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采用调制电化学沉积法在钛合金上制备附着型磷酸八钙涂层。

Adherent octacalciumphosphate coating on titanium alloy using modulated electrochemical deposition method.

作者信息

Lin Shujie, LeGeros Racquel Z, LeGeros John P

机构信息

Department of Biomaterials and Biomimetics, New York University College of Dentistry, 345 East 24th Street, New York, NY 10010, USA.

出版信息

J Biomed Mater Res A. 2003 Sep 15;66(4):819-28. doi: 10.1002/jbm.a.10072.

Abstract

Our aims in this study were (1) to develop an electrochemical method of depositing adherent octacalciumphosphate (OCP) and other calcium phosphate coatings on titanium alloy (Ti6Al4V) substrates of different shapes and surface preparations, (2) to determine the properties of the coating (composition, morphology, thickness, dissolution), and (3) to observe transformation of OCP to carbonatehydroxyapatite (CHA) in simulated body fluid (SBF). Titanium (Ti)-alloy plates, tensile bars with four types of surfaces (grit-blasted with apatitic abrasive, chemically textured, arc-deposited, and Co-Cr-beaded) and dissolution cylinders were electrochemically coated with the use of modulated pulse time electric fields programmed with a custom-made dual microprocessor. Modulated electrochemical deposition (MECD) was carried out with pH and temperature conditions favorable for OCP formation. Coatings were characterized using X-ray diffraction, FT-IR, scanning electron microscopy, tensile strength tests, and solubility tests. XRD and FT-IR analyses showed that pure, uniform OCP coatings were produced on Ti6Al4V surfaces with coating-to-substrate tensile strengths greater than 7,000 psi. Coatings on Ti arc-deposited surfaces, chemically textured surfaces, and Co-Cr-beaded surfaces all gave tensile strengths ranging from 5,000 to 7,000 psi, with no coating shadows in the crevices. Dissolution of OCP coating in 100 mL of 0.1 M Tris buffer solution was determined from the amount of calcium (Ca) released onto the buffer, which was 7.7 +/- 1.0 ppm Ca at pH 7.3 after 4 h, and 22 -/+ 1.4 ppm Ca at pH 3 after 2 h. We found that OCP crystal size can be controlled by the current density and relative pulse time modulation. Our study demonstrated the following: (1) Highly adherent calcium phosphate (e.g., OCP) coating of uniform compositions (e.g., OCP) on Ti-alloy substrates can be obtained at low temperatures with the use of MECD by optimizing pulse time modulation of the electric field, reaction pH, temperature, and electrolyte composition; and (2) OCP readily transforms to CHA when exposed to SBF.

摘要

本研究的目的是

(1)开发一种电化学方法,用于在不同形状和表面处理的钛合金(Ti6Al4V)基底上沉积附着的磷酸八钙(OCP)和其他磷酸钙涂层;(2)确定涂层的性能(组成、形态、厚度、溶解性);(3)观察在模拟体液(SBF)中OCP向碳酸羟基磷灰石(CHA)的转变。使用定制的双微处理器编程的调制脉冲时间电场,对钛(Ti)合金板、具有四种表面类型(用磷灰石磨料喷砂、化学织构化、电弧沉积和钴铬珠化)的拉伸棒以及溶解圆柱体进行电化学涂层处理。在有利于OCP形成的pH和温度条件下进行调制电化学沉积(MECD)。使用X射线衍射、傅里叶变换红外光谱、扫描电子显微镜、拉伸强度测试和溶解性测试对涂层进行表征。XRD和FT-IR分析表明,在Ti6Al4V表面制备出了纯净、均匀的OCP涂层,涂层与基底之间的拉伸强度大于7000 psi。在Ti电弧沉积表面、化学织构化表面和钴铬珠化表面的涂层,其拉伸强度均在5000至7000 psi之间,缝隙中无涂层阴影。通过测定缓冲液中释放的钙(Ca)量来确定OCP涂层在100 mL 0.1 M Tris缓冲溶液中的溶解情况,4小时后在pH 7.3时为7.7±1.0 ppm Ca,2小时后在pH 3时为22±1.4 ppm Ca。我们发现,OCP晶体尺寸可通过电流密度和相对脉冲时间调制来控制。我们的研究表明:(1)通过优化电场的脉冲时间调制、反应pH、温度和电解质组成,利用MECD可在低温下在Ti合金基底上获得组成均匀(如OCP)的高附着力磷酸钙(如OCP)涂层;(2)OCP暴露于SBF时容易转变为CHA。

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