WO2018126738A1 - 一种mn-ga合金及其磁硬化方法 - Google Patents

一种mn-ga合金及其磁硬化方法 Download PDF

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WO2018126738A1
WO2018126738A1 PCT/CN2017/103076 CN2017103076W WO2018126738A1 WO 2018126738 A1 WO2018126738 A1 WO 2018126738A1 CN 2017103076 W CN2017103076 W CN 2017103076W WO 2018126738 A1 WO2018126738 A1 WO 2018126738A1
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alloy
heat
pressure
mold
mpa
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PCT/CN2017/103076
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French (fr)
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路清梅
岳明
李晨辉
张红国
张东涛
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北京工业大学
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—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
    • H01F41/02—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
    • 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
    • H01F41/0266—Moulding; Pressing

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  • the invention discloses a method for magnetically hardening a Mn-Ga alloy, belonging to the technical field of functional materials.
  • Permanent magnet materials have been widely used in the fields of machinery, communication, automation, instrumentation and medical care, and have become one of the supporting materials for modern industry and science and technology.
  • the violent fluctuation of rare earth prices in the international market and the regulatory use of rare earths in various countries have made the development and research of non-rare earth permanent magnet materials with high performance and high stability become international research hotspots.
  • Mn-Ga binary alloys have attracted the attention of researchers due to their rich phase structure, diverse intrinsic magnetic properties and potential applications in many fields.
  • Mn 3 Ga alloys with a face-centered tetragonal D0 22 structure, ferrimagnetic order, high spin polarizability, and high Curie temperature are among the important candidates for novel spin-transfer torque (STT) materials;
  • STT spin-transfer torque
  • the tetragonal L1 0 -MnGa alloy is predicted to have the potential to become the new non-rare earth permanent magnet material with the highest magnetic energy product.
  • Theoretical calculations show that the saturation magnetization Ms of L1 0 -MnGa alloy can reach 116emu/g, and the maximum theoretical magnetic energy product (BH) max can be as high as 28MGOe, which is equivalent to cobalt-based rare earth permanent magnet materials.
  • BH maximum theoretical magnetic energy product
  • the tetragonal Mn-Ga alloy is considered to have potential for application in the field of permanent magnets.
  • many research institutions prepared Mn-Ga alloy on the phase transition, the structure and the intrinsic magnetic properties studied, and has received a saturation magnetization reaches 92emu / g of Mn 1.15 Ga alloy, but on the alloy magnetic rigidification of There are relatively few studies.
  • Plastic deformation of the alloy is an effective way to obtain magnetic hardening, and has been successfully achieved in rare earth permanent magnet alloys Nd-Fe-B and Sm-Co.
  • Thermal deformation is one of the important processes for the manufacture of NdFeB anisotropic materials.
  • the discharge plasma sintering (SPS) equipment has the characteristics of simple operation, uniform heating, fast heating rate and high efficiency.
  • SPS plasma sintering
  • Yue Ming et al. used the SPS thermal deformation method to prepare NdFeB anisotropic permanent magnets with excellent performance.
  • the invention successfully obtains a manganese gallium bulk magnet with large coercive force and certain anisotropy by finely regulating the heating rate, the holding temperature, the heat deformation pressure and the pressing time of the spark plasma sintering process.
  • the invention first obtains a Mn x Ga (1.0 ⁇ x ⁇ 3.0) ingot by smelting, and obtains a tetragonal phase by heat treatment at 400 to 650 ° C, and the tetragonal phase alloy block is sintered by discharge plasma at a pressure of 300 to 700 ° C and 30 to 800 MPa (
  • the SPS) device is thermally deformed to obtain a manganese gallium bulk magnet having a large coercive force and a certain anisotropy.
  • the Mn-Ga alloy block technology obtained by the present invention is as follows:
  • the Mn x Ga ingot is obtained by melting in a smelting furnace under an argon atmosphere, 1.0 ⁇ x ⁇ 3.0;
  • the Mn x Ga ingot obtained in the first step is heat-treated at 400 to 650 ° C in an argon atmosphere to obtain a tetragonal phase alloy block;
  • the tetragonal phase alloy block obtained in the second step is placed in a mold, and the SPS is used for rapid hot pressing deformation treatment.
  • the rapid thermal deformation process parameters are as follows: firstly increase to 400 at a heating rate of 30 to 120 ° C / min. At -700 ° C, a pressure of 30 to 800 MPa is applied, or the temperature is raised simultaneously with the pressurization; and the magnetically hardened manganese gallium magnet is obtained by holding the pressure for 2 to 10 minutes.
  • the smelting and heat treatment processes are carried out under the protection of an inert gas, which may be argon.
  • the mold described in the third step may be a graphite mold or a cemented carbide mold, and a graphite abrasive tool may be used when the heat deformation pressure is below 100 MPa, and a hard alloy abrasive tool is used when the pressure is greater than or equal to 100 MPa.
  • the thermal deformation process described in the third step avoids the occurrence of phase transitions. If the timing of applying pressure may vary according to the composition of the alloy, the plasticity of the Mn-Gagal alloy tetragonal phase ingot will deteriorate with the decrease of Mn content. For alloys with poor plasticity, the temperature should be raised until the alloy has good plasticity. After re-pressurization, for alloys with better plasticity, pressure should be applied as early as possible to shorten the time when the alloy is at a high temperature, or to use a lower temperature to avoid the occurrence of phase transition.
  • the heat treatment temperature and time of the ingot can be adjusted according to the composition of the ingot, so that the alloy phase after the heat treatment is a tetragonal phase;
  • the mold used for the SPS can be a graphite mold or a cemented carbide mold, and preferably can withstand High-pressure cemented carbide mold; using the heat distortion temperature process of the invention, the manganese gallium alloy can ensure sufficient plasticity and phase transformation of the manganese gallium alloy; the pressure used ensures that the alloy has sufficient heat deformation The amount of deformation.
  • the Mn-Ga alloy magnet obtained by the invention has high remanence, large coercive force and excellent magnetic energy product, and has potential application in the field of permanent magnets.
  • Example 1 is a hysteresis loop of a Mn 1.80 Ga alloy thermocompressed magnet prepared in Example 4.
  • Example 1 A technique for magnetic hardening of a Mn 3.0 Ga alloy was carried out as follows:
  • the Mn 3.0 Ga ingot obtained in the first step is heat-treated at 500 ° C for 45 min in an argon atmosphere to obtain a tetragonal phase alloy block;
  • the tetragonal phase alloy block obtained in the second step is placed in a cemented carbide mold for rapid hot pressing deformation, and the rapid thermal deformation process parameter is: rising to 400 ° C at a heating rate of 40 ° C / min, Apply 400MPa pressure, keep warm for 5min.
  • Example 2 A technique for magnetic hardening of a Mn 2.70 Ga alloy was carried out as follows:
  • the tetragonal phase alloy block obtained in the second step is placed in a cemented carbide mold of a certain size for rapid hot pressing deformation, and the rapid hot pressing process parameter is: raising the temperature to 400 at a heating rate of 50 ° C / min. °C, then heat and apply pressure 400MPa, heat preservation for 5min.
  • Example 3 A technique for magnetic hardening of a Mn 2.50 Ga alloy was carried out as follows:
  • the Mn 2.50 Ga ingot obtained in the first step is heat-treated at 600 ° C for 24 hours in an argon atmosphere to obtain a tetragonal phase alloy block;
  • the tetragonal phase alloy block obtained in the second step is placed in a cemented carbide mold for rapid hot pressing deformation, and the rapid thermal deformation process parameter is: raising the temperature to 500 ° C at a heating rate of 60 ° C / min, and then The heat was applied and the pressure was applied at 500 MPa, and the pressure was kept for 10 minutes.
  • Example 4 A technique for magnetic hardening of a Mn 1.80 Ga alloy was carried out as follows:
  • the Mn 1.80 Ga ingot is obtained by melting in a smelting furnace under an argon atmosphere;
  • the Mn 1.80 Ga ingot obtained in the first step is heat-treated at 610 ° C for 7 days in an argon atmosphere to obtain a tetragonal phase alloy block;
  • the tetragonal phase alloy block obtained in the second step is placed in a cemented carbide mold for rapid hot pressing deformation, and the rapid thermal deformation process parameter is: raising the temperature to 400 ° C at a heating rate of 60 ° C / min, and then The heat was applied and the pressure was applied at 500 MPa, and the pressure was kept for 10 minutes.
  • Example 5 A technique for magnetic hardening of a Mn 1.33 Ga alloy was carried out as follows:
  • the Mn 1.33 Ga ingot is obtained by melting in a smelting furnace under an argon atmosphere;
  • the Mn 1.33 Ga ingot obtained in the first step is heat-treated at 520 ° C for 24 hours in an argon atmosphere to obtain a tetragonal phase alloy block;
  • the tetragonal phase alloy block obtained in the second step is placed in a cemented carbide mold of a certain size for rapid hot pressing deformation treatment, and the rapid hot pressing process parameter is: rising to 600 at a heating rate of 80 ° C / min. °C, then heat and apply pressure 300MPa, heat preservation for 5min.
  • Example 6 A technique for magnetic hardening of a Mn 1.15 Ga alloy was carried out as follows:
  • the Mn 1.15 Ga ingot obtained in the first step is heat-treated at 470 ° C for 2 days in an argon atmosphere to obtain a tetragonal alloy alloy block;
  • the tetragonal phase alloy block obtained in the second step is placed in a cemented carbide mold for rapid hot pressing deformation, and the rapid thermal deformation process parameters are: rising to 450 ° C at a heating rate of 80 ° C / min, and then The temperature was kept at 300 MPa, and the pressure was maintained for 2 minutes.
  • VSM vibrating sample magnetometer

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  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
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Abstract

一种Mn-Ga合金及其磁硬化方法，属于功能材料领域。首先通过熔炼获得Mn xGa(1.0≤x≤3.0)铸锭，经400～650℃热处理获得四方相，四方相合金块体在300～700℃和30～800MPa压力下利用放电等离子烧结(SPS)设备进行热变形，获得了具有较大矫顽力的锰镓合金磁体。该Mn-Ga合金磁体具有较高的剩磁、较大的矫顽力和较为优异的磁能积，在永磁领域具有应用潜力。

Description

一种Mn-Ga合金磁硬化的方法 技术领域
本发明公开了一种磁硬化Mn-Ga合金的方法，属于功能材料技术领域。
背景技术
永磁材料在在机械、通信、自动化、仪器仪表和医疗卫生等领域应用广泛，已成为现代工业和科学技术的支撑材料之一。近年来，国际市场稀土价格的剧烈波动以及各国对稀土的调控性使用，使得开发和研究具有高性能、高稳定性的非稀土永磁材料成为国际上的研究热点。Mn-Ga二元合金由于其丰富的相结构、多样的内禀磁性及在众多领域潜在的应用价值而引起了研究者的热切关注。例如，具有面心四方D022结构、亚铁磁有序、高自旋极化率和高居里温度的Mn3Ga合金是新型自旋转移矩(STT)材料的重要候选者之一；而具有低对称性的四方L10-MnGa合金则被预言有成为磁能积最高的新型非稀土永磁材料的潜力。理论计算表明，L10-MnGa合金的饱和磁化强度Ms可达116emu/g，其最大理论磁能积(BH)max则可高达28MGOe，与钴基稀土永磁材料相当。因此，四方结构的Mn-Ga合金被认为具有在永磁领域应用的潜力。目前，很多研究机构对Mn-Ga合金的制备、相转变、结构以及内禀磁性进行了研究，并已经获得了饱和磁化强度达到92emu/g的Mn1.15Ga合金，但是关于合金的磁硬化方面的研究相对较少。
众所周知，优异的内禀磁性是获得高技术磁化特性的基础和先决条件，但能否将这些性能发挥出来，获得高的矫顽力，还取决于磁体的磁硬化过程。要发挥锰镓合金在永磁领域的应用潜力，就必须解决合金磁硬化的问题，尤其是获得四方单相各向异性Mn-Ga块体。然而，目前关于锰镓合金磁硬化的研究仅仅局限在球磨制粉，以及合金粉在石蜡中简单取向，尚且没有研究人员得到各向异性磁体。2015年报道德国学者T.Mix,K.-H.Müller等人在5T磁场下取向了石蜡和Mn55Ga45合金粉制成的样品，观察到了各向异性。并且发现尺寸小于10μm的颗粒取向度优于尺寸10-30μm颗粒的取向度。上述实验证明锰镓合金粉体可以进行取向，但通过混合石蜡得到的样品密度和磁性能太低不足以在实际中进行应用，如何在不降低磁性能的条件下保留其取向效果成了需要解决的问题。
将合金塑性变形是一种获得磁硬化的有效途径，而且已经在稀土永磁合金Nd-Fe-B和Sm-Co中获得了成功。热变形法是制造NdFeB系各向异性材料的重要工艺手段之一。放电等离子烧结(SPS)设备具有操作简单，加热均匀，升温速度快，效率高等特点，利用SPS进行热变形是制备高性能NdFeB材料的有效手段。岳明等人利用SPS热变形法制备了性能优异的NdFeB各向异性永磁体。但是，目前还没有通过合金塑性变形得到致密的磁硬化Mn-Ga合金磁体的先例。
由于锰镓合金相结构丰富，相变复杂，并且不同成分的合金磁性能和塑性不同，因此，Mn-Ga合金热变形的制备需要严格控制热变形工艺条件。本发明通过细致调控放电等离子烧结过程的升温速率、保温温度、热变形压力和加压时间等条件，成功获得了具有较大矫顽力和具有一定各向异性的锰镓块状磁体。
发明内容
本发明首先通过熔炼获得MnxGa(1.0≤x≤3.0)铸锭，经400～650℃热处理获得四方相，四方相合金块体经300～700℃和30～800MPa压力下利用放电等离子烧结(SPS)设备进行热变形，获得了具有较大矫顽力和具有一定各向异性的锰镓块状磁体。
本发明获得磁硬化的Mn-Ga合金块体技术如下：
第一步，将99.9％纯Mn与99.99％的纯Ga按摩尔比x：1完成称重后，利用熔炼炉在氩气氛围下熔炼获得MnxGa铸锭，1.0≤x≤3.0；
第二步，第一步得到的MnxGa铸锭在氩气氛围中于400～650℃下进行热处理，获得四 方相合金块体；
第三步，将第二步得到的四方相合金块体置于模具中，使用SPS进行快速热压变形处理，快速热变形工艺参数为：先以30～120℃/min的升温速率升至400～700℃，再施加30～800MPa的压力，或者升温与加压同时进行；并保温保压2～10min，即可获得磁硬化后的锰镓磁体。
第一步和第二步中为避免氧化，熔炼和热处理过程在惰性气体保护下进行，惰性气体可以是氩气。
第三步中所述的模具可以是石墨模具，也可以是硬质合金模具，热变形压力在100MPa以下时可以采用石墨磨具，超过或等于100MPa时应采用硬质合金磨具。
第三步中所述的热变形工艺避免相转变的发生。如施加压力的时机根据合金成分的不同可不同，随Mn含量降低，Mn-Ga镓合金四方相铸锭的塑性会变差，对于塑性较差的合金，应该先升温至合金具有较好的塑性后再加压，对于塑性较好的合金，应该尽早施加压力，以缩短合金处于高温的时间，或采用较低的温度，避免相转变的发生。
铸锭热处理温度和时间可根据铸锭的成分不同可进行调节，使得热处理后合金物相为四方相；SPS所用的模具可以是石墨模具，也可以是硬质合金模具，优选的是可以承受较大压力的硬质合金模具；采用本发明的热变形温度工艺，既能保证锰镓合金具有足够的塑性，又不能使锰镓合金发生相转变；所采用的压力保证合金在热变形后有足够的变形量。
本发明获得的Mn-Ga合金磁体具有较高的剩磁，较大的矫顽力，较为优异的磁能积，在永磁领域具有应用潜力。
附图说明
图1为实施实例四制备的Mn1.80Ga合金热压磁体磁滞回线。
具体实施方式
以下，结合附图来详细说明本发明的实施方案，但本发明并不限于以下实施例。
实施例1：一种Mn3.0Ga合金磁硬化的技术，按以下步骤实施：
第一步，将99.9％纯Mn与99.99％的纯Ga按比例完成称重后，利用熔炼炉在氩气氛围下熔炼获得Mn3.0Ga铸锭；
第二步，第一步得到的Mn3.0Ga铸锭在氩气氛围中于500℃下进行热处理45min，获得四方相合金块体；
第三步，将第二步得到的四方相合金块体置于硬质合金模具中进行快速热压变形处理，快速热变形工艺参数为：以40℃/min的升温速率升至400℃，同时施加400MPa压力，保温保压5min。
实施例2：一种Mn2.70Ga合金磁硬化的技术，按以下步骤实施：
第一步，将99.9％纯Mn与99.99％的纯Ga按比例完成称重后，利用熔炼炉在氩气氛围下熔炼获得Mn2.70Ga铸锭；
第二步，第一步得到的Mn2.70Ga铸锭在氩气氛围中于500℃下进行热处理45min获得四方相合金块体；
第三步，将第二步得到的四方相合金块体置于一定尺寸的硬质合金模具中进行快速热压变形处理，快速热压工艺参数为：以50℃/min的升温速率升至400℃，然后保温并施加压力400MPa，保温保压5min。
实施例3：一种Mn2.50Ga合金磁硬化的技术，按以下步骤实施：
第一步，将99.9％纯Mn与99.99％的纯Ga按比例完成称重后，利用熔炼炉在氩气氛围 下熔炼获得Mn2.50Ga铸锭；
第二步，第一步得到的Mn2.50Ga铸锭在氩气氛围中于600℃下进行热处理24h，获得四方相合金块体；
第三步，将第二步得到的四方相合金块体置于硬质合金模具中进行快速热压变形处理，快速热变形工艺参数为：以60℃/min的升温速率升至500℃，然后保温并施加压力500MPa，保温保压10min。
实施例4：一种Mn1.80Ga合金磁硬化的技术，按以下步骤实施：
第一步，将99.9％纯Mn与99.99％的纯Ga按比例完成称重后，利用熔炼炉在氩气氛围下熔炼获得Mn1.80Ga铸锭；
第二步，第一步得到的Mn1.80Ga铸锭在氩气氛围中于610℃下进行热处理7天，获得四方相合金块体；
第三步，将第二步得到的四方相合金块体置于硬质合金模具中进行快速热压变形处理，快速热变形工艺参数为：以60℃/min的升温速率升至400℃，然后保温并施加压力500MPa，保温保压10min。
实施例5：一种Mn1.33Ga合金磁硬化的技术，按以下步骤实施：
第一步，将99.9％纯Mn与99.99％的纯Ga按比例完成称重后，利用熔炼炉在氩气氛围下熔炼获得Mn1.33Ga铸锭；
第二步，第一步得到的Mn1.33Ga铸锭在氩气氛围中于520℃下进行热处理24h，获得四方相合金块体；
第三步，将第二步得到的四方相合金块体置于一定尺寸的硬质合金模具中进行快速热压变形处理，快速热压工艺参数为：以80℃/min的升温速率升至600℃，然后保温并施加压力300MPa，保温保压5min。
实施例6：一种Mn1.15Ga合金磁硬化的技术，按以下步骤实施：
第一步，将99.9％纯Mn与99.99％的纯Ga按比例完成称重后，利用熔炼炉在氩气氛围下熔炼获得Mn1.15Ga铸锭；
第二步，第一步得到的Mn1.15Ga铸锭在氩气氛围中于470℃下进行热处理2天，获得四方相合金块体；
第三步，将第二步得到的四方相合金块体置于硬质合金模具中进行快速热压变形处理，快速热变形工艺参数为：以80℃/min的升温速率升至450℃，然后保温并施加压力300MPa，保温保压2min后卸压降温。
性能测试
使用振动样品磁强计(VSM)测试以上实施例制得样品的-3T～3T范围内的室温下磁滞回线，磁体性能如表1所示，其中Ms指3T磁场下的磁化强度：
表1 MnxGa(1.0≤x≤3.0)合金磁硬化前后磁性能对比
Figure PCTCN2017103076-appb-000001
Figure PCTCN2017103076-appb-000002

Claims (5)

  1. 一种Mn-Ga合金磁硬化的方法，其特征在于，包括以下步骤：
    第一步，将99.9％纯Mn与99.99％的纯Ga按摩尔比x：1完成称重后，利用熔炼炉在氩气氛围下熔炼获得MnxGa铸锭，1.0≤x≤3.0；
    第二步，第一步得到的MnxGa铸锭在氩气氛围中于400～650℃下进行热处理，获得四方相合金块体；
    第三步，将第二步得到的四方相合金块体置于模具中，使用SPS进行快速热压变形处理，快速热变形工艺参数为：先以30～120℃/min的升温速率升至400～700℃，再施加30～800MPa的压力，或者升温与加压同时进行；并保温保压2～10min，即可获得磁硬化后的锰镓磁体。
  2. 按照权利要求1所述的方法，其特征在于，热变形温度工艺，不能使锰镓合金发生相转变。
  3. 按照权利要求1所述的方法，其特征在于，第一步和第二步中为避免氧化，熔炼和热处理过程在惰性气体保护下进行。
  4. 按照权利要求1所述的方法，其特征在于，第三步中所述的模具是石墨模具，或是硬质合金模具，热变形压力在100MPa以下时采用石墨磨具，超过或等于100MPa时采用硬质合金磨具。
  5. 按照权利要求1-4任一项所述的方法制备得到的Mn-Ga合金。
PCT/CN2017/103076 2017-01-06 2017-09-25 一种mn-ga合金及其磁硬化方法 WO2018126738A1 (zh)

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