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Chinese Journal of Materials Research  2019, Vol. 33 Issue (2): 138-144    DOI: 10.11901/1005.3093.2018.343
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Preparation of Structure-Modulated Superhard Ti/TiN Nano-Multilayers and Size Effect
Bobo YANG,Hui SUN(),Tianlin YANG(),Xiaolong ZHENG,Tao XU,Fangzheng LI,Shumei SONG
School of Space Science and Physics, Shandong University Weihai, Weihai 264209, China
Cite this article: 

Bobo YANG,Hui SUN,Tianlin YANG,Xiaolong ZHENG,Tao XU,Fangzheng LI,Shumei SONG. Preparation of Structure-Modulated Superhard Ti/TiN Nano-Multilayers and Size Effect. Chinese Journal of Materials Research, 2019, 33(2): 138-144.

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Abstract  

Multilayered films Ti/TiN with 5~40 nm modulation period were prepared on a high-speed steel substrate by multi-arc ion plating technology. The microstructure and mechanical property of the films were characterized by means of scanning electron microscopy (SEM), X-ray energy dispersive spectrometer (EDS), X-ray diffraction (XRD), nanoindentation and scratch test. The effect of modulation period on the performance of multilayered films Ti/TiN was investigated. Results show that the multilayered films Ti/TiN are uniform and dense with lamellar structure but without obvious features of columnar structure. TiN film is preferentially grown along the (111) direction. The film hardness increases firstly and then decreases with the decrease of the modulation period. The maximum hardness of 42.9 GPa and the maximum H/E value werer obtained when the modulation period is 7.5 nm, which indicates that the film possesses good combination of wear resistance and toughness. In addition, the adhesion of the multilayered films Ti/TiN is generally higher than that of the single-layered TiN film. When the modulation period is 7.5 nm, multilayered films Ti/TiN present a relatively high adhesion of (58±0.9) N.

Key words:  metallic materials      nano-multilayer      Ti/TiN      multi-arc ion plating      small modulation period      superhard effect     
Received:  23 May 2018     
ZTFLH:  TG148  
Fund: Shandong Provincial Natural Science Foundation(ZR2018QEM002);Young Scholars Program of Shandong University (Weihai)

URL: 

https://www.cjmr.org/EN/10.11901/1005.3093.2018.343     OR     https://www.cjmr.org/EN/Y2019/V33/I2/138

Fig.1  Schematic diagram of the equipment (a) and the barrel substrate holder (b)
Fig.2  Schematic drawing of Ti/TiN multilayer films
Fig.3  SEM cross section of singlelayer TiN film (a) and 2# Ti/TiN multilayer films (b)
Fig.4  Cross-section of Ti/TiN multilayer films with different modulation periods (a) 1#, (b) 2#, (c) 3#, (d) 4#, (e) 5#
Sample No.Ti/TiN single layer deposition time/s

Ti/TiN single layer

thickness/nm

Modulation

period/nm

Number

of periods

Total thickness/μm
1#Ti48/TiN14410.9/28.339.2301.34
2#Ti24/TiN725.4/14.920.3601.35
3#Ti12/TiN363.2/10.013.21201.32
4#Ti9/TiN211.7/5.87.51801.33
5#Ti6/TiN18-5.22401.27
Table 1  Thin film parameters of Ti/TiN multilayer films
Fig.5  XRD patterns of Ti/TiN multilayers with differ-ent modulation periods
Fig.6  Nano-hardness and elastic modulus of Ti/TiN multilayers
Fig.7  Hall-Petch parameters calculated based on modulation period (a) and larger grain size (b)
Modulation period39.2 nm20.3 nm13.2 nm7.5 nm

5.2 nm

(calculation)

Singlelayer TiN
H/GPa26.928.534.442.933.925.5
E/GPa294.52310.08348.38357.88314.85302.50
H/E0.09210.09180.09860.11980.10780.084
Table 2  Hardness, elastic modulus, and H/E of singlelayer TiN film and Ti/TiN multilayer films
Fig.8  Adhension of Ti/TiN multilayer films with differ-ent modulation periods
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