CN115466944B - 一种陶瓷材料及其制备方法 - Google Patents

一种陶瓷材料及其制备方法 Download PDF

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CN115466944B
CN115466944B CN202211034680.XA CN202211034680A CN115466944B CN 115466944 B CN115466944 B CN 115466944B CN 202211034680 A CN202211034680 A CN 202211034680A CN 115466944 B CN115466944 B CN 115466944B
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刘国栋
姚磊
曾志军
李宜雄
纪连栋
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Xiangya Hospital of Central South University
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Abstract

本发明涉及一种陶瓷材料及其制备方法。本发明通过溶胶‑凝胶法，在医用不锈钢表面制备二氧化钛陶瓷涂层，而后离子注入硬质元素硼对陶瓷涂层进行封孔处理，在提高其耐腐蚀性能的同时提升涂层材料的硬度。研究表明，离子注入适量的硼元素，可以获得耐腐蚀性能、生物相容性和硬度等综合性能优异的改性涂层材料，该改性涂层可应用于医用止血钳等领域。

Description

一种陶瓷材料及其制备方法
技术领域
本发明涉及陶瓷材料领域，具体涉及一种陶瓷材料及其制备方法。
背景技术
止血钳主要用于钳夹血管或出血点，以达到术中止血的目的，是外科手术中最基本的医疗器械。传统的止血钳由医用不锈钢制备而成，其耐腐蚀性和生物相容性都不甚理想。
中国专利CN202110747833.4采用溶胶-凝胶法在医用镁合金表面制备二氧化钛陶瓷材料，而后选用离子注入稀土元素得到TiO2-Ce-Y复合陶瓷材料，用以提高镁合金的耐腐蚀性能。然而，由于该方法制备而得的陶瓷材料硬度较低，难以满足止血钳等医用器械的使用需求。
发明内容
针对现有技术存在的问题，本发明旨在提供一种陶瓷材料及其制备方法，以获得耐腐蚀性能、生物相容性和硬度等综合性能优异的陶瓷涂层材料。
本发明提供了一种陶瓷材料的制备方法，所述陶瓷材料采用溶胶-凝胶法制备而得，制备过程包括以下步骤：
基体选择：以医用不锈钢为基体材料，通过机械线切割将其切割为预设尺寸；
基体预处理：对医用不锈钢进行脱脂、酸洗、抛光、清洗并烘干待用，其中脱脂选用碳酸氢钠溶液，酸洗选用盐酸溶液，抛光选用包含氧化铝微粒的抛光液，清洗选用去离子水，烘干在氮气下进行；
溶胶-凝胶法制备二氧化钛陶瓷材料：以无水乙醇和蒸馏水为混合溶剂制备钛酸四丁酯前驱体溶液，其中钛酸四丁酯的浓度为0.8-1.0mol/L，无水乙醇与蒸馏水的体积比为1∶1-3，并添加溶液体积的5-10％丙三醇作为增稠剂，陈化20-24h得到溶胶，将上述溶胶旋涂于医用不锈钢表面，旋涂速度为2500-3000转/min，而后在烘箱中干燥，干燥温度为150-160℃；
离子注入元素硼：选用元素硼对二氧化钛陶瓷材料进行离子注入处理，元素硼的注入量为7.2×1010-8.5×1013ions/cm2。
进一步地，本发明还提供了一种陶瓷材料，所述陶瓷材料由上述方法制备而得。
本发明通过溶胶-凝胶法，在医用不锈钢表面制备二氧化钛陶瓷涂层，而后离子注入硬质元素硼对陶瓷涂层进行封孔处理，在提高其耐腐蚀性能的同时提升涂层材料的硬度。研究表明，离子注入适量的硼元素，可以获得耐腐蚀性能、生物相容性和硬度等综合性能优异的改性涂层材料，该改性涂层可应用于医用止血钳等领域。
具体实施方式
下面通过具体实施例来验证本发明的技术效果，但是本发明的实施方式不局限于此。
实施例1
基体选择：以医用不锈钢为基体材料，通过机械线切割将其切割为2cm×2cm×5mm的尺寸；
基体预处理：对医用不锈钢进行脱脂、酸洗、抛光、清洗并烘干待用，其中脱脂选用15％的碳酸氢钠溶液，酸洗选用10％的盐酸溶液，抛光选用包含氧化铝微粒的抛光液，清洗选用去离子水，烘干在氮气下进行；
溶胶-凝胶法制备二氧化钛陶瓷材料：以无水乙醇和蒸馏水为混合溶剂制备钛酸四丁酯前驱体溶液，其中钛酸四丁酯的浓度为0.8mol/L，无水乙醇与蒸馏水的积比为1∶1，并添加溶液体积的5％丙三醇作为增稠剂，陈化24h得到溶胶，将上述溶胶旋涂于医用不锈钢表面，旋涂速度为3000转/min，而后在烘箱中干燥，干燥温度为160℃；
离子注入元素硼：选用元素硼对二氧化钛陶瓷材料进行离子注入处理，元素硼的注入量为7.2×1010ions/cm2。
实施例2
基体选择：以医用不锈钢为基体材料，通过机械线切割将其切割为2cm×2cm×5mm的尺寸；
基体预处理：对医用不锈钢进行脱脂、酸洗、抛光、清洗并烘干待用，其中脱脂选用15％的碳酸氢钠溶液，酸洗选用10％的盐酸溶液，抛光选用包含氧化铝微粒的抛光液，清洗选用去离子水，烘干在氮气下进行；
溶胶-凝胶法制备二氧化钛陶瓷材料：以无水乙醇和蒸馏水为混合溶剂制备钛酸四丁酯前驱体溶液，其中钛酸四丁酯的浓度为0.8mol/L，无水乙醇与蒸馏水的积比为1∶1，并添加溶液体积的5％丙三醇作为增稠剂，陈化24h得到溶胶，将上述溶胶旋涂于医用不锈钢表面，旋涂速度为3000转/min，而后在烘箱中干燥，干燥温度为160℃；
离子注入元素硼：选用元素硼对二氧化钛陶瓷材料进行离子注入处理，元素硼的注入量为9×1011ions/cm2。
实施例3
基体选择：以医用不锈钢为基体材料，通过机械线切割将其切割为2cm×2cm×5mm的尺寸；
基体预处理：对医用不锈钢进行脱脂、酸洗、抛光、清洗并烘干待用，其中脱脂选用15％的碳酸氢钠溶液，酸洗选用10％的盐酸溶液，抛光选用包含氧化铝微粒的抛光液，清洗选用去离子水，烘干在氮气下进行；
溶胶-凝胶法制备二氧化钛陶瓷材料：以无水乙醇和蒸馏水为混合溶剂制备钛酸四丁酯前驱体溶液，其中钛酸四丁酯的浓度为0.8mol/L，无水乙醇与蒸馏水的积比为1∶1，并添加溶液体积的5％丙三醇作为增稠剂，陈化24h得到溶胶，将上述溶胶旋涂于医用不锈钢表面，旋涂速度为3000转/min，而后在烘箱中干燥，干燥温度为160℃；
离子注入元素硼：选用元素硼对二氧化钛陶瓷材料进行离子注入处理，元素硼的注入量为8.5×1012ions/cm2。
实施例4
基体选择：以医用不锈钢为基体材料，通过机械线切割将其切割为2cm×2cm×5mm的尺寸；
基体预处理：对医用不锈钢进行脱脂、酸洗、抛光、清洗并烘干待用，其中脱脂选用15％的碳酸氢钠溶液，酸洗选用10％的盐酸溶液，抛光选用包含氧化铝微粒的抛光液，清洗选用去离子水，烘干在氮气下进行；
溶胶-凝胶法制备二氧化钛陶瓷材料：以无水乙醇和蒸馏水为混合溶剂制备钛酸四丁酯前驱体溶液，其中钛酸四丁酯的浓度为0.8mol/L，无水乙醇与蒸馏水的积比为1∶1，并添加溶液体积的5％丙三醇作为增稠剂，陈化24h得到溶胶，将上述溶胶旋涂于医用不锈钢表面，旋涂速度为3000转/min，而后在烘箱中干燥，干燥温度为160℃；
离子注入元素硼：选用元素硼对二氧化钛陶瓷材料进行离子注入处理，元素硼的注入量为8.5×1013ions/cm2。
对比例1
基材选取：以医用不锈钢作为基材，通过机械线切割将其加工为10cm×6cm×2cm；
基体选择：以医用不锈钢为基体材料，通过机械线切割将其切割为2cm×2cm×5mm的尺寸；
基体预处理：对医用不锈钢进行脱脂、酸洗、抛光、清洗并烘干待用，其中脱脂选用15％的碳酸氢钠溶液，酸洗选用10％的盐酸溶液，抛光选用包含氧化铝微粒的抛光液，清洗选用去离子水，烘干在氮气下进行；
溶胶-凝胶法制备二氧化钛陶瓷材料：以无水乙醇和蒸馏水为混合溶剂制备钛酸四丁酯前驱体溶液，其中钛酸四丁酯的浓度为0.8mol/L，无水乙醇与蒸馏水的积比为1∶1，并添加溶液体积的5％丙三醇作为增稠剂，陈化24h得到溶胶，将上述溶胶旋涂于医用不锈钢表面，旋涂速度为3000转/min，而后在烘箱中干燥，干燥温度为160℃；
离子注入元素硼：选用元素硼对二氧化钛陶瓷材料进行离子注入处理，元素硼的注入量为5×108ions/cm2。
对比例2
基体选择：以医用不锈钢为基体材料，通过机械线切割将其切割为2cm×2cm×5mm的尺寸；
基体预处理：对医用不锈钢进行脱脂、酸洗、抛光、清洗并烘干待用，其中脱脂选用15％的碳酸氢钠溶液，酸洗选用10％的盐酸溶液，抛光选用包含氧化铝微粒的抛光液，清洗选用去离子水，烘干在氮气下进行；
溶胶-凝胶法制备二氧化钛陶瓷材料：以无水乙醇和蒸馏水为混合溶剂制备钛酸四丁酯前驱体溶液，其中钛酸四丁酯的浓度为0.8mol/L，无水乙醇与蒸馏水的积比为1∶1，并添加溶液体积的5％丙三醇作为增稠剂，陈化24h得到溶胶，将上述溶胶旋涂于医用不锈钢表面，旋涂速度为3000转/min，而后在烘箱中干燥，干燥温度为160℃；
离子注入元素硼：选用元素硼对二氧化钛陶瓷材料进行离子注入处理，元素硼的注入量为5×1016ions/cm2。
接下来，我们对实施例1-4和对比例1-2中样品的耐腐蚀性能和生物相容性进行测试，具体如下：
耐腐蚀性能：采用电化学工作站在模拟体液中对各样品进行电化学测试，非工作面用指甲油封闭，在室温环境下进行测试；
生物相容性：通过溶血试验评价各样品的血液相容性，其原理在于：将样品与血液直接接触，测定红细胞膜破裂后释放的血红蛋白量，以检测各样品体外溶血程度。血红蛋白的吸收波长为545nm，可用分光光度计检测其浓度。具体操作步骤如下：
(1)从健康家兔心脏采血100mL，加入2％草酸钾5mL，制成新鲜抗凝血。取抗凝血40mL，加入0.9％氯化钠注射液50mL进行稀释。
(2)取3支硅化试管，一支试管装入试验样品和氯化钠注射液10mL，一支试管空白作为阴性对照组加入氯化钠生理盐水10mL，另外一支试管空白作为阳性对照组分别加入10mL蒸馏水。
(3)所有试管在37℃水浴中恒温30min，分别加入5mL抗凝兔血，并在37℃条件下保温60min。
(4)取试管上层清液，在545nm波长处测定吸光度。每一样品进行三次平行试验并取平均值。
溶血率的计算公式如下：
溶血率(％)＝(试样平均吸光度-阴性组吸光度)/(阳性组吸光度-阴性组吸光度)×100。
各样品的实验结果如表1所示。
表1各样品实验数据
编号 自腐蚀电流密度/μA·cm-2 溶血率/％
实施例1 3.692 1.9
实施例2 2.877 2.4
实施例3 2.014 2.5
实施例4 2.264 3.7
对比例1 12.946 1.5
对比例2 3.140 9.4
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。

Claims (2)

1.一种止血钳用陶瓷材料的制备方法，其特征在于，所述陶瓷材料采用溶胶-凝胶法制备而得，制备过程包括以下步骤：
基体选择：以医用不锈钢为基体材料，通过机械线切割将其切割为2cm×2cm×5mm的尺寸；
基体预处理：对医用不锈钢进行脱脂、酸洗、抛光、清洗并烘干待用，其中脱脂选用15％的碳酸氢钠溶液，酸洗选用10％的盐酸溶液，抛光选用包含氧化铝微粒的抛光液，清洗选用去离子水，烘干在氮气下进行；
溶胶-凝胶法制备二氧化钛陶瓷材料：以无水乙醇和蒸馏水为混合溶剂制备钛酸四丁酯前驱体溶液，其中钛酸四丁酯的浓度为0.8mol/L，无水乙醇与蒸馏水的体积比为1∶1，并添加溶液体积的5％丙三醇作为增稠剂，陈化24h得到溶胶，将上述溶胶旋涂于医用不锈钢表面，旋涂速度为3000转/min，而后在烘箱中干燥，干燥温度为160℃；
离子注入元素硼：选用元素硼对二氧化钛陶瓷材料进行离子注入处理，元素硼的注入量为8.5×1012ions/cm2。
2.一种止血钳用陶瓷材料，其特征在于，所述陶瓷材料由权利要求1所述的方法制备而得。
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