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Synthesis and characterization of TiBx (1.2 ≤ x ≤ 2.8) thin films grown by DC magnetron co-sputtering from TiB2 and Ti targets
Surface & Coatings Technology ( IF 5.4 ) Pub Date : 2022-01-14 , DOI: 10.1016/j.surfcoat.2022.128110
Niklas Hellgren 1, 1 , Alexander Sredenschek 1, 1 , Andrejs Petruins 2 , Justinas Palisaitis 3 , Fedor F. Klimashin 2, 2 , Maurico A. Sortica 4 , Lars Hultman 3 , Per O.Å. Persson 3 , Johanna Rosen 1, 2
Affiliation  

Titanium boride, TiBx, thin films were grown by direct current magnetron co-sputtering from a compound TiB2 target and a Ti target at an Ar pressure of 2.2 mTorr (0.3 Pa) and substrate temperature of 450 °C. While keeping the power of the TiB2 target constant at 250 W, and by varying the power on the Ti target, PTi, between 0 and 100 W, the B/Ti ratio in the film could be continuously and controllably varied from 1.2 to 2.8, with close-to-stoichiometric diboride films achieved for PTi = 50 W. This was done without altering the deposition pressure, which is otherwise the main modulator for the composition of magnetron sputtered TiBx diboride thin films. The film structure and properties of the as-deposited films were compared to those after vacuum-annealing for 2 h at 1100 °C. As-deposited films consisted of small (≲50 nm) randomly oriented TiB2 crystallites, interspersed in an amorphous, sometimes porous tissue phase. Upon annealing, some of the tissue phase crystallized, but the diboride average grain size did not change noticeably. The near-stoichiometric film had the lowest resistivity, 122 μΩcm, after annealing. Although this film had growth-induced porosity, an interconnected network of elongated crystallites provides a path for conduction. All films exhibited high hardness, in the 25–30 GPa range, where the highest value of ~32 GPa was obtained for the most Ti-rich film after annealing. This film had the highest density and was nano-crystalline, where dislocation propagation is interrupted by the off-stoichiometric grain boundaries.



中文翻译:

TiB2 和 Ti 靶材直流磁控共溅射生长的 TiBx (1.2 ≤ x ≤ 2.8) 薄膜的合成和表征

在 2.2 mTorr (0.3 Pa) 的 Ar 压力和 450 °C 的衬底温度下,通过直流磁控管共溅射从复合 TiB 2靶和 Ti 靶生长硼化钛 TiB x薄膜。在保持 TiB 2靶的功率恒定在 250 W 的同时,通过改变 Ti 靶上的功率P Ti在 0 和 100 W 之间,薄膜中的 B/Ti 比可以在 1.2 到 1.2 之间连续可控地变化2.8,在P Ti = 50 W 时实现了接近化学计量的二硼化物薄膜 。这是在不改变沉积压力的情况下完成的,否则沉积压力是磁控溅射 TiB x组成的主要调制器二硼化物薄膜。将沉积薄膜的薄膜结构和性能与在 1100 °C 真空退火 2 小时后的薄膜结构和性能进行比较。沉积的薄膜由小的(≲50 nm)随机取向的TiB 2组成微晶,散布在无定形的,有时是多孔的组织相中。退火后,一些组织相结晶,但二硼化物平均晶粒尺寸没有明显变化。近化学计量的薄膜在退火后具有最低的电阻率,为 122 μΩcm。尽管该薄膜具有生长诱导的孔隙率,但相互连接的细长微晶网络提供了传导路径。所有薄膜都表现出高硬度,在 25-30 GPa 范围内,其中退火后最富含 Ti 的薄膜的最高值约为 32 GPa。该薄膜具有最高密度并且是纳米晶体,其中位错传播被非化学计量的晶界中断。

更新日期:2022-01-20
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