CN105624699A - 钕铁硼永磁体的表面处理方法 - Google Patents

钕铁硼永磁体的表面处理方法 Download PDF

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CN105624699A
CN105624699A CN201511005904.4A CN201511005904A CN105624699A CN 105624699 A CN105624699 A CN 105624699A CN 201511005904 A CN201511005904 A CN 201511005904A CN 105624699 A CN105624699 A CN 105624699A
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徐力
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Abstract

本发明公开了一种钕铁硼永磁体的表面处理方法，依次包括预处理、形成结晶层、钝化、封皮、冷热处理等步骤。该表面处理方法经过优化，所用材料均为市场上常见的材料，摒弃了传统处理方法中不易得到和较为昂贵的材料，重点通过优化工艺步骤和技术参数而得到，从而成本较低，且易于掌握。同时，方法中包含有高低温处理的方式，进一步提升了表面层的晶体布局和密度。经实验验证，经该方法处理的钕铁硼永磁体具有较佳的防腐蚀能力。

Description

钕铁硼永磁体的表面处理方法
技术领域
本发明涉及永磁体技术领域，尤其是涉及一种钕铁硼永磁体的表面处理方法。
背景技术
钕铁硼永磁体属于第三代稀土永磁材料，具有体积小、重量轻和磁性强的特点，是目前性能价格比最佳的磁体，在磁学界被誉为磁王。高能量密度的优点使钕铁硼永磁材料在现代工业和电子技术中获得了广泛的应用。在裸磁的状态下，磁力可达到3500高斯左右。预计在未来20年里，不太可能有替代钕铁硼永磁体的磁性材料出现。生产钕铁硼永磁体的主要原材料有稀土金属钕、稀土金属镨、纯铁、铝、硼铁合金以及其他稀土原料。
然而，钕铁硼永磁体在制备中必须进行表面处理，否则防腐能力较差。
发明内容
本发明的目的是提供一种钕铁硼永磁体的表面处理方法，它具有工艺易于掌握，且效果较佳的特点。
本发明所采用的技术方案是：钕铁硼永磁体的表面处理方法，依次包括以下步骤：
(1)预处理：在钕铁硼永磁体表面依次采用去离子水清洗2～3min、采用等重量比的浓度为3～6％的稀硝酸和浓度为2～3％的盐酸的混合液体浸泡60～80s、采用浓度为3～5％的乙酸浸泡3～4min、采用用5-8％的稀硫酸活化处理30～40s、采用浓度为3～5％的乙酸浸泡3～4min；
(2)形成结晶层：将预处理过的钕铁硼永磁体放入处理液中浸泡6～8min，然后在空气中晾干，其中，以重量份计，处理液为：磷酸80～82份，去离子水6～8份，表面活性剂0.1份，草酸0.6份以及缓蚀剂0.5份，且浸泡温度为38～41℃，磷酸、草酸均为工业级纯度；
(3)钝化：将钕铁硼永磁体浸渍在体积浓度为40～120ml/L、温度为室温的1，2-双(三乙氧基硅基)乙烷水溶液中，进行初步钝化10～15min，将初步钝化的钕铁硼永磁体用去离子水清洗后晾干，放入具有质量浓度为6～8g/L的硝酸铈、质量浓度为2～5g/L的硝酸钕的水溶液中进行再次钝化，再次钝化的温度为室温、钝化时间为10～15min，之后，室温晾干；
(4)封皮：采用物理气相沉积处理的方式形成沉积膜，其中，靶功率为300～1000W，气压为0.3～1.0Pa，物理气相沉积膜的厚度为5～10um；
(5)冷热处理：将封皮后的钕铁硼永磁体放置于60～80℃的热水内持续10～20min，然后在2min内放至冰水混合液内持续10～20min，取出后自然放至室温。
本发明和现有技术相比所具有的优点是：工艺易于掌握，且效果较佳。本发明的钕铁硼永磁体的表面处理方法经过优化，所用材料均为市场上常见的材料，摒弃了传统处理方法中不易得到和较为昂贵的材料，重点通过优化工艺步骤和技术参数而得到，从而成本较低，且易于掌握。同时，方法中包含有高低温处理的方式，进一步提升了表面层的晶体布局和密度。经实验验证，经该方法处理的钕铁硼永磁体具有较佳的防腐蚀能力。
具体实施方式
实施例1
钕铁硼永磁体的表面处理方法，依次包括以下步骤：
(1)预处理：在钕铁硼永磁体表面依次采用去离子水清洗2min、采用等重量比的浓度为3％的稀硝酸和浓度为2％的盐酸的混合液体浸泡60s、采用浓度为3％的乙酸浸泡3min、采用5％的稀硫酸活化处理30s、采用浓度为3％的乙酸浸泡3min；
(2)形成结晶层：将预处理过的钕铁硼永磁体放入处理液中浸泡6min，然后在空气中晾干。其中，以重量份计，处理液为：磷酸80份，去离子水6份，表面活性剂0.1份，草酸0.6份以及缓蚀剂0.5份，且浸泡温度为38℃。磷酸、草酸均为工业级纯度。
(3)钝化：将钕铁硼永磁体浸渍在体积浓度为40ml/L、温度为室温的1，2-双(三乙氧基硅基)乙烷水溶液中，进行初步钝化10min，将初步钝化的钕铁硼永磁体用去离子水清洗后晾干，放入具有质量浓度为6g/L的硝酸铈、质量浓度为2g/L的硝酸钕的水溶液中进行再次钝化，再次钝化的温度为室温、钝化时间为10min，之后，室温晾干。
(4)封皮：采用物理气相沉积处理的方式形成沉积膜，其中，靶功率为300W，气压为0.3Pa，物理气相沉积膜的厚度为5um，积膜材料优选采用氮化钛膜。
(5)冷热处理：将封皮后的钕铁硼永磁体放置于60℃的热水内持续10min，然后在2min内放至0℃的冰水内持续10min，取出后自然放至室温。
按照GB/T10125-1997规定分别对处理后的钕铁硼永磁体进行耐中性盐雾试验测试，固化处理后的钕铁硼磁体的经受时间为400小时，说明耐腐蚀能力较佳。
实施例2
钕铁硼永磁体的表面处理方法，依次包括以下步骤：
(1)预处理：在钕铁硼永磁体表面依次采用去离子水清洗2.5min、采用等重量比的浓度为4％的稀硝酸和浓度为2.5％的盐酸的混合液体浸泡70s、采用浓度为4％的乙酸浸泡3.5min、采用6％的稀硫酸活化处理35s、采用浓度为4％的乙酸浸泡3.5min；
(2)形成结晶层：将预处理过的钕铁硼永磁体放入处理液中浸泡7min，然后在空气中晾干。其中，以重量份计，处理液为：磷酸81份，去离子水7份，表面活性剂0.1份，草酸0.6份以及缓蚀剂0.5份，且浸泡温度为39℃，磷酸、草酸均为工业级纯度。
(3)钝化：将钕铁硼永磁体浸渍在体积浓度为70ml/L、温度为室温的1，2-双(三乙氧基硅基)乙烷水溶液中，进行初步钝化12min，将初步钝化的钕铁硼永磁体用去离子水清洗后晾干，放入具有质量浓度为7g/L的硝酸铈、质量浓度为4g/L的硝酸钕的水溶液中进行再次钝化，再次钝化的温度为室温、钝化时间为12min，之后，室温晾干。
(4)封皮：采用物理气相沉积处理的方式形成沉积膜，其中，靶功率为800W，气压为0.6Pa，物理气相沉积膜的厚度为7um。积膜材料优选采用氮化钛膜。
(5)冷热处理：将封皮后的钕铁硼永磁体放置于70℃的热水内持续15min，然后在2min内放至0℃的冰水内持续15min，取出后自然放至室温。
按照GB/T10125-1997规定分别对处理后的钕铁硼永磁体进行耐中性盐雾试验测试，固化处理后的钕铁硼磁体的经受时间为420小时。说明耐腐蚀能力较佳。
实施例3
钕铁硼永磁体的表面处理方法，依次包括以下步骤：
(1)预处理：在钕铁硼永磁体表面依次采用去离子水清洗3min、采用等重量比的浓度为6％的稀硝酸和浓度为3％的盐酸的混合液体浸泡80s、采用浓度为5％的乙酸浸泡4min、采用8％的稀硫酸活化处理40s、采用浓度为5％的乙酸浸泡4min；
(2)形成结晶层：将预处理过的钕铁硼永磁体放入处理液中浸泡8min，然后在空气中晾干。其中，以重量份计，处理液为：磷酸82份，去离子水8份，表面活性剂0.1份，草酸0.6份以及缓蚀剂0.5份，且浸泡温度为41℃，磷酸、草酸均为工业级纯度。
(3)钝化：将钕铁硼永磁体浸渍在体积浓度为120ml/L、温度为室温的1，2-双(三乙氧基硅基)乙烷水溶液中，进行初步钝化15min，将初步钝化的钕铁硼永磁体用去离子水清洗后晾干，放入具有质量浓度为8g/L的硝酸铈、质量浓度为5g/L的硝酸钕的水溶液中进行再次钝化，再次钝化的温度为室温、钝化时间为15min，之后，室温晾干。
(4)封皮：采用物理气相沉积处理的方式形成沉积膜，其中，靶功率为1000W，气压为1Pa，物理气相沉积膜的厚度为10um。积膜材料优选采用氮化钛膜。
(5)冷热处理：将封皮后的钕铁硼永磁体放置于80℃的热水内持续20min，然后在2min内放至0℃的冰水内持续15min，取出后自然放至室温。
按照GB/T10125-1997规定分别对处理后的钕铁硼永磁体进行耐中性盐雾试验测试，固化处理后的钕铁硼磁体的经受时间为410小时。说明耐腐蚀能力较佳。
以上所述仅为本发明的优选实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (1)

1.钕铁硼永磁体的表面处理方法，依次包括以下步骤：
(1)预处理：在钕铁硼永磁体表面依次采用去离子水清洗2～3min、采用等重量比的浓度为3～6％的稀硝酸和浓度为2～3％的盐酸的混合液体浸泡60～80s、采用浓度为3～5％的乙酸浸泡3～4min、采用用5-8％的稀硫酸活化处理30～40s、采用浓度为3～5％的乙酸浸泡3～4min；
(2)形成结晶层：将预处理过的钕铁硼永磁体放入处理液中浸泡6～8min，然后在空气中晾干，其中，以重量份计，处理液为：磷酸80～82份，去离子水6～8份，表面活性剂0.1份，草酸0.6份以及缓蚀剂0.5份，且浸泡温度为38～41℃，磷酸、草酸均为工业级纯度；
(3)钝化：将钕铁硼永磁体浸渍在体积浓度为40～120ml/L、温度为室温的1，2-双(三乙氧基硅基)乙烷水溶液中，进行初步钝化10～15min，将初步钝化的钕铁硼永磁体用去离子水清洗后晾干，放入具有质量浓度为6～8g/L的硝酸铈、质量浓度为2～5g/L的硝酸钕的水溶液中进行再次钝化，再次钝化的温度为室温、钝化时间为10～15min，之后，室温晾干；
(4)封皮：采用物理气相沉积处理的方式形成沉积膜，其中，靶功率为300～1000W，气压为0.3～1.0Pa，物理气相沉积膜的厚度为5～10um；
(5)冷热处理：将封皮后的钕铁硼永磁体放置于60～80℃的热水内持续10～20min，然后在2min内放至冰水混合液内持续10～20min，取出后自然放至室温。
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