CN108723355A - 放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法和应用 - Google Patents
放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法和应用 Download PDFInfo
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- 238000005245 sintering Methods 0.000 title claims abstract description 75
- 239000002131 composite material Substances 0.000 title claims abstract description 69
- 229910017709 Ni Co Inorganic materials 0.000 title claims abstract description 60
- 229910003267 Ni-Co Inorganic materials 0.000 title claims abstract description 60
- 229910003262 Ni‐Co Inorganic materials 0.000 title claims abstract description 60
- 230000005389 magnetism Effects 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 47
- 239000006247 magnetic powder Substances 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011812 mixed powder Substances 0.000 claims abstract description 14
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004411 aluminium Substances 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 3
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明属于复合材料制备技术领域,具体涉及放电等离子烧结制备磁性Sm2Co17/Al‑Ni‑Co复合材料的方法和应用。本发明采用放电等离子烧结制备磁性Sm2Co17/Al‑Ni‑Co复合材料的方法具体如下:首先将Sm2Co17磁粉与铝粉、钴粉、镍粉按比例混合均匀,加入乙醇,在球磨机中湿磨,真空干燥,得到混合粉体;然后用冷等静压压制成型;将得到的复合材料坯锭放入石墨模具中,在放电等离子烧结炉中进行真空烧结,烧结完成后冷却至室温,即得到Sm2Co17/Al‑Ni‑Co复合材料;将复合材料进行充磁,得到磁性Sm2Co17/Al‑Ni‑Co复合材料。本发明的磁性Sm2Co17/Al‑Ni‑Co复合材料磁性较强,永磁效果更好;复合材料组织均匀,结构稳定,具有更强的抗拉强度、屈服强度。本发明的制备工艺过程简单,可控性高,烧结快速、烧结温度低,有望用于生产中。
Description
技术领域
本发明属于复合材料制备技术领域,具体涉及放电等离子烧结制备磁性 Sm2Co17/Al-Ni-Co复合材料的方法和应用。
背景技术
制备磁性复合材料大多采用熔炼法和粉末烧结法制备,熔炼法工序复杂,用时较长,加 热温度高,反应不易控制等缺点。用粉末冶金方法制造的磁性材料是磁性材料领域的一个重 要组成部分,近年来粉末冶金磁性材料飞速发展,尤其是被称为永磁王的Nd-Fe-B永磁材料, 只有采用粉末冶金的工艺才能充分发挥其优异的性能。但传统的粉末冶金法烧结时间长、烧 结温度场不均匀,不利于得到高密度、显微组织细小的烧结体,容易产生偏析等多种缺陷, 影响材料使用性能。
放电等离子烧结(SPS)是一种快速、节能、环保的材料制备加工新技术;该技术是在 加压粉末颗粒间直接通入脉冲电能,由火花放电瞬间产生的等离子体加热颗粒,使烧结体内 各个颗粒均匀地产生焦耳热,进而使颗粒表面活化,实现超快速致密化烧结;与传统的热压、 热等静压技术相比,具有烧结快速、烧结温度低、烧结机理特殊、无需粉末预成形、可直接 烧成致密体等优点。
Al-Ni-Co材料永磁且具有剩磁高、居里温度高且剩磁温度系数小的优点,多用于电气仪 表和通讯机器等要求高可靠性的领域中;根据生产工艺的不同Al-Ni-Co永磁分为铸造磁体和 粉末烧结磁体;铸造铝镍钴型永磁合金由于具有较高的永磁性能和良好的温度稳定性能,因 而在仪表、电子、电力工业和尖端科学技术中得到广泛的应用;由于已有技术的粉末烧结磁 体较之铸造磁体具有材料利用率高、成分偏析小、磁特性波动小的优点,所以粉末烧结磁体 正逐步代替铸造磁体,但总体磁特性略低于铸造磁体,同时粉末烧结工序繁杂,周期较长, 故对工艺控制的要求较高,容易产生缺陷,如气孔、变形、夹杂脏化、密度偏低;因此提高 粉末烧结磁体的磁特性和降低工艺要求,提高产品质量一直是生产上追求的目标。
目前,国内外使用的2:17型Sm-Co磁体最广泛的一类是Sm2(Co Fe Cu Zr)17型合金; 该类磁体居里温度约为820~870℃,剩磁温度系数约为-0.03%/℃,矫顽力温度系数约为 -0.21%/℃,工作温度可高达350℃左右;近年来,随着航空航天技术的高速发展,急需工作 温度更高的磁体,来提高新一代航天器上的发动机机组及其电子元器件的可靠性和安全性, 2:17型Sm-Co永磁体因其较高的居里温度和磁性能成为了首选材料;但其合金中含有大量 的稀缺资源Sm和战略储备资源Co,使其制备成本大大提高,极大的限制了它的产业化发展。
发明内容
本发明的目的在于克服现有技术中存在的缺陷,如:Al-Ni-Co永磁体传统粉末烧结工艺 复杂,周期较长,容易产生缺陷,如气孔、变形、夹杂脏化、密度偏低,磁特性较差,同时 Sm2(Co Fe Cu Zr)17型合金由于其合金中含有大量的稀缺资源Sm和战略储备资源Co,极大 的限制了它的产业化发展等,本发明提供了一种放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co 复合材料的方法。
具体的,本发明采用的技术方案为:
(1)球磨:
将Sm2Co17磁粉与铝粉、钴粉、镍粉按比例混合均匀,加入乙醇,在球磨机中湿磨,将球磨后的粉末放入真空干燥箱中烘干,得到混合粉体;
(2)压制成型:
将步骤(1)中的混合粉体用冷等静压压制成型,得到致密的复合材料坯锭;
(3)放电等离子烧结:
将复合材料坯锭放入石墨模具中,在放电等离子烧结炉中进行真空烧结,烧结完成后冷 却至室温后取出样品,即得到Sm2Co17/Al-Ni-Co复合材料;
(4)充磁:
将步骤(3)得到的Sm2Co17/Al-Ni-Co复合材料放入充磁机充磁,得到磁性Sm2Co17/Al-Ni-Co复合材料;
优选地,步骤(1)中,所述的Sm2Co17磁粉、铝粉、钴粉、镍粉的质量比为1-3:1-3:1-3:1-5;
优选地,步骤(1)中,所述的球磨时间为10-12h;
优选地,步骤(2)中,所述的冷等静压压强为90-100MPa,保压时间为2-5min;
优选地,步骤(3)中,所述烧结温度为450-500℃,升温速率为40-60℃/min,烧结压力为30-40MPa,烧结时间为2-4min;冷却时需要充氩气。
本发明提供了一种磁性Sm2Co17/Al-Ni-Co复合材料的应用,所述磁性Sm2Co17/Al-Ni-Co 复合材料用于生产永磁转子或永磁磁铁。
与现有技术相比较,本发明的有益效果体现如下:
(1)本发明的磁性复合材料,采用Sm2Co17磁粉与Al-Ni-Co两种磁性材料复合,比单一的Al-Ni-Co材料磁性更强,永磁效果更好;
(2)相较于传统粉末烧结工艺,放电等离子烧结技术的优势在于烧结快速、烧结温度低、 烧结机理特殊,整个工艺过程简单,可控性高,解决了Al-Ni-Co永磁体传统粉末烧结工艺复 杂的问题,所制备的复合材料组织均匀,结构稳定,具有更强的抗拉强度、屈服强度和更好 的磁特性,解决了Al-Ni-Co永磁体磁特性较差的问题,本发明制备的Sm2Co17/Al-Ni-Co复合 材料兼备Al-Ni-Co永磁体和Sm2Co17的优点。
(3)和单一的Sm2(Co Fe Cu Zr)17型合金相比,所制备的复合材料大大减少了稀缺资源 Sm和战略储备资源Co的用量,降低了材料制备所需成本。
具体实施方式
下面结合具体实施例对本发明作进一步描述:
实施例1:
(1)制粉:
实验所用铝粉为99.85%纯度的粉末,平均粒径为10μm;通用钴粉,平均粒径2μm;镍粉,平均粒径2μm;工业生产2:17型Sm-Co永磁材料(Sm2Co17磁粉),制粉后平均粒 径约为5μm;
(2)球磨:
称取18gSm2Co17磁粉、18g铝粉、18g钴粉、18g镍粉,将上述粉末混合,加入乙醇, 使乙醇覆盖上述混合粉末,在行星式球磨机中湿磨12h,将球磨后的粉末放入真空干燥箱中烘干,得到混合粉体;
(3)压制成型:
将烘干后的混合粉末经冷等静压压制,加压90MPa,保压5min,得到致密的复合材料坯 锭;
(4)放电等离子烧结:
将步骤(3)中复合材料坯锭放入石墨模具中,在日本Sinter Land公司生产的SPS-3.20MK-Ⅳ型放电等离子烧结系统上进行真空烧结,升温速率为40℃/min,烧结温度为450℃,烧结压力为40MPa,烧结时间为4min,烧结完成后充氩气冷却至100℃以下后取出 样品,即得到Sm2Co17/Al-Ni-Co复合材料;
(5)充磁:
将步骤(4)制得的Sm2Co17/Al-Ni-Co复合材料放入充磁机在3T的磁场下充磁,获得所 需的磁性Sm2Co17/Al-Ni-Co复合材料。
实施例2:
(1)制粉:
实验所用铝粉为99.85%纯度的粉末,平均粒径为10μm;通用钴粉,平均粒径2μm;镍粉,平均粒径2μm;工业生产2:17型Sm-Co永磁材料(Sm2Co17磁粉),制粉后平均粒 径约为5μm;
(2)球磨:
称取25gSm2Co17磁粉、15g铝粉、15g钴粉、15g镍粉,将上述粉末混合,加入乙醇, 使乙醇覆盖上述混合粉末,在行星式球磨机中湿磨10h,将球磨后的粉末放入真空干燥箱中烘干,得到混合粉体;
(3)压制成型:
将烘干后的混合粉末经冷等静压压制,加压100MPa,保压2min,得到致密的复合材料 坯锭;
(4)放电等离子烧结:
将步骤(3)中复合材料坯锭放入石墨模具中,在日本Sinter Land公司生产的SPS-3.20MK-Ⅳ型放电等离子烧结系统上进行真空烧结,升温速率60℃/min,烧结温度为500℃,烧结压力30MPa,烧结时间2min,烧结完成后充氩气冷却至100℃以下后取出样品,即得到Sm2Co17/Al-Ni-Co复合材料;
(5)充磁:
将步骤(4)制得的Sm2Co17/Al-Ni-Co复合材料放入充磁机在3T的磁场下充磁,获得所 需的磁性Sm2Co17/Al-Ni-Co复合材料。
实施例3:
(1)制粉:
实验所用铝粉为99.85%纯度的粉末,平均粒径为10μm;通用钴粉,平均粒径2μm;镍粉,平均粒径2μm;工业生产2:17型Sm-Co永磁材料(Sm2Co17磁粉),制粉后平均粒 径约为5μm;
(2)球磨:
称取36gSm2Co17磁粉、12g铝粉、12g钴粉、12g镍粉,将上述粉末混合,加入乙醇, 使乙醇覆盖上述混合粉末,在行星式球磨机中湿磨11h,将球磨后的粉末放入真空干燥箱中烘干,得到混合粉体;
(3)压制成型:
将烘干后的混合粉末经冷等静压压制,加压95MPa,保压3min,得到致密的复合材料坯 锭;
(4)放电等离子烧结:
将步骤(3)中复合材料坯锭放入石墨模具中,在日本Sinter Land公司生产的SPS-3.20MK-Ⅳ型放电等离子烧结系统上进行真空烧结,升温速率50℃/min,烧结温度为470℃,烧结压力为35MPa,烧结时间3min,烧结完成后充氩气冷却至100℃以下后取出样品,即得到Sm2Co17/Al-Ni-Co复合材料;
(5)充磁:
将步骤(4)制得的Sm2Co17/Al-Ni-Co复合材料放入充磁机在3T的磁场下充磁,获得所 需的磁性Sm2Co17/Al-Ni-Co复合材料。
力学性能测试:
将实施例1-3中制备的磁性Sm2Co17/Al-Ni-Co复合材料,分别用拉力试验机测试其拉伸 强度、屈服强度和延伸率,具体结果如表1所示。
表1实施例1-3中磁性Sm2Co17/Al-Ni-Co复合材料的力学性能
分析表1数据可知,实施例1所获得的磁性Sm2Co17/Al-Ni-Co复合材料,相较于传统Al-Ni-Co永磁体抗拉强度和屈服强度有一定提高,一方面是添加Sm2Co17磁粉的原因,Sm2Co17磁粉本身具有相对于传统Al-Ni-Co永磁体更好的抗拉强度和屈服强度,加入Sm2Co17磁粉相当于在材料中加入脆性相,使材料抗拉强度和屈服强度更好;另一方面应用放电等离子烧结技术虽然大大降低了烧结温度,但相较于传统粉末烧结快速,更加致密,这也使得材料抗拉强度和屈服强度增强。
实施例2所获得磁性Sm2Co17/Al-Ni-Co复合材料,相较于实施例1的复合材料的抗拉强 度和屈服强度有明显提高,一方面是脆性相Sm2Co17磁粉加入量增大的原因;另一方面是放 电等离子烧结的烧结温度和升温速度提高,使材料在烧结过程中颗粒表面活化更充分,各个 颗粒产生的焦耳热更多,烧结更加充分,材料更加致密。
实施例3所获得磁性Sm2Co17/Al-Ni-Co复合材料,相较于实施例2的复合材料的抗拉强 度和屈服强度有明显提高,虽然烧结温度和升温速度相较于实施例2有所降低,但脆性相 Sm2Co17磁粉加入量增大,使复合材料的抗拉强度和屈服强度增强。
磁性能测试:
将实施例1-3中制备的磁性Sm2Co17/Al-Ni-Co复合材料,分别进行磁性能测试(矫顽力、 磁能积、剩磁等),采用Perma-Rema-C750型B-H测试仪(德国Magnet-Physik公 司)。采用Perma-Rema-C750型B-H测试仪来测试磁体的磁性能,最大磁场强度为2T, 测量尺寸均为Ф10*10的标准样品,经充磁后进行检测,测试结果如表2。
表2实施例1-3中磁性Sm2Co17/Al-Ni-Co复合材料的磁性能
分析表2数据可知,实施例1所获得的磁性Sm2Co17/Al-Ni-Co复合材料的剩磁比Sm2Co17磁粉的高,矫顽力优于Al-Ni-Co永磁体,磁能积也要优于Al-Ni-Co永磁体,这主要是由于 加入的Sm2Co17磁粉具有很好的矫顽力,增强了材料的磁性能;同时采用放等离子烧结使 Sm2Co17磁粉在Al-Ni-Co基体中分布均匀,展现出良好的磁性能。
实施例2所获得的磁性Sm2Co17/Al-Ni-Co复合材料的剩磁相较于实施例1所获得的材料 剩磁仅仅降低0.02T,但磁能积却升高26k J·m-3,同时矫顽力也略有提升,主要是由于增加 了Sm2Co17磁粉的用量。
实施例3所获得的磁性Sm2Co17/Al-Ni-Co复合材料,在磁性能方面已基本上达到所用 Sm2Co17磁粉的磁性能,同时大大减少了稀缺资源Sm和战略储备资源Co的用量,降低了材料制备所需成本。
本发明制备得到的磁性Sm2Co17/Al-Ni-Co复合材料,可广泛应用在工业生产中,用于生 产永磁电机里的永磁转子或仪表里的永磁磁铁等。
Claims (9)
1.一种放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法,其特征在于,包括以下步骤:
(1)球磨:
将Sm2Co17磁粉与铝粉、钴粉、镍粉按比例混合均匀,加入乙醇,在球磨机中湿磨,将球磨后的粉末放入真空干燥箱中烘干,得到混合粉体;
(2)压制成型:
将步骤(1)中的混合粉体用冷等静压压制成型,得到致密的复合材料坯锭;
(3)放电等离子烧结:
将复合材料坯锭放入石墨模具中,在放电等离子烧结炉中进行真空烧结,烧结完成后冷却至室温后取出样品,即得到Sm2Co17/Al-Ni-Co复合材料;
(4)充磁:
将步骤(3)得到的Sm2Co17/Al-Ni-Co复合材料放入充磁机充磁,得到磁性Sm2Co17/Al-Ni-Co复合材料。
2.根据权利要求1所述的放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法,其特征在于,步骤(1)中,所述Sm2Co17磁粉、铝粉、钴粉的质量比为1-3:1-3:1-3;钴粉、镍粉的质量比为1-3:1-5。
3.根据权利要求1所述的放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法,其特征在于,步骤(1)中,所述球磨时间为10-12h。
4.根据权利要求1所述的放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法,其特征在于,步骤(2)中,所述冷等静压压强为90-100MPa,保压时间为2-5min。
5.根据权利要求1所述的放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法,其特征在于,步骤(3)中,所述烧结温度为450-500℃,升温速率为40-60℃/min。
6.根据权利要求1所述的放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法,其特征在于,步骤(3)中,所述烧结压力为30-40MPa,烧结时间为2-4min。
7.根据权利要求1所述的放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法,其特征在于,步骤(3)中,所述冷却时需要充氩气。
8.根据权利要求1所述的放电等离子烧结制备磁性Sm2Co17/Al-Ni-Co复合材料的方法,其特征在于,步骤(4)中,所述充磁是在3T的磁场下进行。
9.如权利要求1-8任意一项所述的方法制备的磁性Sm2Co17/Al-Ni-Co复合材料用于生产永磁转子或永磁磁铁。
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