CN114974871B - 高电阻率烧结稀土永磁体的制备方法及其设备 - Google Patents
高电阻率烧结稀土永磁体的制备方法及其设备 Download PDFInfo
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Abstract
本发明涉及烧结稀土永磁体的制备方法，具体为一种高电阻率烧结稀土永磁体的制备方法及其设备。所述制备方法包括如下步骤：S1、制备稀土永磁粉末；S2、在低氧环境下，对稀土永磁粉末进行取向压制，退磁，制成生坯；其中取向磁场方向与压制压力方向垂直；S3、将生坯切割成薄片，其中切割面垂直于压制压力方向；S4、将各薄片表面包覆绝缘层；S5、若干包覆绝缘层的薄片以切割面相互接触且取向方向一致的姿态摞起来，放入热压模具，进行热压烧结，即在烧结的同时对热压模具内摞起来的薄片施加垂直于切割面的压力。通过热压烧结以增加夹层结构的高电阻率烧结稀土永磁体层间强度，避免出现层间分离。
Description
技术领域
本发明涉及烧结稀土永磁体的制备方法及设备，具体为一种高电阻率烧结稀土永磁体的制备方法及其设备。
背景技术
烧结稀土永磁体，特别是R-Fe-B 系烧结永磁体属于金属磁体，电阻低，应用于旋转电 机存在涡流损失大的问题。
为提高烧结稀土永磁体的电阻率，专利号为201410356469 .9的中国专利公开了一种高电阻率稀土铁系R-Fe-B 磁体的制备方法，包括将原料磁体制成磁体粉末的步骤一、将磁体粉末进行取向压型得到压坯的步骤二以及将压坯置入真空烧结炉内烧结获得烧结磁体的步骤三，其特征在于，在进行步骤二的过程中，先向模腔中装入磁粉层，再向该磁粉层的表面装入氧化物或氟化物等的微粉层，如此往复地装料完毕后再进行常规的取向压制；所述高电阻率稀土铁系R-Fe-B 磁体，其由若干层稀土铁系的磁粉与若干薄层氧化物或氟化物的微粉交替填充压合构成的夹层结构，所述夹层结构的主结构层为磁粉层；所述微粉薄层为稀土元素、Al、Zr、Ti、Nb、Hf或半导体元素的氧化物或者氟化物。该现有技术制得的夹层结构的永磁体层间强度低，易出现层间分离（俗称“千层饼”现象），影响了产品的推广应用。
发明内容
本发明解决现有夹层结构的高电阻率烧结稀土永磁体层间强度低，易出现层间分离的问题，提供一种高电阻率烧结稀土永磁体的制备方法及其设备。
本发明是采用如下技术方案实现的：高电阻率烧结稀土永磁体的制备方法，包括如下步骤：
S1、制备稀土永磁粉末；
S2、在低氧环境下，对稀土永磁粉末进行取向压制，退磁，制成生坯；其中取向磁场方向与压制压力方向垂直；
S3、将生坯切割成薄片，其中切割面垂直于压制压力方向（即切割后，生坯在压制压力方向是多层结构）；
S4、将各薄片表面包覆绝缘层；
S5、若干包覆绝缘层的薄片以切割面相互接触且取向方向一致的姿态摞起来，放入热压模具，进行热压烧结，即在烧结的同时对热压模具内摞起来的薄片施加垂直于切割面的压力。
通过热压烧结（传统的烧结稀土永磁体或现有夹层结构的高电阻率烧结稀土永磁体，在烧结时是不加压的）以增加夹层结构的高电阻率烧结稀土永磁体层间强度，避免出现层间分离；同时生坯切片能提高加工效率。
本发明的另一种技术方案：高电阻率烧结稀土永磁体的制备方法，包括如下步骤：
S1、制备稀土永磁粉末；
S2、在低氧环境下，对稀土永磁粉末进行取向压制，退磁，制成生坯薄片；其中取向磁场方向与压制压力方向垂直；
S3、将各生坯薄片表面包覆绝缘层；
S4、若干包覆绝缘层的生坯薄片以被压制面（垂直于压制压力方向的承压表面）相互接触且取向方向一致的姿态摞起来，放入热压模具，进行热压烧结，即在烧结的同时对热压模具内摞起来的生坯薄片施加垂直于被压制面的压力。
单独取向压制生坯薄片并通过热压烧结以增加夹层结构的高电阻率烧结稀土永磁体层间强度，避免出现层间分离。
本发明的再一种技术方案：高电阻率烧结稀土永磁体的制备方法，包括如下步骤：
S1、制备稀土永磁粉末；
S2、先向模腔内加入稀土永磁粉末，在低氧环境下对稀土永磁粉末进行取向压制，退磁，在模腔内制成生坯薄片，然后向模腔内加入（撒或喷）绝缘粉末从而在生坯薄片上表面形成绝缘层，再次向模腔内加入稀土永磁粉末并在低氧环境下对再次加入的稀土永磁粉末进行取向压制，退磁，重复上述过程，直至到达所需的高度尺寸后脱模，得到生坯薄片和绝缘层交替的生坯；其中取向磁场方向与压制压力方向垂直；
S3、将生坯薄片和绝缘层交替的生坯放入热压模具，进行热压烧结，即在烧结的同时对热压模具内的生坯施加垂直于取向方向的压力。
对先加入的稀土永磁粉末进行取向压制及退磁后，再加入绝缘粉末，使得绝缘层与生坯薄片的接触面平整、均匀，有利于提高层间结合力；再通过热压烧结以增加夹层结构的高电阻率烧结稀土永磁体层间强度，避免出现层间分离。
本发明所述的制备方法适用于钕铁硼、钐钴、钐铁氮。
附图说明
图1为实现实施二所述制备方法的设备中磁场压机的结构示意图；
图2为图1的局部放大图；
图3为实现实施二所述制备方法的设备中热压烧结机的结构示意图；
图4为图3的局部放大图；
图5为实现实施三所述制备方法的设备的结构示意图。
图中：1-模具，2-上模冲，3-下模冲，4-加料导板，5-磁粉加料筒，6-绝缘粉加料筒，7-感应加热线圈，8-皮带轮，9-皮带。
具体实施方式
实施例一
高电阻率烧结稀土永磁体的制备方法，包括如下步骤：
S1、制备稀土永磁粉末；
S2、在低氧环境下，对稀土永磁粉末进行取向压制，退磁，制成生坯；其中取向磁场方向与压制压力方向垂直；
S3、将生坯切割成薄片，其中切割面垂直于压制压力方向（即切割后，生坯在压制压力方向是多层结构）；
S4、将各薄片表面包覆绝缘层；
S5、若干包覆绝缘层的薄片以切割面相互接触且取向方向一致的姿态摞起来，放入热压模具，进行热压烧结，即在烧结的同时对热压模具内摞起来的薄片施加垂直于切割面的压力。
具体实施时，绝缘层材料采用熔化温度400-900度的低温陶瓷粉末或低温玻璃粉末或稀土氯化物，或其中任两种任意比例的混合物；低温陶瓷粉末、低温玻璃粉末、稀土氯化物属于低熔点盐类，受热不分解，不溶于水，高电阻率，热压时能把相邻薄片粘接在一起，进一步提高层间结合强度。薄片表面包覆绝缘层具体可采用涂敷或丝网印刷的方式，即将低温陶瓷粉末、低温玻璃粉末、稀土氯化物的粉末（粒度在0.5微米-10微米）溶于液体或溶剂制成悬浮液，然后进行涂敷或丝网印刷。薄片厚度0.5-10毫米（根据几何形状及工作频率确定厚度）。绝缘层10-50微米。热压烧结采用中频感应加热，烧结温度700度-1100度，压力30-100MPa。为增加切割成薄片的成品率，在步骤S3进行生坯切割薄片之前，对步骤S2得到的生坯进行等静压，以增加生坯的密度，确保可靠切割。热压烧结在充满氩气的密封舱内进行，氧含量低于50ppm。按照常规技术，将步骤S4的包覆绝缘层的薄片摆入托盘并装入真空炉，进行低温脱气，中温脱脂、脱氢，然后再进行步骤S5。步骤S5后再进行900度、600度二级时效得到产品；产品外层采用电泳、涂敷高分子有机物以防氧化。
该制备方法适用于钕铁硼、钐钴、钐铁氮。
实例：把常规方法制备的钕铁硼永磁粉末，3.8Kg填入模具，加1.6T磁场压制出80*80*150（长方体状）的生坯。等静压后，切割成厚度2mm的薄片。涂20微米厚的玻璃和氯化铈悬浮液，液体（溶剂）是聚异丁烯融入120号汽油。进行800度真空脱脂、脱气4小时。将所得全部薄片摞起来并在50MPa、950度下热压烧结；900度、600度二级时效。所得夹层结构的钕铁硼永磁体层间结合强度高，整个磁体结构浑然一体。测电阻为1.4欧姆（上下二面间电阻1.4欧姆）；剩磁13.8（没有加绝缘层的剩磁是14.5，降低了700Gs），矫顽力17.5KOe（几乎没有变化）。电阻率是0.42Ωm（欧姆米），没有加绝缘层的电阻率是0.73毫欧姆米，电阻率提高近3个数量级。
实施例二
高电阻率烧结稀土永磁体的制备方法，包括如下步骤：
S1、制备稀土永磁粉末；
S2、先向模腔内加入稀土永磁粉末，在低氧环境下对稀土永磁粉末进行取向压制，退磁，在模腔内制成生坯薄片，然后向模腔内加入（撒或喷）绝缘粉末从而在生坯薄片上表面形成绝缘层，再次向模腔内加入稀土永磁粉末并在低氧环境下对再次加入的稀土永磁粉末进行取向压制，退磁，重复上述过程，直至到达所需的高度尺寸后脱模，得到生坯薄片和绝缘层交替的生坯；其中取向磁场方向与压制压力方向垂直；
S3、将生坯薄片和绝缘层交替的生坯放入热压模具，进行热压烧结，即在烧结的同时对热压模具内的生坯施加垂直于取向方向的压力。
具体实施时，绝缘层材料采用熔化温度400-900度的低温陶瓷粉末或低温玻璃粉末或稀土氯化物，或其中任两种任意比例的混合物；低温陶瓷粉末、低温玻璃粉末、稀土氯化物属于低熔点盐类，受热不分解，不溶于水，高电阻率，热压时能把相邻生坯薄片粘接在一起，进一步提高层间结合强度。绝缘层具体可采用撒或喷（通过惰性气体喷枪喷入）的方式，即将低温陶瓷粉末、低温玻璃粉末、稀土氯化物的粉末（粒度在0.5微米-10微米）撒或喷于生坯薄片上表面。生坯薄片厚度0.5-10毫米（根据几何形状及工作频率确定厚度）。（压制后的）绝缘层10-50微米。热压烧结采用中频感应加热，烧结温度700度-1100度，压力30-100MPa。热压烧结在充满氩气的密封舱内进行，氧含量低于50ppm。按照常规技术，将步骤S2得到的生坯摆入托盘并装入真空炉，进行低温脱气，中温脱脂、脱氢，然后再进行步骤S3。步骤S3后再进行900度、600度二级时效得到产品；产品外层采用电泳、涂敷高分子有机物以防氧化。
该制备方法适用于钕铁硼、钐钴、钐铁氮。
实例:把常规方法制备的钕铁硼永磁粉末，72g加入模具的模腔摊平，进行取向压制及退磁，在模腔内得到50*50*5生坯薄片，生坯薄片上表面喷或撒绝缘层（低温陶瓷粉末），厚度0.1mm。重复上面操作，得到共30层的生坯薄片和绝缘层交替的生坯。生坯常规800度脱气、脱脂12小时。冷却后进行30MPa、1100度下的热压烧结；900度、600度二级时效。所得夹层结构的钕铁硼永磁体层间结合强度高，整个磁体结构浑然一体。测电阻1.26欧姆，剩磁13.6，降低了800Gs；矫顽力17.5KOe，几乎没有变化。电阻率是0.47姆米。
用于本实施例所述制备方法的设备，包括磁场压机和热压烧结机，磁场压机（如图1-2所示）包括模具1、上模冲2、下模冲3，模具1的上端设置有加料导板4，加料导板4的上表面与模具1的上端面齐平，加料导板4上放置有两端敞口的磁粉加料筒5和绝缘粉加料筒6，磁粉加料筒5和绝缘粉加料筒6的一端面与加料导板4保持紧密接触，磁粉加料筒5和绝缘粉加料筒6的横截面尺寸大于等于模具1的横截面尺寸，磁粉加料筒5和绝缘粉加料筒6被驱沿加料导板4运动并通过在模具1上端面处的往复运动实现磁粉、绝缘粉向模具模腔内的加料；热压烧结机（如图3-4所示）包括模具、上模冲、下模冲，模具周围套有感应加热线圈7（在磁场压机的基础上，去掉取向磁场结构，增加感应加热线圈后就是热压烧结机）。磁场压机工作时，下模冲3上移，与模具1上端面保持合适距离（该距离决定生坯薄片的厚度），磁粉加料筒5被驱在模具1上端面往复运动从而把模具1模腔加满并刮平，上模冲2和下模冲3同时作用，对模具1模腔内的磁粉进行取向压制并退磁，得到生坯薄片；下模冲3适当上移，使生坯薄片上表面与模具1上端面保持合适距离（该距离决定绝缘层的厚度），绝缘粉加料筒6被驱在模具1上端面往复运动从而把模具1模腔加满并刮平而形成绝缘层，下模冲3适当下移，使绝缘层上表面与模具1上端面保持合适距离（该距离决定第二个生坯薄片的厚度），磁粉加料筒5被驱在模具1上端面往复运动从而把模具1模腔加满并刮平，上模冲2和下模冲3同时作用，对模具1模腔内的磁粉进行取向压制并退磁，得到（第二个）生坯薄片，重复上述过程，直至到达所需的高度尺寸后脱模，得到生坯薄片和绝缘层交替的生坯；将所得生坯放入热压烧结机的模具内，在热压烧结机的上模冲、下模冲的压力作用下及感应加热线圈7的加热下，完成热压烧结。
实施例三
高电阻率烧结稀土永磁体的制备方法，包括如下步骤：
S1、制备稀土永磁粉末；
S2、在低氧环境下，对稀土永磁粉末进行取向压制，退磁，制成生坯薄片；其中取向磁场方向与压制压力方向垂直；
S3、将各生坯薄片表面包覆绝缘层；
S4、若干包覆绝缘层的生坯薄片以被压制面（垂直于压制压力方向的承压表面）相互接触且取向方向一致的姿态摞起来，放入热压模具，进行热压烧结，即在烧结的同时对热压模具内摞起来的生坯薄片施加垂直于被压制面的压力。
具体实施时，绝缘层材料采用熔化温度400-900度的低温陶瓷粉末或低温玻璃粉末或稀土氯化物，或其中任两种任意比例的混合物；低温陶瓷粉末、低温玻璃粉末、稀土氯化物属于低熔点盐类，受热不分解，不溶于水，高电阻率，热压时能把相邻生坯薄片粘接在一起，进一步提高层间结合强度。生坯薄片表面包覆绝缘层具体可采用涂敷或丝网印刷的方式，即将低温陶瓷粉末、低温玻璃粉末、稀土氯化物的粉末（粒度在0.5微米-10微米）溶于液体或溶剂制成悬浮液，然后进行涂敷或丝网印刷。生坯薄片厚度0.5-10毫米（根据几何形状及工作频率确定厚度）。绝缘层10-50微米。热压烧结采用中频感应加热，烧结温度700度-1100度，压力30-100MPa。热压烧结在充满氩气的密封舱内进行，氧含量低于50ppm。按照常规技术，将步骤S3的包覆绝缘层的生坯薄片摆入托盘并装入真空炉，进行低温脱气，中温脱脂、脱氢，然后再进行步骤S4。步骤S4后再进行900度、600度二级时效得到产品；产品外层采用电泳、涂敷高分子有机物以防氧化。
该制备方法适用于钕铁硼、钐钴、钐铁氮。
用于本实施例所述制备方法的设备（如图5所示），包括磁场压机和热压烧结机，磁场压机包括多个模具1、上模冲2、下模冲3、皮带传输机构及上料机构；皮带传输机构包括两个皮带轮8和环绕两个皮带轮8的闭环皮带9，皮带9的上层从上模冲2和下模冲3之间穿过；模具1为一端封闭、另一端敞口且封闭一端固定于皮带9上，多个模具1均布于皮带9上；当模具1随皮带9运动至皮带上层端口处时，由上料机构向模具1的模腔加入磁粉，当模具1在皮带上层随皮带9运动至上模冲2和下模冲3之间时，上模冲2和下模冲3共同作用，对模具1模腔内的磁粉进行取向压制并退磁，得到生坯薄片，当模具1随皮带9运动至皮带下层时，生坯薄片（依靠重力）脱出模具1；热压烧结机包括模具、上模冲、下模冲，模具周围套有感应加热线圈7。脱出模具1的生坯薄片包覆绝缘层后摞于热压烧结机的模具内，完成热压烧结。该设备的磁场压机由于增设了皮带传输机构，极大地提高了生坯薄片的加工效率。
Claims (7)
1.一种高电阻率烧结稀土永磁体的制备方法，其特征在于包括如下步骤：
S1、制备稀土永磁粉末；
S2、在低氧环境下，对稀土永磁粉末进行取向压制，退磁，制成生坯；其中取向磁场方向与压制压力方向垂直；
S3、将生坯切割成薄片，其中切割面垂直于压制压力方向；
S4、将各薄片表面包覆绝缘层；
S5、若干包覆绝缘层的薄片以切割面相互接触且取向方向一致的姿态摞起来，放入热压模具，进行热压烧结，即在烧结的同时对热压模具内摞起来的薄片施加垂直于切割面的压力。
2.根据权利要求1所述的高电阻率烧结稀土永磁体的制备方法，其特征在于绝缘层材料采用熔化温度400-900度的低温陶瓷粉末或低温玻璃粉末或稀土氯化物，或其中任两种任意比例的混合物。
3.根据权利要求1或2所述的高电阻率烧结稀土永磁体的制备方法，其特征在于热压烧结的压力30-100MPa。
4.根据权利要求3所述的高电阻率烧结稀土永磁体的制备方法，其特征在于在步骤S3进行生坯切割薄片之前，对步骤S2得到的生坯进行等静压。
5.一种高电阻率烧结稀土永磁体的制备方法，其特征在于包括如下步骤：
S1、制备稀土永磁粉末；
S2、在低氧环境下，对稀土永磁粉末进行取向压制，退磁，制成生坯薄片；其中取向磁场方向与压制压力方向垂直；
S3、将各生坯薄片表面包覆绝缘层；
S4、若干包覆绝缘层的生坯薄片以被压制面相互接触且取向方向一致的姿态摞起来，放入热压模具，进行热压烧结，即在烧结的同时对热压模具内摞起来的生坯薄片施加垂直于被压制面的压力。
6.根据权利要求5所述的高电阻率烧结稀土永磁体的制备方法，其特征在于绝缘层材料采用熔化温度400-900度的低温陶瓷粉末或低温玻璃粉末或稀土氯化物，或其中任两种任意比例的混合物。
7.实现权利要求5或6所述高电阻率烧结稀土永磁体的制备方法的设备，其特征在于，包括磁场压机和热压烧结机，磁场压机包括多个模具(1)、上模冲(2)、下模冲(3)、皮带传输机构及上料机构；皮带传输机构包括两个皮带轮(8)和环绕两个皮带轮(8)的闭环皮带(9)，皮带(9)的上层从上模冲(2)和下模冲(3)之间穿过；模具(1)为一端封闭、另一端敞口且封闭一端固定于皮带(9)上，多个模具(1)均布于皮带(9)上；当模具(1)随皮带(9)运动至皮带上层端口处时，由上料机构向模具(1)的模腔加入磁粉，当模具(1)在皮带上层随皮带(9)运动至上模冲(2)和下模冲(3)之间时，上模冲(2)和下模冲(3)共同作用，对模具(1)模腔内的磁粉进行取向压制并退磁，得到生坯薄片，当模具(1)随皮带(9)运动至皮带下层时，生坯薄片脱出模具(1)；热压烧结机包括模具、上模冲、下模冲，模具周围套有感应加热线圈(7)。
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