李东昕,王静静,宓保森,马迅,陈天驹,刘平,李伟.钽掺杂含量对类金刚石薄膜力学性能及生物相容性的影响[J].表面技术,2024,53(20):208-222.
LI Dongxin,WANG Jingjing,MI Baosen,MA Xun,CHEN Tianju,LIU Ping,LI Wei.Effect of Ta Doping Content on Mechanical Properties and Biocompatibility of Diamond-like Carbon Thin Films[J].Surface Technology,2024,53(20):208-222 |
| 钽掺杂含量对类金刚石薄膜力学性能及生物相容性的影响 |
| Effect of Ta Doping Content on Mechanical Properties and Biocompatibility of Diamond-like Carbon Thin Films |
| 投稿时间：2023-11-02 修订日期：2024-02-01 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.20.019 |
| 中文关键词: 类金刚石薄膜 磁控溅射 钽掺杂 摩擦磨损性能 生物相容性 |
| 英文关键词:diamond-like carbon film magnetron sputtering Ta-doped friction and wear property biocompatibility |
| 基金项目:国家自然科学基金(51971148) |
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| Author | Institution |
| LI Dongxin | School of Materials and Chemistry, University of Shanghai for Science and Technology, Shanghai 200093, China |
| WANG Jingjing | School of Materials and Chemistry, University of Shanghai for Science and Technology, Shanghai 200093, China |
| MI Baosen | School of Materials and Chemistry, University of Shanghai for Science and Technology, Shanghai 200093, China |
| MA Xun | School of Materials and Chemistry, University of Shanghai for Science and Technology, Shanghai 200093, China |
| CHEN Tianju | School of Materials and Chemistry, University of Shanghai for Science and Technology, Shanghai 200093, China |
| LIU Ping | School of Materials and Chemistry, University of Shanghai for Science and Technology, Shanghai 200093, China |
| LI Wei | School of Materials and Chemistry, University of Shanghai for Science and Technology, Shanghai 200093, China |
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| 中文摘要: |
| 目的 探索钽(Ta)掺杂类金刚石(DLC)薄膜的结构转变规律，并提升其力学性能、摩擦性能及生物相容性能。方法 采用非平衡性磁控溅射镀膜技术，在0~0.5 kW功率下，制备了不同Ta掺杂含量的DLC薄膜。对其微观形貌、组织成分、摩擦性能、力学性能以及生物相容性进行了详细表征。结果 钽的掺入提升了碳的沉积速率，导致薄膜厚度增加，薄膜中sp3-C含量随Ta掺杂量的增加先升高后降低。在Ta-0.2 kW及以上的DLC薄膜中出现了TaC晶体和Ta—Ta纳米团簇，这导致薄膜表面粗糙度先增后减。与未掺杂的DLC薄膜相比，掺杂Ta的DLC薄膜的膜基结合力从10 N提高到25 N，断裂韧性从0.6 MPa.m1/2提高到1.6 MPa.m1/2以上，干摩擦因数从0.45降低到0.1~0.15，湿摩擦因数0.35降低至约0.1，干摩擦磨损率从4 500× 10−6 mm3/(N.m)降低至7×10−6 mm3/(N.m)以下，湿摩擦磨损率更是降低到1×10−6 mm3/(N.m)。但掺杂Ta的DLC薄膜的弹性模量有所降低，润湿性也略有下降，硬度并没有太大改变。此外，掺杂Ta的薄膜还表现出了良好的诱导羟基磷灰石形成能力，生成的羟基磷灰石层的钙磷原子比(Ca/P)介于1.4~1.65，接近人体的Ca/P比例，并且无论掺杂还是未掺杂的薄膜均未显示出细胞毒性。结论 钽的掺入显著提升了DLC薄膜的膜基结合力、断裂韧性、摩擦磨损性能和促进羟基磷灰石形成能力。因此，这种薄膜具有作为生物保护层应用于植入体表面的潜力。在Ta-0.4 kW时，Ta-DLC薄膜展现出了最佳的综合性能。 |
| 英文摘要: |
| Moderate doping of heterogeneous elements can effectively solve the problem of insufficient adhesion between diamond-like carbon (DLC) thin films and substrates, leading to film detachment. In recent years, tantalum (Ta) has been introduced as a new metal dopant in carbon-based thin films, which can significantly improve the mechanical and tribological properties of the films. As a biocompatible metal with high melting point, wear resistance, corrosion resistance, high ductility, and excellent biocompatibility, tantalum exhibits structure and mechanical properties similar to human bones, promoting the proliferation and osteogenesis of human osteoblast cells. However, there is still limited research on tantalum-doped DLC films, especially regarding their biocompatibility. This study aims to explore the structural transformation of tantalum-doped DLC films and enhance their mechanical properties, tribological performance, and biocompatibility. The non-equilibrium magnetron sputtering technique was employed to deposit the films, and the tantalum doping level was controlled by adjusting the power of the tantalum target. DLC films with different Ta doping levels were prepared at power levels ranging from 0 to 0.5 kW. The films were characterized in terms of microstructure, chemical composition, friction performance, mechanical properties, and biocompatibility. The relationship between tantalum doping level and film performance was investigated to identify the optimal tantalum doping ratio and obtain DLC films with excellent performance, laying a foundation for their widespread applications in surface modification of artificial joints and other fields. The results showed that the inclusion of tantalum increased the carbon deposition rate, leading to an increase in film thickness. The sp3-C content in the films initially increased and then decreased with the increase of the Ta doping level. TaC crystals and Ta—Ta nanoclusters were observed in the DLC films doped with Ta at 0.2 kW and above, which resulted in an initial increase and subsequent decrease in surface roughness. Compared with undoped DLC films, Ta-doped DLC films exhibited several improvements. The film-based bonding force increased from 10 N to 25 N, leading to enhanced adhesion between the film and the substrate. The fracture toughness also improved from 0.6 MPa.m1/2 to a value of 1.6 MPa.m1/2 or higher. This indicated that the Ta-doped DLC films were more resistant to crack propagation, making them more mechanically robust. In terms of friction properties, the dry friction coefficient decreased from 0.45 to a range of 0.1 to 0.15. This meant that the Ta-doped DLC films experience reduced friction when in contact with dry surfaces. Similarly, the wet friction coefficient decreased from 0.35 to around 0.1, indicating improved lubrication and reduced friction under wet conditions. Moreover, the wear rate associated with dry friction diminished significantly from 4 500×10−6 mm3/(N.m) to 7×10−6 mm3/(N.m) or lower. The wet friction wear rate also decreased to 1×10−6 mm3/(N.m). This suggested that Ta-doped DLC films exhibited superior wear resistance, making them more durable in both dry and wet environments. However, there were slight compromises in other aspects. The elastic modulus of Ta-doped DLC films experienced a slight decrease, indicating a slight reduction in their stiffness. Additionally, the wettability of the films also underwent a slight decrease. In addition, by simulating body fluid immersion, Ta doped thin films exhibited good capability in inducing hydroxyapatite formation, with a calcium-to-phosphorus (Ca/P) ratio ranging from 1.4 to 1.65, close to the Ca/P ratio in the human body. No cytotoxicity was observed for either doped or undoped films. In summary, the doping of Ta significantly improves the tribological and mechanical properties of DLC films, as well as the capability to induce hydroxyapatite formation. Therefore, these films have the potential to be used as a bio-protective layer on the surface of implants. The Ta-DLC film exhibits the best overall performance at Ta-0.4 kW. |
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