CN111091944A - Lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material and preparation method thereof - Google Patents

Lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material and preparation method thereof Download PDF

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CN111091944A
CN111091944A CN201911423870.9A CN201911423870A CN111091944A CN 111091944 A CN111091944 A CN 111091944A CN 201911423870 A CN201911423870 A CN 201911423870A CN 111091944 A CN111091944 A CN 111091944A
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CN111091944B (en
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金佳莹
陶永明
严密
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Zhejiang University ZJU
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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
    • H01F1/032—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 hard-magnetic materials
    • H01F1/04—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 hard-magnetic materials metals or alloys
    • H01F1/047—Alloys characterised by their composition
    • H01F1/053—Alloys characterised by their composition containing rare earth metals
    • H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • 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
    • 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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  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material and a preparation method thereof. Based on the characteristics of high temperature rise speed and short heating time and heat preservation time of the spark plasma sintering technology, the interdiffusion and chemical heterogeneity of elements in the lanthanum-cerium-yttrium-rich multi-main-phase magnet are controlled, the appearance, the magnetic hardening and the pinning effect of various core shells are accurately controlled, and the coercive force of the magnet is improved; the rapid sintering is utilized to avoid abnormal growth of crystal grains, the design step-by-step temperature rise, accurate temperature control and uniform heating are realized, the phenomenon that a thick crystal area and a thin crystal area coexist due to overheating of a local area in the sintering process is avoided, the uniformity of the internal organization structure of the magnet is realized, the crystal grains are fine, the average crystal grain size is smaller than 5 mu m, the comprehensive magnetic performance of the lanthanum-cerium-yttrium-rich multi-main-phase rare earth permanent magnet material is improved, and the commercial requirement is met. The preparation method is simple, convenient and easy to operate, can accurately control the element distribution and the organization structure of the multi-main-phase magnet, reduces the preparation period and the cost, and is suitable for large-scale production.

Description

Lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material and preparation method thereof
Technical Field
The invention relates to the field of permanent magnets, in particular to a lanthanum-rich cerium-yttrium multi-main-phase fine-grain rare earth permanent magnet material and a preparation method thereof.
Background
With the continuous expansion of the application of the neodymium iron boron rare earth permanent magnet, the demand of the rare earth element Nd/Pr/Dy/Tb continuously rises, and the price is high; the three rare earth elements of lanthanum La, cerium Ce and yttrium Y are low in price and high in reserves in the crust, so that the rare earth elements are expected to replace Nd/Pr/Dy/Tb and other scarce rare earth elements in large quantities and are used for producing low-cost rare earth elementsThe earth permanent magnet has become a research hotspot in the field of rare earth permanent magnets at home and abroad in recent years. The strong magnetism of the 2:14:1 type rare earth permanent magnet is derived from the intrinsic hard magnetism of a tetragonal phase compound. La2Fe14B saturated magnetic polarization strength Js1.38T, magnetocrystalline anisotropy field HAAbout 20kOe, Ce2Fe14B saturated magnetic polarization strength Js1.17T, magnetocrystalline anisotropy field HAAbout 26kOe, Y2Fe14B saturated magnetic polarization strength Js1.41T, magnetocrystalline anisotropy field HAAbout 26kOe, all less than Nd2Fe141.60T and 73kOe for B. Further, La2Fe14B、Ce2Fe14B and Y2Fe14The Curie temperature of B is also lower than that of Nd2Fe14B. Therefore, the intrinsic magnetic performance of the 2:14:1 phase formed by uniformly substituting Nd by La, Ce and Y is weaker than that of neodymium iron boron, and the magnetic performance of the neodymium iron boron is reduced, so that a remarkable magnetic dilution effect is caused.
Compared with a single-main-phase magnet, the rare earth elements in the multi-main-phase magnet are unevenly distributed, and the long-range and short-range magnetic interaction among local areas with different intrinsic hard magnetism can partially inhibit the magnetic dilution effect caused by lanthanum, cerium and yttrium substitution. However, by adopting the traditional sintering process, the mutual diffusion behavior of the rare earth elements in the multi-main-phase magnet is difficult to accurately control, and in the long-time high-temperature sintering process, elements with high diffusion speed, such as Ce, are easy to form a thicker shell layer rich in high-abundance rare earth elements, have a lower magnetocrystalline anisotropy field, are easy to become nucleation sites in the demagnetization process, and reduce the coercive force. The rare earth-rich phase in the lanthanum, cerium and yttrium-rich magnet is easy to oxidize and has insufficient wettability with the main phase, thus deteriorating the microstructure and reducing the density; in order to improve the compactness, the sintering temperature is increased, the main phase crystal grains grow abnormally, the mutual diffusion of rare earth elements in the main phase is intensified, and the magnetic dilution effect is obvious. Therefore, how to solve the contradiction, accurately regulate and control the distribution of the rare earth elements in the multi-main-phase magnet, and relieve the magnetic dilution effect caused by the addition of lanthanum, cerium and yttrium is the key for preparing the high-performance and high-abundance rare earth permanent magnet, promoting the high-efficiency and balanced utilization of rare earth resources in China and improving the competitiveness of rare earth downstream industries in China.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material and a preparation method thereof.
The invention relates to a lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material which is characterized by comprising two main alloys, wherein the alloy I comprises the following components in percentage by mass (R)xA1-x)yQbalMzBwR is one or more of high-abundance rare earth elements La, Ce and Y, A is one or more of other lanthanide rare earth elements except La, Ce and Y, Q is one or more of Fe, Co and Ni, M is one or more of Al, Cr, Cu, Ga, Mn, Mo, N, Nb, P, Pb, Si, Ta, Ti, V and Zr, and B is boron; x, y, z, w satisfy the following relationship: x is more than or equal to 0.2 and less than or equal to 0.8, y is more than or equal to 26 and less than or equal to 36, z is more than or equal to 0 and less than or equal to 3, and w is more than or equal to 0.8 and less than or equal to 1.3; the component of the alloy II is A'aQ’balM’cBdWherein A ' is one or more of other lanthanide rare earth elements except La, Ce and Y, Q ' is one or more of Fe, Co and Ni, M ' is one or more of Al, Cr, Cu, Ga, Mn, Mo, N, Nb, P, Pb, Si, Ta, Ti, V and Zr, and B is boron; a. c and d satisfy the following relation: a is more than or equal to 26 and less than or equal to 36, c is more than or equal to 0 and less than or equal to 3, and d is more than or equal to 0.8 and less than or equal to 1.3.
The invention relates to a preparation method of a lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material, which comprises the following steps:
1) preparing two types of main alloy magnetic powder by using a rapid hardening casting sheet, a hydrogen crushing and air flow grinding process or a rapid quenching casting belt and HDDR process;
2) uniformly mixing the two main alloy magnetic powders, wherein the first main alloy accounts for 10-90% of the total powder weight;
3) and (3) carrying out orientation compression on the uniformly mixed magnetic powder under a magnetic field, then loading the green body into a discharge plasma device, and carrying out step-by-step discharge plasma sintering: the temperature is rapidly raised to T at a temperature rise rate of 50-400 ℃/min1Keeping the temperature for 5-20 min, and slowly raising the temperature to the final temperature T at the temperature raising speed of 5-15 ℃/min2Keeping the temperature at 10-100 min, and applying pressure20-200 MPa; wherein T is more than or equal to 500 DEG C2≤1000℃，T1＝T2-x，10≤x≤100；
4) The sintered magnet does not need to be subjected to heat treatment, or is subjected to one-step heat treatment or is subjected to two-step heat treatment, wherein the temperature of the one-step heat treatment is 400-1000 ℃, the temperature of the first-stage tempering in the two-step heat treatment is 700-1000 ℃, and the temperature of the second-stage tempering is 400-700 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1) by utilizing the characteristics of high temperature rise speed and short heating time and heat preservation time of the spark plasma sintering technology, the interdiffusion and chemical heterogeneity of elements in the lanthanum-cerium-yttrium-rich multi-main-phase magnet are controlled, the appearance, the magnetic hardening and the pinning effect of various core shells are accurately controlled, and the coercive force of the magnet is improved;
2) the rapid sintering is utilized to avoid abnormal growth of crystal grains, a special step-by-step heating mode is designed, the temperature is accurately controlled, the heating is more uniform, the phenomena that local areas are overheated and thick and thin crystal areas coexist in the sintering process are avoided, the uniformity of the internal organization structure of the magnet is realized, the crystal grains are fine, the average crystal grain size is smaller than 5 mu m (the average crystal grain size in the sintered magnet is usually larger than 5 mu m), the comprehensive magnetic performance of the lanthanum-cerium-yttrium-rich multi-main-phase rare earth permanent magnet material is improved, and the commercial requirement is met;
3) the process flow is easy to operate, the element distribution and the organization structure of the multi-main-phase magnet can be accurately controlled, the preparation period is greatly shortened, and the manufacturing cost is greatly reduced. Is suitable for large-scale production.
Detailed Description
The present invention is further illustrated by the following examples, but is not limited to the following examples:
example 1:
alloy one comprises the following components in percentage by mass [ (Pr, Nd)0.5Ce0.5]31FebalCu0.2Zr0.15B1.0Alloy two comprises the components (Pr, Nd) in percentage by mass31FebalCu0.2Zr0.15B1.0(ii) a Using rapid-hardening cast pieces, hydrogen blasting, air flowMilling to prepare powder, and uniformly mixing the two main alloy magnetic powders, wherein the first main alloy accounts for 90% of the total powder weight; and (3) carrying out orientation compression on the uniformly mixed magnetic powder under a magnetic field, then loading the green body into a discharge plasma device, and carrying out step-by-step discharge plasma sintering: rapidly heating to 600 ℃ at a heating rate of 150 ℃/min, preserving heat for 10min, heating to 650 ℃ at a heating rate of 10 ℃/min, preserving heat for 30min, and applying pressure of 100 MPa; the sintered magnet does not need heat treatment; the average grain size of the magnet was 3.5 μm, and the magnetic property was Br＝12.5kG，Hcj＝10.0kOe，(BH)max＝34.7MGOe。
Example 2:
alloy one comprises the following components in percentage by mass [ (Pr, Nd)0.2Ce0.8]26FebalCu0.5Zr0.2Al0.3Ga0.3B1.0Alloy two comprises the components (Pr, Nd) in percentage by mass36FebalCu0.2Zr0.3B1.05(ii) a Preparing powder by using a rapid hardening casting sheet, a hydrogen crushing process and an air flow milling process, and uniformly mixing magnetic powder of two main alloys, wherein the first main alloy accounts for 10% of the total weight of the powder; and (3) carrying out orientation compression on the uniformly mixed magnetic powder under a magnetic field, then loading the green body into a discharge plasma device, and carrying out step-by-step discharge plasma sintering: rapidly heating to 900 ℃ at a heating rate of 400 ℃/min, preserving heat for 5min, heating to 1000 ℃ at a heating rate of 5 ℃/min, preserving heat for 100min, and applying pressure of 20 MPa; performing two-step heat treatment on the sintered magnet, wherein the primary tempering temperature is 900 ℃, and the secondary tempering temperature is 600 ℃; the average grain size of the magnet was 4.5 μm, and the magnetic property was Br＝13.2kG，Hcj＝15.0kOe，(BH)max＝43.7MGOe。
Example 3:
the alloy one comprises the following components in percentage by mass0.5Ce0.4Y0.1]30FebalGa0.2Cu0.1Al0.1Zr0.1B0.9The second alloy comprises Nd in percentage by mass30FebalGa0.2Cu0.1Al0.1Zr0.1B0.9(ii) a Preparing powder by using a quick quenching melt-spun belt and an HDDR process, and uniformly mixing magnetic powder of two main alloys, wherein the first main alloy accounts for 80% of the total weight of the powder; and (3) carrying out orientation compression on the uniformly mixed magnetic powder under a magnetic field, then loading the green body into a discharge plasma device, and carrying out step-by-step discharge plasma sintering: rapidly heating to 550 ℃ at a heating rate of 400 ℃/min, preserving heat for 20min, heating to 600 ℃ at a heating rate of 15 ℃/min, preserving heat for 20min, and applying pressure of 200 MPa; the sintered magnet does not need heat treatment; the average crystal grain size of the magnet is 340nm, and the magnetic property is Br＝12.7kG，Hcj＝12.0kOe，(BH)max＝39.2MGOe。
Example 4:
the alloy one comprises the following components in percentage by mass0.5Ce0.32La0.18]30FebalCu0.1Al0.1Nb0.1B1.0The second alloy comprises Nd in percentage by mass30FebalCu0.1Al0.1Nb0.1B1.0(ii) a Preparing powder by using a quick quenching melt-spun belt and an HDDR process, and uniformly mixing magnetic powder of two main alloys, wherein the first main alloy accounts for 50% of the total weight of the powder; and (3) carrying out orientation compression on the uniformly mixed magnetic powder under a magnetic field, then loading the green body into a discharge plasma device, and carrying out step-by-step discharge plasma sintering: rapidly heating to 650 ℃ at a heating rate of 200 ℃/min, preserving heat for 10min, heating to 700 ℃ at a heating rate of 5 ℃/min, preserving heat for 20min, and applying pressure of 50 MPa; carrying out one-step heat treatment on the sintered magnet, wherein the temperature of the one-step heat treatment is 580 ℃; the average crystal grain size of the magnet is 380nm, and the magnetic property is Br＝12.8kG，Hcj＝12.2kOe，(BH)max＝40.1MGOe。
Example 5:
alloy one comprises the following components in percentage by mass [ (Pr, Nd)0.8Ce0.2]32FebalCu0.5Zr0.2Ga0.8Al0.6Co0. 6Ti0.3B0.8Alloy two comprises the components (Pr, Nd) in percentage by mass31FebalCu0.5Zr0.2Ga0.8Al0.6Co0.6Ti0.3B1 .0(ii) a Preparing powder by using a rapid hardening casting sheet, a hydrogen crushing process and an air flow milling process, and uniformly mixing magnetic powder of two main alloys, wherein the first main alloy accounts for 10% of the total weight of the powder; and (3) carrying out orientation compression on the uniformly mixed magnetic powder under a magnetic field, then loading the green body into a discharge plasma device, and carrying out step-by-step discharge plasma sintering: rapidly heating to 700 deg.C at a heating rate of 50 deg.C/min, maintaining for 20min, heating to 800 deg.C at a heating rate of 10 deg.C/min, maintaining for 30min, and applying pressure of 20 MPa; performing two-step heat treatment on the sintered magnet, wherein the primary tempering temperature is 890 ℃, and the secondary tempering temperature is 480 ℃; the average grain size of the magnet was 3.9 μm, and the magnetic property was Br＝13.4kG，Hcj＝15.0kOe，(BH)max＝45.7MGOe。

Claims (2)

1. A lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material is characterized by comprising two main alloys, wherein the first alloy comprises the following components in percentage by mass (R)xA1-x)yQbalMzBwR is one or more of high-abundance rare earth elements La, Ce and Y, A is one or more of other lanthanide rare earth elements except La, Ce and Y, Q is one or more of Fe, Co and Ni, M is one or more of Al, Cr, Cu, Ga, Mn, Mo, N, Nb, P, Pb, Si, Ta, Ti, V and Zr, and B is boron; x, y, z, w satisfy the following relationship: x is more than or equal to 0.2 and less than or equal to 0.8, y is more than or equal to 26 and less than or equal to 36, z is more than or equal to 0 and less than or equal to 3, and w is more than or equal to 0.8 and less than or equal to 1.3; the component of the alloy II is A'aQ’balM’cBdWherein A ' is one or more of other lanthanide rare earth elements except La, Ce and Y, Q ' is one or more of Fe, Co and Ni, M ' is one or more of Al, Cr, Cu, Ga, Mn, Mo, N, Nb, P, Pb, Si, Ta, Ti, V and Zr, and B is boron; a. c and d satisfy the following relation: a is more than or equal to 26 and less than or equal to 36, c is more than or equal to 0 and less than or equal to 3, and d is more than or equal to 0.8 and less than or equal to 1.3.
2. A method for preparing the lanthanum-rich cerium-yttrium multi-host-phase fine-crystalline rare earth permanent magnet material of claim 1, comprising the steps of:
1) preparing two types of main alloy magnetic powder by using a rapid hardening casting sheet, a hydrogen crushing and air flow grinding process or a rapid quenching casting belt and HDDR process;
2) uniformly mixing the two main alloy magnetic powders, wherein the first main alloy accounts for 10-90% of the total powder weight;
3) and (3) carrying out orientation compression on the uniformly mixed magnetic powder under a magnetic field, then loading the green body into a discharge plasma device, and carrying out step-by-step discharge plasma sintering: the temperature is rapidly raised to T at a temperature rise rate of 50-400 ℃/min1Keeping the temperature for 5-20 min, and slowly raising the temperature to the final temperature T at the temperature raising speed of 5-15 ℃/min2Keeping the temperature for 10-100 min, and applying pressure of 20-200 MPa; wherein T is more than or equal to 500 DEG C2≤1000℃，T1＝T2-x，10≤x≤100；
4) The sintered magnet does not need to be subjected to heat treatment, or is subjected to one-step heat treatment or is subjected to two-step heat treatment, wherein the temperature of the one-step heat treatment is 400-1000 ℃, the temperature of the first-stage tempering in the two-step heat treatment is 700-1000 ℃, and the temperature of the second-stage tempering is 400-700 ℃.
CN201911423870.9A 2019-12-31 2019-12-31 Lanthanum-cerium-yttrium-rich multi-main-phase fine-grain rare earth permanent magnet material and preparation method thereof Active CN111091944B (en)

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WO2021136366A1 (en) * 2019-12-31 2021-07-08 浙江大学 Method suitable for grain boundary diffusion of bulk rare earth permanent magnet material
CN113130200A (en) * 2021-04-26 2021-07-16 浙江大学 Method for improving magnetic property of Ce-Y-rich rare earth permanent magnet

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021136366A1 (en) * 2019-12-31 2021-07-08 浙江大学 Method suitable for grain boundary diffusion of bulk rare earth permanent magnet material
CN113130200A (en) * 2021-04-26 2021-07-16 浙江大学 Method for improving magnetic property of Ce-Y-rich rare earth permanent magnet

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