Enhancing Osteogenic Response in Selective Laser Melting-Fabricated Titanium through Hierarchical Micro/Nano Surface Engineering via Acid and Iodine Treatments

Selective laser melting (SLM) enables the fabrication of patient-specific titanium (Ti) implants with complex geometries. However, the as-built SLM-Ti surfaces retain partially melted particles that may hinder favorable cellular responses. Because surface topography plays a critical role in regulating osteogenic cell behavior, controlled surface modification is needed to optimize these responses. In this study, SLM-Ti samples were treated with a mixed-acid solution for 1, 3, or 6 h (designated A1, A3, and A6, respectively) to regulate their macro- and microtopography. Surface characteristics were quantified using conventional roughness parameters (Ra and Rz) and fractal dimension (Df), which provided a quantitative measure of hierarchical surface complexity and guided surface optimization. The responses of MC3T3-E1 preosteoblasts to untreated and acid-treated samples were assessed by measuring cell proliferation, alkaline phosphatase (ALP) activity, and extracellular matrix mineralization. Among the acid-treated groups, A1 (Ra = 9.3 μm; Df = 1.187) showed the most favorable combination of cell proliferation and ALP activity, indicating enhanced early osteogenic differentiation. Accordingly, A1 was selected as the optimal macro-/microstructured surface for subsequent hierarchical modification. The A1 surface was then subjected to sequential NaOH-CaCl2-heat-ICl3 treatment to produce the A1-Io surface, which contained an iodine-containing calcium-deficient calcium titanate nanostructured layer superimposed on the microstructured surface. This hierarchical macro-/micro-/nanoarchitecture increased Df to 1.359, reflecting greater multiscale surface complexity. Compared with A1 alone, A1-Io enhanced late-stage extracellular matrix mineralization and further improved cell proliferation and ALP activity. These findings demonstrate that controlled acid etching followed by iodine treatment provides a quantitatively guided strategy for enhancing the osteogenic performance of SLM-fabricated titanium implants.

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Journal
ACS Applied Bio Materials
Published
2026-11-08
DOI
https://doi.org/10.1021/acsabm.6c01470
Primary Topic
Bone Tissue Engineering Materials
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article
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article

Enhancing Osteogenic Response in Selective Laser Melting-Fabricated Titanium through Hierarchical Micro/Nano Surface Engineering via Acid and Iodine Treatments

Seiji Yamaguchi, Morihiro Ito, Seine A. Shintani, Hisashi Kitagaki et al.
ACS Applied Bio Materials
Bone Tissue Engineering Materials
article

Enhancing Osteogenic Response in Selective Laser Melting-Fabricated Titanium through Hierarchical Micro/Nano Surface Engineering via Acid and Iodine Treatments

Seiji Yamaguchi, Morihiro Ito, Seine A. Shintani, Hisashi Kitagaki, Mahmoud Gallab, Tomiharu Matsushita, Le Hong Phuc
article en

Abstract

Selective laser melting (SLM) enables the fabrication of patient-specific titanium (Ti) implants with complex geometries. However, the as-built SLM-Ti surfaces retain partially melted particles that may hinder favorable cellular responses. Because surface topography plays a critical role in regulating osteogenic cell behavior, controlled surface modification is needed to optimize these responses. In this study, SLM-Ti samples were treated with a mixed-acid solution for 1, 3, or 6 h (designated A1, A3, and A6, respectively) to regulate their macro- and microtopography. Surface characteristics were quantified using conventional roughness parameters (Ra and Rz) and fractal dimension (Df), which provided a quantitative measure of hierarchical surface complexity and guided surface optimization. The responses of MC3T3-E1 preosteoblasts to untreated and acid-treated samples were assessed by measuring cell proliferation, alkaline phosphatase (ALP) activity, and extracellular matrix mineralization. Among the acid-treated groups, A1 (Ra = 9.3 μm; Df = 1.187) showed the most favorable combination of cell proliferation and ALP activity, indicating enhanced early osteogenic differentiation. Accordingly, A1 was selected as the optimal macro-/microstructured surface for subsequent hierarchical modification. The A1 surface was then subjected to sequential NaOH-CaCl2-heat-ICl3 treatment to produce the A1-Io surface, which contained an iodine-containing calcium-deficient calcium titanate nanostructured layer superimposed on the microstructured surface. This hierarchical macro-/micro-/nanoarchitecture increased Df to 1.359, reflecting greater multiscale surface complexity. Compared with A1 alone, A1-Io enhanced late-stage extracellular matrix mineralization and further improved cell proliferation and ALP activity. These findings demonstrate that controlled acid etching followed by iodine treatment provides a quantitatively guided strategy for enhancing the osteogenic performance of SLM-fabricated titanium implants.

ACS Applied Bio Materials
Chubu University (JP), Vietnam Academy of Science and Technology (VN), Minia University (EG)
Bone Tissue Engineering Materials
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