VO_2薄膜制备及其应用性能基础研究
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摘要
攀钢(集团)公司是我国最重要的钢铁钒钛基地，攀西地区蕴藏有丰富的钒钛磁铁矿资源，其中钒资源占全国的63%以上。三十多年来，攀钢(集团)公司利用钒钛磁铁矿资源生产了大量的钢材，以及大量的钒渣、V2O5、V2O3、钒铁等钒产品，使我国成为世界上主要的产钒国之一。但是，钒资源的综合利用程度还不够高，钒产品的种类还较少、产品档次和科技含量还比较低。因此研究开发新的、高科技含量的钒产品，从而进一步提高钒资源综合利用水平，是非常必要和迫切的。
对功能材料VO2薄膜的研究倍受人们的关注。因为它的一个重要特性就是在较低温度(68℃)下发生金属—半导体相变(简称M-S相变)，同时伴随光学性质和电学性质的突变。已有的研究中均以纯含钒原料来制备VO2薄膜，迄今为止,尚未见以工业V2O5为原料制备VO2薄膜的研究报道。在攀钢工业V2O5大量存在且价格较低的条件下，研究以它为原料来制备VO2薄膜，具有重大的现实意义。
本研究得出了如下的研究结果(结论)：
(1)在实验室中打通了以片状工业V2O5晶体为原料、用改进无机溶胶-凝胶法制备V2O5溶胶-凝胶的工艺流程。制备V2O5溶胶的适宜工艺参数为：熔化V2O5的温度(800～900)℃、恒温时间(5～20)min；通过控制工艺参数来控制V2O5溶胶向凝胶的转变。该工艺参数为：溶胶中V2O5浓度须大于20 g/L，同时熔化V2O5的温度(800～900)℃，恒温时间(5～15)min。
(2)选择旋涂法和浸涂法作为日常的涂膜方法，可完全满足涂膜试验的要求。采用旋涂法时，胶体粘度越大、转盘转数越小、衬底越靠近旋转中心，则薄膜厚度越大；采用浸涂法时，胶体粘度越大、密度越小，则薄膜厚度越大，反之则越小。适宜的凝胶粘度为(1.0～3.0) Pa·S。
(3)改制和自制的涂膜装置以及研制的薄膜电阻-温度测量装置，均能满足常规实验要求，预期的效果较好。自制的浸涂法涂膜装置提拉速度为(1.5～3.0)mm/S；温度-电阻测量装置的主要性能指标为：使用温度范围为室温～150℃，温度控制精度为±1℃，升温速度(1～2)℃/min，降温速度约2℃/min，当启用冷却系统时，降温速度为(3～5)℃/min。
(4)用H2还原法和N2热分解法由V2O5薄膜制取VO2薄膜，无论在理论上还是在工艺上都是可行的。在实验室中打通了N2热分解法和H2还原法制备VO2薄膜的工艺流程，在普通玻璃衬底和石英玻璃衬底上制备出了具有显著M-S相变特征的VO2薄膜，并得出了适宜的工艺参数。N2热分解法的适宜工艺参数为：热分解温度450℃，恒温时间(13～20) h，薄膜厚度10.4μm，N2流量1 L/min；H2还原法的适宜工艺参数为：薄膜厚度10.4μm，还原温度400℃，恒温时间(3～5)h，H2流量也
为1 L/min。在同等条件下，采用H2还原法、以石英玻璃作衬底是较好的VO2薄膜制备条件。
(5)由N2热分解法制备VO2薄膜的电阻突变数量级在普通玻璃衬底上最大可达2.2，在石英玻璃衬底上最大可达2.6；由H2还原法制得的VO2薄膜的电阻突变数量级在普通玻璃衬底上最大可达2.6，在石英玻璃衬底上最大可达3.2；VO2薄膜的电阻突变温度约为35℃，接近室温，比纯VO2晶体的理论相变温度(68℃)降低了约33℃。采用上述两种方法制备VO2薄膜的电阻突变数量级总体上达到了国内外用纯含钒原料、在非晶体衬底上VO2薄膜的电阻突变数量级水平。
(6)VO2薄膜的电阻突变温度滞后((TMS)为(1～4)℃。制备方法、衬底材质和S值的大小对(TMS有较大影响。由H2还原法制得VO2薄膜的(TMS比N2热分解法的小；石英玻璃衬底上的(TMS比普通玻璃衬底上的小；S值较大时(TMS较小，反之则较大；在自然放置条件下、短时间内VO2薄膜可经受反复多次的M-S相变，其S值及(TMS几乎没有变化，但随放置时间的延长以及受周围环境气氛的影响而逐渐降低。
(7)杂质可使VO2薄膜的电阻突变温度降低，同时又可使电阻突变数量级减小。单一的离子半径较大的杂质或多元的使晶体中键长总体上伸长的杂质，都可使VO2薄膜的电阻突变温度降低；掺入MoO3时VO2薄膜电阻率突变数量级随掺入量的增大而减小，可用推导出的理论公式来预测MoO3掺入量对VO2薄膜电阻突变数量级的影响；由于杂质总含量较多，以工业V2O5为原料制备VO2薄膜的电阻突变温度、电阻突变数量级分别低于、小于以分析纯V2O5为原料制备VO2薄膜的电阻突变温度和电阻突变数量级。
(8)V2O5薄膜和VO2薄膜都会被自来水、H2SO4溶液和KOH溶液侵蚀，侵蚀形式既有脱落又有溶解。随烘干时间延长，V2O5薄膜的耐蚀时间大幅度延长；H2SO4溶液和KOH溶液的浓度越高，则两种薄膜的耐蚀时间越短，反之则越长；VO2薄膜在三种介质中的侵蚀形式均为溶解，其耐蚀时间随薄膜厚度的增大而延长。
PANGANG(group) company is the most important steel iron vanadium titanium base in our country, rich vanadium titanium magnetite resource are stored and vanadium resource storage are more than 63% of nation in PANXI area. In the past 30 years，PANGANG(group) company have produced plenty of steel material, vanadium slag, V2O5, V2O3, the alloy of vanadium iron and other vanadium product as raw material with vanadium titanium magnetite resource, and make China become a important country on produce vanadium in the world. But synthetical application level of vanadium resource is still lower, the kind of vanadium product is fewer comparatively and their contents of science technology and their rank are still lower in our country. Therefore, study and exploiture of new vanadium product with high content of science and technology for heighten on synthetical application level of vanadium resource further are very necessary and urgent.
The study of function material VO2 thin film have gotten the very attention for it’s a important character, It occur metal-semiconductor phase transformation(M-S phase transformation) under lower temperature(68℃), at the same time, it's optical and electrical character occurs the sudden change. The study in the past for gotten VO2 thin film are all based on pure inclusive vanadium raw material, So far, do not discovered any research reports for gotten VO2 thin film are based on industrial V2O5 as raw material. Under this conditions that PANXI area have rich industrial V2O5 and its price is very cheap, So the study for gotten VO2 thin film are based on industrial V2O5 as raw material will be significant and realistic.
The study results (conclusions) in this paper as following:
(1) In laboratory have established a new technology process for gotten V2O5 sol-gel based on industrial V2O5 crystal as raw material by the reformative inorganic sol-gel method. Suitable technology parameter for gotten V2O5 sol as following: the temperature at melt of V2O5 is (800～900)℃, and the time of keep this temperature is (5～20) min; We can control the transformation from V2O5 sol to V2O5 gel by control the technology process parameter, these technology process parameters as following: the concentration of V2O5 in sol must be larger than 20 g/L, at the same time the temperature at melt of V2O5 is (800～900)℃ and the time of keep this temperature is (5～15)min.
(2) Selected the spinning and dipping as daily method for preparation of film, it can satisfy requirement at experiment for preparation of films completely. By the spinning
way, the viscosity of colloid is more bigger and the revolution number of turntable is more littler and substrate is more nearer to revolving center, then the thickness of thin film is more bigger. By the dipping way, the viscosity of colloid is more bigger and its density is more littler, the thickness of thin film is more bigger. Contrarily, they are more littler. The suitable gel viscosity is (1.0～3.0)Pa?S.
(3)The covers colloid equipment by refit and homemade, the developmental resistance-temperature measure equipment, they are all satisfied to conventional experiment requirement, and anticipative effect is better. The pull speed of covers colloid equipment on dipping way by homemade is (1.5～3.0) mm/S; the major property index of temperature-resistance measurement set as following: applied temperature is from room temperature to 150℃, the control precision of temperature is ±1℃, ascending temperature speed is about (1～2) ℃/ min, degressive temperature speed is 2 ℃/ min, degressive temperature speed is (3～5) ℃/min when start using cooling system.
(4) The methods for gotten VO2 thin films based on V2O5 thin films through the deoxidize process by H2 and the thermal decompose process by N2 are feasible not only in theoretics but also in technology. In the laboratory we have established technology process for preparation of VO2 thin film through the deoxidize process by H2 and the thermal decompose process by N2, VO2 thin films that own notable characteristic on M-
对功能材料VO2薄膜的研究倍受人们的关注。因为它的一个重要特性就是在较低温度(68℃)下发生金属—半导体相变(简称M-S相变)，同时伴随光学性质和电学性质的突变。已有的研究中均以纯含钒原料来制备VO2薄膜，迄今为止,尚未见以工业V2O5为原料制备VO2薄膜的研究报道。在攀钢工业V2O5大量存在且价格较低的条件下，研究以它为原料来制备VO2薄膜，具有重大的现实意义。
本研究得出了如下的研究结果(结论)：
(1)在实验室中打通了以片状工业V2O5晶体为原料、用改进无机溶胶-凝胶法制备V2O5溶胶-凝胶的工艺流程。制备V2O5溶胶的适宜工艺参数为：熔化V2O5的温度(800～900)℃、恒温时间(5～20)min；通过控制工艺参数来控制V2O5溶胶向凝胶的转变。该工艺参数为：溶胶中V2O5浓度须大于20 g/L，同时熔化V2O5的温度(800～900)℃，恒温时间(5～15)min。
(2)选择旋涂法和浸涂法作为日常的涂膜方法，可完全满足涂膜试验的要求。采用旋涂法时，胶体粘度越大、转盘转数越小、衬底越靠近旋转中心，则薄膜厚度越大；采用浸涂法时，胶体粘度越大、密度越小，则薄膜厚度越大，反之则越小。适宜的凝胶粘度为(1.0～3.0) Pa·S。
(3)改制和自制的涂膜装置以及研制的薄膜电阻-温度测量装置，均能满足常规实验要求，预期的效果较好。自制的浸涂法涂膜装置提拉速度为(1.5～3.0)mm/S；温度-电阻测量装置的主要性能指标为：使用温度范围为室温～150℃，温度控制精度为±1℃，升温速度(1～2)℃/min，降温速度约2℃/min，当启用冷却系统时，降温速度为(3～5)℃/min。
(4)用H2还原法和N2热分解法由V2O5薄膜制取VO2薄膜，无论在理论上还是在工艺上都是可行的。在实验室中打通了N2热分解法和H2还原法制备VO2薄膜的工艺流程，在普通玻璃衬底和石英玻璃衬底上制备出了具有显著M-S相变特征的VO2薄膜，并得出了适宜的工艺参数。N2热分解法的适宜工艺参数为：热分解温度450℃，恒温时间(13～20) h，薄膜厚度10.4μm，N2流量1 L/min；H2还原法的适宜工艺参数为：薄膜厚度10.4μm，还原温度400℃，恒温时间(3～5)h，H2流量也
为1 L/min。在同等条件下，采用H2还原法、以石英玻璃作衬底是较好的VO2薄膜制备条件。
(5)由N2热分解法制备VO2薄膜的电阻突变数量级在普通玻璃衬底上最大可达2.2，在石英玻璃衬底上最大可达2.6；由H2还原法制得的VO2薄膜的电阻突变数量级在普通玻璃衬底上最大可达2.6，在石英玻璃衬底上最大可达3.2；VO2薄膜的电阻突变温度约为35℃，接近室温，比纯VO2晶体的理论相变温度(68℃)降低了约33℃。采用上述两种方法制备VO2薄膜的电阻突变数量级总体上达到了国内外用纯含钒原料、在非晶体衬底上VO2薄膜的电阻突变数量级水平。
(6)VO2薄膜的电阻突变温度滞后((TMS)为(1～4)℃。制备方法、衬底材质和S值的大小对(TMS有较大影响。由H2还原法制得VO2薄膜的(TMS比N2热分解法的小；石英玻璃衬底上的(TMS比普通玻璃衬底上的小；S值较大时(TMS较小，反之则较大；在自然放置条件下、短时间内VO2薄膜可经受反复多次的M-S相变，其S值及(TMS几乎没有变化，但随放置时间的延长以及受周围环境气氛的影响而逐渐降低。
(7)杂质可使VO2薄膜的电阻突变温度降低，同时又可使电阻突变数量级减小。单一的离子半径较大的杂质或多元的使晶体中键长总体上伸长的杂质，都可使VO2薄膜的电阻突变温度降低；掺入MoO3时VO2薄膜电阻率突变数量级随掺入量的增大而减小，可用推导出的理论公式来预测MoO3掺入量对VO2薄膜电阻突变数量级的影响；由于杂质总含量较多，以工业V2O5为原料制备VO2薄膜的电阻突变温度、电阻突变数量级分别低于、小于以分析纯V2O5为原料制备VO2薄膜的电阻突变温度和电阻突变数量级。
(8)V2O5薄膜和VO2薄膜都会被自来水、H2SO4溶液和KOH溶液侵蚀，侵蚀形式既有脱落又有溶解。随烘干时间延长，V2O5薄膜的耐蚀时间大幅度延长；H2SO4溶液和KOH溶液的浓度越高，则两种薄膜的耐蚀时间越短，反之则越长；VO2薄膜在三种介质中的侵蚀形式均为溶解，其耐蚀时间随薄膜厚度的增大而延长。
PANGANG(group) company is the most important steel iron vanadium titanium base in our country, rich vanadium titanium magnetite resource are stored and vanadium resource storage are more than 63% of nation in PANXI area. In the past 30 years，PANGANG(group) company have produced plenty of steel material, vanadium slag, V2O5, V2O3, the alloy of vanadium iron and other vanadium product as raw material with vanadium titanium magnetite resource, and make China become a important country on produce vanadium in the world. But synthetical application level of vanadium resource is still lower, the kind of vanadium product is fewer comparatively and their contents of science technology and their rank are still lower in our country. Therefore, study and exploiture of new vanadium product with high content of science and technology for heighten on synthetical application level of vanadium resource further are very necessary and urgent.
The study of function material VO2 thin film have gotten the very attention for it’s a important character, It occur metal-semiconductor phase transformation(M-S phase transformation) under lower temperature(68℃), at the same time, it's optical and electrical character occurs the sudden change. The study in the past for gotten VO2 thin film are all based on pure inclusive vanadium raw material, So far, do not discovered any research reports for gotten VO2 thin film are based on industrial V2O5 as raw material. Under this conditions that PANXI area have rich industrial V2O5 and its price is very cheap, So the study for gotten VO2 thin film are based on industrial V2O5 as raw material will be significant and realistic.
The study results (conclusions) in this paper as following:
(1) In laboratory have established a new technology process for gotten V2O5 sol-gel based on industrial V2O5 crystal as raw material by the reformative inorganic sol-gel method. Suitable technology parameter for gotten V2O5 sol as following: the temperature at melt of V2O5 is (800～900)℃, and the time of keep this temperature is (5～20) min; We can control the transformation from V2O5 sol to V2O5 gel by control the technology process parameter, these technology process parameters as following: the concentration of V2O5 in sol must be larger than 20 g/L, at the same time the temperature at melt of V2O5 is (800～900)℃ and the time of keep this temperature is (5～15)min.
(2) Selected the spinning and dipping as daily method for preparation of film, it can satisfy requirement at experiment for preparation of films completely. By the spinning
way, the viscosity of colloid is more bigger and the revolution number of turntable is more littler and substrate is more nearer to revolving center, then the thickness of thin film is more bigger. By the dipping way, the viscosity of colloid is more bigger and its density is more littler, the thickness of thin film is more bigger. Contrarily, they are more littler. The suitable gel viscosity is (1.0～3.0)Pa?S.
(3)The covers colloid equipment by refit and homemade, the developmental resistance-temperature measure equipment, they are all satisfied to conventional experiment requirement, and anticipative effect is better. The pull speed of covers colloid equipment on dipping way by homemade is (1.5～3.0) mm/S; the major property index of temperature-resistance measurement set as following: applied temperature is from room temperature to 150℃, the control precision of temperature is ±1℃, ascending temperature speed is about (1～2) ℃/ min, degressive temperature speed is 2 ℃/ min, degressive temperature speed is (3～5) ℃/min when start using cooling system.
(4) The methods for gotten VO2 thin films based on V2O5 thin films through the deoxidize process by H2 and the thermal decompose process by N2 are feasible not only in theoretics but also in technology. In the laboratory we have established technology process for preparation of VO2 thin film through the deoxidize process by H2 and the thermal decompose process by N2, VO2 thin films that own notable characteristic on M-
引文
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