# Internal Stress of Titanium-Based Nitride with Penetration Depth and Surface Roughness by sin2ψ Method Using HR-XRD

**Authors:** Sungju Yoo, Eunpyo Hong, Youngkue Choi, Heesoo Lee

PMC · DOI: 10.3390/nano15110813 · Nanomaterials · 2025-05-28

## TL;DR

This paper optimizes a method to measure internal stress in titanium-based nitride coatings and shows how carbon doping affects their mechanical properties.

## Contribution

A validated internal stress measurement method for TiN and TiZrN coatings is developed, accounting for penetration depth and surface roughness effects.

## Key findings

- Internal stress measurements remained consistent across different penetration depths and surface roughness up to 0.03 Sa.
- Carbon doping via laser carburization increased compressive internal stress in TiZrN coatings, improving mechanical properties.
- The highest internal stress was observed at a 0.5 μm coating thickness with the highest carbon gradient layer ratio.

## Abstract

The test method for internal stress of titanium-based nitride was optimized via penetration depth and surface roughness. Through the test method, the variations in the mechanical properties due to the ratio of the carbon gradient layer were investigated in terms of internal stress. TiN coatings were deposited on SUS 304 using RF/DC magnetron sputtering, and the penetration depth was adjusted by varying the X-ray power of HR-XRD for test specimens with the same coating thickness of 1 μm. The gradient of diagram for internal stress remained constant regardless of the penetration depth, and this was attributed to the analysis of internal stress focusing on the preferred growth orientation of the coating and excluding the influence of the substrate. In addition, we tested different surface roughness values (0.01 Sa, 0.02 Sa, and 0.03 Sa) to observe the effect on internal stress measurement. The results showed negligible difference in internal stress, confirming that this measurement method is valid for coatings with a surface roughness of 0.03 Sa or less. The test method was applied to analyze the carbon-doped TiZrN coating. TiZrN coatings were deposited on SUS 304, and coating thicknesses of 0.5 μm, 1 μm, and 2 μm were used to control the ratio of the carbon gradient layer. After applying the carbon paste for carbon doping, the TiZrN coating was irradiated with a pulsed laser. The compressive internal stress increased from −1263 MPa to −1687 MPa at a coating thickness of 0.5 μm, where the ratio of the carbon gradient layer was the highest. It was confirmed that the increase in internal stress with the ratio of the carbon gradient layer improved the mechanical properties of the carbon-doped TiZrN coating by laser carburization.

## Linked entities

- **Chemicals:** TiN (PubChem CID 5352426), carbon (PubChem CID 5462310)

## Full-text entities

- **Chemicals:** TiN (MESH:D014001), carbon (MESH:D002244), Titanium (MESH:D014025), Nitride (-)
- **Cell lines:** SUS — Canis lupus familiaris (Dog), Spontaneously immortalized cell line (CVCL_WL70)

## Full text

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## Figures

7 figures with captions in the complete paper: https://tomesphere.com/paper/PMC12157817/full.md

## References

21 references — full list in the complete paper: https://tomesphere.com/paper/PMC12157817/full.md

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Source: https://tomesphere.com/paper/PMC12157817