【作者】 张璐；

【导师】 崔彤；

【作者基本信息】 东北大学 ， 材料工程（专业学位）， 2017， 硕士

【摘要】 随着材料科学的发展,传统的TiC和TiN薄膜材料不能满足切削刀具材料的要求,Ti-Si-N膜具有高硬度、低摩擦因数、良好的热稳定性和化学稳定性等优良特性,非常适合于高速切削刀具的表面保护和模具的现代机械行业的要求,目前在薄膜行业中的应用前景十分广泛。利用磁控溅射技术,通过调整工艺参数:氮流量、溅射温度、溅射功率、沉积时间、渐变时间、调制周期以及调制比,在304不锈钢基体上制备一系列Ti-Si-N 单层膜、Ti-Si-N 梯度膜和 TiN/TiSiN 多层膜。用 Philips X’Pert MPD 全自动衍射仪和JDM-7001F场发射电子扫描显微镜分别研究了样品的晶体结构和微观形貌,401MVDTM显微硬度仪和WS-25型涂层附着力自动划痕仪分别研究了薄膜的硬度、膜基结合力等力学性能。研究了薄膜微观结构、晶体结构和力学性能的相互关系。(1)对于单层Ti-Si-N薄膜,通过氮流量、溅射温度等工艺参数对Ti-Si-N薄膜微观组织、晶体结构和力学性能的影响发现:随着氮流量的增加,均出现γ-Si3N4(511)的特征峰,薄膜的硬度先增加后降低。当氮气流量增加到8 sccm时(Ti-10Si(at%)靶),薄膜晶粒细小均匀、致密度高。当氮流量为10 sccm时(Ti-20Si(at%)靶),晶粒细小,此时薄膜硬度(4181 HV)和结合力达到(41 N)达到最大值,薄膜的综合性能达到了最佳值。随着溅射温度的增加,TiN(200)特征衍射峰逐渐增强。当温度为300℃时,薄膜晶粒显著变小、致密度高,两种靶材溅射薄膜的硬度分别达到3878 HV(Ti-10Si(at%)靶)和 41 81 HV(Ti-20Si(at%)靶)。随着溅射功率的增加,Ti-Si-N薄膜的衍射图谱中以TiN为主。功率增加到600 W和800 W时,薄膜晶粒细小均匀。当功率为800 W时(Ti-20Si(at%)靶),硬度达到最大为4582 HV。随着沉积时间的增加,晶粒尺寸均匀细小,硬度呈线性增加。当沉积时间为 240 min 时(Ti-20Si(at%)靶),硬度达到 4605 HV。(2)对于Ti-Si-N梯度膜,随着渐变时间增加梯度膜中出现Ti、TiN、γ-Si3N4三种物相,梯度膜表面形貌的变化不大。硬度和结合力随着渐变时间的增加先增加后减小,当渐变时间为90 min时,硬度达到最大值为4558 HV,结合力达到了 44 N。与单层膜相比硬度提高了 200 HV,结合力提高了 18N。(3)对于TiN/TiSiN多层膜,出现Ti、TiN、Ti2N和γ-Si3N4四种物相,当调制比为1:2时,薄膜的表面形貌变为胞状,晶粒尺寸较小,且晶粒致密度好,获得的薄膜质量好。调制周期为15层时,结合力随着调制周期的增加先增加后减小,结合力达到了 35 N。更多还原

【Abstract】 With the development of material science,the traditional TiC and TiN film material can not meet the requirements of cutting tool materials,Ti-Si-N film with high hardness,low friction coefficient,good thermal stability and chemical stability,other excellent characteristics,is very suitable for high-speed cutting tool surface protection and requirement of the modern mechanical industry,at present the application prospect is very wide in the film industry.Using magnetron sputtering technology,by adjusting the process parameters:the nitrogen flow,sputtering temperature,sputtering power,deposition time,gradient time,modulation period,and modulation ratio,on the 304 stainless steel substrate,a series of Ti-Si-N monolayers,Ti-Si-N compositional gradient film and TiN/TiSiN multilayered film were prepared on a 304 stainless steel substrate.The crystal structure and microstructure of samples were studied by Philips X ’Pert MPD automatic diffractometer and JDM-7001F field emission scanning electron microscope.The 401MVDTM micro-hardness tester and WS-25 type coating adhesion automatic scoring instrument were respectively the mechanical properties such as hardness,film-base adhesion and so on.The relationship between microstructure,crystal structure and mechanical properties was studied.(1)For single Ti-Si-N films,the effect of process parameters,such as nitrogen flow and sputtering temperature,on the structure and mechanical properties were investigated.With the increase of nitrogen flow,the characteristic peaks ofγ-Si3N4(511)appeared.and the hardness of the films increased at first and then decreased.When the nitrogen flow increased to 8 sccm(Ti-10Si(at%)target),grain size small,and the hardness(4181 HV)and the bonding force(41 N)reach to the maximum value,comprehensive performance had reached the best value of the film.With the increase of sputtering temperature,the characteristic diffraction peak of TiN(200)gradually increased.When the temperature was 300℃ the grain size of the film is obviously small and the density was higher.When the temperature was 300℃,The hardness of the two target sputtered films reached 3878 HV(Ti-10Si(at%)target)and 4181 HV.With the increase of sputtering power,the Ti-Si-N thin film was mainly composed of TiN in the diffraction pattern.When the power was increased to 600 W and 800 W,the grain of the film was fine and uniform.When the power was 800 W(Ti-20Si(at%)target),the hardness reaches a maximum of 4582 HV.With the increase of deposition time,the grain size was uniform and fine,and the hardness increased linearly.When the deposition time increased to 240 min(Ti-20Si(at%)target),the hardness increased to 4605 HV.(2)For the Ti-Si-N gradient film,the Ti,TiN,and γ-Si3N4 phases appear in the gradient film with increasing gradient time,and the surface morphology of the gradient film had little change.Hardness and binding force increase and then decreased with the increase of gradient time.When the gradient time was 90 min,the hardness reached 4558 HV and the binding force reached 44 N.Compared with the single film hardness increased 200 HV,the binding force increased by 18 N.(3)TiN,TiN,Ti2N and y-Si3N4 appeared in TiN/TiSiN multilayers.When the modulation ratio is 1:2,the surface morphology of films became cellular and the grain size was small.When the modulation period was 10.When the modulation period was 15 layers,the binding force increased with the increased of the modulation period,and then decreased.The bonding force reached 35 N.更多还原