CN113764150B - 一种可膨胀烧结钕铁硼磁体及其制备方法和应用 - Google Patents
一种可膨胀烧结钕铁硼磁体及其制备方法和应用 Download PDFInfo
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- Hard Magnetic Materials (AREA)
Abstract
本发明公开一种可膨胀烧结钕铁硼磁体及制备方法和应用,所述磁体包括烧结钕铁硼磁体及涂覆于烧结钕铁硼磁体表面的可膨胀涂层。本发明通过采用涂覆有可膨胀涂层的烧结钕铁硼磁体来代替传统的环氧树脂粘接涂层磁体加灌封树脂胶的装配方式,可将涂覆有可膨胀涂层的磁体***磁钢槽内,利用涂层自身不可逆的膨胀,来实现磁体在磁钢槽的固定。同时本发明可膨胀涂层的使用,大大缩短了电机装配的时间,并提高了电机装配的精度。且本发明涂覆有可膨胀涂层的烧结磁体具有优异的抗高温、抗老化及耐腐蚀性能和结合力强等优异特性。
Description
技术领域
本发明涉及磁性材料表面防护技术领域,具体涉及一种可膨胀烧结钕铁硼磁体及制备方法和应用。
背景技术
烧结钕铁硼磁体因具有优异的剩磁、矫顽力和磁能积,被称为当代“磁王”,因而被广泛应用于能源、交通、机械、医疗、IT、家电等行业,特别是随着新能源的开发和利用,使烧结钕铁硼磁体的需求和应用不断扩大。烧结钕铁硼磁体的出现大大促进了永磁电机的发展,使原先使用铁氧体或钐钴磁体做电机定子或转子的产品都力图使用烧结钕铁硼永磁代替,以减轻电机重量、提高功率系数、并增加输出功率。但是烧结钕铁硼由主相Nd2Fe14B、富Nd相和富B相组成,而其中金属Nd元素的化学活性最强,其在潮湿、高温以及电化学环境中极易被腐蚀,从而严重限制了烧结钕铁硼磁体应用领域的进一步拓展。
目前,电机行业普遍采用电泳环氧树脂涂层进行表面防护,涂层厚度为15-30μm,该涂层与基体的结合力强,并具有耐酸、耐碱等突出优点。然而,在电机装配过程中,需要采用灌封树脂胶进行装配,即:将磁石***到磁钢槽内,再注射树脂胶,并加热固化,以使磁体固定在磁钢槽内部。因而在电机装配过程中,不仅需要考虑树脂胶的流动性、粘结性、导热性、耐油性、环保性等因素,同时由于树脂胶加热固化耗时较长,通常需要加热固化24h以上才能达到电机装配中对粘结力的要求。此外,环氧树脂粘接涂层虽然性能优异,但该涂层硬度较小,耐磨性能极差,在包装运输及电机装配中易发生破损,且由于环氧树脂粘接涂层为阴极保护涂层,一旦涂层发生破损,磁体将遭受严重的腐蚀。因此,如何将磁体固定在磁钢槽内,并使涂层具有较高的硬度和耐磨性能成为本领域亟待解决的技术问题。
发明内容
为了改善上述技术问题,本发明提供一种可膨胀烧结钕铁硼磁体,所述磁体包括烧结钕铁硼磁体及涂覆于烧结钕铁硼磁体表面的可膨胀涂层。
根据本发明的实施方案,所述可膨胀涂层的厚度为50-300μm,优选为80-150μm,示例性为50μm、80μm、110μm、150μm、180μm、200μm、250μm、300μm。
根据本发明的实施方案,所述可膨胀涂层在60-100℃下软化,示例性为在60℃、70℃、80℃、90℃、100℃下软化。
根据本发明的实施方案,在无压力的状态下,所述可膨胀涂层厚度的膨胀率为200%-400%,优选为300-400%,示例性为200%、220%、250%、280%、300%、350%、400%。
本发明的可膨胀涂层在165-210℃加热下,可膨胀涂层内部有机树脂会发生交联,以实现固定成型。
根据本发明的实施方案,所述可膨胀涂层膨胀后,涂层呈蜂窝状。优选地,所述可膨胀涂层膨胀后具有基本上如图1所示的形貌。
本发明中,膨胀率=自由状态下涂层膨胀后的厚度/可膨胀涂层膨胀前的厚度。
根据本发明的实施方案,所述可膨胀涂层中至少含有水溶性树脂和发泡剂。
优选地,所述水溶性树脂选自水溶性丙烯酸树脂、水性环氧树脂和水性聚氨酯树脂中的至少一种。优选选自水溶性丙烯酸树脂。
根据本发明的实施方案,所述可膨胀涂层中,所述水溶性树脂的固体分含量为30-50%,示例性为30%、35%、40%、50%。
优选地,所述发泡剂为热塑性膨胀微球,膨胀微球的直径为5-30μm,优选为5-20μm,示例性为5μm、8μm、10μm、12μm、15μm、18μm、20μm、25μm、30μm。
根据本发明的实施方案,所述可膨胀涂层膨胀后,膨胀微球面积占膨胀涂层截面积的60-90%,示例性为60%、70%、80%、90%。
根据本发明的实施方案,在110-210℃(示例性为110℃、120℃、130℃、140℃、150℃、160℃)下,所述可膨胀涂层内部的膨胀微球呈阶梯性膨胀。
优选地,所述膨胀微球的平均直径为10-15μm,示例性为10μm、12μm、15μm。
优选地,所述膨胀微球的膨胀温度为110-210℃,示例性为110℃、120℃、150℃、160℃、170℃、180℃、200℃。
优选地,所述膨胀微球的最高耐热温度为145-235℃,示例性为145℃、160℃、180℃、200℃、215℃、235℃。
根据本发明的实施方案,所述可膨胀涂层由至少含有水溶性树脂和发泡剂组分的可膨胀涂料涂覆制备而成。
根据本发明的实施方案,所述可膨胀涂料中水溶性树脂的重量百分比为45-65%,例如为50-60%。
根据本发明的实施方案,所述可膨胀涂料中发泡剂的重量百分比为10-30%,例如为15-25%。
根据本发明的实施方案,所述可膨胀涂料中还任选地含有锂皂石。例如,所述锂皂石的重量百分比为0.1-0.5%,又如0.2-0.4%。
根据本发明的实施方案,所述可膨胀涂料中还任选地含有二丙醇丁醚。例如,所述二丙醇丁醚的重量百分比为0.5-3%,又如0.8-2.5%。
根据本发明的实施方案,所述可膨胀涂料中还任选地含有丙二醇。例如,所述丙二醇的重量百分比为1-3%,又如1.5-2.5%。
根据本发明的实施方案,所述可膨胀涂料中还任选地含有丙烯酸增稠剂。例如,所述丙烯酸增稠剂的重量百分比为0.2-0.8%,又如0.3-0.6%。
根据本发明的实施方案,所述可膨胀涂料中还任选地含有分散剂。例如,所述分散剂的重量百分比为0.1-0.5%,又如0.2-0.4%。
优选地,所述分散剂为乙二醇、油酸钠、羧酸盐等。
根据本发明的实施方案,所述可膨胀涂层中还任选地含有流平剂。例如,所述流平剂的重量百分比为0.1-0.5%,又如0.2-0.4%。
优选地,所述流平剂为硅油、有机硅氧烷等。
根据本发明的实施方案,所述可膨胀涂料中还包含水。
根据本发明的实施方案,所述可膨胀涂料中各组分的重量百分比之和为100%。根据本发明的实施方案,所述可膨胀涂料的制备方法,包括将上述各组分进行混合,得到所述可膨胀涂料。
优选地,所述可膨胀涂料的制备方法还包括将混合后的各组分分散于水中得到分散液。进一步地,还包括对上述分散液进行搅拌,使其混合均匀。
本发明中,通过筛分机对膨胀微球进行筛分,以选取粒径范围在5-30μm的膨胀微球,并将其与水溶性树脂混合,在常温下搅拌30-60min。
根据本发明的实施方案,所述可膨胀涂层由包括如下重量百分比组分的可膨胀涂料涂覆制备得到:水溶性树脂45-65%、发泡剂10-30%、锂皂石0.1-0.5%、二丙醇丁醚0.5-3%、丙二醇1-3%、丙烯酸增稠剂0.2-0.8%、分散剂0.1-0.5%、流平剂0.1-0.5%。
本发明的发明人意外发现,在加热膨胀过程中,需将膨胀率控制在300-400%范围内,当膨胀率小于200%时,磁体与磁钢槽间的缝隙无法填充密实;而如果膨胀率大于400%,则会破坏涂层内部的交联,从而使推出力不足。且膨胀率与涂层中微球的含量、粒径、膨胀温度、膨胀时间、涂层厚度等条件有关,本发明通过优化可膨胀涂层中各组分原料的用量和膨胀条件,可将膨胀倍率控制在合适范围内,以进一步制备得到具有优异粘结推出力的烧结钕铁硼磁体。
根据本发明的实施方案,所述烧结钕铁硼磁体由主相Nd2Fe14B、富Nd相和富B相组成。
本发明还提供上述可膨胀烧结磁体的制备方法,将包括上述各组分的可膨胀涂料涂覆于烧结钕铁硼磁体表面,经预固化处理制备得到所述可膨胀烧结磁体。
根据本发明的实施方案,所述烧结钕铁硼磁体在涂覆可膨胀涂料前还包括对其进行表面预处理的步骤。
根据本发明的一个实施方案,所述表面预处理包括对烧结钕铁硼磁体的表面进行化学超声除油、酸洗、水洗的过程。
优选地,所述除油过程中采用的除油液为碱及表面活性剂的复合溶液。
优选地,所述碱为氢氧化钠或碳酸钠,其浓度为10-20g/L,示例性为10g/L、15g/L、20g/L。
优选地,所述表面活性剂为十二烷基磺酸钠或十二烷基硫酸钠,其浓度为2-6g/L,示例性为2g/L、3g/L、4g/L、5g/L、6g/L。
优选地,所述除油液温度为30-70℃,示例性为30℃、40℃、50℃、60℃、70℃。进一步地,所述除油时间1-20min,示例性为1min、5min、10min、15min、20min。
优选地,所述酸洗采用的酸可以为硝酸或柠檬酸水溶液。
优选地,所述酸洗采用的酸液浓度为5-30wt%,示例性为5wt%、10wt%、15wt%、20wt%、25wt%、30wt%。进一步地,所述酸洗的时间为5-30s,示例性为5s、10s、15s、20s、25s、30s。
优选地,所述水洗包括使用纯水进行超声波水洗。进一步地,所述水洗时间为20-120s,示例性为20s、30s、50s、80s、100s、120s。
根据本发明的实施方案,所述涂覆方式包括但不限于喷涂、印刷、浸沾、涂抹等。优选为喷涂。
根据本发明的实施方案,所述涂覆的厚度为50-300μm,优选厚度为80-150μm,示例性为50μm、80μm、110μm、150μm、180μm、200μm、250μm、300μm。
本发明的发明人意外发现,可膨胀涂层的涂覆厚度过薄,在装配过程中会存在膨胀力不足,因而达不到预定的推出力要求。但若可膨胀涂层的涂覆厚度太厚,则涂层表面易脱落、龟裂。且可膨胀涂层的涂覆厚度与磁钢槽预留的尺寸有关,预留的尺寸越大,需要的涂层厚度越厚。发明人意外发现,当涂层膨胀后,涂层在磁钢槽内的膨胀压缩率为35-65%之间时效果最佳,此时磁体和磁钢槽的粘结力最佳,磁体在磁钢槽内的推出力最大。
膨胀压缩率m=(H1-H0)/(H2-H0);
其中:H0为可膨胀涂层的涂覆厚度,H1为可膨胀涂层在磁钢槽内膨胀后的厚度,H2为可膨胀涂层在自然状态下膨胀后的厚度。
根据本发明的实施方案,所述预固化处理可以为将涂层在常温条件下(15-35℃)自然晾干,也可以为在中低温(35-90℃)烘烤条件下进行干燥,以形成完整涂层。
本发明还提供上述可膨胀烧结烧结钕铁硼磁体在电机转子中的应用。
本发明还提供一种电机转子工件,其含有上述可膨胀烧结烧结钕铁硼磁体。
本发明还提供上述电机转子工件的装配方法,包括将上述可膨胀烧结钕铁硼磁体装配到磁钢槽中,经加热膨胀处理,制得所述电机转子工件。
本发明的发明人意外发现,膨胀涂层最终的使用性能与膨胀装配过程中的膨胀温度、升温速率、保温时间有关,膨胀温度会对最终膨胀涂层的结构产生直接影响。
根据本发明的实施方案,所述加热膨胀处理采用二段式升温法,第一膨胀阶段的膨胀温度为110℃-160℃,示例性为110℃、120℃、130℃、140℃、150℃、160℃。进一步地,第一膨胀阶段的升温速率为5℃/min-15℃/min,示例性为5℃/min、10℃/min、15℃/min。
当第一膨胀阶段的膨胀温度低于110℃时,将有大量微球未能膨胀,达不到所需膨胀倍率;但当第一膨胀阶段的膨胀温度高于160℃时,微球将快速膨胀,但由于涂层中的微球粒径大小不同,会导致小粒径的微球快速膨胀破裂,导致涂层提前坍塌,因而得不到相应的支撑力。且当第一膨胀阶段的升温速率控制在5-15℃/min时,则可以使膨胀涂层均匀膨胀,膨胀微球在升温的过程中体内的液化烃气体充分气化,使涂层缓慢而均匀地膨胀。
根据本发明的实施方案,所述加热膨胀处理的第二膨胀温度为180℃-210℃,示例性为180℃、190℃、200℃、210℃。进一步地,第二膨胀阶段的升温速率为30-60℃/min,示例性为30℃/min、40℃/min、50℃/min、60℃/min。涂层在均匀膨胀后,加速升温,以使涂层内的热塑性树脂快速固化。
本发明的热塑性膨胀微球由包含热塑性树脂外壳和包裹在其中的推进剂组成,推进剂70%以上由异辛烷构成。除了异辛烷以外,推进剂还可以选自丁烷、戊烷、庚烷等其他合适沸点范围内的液体。在加热膨胀过程中,膨胀微球内液态的推进剂达到沸点后,推进剂蒸发使微球内压升高而引起推进剂的体积变化,使受热后变得柔软的外壳变形膨胀,同时外壳软化,导致微球限制膨胀。膨胀开始时的温度为Tstar,达到最大膨胀度时的温度是Tmax,当温度超过Tmax时,推进剂经热塑性树脂外壳释出至微球开始破裂的程度。
在第一膨胀阶段,涂层中的高沸点溶剂挥发,溶解粒径<10μm,壁厚<3μm的膨胀微球外壳,使外壳壁变薄,在未达到最大膨胀温度时就破裂。膨胀涂层中>60%的微球破裂,破裂后,微球中的推进剂释放,微球不再加速膨胀,以形成孔洞结构,微球外壁的热塑性树脂与涂层中的水溶性树脂交联,形成网状结构,以增加磁体在磁钢槽内的粘结力。
在第二膨胀阶段,涂层中粒径>10μm的膨胀微球微球继续膨胀,但此时涂层中的高沸点溶剂已经挥发,不会加速膨胀微球外壳破裂。此时第二膨胀阶段的最大膨胀温度要低于粒径>10μm的微球的最大膨胀温度,推进剂释放速度放缓。
本发明的膨胀微球中释放剂是由70%以上的异辛烷组成的,因此,通过检测膨胀过程中异辛烷的释放量,可以控制涂层的膨胀速率,进而控制涂层中60%以上的微球破裂,进而与水溶性树脂交联形成网状结构。
本发明可以通过检测收集的气体,以确定膨胀过程中异辛烷的气体释放量,从而控制膨胀微球破裂的比例。检测方法如下:
取一块涂覆有膨胀涂层的磁体(规格为35.5mm*16.5mm*5.5mm),置于密封的取样瓶内,在与膨胀装配过程中的膨胀工艺条件相同的加热温度及升温速率下进行加热,加热结束后,自然冷却至60℃,使用氮气将取样瓶内的气体吹扫到气相色柱内进行检测,记录此时异辛烷含量w1;
将取样瓶内的磁体继续升温,在高于膨胀微球最大膨胀温度Tmax的温度下(240℃)加热3h,使膨胀涂层中的微球彻底破裂,微球内的异辛烷彻底释放,记录此时异辛烷含量w2。
根据异辛烷的释放量,从而计算微球的破裂比例q=w1/(w1+w2)。
发明人经大量试验意外发现:微球的破裂比例q在60-85%范围内,膨胀涂层均具有优异的支撑效果,在使用环境中,膨胀磁体均具有较高的推出力,且涂层粘结效果最好。
膨胀涂层先经历软化过程,涂层内的膨胀微球因受热导致体积增大,膨胀涂层整体厚度增加,对电机工装内壁产生挤压力,同时膨胀涂层内的热熔树脂软化后会产生一定的粘结力,将烧结磁体固定于电机工装中,以完成装配过程。
本发明的有益效果:
(1)本发明通过采用涂覆有可膨胀涂层的烧结钕铁硼磁体来代替传统的环氧树脂粘接涂层磁体加灌封树脂胶的装配方式,可将涂覆有可膨胀涂层的磁体***磁钢槽内,利用涂层自身不可逆的膨胀,来实现磁体在磁钢槽的固定。同时本发明可膨胀涂层的使用,大大缩短了电机装配的时间,并提高了电机装配的精度。且本发明涂覆有可膨胀涂层的烧结磁体具有优异的抗高温、抗老化及耐腐蚀性能和结合力强等优异特性。
(2)本发明采用特殊配方的环保水性膨胀涂料,代替传统的灌胶树脂,因而能够减少溶剂型粘结剂造成的VOC排放及环境问题。
(3)本发明通过将可膨胀涂层中膨胀微球的含量控制在10-30%,当受热膨胀后,水溶性树脂与膨胀微球会相互交联,形成蜂窝状的多孔结构,其中孔隙率达到60-90%,常温下在工装中的粘结推力大于1000N/cm2。
(4)本发明制得的膨胀涂层常温(25℃)条件下硬度达到三菱铅笔H以上,耐磨性强,在运输过程中涂层表面不易被破坏。且本发明的膨胀涂层在10%盐酸、10%氢氧化钠溶液中浸泡24h以上,该涂层不会出现***、溶解、脱落等缺陷,因而显示出较高的耐酸碱性能。同时涂层于170℃机油中浸泡500h以上,涂层仍不会出现***、鼓泡、脱落等问题,因而显示出较高的耐热油性能。
附图说明
图1为实施例1制得的可膨胀涂层膨胀后的电镜照片(放大300倍)。
图2为实施例5制得的可膨胀涂层(样品5)膨胀后的电镜照片(放大250倍)。
图3为实施例6制得的可膨胀涂层(样品6)膨胀后的电镜照片(放大250倍)。
图4为实施例10制得的可膨胀涂层(样品10)膨胀后的电镜照片(放大500倍)。
具体实施方式
下文将结合具体实施例对本发明的技术方案做更进一步的详细说明。应当理解,下列实施例仅为示例性地说明和解释本发明,而不应被解释为对本发明保护范围的限制。凡基于本发明上述内容所实现的技术均涵盖在本发明旨在保护的范围内。
除非另有说明,以下实施例中使用的原料和试剂均为市售商品,或者可以通过已知方法制备。
实施例1
本实施例中采用规格为35.5mm*16.5mm*5.5mm的烧结钕铁硼磁体(未充磁),带装配的电机转子的磁钢槽尺寸是36mm*17mm*6mm。
磁体表面预处理:采用氢氧化钠浓度为15g/L,十二烷基磺酸钠浓度为3g/L的复合除油液,于60℃下对烧结钕铁硼磁体进行除油,除油时间为2min,然后采用25wt%的柠檬酸水溶液酸洗15s,最后将烧结钕铁硼磁体放入去离子水中超声清洗2min。
制备可膨胀涂料:按照以下组分配置可膨胀涂料(以重量百分比计算):水溶性丙烯酸树脂55%,水30%,发泡剂10%,锂皂石0.2%,二丙醇丁醚1.5%,丙二醇2%,丙烯酸增稠剂0.5%,乙二醇0.4%,聚二甲基硅氧烷0.4%,发泡剂选用热塑性膨胀微球,其平均直径为13μm。
涂覆处理:采用压缩空气喷涂方式在磁体表面涂覆上述可膨胀涂料,喷涂速度为120mm/s,涂覆厚度为110μm,喷嘴距工件的距离为15cm,喷枪与工件的角度为25°,喷枪的氩气压力为0.6MPa。
预固化处理:将涂覆可膨胀涂料后的磁体表面加热至50℃,进行预固化处理,得到涂层厚度为110μm。
涂层膨胀:在无压力状态下,将涂覆有膨胀涂层的磁体放入高温烘箱中,采用两分段式加热,首先加热至120℃,保温5min;然后快速升温至170℃,保温3min。其中:第一段加热的升温速率是5℃/min,第二段加热的升温速率是50℃/min。随着温度的升高,膨胀微球壳内气体压力增加,其热塑性外壳软化,微球膨胀体积显著增加,此时膨胀涂层内部树脂软化,膨胀涂层的厚度随着膨胀微球体积的增大而增加。如图1所示,从图中可以看出:微球均匀膨胀,微球壁和树脂相互交联,形成了稳定的支撑结构。膨胀涂层由水溶性丙烯酸树脂和膨胀微球组成。膨胀涂层的厚度由预固化处理后的110μm膨胀至394μm,膨胀率达358%。且膨胀后,膨胀涂层呈蜂窝状,膨胀微球截面积占膨胀涂层截面积的82%。(本发明中,一个截面中膨胀微球截面积占膨胀涂层截面积的比例,计算方法如下:首先,取膨胀后涂层截面的扫描电镜照片,然后通过图像识别该截面中的空隙,计算出空隙面积的总和,将空隙面积作为膨胀微球截面积占膨胀涂层截面积的比例)。
将涂覆有膨胀涂层的磁体装配到电机转子的磁钢槽中,放入高温烘箱中,采用两分段式加热,首先加热至120℃,保温5min,然后快速升温至170℃,保温3min。其中:第一段加热的升温速度是5℃/min,第二段加热的升温速度是50℃/min。(磁体安装在磁钢槽内,膨胀涂层因受热膨胀,对磁钢槽内壁产生挤压,将磁钢槽与磁体缝隙填满,同时涂层内部树脂与膨胀微球发生交联,产生蜂窝状涂层结构。因磁钢槽内壁的限制,导致膨胀过程中涂层不能膨胀到最大限度,从而使膨胀后蜂窝状的结构受到压缩,成褶皱状。)加热结束后,将电机转子在自然条件下冷却,因环境温度改变导致膨胀微球体积增大,且改变是不可逆的,由于涂层体积的增加,使磁体和磁钢槽内壁的空隙被填满,以将磁体紧密固定在磁钢内部,此时得到的磁体产品命名为样品1。
在该状态下,检测磁体的常温粘结推出力和高温粘结推出力,常温(25℃)下粘结推出力为:1200N/cm2,高温(170℃)下粘结推力为530N/cm2。
实施例2-5
表面预处理方法、可膨胀涂料、涂覆处理工艺同实施例1,将带有膨胀涂层厚度为110μm的磁体,***到磁钢槽中,采用不同的第一膨胀温度、第二膨胀温度、升温速率、膨胀时间,得到最佳的装配工艺条件,结果如下表1所示。
表1
*其中:W1、W2是异辛烷的含量,q为微球破裂率。
由表1中结果可知,常温推力、高温推力与膨胀温度和升温速率相关,通过优化可以得出最佳的装配工序条件。
同时通过检测异辛烷的释放量,推算得出微球破裂率,可知微球破裂率在60-85%之间,破裂的微球与树脂涂层相互交联,得到的涂层具有稳定结构,可以稳定支撑磁体和磁钢槽内的空隙。
图1为样品1膨胀后的涂层状态,从图中可以看出:微球均匀膨胀,使微球壁和树脂相互交联,从而形成了稳定的支撑结构。
图2为样品5膨胀后的涂层状态,从图中可以看出:微球破裂较多,且微球和微球之间融合黏连,造成较大的空洞,导致涂层在高温状态下粘结力较低。
实施例6
本实施例中采用规格为35.5mm*16.5mm*5.5mm的烧结钕铁硼磁体(未充磁),带装配的电机转子的磁钢槽尺寸是36mm*17mm*6mm。
采用与实施例1相同的表面预处理方式,采用氢氧化钠浓度为15g/L,十二烷基磺酸钠浓度为3g/L的复合除油液,于60℃下对烧结钕铁硼磁体进行除油,除油时间为2min,然后采用25wt%的柠檬酸水溶液酸洗15s,最后将烧结钕铁硼磁体放入去离子水中超声清洗2min。
选用AKZO-Nobel公司生产的可膨胀粉末涂料,涂料由50%的环氧树脂粉末、20%的固化剂、10%弹性体树脂、20%的热塑性膨胀微球组成。采用压缩空气喷涂方式在磁体表面涂覆上述可膨胀涂料,喷涂速度为60mm/s,涂覆厚度为110μm,喷嘴距工件的距离为10cm,喷枪与工件的角度为25°,喷枪的氩气压力为0.6MPa。
将涂覆有膨胀涂层的磁体装配到电机转子的磁钢槽中,放入高温烘箱中,通过施加190℃的温度,加热20min。热塑性膨胀微球因温度变化导致的体积增大,从而引起整体涂层的膨胀,与此同时,环氧树脂固化,使得涂层稳定不回缩。使用电子显微镜观察膨胀涂层断面结构,如图3所示,膨胀涂层的厚度由预固化处理后的110μm膨胀至180μm,膨胀率达163%。且膨胀后,可以清楚地看到。可以清晰地看到热塑性膨胀微球的边缘,膨胀微球在受热条件下,仅仅因微球内的液态烷烃气化导致微球体积增大。通过检测膨胀微球中异辛烷的释放量,来推测涂层内微球是否破裂。检测得知,在190℃下加热20min,异辛烷的释放量w1为1.52mg/l。升温至240℃,保持3h,致使涂层中膨胀微球完全破裂,异辛烷的释放量w2是5.34mg/l。根据公式计算,可以推算出在实际装配过程中,膨胀微球的破裂率为q=w1/(w1+w2)=1.52/(1.52+5.34)=22%。
由图3可以看出,膨胀微球的截面积占膨胀涂层的35%。
在该状态下,检测磁体的常温粘结推出力和高温粘结推出力,常温(25℃)下粘结推出力为:920N/cm2,高温(170℃)下粘结推力为310N/cm2。
实施例7-14
本实施例中采用规格为35.5mm*16.5mm*5.5mm的烧结钕铁硼磁体(未充磁),带装配的电机转子的磁钢槽尺寸是36mm*17mm*6mm。
采用与实施例1相同的的表面预处理过程和可膨胀涂料,采用压缩空气喷涂方式在磁体表面涂覆上述可膨胀涂料,喷涂的厚度分别为80μm、90μm、100μm、110μm、120μm、130μm、140μm、150μm。
将涂覆有膨胀涂层的磁体装配到电机转子的磁钢槽中,放入高温烘箱中,采用两分段式加热,首先加热至120℃,保温5min,然后快速升温至170℃,保温3min。其中:第一段加热的升温速度是5℃/min,第二段加热的升温速度是50℃/min。检测工作状态下磁体的常温推出力和高温推出力,结果如下表2所示:
膨胀率=H2/H0
压缩率=(H1-H0)/(H2-H0)
其中H0为涂布厚度,H1为可膨胀涂层在磁钢槽内膨胀后的厚度,H2为可膨胀涂层在自然状态下膨胀后的厚度。
表2
图4为样品10在磁钢槽内的涂层状态,从图4中可以看出:涂层在膨胀过程中,因受磁钢槽内壁的限制,使得膨胀涂层受到压缩,成褶皱状。
当膨胀涂层受到严重压缩时,膨胀涂层的接触面与磁钢槽内壁的接触面产生较大的应力,涂层单位面积上的应力增大,涂层内部缺陷呈指数增加,从而使胶层内聚强度下降,因此,通过将压缩率控制在35%以上,即可制得具有较好的常温推出力和高温推出力的磁体。
压缩率越大,取得的经济效果越好,发明人经大量实验意外发现:当压缩率大于65%时,涂层对温度变化引起的收缩应力和热应力越敏感,从而会=致使磁体内聚强度的损失,因而使磁体的常温推出力和高温推出力降低。
以上,对本发明的实施方式进行了说明。但是,本发明不限定于上述实施方式。凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (38)
1.一种可膨胀烧结钕铁硼磁体的制备方法,其特征在于,所述制备方法包括将可膨胀涂料涂覆于烧结钕铁硼磁体表面,经预固化处理制备得到可膨胀烧结钕铁硼磁体;
其中,所述可膨胀涂料包括如下重量百分比的组分:水溶性树脂45-65%、发泡剂10-30%、锂皂石0.1-0.5%、二丙醇丁醚0.5-3%、丙二醇1-3%、丙烯酸增稠剂0.2-0.8%、分散剂0.1-0.5%、流平剂0.1-0.5%;
所述水溶性树脂的固体分含量为30-50%;
所述发泡剂为热塑性膨胀微球,所述热塑性膨胀微球由包含热塑性树脂外壳和包裹在其中的推进剂组成,推进剂70%以上由异辛烷、丁烷、戊烷或庚烷构成,所述热塑性膨胀微球的直径为5-30μm;
所述可膨胀烧结钕铁硼磁体包括烧结钕铁硼磁体及涂覆于烧结钕铁硼磁体表面的可膨胀涂层,其中,所述可膨胀涂层由所述可膨胀涂料涂覆制备得到;
所述可膨胀涂料的涂覆厚度为50-300μm;
其中,在无压力的状态下和110-210℃下加热膨胀时,所述可膨胀涂层厚度的膨胀率为200%-400%;
所述加热膨胀处理采用二段式升温法,第一膨胀阶段的温度为110℃-160℃,升温速率为5℃/min-15℃/min;第二膨胀阶段的温度为180℃-210℃,升温速率为30-60℃/min;
所述可膨胀涂层膨胀后,膨胀微球面积占膨胀涂层截面积的60-90%。
2.如权利要求1所述的制备方法,其特征在于,所述可膨胀涂层在60-100℃下软化。
3.如权利要求1所述的制备方法,其特征在于,在无压力的状态下和110-210℃下加热膨胀时,所述可膨胀涂层厚度的膨胀率为300-400%。
4.如权利要求1所述的制备方法,其特征在于,所述可膨胀涂层膨胀后,涂层呈蜂窝状。
5.如权利要求1所述的制备方法,其特征在于,所述水溶性树脂选自水溶性丙烯酸树脂、水性环氧树脂和水性聚氨酯树脂中的至少一种。
6.如权利要求1所述的制备方法,其特征在于,所述膨胀微球的直径为5-20μm。
7.如权利要求6所述的制备方法,其特征在于,所述膨胀微球的平均直径为10-15μm。
8.如权利要求1所述的制备方法,其特征在于,所述膨胀微球的膨胀温度为110-210℃。
9.如权利要求1所述的制备方法,其特征在于,所述膨胀微球的最高耐热温度为145-235℃。
10.如权利要求1-9任一项所述的制备方法,其特征在于,所述可膨胀涂料中水溶性树脂的重量百分比为50-60%。
11.如权利要求1-9任一项所述的制备方法,其特征在于,所述可膨胀涂料中发泡剂的重量百分比为15-25%。
12.如权利要求1-9任一项所述的制备方法,其特征在于,所述锂皂石的重量百分比0.2-0.4%。
13.如权利要求1-9任一项所述的制备方法,其特征在于,所述二丙醇丁醚的重量百分比0.8-2.5%。
14.如权利要求1-9任一项所述的制备方法,其特征在于,所述丙二醇的重量百分比为1.5-2.5%。
15.如权利要求1-9任一项所述的制备方法,其特征在于,所述丙烯酸增稠剂的重量百分比为0.3-0.6%。
16.如权利要求1-9任一项所述的制备方法,其特征在于,所述分散剂的重量百分比为0.2-0.4%。
17.如权利要求1-9任一项所述的制备方法,其特征在于,所述分散剂选自乙二醇、油酸钠、羧酸盐。
18.如权利要求1-9任一项所述的制备方法,其特征在于,所述流平剂的重量百分比为0.2-0.4%。
19.如权利要求1-9任一项所述的制备方法,其特征在于,所述流平剂选自硅油、有机硅氧烷。
20.如权利要求1-9任一项所述的制备方法,其特征在于,所述可膨胀涂料中还包含水。
21.如权利要求20所述的制备方法,其特征在于,所述可膨胀涂料中各组分的重量百分比之和为100%。
22.如权利要求1-9任一项所述的制备方法,其特征在于,所述烧结钕铁硼磁体由主相Nd2Fe14B、富Nd相和富B相组成。
23.如权利要求1-9任一项所述的制备方法,其特征在于,所述烧结钕铁硼磁体在涂覆可膨胀涂料前还包括对其进行表面预处理的步骤。
24.如权利要求23所述的制备方法,其特征在于,所述表面预处理包括对烧结钕铁硼磁体的表面进行化学超声除油、酸洗、水洗的过程。
25.如权利要求24所述的制备方法,其特征在于,所述除油过程中采用的除油液为碱及表面活性剂的复合溶液。
26.如权利要求25所述的制备方法,其特征在于,所述碱为氢氧化钠或碳酸钠,其浓度为10-20g/L。
27.如权利要求26所述的制备方法,其特征在于,所述表面活性剂为十二烷基磺酸钠或十二烷基硫酸钠,其浓度为2-6g/L。
28.如权利要求25-27任一项所述的制备方法,其特征在于,所述除油液温度为30-70℃,所述除油时间1-20min。
29.如权利要求24所述的制备方法,其特征在于,所述酸洗采用的酸选自硝酸或柠檬酸水溶液。
30.如权利要求24所述的制备方法,其特征在于,所述酸洗采用的酸液浓度为5-30wt%,所述酸洗的时间为5-30s。
31.如权利要求24所述的制备方法,其特征在于,所述涂覆方式选自喷涂、印刷、浸沾、涂抹。
32.如权利要求31所述的制备方法,其特征在于,所述涂覆方式为喷涂。
33.如权利要求1-9任一项所述的制备方法,其特征在于,所述可膨胀涂料的涂覆的厚度为80-150μm。
34.一种可膨胀烧结钕铁硼磁体,其由权利要求1-33任一项所述的制备方法制备。
35.权利要求34所述的可膨胀烧结钕铁硼磁体在电机转子中的应用。
36.一种电机转子工件,其特征在于,所述电机转子工件含有权利要求34所述的可膨胀烧结钕铁硼磁体。
37.一种如权利要求36所述电机转子工件的装配方法,其特征在于,所述装配方法包括将权利要求34所述的可膨胀烧结钕铁硼磁体装配到磁钢槽中,经加热膨胀处理,制得所述电机转子工件。
38.如权利要求37所述电机转子工件的装配方法,其特征在于,所述加热膨胀处理采用二段式升温法,第一膨胀阶段的膨胀温度为110℃-160℃,第一膨胀阶段的升温速率为5℃/min-15℃/min;
所述加热膨胀处理的第二膨胀温度为180℃-210℃,第二膨胀阶段的升温速率为30-60℃/min。
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