常壓等離子體還原氧化銅工藝的研究
發(fā)布時間：2019-01-14 09:41
【摘要】：射流型常壓等離子體還原方法由于其具有清潔、高效、設(shè)備簡單和對材料性能影響小等一系列優(yōu)點,被廣泛用于高分子、金屬、半導體、PCB電路板等的表面處理。該技術(shù)用于電路板,可以解決銅板使用前必須去除氧化皮的問題。將該技術(shù)代替電鍍前的活化處理,既高效又環(huán)保。常壓等離子還原技術(shù)還可以用于陶瓷與金屬的連接。但是用于還原過程的射流型等離子體,其氣體介質(zhì)通常采用氫氣,氫氣在運輸、貯存和使用過程中存在許多安全隱患,同時對于等離子體還原的機理研究較少。因此本文旨在尋找一種能夠代替氫氣的氣體作為等離子體發(fā)生氣,利用掃描電鏡(SEM)、能譜儀(EDS)、X射線衍射儀(XRD)等手段研究了氣體介質(zhì)和工藝參數(shù)對常壓等離子體還原CuO的微觀形貌、相組成和元素分布的影響,討論了各參數(shù)的作用規(guī)律,優(yōu)化還原工藝,并結(jié)合檢測結(jié)果分析了等離子體還原的機制,為等離子還原技術(shù)的其他應用提供理論指導和技術(shù)支持。分別以N_2、N_2~+冷NH_3和N_2~+熱分解NH3作為等離子體發(fā)生氣,結(jié)合等離子體的產(chǎn)生原理、三種氣體介質(zhì)中的活性物種及物相檢測結(jié)果推出三種氣體介質(zhì)的還原性強弱順序為:N2+熱分解NH_3N_2+冷NH_3N_2。等離子體還原時間對CuO還原有重要影響:隨著還原時間延長還原產(chǎn)物Cu的相對含量先增加后減少,70s時的含量最高,為34.38%;試樣表面的顏色隨還原時間發(fā)生明顯變化,由黑色轉(zhuǎn)變?yōu)榛疑?然后變成磚紅色、橘紅色,這是還原產(chǎn)物發(fā)生變化引起的;隨還原時間的增加,試樣表面的顆粒熔融現(xiàn)象加劇,伴隨著顆粒團聚現(xiàn)象。隨著設(shè)備輸出功率增大,試樣表面的還原產(chǎn)物Cu的相對含量先增加后減少,而中間相Cu2O的含量則逐漸增加;當輸出功率較小時,試樣表面呈現(xiàn)棕紅色,隨著功率增大,試樣表面的紅色變深。輸出功率過大會導致還原產(chǎn)物重新被氧化;在功率增大過程中,試樣表面的顆粒熔融聚集,冷卻時表面留下細小孔洞,新相從聚集體表面形成然后表面被融化。在等離子體還原過程中,存在還原反應和氧化反應相互競爭的行為。反應時活性粒子在試樣表面發(fā)生碰撞、濺射,將能量轉(zhuǎn)移給氧化物粒子使其能量高于反應活化能促使還原反應發(fā)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.
【學位授予單位】：長安大學
【學位級別】：碩士
【學位授予年份】：2016
【分類號】：TG178
本文編號：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.
【學位授予單位】：長安大學
【學位級別】：碩士
【學位授予年份】：2016
【分類號】：TG178
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