摘要
在 0 .0 1 0 5 mol/L Ca( NO3) 2 ,0 .0 0 63 mol/L NH4 H2 PO4 ,0 .1 mol/L Na NO3,p H=4.6的电解液中 ,控制温度 60～ 2 0 0℃ ,恒电流 0 .4m A/cm2 ,通过水热电沉积法制备羟基磷灰石涂层 .实验结果表明 ,涂层晶体端面呈六边形棒状结构 ,涂层组分为缺钙磷灰石 Ca1 0 - x( HPO4 ) x( PO4 ) 6 - x( OH) 2 - x.经 80 0℃烧结后涂层分解为 HA和 β-TCP的混合物 .随温度升高 ,涂层 n( Ca) /n( P)不断增大 ,涂层组分逐渐接近计量比的HA.涂层质量和结合强度随温度升高先增后减 ,在 1 60℃时达到最大值 1 6.
Hydroxyapatite coatings were formed on titanium electrode by using the hydrothermal electrodeposition method in an autoclave. The electrolyte contained 0.010 5 mol/L Ca(NO_3)_2, 0.006 3 mol/L NH_4H_2PO_4 and 0.1 mol/L NaNO_3. The electrolyte temperature was controlled at 60—200 ℃ and pH value was adjusted at 4.6. After loading of a constant current at 0.4 mA/cm 2 for 2 h, the deposits were characterized by XRD, FTIR, environment scanning electron microscopy and energy dispersive X-ray spectroscopy. The experiment results show that the deposit crystals are rods in shape, the edge face of rod is a defined flat hexagon and the width and length of the crystal rods increases continuously with increasing the electrolyte temperature. The component of coatings is calcium-deficient hydroxyapatite {[Ca_ 10-x(HPO_4)_x(PO_4)_ 6-x}(OH)_ 2-x, 0≤x≤1], which decomposed into the mixture of hydroxyapatite and β-calcium phosphate after sintering at 800 ℃. The n(Ca)/n(P) ratio of the coatings increased and was close at 1.67 with the electrolyte temperature increasing. These results suggest that the component of coating is continuously close to stoichiometric hydroxyapatite with the electrolyte temperature increasing. Furthermore, mass gain of the coatings and bonding strength of coatings increase with electrolyte temperature increasing up to 160 ℃. The bonding strength of coatings after sintering at 800 ℃ for 6 h attained 16.7 MPa when the electrolyte temperature was controlled at 160 ℃.
出处
《高等学校化学学报》
SCIE
EI
CAS
CSCD
北大核心
2004年第2期304-308,共5页
Chemical Journal of Chinese Universities
基金
福建省自然科学基金重大项目 (批准号 :2 0 0 0 F0 0 3 )资助
