Method for high-throughput preparation of RE-Fe-M-B diffusion couple

RE-Fe-M-B diffusion couples are prepared by discharge plasma sintering technology and layered interleaved pile chopping method, which solves the problems of intimate diffusion interface bonding and inaccurate acquisition of phase change thermodynamic information in the prior art, and realizes Qualcomm Efficient preparation and testing of alloy diffusion couples.

CN119446760APending Publication Date: 2025-02-14ZHEJIANG UNIV
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Patent Information

Application Number
CN202411567860.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-05
Publication Date
2025-02-14

AI Technical Summary

Technical Problem

In the prior art, when preparing diffusion couples of neodymium iron boron permanent magnet materials, there are problems such as uncontrollable force and easy unloading of force at high temperatures, resulting in voids or inconsistencies at the diffusion interface, and the heating and cooling rates limit the phase. Accurate acquisition of variable thermodynamic information.

Method used

Discharge plasma sintering technology is used to achieve precise control of lifting, cooling and pressure. Instruments of different components are placed into the discharge plasma device for sintering through layered interleaving piles and chopping, completing the preparation of high-throughput alloy diffusion couples.

Benefits of technology

It improves the interface combination effect, shortens the experimental cycle, saves costs and manpower, achieves precise control of the solid-state diffusion process, and clarifies the phase formation rules and phase relationships of the RE-Fe-M-B system.

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Abstract

The invention discloses a method for preparing an RE-Fe-M-B diffusion couple at high flux. The method mainly comprises the steps that proportioning is conducted according to RExFebalMyBz and RE 'tM100-t component design, and two types of cast ingots are obtained through vacuum melting; carrying out long-time homogenization heat treatment on each smelted cast ingot; and after cutting and surface treatment are conducted, the RExFebalMyBz cast ingot and the RE'tM100-t cast ingot are put into a discharge plasma device in a layered staggered stacking mode and pressurized, discharge plasma sintering is conducted, and preparation of the high-flux alloy diffusion couple is completed. And then the high-flux alloy diffusion couple is subjected to vacuum quartz glass tube sealing, heat preservation annealing is conducted, then quenching is conducted, and the RE-Fe-M-B diffusion couple is obtained. And subsequently analyzing the components and phase composition of the quenched diffusion even section. According to the method, the research and development period of the material is greatly shortened, and guidance is provided for component design and preparation process optimization of the rare earth iron boron magnet.
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Description

Technical Field

[0001] The invention relates to the field of rare earth permanent magnetic materials, and in particular to a method for preparing a RE-Fe-MB diffusion couple with high throughput. Background Art

[0002] The third generation of rare earth permanent magnet NdFeB has a high magnetic energy product that is unmatched by other permanent magnet materials. It is widely used in computer technology, information technology, aerospace technology, automation technology, medical equipment, etc. As an important material basis for the development of high-tech and social progress, NdFeB materials have developed very rapidly, accounting for ~2 / 3 of the output value of permanent magnet materials. The application areas of NdFeB products on the market are also roughly divided into three categories. The first category is high-end fields, such as nuclear magnetic resonance equipment and voice coil motors; the second category is traditional industries, such as speakers; and the third category is relatively low-end products. For the first category of high-end fields, with the development of new energy and low-carbon economy, the demand for wind turbines and new energy vehicle motors has grown rapidly in recent years, which has also put forward higher performance requirements for high-end NdFeB permanent magnet products.

[0003] The improvement of performance is inseparable from the optimization design of NdFeB permanent magnet composition and process. If the traditional alloy sample preparation method is still used, a large number of samples are required, the cost is high, it takes a long time, and some phase components are easy to be ignored. In the past, the preparation of diffusion couples was often fired in an ordinary tubular furnace. Due to the problems of uncontrollable force on the fixture and easy unloading of force at high temperature, there are often problems such as voids or loose bonding at the diffusion interface. In addition, the heating and cooling rates of ordinary tubular furnaces are limited. During the preparation of diffusion couples, some atoms have already diffused, which affects the accurate acquisition of phase change thermodynamic information. Summary of the invention

[0004] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a method for preparing RE-Fe-MB diffusion couples with high throughput. The present invention adopts spark plasma sintering technology to achieve precise control of temperature and pressure, thereby improving the bonding effect of the interface. The present invention is helpful to explore the phase formation law and the relationship between each phase of the RE-Fe-MB system, and to obtain the RE-Fe-MB intermediate phase of the rare earth alloy by high-throughput preparation and testing, which can greatly shorten the experimental cycle compared with traditional methods.

[0005] The present invention first provides a method for preparing RE-Fe-MB diffusion couples with high throughput, which mainly comprises the following steps:

[0006] 1) According to RE x Fe bal M y B z and RE' t M 100-t The composition design is used to prepare the ingots, and several REx Fe bal M y B z Ingots and several RE' t M 100-t Ingot, wherein RE and RE' are one or more of La, Ce, Pr, Nd, Dy, Tb, M is one or more of the metal elements Co, Al, Cu, Ga, Nb, Ni, Zn, Si and Zr, 10≤x≤60, 0.5≤y≤20, 0.85≤z≤1.5, 10≤t≤90;

[0007] 2) subjecting the smelted ingots to a long-term homogenization heat treatment;

[0008] 3) Each ingot is cut and surface treated to obtain several RE x Fe bal M y B z Discs and several RE' t M 100-t disc, the obtained RE x Fe bal M y B z Wafer and RE' t M 100-t The discs are placed in a spark plasma device in a layered staggered stacking manner and pressurized to perform spark plasma sintering to complete the preparation of high-flux alloy diffusion couples;

[0009] 4) The high-flux alloy diffusion couple is sealed in a vacuum quartz glass tube, annealed at a required temperature and for a required time, and then quenched to obtain a RE-Fe-MB diffusion couple.

[0010] Furthermore, in step (1), during the batching process, by changing RE x Fe bal M y B z or RE' t M 100-t The element type or content in the sample can be used to obtain several RE with different compositions. x Fe bal M y B z Ingot or several RE's of different compositions t M 100-t Ingots. The several types may be one or more. Preferably, the total number of ingot types is ≥3, more preferably ≥5, so as to conduct diffusion studies of different components at high throughput simultaneously.

[0011] Furthermore, the homogenization heat treatment in step (2) is achieved by vacuum sealing, requiring the sealing atmosphere to be 0.03-0.06 MPa argon atmosphere, and the heat preservation time is ≥180 h.

[0012] Furthermore, in step (3), each ingot is cut into discs of Φd*h, measured in millimeters, 10≤d≤50, 1≤h≤5, wherein d is the diameter of the disc and h is the thickness; wherein d needs to be the same in ingots of different compositions.

[0013] Furthermore, the surface treatment in step (3) is to grind and polish with 400#, 600#, 800#, 1000#, 1200#, and 1500# sandpaper in sequence until a smooth and flat sample surface is obtained.

[0014] Furthermore, the layered staggered stacking method in step (3) refers to any two adjacent layers of wafers, one of which is RE x Fe bal M y B z disc, the other layer is RE' t M 100-t When there are multiple different RE x Fe bal M y B z Wafer or multiple different RE' t M 100-t When the wafer is round, it still follows a layer of RE x Fe bal M y B z Wafer, one layer of RE' t M 100-t The specific composition of each layer can be determined from the various RE prepared. x Fe bal M y B z Wafer or RE' t M 100-t Different compositions of RE x Fe bal M y B z The discs cannot be stacked adjacent to each other, and RE' t M 100-t The discs cannot be stacked adjacent to each other. The total number of stacking layers N ≥ 5.

[0015] Furthermore, during the spark plasma sintering process in step (3), the temperature is rapidly raised to 400-900° C. at a heating rate of 50-400° C. / min, kept at this temperature for 5-30 minutes, and a pressure of 2-10 kN is applied.

[0016] Furthermore, the heat treatment in step (4) is achieved by vacuum sealing, requiring the sealing atmosphere to be 0.03-0.06 MPa argon atmosphere, the heat treatment temperature to be 500-1100° C., and the time to be 5-30 days.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] The method for preparing RE-Fe-MB diffusion couple based on high-flux alloy diffusion couple provided by the present invention can obtain multiple three-phase and two-phase equilibrium relationships in one sample, avoid repeated preparation and testing of multiple samples, and is lower in cost and higher in efficiency than traditional methods, saving a lot of time and manpower; two ingots are sintered to form diffusion layers through sintering, and each diffusion layer can obtain its phase structure, and after measurement, the solid solubility of intermetallic compounds or a certain type of specific elements therein can be obtained; by using spark plasma sintering technology, precise regulation of temperature and pressure can be achieved, and precise control of the solid-state diffusion process can be achieved, and the clarity of the diffusion layer interface of the diffusion couple is greatly improved, and the bonding effect of the interface is improved; at the same time, the diffusion of the sample before heat treatment can be reduced, which is more conducive to clarifying the phase formation law and the phase relationship of each phase of the RE-Fe-MB system. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 Schematic diagram of the prepared RE-Fe-MB system high-flux alloy diffusion couple.

[0020] Figure 2 The (Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.5 Nb 0.2 B1 / Nd 70 Al 10 Cu 10 Ga 10 / (Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.5 Nb 0.2 B1 interface scanning electron microscope image. DETAILED DESCRIPTION

[0021] The present invention is further described below in conjunction with specific embodiments, but the present invention is not limited to the following embodiments:

[0022] Embodiment 1:

[0023] (1) Select three types of RE x Fe bal M y B z Ingredients and two RE' t M 100-t as follows:

[0024] <![CDATA[RE x Fe bal M y B z Ingredients]]> <![CDATA[RE’ t M 100-t Ingredients]]> <![CDATA[(Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.5 Nb 0.2 B1]]> <h2 style=";text-align:left;direction:ltr"><![CDATA[Nd <h2 style=";text-align:left;direction:ltr"> 70 <h2 style=";text-align:left;direction:ltr"> Al<h2 style=";text-align:left;direction:ltr"> 20 <h2 style=";text-align:left;direction:ltr"> Ga<h2 style=";text-align:left;direction:ltr"> 10 <h2 style=";text-align:left;direction:ltr"><!-- 2 --> ]]><h2 style=";text-align:left;direction:ltr"> <![CDATA[(Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.8 Nb 0.2 B1]]> <![CDATA[Nd 70 the 10 With 10 Ga 10 ]]> <![CDATA[(Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.3 Nb 0.2 B1]]> /

[0025] The above five components are prepared respectively and the corresponding ingots are obtained by vacuum melting;

[0026] (2) The smelted ingots are subjected to a long-term homogenization heat treatment for 180 hours.

[0027] (3) Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.5 Nb 0.2 B1、(Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.8 Nb 0.2 B1、(Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.3 Nb 0.2 B1 ingots are cut into Φ15*3mm 3 The disc, Nd 70 Al 20 Ga 10 and Nd 70 Al 10 Cu 10 Ga 10 The ingot is cut into two pieces of Φ15*1mm 3 The cut surfaces of the discs were polished with 400#, 600#, 800#, 1000#, 1200#, and 1500# sandpapers to obtain (Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga0.5 Nb 0.2 B1 wafer, Nd 70 Al 10 Cu 10 Ga 10 Wafer, (Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.8 Nb 0.2 B1 wafer, Nd 70 Al 20 Ga 10 Disc and (Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.3 Nb 0.2 B1 discs are arranged in a layered staggered stack, such as Figure 1 As shown, two layers of RE are required x Fe bal M y B z A layer of RE' is set between the discs t M 100-t The discs were arranged and placed in a spark plasma device for spark plasma sintering. The temperature was rapidly raised to 500°C at a heating rate of 100°C / min, kept at this temperature for 10 min, and a pressure of 5 kN was applied to complete the preparation of the high-flux alloy diffusion couple.

[0028] (4) The high-flux alloy diffusion couple was sealed with a vacuum quartz glass tube and filled with 0.05 MPa argon. According to the temperature requirements of the subsequent experiments, three groups of parallel experiments were set up with different insulation temperatures (700, 800, and 900°C) to study the diffusion of the diffusion couples prepared at different insulation temperatures. The three groups of samples were annealed at 700, 800, and 900°C for 15 days, respectively, to obtain RE-Fe-MB diffusion couples.

[0029] Attached Figure 2 is(Nd 0.8 Pr 0.2 ) 30 Fe bal Al 0.2 Ga 0.5 Nb 0.2 B1 / Nd 70 Al 10 Cu 10 Ga 10 / (Nd 0.8 Pr 0.2 ) 30 Febal Al 0.2 Ga 0.3 Nb 0.2 From the electron microscope image of the B1 interface after plasma sintering, it can be seen that the prepared diffusion couple interface is tightly fitted, no cracks are generated, and almost no element diffusion occurs.

[0030] Embodiment 2:

[0031] (1) Select four REs x Fe bal M y B z Ingredients and three RE' t M 100-t The ingredients are as follows:

[0032] <![CDATA[RE x Fe bal M y B z Ingredients]]> <![CDATA[RE’ t M 100-t Ingredients]]> <h2 style=";text-align:left;direction:ltr"><![CDATA[(Nd <h2 style=";text-align:left;direction:ltr"> 0.9 <h2 style=";text-align:left;direction:ltr"> No<h2 style=";text-align:left;direction:ltr"> 0.1 <h2 style=";text-align:left;direction:ltr"> )<h2 style=";text-align:left;direction:ltr"> 30.5 <h2 style=";text-align:left;direction:ltr"> Fe<h2 style=";text-align:left;direction:ltr"> bal <h2 style=";text-align:left;direction:ltr"> Al<h2 style=";text-align:left;direction:ltr"> 0.15 <h2 style=";text-align:left;direction:ltr"> Ga<h2 style=";text-align:left;direction:ltr"> 0.45 <h2 style=";text-align:left;direction:ltr"> Co<h2 style=";text-align:left;direction:ltr"> 0.2 <h2 style=";text-align:left;direction:ltr"> Zr<h2 style=";text-align:left;direction:ltr"> 0.15 <h2 style=";text-align:left;direction:ltr"> B<h2 style=";text-align:left;direction:ltr"> 0.9 <h2 style=";text-align:left;direction:ltr"> ]]><h2 style=";text-align:left;direction:ltr"> <![CDATA[Pr 60 Those 20 Already 20 ]]> <h2 style=";text-align:left;direction:ltr"><![CDATA[(Nd <h2 style=";text-align:left;direction:ltr"> 0.7 <h2 style=";text-align:left;direction:ltr"> No<h2 style=";text-align:left;direction:ltr"> 0.3 <h2 style=";text-align:left;direction:ltr"> )<h2 style=";text-align:left;direction:ltr"> 30.5 <h2 style=";text-align:left;direction:ltr"> Fe<h2 style=";text-align:left;direction:ltr"> bal <h2 style=";text-align:left;direction:ltr"> Al<h2 style=";text-align:left;direction:ltr"> 0.15 <h2 style=";text-align:left;direction:ltr"> Ga<h2 style=";text-align:left;direction:ltr"> 0.45 <h2 style=";text-align:left;direction:ltr"> Co<h2 style=";text-align:left;direction:ltr"> 0.2 <h2 style=";text-align:left;direction:ltr"> Zr<h2 style=";text-align:left;direction:ltr"> 0.15 <h2 style=";text-align:left;direction:ltr"> B<h2 style=";text-align:left;direction:ltr"> 0.9 <h2 style=";text-align:left;direction:ltr"> ]]><h2 style=";text-align:left;direction:ltr"> <![CDATA[Pr 70 Those 10 Already 20 ]]> <h2 style=";text-align:left;direction:ltr"><![CDATA[(Nd <h2 style=";text-align:left;direction:ltr"> 0.5 <h2 style=";text-align:left;direction:ltr"> No<h2 style=";text-align:left;direction:ltr"> 0.5 <h2 style=";text-align:left;direction:ltr"> )<h2 style=";text-align:left;direction:ltr"> 30.5 <h2 style=";text-align:left;direction:ltr"> Fe<h2 style=";text-align:left;direction:ltr"> bal <h2 style=";text-align:left;direction:ltr"> Al<h2 style=";text-align:left;direction:ltr"> 0.15 <h2 style=";text-align:left;direction:ltr"> Ga<h2 style=";text-align:left;direction:ltr"> 0.45 <h2 style=";text-align:left;direction:ltr"> Co<h2 style=";text-align:left;direction:ltr"> 0.2 <h2 style=";text-align:left;direction:ltr"> Zr<h2 style=";text-align:left;direction:ltr"> 0.15 <h2 style=";text-align:left;direction:ltr"> B<h2 style=";text-align:left;direction:ltr"> 0.9 <h2 style=";text-align:left;direction:ltr"> ]]><h2 style=";text-align:left;direction:ltr"> <![CDATA[Pr 60 Those 20 Already 10 Zn 10 ]]> <h2 style=";text-align:left;direction:ltr"><![CDATA[(Nd <h2 style=";text-align:left;direction:ltr"> 0.3 <h2 style=";text-align:left;direction:ltr"> No<h2 style=";text-align:left;direction:ltr"> 0.7 <h2 style=";text-align:left;direction:ltr"> )<h2 style=";text-align:left;direction:ltr"> 30.5 <h2 style=";text-align:left;direction:ltr"> Fe<h2 style=";text-align:left;direction:ltr"> bal <h2 style=";text-align:left;direction:ltr"> Al<h2 style=";text-align:left;direction:ltr"> 0.15 <h2 style=";text-align:left;direction:ltr"> Ga<h2 style=";text-align:left;direction:ltr"> 0.45 <h2 style=";text-align:left;direction:ltr"> Co<h2 style=";text-align:left;direction:ltr"> 0.2 <h2 style=";text-align:left;direction:ltr"> Zr<h2 style=";text-align:left;direction:ltr"> 0.15 <h2 style=";text-align:left;direction:ltr"> B<h2 style=";text-align:left;direction:ltr"> 0.95 <h2 style=";text-align:left;direction:ltr"> ]]><h2 style=";text-align:left;direction:ltr"> /

[0033] The above seven components are prepared respectively and the corresponding ingots are obtained by vacuum melting;

[0034] (2) The smelted ingots are subjected to a long-term homogenization heat treatment for 180 hours.

[0035] (3) Cut each ingot into Φ20*2mm 3 The cut surface was polished with 400#, 600#, 800#, 1000#, 1200#, and 1500# sandpaper, and the obtained discs were sequentially processed according to (Nd 0.9 La 0.1 ) 30.5 Fe ba l Al 0.15 Ga 0.45 Co 0.2 Zr 0.15 B 0.95 Wafer, Pr 60 Dy 20 Al 20 Round piece,

[0036] (Nd 0.7 La 0.3 ) 30.5 Fe bal Al 0.15 Ga 0.45 Co 0.2 Zr 0.15 B 0.95 Wafer, Pr 70 Dy 10 Al 20 Round piece,

[0037] (Nd 0.5 La 0.5 )30.5 Fe bal Al 0.15 Ga 0.45 Co 0.2 Zr 0.15 B 0.95 Wafer, Pr 60 Dy 20 Al 10 Zn 10 Disc and (Nd 0.3 La 0.7 ) 30.5 Fe bal Al 0.15 Ga 0.45 Co 0.2 Zr 0.15 B 0.95 The order of the wafers is in a layered stacking manner (satisfying two layers of RE x Fe bal M y B z A layer of RE' is set between the discs t M 100-t The wafer was placed in a spark plasma device for spark plasma sintering, and the temperature was rapidly raised to 450°C at a heating rate of 100°C / min, kept at this temperature for 5 minutes, and a pressure of 4.5 kN was applied to complete the preparation of the high-flux alloy diffusion couple.

[0038] (4) The high-flux alloy diffusion couple was sealed with a vacuum quartz glass tube and filled with 0.05 MPa argon. According to the temperature requirements of the subsequent experiments, four groups of parallel experiments with different insulation temperatures (600, 700, 800, and 900°C) were set up to study the diffusion of the diffusion couples prepared at different insulation temperatures. The four groups of samples were annealed at 600, 700, 800, and 900°C for 14 days to obtain Nd-Fe-MB diffusion couples.

[0039] Embodiment 3:

[0040] (1) Select three types of RE x Fe bal M y B z Ingredients and two RE' t M 100-t The ingredients are as follows:

[0041] <![CDATA[RE x Fe bal M y B z Ingredients]]> <![CDATA[RE’ t M 100-t Ingredients]]> <![CDATA[(Nd 0.8 Fr. 0.1 Dy 0.1 ) 30.5 Fe bal With 0.25 the 0.25 Ga 0.5 Co5Ti 0.2 B 0.95 ]]> <![CDATA[Nd 60 Tb 20 Ga 10 What 10 ]]> <![CDATA[(Nd 0.65 Pr 0.15 Dy 0.2 , 30.5 Fe bal Al 0.15 Ga 0.5 Co 10 Ti 0.3 B 0.92 , <![CDATA[Nd 50 Tb 30 Ga 10 What 10 ]]> <![CDATA[(Nd 0.75 Pr 0.1 Dy 0.15 ) 31 Fe bal Al 0.25 Ga 0.35 Nb 0.2 B1]]> /

[0042] The above five components are prepared respectively and the corresponding ingots are obtained by vacuum melting;

[0043] (2) The smelted ingots are subjected to a long-term homogenization heat treatment for 180 hours.

[0044] (3) Nd 0.8 Pr 0.1 Dy 0.1 ) 30.5 Fe bal Cu 0.25 Al 0.25 Ga 0.5 Co5Ti 0.2 B 0.95 Ingot, (Nd 0.65 Pr 0.15 Dy 0.2 ) 30.5 Fe bal Al 0.15 Ga 0.5 Co 10 Ti 0.3 B 0.92 Ingot and (Nd 0.75 Pr 0.1 Dy 0.15 ) 31 Fe bal Al 0.25 Ga 0.35 Nb 0.2 B1 ingots are cut into Φ20*3mm 3 The disc, Nd 60 Tb 20 Ga 10 Co 10 and Nd 50 Tb 30 Ga 10 Co 10 The ingot is cut into two pieces of Φ20*1.5mm 3 The cut surface was polished with 400#, 600#, 800#, 1000#, 1200#, and 1500# sandpaper, and the obtained disc was (Nd 0.8 Pr 0.1 Dy 0.1 ) 30.5 Fe bal Cu 0.25 Al 0.25 Ga 0.5 Co5Ti 0.2 B 0.95 Wafer, Nd 60 Tb 20 Ga 10 Co 10 Wafer, (Nd 0.65 Pr 0.15 Dy 0.2 ) 30.5 Fe bal Al 0.15 Ga0.5 Co 10 Ti 0.3 B 0.92 Wafer, Nd 50 Tb 30 Ga 10 Co 10 Disc and (Nd 0.75 Pr 0.1 Dy 0.15 ) 31 Fe bal Al 0.25 Ga 0.35 Nb 0.2 The order of B1 discs is in a layered interleaving manner (satisfying two layers of RE x Fe bal M y B z A layer of RE' is set between the discs t M 100-t The wafer was placed in a spark plasma device for spark plasma sintering, and the temperature was rapidly raised to 450°C at a heating rate of 100°C / min, kept at this temperature for 5 minutes, and a pressure of 4.5 kN was applied to complete the preparation of the high-flux alloy diffusion couple.

[0045] (4) The high-flux alloy diffusion couple was sealed with a vacuum quartz glass tube and filled with 0.05 MPa argon. According to the temperature requirements of the subsequent experiments, four groups of parallel experiments with different insulation temperatures (600, 700, 800, and 900°C) were set up to study the diffusion of the diffusion couples prepared at different insulation temperatures. The four groups of samples were annealed at 600, 700, 800, and 900°C for 14 days to obtain Nd-Fe-MB diffusion couples.

[0046] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the present invention. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the attached claims.

Claims

1. A method for high-throughput preparation of RE-Fe-MB diffusion couples, mainly comprising the following steps: 1) According to RE x Fe bal M y B z and RE' t M 100-t The composition design is used to prepare the ingots, and several RE x Fe bal M y B z Ingots and several RE' t M 100-t Ingot, of which, RE and RE' are one or more of La, Ce, Pr, Nd, Dy, Tb, M is one or more of the metal elements Co, Al, Cu, Ga, Nb, Ni, Zn, Si and Zr, 10≤x≤60, 0.5≤y≤20, 0.85≤z≤1.5, 10≤t≤90; 2) subjecting the smelted ingots to a long-term homogenization heat treatment; 3) Each ingot is cut and surface treated to obtain several RE x Fe bal M y B z Discs and several RE' t M 100-t disc, the obtained RE x Fe bal M y B z Wafer and RE' t M 100-t The discs are placed in a spark plasma device in a layered staggered stacking manner and pressurized to perform spark plasma sintering to complete the preparation of high-flux alloy diffusion couples; 4) The high-flux alloy diffusion couple is sealed in a vacuum quartz glass tube, annealed at a required temperature and for a required time, and then quenched to obtain a RE-Fe-MB diffusion couple.

2. The method for high-throughput preparation of RE-Fe-MB diffusion couples according to claim 1, characterized in that: In step (1), during the batching process, by changing RE x Fe bal M y B z or RE' t M 100-t The element type or content in the sample can be used to obtain several RE with different compositions. x Fe bal M y B z Ingot or several RE's of different compositions t M 100-t Ingot.

3. The method for high-throughput preparation of RE-Fe-MB diffusion couples according to claim 1, characterized in that: The homogenization heat treatment in step (2) is achieved by vacuum sealing, and the sealing atmosphere is required to be 0.03-0.06MPa argon atmosphere, and the insulation heat treatment time is ≥180h.

4. The method for high-throughput preparation of RE-Fe-MB diffusion couples according to claim 1, characterized in that: In step (3), each ingot is cut into a disc of Φd*h, measured in millimeters, 10≤d≤50, 1≤h≤5, where d is the diameter of the disc and h is the thickness; wherein d needs to remain consistent in ingots of different compositions.

5. The method for high-throughput preparation of RE-Fe-MB diffusion couples according to claim 1, characterized in that: In step (3), the layered staggered stacking method refers to any two adjacent layers of discs, one of which is RE x Fe bal M y B z disc, the other layer is RE' z Fe 100-z Wafers, total stacking number N ≥ 5.

6. The method for high-throughput preparation of RE-Fe-MB diffusion couples according to claim 1, characterized in that: During the spark plasma sintering process in step (3), the temperature is rapidly raised to 400-900° C. at a heating rate of 50-400° C. / min, kept at this temperature for 5-30 minutes, and a pressure of 2-10 kN is applied.

7. The method for high-throughput preparation of RE-Fe-MB diffusion couples according to claim 1, characterized in that: The heat treatment in step (4) is achieved by vacuum sealing, requiring the sealing atmosphere to be 0.03-0.06 MPa argon atmosphere, the insulation heat treatment temperature to be 500-1100° C., and the time to be 5-30 days.

Citation Information

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