CN115383122A - 一种2:17型烧结钐钴永磁体的氢碎制备方法 - Google Patents
一种2:17型烧结钐钴永磁体的氢碎制备方法 Download PDFInfo
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Abstract
本发明涉及一种2:17型烧结钐钴永磁体的氢碎制备方法,属于磁性材料制备技术领域,解决钐钴合金吸氢及脱氢难、磁体取向差的技术问题,包括以下步骤:S1、称取钐钴永磁体合金原料,制备合金铸锭或者速凝薄带合金片并机械破碎,得到合金颗粒;S2、将合金颗粒与催化剂CuF2粉末混合,氢碎处理后制得氢碎粉末;S3、氢碎粉末经过气流磨制粉制得钐钴合金粉末;S4、钐钴合金粉末经磁场取向成型、冷等静压压制成型,制得生坯;S5、生坯经烧结固溶和时效处理制得2:17型烧结钐钴永磁体。本发明提供的制备方法有效降低了钐钴合金的吸放氢压力和温度,易于操作控制和产业化,并且降低了能耗,制备出的烧结钐钴磁体磁性能优异。
Description
技术领域
本发明属于磁性材料制备技术领域,具体涉及一种2:17型烧结钐钴永磁体的氢碎制备方法。
背景技术
稀土永磁材料自20世纪60年代问世以来,以其优秀的磁性能而备受青睐,在科研、生产和应用方面都得到了迅速发展。其中作为第二代稀土永磁材料的2:17型钐钴永磁材料,因具有优异的磁性能、高的居里温度、良好的温度稳定性以及出色的抗氧化和抗腐蚀性等特点,被广泛应用于国防军工、航空航天、高精度仪表、医疗器械、微波器件、传感器、各种磁性传动装置、高端电机等众多领域。
氢破碎作为稀土永磁材料的高效制粉方法已广泛应用于烧结Nd-Fe-B永磁材料的制备,通过氢***理,钕铁硼合金速凝薄带与氢发生反应生成氢化物,由于氢化物生成时晶格膨胀,所产生的巨大应力使NdFeB晶体内产生许多微裂纹,材料变得疏松乃至成为粗粉末,经过进一步气流磨制粉,可以形成单晶颗粒,有效提高了终态磁体取向,改善了磁体综合磁性能。而2:17型烧结钐钴合金铸锭由于存在吸放氢困难等问题,因此生产上普遍采用机械破碎+球磨/气流磨的方法来制备合金粉末。由于机械破碎+球磨/气流磨制粉破碎效果较差,使许多钐钴合金粉末颗粒不能破碎为单晶,导致钐钴磁体取向度差,磁性能降低。
现有技术中,专利“一种钐钴系烧结材料的制备方法”(授权公告号:CN102651263B)是采用将合金铸带进行氢化歧化反应,再经气流磨制粉来制备磁粉,其目的是保证晶粒完整,降低粉末氧化,从而保证了磁体的磁性能。专利“一种烧结钐钴永磁体材料及其制备方法”(授权公告号:CN104637642B)是在熔炼炉中对铸锭进行吸氢,再进行气流磨制粉,从而节约了生产步骤,降低能耗。另外,专利“一种钐钴永磁材料的制备方法”(授权公告号:CN105304249B),是对两种成分合金铸锭分别吸氢及脱氢,再分别进行气流磨制粉,之后再进行混粉来制备钐钴永磁体。
发明内容
为了克服现有技术的不足,解决钐钴合金吸氢及脱氢难、磁体取向差的技术问题,本发明提供一种利用催化剂促进氢碎制粉来制备2:17型烧结钐钴磁体的方法,从而降低能耗,提高氢碎效率,改善磁体取向度,有效提高2:17型钐钴磁体的综合磁性能。
为了实现以上目的,本发明通过以下技术方案予以实现。
一种2:17型烧结钐钴永磁体的氢碎制备方法,包括以下步骤:
S1、首先,按照如下成分及其重量百分比称取钐钴永磁体合金原料:(Sm1-xRex):25%~26.5%,Fe:6.5%~22.5%,Zr:2.0%~3.5%,Cu:3.5%~5.5%,其余为Co;其中,0≤x≤0.4,Re为Pr、Nd、Gd、Dy、Tb、Er、Y、Ho中的一种或几种;
然后,将称取的钐钴永磁体合金原料在中频感应熔炼炉中熔炼,制得合金铸锭;或者将称取的钐钴永磁体合金原料在真空速凝薄带炉中熔炼,制得速凝薄带合金片;
最后,将合金铸锭或者速凝薄带合金片机械破碎为粒径为0.5mm~3mm的合金颗粒;
S2、将步骤S1制备的合金颗粒采用催化氢碎的方法制成平均粒径为10μm~500μm的氢碎粉末,所述催化氢碎的方法包括以下步骤:
S2-1、将步骤S1制备的合金颗粒与催化剂CuF2粉充分混合,混粉时间为0.5h~1h;其中合金颗粒与催化剂CuF2粉的质量百分比为:90%~99%合金颗粒,其余为催化剂CuF2粉末;
S2-2、将步骤S2-1制备的混合粉末在氢碎炉中依次进行活化处理与循环吸放氢处理,制得氢碎粉末;
S3、采用气流磨的方法将步骤S2制备的氢碎粉末制成平均粒径为2.5μm~5μm的钐钴合金粉末;
S4、将步骤S3制备的钐钴合金粉末在空气氛围中称重,然后在大于1.5T磁场下取向成型,最后再在230MPa压力下进行冷等静压压制成型,制得生坯;
S5、首先,将步骤S4制得的生坯在1205℃~1220℃温度条件中烧结0.5h~2h;然后,将烧结后的坯料随炉冷却到1140℃~1190℃进行固溶处理,保温时间为2h~10h,固溶处理后快速风冷至室温;最后,坯料再次加热至800℃~850℃,保温8h~20h后控温冷却到400℃,保温1h后风冷至室温,制得2:17型烧结钐钴永磁体。
进一步地,在所述步骤S1中,制得的合金铸锭的厚度为8mm~12mm,制得的速凝薄带合金片的厚度为0.5mm~1mm。
进一步地,在所述步骤S2-1中,混粉过程是在高纯氮气气氛保护下进行的。
进一步地,在所述步骤S2-2中,循环吸氢温度为20℃~80℃,吸氢氢气压力为0.2MPa~1MPa,吸氢时间1h~2h;循环放氢温度为20℃~80℃;吸放氢循环次数为1次~3次。
进一步地,在所述步骤S2-2中,脱氢后合金粉末的氢含量为500ppm~2000ppm。
进一步地,在所述步骤S5中,烧结升温过程中在400℃保温0.5h~1h,进一步脱去磁体中残余氢气。
进一步地,在所述步骤S5中,控温冷却降温速度为0.5℃/min~1℃/min。
与现有技术相比本发明的有益效果为:
1、本发明通过采用催化氢碎法,将钐钴合金颗粒与催化剂CuF2粉末混合后进行氢碎。CuF2粉末的加入不仅可以加速氢分子在合金颗粒表面解离成氢原子,进而促进合金颗粒吸氢,还可以与钐钴合金发生氧化还原反应生成稀土氟化物,进而促进氢碎过程,有效降低了钐钴合金的吸放氢温度及吸氢压力,从而降低能耗,提升了吸氢效率;
2、本发明利用催化氢碎法,使合金可以形成Sm2Co17Hx和SmCo5Hy间隙化合物,引起晶格膨胀破碎,形成单晶颗粒,有利于磁体成型过程中取向,提高了磁体剩磁和磁能积;
3、本发明通过添加催化剂CuF2粉末,使其在氢碎过程中与钐钴合金发生氧化还原反应,生成Cu单质,并且Cu单质均匀分布,在之后热处理过程中可以改善晶界处胞状组织结构及胞壁处Cu元素分布,从而可以提高钐钴磁体的膝点磁场和内禀矫顽力。
总之,本发明提供的制备方法易于操作控制和产业化,制备出的烧结钐钴磁体性能优异。
附图说明
图1为本发明使用催化氢碎法制备钐钴磁体的工艺流程图。
具体实施方式
本发明提供了一种2:17型烧结钐钴永磁体的氢碎制备方法,包括以下步骤:
S1、首先,按照如下成分及其重量百分比称取钐钴永磁体合金原料:(Sm1-xRex):25%~26.5%,Fe:6.5%~22.5%,Zr:2.0%~3.5%,Cu:3.5%~5.5%,其余为Co;其中,0≤x≤0.4,Re为Pr、Nd、Gd、Dy、Tb、Er、Y、Ho中的一种或几种;
然后,将称取的钐钴永磁体合金原料在中频感应熔炼炉中熔炼,制得合金铸锭;或者将称取的钐钴永磁体合金原料在真空速凝薄带炉中熔炼,制得速凝薄带合金片;
最后,将合金铸锭或者速凝薄带合金片机械破碎为粒径为0.5mm~3mm的合金颗粒;
熔炼制备的合金铸锭或速凝薄带合金片中均包含了2:17H相和1:5H相,其中2:17H相有相对较高的Fe、Co含量,1:5H相含有相对较高的稀土含量,其均可以在后续吸氢过程中吸收一定的H原子,生成间隙氢化物,并且发生晶格膨胀,使合金易粉碎,因此,合金铸锭或速凝薄带合金片均可以用做氢碎的基础合金。将合金铸锭或者速凝薄带合金片机械破碎为粒径为0.5~3mm的合金颗粒,将更有利于合金吸放氢破碎。
S2、将步骤S1制备的合金颗粒采用催化氢碎的方法制成平均粒径为10μm~500μm的氢碎粉末,所述催化氢碎的方法包括以下步骤:
S2-1、将步骤S1制备的合金颗粒与催化剂CuF2粉充分混合,混粉时间为0.5h~1h;其中合金颗粒与催化剂CuF2粉的质量百分比为:90%~99%合金颗粒,其余为催化剂CuF2粉末;
CuF2粉末不仅能加速氢分子在合金颗粒表面解离成氢原子来促进合金颗粒吸氢,还可以与钐钴合金发生氧化还原反应生成稀土氟化物来促进氢碎过程;此外,CuF2粉末还能与钐钴合金发生氧化还原反应,生成单质Cu。单质Cu可以在热处理过程中改善晶界处胞状组织结构及胞壁处Cu元素分布,从而提高磁体膝点磁场和内禀矫顽力;
S2-2、将步骤S2-1制备的混合粉末在氢碎炉中依次进行活化处理与循环吸放氢处理,制得氢碎粉末;
活化处理的目的是使合金颗粒可以最大限度的循环吸放氢。当充入一定量的氢气时,受金属原子作用,H-H键解离,原子态的氢进入合金内部晶格间隙生成氢化物Sm2Co17Hx和SmCo5Hy,引起晶格膨胀破碎,再配合之后的气流磨制粉,可以制备出接近单晶颗粒的合金粉末。
S3、采用气流磨的方法将步骤S2制备的氢碎粉末制成平均粒径为2.5μm~5μm的钐钴合金粉末。
S4、将步骤S3制备的钐钴合金粉末在空气氛围中称重,然后在大于1.5T磁场下取向成型,最后再在230MPa压力下进行冷等静压压制成型,制得生坯;由于加入了催化氢碎方法,因此更容易形成单晶合金粉末,有利于粉末磁场取向成型,提高磁体取向度。
S5、首先,将步骤S4制得的生坯在1205℃~1220℃温度条件中烧结0.5h~2h;然后,将烧结后的坯料随炉冷却到1140℃~1190℃进行固溶处理,保温时间为2h~10h,固溶处理后快速风冷至室温;最后,坯料再次加热至800℃~850℃,保温8h~20h后控温冷却到400℃,保温1h后风冷至室温,制得2:17型烧结钐钴永磁体。
进一步地,在所述步骤S1中,制得的合金铸锭的厚度为8mm~12mm,制得的速凝薄带合金片的厚度为0.5mm~1mm,有利于合金获得理想的显微组织结构和相组成,使其在后续过程中更好地进行氢破碎。
进一步地,在所述步骤S2-1中,混粉过程是在高纯氮气气氛保护下进行的,防止合金颗粒氧化。
进一步地,在所述步骤S2-2中,循环吸氢温度为20℃~80℃,吸氢氢气压力为0.2MPa~1MPa,吸氢时间1h~2h;循环放氢温度为20℃~80℃;吸放氢循环次数为1次~3次。由于加入催化剂CuF2粉末,钐钴合金颗粒可以在较低的温度和压力下吸氢,并且放氢温度也较低。通过进行循环吸放氢,可以使合金颗粒更加充分有效破碎。
进一步地,在所述步骤S2-2中,脱氢后合金粉末的氢含量为500ppm~2000ppm,可以在后续称料、磁场取向成型、冷等静压过程中防止钐钴合金粉末氧化,从而避免磁体因为氧含量过高而造成的磁性能变差。此外,500 ppm ~2000ppm的较低氢含量可以在400℃烧结保温中完全排除,从而不影响最终磁体的性能。
进一步地,在所述步骤S5中,烧结升温过程中在400℃保温0.5h~1h,进一步脱去磁体中残余氢气。
进一步地,在所述步骤S5中,控温冷却降温速度为0.5℃/min~1℃/min。控温冷却降温速度保持0.5~1℃/min缓慢冷却,可以使Cu元素向胞壁处富集,从而提高胞壁对畴壁的钉扎力,有利于磁体获得高矫顽力。
以下实施例用于说明本发明,但不用来限制本发明的范围。若未特别指明,实施例均按照常规实验条件。
实施例1
一种2:17型烧结钐钴永磁体的氢碎制备方法,包括以下步骤:
S1、首先,按照如下成分及其重量百分比称取钐钴永磁体合金原料:Sm:25%、Fe:15%、Zr:3%、Cu:3.5%、Co:53.5%;然后,将称取的钐钴永磁体合金原料在中频感应熔炼炉中熔炼制得厚度约为10mm的合金铸锭;最后,将合金铸锭机械破碎为粒径为0.5mm~3mm的合金颗粒;
S2、将步骤S1制备的合金颗粒采用催化氢碎法制成平均粒径为10μm~500μm的氢碎粉末,所述催化氢碎法制粉包括以下步骤:
S2-1、将步骤S1制备的合金颗粒与催化剂CuF2粉充分混合,混粉时间为1h;其中合金颗粒与催化剂CuF2粉的质量百分比为:95%合金颗粒,5%催化剂CuF2粉末;
S2-2、将步骤S2-1制备的混合粉末在氢碎炉中依次进行活化处理与循环吸放氢处理,循环吸氢温度为60℃,吸氢氢气压力为0.2MPa,吸氢时间1.5h;循环放氢温度为80℃;吸放氢循环次数为2次,制得氢碎粉末;
S3、采用气流磨的方法将步骤S2制备的氢碎粉末制成平均粒径为3.8μm的钐钴合金粉末;
S4、将步骤S3制备的钐钴合金粉末在空气氛围中称重,然后在大于1.5T磁场下取向成型,最后再在230MPa压力下进行冷等静压压制成型,制得生坯;
S5、首先,将步骤S4制得的生坯在1210℃温度条件中烧结1h;然后,烧结后的坯料随炉冷却到1170℃进行固溶处理,保温时间为4h,固溶处理后快速风冷至室温;最后,坯料再次加热至820℃,保温15h后以0.5℃/min速度冷却到400℃,保温1h后风冷至室温,得到2:17型烧结钐钴永磁体。
本实施例1制备的2:17型烧结钐钴永磁体磁性能为:剩磁Br=10.77kGs,磁能积(BH)m=27.63MGOe,内禀矫顽力Hcj=38.17kOe。
实施例2
一种2:17型烧结钐钴永磁体的氢碎制备方法,包括以下步骤:
S1、首先,按照如下成分及其重量百分比称取钐钴永磁体合金原料:Sm:26.5%、Fe:6.5%、Zr:3.5%、Cu:3.5%、Co:60%;然后,将称取的钐钴永磁体合金原料在中频感应熔炼炉中熔炼制得厚度约为10mm的合金铸锭;最后,将合金铸锭机械破碎为粒径为0.5mm~3mm的合金颗粒;
S2、将步骤S1制备的合金颗粒采用催化氢碎法制成平均粒径为10μm~500μm的氢碎粉末,所述催化氢碎法制粉包括以下步骤:
S2-1、将步骤S1制备的合金颗粒与催化剂CuF2粉充分混合,混粉时间为1h;其中合金颗粒与催化剂CuF2粉的质量百分比为:90%合金颗粒,10%催化剂CuF2粉末;
S2-2、将步骤S2-1制备的混合粉末在氢碎炉中依次进行活化处理与循环吸放氢处理,循环吸氢温度为50℃,吸氢氢气压力为0.7MPa,吸氢时间1h;循环放氢温度为70℃;吸放氢循环次数为1次,制得氢碎粉末;
S3、采用气流磨的方法将步骤S2制备的氢碎粉末制成平均粒径为4.2μm的钐钴合金粉末;
S4、将步骤S3制备的钐钴合金粉末在空气氛围中称重,然后在大于1.5T磁场下取向成型,最后再在230MPa压力下进行冷等静压压制成型,制得生坯;
S5、首先,将步骤S4制得的生坯在1220℃温度条件中烧结1h;然后,烧结后的坯料随炉冷却到1180℃进行固溶处理,保温时间为4h,固溶处理后快速风冷至室温;最后,坯料再次加热至830℃,保温10h后以0.5℃/min速度冷却到400℃,保温1h后风冷至室温,得到2:17型烧结钐钴永磁体。
本实施例2制备的2:17型烧结钐钴永磁体磁性能为:剩磁Br=9.38kGs,磁能积(BH)m=20.1MGOe,内禀矫顽力Hcj=36.83kOe。
实施例3
一种2:17型烧结钐钴永磁体的氢碎制备方法,包括以下步骤:
S1、首先,按照如下成分及其重量百分比称取钐钴永磁体合金原料:Sm:25.5%、Fe:20%、Zr:2.5%、Cu:4%、Co:48%;然后,将称取的钐钴永磁体合金原料在真空速凝薄带炉中熔炼制得厚度约为0.6mm的速凝薄带合金片;最后,将速凝薄带合金片机械破碎为粒径为0.5mm~3mm的合金颗粒;
S2、将步骤S1制备的合金颗粒采用催化氢碎法制成平均粒径为10μm~500μm的氢碎粉末,所述催化氢碎法制粉包括以下步骤:
S2-1、将步骤S1制备的合金颗粒与催化剂CuF2粉充分混合,混粉时间为0.5h;其中合金颗粒与催化剂CuF2粉的质量百分比为:99%合金颗粒,1%催化剂CuF2粉末;
S2-2、将步骤S2-1制备的混合粉末在氢碎炉中依次进行活化处理与循环吸放氢处理,循环吸氢温度为80℃,吸氢氢气压力为1MPa,吸氢时间2h;循环放氢温度为80℃;吸放氢循环次数为3次,制得氢碎粉末;
S3、采用气流磨的方法将步骤S2制备的氢碎粉末制成平均粒径为3.5μm的钐钴合金粉末;
S4、将步骤S3制备的钐钴合金粉末在空气氛围中称重,然后在大于1.5T磁场下取向成型,最后再在230MPa压力下进行冷等静压压制成型,制得生坯;
S5、首先,将步骤S4制得的生坯在1205℃温度条件中烧结1h;然后,烧结后的坯料随炉冷却到1150℃进行固溶处理,保温时间为10h,固溶处理后快速风冷至室温;最后,坯料再次加热至830℃,保温12h后以1℃/min速度冷却到400℃,保温1h后风冷至室温,得到2:17型烧结钐钴永磁体。
本实施例3制备的2:17型烧结钐钴永磁体磁性能为:剩磁Br=11.75kGs,磁能积(BH)m=32.84MGOe,内禀矫顽力Hcj=29.5kOe。
实施例4
一种2:17型烧结钐钴永磁体的氢碎制备方法,包括以下步骤:
S1、首先,按照如下成分及其重量百分比称取钐钴永磁体合金原料Sm:20%、Gd:5.3%、Fe:15.5%、Zr:2.8%、Cu:5%、Co:51.4%;然后,将称取的钐钴永磁体合金原料在真空速凝薄带炉中熔炼制得厚度约为1mm的速凝薄带合金片;最后,将速凝薄带合金片机械破碎为粒径为0.5mm~3mm的合金颗粒;
S2、将步骤S1制备的合金颗粒采用催化氢碎法制成平均粒径为10μm~500μm的氢碎粉末,所述催化氢碎法制粉包括以下步骤:
S2-1、将步骤S1制备的合金颗粒与催化剂CuF2粉充分混合,混粉时间为0.5h;其中合金颗粒与催化剂CuF2粉的质量百分比为:97%合金颗粒,3%催化剂CuF2粉末;
S2-2、将步骤S2-1制备的混合粉末在氢碎炉中依次进行活化处理与循环吸放氢处理,循环吸氢温度为70℃,吸氢氢气压力为0.7MPa,吸氢时间1.5h;循环放氢温度为70℃;吸放氢循环次数为2次,制得氢碎粉末;
S3、采用气流磨的方法将步骤S2制备的氢碎粉末制成平均粒径为3.6μm的钐钴合金粉末;
S4、将步骤S3制备的钐钴合金粉末在空气氛围中称重,然后在大于1.5T磁场下取向成型,最后再在230MPa压力下进行冷等静压压制成型,制得生坯;
S5、首先,将步骤S4制得的生坯在1210℃温度条件中烧结1h;然后,烧结后的坯料随炉冷却到1180℃进行固溶处理,保温时间为4h,固溶处理后快速风冷至室温;最后,坯料再次加热至830℃,保温10h后以0.5℃/min速度冷却到400℃,保温1h后风冷至室温,得到2:17型烧结钐钴永磁体。
本实施例4制备的2:17型烧结钐钴永磁体磁性能为:剩磁Br=10.3kGs,磁能积(BH)m=24.56MGOe,内禀矫顽力Hcj=37.13kOe。
实施例5
一种2:17型烧结钐钴永磁体的氢碎制备方法,包括以下步骤:
S1、首先,按照如下成分及其重量百分比称取钐钴永磁体合金原料:Sm:22%、Pr:3%、Dy:0.4%、Fe:17%、Zr:2.5%、Cu:5.5%、Co:49.6%;然后,将称取的钐钴永磁体合金原料在真空速凝薄带炉中熔炼制得厚度约为0.8mm的速凝薄带合金片;最后,将速凝薄带合金片机械破碎为粒径为0.5mm~3mm的合金颗粒;
S2、将步骤S1制备的合金颗粒采用催化氢碎法制成平均粒径为10μm~500μm的氢碎粉末,所述催化氢碎法制粉包括以下步骤:
S2-1、将步骤S1制备的合金颗粒与催化剂CuF2粉充分混合,混粉时间为0.5h;其中合金颗粒与催化剂CuF2粉的质量百分比为:99%合金颗粒,1%催化剂CuF2粉末;
S2-2、将步骤S2-1制备的混合粉末在氢碎炉中依次进行活化处理与循环吸放氢处理,循环吸氢温度为80℃,吸氢氢气压力为0.8MPa,吸氢时间2h;循环放氢温度为80℃;吸放氢循环次数为2次,制得氢碎粉末;
S3、采用气流磨的方法将步骤S2制备的氢碎粉末制成平均粒径为4.2μm的钐钴合金粉末;
S4、将步骤S3制备的钐钴合金粉末在空气氛围中称重,然后在大于1.5T磁场下取向成型,最后再在230MPa压力下进行冷等静压压制成型,制得生坯;
S5、首先,将步骤S4制得的生坯在1215℃温度条件中烧结1h;然后,烧结后的坯料随炉冷却到1180℃进行固溶处理,保温时间为8h,固溶处理后快速风冷至室温;最后,坯料再次加热至830℃,保温15h后以0.5℃/min速度冷却到400℃,保温1h后风冷至室温,得到2:17型烧结钐钴永磁体。
本实施例5制备的2:17型烧结钐钴永磁体磁性能为:剩磁Br=11.03kGs,磁能积(BH)m=28.79MGOe,内禀矫顽力Hcj=21.58kOe。
实施例6
一种2:17型烧结钐钴永磁体的氢碎制备方法,包括以下步骤:
S1、首先,按照如下成分及其重量百分比称取钐钴永磁体合金原料:Sm:25.5%、Fe:18%、Zr:2.5%、Cu:4.5%、Co:49.5%;然后,将称取的钐钴永磁体合金原料在真空速凝薄带炉中熔炼制得厚度约为0.5mm的速凝薄带合金片;最后,将速凝薄带合金片机械破碎为粒径为0.5mm~3mm的合金颗粒;
S2、将步骤S1制备的合金颗粒采用催化氢碎法制成平均粒径为10μm~500μm的氢碎粉末,所述催化氢碎法制粉包括以下步骤:
S2-1、将步骤S1制备的合金颗粒与催化剂CuF2粉充分混合,混粉时间为0.5h;其中合金颗粒与催化剂CuF2粉的质量百分比为:98%合金颗粒,2%催化剂CuF2粉末;
S2-2、将步骤S2-1制备的混合粉末在氢碎炉中依次进行活化处理与循环吸放氢处理,循环吸氢温度为60℃,吸氢氢气压力为0.8MPa,吸氢时间2h;循环放氢温度为70℃;吸放氢循环次数为3次,制得氢碎粉末;
S3、采用气流磨的方法将步骤S2制备的氢碎粉末制成平均粒径为4.1μm的钐钴合金粉末;
S4、将步骤S3制备的钐钴合金粉末在空气氛围中称重,然后在大于1.5T磁场下取向成型,最后再在230MPa压力下进行冷等静压压制成型,制得生坯;
S5、首先,将步骤S4制得的生坯在1210℃温度条件中烧结1h;然后,烧结后的坯料随炉冷却到1150℃进行固溶处理,保温时间为10h,固溶处理后快速风冷至室温;最后,坯料再次加热至830℃,保温12h后以1℃/min速度冷却到400℃,保温1h后风冷至室温,得到2:17型烧结钐钴永磁体。
本实施例6制备的2:17型烧结钐钴永磁体磁性能为:剩磁Br=11.34kGs,磁能积(BH)m=30.37MGOe,内禀矫顽力Hcj=35.6kOe。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以所述权利要求的保护范围为准。
Claims (7)
1.一种2:17型烧结钐钴永磁体的氢碎制备方法,其特征在于,包括以下步骤:
S1、首先,按照如下成分及其重量百分比称取钐钴永磁体合金原料:(Sm1-xRex):25%~26.5%,Fe:6.5%~22.5%,Zr:2.0%~3.5%,Cu:3.5%~5.5%,其余为Co;其中,0≤x≤0.4,Re为Pr、Nd、Gd、Dy、Tb、Er、Y、Ho中的一种或几种;
然后,将称取的钐钴永磁体合金原料在中频感应熔炼炉中熔炼,制得合金铸锭;或者将称取的钐钴永磁体合金原料在真空速凝薄带炉中熔炼,制得速凝薄带合金片;
最后,将合金铸锭或者速凝薄带合金片机械破碎为粒径为0.5mm~3mm的合金颗粒;
S2、将步骤S1制备的合金颗粒采用催化氢碎的方法制成平均粒径为10μm~500μm的氢碎粉末,所述催化氢碎的方法包括以下步骤:
S2-1、将步骤S1制备的合金颗粒与催化剂CuF2粉充分混合,混粉时间为0.5h~1h;其中合金颗粒与催化剂CuF2粉的质量百分比为:90%~99%合金颗粒,其余为催化剂CuF2粉末;
S2-2、将步骤S2-1制备的混合粉末在氢碎炉中依次进行活化处理与循环吸放氢处理,制得氢碎粉末;
S3、采用气流磨的方法将步骤S2制备的氢碎粉末制成平均粒径为2.5μm~5μm的钐钴合金粉末;
S4、将步骤S3制备的钐钴合金粉末在空气氛围中称重,然后在大于1.5T磁场下取向成型,最后再在230MPa压力下进行冷等静压压制成型,制得生坯;
S5、首先,将步骤S4制得的生坯在1205℃~1220℃温度条件中烧结0.5h~2h;然后,将烧结后的坯料随炉冷却到1140℃~1190℃进行固溶处理,保温时间为2h~10h,固溶处理后快速风冷至室温;最后,坯料再次加热至800℃~850℃,保温8h~20h后控温冷却到400℃,保温1h后风冷至室温,制得2:17型烧结钐钴永磁体。
2.根据权利要求1所述的一种2:17型烧结钐钴永磁体的氢碎制备方法,其特征在于:在所述步骤S1中,制得的合金铸锭的厚度为8mm~12mm,制得的速凝薄带合金片的厚度为0.5mm~1mm。
3.根据权利要求1所述的一种2:17型烧结钐钴永磁体的氢碎制备方法,其特征在于:在所述步骤S2-1中,混粉过程是在高纯氮气气氛保护下进行的。
4.根据权利要求1所述的一种2:17型烧结钐钴永磁体的氢碎制备方法,其特征在于:在所述步骤S2-2中,循环吸氢温度为20℃~80℃,吸氢氢气压力为0.2MPa~1MPa,吸氢时间1h~2h;循环放氢温度为20℃~80℃;吸放氢循环次数为1次~3次。
5.根据权利要求1所述的一种2:17型烧结钐钴永磁体的氢碎制备方法,其特征在于:在所述步骤S2-2中,脱氢后合金粉末的氢含量为500ppm~2000ppm。
6.根据权利要求1所述的一种2:17型烧结钐钴永磁体的氢碎制备方法,其特征在于:在所述步骤S5中,烧结升温过程中在400℃保温0.5h~1h。
7.根据权利要求1所述的一种2:17型烧结钐钴永磁体的氢碎制备方法,其特征在于:在所述步骤S5中,控温冷却降温速度为0.5℃/min~1℃/min。
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