常压等离子体还原氧化铜工艺的研究
发布时间：2019-01-14 09:41
【摘要】：射流型常压等离子体还原方法由于其具有清洁、高效、设备简单和对材料性能影响小等一系列优点,被广泛用于高分子、金属、半导体、PCB电路板等的表面处理。该技术用于电路板,可以解决铜板使用前必须去除氧化皮的问题。将该技术代替电镀前的活化处理,既高效又环保。常压等离子还原技术还可以用于陶瓷与金属的连接。但是用于还原过程的射流型等离子体,其气体介质通常采用氢气,氢气在运输、贮存和使用过程中存在许多安全隐患,同时对于等离子体还原的机理研究较少。因此本文旨在寻找一种能够代替氢气的气体作为等离子体发生气,利用扫描电镜(SEM)、能谱仪(EDS)、X射线衍射仪(XRD)等手段研究了气体介质和工艺参数对常压等离子体还原CuO的微观形貌、相组成和元素分布的影响,讨论了各参数的作用规律,优化还原工艺,并结合检测结果分析了等离子体还原的机制,为等离子还原技术的其他应用提供理论指导和技术支持。分别以N_2、N_2~+冷NH_3和N_2~+热分解NH3作为等离子体发生气,结合等离子体的产生原理、三种气体介质中的活性物种及物相检测结果推出三种气体介质的还原性强弱顺序为:N2+热分解NH_3N_2+冷NH_3N_2。等离子体还原时间对CuO还原有重要影响:随着还原时间延长还原产物Cu的相对含量先增加后减少,70s时的含量最高,为34.38%;试样表面的颜色随还原时间发生明显变化,由黑色转变为灰色,然后变成砖红色、橘红色,这是还原产物发生变化引起的;随还原时间的增加,试样表面的颗粒熔融现象加剧,伴随着颗粒团聚现象。随着设备输出功率增大,试样表面的还原产物Cu的相对含量先增加后减少,而中间相Cu2O的含量则逐渐增加;当输出功率较小时,试样表面呈现棕红色,随着功率增大,试样表面的红色变深。输出功率过大会导致还原产物重新被氧化;在功率增大过程中,试样表面的颗粒熔融聚集,冷却时表面留下细小孔洞,新相从聚集体表面形成然后表面被融化。在等离子体还原过程中,存在还原反应和氧化反应相互竞争的行为。反应时活性粒子在试样表面发生碰撞、溅射,将能量转移给氧化物粒子使其能量高于反应活化能促使还原反应发生。
[Abstract]:Due to its many advantages such as cleanliness, high efficiency, simple equipment and little influence on material properties, jet plasma reduction method has been widely used in surface treatment of polymer, metal, semiconductor, PCB circuit board and so on. This technology can be used in circuit board to solve the problem of removing oxide coating before copper plate is used. The technology is effective and environmentally friendly instead of the activation treatment before electroplating. Atmospheric pressure plasma reduction technology can also be used for ceramic and metal connection. However, there are many safety risks in the gas medium of jet plasma, which is used in the process of reduction, such as transportation, storage and use of hydrogen. At the same time, there are few researches on the mechanism of plasma reduction. Therefore, the purpose of this paper is to find a kind of gas that can replace hydrogen as plasma gas, and use scanning electron microscope (SEM) (SEM), energy spectrometer (EDS),). The effects of gas medium and process parameters on the micromorphology, phase composition and element distribution of CuO reduction by atmospheric pressure plasma were studied by means of X-ray diffractometer (XRD), and the action law of each parameter was discussed, and the reduction process was optimized. The mechanism of plasma reduction is analyzed based on the test results, which provides theoretical guidance and technical support for other applications of plasma reduction technology. Taking N2C NH_3 and NSCT NH3 as plasma generation gases, respectively, combined with the principle of plasma generation, The results of active species and phase detection in three gas media show that the order of reductivity of the three gas media is: N2 thermal decomposition NH_3N_2 cold NH_3N_2. The plasma reduction time has an important effect on the reduction of CuO: with the prolongation of the reduction time, the relative content of Cu increases first and then decreases, the highest content is 34.38 at 70s; The color of the sample surface changed obviously with the reduction time, from black to gray, then to brick red and orange, which was caused by the change of reduction product. With the increase of reduction time, the melting of particles on the surface of the sample is aggravated, accompanied by the phenomenon of particle agglomeration. With the increase of the output power of the equipment, the relative content of Cu on the surface of the sample increases first and then decreases, while the content of mesophase Cu2O increases gradually. When the output power is small, the sample surface appears brown red, with the increase of power, the red surface of the sample becomes deeper. When the output power is too high, the reduction product is oxidized again. In the process of increasing the power, the particles on the surface of the sample melt and aggregate, the surface of the sample is cooled with small pores, and the new phase forms from the surface of the aggregate and then the surface is melted. In the process of plasma reduction, the reduction reaction and the oxidation reaction compete with each other. During the reaction, the active particles collide on the surface of the sample, sputtering and transferring the energy to the oxide particles so that their energy is higher than the activation energy of the reaction to promote the reduction reaction.
【学位授予单位】：长安大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：TG178
本文编号：2408574
[Abstract]:Due to its many advantages such as cleanliness, high efficiency, simple equipment and little influence on material properties, jet plasma reduction method has been widely used in surface treatment of polymer, metal, semiconductor, PCB circuit board and so on. This technology can be used in circuit board to solve the problem of removing oxide coating before copper plate is used. The technology is effective and environmentally friendly instead of the activation treatment before electroplating. Atmospheric pressure plasma reduction technology can also be used for ceramic and metal connection. However, there are many safety risks in the gas medium of jet plasma, which is used in the process of reduction, such as transportation, storage and use of hydrogen. At the same time, there are few researches on the mechanism of plasma reduction. Therefore, the purpose of this paper is to find a kind of gas that can replace hydrogen as plasma gas, and use scanning electron microscope (SEM) (SEM), energy spectrometer (EDS),). The effects of gas medium and process parameters on the micromorphology, phase composition and element distribution of CuO reduction by atmospheric pressure plasma were studied by means of X-ray diffractometer (XRD), and the action law of each parameter was discussed, and the reduction process was optimized. The mechanism of plasma reduction is analyzed based on the test results, which provides theoretical guidance and technical support for other applications of plasma reduction technology. Taking N2C NH_3 and NSCT NH3 as plasma generation gases, respectively, combined with the principle of plasma generation, The results of active species and phase detection in three gas media show that the order of reductivity of the three gas media is: N2 thermal decomposition NH_3N_2 cold NH_3N_2. The plasma reduction time has an important effect on the reduction of CuO: with the prolongation of the reduction time, the relative content of Cu increases first and then decreases, the highest content is 34.38 at 70s; The color of the sample surface changed obviously with the reduction time, from black to gray, then to brick red and orange, which was caused by the change of reduction product. With the increase of reduction time, the melting of particles on the surface of the sample is aggravated, accompanied by the phenomenon of particle agglomeration. With the increase of the output power of the equipment, the relative content of Cu on the surface of the sample increases first and then decreases, while the content of mesophase Cu2O increases gradually. When the output power is small, the sample surface appears brown red, with the increase of power, the red surface of the sample becomes deeper. When the output power is too high, the reduction product is oxidized again. In the process of increasing the power, the particles on the surface of the sample melt and aggregate, the surface of the sample is cooled with small pores, and the new phase forms from the surface of the aggregate and then the surface is melted. In the process of plasma reduction, the reduction reaction and the oxidation reaction compete with each other. During the reaction, the active particles collide on the surface of the sample, sputtering and transferring the energy to the oxide particles so that their energy is higher than the activation energy of the reaction to promote the reduction reaction.
【学位授予单位】：长安大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：TG178
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