Cu-Ti_3SiC_2复合材料的电弧侵蚀行为研究
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摘要
三元化合物Ti3SiC2，是MAX家族中获得最多关注的一种陶瓷材料。由于它具有多种优异性能，近年来吸引着大量的科研人员对其进行研究。Ti3SiC2具有比金属Ti更高的导电率和导热率，具有抗高温氧化性能，此外还具备较高的高温强度、热稳定性、抗热震性能以及较好的可加工性等特性。Ti3SiC2陶瓷具备的这些特点使其满足作为电接触材料的基本要求，目前国外已经有用Ti3SiC2薄膜作为SiC半导体器件间电接触材料的报道。本实验制备了以Ti3SiC2作为增强体的Cu基复合材料，并研究了它的真空电弧侵蚀机理。
本研究通过X射线衍射(XRD)，扫描电子显微镜(SEM)，能谱分析(EDX)，和微区拉曼光谱等方法，对高纯Ti3SiC2的真空电弧侵蚀机理进行研究。结果发现，由于真空电弧的高能量和高温度，Ti3SiC2在受到真空电弧影响时并不稳定，阴极表面的Ti3SiC2会发生分解生成TiCx，TiCx喷溅到阳极表面而Si则挥发到真空中。同时，微区拉曼光谱测试到少量的C，因此，可以认为C也应该作为该分解过程的副产物出现，在本研究中没有检测出是因为Si以蒸气的形式挥发到真空中。实验还研究了Ti3SiC2阳极的真空电弧侵蚀，微区拉曼光谱检测到作为阳极的Ti3SiC2分解成TiCx、非晶态C和其它副产品。用SEM和3D超景深数码显微镜观察了阳极表面形貌，发现阳极蚀坑尺寸从几微米到几百微米不等。其中较小的蚀坑呈现花瓣形状，有圆形突起物存在于蚀坑的底部。较大的蚀坑的直径大于100μm，但是蚀坑的底部中央不存在突起物，蚀坑的周围被裂纹和塌陷包围。
Cu-Ti3SiC2复合材料阴极被电弧侵蚀后，部分被侵蚀的Ti3SiC2被证实转变为TiCx，微观组织分析发现Ti3SiC2比Cu更容易被电弧侵蚀。由于真空电弧的极端高温，在Cu-Ti3SiC2阴极剖切面将由于Cu和Ti3SiC2相互反应而出现新相。实验还发现，随着燃弧次数增加，Cu-Ti3SiC2复合材料中的Ti元素和Si元素会逐渐消耗。受高温电弧的影响，Cu和Ti3SiC2相互反应不仅出现在阴极，还会出现在低电流情况下相对不活泼的阳极。一次燃弧过后，Ti3SiC2含量越高的Cu-Ti3SiC2阴极样品，其表面越粗糙，同时还发现，Ti3SiC2含量越高的样品质量损失速率也越大，其中Ti3SiC2质量分数为25wt.%的Cu-Ti3SiC2样品的质量损失速率为纯铜的两倍。
由于在电弧作用下Ti3SiC2会分解出TiC，而WC陶瓷有应用于电触头材料的实例，为了和Ti3SiC2相比较，本研究也对WC和TiC的真空电弧侵蚀行为进行研究。在一次燃弧的TiC阴极表面发现很多微裂纹，而50次燃弧过后，TiC阴极表面会崩裂成许多小碎片，对其断面进行观察发现脆性穿晶断裂是主要的断裂方式。实验还证明了受电弧侵蚀后阴极的TiC也会发生分解，在TiC对面的阳极上发现沉积着非晶态碳。一次燃弧的WC阴极表面只出现一些微裂纹，经过多次真空电弧侵蚀后(100次)，裂纹才变宽。在电弧作用下WC也会分解，生成非晶态碳，但实验证明WC要比TiC稳定得多。在WC和TiC阳极表面分别观察到阳极蚀坑，TiC阳极上的蚀坑被Cu颗粒包围着，在蚀坑的中心检测到单质C的存在，因此可以断定TiC发生了分解。随着燃弧次数的增加，WC阳极上的蚀坑变大变深，经15次燃弧后WC阳极覆盖着一层Cu。WC和TiC阳极表面蚀坑形貌的差异可归因于两种陶瓷材料的不同特性。
本文研究了Cu-WC和Cu-TiC复合材料的电弧侵蚀机理。相比于Cu，TiC在真空击穿过程中更容易受电弧侵蚀，一次燃弧后，TiC含量高的Cu-TiC阴极样品表面更粗糙。由于具有较高的熔点，WC的熔融过程将吸收大量的能量，未熔融的WC也可以有效降低阴极表面的喷溅并阻止熔池进一步扩大。相比Ti3SiC2和TiC，WC的耐电弧侵蚀性能更好。
The ternary compound Ti3SiC2is the most studied member of the MAX phasefamily. In the recent years, it has triggered intense research efforts due to its uniqueproperties. It has higher electrical and thermal conductivity than those of titaniummetal, and has high-temperature-oxidation resistance. Ti3SiC2also exhibits excellentproperties such as high strength at high temperatures, high thermal stability,high-thermal shock resistance, good machinability, etc. Its overall properties satisfy thebasic requirements of electrical contact materials. It has been declared that Ti3SiC2film has the possibility to be used as an electrical contact for silicon carbide devices. Inthis paper, the vacuum arc erosion characteristics of Ti3SiC2particles reinforcedCu-matrix composites were investigated.
The arc erosion behavior of high-purity Ti3SiC2in vacuum was investigated byX-ray diffraction (XRD), scanning electron microscope (SEM), Energy DispersiveX-Ray Spectroscopy (EDX), and micro-Raman Spectroscopy. From the resultsobtained, Ti3SiC2is unstable due to the high energy intensity and high temperature ofthe vacuum arc. The dissociation of Ti3SiC2takes place at the sample surface, resultingin the formation of solid TiCxand gaseous Si. TiCxis ejected from cathode to thesurface of anode while Si is evaporated to the vacuum chamber. The micro-Ramanresults reveal that, small amounts of carbon appeared as a by-product of thedissociation. The decomposition of Ti3SiC2into non-stoichiometric TiCx, amorphouscarbon and other by-products was detected on the anode surface. The surfacemorphology was revealed by scanning electron microscope and3D super depth digitalmicroscope. Different kinds of anode craters with diameters varying from a fewmicrons to a few hundred microns were observed on the anode surface. The smallercraters are flower-like shaped with a sphoiroidal protrusion pointing out from thecenter of the crater bottom. The larger craters have a diameters greater than onehundred microns but without the central protrusion and the crater is surrounded bycollapse-fissure.
The Ti3SiC2particles on the Cu-Ti3SiC2cathode surface are also proved to produce TiCxunder the impact of the vacuum arc. Ti3SiC2is more prone to be erodedthan Cu matrix in the vacuum breakdown process. Different reaction phases will beformed on the the cross section of Cu-Ti3SiC2cathode, due to the extreme temperatureof the vacuum arc. It seems that Ti element and Si element have the tendency to bedepleted after long period of vacuum breakdown test. The reactions between Cu andTi3SiC2could be detected on the surface of a Cu-Ti3SiC2cathode after the vacuumbreakdown. Even on the inert Cu-Ti3SiC2anode, the temperature is so high thatmaking the reaction between Cu and Ti3SiC2possible. It is also found that, after thefirst vacuum breakdown, the Cu-Ti3SiC2sample with a higher content of Ti3SiC2obtained a rougher surface. At the meantime, the cathode erosion rate of Cu-Ti3SiC2composites is found increasing with the increase of Ti3SiC2content. The cathodeerosion rate of sample CuTSC25is twice that of pure Cu.
The arc erosion behavior of WC and TiC in vacuum were investigated forcomparison. Cracks were found on the surface of a TiC cathode after the firstbreakdown. The TiC cathode is crushed after exposed to50arcings. Inspection of themicrograph reveals that brittle intergranular fracture is the dominant mode of failure.The deposition of amorphous carbon on the Mo anode indicated that the decompositionof TiC on its counterpart TiC cathode. Some microcracks were also found on thesurface of WC cathode after the first breakdown. Bigger cracks appear on the surfaceof WC cathode under100arcings, indicating that it is ceramic in nature. Amorphouscarbon is also proven to be one of the decomposition products of WC. However, WC isproven to be much stable than TiC under the impact of the vacuum arc.
The arc erosion characteristics of WC and TiC particles reinforced Cu-matrixcomposites were investigated. TiC is more prone to be eroded than Cu matrix duringthe vacuum breakdown process. After the first vacuum breakdown, the Cu-TiC samplewith a higher content of TiC obtained a rougher surface. Due to the addition of brittleTiC, Cu-TiC composite may exhibit good anti-welding capability. The melting of WCin Cu-WC composite can absorb a great deal of energy due to its high melts point. Theunmelted WC particles can alleviate sputtering on the cathode surface, and restrain theerosion pools from further expansion. WC is much stable than Ti3SiC2and TiC under influence of the vacuum arc.
Anode craters were observed on the surface of TiC and WC anode, respectively.The anode crater on TiC anode is surrounding by Cu particles and the anode crater onWC is covered by Cu depositions. These differences in appearance maybe come fromthe different characters of TiC and WC.
本研究通过X射线衍射(XRD)，扫描电子显微镜(SEM)，能谱分析(EDX)，和微区拉曼光谱等方法，对高纯Ti3SiC2的真空电弧侵蚀机理进行研究。结果发现，由于真空电弧的高能量和高温度，Ti3SiC2在受到真空电弧影响时并不稳定，阴极表面的Ti3SiC2会发生分解生成TiCx，TiCx喷溅到阳极表面而Si则挥发到真空中。同时，微区拉曼光谱测试到少量的C，因此，可以认为C也应该作为该分解过程的副产物出现，在本研究中没有检测出是因为Si以蒸气的形式挥发到真空中。实验还研究了Ti3SiC2阳极的真空电弧侵蚀，微区拉曼光谱检测到作为阳极的Ti3SiC2分解成TiCx、非晶态C和其它副产品。用SEM和3D超景深数码显微镜观察了阳极表面形貌，发现阳极蚀坑尺寸从几微米到几百微米不等。其中较小的蚀坑呈现花瓣形状，有圆形突起物存在于蚀坑的底部。较大的蚀坑的直径大于100μm，但是蚀坑的底部中央不存在突起物，蚀坑的周围被裂纹和塌陷包围。
Cu-Ti3SiC2复合材料阴极被电弧侵蚀后，部分被侵蚀的Ti3SiC2被证实转变为TiCx，微观组织分析发现Ti3SiC2比Cu更容易被电弧侵蚀。由于真空电弧的极端高温，在Cu-Ti3SiC2阴极剖切面将由于Cu和Ti3SiC2相互反应而出现新相。实验还发现，随着燃弧次数增加，Cu-Ti3SiC2复合材料中的Ti元素和Si元素会逐渐消耗。受高温电弧的影响，Cu和Ti3SiC2相互反应不仅出现在阴极，还会出现在低电流情况下相对不活泼的阳极。一次燃弧过后，Ti3SiC2含量越高的Cu-Ti3SiC2阴极样品，其表面越粗糙，同时还发现，Ti3SiC2含量越高的样品质量损失速率也越大，其中Ti3SiC2质量分数为25wt.%的Cu-Ti3SiC2样品的质量损失速率为纯铜的两倍。
由于在电弧作用下Ti3SiC2会分解出TiC，而WC陶瓷有应用于电触头材料的实例，为了和Ti3SiC2相比较，本研究也对WC和TiC的真空电弧侵蚀行为进行研究。在一次燃弧的TiC阴极表面发现很多微裂纹，而50次燃弧过后，TiC阴极表面会崩裂成许多小碎片，对其断面进行观察发现脆性穿晶断裂是主要的断裂方式。实验还证明了受电弧侵蚀后阴极的TiC也会发生分解，在TiC对面的阳极上发现沉积着非晶态碳。一次燃弧的WC阴极表面只出现一些微裂纹，经过多次真空电弧侵蚀后(100次)，裂纹才变宽。在电弧作用下WC也会分解，生成非晶态碳，但实验证明WC要比TiC稳定得多。在WC和TiC阳极表面分别观察到阳极蚀坑，TiC阳极上的蚀坑被Cu颗粒包围着，在蚀坑的中心检测到单质C的存在，因此可以断定TiC发生了分解。随着燃弧次数的增加，WC阳极上的蚀坑变大变深，经15次燃弧后WC阳极覆盖着一层Cu。WC和TiC阳极表面蚀坑形貌的差异可归因于两种陶瓷材料的不同特性。
本文研究了Cu-WC和Cu-TiC复合材料的电弧侵蚀机理。相比于Cu，TiC在真空击穿过程中更容易受电弧侵蚀，一次燃弧后，TiC含量高的Cu-TiC阴极样品表面更粗糙。由于具有较高的熔点，WC的熔融过程将吸收大量的能量，未熔融的WC也可以有效降低阴极表面的喷溅并阻止熔池进一步扩大。相比Ti3SiC2和TiC，WC的耐电弧侵蚀性能更好。
The ternary compound Ti3SiC2is the most studied member of the MAX phasefamily. In the recent years, it has triggered intense research efforts due to its uniqueproperties. It has higher electrical and thermal conductivity than those of titaniummetal, and has high-temperature-oxidation resistance. Ti3SiC2also exhibits excellentproperties such as high strength at high temperatures, high thermal stability,high-thermal shock resistance, good machinability, etc. Its overall properties satisfy thebasic requirements of electrical contact materials. It has been declared that Ti3SiC2film has the possibility to be used as an electrical contact for silicon carbide devices. Inthis paper, the vacuum arc erosion characteristics of Ti3SiC2particles reinforcedCu-matrix composites were investigated.
The arc erosion behavior of high-purity Ti3SiC2in vacuum was investigated byX-ray diffraction (XRD), scanning electron microscope (SEM), Energy DispersiveX-Ray Spectroscopy (EDX), and micro-Raman Spectroscopy. From the resultsobtained, Ti3SiC2is unstable due to the high energy intensity and high temperature ofthe vacuum arc. The dissociation of Ti3SiC2takes place at the sample surface, resultingin the formation of solid TiCxand gaseous Si. TiCxis ejected from cathode to thesurface of anode while Si is evaporated to the vacuum chamber. The micro-Ramanresults reveal that, small amounts of carbon appeared as a by-product of thedissociation. The decomposition of Ti3SiC2into non-stoichiometric TiCx, amorphouscarbon and other by-products was detected on the anode surface. The surfacemorphology was revealed by scanning electron microscope and3D super depth digitalmicroscope. Different kinds of anode craters with diameters varying from a fewmicrons to a few hundred microns were observed on the anode surface. The smallercraters are flower-like shaped with a sphoiroidal protrusion pointing out from thecenter of the crater bottom. The larger craters have a diameters greater than onehundred microns but without the central protrusion and the crater is surrounded bycollapse-fissure.
The Ti3SiC2particles on the Cu-Ti3SiC2cathode surface are also proved to produce TiCxunder the impact of the vacuum arc. Ti3SiC2is more prone to be erodedthan Cu matrix in the vacuum breakdown process. Different reaction phases will beformed on the the cross section of Cu-Ti3SiC2cathode, due to the extreme temperatureof the vacuum arc. It seems that Ti element and Si element have the tendency to bedepleted after long period of vacuum breakdown test. The reactions between Cu andTi3SiC2could be detected on the surface of a Cu-Ti3SiC2cathode after the vacuumbreakdown. Even on the inert Cu-Ti3SiC2anode, the temperature is so high thatmaking the reaction between Cu and Ti3SiC2possible. It is also found that, after thefirst vacuum breakdown, the Cu-Ti3SiC2sample with a higher content of Ti3SiC2obtained a rougher surface. At the meantime, the cathode erosion rate of Cu-Ti3SiC2composites is found increasing with the increase of Ti3SiC2content. The cathodeerosion rate of sample CuTSC25is twice that of pure Cu.
The arc erosion behavior of WC and TiC in vacuum were investigated forcomparison. Cracks were found on the surface of a TiC cathode after the firstbreakdown. The TiC cathode is crushed after exposed to50arcings. Inspection of themicrograph reveals that brittle intergranular fracture is the dominant mode of failure.The deposition of amorphous carbon on the Mo anode indicated that the decompositionof TiC on its counterpart TiC cathode. Some microcracks were also found on thesurface of WC cathode after the first breakdown. Bigger cracks appear on the surfaceof WC cathode under100arcings, indicating that it is ceramic in nature. Amorphouscarbon is also proven to be one of the decomposition products of WC. However, WC isproven to be much stable than TiC under the impact of the vacuum arc.
The arc erosion characteristics of WC and TiC particles reinforced Cu-matrixcomposites were investigated. TiC is more prone to be eroded than Cu matrix duringthe vacuum breakdown process. After the first vacuum breakdown, the Cu-TiC samplewith a higher content of TiC obtained a rougher surface. Due to the addition of brittleTiC, Cu-TiC composite may exhibit good anti-welding capability. The melting of WCin Cu-WC composite can absorb a great deal of energy due to its high melts point. Theunmelted WC particles can alleviate sputtering on the cathode surface, and restrain theerosion pools from further expansion. WC is much stable than Ti3SiC2and TiC under influence of the vacuum arc.
Anode craters were observed on the surface of TiC and WC anode, respectively.The anode crater on TiC anode is surrounding by Cu particles and the anode crater onWC is covered by Cu depositions. These differences in appearance maybe come fromthe different characters of TiC and WC.
引文
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