鎳鈦合金表面電沉積羥基磷灰石以及EDTA-2Na的影響
發(fā)布時間：2019-06-02 23:09
【摘要】：鎳鈦合金是一種由鈦和鎳元素等原子構(gòu)成的合金，具有形狀記憶特性和超彈性，在臨床上可用于脊柱側(cè)彎矯正和牙齒矯正，可用于制作血管支架、醫(yī)用導(dǎo)線等。但是鎳鈦合金是一種金屬材料，且鎳本身對身體有毒性，材料生物相容性差。為了將鎳鈦合金優(yōu)良的機(jī)械性能用于醫(yī)學(xué)上，就要對其進(jìn)行生物活化處理。近年來，羥基磷灰石的研究引起了人們廣泛關(guān)注，它是脊椎動物骨骼無機(jī)成分，具有優(yōu)良的生物活性，且可以通過體外化學(xué)合成，使得大量生產(chǎn)成為可能。但是羥基磷灰石機(jī)械性能差，不能用于承重部位。鑒于鎳鈦合金和羥基磷灰石各自具有的長處和不足，人們設(shè)想將兩種材料結(jié)合在一起，以期充分發(fā)揮羥基磷灰石的生物活性和鎳鈦合金的機(jī)械性能。合成的方法有多種，像等離子體噴涂法、凝膠溶膠法、仿生礦化法和電化學(xué)沉積法等。電化學(xué)沉積法由于反應(yīng)條件溫和，周期短，條件易于控制的優(yōu)點(diǎn)得到人們的重視。本文采用的方法就是電化學(xué)沉積法。 本文首先對電化學(xué)沉積法的條件進(jìn)行了探索，分析了電流密度、沉積時間、絡(luò)合劑乙二胺四乙酸二鈉（EDTA-2Na）對電化學(xué)沉積的影響，分析了陽極腐蝕、雙氧水處理和堿熱處理（NaOH）對于提高鎳鈦合金的生物活性的作用。實(shí)驗(yàn)結(jié)果表明：陽極腐蝕可以形成疏松多孔的形貌，有利于擴(kuò)大材料的表面積，有利于羥基磷灰石的礦化；雙氧水處理形成了氧化物層，在鎳鈦合金基底和羥基磷灰石涂層間形成了過渡層，減弱了熱膨脹系數(shù)的差距；堿熱處理在表面形成了能夠誘導(dǎo)羥基磷灰石形核生長的鈦酸鈉（Na2TiO3）；電流密度為1mA/cm2為好，這時單個羥基磷灰石生長的較為充分，對鎳鈦合金基底的覆蓋充分；電沉積時間為一小時為宜，此時單個羥基磷灰石生長充分，對基底的覆蓋較好，沒有出現(xiàn)結(jié)晶；電沉積液中EDTA-2Na的物質(zhì)的量濃度在1.5~2.5×10-4mol/L為好，此時羥基磷灰石致密，對鎳鈦合金基底覆蓋充分，羥基磷灰石間疏松，有間隙，末端盤繞，，這種結(jié)構(gòu)有利于細(xì)胞偽足附著；EDTA-2Na的加入使得羥基磷灰石更為纖細(xì)、致密，它的形貌表現(xiàn)出末端出現(xiàn)聚攏；EDTA-2Na使得所得羥基磷灰石的羥基的峰更為明銳，并有效抑制了碳酸根的生長；EDTA-2Na使得羥基磷灰石生長的緩慢而均勻，在其他實(shí)驗(yàn)條件一致的情況下，對鎳有比對鈦更強(qiáng)的抑制作用；模擬生理液浸泡實(shí)驗(yàn)表明，僅僅經(jīng)過化學(xué)拋光的鎳鈦合金表面僅僅有零星礦化，陽極腐蝕后出現(xiàn)較多的礦化，雙氧水處理后礦化明顯增多，EDTA-2Na的加入使得礦化更為均勻平滑，能譜圖（EDS）表明EDTA-2Na的加入使得礦化速度變慢；成骨細(xì)胞能夠在含有EDTA-2Na的羥基磷灰石涂層表面很好的粘附，說明含有EDTA-2Na的羥基磷灰石涂層具有好的生物活性；拉伸試驗(yàn)結(jié)果表明，EDTA-2Na的加入使得羥基磷灰石與鎳鈦合金基底的結(jié)合強(qiáng)度提高了一倍；腐蝕實(shí)驗(yàn)表明EDTA-2Na的加入能提高涂層的耐腐蝕性；XRD結(jié)果表明EDTA-2Na促使羥基磷灰石沿c軸擇優(yōu)生長。
[Abstract]:The nickel-titanium alloy is an alloy made of atoms such as titanium and nickel elements, has shape memory property and super-elasticity, can be clinically used for scoliosis correction and tooth correction, and can be used for manufacturing a vascular stent, a medical wire, and the like. However, that nickel-titanium alloy is a metal material, and the nickel itself is toxic to the body, and the biocompatibility of the material is poor. In order to use the excellent mechanical properties of the nickel-titanium alloy for medical use, it is subject to a biological activation treatment. In recent years, the research of hydroxyapatite has attracted a wide range of attention, which is an inorganic component of a vertebrate bone, has excellent biological activity, and can be chemically synthesized in vitro, so that a large amount of production becomes possible. However, that mechanical property of the hydroxyapatite cannot be used for the load-bearing part. In view of the advantages and disadvantages of the nickel-titanium alloy and the hydroxyapatite, it is envisaged that the two materials are combined to give full play to the biological activity of the hydroxyapatite and the mechanical properties of the nickel-titanium alloy. There are many methods for synthesis, such as plasma spraying, gel sol, biomimetic mineralization and electrochemical deposition. The electrochemical deposition method has the advantages of mild reaction conditions, short period and easy control of conditions. The method adopted in this paper is the electrochemical deposition method. In this paper, the conditions of the electrochemical deposition method are explored, and the influence of current density, deposition time, complexing agent ethylenediaminetetraacetic acid disodium (EDTA-2Na) on the electrochemical deposition is analyzed, and the corrosion of the anode is analyzed. To improve the biological activity of nickel-titanium alloy by etching, hydrogen peroxide treatment and alkali heat treatment (NaOH) The experimental results show that the corrosion of the anode can form a loose and porous morphology, which is beneficial to the surface area of the material, and is beneficial to the mineralization of the hydroxyapatite. The treatment of the hydrogen peroxide forms an oxide layer, and a transition is formed between the nickel-titanium alloy substrate and the hydroxyapatite coating. And the current density is 1 mA/ cm2. At this time, the growth of the single hydroxyapatite is sufficient, and the covering and filling of the nickel-titanium alloy substrate are carried out. And the concentration of the EDTA-2Na in the electrodeposition solution is between 1.5 and 2.5 to 10-4mol/ L, at the time, the hydroxyapatite is compact and the nickel-titanium alloy base is covered and filled. The hydroxyapatite is more slender and dense with the addition of EDTA-2Na, and the morphology of the hydroxyapatite is more slender and dense, and the appearance of the hydroxyapatite is more and more dense, and the peak of the hydroxyl group of the obtained hydroxyapatite is more clear by the EDTA-2Na. The growth of the carbonate is effectively inhibited, the growth of the carbonate is effectively inhibited, the growth of the hydroxyapatite is slow and uniform by the EDTA-2Na, and the inhibition effect on the nickel is stronger than that of the titanium under the condition that other experimental conditions are consistent; and the experimental table for soaking the physiological fluid is simulated. It is clear that only the surface of the chemically polished nickel-titanium alloy is only sporadically mineralized, and after the corrosion of the anode, the mineralization is more and the mineralization is obviously increased. The addition of the EDTA-2Na makes the mineralization more uniform and smooth, and the energy spectrum graph (EDS) shows that the addition of the EDTA-2Na makes the mineralization speed change. The results of the tensile test show that the bonding strength of the hydroxyapatite and the nickel-titanium alloy substrate is improved by the addition of the EDTA-2Na. The results show that the addition of EDTA-2Na can improve the corrosion resistance of the coating. The results show that the EDTA-2Na promotes the preferential growth of the hydroxyapatite along the c-axis.
【學(xué)位授予單位】：電子科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2012
【分類號】：R318.08
本文編號：2491489
[Abstract]:The nickel-titanium alloy is an alloy made of atoms such as titanium and nickel elements, has shape memory property and super-elasticity, can be clinically used for scoliosis correction and tooth correction, and can be used for manufacturing a vascular stent, a medical wire, and the like. However, that nickel-titanium alloy is a metal material, and the nickel itself is toxic to the body, and the biocompatibility of the material is poor. In order to use the excellent mechanical properties of the nickel-titanium alloy for medical use, it is subject to a biological activation treatment. In recent years, the research of hydroxyapatite has attracted a wide range of attention, which is an inorganic component of a vertebrate bone, has excellent biological activity, and can be chemically synthesized in vitro, so that a large amount of production becomes possible. However, that mechanical property of the hydroxyapatite cannot be used for the load-bearing part. In view of the advantages and disadvantages of the nickel-titanium alloy and the hydroxyapatite, it is envisaged that the two materials are combined to give full play to the biological activity of the hydroxyapatite and the mechanical properties of the nickel-titanium alloy. There are many methods for synthesis, such as plasma spraying, gel sol, biomimetic mineralization and electrochemical deposition. The electrochemical deposition method has the advantages of mild reaction conditions, short period and easy control of conditions. The method adopted in this paper is the electrochemical deposition method. In this paper, the conditions of the electrochemical deposition method are explored, and the influence of current density, deposition time, complexing agent ethylenediaminetetraacetic acid disodium (EDTA-2Na) on the electrochemical deposition is analyzed, and the corrosion of the anode is analyzed. To improve the biological activity of nickel-titanium alloy by etching, hydrogen peroxide treatment and alkali heat treatment (NaOH) The experimental results show that the corrosion of the anode can form a loose and porous morphology, which is beneficial to the surface area of the material, and is beneficial to the mineralization of the hydroxyapatite. The treatment of the hydrogen peroxide forms an oxide layer, and a transition is formed between the nickel-titanium alloy substrate and the hydroxyapatite coating. And the current density is 1 mA/ cm2. At this time, the growth of the single hydroxyapatite is sufficient, and the covering and filling of the nickel-titanium alloy substrate are carried out. And the concentration of the EDTA-2Na in the electrodeposition solution is between 1.5 and 2.5 to 10-4mol/ L, at the time, the hydroxyapatite is compact and the nickel-titanium alloy base is covered and filled. The hydroxyapatite is more slender and dense with the addition of EDTA-2Na, and the morphology of the hydroxyapatite is more slender and dense, and the appearance of the hydroxyapatite is more and more dense, and the peak of the hydroxyl group of the obtained hydroxyapatite is more clear by the EDTA-2Na. The growth of the carbonate is effectively inhibited, the growth of the carbonate is effectively inhibited, the growth of the hydroxyapatite is slow and uniform by the EDTA-2Na, and the inhibition effect on the nickel is stronger than that of the titanium under the condition that other experimental conditions are consistent; and the experimental table for soaking the physiological fluid is simulated. It is clear that only the surface of the chemically polished nickel-titanium alloy is only sporadically mineralized, and after the corrosion of the anode, the mineralization is more and the mineralization is obviously increased. The addition of the EDTA-2Na makes the mineralization more uniform and smooth, and the energy spectrum graph (EDS) shows that the addition of the EDTA-2Na makes the mineralization speed change. The results of the tensile test show that the bonding strength of the hydroxyapatite and the nickel-titanium alloy substrate is improved by the addition of the EDTA-2Na. The results show that the addition of EDTA-2Na can improve the corrosion resistance of the coating. The results show that the EDTA-2Na promotes the preferential growth of the hydroxyapatite along the c-axis.
【學(xué)位授予單位】：電子科技大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2012
【分類號】：R318.08
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