Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy 

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These alterations can lead to substantial improvements in mechanical properties, hydrophilicity, osseointegration, and antibacterial performance, as well as positively influencing osteoblast activity and bone formation processes. This paper investigates the effect of the combination of acid etching on titanium alloys’ surface morphology, roughness, and hydrophilicity. Methods A titanium alloy (Ti6Al4V) disc with a diameter of 12 mm and thickness of 2 mm was sandblasted using aluminum oxide Al2O3 by particle sizes 100 μm, 250 μm, and 500 μm and followed by acid etching. Acid etching was carried out on these samples using different combinations of acid, i.e., hydrofluoric acid (HF), hydrochloric acid (HCL), and sulfuric acid (H2SO4), with the same temperature and time exposure. All titanium surfaces were characterized using a scanning electron microscope (SEM) and contact profilometer. Results This study showed that the type of acid combination influenced the surface morphology and roughness profile. After sandblast and acid etching, the titanium alloy has roughness between 1.369 μm – 4.304 μm. There is no significant difference in surface roughness between using a combination of HF, HCL, H2SO4 and only the combination of HCL and H2SO4. Conclusions Titanium alloy has achieved the desired morphology and roughness after sandblasting with Al2O3 250 μm and acid-etching with HCL and H2SO4. Acid etching with a combination of HCL and H2SO4 at 120 degrees can produce micro-topography in a shorter duration. 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F1000Research 2025, 14 :216 ( https://doi.org/10.12688/f1000research.159566.1 ) NOTE: If applicable, it is important to ensure the information in square brackets after the title is included in all citations of this article. Close Copy Citation Details Export Export Citation Sciwheel EndNote Ref. Manager Bibtex ProCite Sente EXPORT Select a format first Track Share ▬ ✚ Brief Report Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy [version 1; peer review: 2 approved with reservations] Fakhrana Ariani Ayub https://orcid.org/0000-0001-7510-1568 1 , Sunarso Sunarso https://orcid.org/0000-0003-0035-4821 2 , Ratna Sari Dewi https://orcid.org/0000-0002-8411-4755 1 Fakhrana Ariani Ayub https://orcid.org/0000-0001-7510-1568 1 , Sunarso Sunarso https://orcid.org/0000-0003-0035-4821 2 , Ratna Sari Dewi https://orcid.org/0000-0002-8411-4755 1 PUBLISHED 17 Feb 2025 Author details Author details 1 Department of Prosthodontics, Faculty of Dentistry, Universitas Indonesia, Jakarta, DKI Jakarta, 10430, Indonesia 2 Department of Dental Materials Science, Universitas Indonesia, Jakarta, DKI Jakarta, 10430, Indonesia Fakhrana Ariani Ayub Roles: Data Curation, Formal Analysis, Writing – Original Draft Preparation, Writing – Review & Editing Sunarso Sunarso Roles: Methodology, Supervision, Validation, Writing – Review & Editing Ratna Sari Dewi Roles: Funding Acquisition, Supervision, Validation, Writing – Original Draft Preparation OPEN PEER REVIEW DETAILS REVIEWER STATUS Abstract Background Surface modifications of titanium alloys used in dental implants can significantly change the implants’ micro and nano topography and composition. These alterations can lead to substantial improvements in mechanical properties, hydrophilicity, osseointegration, and antibacterial performance, as well as positively influencing osteoblast activity and bone formation processes. This paper investigates the effect of the combination of acid etching on titanium alloys’ surface morphology, roughness, and hydrophilicity. Methods A titanium alloy (Ti6Al4V) disc with a diameter of 12 mm and thickness of 2 mm was sandblasted using aluminum oxide Al 2 O 3 by particle sizes 100 μm, 250 μm, and 500 μm and followed by acid etching. Acid etching was carried out on these samples using different combinations of acid, i.e., hydrofluoric acid (HF), hydrochloric acid (HCL), and sulfuric acid (H 2 SO 4 ), with the same temperature and time exposure. All titanium surfaces were characterized using a scanning electron microscope (SEM) and contact profilometer. Results This study showed that the type of acid combination influenced the surface morphology and roughness profile. After sandblast and acid etching, the titanium alloy has roughness between 1.369 μm – 4.304 μm. There is no significant difference in surface roughness between using a combination of HF, HCL, H 2 SO 4 and only the combination of HCL and H 2 SO 4 . Conclusions Titanium alloy has achieved the desired morphology and roughness after sandblasting with Al 2 O 3 250 μm and acid-etching with HCL and H 2 SO 4 . Acid etching with a combination of HCL and H 2 SO 4 at 120 degrees can produce micro-topography in a shorter duration. READ ALL READ LESS Keywords Acid etching, contact angle, roughness, sandblasting, surface morphology, titanium alloy Corresponding Author(s) Ratna Sari Dewi ( [email protected] ) Close Corresponding author: Ratna Sari Dewi Competing interests: No competing interests were disclosed. Grant information: This study was funded by Hibah PUTI Q1 2024 Universitas Indonesia (NKB-333/UN2.RST/HKP.05.00/2024). The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript. The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript. Copyright: © 2025 Ayub FA et al . This is an open access article distributed under the terms of the Creative Commons Attribution License , which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. How to cite: Ayub FA, Sunarso S and Dewi RS. Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy [version 1; peer review: 2 approved with reservations] . F1000Research 2025, 14 :216 ( https://doi.org/10.12688/f1000research.159566.1 ) First published: 17 Feb 2025, 14 :216 ( https://doi.org/10.12688/f1000research.159566.1 ) Latest published: 17 Feb 2025, 14 :216 ( https://doi.org/10.12688/f1000research.159566.1 ) Introduction Surface modification of titanium significantly enhances its topography and composition for dental implants, optimizing roughness, wettability, and antibacterial properties to promote osteoblast attachment and facilitate osseointegration. The method of implant surface modification can be categorized into two groups: subtraction and addition. Subtraction techniques, such as sandblasting, acid etching, sandblasting acid-etched (SLA), anodizing, and laser radiation, effectively modify the titanium surface’s roughness, hardness, and oxidation of Ti. In contrast, addition techniques involve coating the titanium surface with various substances, significantly altering its composition and enhancing biological properties through plasma spraying and sol-gel. 1 , 2 Acid-etching is often performed using hydrofluoric (HF), nitric (HNO 3 ), sulfuric (H 2 SO 4 ), hydrochloric (HCL) acids, and combinations thereof. The surface features after acid etching may vary depending on the time, type, and concentration of the acid. 1 Regarding implant surface roughness, previous research concludes that osteoblast activity increases with a moderately micro-roughness profile with a Ra value range from 1 to 2 μm. The implant surface topography can be classified as smooth (Ra 2.0 μm). 3 The microtopographic features of the implant surface, such as peaks and valleys, are an essential factor in the biological response and the configuration of the bone-implant interface. However, optimal roughness and superficial morphology are still controversial and must be more clearly defined. Therefore, the present study aimed to investigate the effect of the combination of acid etching on titanium alloys’ surface morphology, roughness, and hydrophilicity. SEM analysis has shown that the combination of sandblasting followed by acid etching produces a honeycomb-like pattern. Methods Sample preparation Titanium alloy (Ti6Al4V) discs with a diameter of 12 mm and thickness of 2 mm (n=12) were machined using a 5-axis milling machine, as shown in Figure 1 . Ti-disc was blasted with large grit aluminum oxide Al 2 O 3 by particle size 100 μm, 250 μm, and 500 μm for 30 seconds from a distance of 10 mm, with a pressure of 5 bar. These machine Ti-discs were cleaned in an ultrasonic cleaner using acetone, ethanol, and distilled water for 5 minutes each to remove machining chips, oil, and any organic contamination. After cleaning, samples were dried in a vacuum oven 60-80°C. Acid etching was carried out on these samples in hydrofluoric acid (HF) 48%, hydrochloric acid (HCL) 37%, and sulfuric acid (H 2 SO 4 ) 97%. The etching process in this research was carried out in two methods, which included immersion of titanium in HF at room temperature for 30 seconds followed by immersion in a mixture of HCL and H 2 SO 4 in a ratio of 2:1 at 120 degrees for 5 minutes and the other method was immersion of titanium in a mixture of HCL, H 2 SO 4 , H2O in a ratio of 2:1:1 at 120 degrees for 5 minutes. After the completion of the etching process, the specimens were subjected to ultrasonic cleaning using distilled water and then dried. Figure 1. (a) Ti-disc specimen blasted with large grit aluminum oxide Al 2 O 3 100 μm, 250 μm, and 500 μm (b) SEM images of Ti after sandblasted with large grit aluminum oxide Al 2 O 3 100 μm, 250 μm, and 500 μm. Surface morphology, roughness, and contact angle Evaluation of implant surface morphology using Scanning Electron Microscope (SEM) (Thermoscientific Quanta 650) with 1000× and 3000× magnification. The surface roughness of the titanium sample was also measured with a contact profilometer (MarSurf PS 10, Mahr GmbH) to obtain the Ra value. Surface wettability was tested through contact angle measurement using the sessile drop method. Analysis and measurement of contact angle were done with ImageJ software. Results The acid type significantly affects the titanium alloy’s morphology (Ti6Al4V) surface. Figure 1 presents the Ti-disc specimen and SEM images after sandblasting with Al 2 O 3 particles. After sandblasting, SEM results show a heterogeneous and irregular titanium surface with varying degrees of roughness, depending on the size of the Al 2 O 3 particles used. SEM results show that the sandblasting process on the surface of titanium alloy using Al 2 O 3 particles produces a unique and irregular surface topography with peaks and valleys of varying sizes ranging from shallow and small depressions to more extensive and more profound depressions. The difference in Al 2 O 3 particle size also affects the surface morphology. SEM results show that titanium sandblasted using Al 2 O 3 500 μm produces a more extensive and deeper valley shape when compared to Al 2 O 3 100 μm. The results of etching specimens using HF at room temperature for 30 seconds and continued with a mixture of HCL and H 2 SO 4 (2:1) at 120 degrees for 5 minutes are shown in Figure 2 . Based on the SEM results, the titanium surface topography still shows an irregular surface with varying width and depth, but the etching process creates micro-roughness on the surface after sandblasting. The etching results with this method produce a topographic structure of the titanium surface that shows an irregular surface, more of a rounded porous structure, the peak area is still clearly visible, and the surface texture is less homogeneous. The white structure resulting from the reaction of titanium with H 2 SO 4 and HCL appears to produce deposits and may be attached to the titanium surface. Figure 2. SEM images of Ti after etching using HF at room temperature for 30 seconds, followed by etching using a mixture of HCL and H 2 SO 4 in a ratio of 2:1 at 120 degrees for 5 minutes. The results of etching with HCL, H 2 SO 4 , and H 2 O (2:1:1) at 120 degrees for 5 minutes are shown in Figure 3 . Based on the SEM results, the peak area is reduced and becomes flatter, the sandblast character is less visible, and the resulting surface texture is more homogeneous than the previous method. The combination of sandblasting followed by acid etching with this method results in a honeycomb-like pattern on the titanium surface. In addition, SEM analysis also shows the surface characteristics of titanium with a more even texture and a smaller cavity size than the previous method. Figure 3. SEM images of Ti after etching using a mixture of HCL, H 2 SO 4 , H 2 O in a ratio of 2:1:1 at 120 degrees for 5 minutes. Based on Table 1 , the average roughness of titanium alloy after etching using a combination of HF, HCL, and H 2 SO 4 is higher when compared to using only HCL and H 2 SO 4 . Titanium alloy specimen has roughness between 1.369 μm – 4.304 μm depending on the size of Al 2 O 3. There is no significant difference in surface roughness between using a combination of HF, HCL, H 2 SO 4 and only the combination of HCL and H 2 SO 4 without HF. Table 1. Means and standard deviations of surface roughness for each group of acid. Al 2 O 3 particle size Ra Value (Mean ± SD) p-value HF, HCL + H 2 SO 4 HCL + H 2 SO 4 + H 2 O 100 μm 1.482 ± 0.025 1.369 ± 0.114 0.226 250 μm 2.224 ± 0.050 2.016 ± 0.150 0.127 500 μm 4.312 ± 0.263 4.304 ± 0.225 0.970 Titanium surface modification not only shows an increase in surface roughness but also undergoes chemical modification that will affect the wettability and interaction with biological fluids. The hydrophilicity of the titanium alloy surface after sandblasting and acid etching was determined by measuring the contact angle using the sessile drop method. The results of contact angle measurement are shown in Figure 4 . In general, all titanium specimens show contact angle values < 90°, so it can be concluded that the surface is hydrophilic. Figure 4. Contact angle evaluation after sandblast and acid etching of Ti-disc specimen. Discussion The present study’s finding has proved that acid etching is a relatively dominant factor in deciding the surface texture and roughness. The SEM figure shows that the different acids used to modify the implant surfaces lead to different surface morphology. In this study, the etching of titanium alloy (Ti6Al4V) was optimized to obtain micro- and nano-topography and to improve hydrophilicity and surface roughness. The etching process in this study uses three different acids: hydrofluoric acid (HF) 48%, hydrochloric acid (HCL) 37%, and sulfuric acid (H 2 SO 4 ) 97%. Etching on titanium surfaces significantly affects titanium’s surface morphology and mechanical properties. Each acid contributes uniquely during the etching process to improve surface roughness. HF is known to have aggressive etching ability even at low concentrations. In addition, HF and HCL also contribute effectively to removing the passive oxide layer on the titanium surface, while H 2 SO 4 increases the overall surface roughness due to its strong corrosive properties. Combining these acids will produce a more significant etching effect than using each acid individually. 4 Liang et al. 5 showed that HF can create micro- and nanostructured surfaces on titanium surfaces, significantly improving osteogenic activity and cell attachment. HF effectively removes the passive oxide layer because it naturally reacts with titanium in the TiO 2 layer to promote better cell adhesion. In addition, the concentration and duration of HF etching also play an essential role in determining the surface characteristics of titanium. Zahran et al. 6 found that etching time significantly affects the topography and chemical composition of the titanium surface. In that study, it was observed that fluoride ions began to appear on the surface after the titanium was etched for two minutes using HF. HCL and H 2 SO 4 are the most widely used acid types for etching titanium. The etching process is done by mixing HCL and H 2 SO 4 to accelerate the etching process. In addition, no reaction occurs due to the mixing of the two acids. Previous research showed that the etching process of titanium using HCL and H 2 SO 4 at room temperature takes a very long time to obtain micro-textures on the titanium surface because both acids have a low etching rate at room temperature. Nadar et al. 7 found that although the sandblasting process increased surface roughness, etching performed afterward at high temperatures could produce smoother titanium alloy surfaces. Another study by Hung et al. 4 also showed that higher etching temperatures resulted in lower surface roughness for titanium alloy (Ti6Al4V) when etched using HCL. This phenomenon is related to increased activation energy at higher temperatures, which results in more uniform etching and reduces the formation of sharp microstructures that affect roughness. Although higher temperatures can reduce roughness, it is crucial to consider the balance between achieving the desired surface characteristics and maintaining the roughness required for biological interactions. In this study, titanium alloy etching with HF, HCL, and H 2 SO 4 showed an irregular surface, and the surface texture is less homogeneous than the acid etching method without HF. These results align with a previous study by Madaan et al., which found that using HF has disadvantages, including the potential to create a non-uniform surface profile. Prolonged etching time can also lead to the dissolution of the titanium oxide layer, which can potentially cause excessive roughness and impair mechanical properties, including reduced ductility and increased brittleness of the titanium alloy. This is particularly relevant in the development of dental implants, where the mechanical stability of the implant is crucial. 8 Etching using HF can also contribute to the release of fluoride ions into the surrounding environment, which can potentially cause cytotoxicity and have negative impacts on cell function and viability. Due to these factors, the use of HF for etching titanium alloys requires careful consideration and strict safety protocols, so additional etching methods are needed to achieve optimal results for titanium surface modification. 8 , 9 In this study, an HF solution with a concentration of 48% was used. The etching rate of titanium in 48% HF is very high, which can be advantageous for achieving precise desired surface characteristics within a short time. In this study, titanium alloy etching with HF, HCL, and H 2 SO 4 showed a higher roughness value with a 1.482 μm – 4.312 μm range. However, there is no significant difference in surface roughness between using a combination of HF, HCL, H 2 SO 4 and the combination of HCL and H 2 SO 4 . Based on previous research, the average roughness of commercial titanium implants was about 1-2 μm. 10 Therefore, in this study, the Ti-disc specimen, after being sandblasted using 250 μm Al 2 O 3 followed by etched with a combination of HCL and H 2 SO 4 had a surface roughness close to the roughness of commercial implants and had the desired surface morphology. The effect of sandblasting and acid etching on surface roughness has been highlighted in various studies. 11 Acid etching, in conjunction with sandblasting, refines the surface topography further. This technique introduces micro-roughness on the already roughened surface, creating a more complex topography. The roughness of titanium surfaces and irregular surface features created by these methods can significantly improve the mechanical interlocking between the implant and surrounding bone tissue and improve biological responses from osteoblasts. 12 , 13 All titanium specimens show contact angle values < 90°, so it can be concluded that the surface is hydrophilic. The contact angle of dental implants is an important factor affecting their wettability, which can affect osseointegration and overall implant success. Various surface treatments can significantly change the contact angle of titanium implants, thereby improving their biological performance. This study’s results align with research conducted by Yang and Huang, which showed that the titanium surface after sandblasting and acid etching indicated a moderate level of wettability. Although titanium surfaces are not entirely hydrophilic, they have better wettability than untreated ones, which usually have a higher contact angle. 14 This relationship is crucial for the design of titanium implants to improve osseointegration and overall biocompatibility. Conclusion From the result of this study, it was suggested that sandblast followed by acid etching method was an effective way to roughen titanium alloy surface for dental implant application. Although acid etching creates a rough surface, the etching process must proceed with a control condition. A combination of HCL and H 2 SO 4 seems to be an effective solution for etching in getting the desirable roughness and surface morphology in terms of the micro pit presence and homogenous texture, which may lead to good attachment of cells and might increase bone-to-implant contact. However, further study must evaluate the in vitro and in vivo bone response to these surfaces. Ethics and consent Ethical approval and consent were not required. Data availability Figshare: SEM Images of Titanium Alloy Disc after Sandblasting and Acid Etching, https://doi.org/10.6084/m9.figshare.27987959 . 15 This project contains the following underlying data: • All raw SEM images Figshare: Roughness Measurement of Titanium Alloy Disc after Sandblasting and Acid Etching, https://doi.org/10.6084/m9.figshare.27987935 . 16 This project contains the following underlying data: • Output files for roughness testing. Data are available under the terms of the Creative Commons Attribution 4.0 International license (CC-BY 4.0). References 1. Marenzi G, Impero F, Scherillo F, et al. : Effect of different surface treatments on titanium dental implant micro-morphology. Materials (Basel). 2019; 12 (733): 1–14. Publisher Full Text 2. Tuikampee S, Chaijareenont P, Rungsiyakull P, et al. : Titanium Surface Modification Techniques to Enhance Osteoblasts and Bone Formation for Dental Implants: A Narrative Review on Current Advances. Metals (Basel). 2024; 14 (5): 1–28. Publisher Full Text 3. Nicolas-Silvente AI, Velasco-Ortega E, Ortiz-Garcia I, et al. : Influence of the titanium implant surface treatment on the surface roughness and chemical composition. Materials (Basel). 2020; 13 (314): 1–13. Publisher Full Text 4. Hung KY, Lin YC, Feng HP: The effects of acid etching on the nanomorphological surface characteristics and activation energy of titanium medical materials. Materials (Basel). 2017; 10 (1164): 1–14. Publisher Full Text 5. Liang J, Xu S, Shen M, et al. : Osteogenic activity of titanium surfaces with hierarchical micro-/nano-structures obtained by hydrofluoric acid treatment. Int. J. Nanomedicine. 2017; 12 : 1317–1328. PubMed Abstract | Publisher Full Text | Free Full Text 6. Zahran R, Rosales Leal JI, Rodríguez Valverde MA, et al. : Effect of hydrofluoric acid etching time on titanium topography, chemistry, wettability, and cell adhesion. PLoS One. 2016; 11 (11): 1–12. Publisher Full Text 7. Nadar YS, Kutty MG, Abdul Aziz AR: Relative effect of sand blasting and acid etching on the surface roughness of pure titanium and titanium alloy for dental implants. Adv. Mater. Res. 2014; 1043 : 145–148. Publisher Full Text 8. Madaan V, Padhye AM, Mapara M: Comparative Evaluation of Microroughness created on Titanium Alloy for use in Dental Implants subjected to Two Different Acid Etching Techniques: An in vitro Study. J. Contemp. Dent. 2016; 6 (1): 1–8. Publisher Full Text 9. Chauhan P, Koul V, Bhatnagar N: Critical role of etching parameters in the evolution of nano micro sla surface on the ti6al4v alloy dental implants. Materials (Basel). 2021; 14 (6344): 1–21. Publisher Full Text 10. Jemat A, Ghazali MJ, Razali M, et al. : Surface modifications and their effects on titanium dental implants. Biomed. Res. Int. 2015; 791725 : 1–11. 11. De Tullio I, Berardini M, Di Iorio D, et al. : Comparative evaluation among laser-treated, machined, and sandblasted/acid-etched implant surfaces: an in vivo histologic analysis on sheep. Int. J. Implant. Dent. 2020; 6 (1): 4–11. Publisher Full Text 12. Schupbach P, Glauser R, Bauer S: Al2O3 Particles on Titanium Dental Implant Systems following Sandblasting and Acid-Etching Process. Int. J. Biomater. 2019; 2019 (6318429): 1–11. PubMed Abstract | Publisher Full Text | Free Full Text 13. Wang J, Yang B, Guo S, et al. : Manufacture of titanium alloy materials with bioactive sandblasted surfaces and evaluation of osseointegration properties. Front. Bioeng. Biotechnol. 2023; 11 (August): 1–17. Publisher Full Text 14. Yang WE, Huang HH: TiO2 Nanonetwork on Rough Ti Enhanced Osteogenesis in vitro and In Vivo. J. Dent. Res. 2021; 100 (10): 1186–1193. PubMed Abstract | Publisher Full Text 15. Ayub FA: SEM Images of Titanium Alloy Disc after Sandblasting and Acid Etching. [Dataset] Figshare. 2024. Publisher Full Text 16. Ayub FA: Roughness Measurement of Titanium Alloy Disc after Sandblasting and Acid Etching. [Dataset] Figshare. 2024. Publisher Full Text Comments on this article Comments (0) Version 1 VERSION 1 PUBLISHED 17 Feb 2025 ADD YOUR COMMENT Comment Author details Author details 1 Department of Prosthodontics, Faculty of Dentistry, Universitas Indonesia, Jakarta, DKI Jakarta, 10430, Indonesia 2 Department of Dental Materials Science, Universitas Indonesia, Jakarta, DKI Jakarta, 10430, Indonesia Fakhrana Ariani Ayub Roles: Data Curation, Formal Analysis, Writing – Original Draft Preparation, Writing – Review & Editing Sunarso Sunarso Roles: Methodology, Supervision, Validation, Writing – Review & Editing Ratna Sari Dewi Roles: Funding Acquisition, Supervision, Validation, Writing – Original Draft Preparation Competing interests No competing interests were disclosed. Grant information This study was funded by Hibah PUTI Q1 2024 Universitas Indonesia (NKB-333/UN2.RST/HKP.05.00/2024). The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript. The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript. Article Versions (1) version 1 Published: 17 Feb 2025, 14:216 https://doi.org/10.12688/f1000research.159566.1 Copyright © 2025 Ayub FA et al . This is an open access article distributed under the terms of the Creative Commons Attribution License , which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. Download Export To Sciwheel Bibtex EndNote ProCite Ref. Manager (RIS) Sente metrics Views Downloads F1000Research - - PubMed Central info_outline Data from PMC are received and updated monthly. - - Citations open_in_new 0 open_in_new 0 open_in_new SEE MORE DETAILS CITE how to cite this article Ayub FA, Sunarso S and Dewi RS. Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy [version 1; peer review: 2 approved with reservations] . F1000Research 2025, 14 :216 ( https://doi.org/10.12688/f1000research.159566.1 ) NOTE: If applicable, it is important to ensure the information in square brackets after the title is included in all citations of this article. COPY CITATION DETAILS track receive updates on this article Track an article to receive email alerts on any updates to this article. TRACK THIS ARTICLE Share Open Peer Review Current Reviewer Status: ? Key to Reviewer Statuses VIEW HIDE Approved The paper is scientifically sound in its current form and only minor, if any, improvements are suggested Approved with reservations A number of small changes, sometimes more significant revisions are required to address specific details and improve the papers academic merit. Not approved Fundamental flaws in the paper seriously undermine the findings and conclusions Version 1 VERSION 1 PUBLISHED 17 Feb 2025 Views 0 Cite How to cite this report: Bang LT. Reviewer Report For: Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy [version 1; peer review: 2 approved with reservations] . F1000Research 2025, 14 :216 ( https://doi.org/10.5256/f1000research.175315.r367244 ) The direct URL for this report is: https://f1000research.com/articles/14-216/v1#referee-response-367244 NOTE: it is important to ensure the information in square brackets after the title is included in this citation. Close Copy Citation Details Reviewer Report 14 Mar 2025 Le Thi Bang , School of Materials Science and Engineering, Hanoi University of Science and Technology, Hanoi, Vietnam Approved with Reservations VIEWS 0 https://doi.org/10.5256/f1000research.175315.r367244 The report is on surface modification of titanium in terms of roughening by sandblast and acid etching using various combination of acidic solution. The characterization technique includes SEM, surface roughness and contact angle. Base on the results ... Continue reading READ ALL The report is on surface modification of titanium in terms of roughening by sandblast and acid etching using various combination of acidic solution. The characterization technique includes SEM, surface roughness and contact angle. Base on the results obtained, it was suggested that combination of HCl and H 2 SO 4 is an effective solution to provide pit and homogeneous texture for the surface. The results from this study reflects purpose of research. However, there are some questions need to be addressed: 1) what are the surface roughness and contact angle of Ti after sandblast, and how do they compare with those of the sample after acid etching? Why is sandblasting needed prior to acid etching? 2) It is not clear from the experimental method whether the treatment of HF is applied before the follow-up treatment in the two acidic solution? If not, please revise the method. 3) What the impacts of using HCl+H2SO4 and HCl+H2SO4+H2O for the titanium surface? 4) the author stated that HF 48% is the proper concentration for a desired surface characteristics but etching with HF prior to etching with HCl + H2SO4 is not recommended, as mentioned in the conclusion. Please clarify this contradiction. 5) Typo error: HCL -->HCl 6) The hydrophilicity and surface roughness of Ti after treatments are not significant between the groups, how did the author drawn a conclusion based only on SEM? Is the work clearly and accurately presented and does it cite the current literature? Yes Is the study design appropriate and is the work technically sound? Yes Are sufficient details of methods and analysis provided to allow replication by others? Yes If applicable, is the statistical analysis and its interpretation appropriate? Not applicable Are all the source data underlying the results available to ensure full reproducibility? Yes Are the conclusions drawn adequately supported by the results? Yes Competing Interests: No competing interests were disclosed. Reviewer Expertise: Biomaterials, surface modification of metal implants, material engineering I confirm that I have read this submission and believe that I have an appropriate level of expertise to confirm that it is of an acceptable scientific standard, however I have significant reservations, as outlined above. Close READ LESS CITE CITE HOW TO CITE THIS REPORT Bang LT. Reviewer Report For: Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy [version 1; peer review: 2 approved with reservations] . F1000Research 2025, 14 :216 ( https://doi.org/10.5256/f1000research.175315.r367244 ) The direct URL for this report is: https://f1000research.com/articles/14-216/v1#referee-response-367244 NOTE: it is important to ensure the information in square brackets after the title is included in all citations of this article. COPY CITATION DETAILS Report a concern Respond or Comment COMMENT ON THIS REPORT Views 0 Cite How to cite this report: Abdulla MA. Reviewer Report For: Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy [version 1; peer review: 2 approved with reservations] . F1000Research 2025, 14 :216 ( https://doi.org/10.5256/f1000research.175315.r367242 ) The direct URL for this report is: https://f1000research.com/articles/14-216/v1#referee-response-367242 NOTE: it is important to ensure the information in square brackets after the title is included in this citation. Close Copy Citation Details Reviewer Report 03 Mar 2025 Mohammed A Abdulla , University of Mosul, Mosul, Iraq Approved with Reservations VIEWS 0 https://doi.org/10.5256/f1000research.175315.r367242 Dear Editor, Thanks for referring to this article for review. The method is well-structured, and the extracted data is informative. There are a few points that I would like the authors to correct before indexed the article. ... Continue reading READ ALL Dear Editor, Thanks for referring to this article for review. The method is well-structured, and the extracted data is informative. There are a few points that I would like the authors to correct before indexed the article. Reviewer Comments for Authors: Dear authors, There are a few points that should be corrected as follows: Title : I think the title needs to be modified: Influence of Acid Composition ( Combination ) on Morphology and Physical Properties of Titanium Alloy Abstract Methods : Please add detailed information about statistical analysis Result : After sandblast ( delete ) ( sandblasting ) and acid etching, the titanium alloy……. Introduction What about the hypothesis ?? Methods An important observation is the lack of a control group that did not get any surface treatment, which would serve as a reference point for comparison!? In paragraph no. 1: The etching process in this research was carried out in two methods, which ( first ) included immersion of titanium in HF at room temperature for 30 seconds followed by immersion in a mixture of HCL and H2SO4 in a ratio of 2:1 at 120 degrees for 5 minutes. and the other ( second )method was immersion of titanium……. In correct Figure 1. (a) Ti-disc specimen blasted with large grit aluminum oxide Al2O3 100μm, 250 μm, and 500 μm. (b) SEM images of Ti after sandblasted with large grit aluminum oxide Al2O3 100 μm, 250 μm, and 500 μm. ( delete ) Correct Figure 1. Ti-disc specimens blasted with large grit aluminum oxide Al2O3 100μm, 250 μm, and 500 μm. Results Number the figures as follows: Figure 2 . SEM images of Ti after sandblasted with large grit aluminum oxide Al2O3 100 μm, 250 μm, and 500 μm. Figure 3 . SEM images of Ti after etching using HF at room temperature for 30 seconds, followed by etching using a mixture of HCL and H2SO4 in a ratio of 2:1 at 120 degrees for 5 minutes. Figure 4 . SEM images of Ti after etching using a mixture of HCL, H2SO4, and H2O in a ratio of 2:1:1 at 120 degrees for 5 minutes. Figure 5. Contact angle evaluation after sandblast and acid etching of Ti-disc specimen. In the paragraphs: Paragraph no. 1, Line no. 1 Figure 1 presents the Ti-disc specimen and ( delete ) Figure 2. presents SEM images after sandblasting with Al2O3 particles. Paragraph no. 4 Based on Table 1, the average roughness of titanium alloy after etching using a combination of HF, HCL, and H2SO4 is higher when compared to using only HCL and H2SO4 and H2O . The titanium alloy specimen has roughness between 1.369 μm – 4.304 μm depending on the size of Al2O3. There is no significant difference in surface roughness between using a combination of HF, HCL, and H2SO4 and only ( delete ) compared with the combination of HCL and H2SO4 without HF. Discussion Paragraph no. 1 The SEM, figure shows ( delete ) ( figures showed ) that the different acids used to.... Paragraph no. 3 In that study it was ( delete ) ( and ) observed that fluoride ions began to Paragraph no. 4 In addition, no reaction ( please explain type of reaction ?) occurs due to the mixing of the two acids. Paragraph no. 5 Etching using HF can also contribute to the release of fluoride ions into the surrounding environment, which can potentially cause cytotoxicity and have negative impacts on cell function and viability ( the authors do not test the cytotoxicity and cell function and viability! This explanation needs references ) Explain the summary of key findings (primary outcome measures, secondary outcome measures, results relating to a hypothesis). What does this study add to the available evidence, what effects on patient benefit ? Future research directions (for this research collaboration, underlying mechanisms, clinical research). The limitations of the study need to be clarified. Conclusion From the result of this study, it was suggested ( delete ) ( concluded ) that sandblast ( delete ) ( sandblasting ) followed by acid etching……. which may lead to( delete ) ( predict a ) good attachment of cells and might increase bone-to-implant contact. References References no. 15 and 16 not mentioned in the main text !? Please can you add the following references to support your current study As a reference no. 12 Abdulla MA, Hasan RH, Al-Hyani OH. Impact of Er,Cr:YSGG laser, sandblast, and acid etching surface modification on surface topography of biodental titanium implants. J Lasers Med Sci. 2023;14:e38. doi:10.34172/jlms.2023.38.(Refer 1) As a reference no. 15 Abdulla MA, Hasan RH, Al-Hyani OH. Radiographic and histologic assessment of osseointegration for surface-treated titanium dental implants: An experimental study in dogs. J Dent Res Dent Clin Dent Prospects, 2024, 18(1), 44-54.doi: 10.34172/joddd.41009(Refer 2) Is the work clearly and accurately presented and does it cite the current literature? Yes Is the study design appropriate and is the work technically sound? Yes Are sufficient details of methods and analysis provided to allow replication by others? Yes If applicable, is the statistical analysis and its interpretation appropriate? Yes Are all the source data underlying the results available to ensure full reproducibility? Yes Are the conclusions drawn adequately supported by the results? Yes References 1. Abdulla MA, Hasan RH, Al-Hyani OH: Impact of Er,Cr:YSGG Laser, Sandblast, and Acid Etching Surface Modification on Surface Topography of Biodental Titanium Implants. J Lasers Med Sci . 2023; 14 : e38 PubMed Abstract | Publisher Full Text 2. Abdulla MA, Hasan RH, Al-Hyani OH: Radiographic and histologic assessment of osseointegration for surface-treated titanium dental implants: An experimental study in dogs. J Dent Res Dent Clin Dent Prospects . 2024; 18 (1): 44-54 PubMed Abstract | Publisher Full Text Competing Interests: No competing interests were disclosed. Reviewer Expertise: Dental Implants, Prosthodontics I confirm that I have read this submission and believe that I have an appropriate level of expertise to confirm that it is of an acceptable scientific standard, however I have significant reservations, as outlined above. Close READ LESS CITE CITE HOW TO CITE THIS REPORT Abdulla MA. Reviewer Report For: Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy [version 1; peer review: 2 approved with reservations] . F1000Research 2025, 14 :216 ( https://doi.org/10.5256/f1000research.175315.r367242 ) The direct URL for this report is: https://f1000research.com/articles/14-216/v1#referee-response-367242 NOTE: it is important to ensure the information in square brackets after the title is included in all citations of this article. COPY CITATION DETAILS Report a concern Respond or Comment COMMENT ON THIS REPORT Comments on this article Comments (0) Version 1 VERSION 1 PUBLISHED 17 Feb 2025 ADD YOUR COMMENT Comment keyboard_arrow_left keyboard_arrow_right Open Peer Review Reviewer Status info_outline Alongside their report, reviewers assign a status to the article: Approved The paper is scientifically sound in its current form and only minor, if any, improvements are suggested Approved with reservations A number of small changes, sometimes more significant revisions are required to address specific details and improve the papers academic merit. Not approved Fundamental flaws in the paper seriously undermine the findings and conclusions Reviewer Reports Invited Reviewers 1 2 Version 1 17 Feb 25 read read Mohammed A Abdulla , University of Mosul, Mosul, Iraq Le Thi Bang , Hanoi University of Science and Technology, Hanoi, Vietnam Comments on this article All Comments (0) Add a comment Sign up for content alerts Sign Up You are now signed up to receive this alert Browse by related subjects keyboard_arrow_left Back to all reports Reviewer Report 0 Views copyright © 2025 Bang L. This is an open access peer review report distributed under the terms of the Creative Commons Attribution License , which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. 14 Mar 2025 | for Version 1 Le Thi Bang , School of Materials Science and Engineering, Hanoi University of Science and Technology, Hanoi, Vietnam 0 Views copyright © 2025 Bang L. This is an open access peer review report distributed under the terms of the Creative Commons Attribution License , which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. format_quote Cite this report speaker_notes Responses (0) Approved With Reservations info_outline Alongside their report, reviewers assign a status to the article: Approved The paper is scientifically sound in its current form and only minor, if any, improvements are suggested Approved with reservations A number of small changes, sometimes more significant revisions are required to address specific details and improve the papers academic merit. Not approved Fundamental flaws in the paper seriously undermine the findings and conclusions The report is on surface modification of titanium in terms of roughening by sandblast and acid etching using various combination of acidic solution. The characterization technique includes SEM, surface roughness and contact angle. Base on the results obtained, it was suggested that combination of HCl and H 2 SO 4 is an effective solution to provide pit and homogeneous texture for the surface. The results from this study reflects purpose of research. However, there are some questions need to be addressed: 1) what are the surface roughness and contact angle of Ti after sandblast, and how do they compare with those of the sample after acid etching? Why is sandblasting needed prior to acid etching? 2) It is not clear from the experimental method whether the treatment of HF is applied before the follow-up treatment in the two acidic solution? If not, please revise the method. 3) What the impacts of using HCl+H2SO4 and HCl+H2SO4+H2O for the titanium surface? 4) the author stated that HF 48% is the proper concentration for a desired surface characteristics but etching with HF prior to etching with HCl + H2SO4 is not recommended, as mentioned in the conclusion. Please clarify this contradiction. 5) Typo error: HCL -->HCl 6) The hydrophilicity and surface roughness of Ti after treatments are not significant between the groups, how did the author drawn a conclusion based only on SEM? Is the work clearly and accurately presented and does it cite the current literature? Yes Is the study design appropriate and is the work technically sound? Yes Are sufficient details of methods and analysis provided to allow replication by others? Yes If applicable, is the statistical analysis and its interpretation appropriate? Not applicable Are all the source data underlying the results available to ensure full reproducibility? Yes Are the conclusions drawn adequately supported by the results? Yes Competing Interests No competing interests were disclosed. Reviewer Expertise Biomaterials, surface modification of metal implants, material engineering I confirm that I have read this submission and believe that I have an appropriate level of expertise to confirm that it is of an acceptable scientific standard, however I have significant reservations, as outlined above. reply Respond to this report Responses (0) Bang LT. Peer Review Report For: Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy [version 1; peer review: 2 approved with reservations] . F1000Research 2025, 14 :216 ( https://doi.org/10.5256/f1000research.175315.r367244) NOTE: it is important to ensure the information in square brackets after the title is included in this citation. The direct URL for this report is: https://f1000research.com/articles/14-216/v1#referee-response-367244 keyboard_arrow_left Back to all reports Reviewer Report 0 Views copyright © 2025 Abdulla M. This is an open access peer review report distributed under the terms of the Creative Commons Attribution License , which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. 03 Mar 2025 | for Version 1 Mohammed A Abdulla , University of Mosul, Mosul, Iraq 0 Views copyright © 2025 Abdulla M. This is an open access peer review report distributed under the terms of the Creative Commons Attribution License , which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. format_quote Cite this report speaker_notes Responses (0) Approved With Reservations info_outline Alongside their report, reviewers assign a status to the article: Approved The paper is scientifically sound in its current form and only minor, if any, improvements are suggested Approved with reservations A number of small changes, sometimes more significant revisions are required to address specific details and improve the papers academic merit. Not approved Fundamental flaws in the paper seriously undermine the findings and conclusions Dear Editor, Thanks for referring to this article for review. The method is well-structured, and the extracted data is informative. There are a few points that I would like the authors to correct before indexed the article. Reviewer Comments for Authors: Dear authors, There are a few points that should be corrected as follows: Title : I think the title needs to be modified: Influence of Acid Composition ( Combination ) on Morphology and Physical Properties of Titanium Alloy Abstract Methods : Please add detailed information about statistical analysis Result : After sandblast ( delete ) ( sandblasting ) and acid etching, the titanium alloy……. Introduction What about the hypothesis ?? Methods An important observation is the lack of a control group that did not get any surface treatment, which would serve as a reference point for comparison!? In paragraph no. 1: The etching process in this research was carried out in two methods, which ( first ) included immersion of titanium in HF at room temperature for 30 seconds followed by immersion in a mixture of HCL and H2SO4 in a ratio of 2:1 at 120 degrees for 5 minutes. and the other ( second )method was immersion of titanium……. In correct Figure 1. (a) Ti-disc specimen blasted with large grit aluminum oxide Al2O3 100μm, 250 μm, and 500 μm. (b) SEM images of Ti after sandblasted with large grit aluminum oxide Al2O3 100 μm, 250 μm, and 500 μm. ( delete ) Correct Figure 1. Ti-disc specimens blasted with large grit aluminum oxide Al2O3 100μm, 250 μm, and 500 μm. Results Number the figures as follows: Figure 2 . SEM images of Ti after sandblasted with large grit aluminum oxide Al2O3 100 μm, 250 μm, and 500 μm. Figure 3 . SEM images of Ti after etching using HF at room temperature for 30 seconds, followed by etching using a mixture of HCL and H2SO4 in a ratio of 2:1 at 120 degrees for 5 minutes. Figure 4 . SEM images of Ti after etching using a mixture of HCL, H2SO4, and H2O in a ratio of 2:1:1 at 120 degrees for 5 minutes. Figure 5. Contact angle evaluation after sandblast and acid etching of Ti-disc specimen. In the paragraphs: Paragraph no. 1, Line no. 1 Figure 1 presents the Ti-disc specimen and ( delete ) Figure 2. presents SEM images after sandblasting with Al2O3 particles. Paragraph no. 4 Based on Table 1, the average roughness of titanium alloy after etching using a combination of HF, HCL, and H2SO4 is higher when compared to using only HCL and H2SO4 and H2O . The titanium alloy specimen has roughness between 1.369 μm – 4.304 μm depending on the size of Al2O3. There is no significant difference in surface roughness between using a combination of HF, HCL, and H2SO4 and only ( delete ) compared with the combination of HCL and H2SO4 without HF. Discussion Paragraph no. 1 The SEM, figure shows ( delete ) ( figures showed ) that the different acids used to.... Paragraph no. 3 In that study it was ( delete ) ( and ) observed that fluoride ions began to Paragraph no. 4 In addition, no reaction ( please explain type of reaction ?) occurs due to the mixing of the two acids. Paragraph no. 5 Etching using HF can also contribute to the release of fluoride ions into the surrounding environment, which can potentially cause cytotoxicity and have negative impacts on cell function and viability ( the authors do not test the cytotoxicity and cell function and viability! This explanation needs references ) Explain the summary of key findings (primary outcome measures, secondary outcome measures, results relating to a hypothesis). What does this study add to the available evidence, what effects on patient benefit ? Future research directions (for this research collaboration, underlying mechanisms, clinical research). The limitations of the study need to be clarified. Conclusion From the result of this study, it was suggested ( delete ) ( concluded ) that sandblast ( delete ) ( sandblasting ) followed by acid etching……. which may lead to( delete ) ( predict a ) good attachment of cells and might increase bone-to-implant contact. References References no. 15 and 16 not mentioned in the main text !? Please can you add the following references to support your current study As a reference no. 12 Abdulla MA, Hasan RH, Al-Hyani OH. Impact of Er,Cr:YSGG laser, sandblast, and acid etching surface modification on surface topography of biodental titanium implants. J Lasers Med Sci. 2023;14:e38. doi:10.34172/jlms.2023.38.(Refer 1) As a reference no. 15 Abdulla MA, Hasan RH, Al-Hyani OH. Radiographic and histologic assessment of osseointegration for surface-treated titanium dental implants: An experimental study in dogs. J Dent Res Dent Clin Dent Prospects, 2024, 18(1), 44-54.doi: 10.34172/joddd.41009(Refer 2) Is the work clearly and accurately presented and does it cite the current literature? Yes Is the study design appropriate and is the work technically sound? Yes Are sufficient details of methods and analysis provided to allow replication by others? Yes If applicable, is the statistical analysis and its interpretation appropriate? Yes Are all the source data underlying the results available to ensure full reproducibility? Yes Are the conclusions drawn adequately supported by the results? Yes References 1. Abdulla MA, Hasan RH, Al-Hyani OH: Impact of Er,Cr:YSGG Laser, Sandblast, and Acid Etching Surface Modification on Surface Topography of Biodental Titanium Implants. J Lasers Med Sci . 2023; 14 : e38 PubMed Abstract | Publisher Full Text 2. Abdulla MA, Hasan RH, Al-Hyani OH: Radiographic and histologic assessment of osseointegration for surface-treated titanium dental implants: An experimental study in dogs. J Dent Res Dent Clin Dent Prospects . 2024; 18 (1): 44-54 PubMed Abstract | Publisher Full Text Competing Interests No competing interests were disclosed. Reviewer Expertise Dental Implants, Prosthodontics I confirm that I have read this submission and believe that I have an appropriate level of expertise to confirm that it is of an acceptable scientific standard, however I have significant reservations, as outlined above. reply Respond to this report Responses (0) Abdulla MA. Peer Review Report For: Influence of Acid Composition on Morphology and Physical Properties of Titanium Alloy [version 1; peer review: 2 approved with reservations] . 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