CN112404452B - 一种镁基磁性微球的制备方法 - Google Patents

一种镁基磁性微球的制备方法 Download PDF

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CN112404452B
CN112404452B CN202011132320.4A CN202011132320A CN112404452B CN 112404452 B CN112404452 B CN 112404452B CN 202011132320 A CN202011132320 A CN 202011132320A CN 112404452 B CN112404452 B CN 112404452B
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梁军浩
贺辛亥
刘明霞
李海燕
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Xian Polytechnic University
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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    • C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel

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Abstract

本发明的一种镁基磁性微球的制备方法，首先将碳纳米管通过化学镀的方法进行磁改性，在碳纳米管表面均匀镀一层5nm～10nm的磁性颗粒，然后将改性后的碳纳米管与镁在一定条件下进行搅拌复合后，得到碳纳米管质量含量5％～10％的镁基复合材料，最后利用金属微滴喷射技术将复合材料在630℃～650℃下喷射成形50μm～100μm的磁性微球。该镁基磁性微球既具有良好的机械强度，又可以利用镁与人体相容性高的特点使制备的磁性微球具有通用性。

Description

一种镁基磁性微球的制备方法
技术领域
本发明属于磁性复合材料技术领域，具体涉及一种镁基磁性微球的制备方法。
背景技术
磁性微球是一种新型的功能材料，在生物医学、细胞学和生物工程学等领域被广泛地应用于生物目标产品的快速分离，在临床医学方面被广泛应用于靶向给药。常见的磁性微球为的基体为高分子材料，高分子材料与身体蛋白容易出现非特异性，很难具有通用性。因此，开发一种金属材料、与身体的相容性非常好磁性微球是十分有必要的。
发明内容
本发明的目的是提供一种镁基磁性微球的制备方法，解决了现有技术中存在的高分子磁性微球与人体蛋白存在非特异性的问题。
本发明所采用的技术方案是，一种镁基磁性微球的制备方法，首先将碳纳米管通过化学镀的方法进行磁改性，即在碳纳米管表面均匀镀一层10nm～20nm厚的磁性颗粒，得到改性后的碳纳米管，然后将改性后的碳纳米管与镁进行搅拌复合后，得到碳纳米管质量含量为5％～10％的镁基复合材料，最后利用金属微滴喷射技术将镁基复合材料在630℃～650℃、SJ-5覆盖剂保护下喷射成形50μm～100μm磁性微球。
本发明的特点还在于：
磁性颗粒为钴、镍及其钴、镍合金或氧化物中的一种。
碳纳米管为多壁碳纳米管、单壁碳纳米管中的一种。
镁为纯镁、AZ31镁合金中任意一种。
搅拌为固态搅拌或半固态搅拌：
半固态搅拌时，在真空度5×104Pa～1×105Pa或RJ-5覆盖剂下，温度为520℃～560℃，搅拌速度1000rpm～1500rpm条件下进行机械搅拌，然后在620℃温度下，浇注至预热200℃的钢模中，取复合材料放入压电式金属微滴喷射装置的坩埚中；
固态搅拌时，在Ar气或CO2+SF6气体保护下进行搅拌摩擦加工，旋转速度800～1200rpm，行进速度20～50mm/min。
其中金属微滴喷射技术为连续式和按需式喷射。
本发明的有益效果是
本发明的一种镁基磁性微球的制备方法，首先将碳纳米管通过化学镀的方法进行磁改性，在碳纳米管表面均匀镀一层5nm～10nm的磁性颗粒，然后将改性后的碳纳米管与镁在一定条件下进行搅拌复合后，得到碳纳米管质量含量5％～10％的镁基复合材料，最后利用金属微滴喷射技术将复合材料在630℃～650℃下喷射成形50μm～100μm的磁性微球。该镁基磁性微球既具有良好的机械强度，又可以利用镁与人体相容性高的特点使制备的磁性微球具有通用性。
具体实施方式
下面结合具体实施方式对本发明进行详细说明。
本发明提供了一种磁吸附局部真空蒸镀的方法，具体包括以下步骤：首先将碳纳米管通过化学镀的方法进行磁改性，在碳纳米管表面均匀镀一层5nm～10nm的磁性颗粒，然后将改性后的碳纳米管与镁在一定条件下进行搅拌复合后，得到碳纳米管质量含量5％～10％的镁基复合材料，最后利用金属微滴喷射技术将复合材料在630℃～650℃下喷射成形50μm～100μm的磁性微球。
半固态搅拌时，在真空度5×104Pa～1×105Pa或RJ-5覆盖剂下，温度为520℃～560℃，搅拌速度1000rpm～1500rpm条件下进行机械搅拌，然后在620℃温度下，浇注至预热200℃的钢模中，取复合材料放入压电式金属微滴喷射装置的坩埚中；
固态搅拌时，在Ar气或CO2+SF6气体保护下进行搅拌摩擦加工，旋转速度800～1200rpm，行进速度20～50mm/min。
实施例1
首先将碳纳米管加入到由CoSO4、NaH2PO2、Pb(NO3)2、Na3C6H5O7组成的镀液中，镀液pH值为5，施镀温度为60℃，施镀时间20分钟，在碳纳米管表面镀一层均匀5nm的钴镀层，将镀钴碳纳米管预埋入纯镁中，在Co2+SF6气体保护下，旋转速度1000rpm，行进速度50mm/min，通过搅拌摩擦工艺进行复合，取复合材料放入压电式金属微滴喷射装置的坩埚中，在630℃、SJ-5覆盖剂保护、沉积距离100mm下，喷射成形50μm-100μm的磁性微球。
实施例2
首先将碳纳米管加入到由NiSO4·6H2O、NaH2PO2·2H2O、NH4Cl、Na3C6H5O7·2H2O和PdCI2组成的镀液中，镀液pH值为7，施镀温度为90℃，施镀时间30分钟，在碳纳米管表面镀一层均匀7nm的钴镀层，将镀镍碳纳米管预埋入AZ31镁合金中，在温度为530℃，在真空度1×105Pa，搅拌速度1000rpm条件下进行机械搅拌，在620℃温度下，浇注至预热200℃的钢模中，取复合材料放入压电式金属微滴喷射装置的坩埚中，在620℃、Ar气保护、沉积距离120mm下，喷射成形50μm-100μm的磁性微球。
实施例2
首先将碳纳米管加入到由NiSO4·6H2O、NaH2PO2·2H2O、NH4Cl、Na3C6H5O7·2H2O和PdCI2组成的镀液中，镀液pH值为8，施镀温度为90℃，施镀时间30分钟，在碳纳米管表面镀一层均匀10nm的钴镍层，将镀镍碳纳米管预埋入AZ31镁合金中，在温度为530℃，在真空度1×105Pa，搅拌速度1000rpm条件下进行机械搅拌，在620℃温度下，浇注至预热200℃的钢模中，取复合材料放入压电式金属微滴喷射装置的坩埚中，在630℃、Ar气保护、沉积距离120mm下，喷射成形50μm-100μm的磁性微球。
实施例3
首先将碳纳米管加入到由NiSO4·6H2O、NaH2PO2·2H2O、NH4Cl、Na3C6H5O7·2H2O和PdCI2组成的镀液中，镀液pH值为8，施镀温度为90℃，施镀时间30分钟，在碳纳米管表面镀一层均匀10nm的镍镀层，将镀镍碳纳米管预埋入AZ31镁合金中，在温度为530℃，添加RJ-5覆盖剂，搅拌速度1300rpm条件下进行机械搅拌；最后在620℃温度下，浇注至预热200℃的钢模中，取复合材料放入压电式金属微滴喷射装置的坩埚中，在630℃、Ar气保护、沉积距离120mm下，喷射成形50μm-100μm的磁性微球。
实施例4
首先将多壁碳纳米管加入到由CoSO4、NaH2PO2、Pb(NO3)2、Na3C6H5O7组成的镀液中，镀液pH值为5，施镀温度为60℃，施镀时间20分钟，在碳纳米管表面镀一层均匀5nm的钴镀层，将镀钴碳纳米管预埋入纯镁中，在Co2+SF6气体保护下，旋转速度800rpm，行进速度20mm/min，通过搅拌摩擦工艺进行复合，取复合材料放入压电式金属微滴喷射装置的坩埚中，在650℃、SJ-5覆盖剂保护、沉积距离100mm下，喷射成形50μm-100μm的磁性微球。
实施例5
首先将单壁碳纳米管加入到由CoSO4、NaH2PO2、Pb(NO3)2、Na3C6H5O7组成的镀液中，镀液pH值为5，施镀温度为60℃，施镀时间20分钟，在碳纳米管表面镀一层均匀5nm的钴镀层，将镀钴碳纳米管预埋入纯镁中，在Co2+SF6气体保护下，旋转速度1200rpm，行进速度50mm/min，通过搅拌摩擦工艺进行复合，取复合材料放入压电式金属微滴喷射装置的坩埚中，在650℃、SJ-5覆盖剂保护、沉积距离100mm下，喷射成形50μm-100μm的磁性微球。
实施例6
首先将单壁碳纳米管加入到由CoSO4、NaH2PO2、Pb(NO3)2、Na3C6H5O7组成的镀液中，镀液pH值为5，施镀温度为60℃，施镀时间20分钟，在碳纳米管表面镀一层均匀5nm的钴镀层，将镀钴碳纳米管预埋入AZ31镁合金中，在温度为560℃，在真空度5×104Pa，搅拌速度1500rpm条件下进行机械搅拌，在620℃温度下，浇注至预热200℃的钢模中，取复合材料放入压电式金属微滴喷射装置的坩埚中，取复合材料放入压电式金属微滴喷射装置的坩埚中，在650℃、SJ-5覆盖剂保护、沉积距离100mm下，喷射成形50μm-100μm的磁性微球。
本发明制备的磁性微球可以应用在靶向药物输送、生物检测和生物分离等众多领域。

Claims (3)

1.一种镁基磁性微球的制备方法，其特征在于：首先将碳纳米管通过化学镀的方法进行磁改性，即在碳纳米管表面均匀镀一层10nm~20nm厚的磁性颗粒，得到改性后的碳纳米管，然后将改性后的碳纳米管与镁进行搅拌复合后，得到碳纳米管质量含量为5%~10%的镁基复合材料，最后利用金属微滴喷射技术将镁基复合材料在630℃~650℃下喷射成形50μm~100μm磁性微球；其中金属微滴喷射技术为连续式和按需式喷射；
所述磁性颗粒为钴、镍及其钴、镍合金或氧化物中的一种；
所述搅拌为固态搅拌或半固态搅拌；
半固态搅拌时，在真空度5×104Pa~1×105Pa或RJ-5覆盖剂下，温度为520℃~560℃，搅拌速度1000 rpm~1500rpm条件下进行机械搅拌，然后在620℃温度下，浇注至预热200℃的钢模中，取复合材料放入压电式金属微滴喷射装置的坩埚中；
固态搅拌时，在Ar气或CO2+SF6气体保护下进行搅拌摩擦加工，旋转速度800~1200 rpm，行进速度20~50mm/min。
2.如权利要求1所述的一种镁基磁性微球的制备方法，其特征在于：所述碳纳米管为多壁碳纳米管、单壁碳纳米管中的一种。
3.如权利要求1所述的一种镁基磁性微球的制备方法，其特征在于：所述镁为纯镁、AZ31镁合金中任意一种。
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