduction temperature of 200 °C. The same reduction had not been achieved when using molecular hydrogen. The reaction proceeded by the sequential reduction of CuO(CuO-^Cu2O~* Cu). Similar to the reduction of ferric oxide, the thickness of the reduced layer increased with the reduction time and was influenced by the change of plasma sheath on the sample surface. Between 160"C and 300°C, the reduction of CuO with hydrogen cold plasma was independent of treatment temperature. It was also found that the inherent characteristics of the product metal had significant influence on the reductions.The reduction of refractory oxide TiO2 to T12O3 with hydrogen cold plasma generated by a DC pulsed glow discharge was realized at 2500Pa, 960°C and 60min. Only a few of TiioOig and TigOn were detected for using molecular hydrogen. Through more experiments, it might be possible for Ti2O3 to be further reduced. The present experimental technique is not suited to producing metallic titanium. It might be related to the reaction kinetics and the concentration of active hydrogen species on the sample surface. Further investigations should be required for the complete reduction of TiO2.In cold hydrogen plasma with moderate pressures, the main chemically active species are H, H+,H+2 and H+3.The density of monatomic hydrogen is greater that of ionic one. The order of the reducibility for these species is H+>H2+>H3+ >H. Though the densities of ionic hydrogen species are less, their reducing potentials are much higher in terms of thermodynamics. More ionic species in plasma are highly advantageous to the reductions of refractory oxides. The reduction ability for monatomic hydrogen was also discussed. It could reduce stable oxides such as Cr2O3, MnO and SiO2 to produce metals at the reduced temperature. This chapter is instructive to reduce refractory oxides with plasma hydrogen and to understand the mechanism on oxides reduction at lower temperature.Based on the above experimental results and plasma chemistry, the steps involved in the reduction of oxides with cold plasma hydrogen and their mathematical descriptions were analyzed in detail. The rate-limiting step was also discussed. When
本文在综述了相关的研究进展情况和分析了低温等离子体及其化学特性基础上,选择具有不同还原难易程度的CuO、Fe_2O_3和TiO_2进行了实验,利用直流脉冲电场产生辉光冷等离子体氢对金属氧化物进行还原。
冷等离子体氢还原Fe_2O_3实验研究发现,在分子氢不能还原的条件下(1500Pa,490℃),利用冷等离子氢实现了Fe_2O_3的低温还原。冷等离子体氢还原Fe_2O_3符合逐级还原规律:Fe_2O_3→Fe_3O_4→Fe。随着还原时间的增长,还原过程出现一个加速阶段,这可能是由于试样表面等离子体鞘层的变化导致更多高能量、具有更强还原势的离子氢参加还原过程引起的。进一步的实验结果验证了这一推断。这表明等离子体相中带正电的离子氢和中性的原子氢一样都参加了还原反应,过程中氧化物在反应系统中的电位变化会影响还原的进程,这个结论对工业装置和工艺过程的设计具指导意义。在390℃～530℃范围内,温度变化对还原层厚度影响不大。在680℃的较高温条件下,利用分子氢还原Fe_2O_3仅得到少量的金属Fe和部分FeO,而利用等离子体氢(气体压力为1850Pa,等离子体的输入电压为500V、放电电流为0.3A,还原时间为15min)还原后的试样表面检测全部为金属铁相,这表明等离子体氢的还原能力比单纯的分子氢大得多。随着放电电压、气压、脉冲占空比的增加,还原层的厚度增大,增大的趋势与等离子体中产生的活性氢粒子浓度的大小密切相关。实验证明,把试样放置在活性氢粒子浓度较大的阴极区才能实现氧化物的有效还原。
容易还原的CuO可以在更低的放电气压和电压下得到还原。在体系压力为450Pa、温度为200℃下,与分子态的氢不同,等离子体氢可以还原CuO为Cu,还原过程按CuO→Cu_2O→Cu的规律逐级进行。与Fe_2O_3还原相似,随着还原时间
Reduction of oxides with hydrogen in place of carbon is considered as a green process, which is in accord with the continuable development policy. If hydrogen is applied as a reductant in metallurgical process, besides a solution to low-cast hydrogen source and its safe storage, it's necessary to find out a novel way to enhance the reduction of oxides with hydrogen at low temperature. In this paper, the reduction of oxides with hydrogen cold plasma was investigated. In terms of thermodynamics, the comparative research on reduction with plasma hydrogen and molecular one had been carried out. The effects of cold plasma on the reduction with hydrogen were explored. All done in this work are directive for the application of hydrogen reduction.On the basis of brief review of previous research work and the analysis of the chemical characteristics of cold plasma, a wide range of oxides with different reducibility, CuO, Fe_2O_3 and TiO_2, were used to be reduced in this study. The cold plasma hydrogen was generated by a DC pulsed electric field.The reduction of metal oxide Fe_2O_3 to metal Fe with cold hydrogen plasma was realized under 1500Pa ,490℃, but this reduction did not happen for using molecular hydrogen. The reaction path was as follows: Fe_2O_3→Fe_3O_4→Fe. As the reduction proceeded, the reaction started to accelerate. The reason might be that more active hydrogen species, which are of better reducing potential, participated in the reduction with the modification of the plasma sheath on the sample surface. The results of an additional experiment with a sample placed on a small insulting flake confirmed the above explanation. From this, it could be assumed that ionic and atomic hydrogen species were all involved in reduction and the sample potential was important. This provides a base for the design of the industrial equipments and technologic process. Between 390℃ and 530℃, the reaction temperature had no obvious influence on the reduction. At a high temperature of 680℃,a pressure of 1850Pa and the treatment time of 15min, Fe_2O_3 to Fe with hydrogen cold plasma(the discharge conditions are voltage-500V and current-0.3A.) was realized and only a few of Fe and FeO were detected when using molecular hydrogen. The plasma hydrogen is obviously more reactive than molecular one. With the increase of discharge voltage, gas pressure and the ratio of pulse duty, the thickness of reduced layer also increased. This
had a close relation to the density of active plasma hydrogen species. Only could oxides placed on the cathode be reduced with cold plasma hydrogen generated by DC glow discharge.The reduction of CuO to metallic Cu with cold hydrogen plasma produced by a DC pulsed glow discharge was investigated under a pressure of 450Pa and a reduction temperature of 200 °C. The same reduction had not been achieved when using molecular hydrogen. The reaction proceeded by the sequential reduction of CuO(CuO-^Cu2O~* Cu). Similar to the reduction of ferric oxide, the thickness of the reduced layer increased with the reduction time and was influenced by the change of plasma sheath on the sample surface. Between 160"C and 300°C, the reduction of CuO with hydrogen cold plasma was independent of treatment temperature. It was also found that the inherent characteristics of the product metal had significant influence on the reductions.The reduction of refractory oxide TiO2 to T12O3 with hydrogen cold plasma generated by a DC pulsed glow discharge was realized at 2500Pa, 960°C and 60min. Only a few of TiioOig and TigOn were detected for using molecular hydrogen. Through more experiments, it might be possible for Ti2O3 to be further reduced. The present experimental technique is not suited to producing metallic titanium. It might be related to the reaction kinetics and the concentration of active hydrogen species on the sample surface. Further investigations should be required for the complete reduction of TiO2.In cold hydrogen plasma with moderate pressures, the main chemically active species are H, H+,H+2 and H+3.The density of monatomic hydrogen is greater that of ionic one. The order of the reducibility for these species is H+>H2+>H3+ >H. Though the densities of ionic hydrogen species are less, their reducing potentials are much higher in terms of thermodynamics. More ionic species in plasma are highly advantageous to the reductions of refractory oxides. The reduction ability for monatomic hydrogen was also discussed. It could reduce stable oxides such as Cr2O3, MnO and SiO2 to produce metals at the reduced temperature. This chapter is instructive to reduce refractory oxides with plasma hydrogen and to understand the mechanism on oxides reduction at lower temperature.Based on the above experimental results and plasma chemistry, the steps involved in the reduction of oxides with cold plasma hydrogen and their mathematical descriptions were analyzed in detail. The rate-limiting step was also discussed. When
引文
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