Cu_2O-Cu金属陶瓷制备及组织性能研究
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摘要
本文以铝电解用惰性阳极材料为主要应用背景,提出了新的Cu_2O-Cu金属陶瓷材料体系,设计和制备了含有不同形貌和尺寸Cu颗粒的Cu_2O-Cu金属陶瓷。利用X射线衍射仪(XRD)、光学显微镜(OM)和扫描电镜(SEM)等手段分析和观察了Cu_2O-Cu金属陶瓷及其腐蚀产物的相组成和微观组织特征。利用电子万能材料试验机、热膨胀分析仪、热导率测试仪和电导率测试仪等设备测试了Cu_2O-Cu金属陶瓷的力学性能和物理性能,采用热腐蚀方法考察了Cu_2O-Cu金属陶瓷在铝电解熔盐中的耐腐蚀性能,系统地研究了Cu含量、颗粒形貌及尺寸对Cu_2O-Cu金属陶瓷宏观性能的影响规律,并分析了其影响机理,为惰性阳极材料以及双相复合材料的研究提供了一定的理论依据。
研究表明,通过选择合理的工艺参数可以获得所设计的Cu_2O-Cu金属陶瓷。金属陶瓷中的真实Cu含量与名义Cu含量一致,枝状Cu粉制备的ZR体系试样中Cu颗粒为具有较大长宽比和形状因子的蠕虫状形貌。球形Cu粉制备的QR200、QR300和QR400体系试样中的Cu颗粒基本为球形形貌。在不同体系试样中,Cu_2O晶粒基本都呈等轴状,其晶粒尺寸受引入基体中的Cu含量及颗粒尺寸影响。
Cu_2O-Cu金属陶瓷的弹性模量、强度和韧性均随着材料中Cu含量的增加而增大。在相同Cu含量条件下,Cu颗粒的形状因子越大、尺寸越小,金属陶瓷的弹性模量越高且强韧化效果越好。Cu_2O-Cu金属陶瓷热震后的剩余弯曲强度随热震温差的增大呈现先下降后增加的趋势。在相同温差热震后的试样剩余弯曲强度随着材料中Cu含量的增加而增大。在Cu含量相同条件下,Cu颗粒的形状因子越大、尺寸越小,试样热震后的剩余弯曲强度越高。
Cu_2O-Cu金属陶瓷的电导率随着Cu含量的增加呈现典型的渗流导电行为,其变化规律可用有效介质普适方程(GEM方程)来描述,发生渗流导通后,试样的电导率可达到10~4~10~6Ω~(-1)·m~(-1)数量级。Cu颗粒形貌对材料渗流阈值的影响较大,高形状因子的Cu颗粒可以使试样在较低Cu含量下形成渗流导通结构;Cu颗粒尺寸对材料渗流阈值的影响不大,材料的导通渗流阈值随着Cu颗粒尺寸的减小而略有降低。Cu_2O-Cu金属陶瓷在不同Cu含量下对应不同的导电机制。
Cu_2O-Cu金属陶瓷的热膨胀系数随着温度的升高而增大,其变化过程与材料中的热应力状态和释放机理密切相关。在相同温度条件下,Cu含量越高、颗粒形状因子越大,金属陶瓷的热膨胀系数越大。Cu颗粒尺寸对试样热膨胀系数的影响与Cu含量有关。
Cu含量和颗粒形貌对Cu_2O-Cu金属陶瓷的热导率影响显著。材料中Cu含量越高、颗粒形状因子越大,金属陶瓷的热导率越高。Cu颗粒尺寸对试样热导率的影响程度取决于材料中的Cu含量,当Cu含量较低时,颗粒尺寸对金属陶瓷的热导率影响较小,而当Cu含量较高时,小尺寸Cu颗粒可以使金属陶瓷获得较高的热导率。
在铝电解熔盐腐蚀过程中,Cu_2O-Cu金属陶瓷在表面形成CuAlO_2保护层,从而降低了其腐蚀速率。材料中Cu含量越高、颗粒形状因子越大、尺寸越小,金属陶瓷的腐蚀速率越大。Cu_2O-Cu金属陶瓷在熔盐中的腐蚀机理主要为金属陶瓷组分的溶解、Cu_2O与Al_2O_3的化学反应以及金属Cu的物理迁移。
A new Cu_2O-Cu cermet material with different Cu shape and size was prepared as candidate inert anode material for Al production. The microstructure of the cermet and the products after corrosion tests were observed and analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM) and optical microscope (OM). Mechanical properties, thermal expansion coefficient, thermal conductivity and electrical conductivity of the cermets were tested. The corrosion rate of the cermets in electrolyte (Na3AlF6) was measured as well. The relationship between the properties of the cermet and the Cu content, shape and size was investigated, and the mechanisms of these relationships were demonstrated.
The results show that the Cu_2O-Cu cermet with branched Cu (ZR) and spherical Cu (QR) could be obtained with processing parameter controlling, and the real Cu content was well agree with the calculated Cu content. The Cu structure in Cu_2O-Cu cermet prepared with branched Cu is worm like, and the one prepared with spherical Cu (QR200, QR300, QR400) is basically spherical shape. In all Cu_2O-Cu cermet, the crystals of the Cu_2O matrix are isometric, and the size of them is affected by the Cu content and size.
The elastic modulus, strength and toughness of the Cu_2O-Cu cermet increase with increasing Cu content. With same Cu content, the elastic modulus and toughness increase with increasing shape factor and decreasing size of the Cu phase. The thermal shock resistance property of the Cu_2O-Cu cermet has a fluctuation phenomenon with increasing of thermal shock temperature difference. The thermal shock resistance property increases with increasing of Cu content. The remaining flexural strength after thermal shock increases with increasing aspect ratio and decreasing size of the Cu phase.
The results of the electrical conductivity tests show the typical percolation phenomenon, and the regularity of it can be described by using GEM (General Effective Method) equation. After the percolation, the electrical conductivity was about 10~4~10~6Ω~(-1)·m~(-1). The percolation threshold is largely influenced by the shape factor of the conductors. The Cu_2O-Cu cermet prepared with branched Cu has a lower percolation threshold than the one prepared with spherical Cu. The conductive mechanism of the Cu_2O-Cu cermet is different with different Cu content.
The thermal expansion coefficient of the Cu_2O-Cu cermet increases with increasing temperature. The variation process is largely influenced by the internal thermal stress state and release mechanisms. Under the same temperature, the thermal expansion coefficient increases with increasing Cu content and aspect ratio of Cu phase. The size effect is affected by the Cu content.
The thermal conductivity of the Cu_2O-Cu cermet is largely influenced by Cu content and Cu shape. The thermal conductivity increases with increasing of Cu content and aspect ratio of Cu phase. The size effect is affected by the Cu content. The size effect with lower Cu content is smaller than the one with higher Cu content.
During the corrosion tests, there is a CuAlO_2 layer formed and protected the Cu_2O-Cu cermet. This protective layer decreases the corrosion rate. The corrosion rate increases with increasing content, aspect ratio, and decreasing size of the Cu phase. The corrosion mechanism of Cu_2O-Cu cermet in the electrolyte is mainly resulted from the dissolve of the cermet, the chemical reaction of Cu_2O and Al_2O_3, and the physical migration of Cu.
研究表明,通过选择合理的工艺参数可以获得所设计的Cu_2O-Cu金属陶瓷。金属陶瓷中的真实Cu含量与名义Cu含量一致,枝状Cu粉制备的ZR体系试样中Cu颗粒为具有较大长宽比和形状因子的蠕虫状形貌。球形Cu粉制备的QR200、QR300和QR400体系试样中的Cu颗粒基本为球形形貌。在不同体系试样中,Cu_2O晶粒基本都呈等轴状,其晶粒尺寸受引入基体中的Cu含量及颗粒尺寸影响。
Cu_2O-Cu金属陶瓷的弹性模量、强度和韧性均随着材料中Cu含量的增加而增大。在相同Cu含量条件下,Cu颗粒的形状因子越大、尺寸越小,金属陶瓷的弹性模量越高且强韧化效果越好。Cu_2O-Cu金属陶瓷热震后的剩余弯曲强度随热震温差的增大呈现先下降后增加的趋势。在相同温差热震后的试样剩余弯曲强度随着材料中Cu含量的增加而增大。在Cu含量相同条件下,Cu颗粒的形状因子越大、尺寸越小,试样热震后的剩余弯曲强度越高。
Cu_2O-Cu金属陶瓷的电导率随着Cu含量的增加呈现典型的渗流导电行为,其变化规律可用有效介质普适方程(GEM方程)来描述,发生渗流导通后,试样的电导率可达到10~4~10~6Ω~(-1)·m~(-1)数量级。Cu颗粒形貌对材料渗流阈值的影响较大,高形状因子的Cu颗粒可以使试样在较低Cu含量下形成渗流导通结构;Cu颗粒尺寸对材料渗流阈值的影响不大,材料的导通渗流阈值随着Cu颗粒尺寸的减小而略有降低。Cu_2O-Cu金属陶瓷在不同Cu含量下对应不同的导电机制。
Cu_2O-Cu金属陶瓷的热膨胀系数随着温度的升高而增大,其变化过程与材料中的热应力状态和释放机理密切相关。在相同温度条件下,Cu含量越高、颗粒形状因子越大,金属陶瓷的热膨胀系数越大。Cu颗粒尺寸对试样热膨胀系数的影响与Cu含量有关。
Cu含量和颗粒形貌对Cu_2O-Cu金属陶瓷的热导率影响显著。材料中Cu含量越高、颗粒形状因子越大,金属陶瓷的热导率越高。Cu颗粒尺寸对试样热导率的影响程度取决于材料中的Cu含量,当Cu含量较低时,颗粒尺寸对金属陶瓷的热导率影响较小,而当Cu含量较高时,小尺寸Cu颗粒可以使金属陶瓷获得较高的热导率。
在铝电解熔盐腐蚀过程中,Cu_2O-Cu金属陶瓷在表面形成CuAlO_2保护层,从而降低了其腐蚀速率。材料中Cu含量越高、颗粒形状因子越大、尺寸越小,金属陶瓷的腐蚀速率越大。Cu_2O-Cu金属陶瓷在熔盐中的腐蚀机理主要为金属陶瓷组分的溶解、Cu_2O与Al_2O_3的化学反应以及金属Cu的物理迁移。
A new Cu_2O-Cu cermet material with different Cu shape and size was prepared as candidate inert anode material for Al production. The microstructure of the cermet and the products after corrosion tests were observed and analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM) and optical microscope (OM). Mechanical properties, thermal expansion coefficient, thermal conductivity and electrical conductivity of the cermets were tested. The corrosion rate of the cermets in electrolyte (Na3AlF6) was measured as well. The relationship between the properties of the cermet and the Cu content, shape and size was investigated, and the mechanisms of these relationships were demonstrated.
The results show that the Cu_2O-Cu cermet with branched Cu (ZR) and spherical Cu (QR) could be obtained with processing parameter controlling, and the real Cu content was well agree with the calculated Cu content. The Cu structure in Cu_2O-Cu cermet prepared with branched Cu is worm like, and the one prepared with spherical Cu (QR200, QR300, QR400) is basically spherical shape. In all Cu_2O-Cu cermet, the crystals of the Cu_2O matrix are isometric, and the size of them is affected by the Cu content and size.
The elastic modulus, strength and toughness of the Cu_2O-Cu cermet increase with increasing Cu content. With same Cu content, the elastic modulus and toughness increase with increasing shape factor and decreasing size of the Cu phase. The thermal shock resistance property of the Cu_2O-Cu cermet has a fluctuation phenomenon with increasing of thermal shock temperature difference. The thermal shock resistance property increases with increasing of Cu content. The remaining flexural strength after thermal shock increases with increasing aspect ratio and decreasing size of the Cu phase.
The results of the electrical conductivity tests show the typical percolation phenomenon, and the regularity of it can be described by using GEM (General Effective Method) equation. After the percolation, the electrical conductivity was about 10~4~10~6Ω~(-1)·m~(-1). The percolation threshold is largely influenced by the shape factor of the conductors. The Cu_2O-Cu cermet prepared with branched Cu has a lower percolation threshold than the one prepared with spherical Cu. The conductive mechanism of the Cu_2O-Cu cermet is different with different Cu content.
The thermal expansion coefficient of the Cu_2O-Cu cermet increases with increasing temperature. The variation process is largely influenced by the internal thermal stress state and release mechanisms. Under the same temperature, the thermal expansion coefficient increases with increasing Cu content and aspect ratio of Cu phase. The size effect is affected by the Cu content.
The thermal conductivity of the Cu_2O-Cu cermet is largely influenced by Cu content and Cu shape. The thermal conductivity increases with increasing of Cu content and aspect ratio of Cu phase. The size effect is affected by the Cu content. The size effect with lower Cu content is smaller than the one with higher Cu content.
During the corrosion tests, there is a CuAlO_2 layer formed and protected the Cu_2O-Cu cermet. This protective layer decreases the corrosion rate. The corrosion rate increases with increasing content, aspect ratio, and decreasing size of the Cu phase. The corrosion mechanism of Cu_2O-Cu cermet in the electrolyte is mainly resulted from the dissolve of the cermet, the chemical reaction of Cu_2O and Al_2O_3, and the physical migration of Cu.
引文
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