CN104293008B - 一种高硅钢用环保半有机绝缘涂层的制备方法 - Google Patents

一种高硅钢用环保半有机绝缘涂层的制备方法 Download PDF

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CN104293008B
CN104293008B CN201410529293.2A CN201410529293A CN104293008B CN 104293008 B CN104293008 B CN 104293008B CN 201410529293 A CN201410529293 A CN 201410529293A CN 104293008 B CN104293008 B CN 104293008B
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秦镜
杨平
毛卫民
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Abstract

一种高硅钢用环保半有机绝缘涂层的制备方法，属于硅钢绝缘涂层制备技术领域。涂覆前先对高硅钢表面进行预处理，然后配置高硅钢用环保半有机绝缘涂层溶液，以涂层溶液的总质量计，其组分及相应的质量百分比为：苯丙乳液，10%~15%；磷酸二氢铝溶液，20%~30%；甘油，2%~3%；余量为去离子水。最后讲绝缘涂层溶液涂覆在经过预处理后的高硅钢表面，涂覆量控制在0.8g/m2~1.2g/m2，经过固化烧结制得绝缘涂层，烧结温度为200℃~300℃，烧结时间为0.5min~1min。本发明的半有机绝缘涂层适用于高硅钢（含4.5%~6.7%Si的铁硅合金），不含铬等重金属元素，安全环保，具有良好的附着性、绝缘性、耐蚀性、耐热性及冲片性能，能够满足高硅钢相关性能要求。

Description

一种高硅钢用环保半有机绝缘涂层的制备方法
技术领域
本发明涉及一种高硅钢用环保半有机绝缘涂层的制备方法，属于硅钢绝缘涂层制备技术领域。
技术背景
高硅钢(含4.5％～6.7％Si的铁硅合金)比3％普通硅钢电阻率更高，磁致伸缩系数更小，铁损更低，在较高频率下具有优异的软磁性能，在节能降噪等领域具有广泛的应用前景。为了减少高硅钢叠片间的涡流损耗，需要在钢片表面涂一层绝缘膜。目前无取向硅钢表面绝缘涂层主要有无机涂层、有机涂层，半有机涂层三大类。对于硅含量高、硬度大、冲片性低的高硅钢来说，采用无机涂层冲片性能会更差，对冲剪模具磨损更大，表面加工性能不佳。采用有机涂层表面绝缘系数偏低且耐热性不好，而半有机涂层既有无机涂层良好的焊接性和耐热性，又具备有机涂层优良的耐水、冲片润滑和粘附性，具有良好的综合性能。随着欧盟Hors指令的实施，无铬环保涂层的发展和应用已成为国际社会关注的焦点。
尽管目前已有专利“一种无取向硅钢用半无机环保绝缘涂料及其涂层制备方法(CN103013195A)”、“无取向电工钢的无机/半有机绝缘涂层(CN1227860A)”、“一种无取向硅钢用无铬绝缘涂层涂料(CN102433055A)”和“一种有机-无机环保绝缘涂层溶液及其应用(CN102101961A)”、“一种无取向电工钢无铬绝缘涂料(CN101255298A)”和文献“无取向硅钢磷酸盐环保绝缘涂层制备工艺”(北京科技大学学报,2007,29(S2):108.)涉及到以磷酸盐和有机树脂为主要成分的的普通无取向硅钢用环保半有机绝缘涂层的制备及应用，但对于高硅钢来说，国外日本JFE生产的高硅钢仍采用含铬绝缘涂层，国内外尚无高硅钢用环保绝缘涂层及该类涂层在高硅钢表面上应用的报道，因此亟需开发一种高硅钢用无铬环保半有机涂层。由于高硅钢硅含量较普通硅钢(含硅量3％)要高，因此在退火过程中表面更容易被氧化，生成以SiO2为主的内氧化层。氧化层过厚会造成表面绝缘涂层附着性差，容易脱落。因此在涂覆绝缘膜之前，有必要先对高硅钢退火板表面进行预处理，提高涂层的附着性，这方面尚无文献及专利提及。
本专利在普通磷酸盐环保半有机绝缘涂层的基础上，提出一种高硅钢用环保半有机绝缘涂层制备及涂覆前高硅钢表面预处理方法。
发明内容
本发明的目的在于提供一种高硅钢用无铬环保半有机绝缘涂层，解决了铬元素造成的环境污染问题，同时保证了该涂层具有良好的附着性、绝缘性、耐蚀性、耐热性及冲片性能，能够满足高硅钢相关性能要求，并提出一种高硅钢绝缘涂层涂覆前表面预处理方法，处理后的高硅钢再涂半有机绝缘涂层时，涂层附着性好。
一种高硅钢用环保半有机绝缘涂层的制备方法，其特征在于制备步骤如下：
(1)涂覆前先对高硅钢表面进行预处理；
(2)配置高硅钢用环保半有机绝缘涂层溶液，以涂层溶液的总质量计，其组分及相应的质量百分比为：苯丙乳液，10％～15％；磷酸二氢铝溶液，20％～30％；甘油，2％～3％；余量为去离子水；
(3)将绝缘涂层溶液涂覆在经过预处理后的高硅钢表面，涂覆量控制在0.8g/m2～1.2g/m2，经过固化烧结制得绝缘涂层。
上述步骤(1)所述的高硅钢表面进行预处理的方法是先用5％～10％磷酸溶液酸洗，再用尼龙刷研磨，去掉表面氧化物、元素富集层杂质，经过3％～5％氢氟酸溶液酸洗，使SiO2层疏松并露出金属基体，清水洗净烘干。
步骤(2)所述苯丙乳液固含量为40％～45％，pH＝7～8，乳液中颗粒的平均粒度在100nm～150nm之间，所述磷酸二氢铝溶液，由磷酸和氢氧化铝在去离子水中反应制得，质量分数为45％～50％，pH＝0.9～1.1。
步骤(3)所述烧结温度为200℃～300℃，烧结时间为0.5min～1min。
本发明中苯丙乳液能够改善涂层附着性及冲片性，若其含量低，则冲片性能变差，若其含量高，则钢板在去应力退火后，绝缘性和耐热性恶化。
磷酸二氢铝作为涂层的无机部分，具有耐高温、抗震、抗脱落和绝缘性能良好的特点。
甘油能与自由PO43-反应形成稳定的磷酸盐，可抑制涂料烧结后的吸湿性。
本发明适用于退火后表面有铁氧化物及SiO2内氧化层的高硅钢(含4.5％～6.7％Si的铁硅合金)。
本发明的高硅钢用无铬环保半有机绝缘涂层，不但具有较高的层间电阻，同时无铬环保，解决了铬元素造成的环境污染问题，在不添加铬元素的条件下，仍具有良好的附着性、耐蚀性和耐热性。该涂层既具备无机涂层良好的焊接性和耐热性，又具备有机涂层优良的耐水、冲片润滑和粘附性，具有良好的综合性能，能够满足高硅钢相关性能的要求。具有环保绝缘涂层的高硅钢片可应用于高速高频电机、音频和高频变压器中。
具体实施方式
下面结合具体实施例进一步阐述本发明，应理解，这些实施例仅用于说明本发明而不用于限制本发明的保护范围。
对成品退火后的高硅钢(硅含量6.5％)表面先用5％～10％磷酸溶液酸洗，再用尼龙刷研磨，去掉表面氧化物、元素富集层等杂质，经过3％～5％氢氟酸溶液酸洗，使SiO2层疏松并露出金属基体，清水洗净烘干，以上酸溶液浓度均为质量百分比，处理后的表面质量如表1所示。
表1预处理后高硅钢的表面质量
编号 磷酸溶液(质量百分数) 氢氟酸溶液(质量百分数) 处理后的表面质量
实施例1 5％ 5％ 表面光亮、良好
实施例2 8％ 5％ 表面光亮、良好
实施例3 10％ 3％ 表面光亮、良好
实施例4 10％ 5％ 表面光亮、良好
对比例1 4％ 3％ 表面浅灰、较差
对比例2 10％ 8％ 表面略黑、较差
按如表2所示的配方制备出的绝缘涂层溶液涂覆在处理(表1中实施例4)后的高硅钢板上，在250℃～300℃下进行30s-60s固化处理，得到绝缘涂层。
涂层溶液具体制备步骤如下：按表2的配方比例，将相应量的磷酸二氢铝溶液、苯丙乳液和甘油混合，采用磁力搅拌器将混合物搅拌均匀，添加去离子水继续搅拌确保涂料溶液混合均匀，各组分的配方及涂层涂覆量如表2所示(余量为去离子水)：
表2涂层溶液成分的组成及涂覆量
注：余量为去离子水(质量百分比)。
实施例1～12中使用的磷酸二氢铝溶液，由磷酸和氢氧化铝在去离子水中反应制得，质量分数为45％～50％，pH＝0.9～1.1。
实施例1～12中使用的苯丙乳液，是以去离子水为溶剂，采用缓慢均匀滴加单体的方法，将苯乙烯、丙烯酸丁酯及丙烯酸在引发剂存在下进行共聚制得。固含量为40％～45％，pH＝7～8，乳液中颗粒的平均粒度在100nm～150nm之间。
对比例1～3与实施例1～12中使用的苯丙乳液、磷酸二氢铝溶液、甘油为同一批原料。
表3是表示按表1的配方和方法制备的涂层的各种性能。涂层外观评价通过肉眼观察判断，由于高硅钢室温塑性差、硬脆且不易弯曲，涂层附着性按照GB/T9286-1998来评定涂层的附着性。涂层硬度按照GB/T6739-2006在QHQ型铅笔划痕硬度仪上进行测试。层间电阻按照GB/T2522-2007规定的方法测定。其中，各项特性涂层性能良好时用☆表示，一般用△表示，差用×表示。
表3涂层性能的比较
从表3可知，随着涂覆量的增加，涂层附着性变差，硬度值降低，而层间电阻不断增大。当每面涂覆量超过0.7g/m2时，层间电阻保持在5Ω·cm2/片以上，表明本试验制备的半有机涂层具有优良的绝缘性，满足高硅钢叠片间对绝缘性能的要求。虽然增加涂覆量可以提高绝缘性能，但是附着性、硬度、焊接性能会降低，同时也会降低铁芯的叠片系数，因此涂覆量需控制在合理的范围内，综合各方面因素考虑，将涂层每面涂覆量控制在0.8g/m2～1.2g/m2。

Claims (3)

1.一种高硅钢用环保半有机绝缘涂层的制备方法，其特征在于制备步骤如下：
(1)涂覆前先对高硅钢表面进行预处理；
(2)配置高硅钢用环保半有机绝缘涂层溶液，以涂层溶液的总质量计，其组分及相应的质量百分比为：苯丙乳液，10％～15％；磷酸二氢铝溶液，20％～30％；甘油，2％～3％；余量为去离子水；
(3)将绝缘涂层溶液涂覆在经过预处理后的高硅钢表面，涂覆量控制在0.8g/m2～1.2g/m2，经过固化烧结制得绝缘涂层；
步骤(1)所述的高硅钢表面进行预处理的方法是先用5％～10％磷酸溶液酸洗，再用尼龙刷研磨，去掉表面氧化物、元素富集层杂质，经过3％～5％氢氟酸溶液酸洗，使SiO2层疏松并露出金属基体，清水洗净烘干。
2.如权利要求1所述一种高硅钢用环保半有机绝缘涂层的制备方法，其特征在于，所述苯丙乳液固含量为40％～45％，pH＝7～8，乳液中颗粒的平均粒度在100nm～150nm之间，所述磷酸二氢铝溶液，由磷酸和氢氧化铝在去离子水中反应制得，质量百分数为45％～50％，pH＝0.9～1.1。
3.如权利要求1所述一种高硅钢用环保半有机绝缘涂层的制备方法，其特征在于，步骤(3)所述固化烧结温度为200℃～300℃，烧结时间为0.5min～1min。
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