High-throughput optimization method for neodymium-iron-boron magnet alloy preparation parameters
Optimizing the preparation method of neodymium iron boron magnet alloy through high throughput technology, the problems of long preparation process and high cost in traditional methods are solved, and efficient alloy formula and process parameters are achieved, which significantly shortens the research cycle.
Patent Information
- Application Number
- CN202510573016.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-06
- Publication Date
- 2025-07-18
AI Technical Summary
The traditional NdFeB magnet alloy preparation method has the problems of long preparation process and high R&D costs, which limits the development process of new materials.
High-throughput technology is adopted to mix original formula magnetic powders with different mass ratios, magnetic field orientation molding, vacuum sintering and vacuum heat treatment are carried out, and the alloy formula and process parameters are optimized in combination with magnetic performance analysis.
The research cycle has been significantly shortened, the research efficiency has been improved, and the efficient preparation and optimization of neodymium iron boron magnet alloys have been achieved.
Smart Images

Figure BDA0005387691170000111 
Figure BDA0005387691170000121
Abstract
Description
Technical Field
[0001] The present invention relates to the field of preparation of rare earth permanent magnet materials, and particularly to a high-throughput optimization method for preparation parameters of Nd-Fe-B magnet alloys, and more particularly to a high-throughput optimization method for formula and / or process conditions in the preparation of Nd-Fe-B magnet alloys. Background Art
[0002] At present, sintered Nd-Fe-B permanent magnets are widely used in various industrial and technological fields due to their high magnetic energy product and good magnetic properties.
[0003] For example, CN105513736A discloses a sintered Nd-Fe-B magnet, and the composition of the magnet is R x M y B z Fe 余量 , where R is one or more of La, Ce, Pr, Nd, Gd, Ho, Dy, the total mass fraction of R is x, M is one or more of Co, Al, Cu, Nb, Zr, Ga, the total mass fraction of M is y, x = 29 - 33 wt%, y = 0 - 2 wt%, and z = 0.9 - 1.1 wt%.
[0004] Among them, the alloy formula, as one of the important parameters in the sintered Nd-Fe-B process, is strongly related to its magnetic properties and application prospects. However, traditional preparation methods have defects such as long preparation processes and high R & D costs when optimizing alloy formulas or process parameters, which limit the process of new material R & D. Summary of the Invention
[0005] In view of the problems existing in the prior art, the purpose of the present invention is to provide a high-throughput optimization method for preparation parameters of Nd-Fe-B magnet alloys, so as to achieve efficient optimization of the formula and process of high-performance sintered Nd-Fe-B magnet alloys and cost reduction, and accelerate the process of new material R & D.
[0006] To achieve this purpose, the present invention adopts the following technical solutions:
[0007] The present invention provides a high-throughput optimization method for preparation parameters of Nd-Fe-B magnet alloys, and the high-throughput optimization method includes:
[0008] Formula screening: According to the mass ratio of M1:M2:……:M n Mix n kinds of original formula magnetic powders to obtain different basic formula magnetic powders, where n≥2; successively subject the obtained basic formula magnetic powders to magnetic field orientation forming, vacuum sintering, and vacuum heat treatment to obtain Nd-Fe-B magnet alloy samples; perform magnetic property analysis on the obtained Nd-Fe-B magnet alloy samples, and perform formula screening according to the magnetic property analysis results;
[0009] And / or, process parameter optimization: The single-formula magnetic powder is successively subjected to magnetic field orientation forming, vacuum sintering, and vacuum heat treatment to obtain a neodymium-iron-boron magnet alloy sample; the magnetic properties of the obtained neodymium-iron-boron magnet alloy sample are analyzed, and the process parameters are optimized according to the magnetic property analysis results;
[0010] The optimized parameters in the process parameter optimization include one or a combination of at least two of the magnetic field orientation forming parameters, vacuum sintering parameters, or vacuum heat treatment parameters.
[0011] The high-throughput optimization method provided by the present invention realizes the efficient screening of the formulation composition and the efficient optimization of the preparation process parameters in the preparation process of the neodymium-iron-boron magnet alloy by using high-throughput technology, can significantly shorten the research cycle, and improve the research efficiency.
[0012] As a preferred technical solution of the present invention, in the mass ratio, M n has a value range of 0 < M n < 1, and M1 + M2 +... + M n = 1.
[0013] As a preferred technical solution of the present invention, the original formulation magnetic powder includes: at least one main magnetic powder R x M y B z Fe 余量 , where R is a combination of one or at least two of La, Ce, Pr, Nd, Gd, Ho, or Dy, and M is a combination of one or at least two of Co, Al, Cu, Nb, Zr, or Ga. In terms of mass percentage, x = 29 - 33 wt%, y = 0 - 2 wt%, and z = 0.9 - 1.1 wt%.
[0014] Preferably, the original formulation magnetic powder further includes: at least one elemental powder and / or at least one alloy powder.
[0015] As a preferred technical solution of the present invention, the orientation magnetic field in the magnetic field orientation forming is 2 - 3 T.
[0016] Preferably, the density of the green body obtained by the magnetic field orientation forming is ≤ 4.1 g / cm 3 .
[0017] As a preferred technical solution of the present invention, the temperature of the vacuum sintering is 1050 - 1080 °C.
[0018] Preferably, the time of the vacuum sintering is 3 - 6 h.
[0019] As a preferred technical solution of the present invention, the vacuum heat treatment includes a first heat treatment and a second heat treatment carried out in sequence.
[0020] Preferably, the holding temperature of the first heat treatment is 880 - 920 °C.
[0021] Preferably, the holding time of the first heat treatment is 2 - 5 h.
[0022] Preferably, the holding temperature of the second heat treatment is 480 - 520 °C.
[0023] Preferably, the holding time of the second heat treatment is 2 - 5 h.
[0024] As a preferred technical solution of the present invention, the magnetic property analysis results include: remanence Br, coercivity Hc, and maximum energy product BHmax.
[0025] As a preferred technical solution of the present invention, the magnetic field orientation forming parameters include: magnetic field strength. When optimizing, a set of magnetic field strength numbers is selected for magnetic field orientation forming.
[0026] As a preferred technical solution of the present invention, the vacuum sintering parameters include: vacuum sintering temperature and / or vacuum sintering time. When optimizing, a data set of vacuum sintering temperature and / or a data set of vacuum sintering time are selected for vacuum sintering.
[0027] As a preferred technical solution of the present invention, the vacuum heat treatment parameters include: heat treatment holding temperature and / or heat treatment holding time. When optimizing, a data set of heat treatment holding temperature and / or a data set of heat treatment holding time are selected for vacuum sintering.
[0028] Compared with the prior art solutions, the present invention has the following beneficial effects:
[0029] By using high-throughput technology, the present invention can efficiently achieve the optimized preparation of sintered Nd-Fe-B alloy formulations. It can not only achieve the efficient preparation of different formulations with the same process, but also achieve the rapid optimization of the same formulation with different processes. Compared with traditional single process methods, the research cycle is significantly shortened and the research efficiency is improved. Specific Embodiments
[0030] To better illustrate the present invention and facilitate understanding of its technical solutions, the typical but non-limiting embodiments of the present invention are as follows:
[0031] Currently, when optimizing the formulations and process parameters of sintered Nd-Fe-B magnets alloys, the traditional optimization process has defects such as a small number of samples, a cumbersome and complex process, and unstable obtained samples. Based on this, the present invention provides a method for screening the formulations of sintered Nd-Fe-B magnet alloys and optimizing the process based on high-throughput technology to achieve the efficient preparation of different formulations with the same process, and at the same time, it can also achieve the rapid optimization of the same formulation with different processes, as follows:
[0032] This embodiment provides a high-throughput optimization method for the preparation parameters of a neodymium-iron-boron magnet alloy. The high-throughput optimization method includes:
[0033] Formula screening: According to the mass ratio of M1:M2:……:M n Mix n kinds of original formula magnetic powders to obtain different basic formula magnetic powders, where n≥2; successively subject the obtained basic formula magnetic powders to magnetic field orientation molding, vacuum sintering, and vacuum heat treatment to obtain neodymium-iron-boron magnet alloy samples; perform magnetic property analysis on the obtained neodymium-iron-boron magnet alloy samples, and conduct formula screening according to the magnetic property analysis results;
[0034] And / or, process parameter optimization: Subject a single formula magnetic powder to magnetic field orientation molding, vacuum sintering, and vacuum heat treatment in sequence to obtain a neodymium-iron-boron magnet alloy sample; perform magnetic property analysis on the obtained neodymium-iron-boron magnet alloy sample, and optimize the process parameters according to the magnetic property analysis results.
[0035] In the present invention, during formula screening, ensure that the process parameters are constant to avoid the influence of process parameters on formula screening. Similarly, keep the formula composition unchanged during process parameter optimization. However, if it is necessary to simultaneously perform formula screening and process parameter optimization, that is, to study the requirements of different formula compositions for process parameters, then adjustment and combination can be carried out synchronously to achieve high-throughput formula optimization and process parameter optimization.
[0036] In the present invention, the acquisition of the original formula magnetic powder can be selected through conventional preparation processes in the art, such as obtaining rare earth elements, alloy elements, etc. through rapid solidification melting, hydrogenation pulverization, and air jet milling, or directly purchasing commercially available related required products.
[0037] Among them, in the mass ratio, M n has a value range of 0<M n <1, and M1+M2+……+M n =1.
[0038] In the present invention, the particle size of the magnetic powder is specifically selected reasonably according to the actual situation. Exemplarily, such as the D50 particle size of the magnetic powder is 1-5μm. During formula screening, the particle size of the magnetic powder can also be designed to achieve the screening and optimization of the particle size and component content of the magnetic powder.
[0039] Among them, the original formula magnetic powder includes: at least one main magnetic powder R x M y B z Fe 余量, wherein R is one or a combination of at least two of La, Ce, Pr, Nd, Gd, Ho or Dy, M is one or a combination of at least two of Co, Al, Cu, Nb, Zr or Ga, and by mass percentage, x = 29 - 33 wt%, y = 0 - 2 wt%, z = 0.9 - 1.1 wt%.
[0040] Wherein, the original formula magnetic powder further comprises: at least one elemental powder and / or at least one alloy powder.
[0041] In the present invention, the elemental powder can be selected from one of R powder, B powder, Fe powder, Co powder, Al powder, Cu powder, Nb powder, Zr powder or Ga powder. When multiple elemental powders are selected, for example, it can be a mixed powder of R powder, a mixed powder of R powder and B powder, a mixed powder of B powder, Fe powder and Co powder, a mixed powder of Co powder, Al powder and Cu powder, a mixed powder of Nb powder, Zr powder and Ga powder, etc.
[0042] In the present invention, the alloy powder can be selected from one alloy powder or a mixed powder of at least 2 alloy powders among alloy powders composed of at least two elements of La, Ce, Pr, Nd, Gd, Ho, Dy, Co, Al, Cu, Nb, Zr, Ga, B or Fe. Exemplary mixed powders of alloy powders are, for example, a mixed powder of CuFe alloy powder and AlCu alloy powder, a mixed powder of CuCo alloy powder and ZrB alloy powder, etc.
[0043] Wherein, the orientation magnetic field in the magnetic field orientation forming is 2 - 3 T. For example, it can be 2 T, 2.1 T, 2.2 T, 2.3 T, 2.4 T, 2.5 T, 2.6 T, 2.7 T, 2.8 T, 2.9 T or 3 T, etc., but not limited to the listed values, and other values within this range also meet the requirements.
[0044] Wherein, the density of the green body obtained by the magnetic field orientation forming is ≤ 4.1 g / cm 3 .
[0045] Wherein, the temperature of the vacuum sintering is 1050 - 1080 °C. For example, it can be 1050 °C, 1055 °C, 1060 °C, 1065 °C, 1070 °C, 1075 °C or 1080 °C, etc., but not limited to the listed values, and other values within this range also meet the requirements.
[0046] Wherein, the time of the vacuum sintering is 3 - 6 h. For example, it can be 3 h, 3.5 h, 4 h, 4.5 h, 5 h, 5.5 h or 6 h, etc., but not limited to the listed values, and other values within this range also meet the requirements.
[0047] Wherein, the vacuum heat treatment includes a first heat treatment and a second heat treatment carried out in sequence.
[0048] Among them, the holding temperature of the first heat treatment is 880 - 920 °C. For example, it can be 880 °C, 885 °C, 890 °C, 895 °C, 900 °C, 905 °C, 910 °C, 915 °C or 920 °C, etc., but not limited to the listed values, and other values within this range also meet the requirements.
[0049] Among them, the holding time of the first heat treatment is 2 - 5 h. For example, it can be 2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h or 5 h, etc., but not limited to the listed values, and other values within this range also meet the requirements.
[0050] Among them, the holding temperature of the second heat treatment is 480 - 520 °C. For example, it can be 480 °C, 485 °C, 490 °C, 495 °C, 500 °C, 505 °C, 510 °C, 515 °C or 520 °C, etc., but not limited to the listed values, and other values within this range also meet the requirements.
[0051] Among them, the holding time of the second heat treatment is 2 - 5 h. For example, it can be 2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h or 5 h, etc., but not limited to the listed values, and other values within this range also meet the requirements.
[0052] In the present invention, the temperature uniformity in the holding cavity used in vacuum sintering and / or vacuum heat treatment is < ±5 °C.
[0053] Among them, the magnetic property analysis results include: remanence Br, coercivity Hc and maximum energy product BHmax.
[0054] Among them, the magnetic field orientation forming parameters include: magnetic field intensity. When optimizing, a set of magnetic field intensity numbers is selected for magnetic field orientation forming. For example, when selecting the magnetic field intensity data set as {2 T, 2.1 T, 2.2 T, 2.3 T, 2.4 T, 2.5 T, 2.6 T, 2.7 T, 2.8 T, 2.9 T, 3 T} or its subset for optimization tests, and the magnetic field intensity that meets the design requirements is selected through the magnetic property analysis results.
[0055] Among them, the vacuum sintering parameters include: vacuum sintering temperature and / or vacuum sintering time. When optimizing, a vacuum sintering temperature data set and / or a vacuum sintering time data set are selected for vacuum sintering. For example, when selecting the sintering temperature data set as {1050 °C, 1055 °C, 1060 °C, 1065 °C, 1070 °C, 1075 °C, 1080 °C} or its subset, and / or the sintering time data set as {3 h, 3.5 h, 4 h, 4.5 h, 5 h, 5.5 h, 6 h} or its subset for optimization tests, and the temperature and / or time that meet the design requirements are selected through the magnetic property analysis results.
[0056] Among them, the vacuum heat treatment parameters include: heat treatment holding temperature and / or heat treatment holding time. When optimizing, select the heat treatment holding temperature data set and / or heat treatment holding time data set for vacuum sintering. For example, select the first heat treatment holding temperature data set as {880 °C, 885 °C, 890 °C, 895 °C, 900 °C, 905 °C, 910 °C, 915 °C, 920 °C} or its subset, the first heat treatment holding time data set as {2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h, 5 h} or its subset, the second heat treatment holding temperature data set as {480 °C, 485 °C, 490 °C, 495 °C, 500 °C, 505 °C, 510 °C, 515 °C, 520 °C} or its subset, or the second heat treatment holding time data set as {2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h, 5 h} or its subset. Select one data set or a combination of at least 2 data sets for the optimization test, and select the temperature and / or time that meet the design requirements through the magnetic property analysis results.
[0057] Furthermore, the present embodiment provides the following high-throughput optimization device to implement the foregoing high-throughput optimization method, specifically as follows:
[0058] It includes a powder mixing unit, a forming unit, and a sintering-heat treatment unit connected in sequence.
[0059] The powder mixing unit includes: m powder mixing devices, where m = C(n, 1) + C(n, 2) + …… + C(n, k), and k ≤ n.
[0060] The sintering-heat treatment unit includes a transition zone and at least 3 heat preservation-cooling zones connected in sequence.
[0061] The heat preservation-cooling zone includes a heat preservation zone and a cooling zone connected in sequence.
[0062] Furthermore, in order to clarify the optimization stability and reliability that can be achieved by the high-throughput optimization method for preparing the parameters of the neodymium iron boron magnet alloy provided by the present invention, the following actual examples are used for exemplary illustration, specifically as follows:
[0063] Example 1
[0064] The present embodiment provides a method for screening the formula and optimizing the process of sintered neodymium iron boron magnet alloy based on high-throughput technology, and its specific steps are as follows:
[0065] Original formula A: The alloy composition is Nd 29.3 B 0.96 Co 1.2 G a0.1 Cu 0.15 Zr 0.25 Fe bal ; Original formula B: The alloy composition is Tb70 Cu 30 The two alloy components are subjected to rapid solidification melting, hydrogen pulverization, and air jet milling to obtain the corresponding original formula magnetic powders A (D50 particle size is 3.9 μm) and original formula magnetic powder B (D50 particle size is 3 μm).
[0066] Place the original formula magnetic powder A and the original formula magnetic powder B at the independent feeding ports of a fully automatic press. Through the automatic press control system, input the mass ratios of the original formula magnetic powder A and the original formula magnetic powder B as 1:0, 0.99:0.01, 0.98:0.02, 0.97:0.03, 0.96:0.04. Weigh the powders of the original formula magnetic powder A and the original formula magnetic powder B according to the input ratios through an automatic powder weighing mechanism and mix them evenly by a manipulator. The mixing time is 3 min.
[0067] The magnet powders with different mass ratios that are uniformly mixed are subjected to magnetic field orientation forming by an automatic press. The forming density is ~4.1 g / cm 3 , the orientation magnetic field is 2.5 T, to obtain green compacts I, II, III, IV, and V with different alloy component ratios.
[0068] Transfer the obtained green compacts to the vacuum sintering chamber of a continuous sintering furnace for high-vacuum sintering. The absolute vacuum degree is 4×10 -3 Pa, the sintering temperature is 1065 °C, the heating rate is 5 °C / min, the sintering holding time is 3.5 h. After sintering, transfer them to the vacuum cooling chamber for air cooling to room temperature to obtain sintered magnets.
[0069] Transfer the obtained sintered magnets to the vacuum sintering chamber of a continuous sintering furnace for high-vacuum primary heat treatment. The absolute vacuum degree is 4×10 -3 Pa, the primary heat treatment temperature is 900 °C, the heating rate is 5 °C / min, and the primary heat treatment time is 3 h. After the heat treatment, transfer them to the vacuum cooling chamber for air cooling to room temperature to obtain primary heat-treated magnets.
[0070] Transfer the primary heat-treated magnets to the sintering chamber of a continuous sintering furnace for secondary heat treatment. The absolute vacuum degree is 4×10 -3 Pa, the secondary heat treatment temperature is 500 °C, the heating rate is 5 °C / min, and the secondary heat treatment time is 3.5 h. After the heat treatment, transfer them to the vacuum cooling chamber for air cooling to room temperature to obtain the final finished magnets I, II, III, IV, and V with different composition ratios.
[0071] Perform magnetic property tests on the obtained finished magnets. After testing, the magnetic properties of the magnets are shown in Table 1.
[0072] Table 1
[0073] <![CDATA[Residual magnetism B r (kG)]]> <![CDATA[Coercivity H ci (kA / m)]]> <![CDATA[Maximum energy product (BH) max (kJ / m 3 )]]> Finished Magnet I 1.469 955.4 413.6 Finished Magnet II 1.451 1210.9 404.8 Finished Magnet III 1.432 1437.3 402.4 Finished Magnet IV 1.413 1684.2 398.7 Finished Magnet V 1.388 1812.7 379.6
[0074] Example 2
[0075] This example provides a method for screening the alloy formula of sintered Nd-Fe-B magnets and optimizing the process based on high-throughput technology. Specifically, the process parameters are optimized, and the specific steps are as follows:
[0076] The original formula: The alloy composition is Nd 29.3 B 0.96 Co 1.2 G a0.1 Cu 0.15 Zr 0.25 Fe bal ; Through rapid solidification melting, hydrogen decrepitation, and air jet milling, the corresponding original formula magnetic powder (D50 particle size is 3.9 μm) is obtained;
[0077] Place the original formula magnetic powder at the feeding port of the fully automatic press, input the mass of the original formula magnetic powder through the automatic press control system and conduct powder weighing. The weighed original formula magnetic powder is subjected to magnetic field orientation forming by the automatic press, and the forming density is ~4.1 g / cm 3 , the orientation magnetic field is 2.5 T, and a green compact with the same composition is obtained;
[0078] Transfer the obtained green compact to the vacuum sintering chamber of the continuous sintering furnace for high-vacuum sintering. The absolute vacuum degree is 4×10 -3 Pa, the sintering temperatures are 1060 °C, 1065 °C, and 1070 °C respectively, the heating rate is 5 °C / min, the sintering holding time is 3.5 h, and after sintering, it is air-cooled to room temperature to obtain a sintered magnet;
[0079] Transfer the obtained sintered magnet to the vacuum sintering chamber of the continuous sintering furnace for high-vacuum primary heat treatment. The absolute vacuum degree is 4×10 -3 Pa, the primary heat treatment temperatures are 890 °C, 900 °C, and 910 °C respectively, the heating rate is 5 °C / min, and the primary heat treatment time is 3 h; after heat treatment, it is air-cooled to room temperature to obtain a primary heat-treated magnet;
[0080] Transfer the obtained primary heat-treated magnet to the vacuum sintering chamber of the continuous sintering furnace for secondary heat treatment. The absolute vacuum degree is 4×10 -3Pa, the secondary heat treatment temperatures are 480°C, 500°C, and 520°C respectively, the heating rate is 5°C / min, and the secondary heat treatment time is 3.5 h; after the heat treatment, air cooling is carried out to room temperature to obtain finished magnets 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27;
[0081] The temperature parameters corresponding to the finished magnets are:
[0082] Finished magnet 1: 1070°C - 910°C - 520°C;
[0083] Finished magnet 2: 1070°C - 910°C - 500°C;
[0084] Finished magnet 3: 1070°C - 910°C - 480°C;
[0085] Finished magnet 4: 1070°C - 900°C - 520°C;
[0086] Finished magnet 5: 1070°C - 900°C - 500°C;
[0087] Finished magnet 6: 1070°C - 900°C - 480°C;
[0088] Finished magnet 7: 1070°C - 890°C - 520°C;
[0089] Finished magnet 8: 1070°C - 890°C - 500°C;
[0090] Finished magnet 9: 1070°C - 890°C - 480°C;
[0091] Finished magnet 10: 1065°C - 910°C - 520°C;
[0092] Finished magnet 11: 1065°C - 910°C - 500°C;
[0093] Finished magnet 12: 1065°C - 910°C - 480°C;
[0094] Finished magnet 13: 1065°C - 900°C - 520°C;
[0095] Finished magnet 14: 1065°C - 900°C - 500°C;
[0096] Finished magnet 15: 1065°C - 900°C - 480°C;
[0097] Finished magnet 16: 1065°C - 890°C - 520°C
[0098] Finished magnet 17: 1065°C - 890°C - 500°C;
[0099] Finished magnet 18: 1065°C - 890°C - 480°C
[0100] Finished magnet 19: 1060°C - 910°C - 520°C;
[0101] Finished magnet 20: 1060°C - 910°C - 500°C;
[0102] Finished magnet 21: 1060°C - 910°C - 480°C;
[0103] Finished magnet 22: 1060°C - 900°C - 520°C;
[0104] Finished magnet 23: 1060°C - 900°C - 500°C;
[0105] Finished magnet 24: 1060°C - 900°C - 480°C;
[0106] Finished magnet 25: 1060°C - 890°C - 520°C;
[0107] Finished magnet 26: 1060°C - 890°C - 500°C;
[0108] Finished magnet 27: 1060°C - 890°C - 480°C.
[0109] The obtained finished magnets were subjected to magnetic tests. The magnetic properties of the magnets are shown in Table 2.
[0110] Table 2
[0111]
[0112]
[0113] From the results of the above embodiments, it can be seen that the high-throughput optimization method provided by the present invention realizes the efficient screening of the formulation composition and the efficient optimization of the preparation process parameters in the preparation process of neodymium-iron-boron magnet alloys by using high-throughput technology, which can significantly shorten the research cycle and improve the research efficiency.
[0114] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, and these simple modifications all fall within the protection scope of the present invention.
[0115] In addition, it should be noted that, in the above specific embodiments, the various specific technical features described can be combined in any appropriate manner without contradiction. To avoid unnecessary repetition, the present invention will not separately describe various possible combination manners.
[0116] Furthermore, any combination can be made among various different embodiments of the present invention as long as it does not violate the idea of the present invention, and it should also be regarded as the content disclosed by the present invention.
Claims
1. A high-throughput optimization method for preparation parameters of a neodymium-iron-boron magnet alloy, characterized in that The high-throughput optimization method includes: Formula screening: According to the mass ratio of M1:M2:……:M n Mix n kinds of original formula magnetic powders to obtain different basic formula magnetic powders, where n≥2; successively subject the obtained basic formula magnetic powders to magnetic field orientation forming, vacuum sintering and vacuum heat treatment to obtain NdFeB magnet alloy samples; conduct magnetic property analysis on the obtained NdFeB magnet alloy samples, and conduct formula screening according to the magnetic property analysis results; And / or, process parameter optimization: subjecting a single-formula magnetic powder to magnetic field orientation forming, vacuum sintering, and vacuum heat treatment in sequence to obtain a neodymium iron boron magnet alloy sample; performing magnetic property analysis on the obtained neodymium iron boron magnet alloy sample, and optimizing process parameters according to the magnetic property analysis results. The parameters optimized in the process parameter optimization include one or a combination of at least two of the magnetic field orientation forming parameters, vacuum sintering parameters, or vacuum heat treatment parameters.
2. The high-throughput optimization method according to claim 1, wherein, In the mass ratio, M n has a value range of 0 < M n < 1, and M1 + M2 + …… + M n = 1.
3. The high-throughput optimization method according to claim 1 or 2, characterized in that, The original formulated magnetic powder includes: at least one main magnetic powder R x M y B z Fe 余量 , where R is a combination of one or at least two of La, Ce, Pr, Nd, Gd, Ho or Dy, M is a combination of one or at least two of Co, Al, Cu, Nb, Zr or Ga, and in terms of mass percentage, x = 29 - 33 wt%, y = 0 - 2 wt%, z = 0.9 - 1.1 wt%; Preferably, the original formula magnetic powder further includes: at least one elemental powder and / or at least one alloy powder.
4. The high-throughput optimization method according to any one of claims 1-3, characterized in that In the magnetic field orientation forming, the orientation magnetic field is 2-3T. Preferably, the density of the green body obtained by magnetic field orientation forming is ≤ 4.1 g / cm 3 .
5. The high-throughput optimization method according to any one of claims 1-4, characterized in that The temperature of the vacuum sintering is 1050-1080°C. Preferably, the time of the vacuum sintering is 3-6h.
6. The high-throughput optimization method according to any one of claims 1-5, characterized in that, The vacuum heat treatment includes a first heat treatment and a second heat treatment performed in sequence. Preferably, the holding temperature of the first heat treatment is 880-920°C. Preferably, the holding time of the first heat treatment is 2-5h. Preferably, the holding temperature of the second heat treatment is 480-520°C. Preferably, the holding time of the second heat treatment is 2-5h.
7. The high-throughput optimization method according to any one of claims 1-6, characterized in that, The magnetic property analysis results include: remanence Br, coercivity Hc, and maximum energy product BHmax.
8. The high-throughput optimization method according to any one of claims 1-7, characterized in that The magnetic field orientation forming parameters include: magnetic field strength. When optimizing, a magnetic field strength data set is selected for magnetic field orientation forming.
9. The high-throughput optimization method according to any one of claims 1-8, characterized in that, The vacuum sintering parameters include: vacuum sintering temperature and / or vacuum sintering time. When optimizing, a vacuum sintering temperature data set and / or a vacuum sintering time data set are selected for vacuum sintering.
10. The high-throughput optimization method according to any one of claims 1-9, characterized in that, The vacuum heat treatment parameters include: heat treatment holding temperature and / or heat treatment holding time. When optimizing, a heat treatment holding temperature data set and / or a heat treatment holding time data set are selected for vacuum sintering.
Citation Information
Patent Citations
Sintered neodymium-iron-boron magnet
CN105513736A