β-SiC粉体表面改性铜膜的制备及表征

发布时间：2018-10-25 14:57

【摘要】：20世纪以来,随着电子技术、航空航天、能源、计算机、激光、通信、光电子学、生物医学以及环境保护等新技术的兴起,新技术的发展对材料提出了更高的要求,促进了无机非金属材料的迅速发展。而无机非金属材料具有的耐压强度高、硬度大、耐高温、抗腐蚀等优异的特性,是金属材料和高分子材料所不及的。SiC作为一种性能优良的无机非金属材料,被广泛应用于电子、信息、精密加工技术、军工、航空航天、特种陶瓷材料和增强材料等领域,越来越受到人们的关注。本试验利用化学镀技术和磁控溅射技术在β-SiC粉体(β-SiC)表面包覆金属铜膜,对表面铜膜的形貌、相组成、表面粗糙度、膜层与基体的结合力、膜层厚度及薄膜沉积过程和沉积机理进行了深入的研究,对试验结果给出了合理的解释,对化学镀方法和磁控溅射方法在粉体表面改性方面的应用做了详细的比较。采用本课题组优化后的化学镀工艺参数,在β-SiC表面成功地制备了金属铜膜,膜层均匀、致密,与基体结合良好。通过机械搅拌,粉体可在镀液中保持良好的分散状态,使得化学镀技术容易实现在微米β-SiC颗粒(β-SiCp)、β-SiC晶须(β-SiCw)和纳米β-SiC颗粒(纳米β-SiCp)等超细粉体表面镀膜。由于粉体过细,化学镀过程中在纳米β-SiCp表面生成的微晶铜极易吸附镀液中的O,生成Cu2O杂质相。化学镀铜表面薄膜生长过程属于岛状沉积模式,被还原出来的Cu原子附着在活化后β-SiC表面的具有催化作用的粒子(质点)上,Cu原子在质点周围沉积,并相互连接,最终形成连续的Cu薄膜。利用多功能磁控溅射镀膜装置成功地实现了在β-SiCp表面包覆金属铜膜。与化学镀铜膜相比,磁控溅射铜膜更加均匀、致密、完整,与β-SiCp结合力优于化学镀铜膜与β-SiCp结合力。通过调节设备自带的超声系统功率和机械摆动频率,保证了β-Si Cp每个面的溅射镀膜。研究了溅射时间、溅射功率和基底温度对铜膜质量的影响。溅射试验结果表明:β-SiCp表面铜膜的结晶度、膜层厚度、表面粗糙度及表面铜晶粒尺寸均随着溅射时间的延长、溅射功率的增加、基底温度的升高而增大。β-SiCp表面磁控溅射铜膜沉积为动态沉积,动态薄膜沉积的机制为岛状为主、层状为辅的混合生长机制。尽管化学镀和磁控溅射两种方法都可以在β-SiC粉体表面形成铜膜,但是从工艺原理、操作过程、改性层质量、试验成本以及应用领域等方面各不相同。化学镀铜薄膜厚度、表面粗糙度均大于磁控溅射镀铜薄膜,但是化学镀铜薄膜的致密性和结合力比磁控溅射铜薄膜的差。化学镀是一种化学方法,操作复杂,产生的废水、废气易对环境造成影响。磁控溅射是一种真空镀膜方法,薄膜是通过原子沉积形成的,该方法所镀薄膜均匀、致密且纯度高,但是磁控溅射方法制备成本约为化学镀制备成本的3-5倍。
[Abstract]:Since the 20th century, with the rise of electronic technology, aerospace, energy, computer, laser, communication, optoelectronics, biomedicine and environmental protection, the development of new technology has put forward higher requirements for materials. It promotes the rapid development of inorganic non-metallic materials. However, inorganic nonmetallic materials have many excellent properties, such as high pressure resistance, high hardness, high temperature resistance, corrosion resistance and so on. SiC, as a kind of inorganic nonmetallic materials with excellent properties, is widely used in electronics. More and more attention has been paid to the fields of information, precision machining, military industry, aerospace, special ceramic materials and reinforcements. In this experiment, electroless plating and magnetron sputtering were used to coat the metal copper film on the surface of 尾-SiC powder (尾-SiC). The morphology, phase composition, surface roughness and adhesion between the film and the substrate were investigated. The film thickness, deposition process and deposition mechanism were studied, the experimental results were explained reasonably, and the application of electroless plating method and magnetron sputtering method in powder surface modification was compared in detail. Using the optimized process parameters of electroless plating, copper film was successfully prepared on the surface of 尾-SiC. The coating was uniform, compact and well bonded to the substrate. By mechanical agitation, the powder can be dispersed in the bath, and the electroless plating technology is easy to realize the coating on the surface of micron 尾-SiC (尾-SiCp), 尾-SiC whisker (尾-SiCw) and nano 尾-SiC (nano 尾-SiCp). Because the powder is too fine, the microcrystalline copper formed on the surface of nanometer 尾-SiCp during electroless plating is easy to adsorb the O in the bath and form the Cu2O impurity phase. The growth process of electroless copper-plated surface films belongs to the island deposition model. The reduced Cu atoms are attached to the catalytic particles (particles) on the activated 尾-SiC surface, and the Cu atoms are deposited around the particles and connected with each other. Finally, continuous Cu films were formed. Metal copper films were successfully coated on 尾-SiCp by multifunctional magnetron sputtering device. Compared with electroless copper coating, magnetron sputtering copper film is more uniform, compact and complete, and the binding force with 尾-SiCp is better than that of electroless copper plating film and 尾-SiCp film. By adjusting the power of ultrasonic system and the frequency of mechanical swing, the sputtering coating on each surface of 尾-Si Cp is ensured. The effects of sputtering time, sputtering power and substrate temperature on the quality of copper film were studied. The results of sputtering test show that the crystallinity, thickness, surface roughness and grain size of copper on 尾-SiCp surface increase with the increase of sputtering time, and the sputtering power increases with the increase of sputtering time. With the increase of substrate temperature, the deposition of 尾-SiCp surface magnetron sputtering copper film is dynamic deposition, the mechanism of dynamic film deposition is island-like and layered mixed growth mechanism. Although both electroless plating and magnetron sputtering can form copper film on the surface of 尾-SiC powder, the process principle, operation process, modified layer quality, test cost and application field are different. The thickness and surface roughness of electroless copper thin film are higher than that of magnetron sputtering copper film, but the density and adhesion of electroless copper plating film are worse than that of magnetron sputtering copper film. Electroless plating is a kind of chemical method. The operation is complicated, the waste water and waste gas are easy to affect the environment. Magnetron sputtering is a vacuum coating method, which is formed by atomic deposition. The film is uniform, compact and pure, but the preparation cost of magnetron sputtering is about 3-5 times as much as that of electroless plating.
【学位授予单位】：佳木斯大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB306

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