CN110997950B - 一种合金工件或金属工件的连续热处理装置以及方法 - Google Patents
一种合金工件或金属工件的连续热处理装置以及方法 Download PDFInfo
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- CN110997950B CN110997950B CN201880028565.7A CN201880028565A CN110997950B CN 110997950 B CN110997950 B CN 110997950B CN 201880028565 A CN201880028565 A CN 201880028565A CN 110997950 B CN110997950 B CN 110997950B
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 249
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 34
- 239000000956 alloy Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 title abstract description 22
- 239000002184 metal Substances 0.000 title abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 167
- 229910001172 neodymium magnet Inorganic materials 0.000 claims description 44
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- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052779 Neodymium Inorganic materials 0.000 description 3
- 229910052777 Praseodymium Inorganic materials 0.000 description 3
- 229910052771 Terbium Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 238000005496 tempering Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
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- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
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- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- -1 neodymium iron boron rare earth Chemical class 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
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Classifications
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- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
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- C—CHEMISTRY; METALLURGY
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- C21—METALLURGY OF IRON
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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- C—CHEMISTRY; METALLURGY
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Hard Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
- Heat Treatment Of Articles (AREA)
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- Disintegrating Or Milling (AREA)
Abstract
本发明公开了一种合金工件或金属工件的连续热处理装置以及方法,包括依次连续设置的第一热处理室、第一冷却室、第二热处理室、第二冷却室、以及设置在各个室之间的用以运送所述合金工件或金属工件的运送系统,所述第一冷却室和所述第二冷却室均采用风冷系统,所述第一冷却室的冷却风温度在25℃以上、并与所述第一热处理室的热处理温度至少相差450℃,所述第二冷却室的冷却风温度在25℃以上、并与所述第二热处理室的热处理温度至少相差300℃,所述冷却室的压力50kPa‑100kPa。该连续热处理装置和连续热处理方法可以提升冷却速率和生产效率,提高产品的性能和一致性。
Description
技术领域
本发明涉及热处理装置及热处理方法,具体地涉及合金工件或金属工件的连续热处理装置以及连续热处理方法。
背景技术
钕铁硼稀土永磁材料是目前磁能积最高的工业量产化磁体,广泛应用在风力发电、伺服电机、家电压缩机和新能源汽车电机等领域,相比其他磁体,具有体积小和效率高等优势。
钕铁硼材料通常需要通过熔炼、破碎、压制、烧结、热处理等工序,才能得到所需性能的磁体。其中,热处理包含第一级热处理和第二级热处理,通常分别在800℃-950℃和400℃-650℃。
现有的技术中,使用单室热处理炉对钕铁硼材料进行热处理,重复发生升温和降温,升温和降温的速率难以控制,能耗增大。因此,现有的单室热处理炉很难制作出性能和一致性良好的高性能钕铁硼材料。另外,由于单室炉一般为圆柱形炉体,其热源为圆柱形炉体的内壁,物料大都是多列立体堆垛式摆放,导致不同位置物料距离热源距离不一,因此炉内温度一致性和均匀性较差,尤其体现在芯部物料和外围物料的温度差。这种摆放方式也限制了单室炉的快速降温能力。
发明内容
鉴于上述问题,本发明提供一种合金工件或金属工件的连续热处理装置,该连续热处理装置可以提升冷却速率和生产效率,提高产品一致性。
本发明采用的技术方案如下:
一种合金工件或金属工件的连续热处理装置,其特征在于:包括通过气密装置依序设置的第一热处理室、第一冷却室、第二热处理室、第二冷却室、以及设置在各个室之间的用以运送所述合金工件或金属工件的运送系统,所述第一冷却室和所述第二冷却室均采用风冷系统,所述第一冷却室的冷却风温度在25℃以上、并与所述第一热处理室的热处理温度至少相差450℃,所述第二冷却室的冷却风温度在25℃以上、并与所述第二热处理室的热处理温度至少相差300℃,所述冷却室的压力50kPa-100kPa。
本发明中,采用单独设置热处理室和冷却室(使用风冷系统方式),并限定冷却室的冷却风温度,在物料热处理完成后,可根据需要的冷却工艺,实现热处理后高温段的快速均匀冷却,优化合金工件或金属工件的晶界微观组织相成分和分布。风冷系统可以强制对流换热,快速带走物料热量,可根据风机的变速,实现冷却速度控制。
本发明中,冷却室的压力为50kPa-100kPa为本行业的常规选择,因此,在实施例中,没有对上述含量范围加以试验和验证。
本发明的另一目的在于提供一种合金工件或金属工件的连续热处理方法。该连续热处理方法可以提升冷却速率和生产效率,提高产品的性能和一致性。
本发明采用的技术方案如下:
一种合金工件或金属工件的连续热处理方法,其特征在于:包括依序在相互气密的分室进行的第一级热处理、第一级风冷却处理、第二级热处理、和第二级风冷却处理,所述第一级风冷却处理的冷却风温度在25℃以上、并与所述第一级热处理的热处理温度至少相差450℃,所述第二级风冷却处理的冷却风温度在25℃以上、并与所述第二级热处理的温度至少相差300℃。
需要说明的是,本发明中公布的数字范围包括这个范围内的所有点值。
具体实施方式
以下结合实施例对本发明作进一步详细说明。
在推荐的实施方式中,所述合金工件为Nd-Fe-B系烧结磁体。这是由于,申请人在研究过程中发现,Nd-Fe-B系烧结磁体经过分室进行热处理和高温段快速冷却之后,可以提高产品的方形度、内禀矫顽力和产品一致性,特别是内禀矫顽力得到显著提高。这一作用机制在现阶段还是不清楚的。
在推荐的实施方式中,所述风冷系统为采用惰性气体的风冷系统。这里的惰性气体选自氦、氖、氩、氪、氙、氡或氮气等在上述热处理或冷却处理中不与合金工件或金属工件反应的气体。
在推荐的实施方式中,所述第一热处理室的热处理温度为800℃-950℃,所述第一冷却室的冷却风温度为25℃-150℃,所述第二处理室的热处理温度为400℃-650℃,所述第二冷却室的冷却风温度为25℃-100℃。这样就可以使得钕铁硼物料快速通过共晶点,获得良好的方形度和矫顽力。
这其中,第一热处理室的温度为800℃-950℃和第二热处理室的温度为400℃-650℃等的含量范围为Nd-Fe-B系烧结磁体领域热处理工艺的常规选择,因此,在实施例中,没有对上述含量范围加以试验和验证。
一般来讲,第一冷却室、第二冷却室的初始温度与相应的冷却风温度相同。
在推荐的实施方式中,所述第一热处理室呈现方形结构,并包括两个相向设置在所述方形结构内壁的加热区域,所述合金工件或所述金属工件直接放置在所述方形结构中部的料架上,或所述合金工件或所述金属工件先放置在料盒内而后将所述料盒放置在所述方形结构中部的料架上;同样地,所述第二热处理室呈现方形结构,并包括两个对向设置在所述方形结构内壁的加热区域,所述合金工件或所述金属工件直接放置在所述方形结构中部的料架上,或所述合金工件或所述金属工件先放置在料盒内而后将所述料盒放置在所述方形结构中部的料架上。通过上述的结构,实现物料温度的高均匀性,控制温度波动。
在推荐的实施方式中,所述加热区域的面积超过所述料架的纵截面面积。如此,可以保证所有料盒都能得到均一的热处理,使热处理后的合金工件或金属工件性能趋于一致。
在推荐的实施方式中,所述第二热处理室中,所述料盒或合金工件或金属工件距两个相向设置的所述加热区域的距离相同,为2cm-30cm,优选为5cm-20cm。申请人在生产过程中发现,Nd-Fe-B系磁体对二级回火温差极为敏感,二级回火温差的控制可显著提高Nd-Fe-B系磁体性能和各区域Nd-Fe-B系磁体的一致性。本申请中,选择将料盒靠近加热区域设置,特别是在将距离控制在5cm-20cm以后,在最佳的实施方式中,可将各区域料盒或各区域合金工件或各区域金属工件或料盒不同区域的温差控制在±5℃以内,实现物料温度的高均匀性,极大地提升了同一批次Nd-Fe-B系磁体的性能一致性。
在推荐的实施方式中,所述Nd-Fe-B系磁体为TRE(稀土总含量)为28.8wt%-34.0wt%的Nd-Fe-B系磁体,优选为TRE(稀土总含量)为28.8wt%-30.5wt%的Nd-Fe-B系磁体。在研究过程中发现,TRE(稀土总含量)为28.8wt%-30.5wt%的磁体对二级回火温差最为敏感,对热处理温度控制要求更高。
本发明中提及的Nd-Fe-B系磁体为包括Nd2Fe14B型主相的磁铁。
在推荐的实施方式中,包括通过气密装置依序设置的第一升温室、第二升温室、第一热处理室、第一冷却室、第三升温室、第二热处理室和第二冷却室。这是由于,升温至800℃-950℃大约是第一热处理室热处理时间的2倍左右,通过设置两个升温室,将两个升温室的处理时间调整到与第一热处理室的热处理时间相当,节拍一致,从而使得生产有续进行。
在推荐的实施方式中,所述第二级热处理中,不同区域的所述合金工件或金属工件的温差在±5℃以下。
在推荐的实施方式中,所述第一级冷却处理中,所述合金工件或所述金属工件的最初10min的平均冷却速度为6℃/min-15℃/min,所述第二级冷却处理中,所述合金工件或所述金属工件的最初10min的平均冷却速度为6℃/min-15℃/min。
本发明中,通过不断的试验验证,选择监控最初10min的平均冷却速度,当然,可以根据产品的需要,选择监控最初5min-30min的平均冷却速度。
各实施例所获得的烧结磁铁均使用如下的检测方式测定。
磁性能评价过程:烧结磁铁使用中国计量院的NIM-10000H型BH大块稀土永磁无损测量系统进行磁性能检测。
实施例1
连续热处理设备,包括依次连续设置的第一升温室、第二升温室、第一热处理室、第一冷却室、第三升温室、第二热处理室和第二冷却室,第一升温室、第二升温室、第一热处理室、第一冷却室、第三升温室、第二热处理室和第二冷却室之间设置气密阀,以及设置在各个室之间的用以运送Nd-Fe-B系烧结磁体的运送系统。
连续热处理过程如下:
(1)装料
按质量百分比wt%,取组成为Pr为7.25%、Nd为21.75%、Dy为1.5%、Fe为bal.(余量)、B为0.97%、Cu为0.15%、Ga为0.2%、Nb为0.2%、Co为0.8%的原料,并采用熔炼、甩带、氢破碎、气流破碎、压形和烧结,制得Nd-Fe-B系烧结磁体。
经检测,Nd-Fe-B系烧结磁体的性能为Hcj=16.50kOe,Br=13.70kGs,方形度为98%。
将Nd-Fe-B系烧结磁体放置在带有通孔的料盒内,将料盒按照双列堆叠,放置在料架上,送入第一升温室内。值得一提的是,依据不同的生产需求,在变换的实施例中,也可以使用密闭的料盒。
(2)第一级升温
当第一升温室的真空度达到100Pa时,启动加热程序,从室温开始升温165min,在温度达到370℃-400℃之后,保温15min。保温结束后,从第一升温室向第二升温室输送装有料盒的料架。
(3)第二级升温
装有料盒的料架进入第二升温室后,当真空度达到100Pa时,加热升温165min,在温度达到800℃-850℃之后,保温15min。保温结束后,从第二升温室向第一热处理室输送装有料盒的料架。
(4)第一级热处理
第一热处理室呈现方形结构,并包括两个相向设置在方形结构内壁的加热区域,加热区域的面积超过料架的纵截面面积。料盒进入第一热处理室后,放置在与两个加热区域均为25cm距离的位置。
当真空度达到100Pa时,加热升温10min,至第一热处理室的热处理温度(不同料盒内不同位置处检测)为880℃-895℃,保温170min。保温结束后,从第一级热处理室向第一冷却室输送装有料盒的料架。
(5)第一级冷却
装有料盒的料架进入第一冷却室后,抽真空,向冷却室充入78kPa的惰性气体,然后进行风机循环冷却,冷却时间为180min。第一冷却室的惰性气体温度如表1中所示,惰性气体温度在吸气式循环风的出气口处检测。
(6)第三级升温
双列堆叠的料盒进入第三升温室后,当真空度达到100Pa时,加热升温165min,至温度达到460℃-470℃之后,保温15min。保温结束后,从第三升温室向第二热处理室输送装有料盒的料架。
(7)第二级热处理
第二热处理室呈现方形结构,并包括两个相向设置在方形结构内壁的加热区域,加热区域的面积超过料架的纵截面面积。料盒进入第二热处理室后,放置在与两个加热区域均为25cm距离的位置。
当真空度达到100Pa时,加热升温15min,在热处理温度(不同料盒内不同位置处检测)达到500℃-515℃之后,保温165min。保温结束后,从第二热处理室向第二冷却室输送装有料盒的料架。
(8)第二级冷却
装有料盒的料架进入所述第二级冷却室后,抽真空,向冷却室充入78kPa的惰性气体,然后进行风机循环冷却,冷却时间为180min。将装有料盒的料架出炉。第二冷却室的惰性气体温度如表1中所示,惰性气体温度在吸气式循环风的出气口处检测。
如此,装有料盒的料架在第一升温室进行升温和短时保温后,进入第二升温室升温和短时保温。之后,进入第一热处理室短时升温和保温。在第一热处理室保温结束后,进入第一冷却室冷却。在第一冷却室冷却结束后,进入第三升温室进行升温和短时保温。在第三升温室保温结束后,进入第二级热处理室进行短时升温和保温。保温结束后,进入第二冷却室进行冷却。冷却结束后,出料。
经上述热处理和冷却处理后,磁铁性能如表1中所示。
表1第一、第二冷却室的惰性气体温度、以及经热处理和冷却处理后的磁铁性能
经检测,实施例1.4、实施例1.5和实施例1.6的第一级冷却处理中,Nd-Fe-B系烧结磁体的最初10min的平均冷却速度为6℃/min-15℃/min,实施例1.3、实施例1.4、实施例1.5和实施例1.6的第二级冷却处理中,Nd-Fe-B系烧结磁体的最初10min的平均冷却速度为6℃/min-15℃/min。而实施例1.1、实施例1.2和实施例1.3的第一级冷却处理中,Nd-Fe-B系烧结磁体的最初10min的平均冷却速度小于6℃/min,实施例1.1和实施例1.2的第二级冷却处理中,Nd-Fe-B系烧结磁体的最初10min的平均冷却速度同样小于6℃/min。
从表1中可以看到,第一冷却室的冷却风温度高于25℃,并低于第一热处理室的热处理温度至少450℃,同时第二冷却室的惰性气体温度高于25℃,并低于所述第二热处理室的热处理温度至少300℃,热处理后磁体的磁性能更好,尤其是Hcj明显提高,SQ改善。这是因为,上述温度区间内有助于提高磁体热处理后高温段的冷却速度,从而优化晶界微观组织相成分和分布。
实施例2
连续热处理设备,包括依次连续设置的第一升温室、第二升温室、第一热处理室、第一冷却室、第三升温室、第二热处理室和第二冷却室,第一升温室、第二升温室、第一热处理室、第一冷却室、第三升温室、第二热处理室和第二冷却室之间设置气密阀,以及设置在各个室之间的用以运送Nd-Fe-B系烧结磁体的运送系统。
连续热处理过程如下:
(1)装料
按质量百分比wt%,取组成为Pr为7.12%、Nd为21.38%、Tb为1.5%、Fe为bal.(余量)、B为0.96%、Cu为0.15%、Ga为0.2%、Nb为0.2%、Co为0.8%的原料,并采用熔炼、甩带、氢破碎、气流破碎、压形和烧结,制得Nd-Fe-B系烧结磁体。
经检测,Nd-Fe-B系烧结磁体的性能为Hcj=16.5kOe,Br=14.2kGs,方形度为97%。
将Nd-Fe-B系烧结磁体放置在网格料盒内,将料盒按照单列堆叠,放置在料架上,送入第一升温室内。
(2)第一级升温
当第一升温室的真空度达到150Pa时,启动加热程序,从室温开始升温150min,在温度达到350-380℃之后,保温30min。保温结束后,从第一升温室向第二升温室输送装有料盒的料架。
(3)第二级升温
装有料盒的料架进入第二升温室后,当真空度达到150Pa时,加热升温150min,在温度达到820-860℃之后,保温30min。保温结束后,从第二升温室向第一热处理室输送装有料盒的料架。
(4)第一级热处理
第一热处理室呈现方形结构,并包括两个相向设置在方形结构的内壁的加热区域,加热区域的面积超过料架的纵截面面积。料盒进入第一热处理室后,放置在与两个加热区域均为2-30cm距离的位置,具体如表2中所示。
当真空度达到150Pa时,加热升温5min,检测各区域不同料盒内不同位置处的热处理温度,具体如表2中所示,保温175min。保温结束后,从第一级热处理室向第一冷却室输送装有料盒的料架。
(5)第一级冷却
装有料盒的料架进入第一冷却室后,抽真空,抽真空,向冷却室充入40℃-50℃的76kPa的惰性气体,然后进行风机循环冷却,冷却时间为180min,Nd-Fe-B系烧结磁体的最初10min的平均冷却速度为15℃/min。惰性气体温度在吸气式循环风的出气口处检测。
(6)第三级升温
装有料盒的料架进入第三升温室后,当真空度达到150Pa时,加热升温170min,至温度达到380℃-420℃之后,保温10min。保温结束后,从第三升温室向第二热处理室输送装有料盒的料架。
(7)第二级热处理
第二热处理室呈现方形结构,并包括两个相向设置在方形结构的内壁的加热区域,加热区域的面积超过料架的纵截面面积。料盒进入第二热处理室后,放置在与两个加热区域均为2-30cm距离的位置,具体如表2中所示。
当真空度达到150Pa时,加热升温10min,检测各区域不同料盒内不同位置处的热处理温度,具体如表2中所示,保温170min。保温结束后,从第二热处理室向第二冷却室输送装有料盒的料架。
(8)第二级冷却
装有料盒的料架进入所述第二级冷却室后,抽真空,向冷却室充入40℃-50℃的76kPa的惰性气体,然后进行风机循环冷却,冷却时间为180min,Nd-Fe-B系烧结磁体的最初10min的平均冷却速度为9.0℃/min。将装有料盒的料架出炉。惰性气体温度在吸气式循环风的出气口处检测。
经上述热处理和冷却处理后,磁铁性能如表2中所示。表2中距离为单列堆叠的料盒与两侧加热区域之间的距离。
从不同区域取20块Nd-Fe-B系烧结磁体,测量其Br、Hcj、BH(max)和SQ,测量一致性。一致性用产品性能指标的波动性来描述,波动性定义为(最大值-最小值)/最小值。波动性越小,一致性越好。
表2第一级、第二级热处理的热处理温度、以及经热处理和冷却处理后的磁铁性能
从表2中可以看到,第二级热处理温度的波动越小,Br基本保持稳定,Hcj和SQ的波动性都越小。这是因为第二级热处理温度与磁体的晶界微观组织相成分和分布密切相关,温度波动越大,性能波动越大。
微观组织的状态对NdFeB的性能影响非常大,微观组织越均匀、晶粒越细小材料的性能就越好性能一致性越高,而烧结NdFeB材料的微观组织的优化主要是发生在热处理阶段。因而热处理工艺对材料的性能影响非常大,同一个配方因为热处理工艺的不同磁性能可能千差万别,本发明在通过提高温度均匀性的基础上提高组织的均匀性再通过快速的冷却速度将均匀的组固化使每个产品的组织均匀一致,从达到提高材料性能和均匀性的目的。
实施例3
连续热处理设备,包括依次连续设置的第一升温室、第二升温室、第一热处理室、第一冷却室、第三升温室、第二热处理室和第二冷却室,第一升温室、第二升温室、第一热处理室、第一冷却室、第三升温室、第二热处理室和第二冷却室之间设置气密阀,以及设置在各个室之间的用以运送Nd-Fe-B系烧结磁体的运送系统。
连续热处理过程如下:
(1)装料
按质量百分比wt%,取组成为Pr为8%、Nd为19%-21.5%(根据表3中TRE调整)、Tb为1.5%、Fe为bal.(余量)、B为0.97%、Cu为0.1%、Ga为0.1%、Nb为0.1%、Co为1%的原料,并采用熔炼、甩带、氢破碎、气流破碎、压形和烧结,制得Nd-Fe-B系烧结磁体。TRE含量的含量配比和磁铁性能如表3中所示。
将Nd-Fe-B系烧结磁体放置在网格料盒内,将料盒按照单列堆叠,放置在料架上,送入第一升温室内。
(2)第一级升温
当第一升温室的真空度达到10-1Pa时,启动加热程序,从室温开始升温130min,在温度达到360-400℃之后,保温20min。保温结束后,从第一升温室向第二升温室输送装有料盒的料架。
(3)第二级升温
装有料盒的料架进入第二升温室后,当真空度达到10-1Pa时,加热升温130min,在温度达到810-830℃之后,保温20min。保温结束后,从第二升温室向第一热处理室输送装有料盒的料架。
(4)第一级热处理
第一热处理室呈现方形结构,并包括两个相向设置在方形结构的内壁的加热区域,加热区域的面积超过料架的纵截面面积。装有料盒的料架进入第一热处理室后,放置在与两个加热区域均为5cm距离的位置。
当真空度达到10-1Pa时,加热升温10min,至第一热处理室的热处理温度(不同料盒内不同位置处检测)为905℃-910℃,保温140min。保温结束后,从第一级热处理室向第一冷却室输送装有料盒的料架。
(5)第一级冷却
装有料盒的料架进入第一冷却室后,当真空度达到10-1Pa时,向冷却室充入70℃-90℃的80kPa的惰性气体,然后进行风机循环冷却,冷却时间为150min,Nd-Fe-B系烧结磁体的最初10min的平均冷却速度为6.5℃/min。惰性气体温度在吸气式循环风的出气口处检测。
(6)第三级升温
装有料盒的料架进入第三升温室后,当真空度达到10-1Pa时,加热升温140min,至温度达到400℃-425℃之后,保温10min。保温结束后,从第三升温室向第二热处理室输送装有料盒的料架。
(7)第二级热处理
第二热处理室呈现方形结构,并包括两个相向设置在方形结构的内壁的加热区域,加热区域的面积超过料架的纵截面面积。装有料盒的料架进入第二热处理室后,放置在与两个加热区域均为5cm距离的位置。
装有料盒的料架进入第二热处理室后,当真空度达到10-1Pa时,加热升温10min,至第二热处理室的热处理温度(不同料盒内不同位置处检测)达到535℃-540℃,保温140min。保温结束后,从第二热处理室向第二冷却室输送装有料盒的料架。
(8)第二级冷却
装有料盒的料架进入所述第二级冷却室后,当真空度达到10-1Pa时,向冷却室充入30℃-60℃的80kPa的惰性气体,然后进行风机循环冷却,冷却时间为150min,Nd-Fe-B系烧结磁体的最初10min的平均冷却速度为6.0℃/min。将装有料盒的料架出炉。惰性气体温度在吸气式循环风的出气口处检测。
经上述热处理和冷却处理后,磁铁性能如表3中所示。
表3TRE含量、以及热处理和冷却处理前后的磁铁性能
热处理和冷却处理前的磁铁的Br波动性(%)、Hcj波动性(%)和SQ波动性(%)为0。
在现有的热处理过程中,一般来说,TRE超过30.5%的磁铁在热处理过程中一致性较好,而TRE为28.8wt%-30.5wt%的磁铁在热处理过程中,Br波动性(%)、Hcj波动性(%)和SQ波动性(%)的其中一项或者几项会达到5%以上,进而影响产品的一致性。
而本申请人发现,TRE为28.8wt%-30.5wt%的磁铁在上述温差较小、且最初10min的平均冷却速度受控的热处理设备中进行热处理,Br波动性(%)、Hcj波动性(%)和SQ波动性(%)均减少,可以显著提高一致性。
从表3中可以看到,提高平面热处理设备的温度均匀性,并控制其冷却速度,对于提高低稀土含量的钕铁硼性能一致性具有非常重要正向作用。
对比例
连续热处理设备,包括依次连续设置的第一热处理室和第二热处理室,第一热处理室和第二热处理室之间设置气密阀,以及设置在两室之间的用以运送Nd-Fe-B系烧结磁体的运送系统。
连续热处理过程如下:
取质量百分比wt%组成为Pr为8%、Nd为20%、Tb为1.5%、Fe为bal.(余量)、B为0.97%、Cu为0.1%、Ga为0.1%、Nb为0.1%、Co为1%的原料,并采用熔炼、甩带、氢破碎、气流破碎、压形和烧结,具体工艺参数与实施例3相同,制得Nd-Fe-B系烧结磁体。
将Nd-Fe-B系烧结磁体放置在网格料盒内,将料盒按照单列堆叠,放置在料架上,送入第一热处理室内。
装有料盒的料架进入第一热处理室后,放置在与两个加热区域均为5cm距离的位置,当真空度达到10-1Pa时,加热升温180min,至第一热处理室的热处理温度(不同料盒内不同位置处检测)为905℃-910℃,保温140min。保温结束后,向第一热处理室充入70℃-90℃的80kPa的惰性气体,然后进行风机循环冷却,冷却时间为150min,惰性气体温度在吸气式循环风的出气口处检测。Nd-Fe-B系烧结磁体的最初10min的平均冷却速度为5℃/min。将装有料盒的料架从第一热处理室运送到第二热处理室。
装有料盒的料架进入第二热处理室后,放置在与两个加热区域均为5cm距离的位置,当真空度达到10-1Pa时,加热升温90min,至第二热处理室的热处理温度(不同料盒内不同位置处检测)达到535℃-540℃,保温140min。保温结束后,向第二热处理室充入30℃-60℃的80kPa的惰性气体,然后进行风机循环冷却,冷却时间为150min,惰性气体温度在吸气式循环风的出气口处检测。Nd-Fe-B系烧结磁体的最初10min的平均冷却速度为4.5℃/min。
表4 TRE含量、以及经单室热处理和冷却处理前后的磁铁性能
设热处理和冷却处理前的磁铁的Br波动性(%)、Hcj波动性(%)和SQ波动性(%)为0。
从表3和表4中可以看到,在单室进行热处理和冷却处理,高温段的冷却速度较低,单室处理的Br、SQ略有下降,Hcj下降较为明显,且三者的波动性明显变大。
上述实施例仅用来进一步说明本发明的几种具体的实施方式,但本发明并不局限于实施例,凡是依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均落入本发明技术方案的保护范围内。
Claims (6)
1.一种合金工件的连续热处理方法,其特征在于:所述合金工件为Nd-Fe-B系烧结磁体,所述Nd-Fe-B系烧结磁体为TRE为28.8wt%-30.5wt%的Nd-Fe-B系烧结磁体,包括依序在相互气密的分室进行的第一级热处理、第一级风冷却处理、第二级热处理、和第二级风冷却处理,所述第一级风冷却处理的冷却风温度在25℃以上、并与所述第一级热处理的温度至少相差450℃,所述第二级风冷却处理的冷却风温度在25℃以上、并与所述第二级热处理的温度至少相差300℃;所述第二级热处理中,不同区域的所述合金工件温差在±5℃以下;所述第一级风冷却处理中,所述合金工件的最初10min的平均冷却速度为6℃/min-15℃/min,所述合金工件的所述第二级风冷却处理中,最初10min的平均冷却速度为6℃/min-15℃/min。
2.根据权利要求1中所述的一种合金工件的连续热处理方法,其特征在于:所述第一级热处理的热处理温度为800℃-950℃。
3.根据权利要求1中所述的一种合金工件的连续热处理方法,其特征在于:所述第二级热处理的热处理温度为400℃-650℃。
4.根据权利要求1中所述的一种合金工件的连续热处理方法,其特征在于:所述第一级风冷却处理和第二级风冷却处理采用惰性气体进行风冷。
5.根据权利要求1中所述的一种合金工件的连续热处理方法,其特征在于:所述第一级风冷处理中,冷却风的温度为25℃-150℃。
6.根据权利要求1中所述的一种合金工件的连续热处理方法,其特征在于:所述第二级风冷处理中,冷却风的温度为25℃-100℃。
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CN110106334B (zh) | 2021-06-22 |
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JP2020535312A (ja) | 2020-12-03 |
US20210142943A1 (en) | 2021-05-13 |
KR102378901B1 (ko) | 2022-03-25 |
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EP3626839A1 (en) | 2020-03-25 |
CN110997950A (zh) | 2020-04-10 |
CN110663107B (zh) | 2022-10-11 |
JP2020535311A (ja) | 2020-12-03 |
KR20200019969A (ko) | 2020-02-25 |
KR102242966B1 (ko) | 2021-04-21 |
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JP7130034B2 (ja) | 2022-09-02 |
US11636976B2 (en) | 2023-04-25 |
US11508519B2 (en) | 2022-11-22 |
JP7108688B2 (ja) | 2022-07-28 |
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