CN102921950B - For producing the sintering aging technique of Nd-Fe-Bo permanent magnet material - Google Patents
For producing the sintering aging technique of Nd-Fe-Bo permanent magnet material Download PDFInfo
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- CN102921950B CN102921950B CN201210390305.9A CN201210390305A CN102921950B CN 102921950 B CN102921950 B CN 102921950B CN 201210390305 A CN201210390305 A CN 201210390305A CN 102921950 B CN102921950 B CN 102921950B
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Abstract
A kind of sintering aging technique for producing Nd-Fe-Bo permanent magnet material, the steps include: that Nd-Fe-Bo permanent magnet material body in freezing of a furnace is configured such that in the mode of carrying out aging sequence cooling to cool continuously Nd-Fe-Bo permanent magnet material body with the air quantity of low wind speed, do not re-use discontinuous air-cooled, more accurate to the control of cooling velocity, reduce the thermograde in neodymium-iron-boron surface and heart portion, therefore avoid the generation occurring cracking phenomena.
Description
Technical field
The present invention relates to a kind of sintering aging technique, especially a kind of sintering aging technique for producing Nd-Fe-Bo permanent magnet material.
Background technology
Particularly at artificial satellite in the industry such as computer, communication, in the travelling-wave tubes of the aspects such as radar, circulator and upper the obtaining of micromachine, micro recorder, aeronautical instrument, electronic watch, seismic detector and some other electronic instrument apply widely, current rare earth permanent magnet application has penetrated into the aspects such as automobile, household electrical appliance, electronic instrument, NMR imaging instrument, stereo set, small and special electric machine, mobile phone, in medical, use rare earth permanent-magnetic material to carry out " acipoint magnetotheraphy ", curative effect is greatly improved, thus facilitates the rapid popularization of " acipoint magnetotheraphy ", therefore Nd-Fe-Bo permanent magnet material is the permanent-magnet material that a kind of combination property is the highest, when producing Nd-Fe-Bo permanent magnet material, need to carry out according to the process route of batching-melting-powder process-shaping-sintering-timeliness, sintering aging sequence is the important stage producing Nd-Fe-Bo permanent magnet material, existing for producing in the sintering aging technique of Nd-Fe-Bo permanent magnet material, all when carrying out timeliness after sintering, adopt chilling or inflate self cooling or be interrupted air-cooled mode Nd-Fe-Bo permanent magnet material body is cooled, air-cooled owing to have employed interruption, control the air-cooled accuracy of interruption not high, thus cause Nd-Fe-Bo permanent magnet material body to occur that cracking phenomena occurs, Fig. 1 is that existing routine is around the first artwork of knot timeliness, Fig. 2 is that existing routine is around knot timeliness the second artwork, Fig. 3 is that existing routine is around the third artwork of knot timeliness.
Summary of the invention
In order to overcome above-mentioned technical disadvantages, the object of this invention is to provide a kind of method of the sintering aging technique for producing iron B permanent magnetic material, therefore avoiding the generation occurring cracking phenomena.
For achieving the above object, the technical scheme that the present invention takes is: the steps include: that Nd-Fe-Bo permanent magnet material body in freezing of a furnace is configured such that in the mode of carrying out aging sequence cooling and to cool continuously Nd-Fe-Bo permanent magnet material body with the air quantity of low wind speed.
Owing to designing the cooling of air-cooled continuity, do not re-use discontinuous air-cooled, more accurate to distinguished and admirable control, maintain the identical speed of cooling of Nd-Fe-Bo permanent magnet material body, therefore avoid the generation occurring cracking phenomena.
The present invention devises, and the steps include:
The steps include:
1, Nd-Fe-Bo permanent magnet material body is placed in freezing of a furnace, use vavuum pump, the vacuum around freezing of a furnace is made to be 0.01-0.001Pa, according to the mode of heating of 5-8 DEG C/min, make the temperature around freezing of a furnace reach 1040-1100 DEG C, keep 3-5h, then make Nd-Fe-Bo permanent magnet material body vacuum be 0.01-0.001Pa in freezing of a furnace, naturally cooling to temperature T1 is 150-500 DEG C, namely carries out sintering circuit.
2, opposing connection freezing of a furnace is heated to 850-950 DEG C again, keep 1-4h, then opposing connection freezing of a furnace is heated to, and opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T2 to be 100-300 DEG C, is the first aging sequence.
3, opposing connection freezing of a furnace is heated to 450-650 DEG C again, keeps 2-5h, and opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T3 to be 25-150 DEG C, is the second aging sequence.
The present invention devises,
The steps include:
1, the Nd-Fe-Bo permanent magnet material pressed compact body being 120mm ╳ 100mm ╳ 50mm specification is placed in freezing of a furnace, use vavuum pump, the vacuum around freezing of a furnace is made to be 0.005Pa, according to the mode of heating of 5 DEG C/min, make the temperature around freezing of a furnace reach 1090 DEG C, keep 4h, then make Nd-Fe-Bo permanent magnet material body vacuum be 0.005Pa in freezing of a furnace, naturally cooling to temperature T1 is 350 DEG C, namely carries out sintering circuit;
2, opposing connection freezing of a furnace is heated to 880 DEG C again, keeps 3h, is the power that the frequency control blower fan power of fan of 25KW is adjusted to 1/3 of normal value by peak power, and opposing connection freezing of a furnace keeps low speed air-cooled continuously, is cooled to temperature T2 to be 150 DEG C, is the first aging sequence;
3, opposing connection freezing of a furnace is heated to 490 DEG C again, keeps 4h, is the power that the frequency control blower fan power of fan of 25KW is adjusted to 1/3 of normal value by peak power, and opposing connection freezing of a furnace keeps low speed air-cooled continuously, is cooled to temperature T3 to be 100 DEG C, is the second aging sequence.
Technique effect of the present invention is: compare with existing process for cooling, the product implemented after the air-cooled technique of speed governing has greatly improved in magnetic property uniformity, and the implosion tendency of product obviously reduces, sintering time also significantly shortens, simultaneously, because squareness and coercitive improvement significantly can also reduce formulation cost, remarkable in economical benefits, substantially reach former imagination requirement.Solve and reduce high trade mark product fragility, in elimination, large gauge product is hidden splits and the technical barrier of three puzzlement Nd-Fe-Bo permanent magnet material bodies such as large gauge product magnetic property uniformity in improving, while improving product quality, reduce formulation cost, reduce supplementary product onsumption, shorten the production cycle, improve yield rate.
Accompanying drawing explanation
Fig. 1 is existing routine around the first artwork of knot timeliness:
Fig. 2 is existing routine around knot timeliness the second artwork:
Fig. 3 is existing routine around the third artwork of knot timeliness:
Fig. 4 is of the present invention around knot aging technique figure.
Detailed description of the invention
Below in conjunction with embodiment, further describe the present invention, following examples are intended to the present invention instead of limitation of the invention further are described.First embodiment of the present invention.
The steps include:
1, Nd-Fe-Bo permanent magnet material body is placed in freezing of a furnace, use vavuum pump, the vacuum around freezing of a furnace is made to be 0.001Pa, according to the mode of heating of 5 DEG C/min, make the temperature around freezing of a furnace reach 1040 DEG C, keep 3h, then make Nd-Fe-Bo permanent magnet material body vacuum be 0.001Pa in freezing of a furnace, naturally cooling to temperature T1 is 150 DEG C, namely carries out sintering circuit.
2, opposing connection freezing of a furnace is heated to 850 DEG C again, keep 1h, then opposing connection freezing of a furnace is heated to, and opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T2 to be 100 DEG C, is the first aging sequence.
(3), again opposing connection freezing of a furnace be heated to 450 DEG C, keep 2h, opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T3 to be 25 DEG C, is the second aging sequence.
In the present embodiment, using frequency control blower fan to be connected with the air-cooled port around freezing of a furnace, by setting the parameter of frequency control blower fan, ensureing around freezing of a furnace distinguished and admirable continuously, thus achieve opposing connection freezing of a furnace and carry out the air-cooled technological means of continuity.
Be the Nd-Fe-Bo permanent magnet material body of 1.1Kg to weight, sinter timeliness respectively according to process route in the technical scheme of Fig. 1, Fig. 2, Fig. 3 and the present embodiment, obtain different Nd-Fe-Bo permanent magnet material bodies, its performance indications are as figure below.
In this form, technique one refers to and sinters timeliness respectively according to existing routine process route in the technical scheme of knot timeliness the first artwork, obtain different Nd-Fe-Bo permanent magnet material bodies, technique two refers to and sinters timeliness respectively according to existing routine process route in the technical scheme of knot timeliness the second artwork, obtain different Nd-Fe-Bo permanent magnet material bodies, and technique three refers to and sinters timeliness respectively according to existing routine process route in the technical scheme of the third artwork of knot timeliness, obtain different Nd-Fe-Bo permanent magnet material bodies.
Second embodiment of the present invention.
The steps include:
1, Nd-Fe-Bo permanent magnet material body is placed in freezing of a furnace, use vavuum pump, the vacuum around freezing of a furnace is made to be 0.01Pa, according to the mode of heating of 8 DEG C/min, make the temperature around freezing of a furnace reach 1100 DEG C, keep 5h, then make Nd-Fe-Bo permanent magnet material body vacuum be 0.01Pa in freezing of a furnace, naturally cooling to temperature T1 is 500 DEG C, namely carries out sintering circuit.
2, opposing connection freezing of a furnace is heated to 950 DEG C again, keep 4h, then opposing connection freezing of a furnace is heated to, and opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T2 to be 300 DEG C, is the first aging sequence.
(3), again opposing connection freezing of a furnace be heated to 650 DEG C, keep 5h, opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T3 to be 150 DEG C, is the second aging sequence.
3rd embodiment of the present invention.
The steps include:
1, Nd-Fe-Bo permanent magnet material body is placed in freezing of a furnace, use vavuum pump, the vacuum around freezing of a furnace is made to be 0.006Pa, according to the mode of heating of 6.5 DEG C/min, make the temperature around freezing of a furnace reach 1070 DEG C, keep 4h, then make Nd-Fe-Bo permanent magnet material body vacuum be 0.006Pa in freezing of a furnace, naturally cooling to temperature T1 is 300 DEG C, namely carries out sintering circuit.
2, opposing connection freezing of a furnace is heated to 900 DEG C again, keep 2.5h, then opposing connection freezing of a furnace is heated to, and opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T2 to be 200 DEG C, is the first aging sequence.
(3), again opposing connection freezing of a furnace be heated to 550 DEG C, keep 3.5h, opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T3 to be 80 DEG C, is the second aging sequence.
4th embodiment of the present invention.
The steps include:
1, Nd-Fe-Bo permanent magnet material body is placed in freezing of a furnace, use vavuum pump, the vacuum around freezing of a furnace is made to be 0.008-0.004Pa, according to the mode of heating of 4-6 DEG C/min, make the temperature around freezing of a furnace reach 1080-1000 DEG C, keep 3.5-4.5h, then make Nd-Fe-Bo permanent magnet material body vacuum be 0.008-0.004Pa in freezing of a furnace, naturally cooling to temperature T1 is 180-200 DEG C, namely carries out sintering circuit.
2, opposing connection freezing of a furnace is heated to 880-920 DEG C again, keep 1-4h, then opposing connection freezing of a furnace is heated to, and opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T2 to be 150-220 DEG C, is the first aging sequence.
(3), again opposing connection freezing of a furnace be heated to 490-550 DEG C, keep 3.5-4h, opposing connection freezing of a furnace uses frequency control blower fan to keep low wind speed continuous coo1ing, is cooled to temperature T3 to be 80-100 DEG C, is the second aging sequence.
5th embodiment of the present invention, the steps include:
1, the Nd-Fe-Bo permanent magnet material pressed compact body being 120mm ╳ 100mm ╳ 50mm specification is placed in freezing of a furnace, use vavuum pump, the vacuum around freezing of a furnace is made to be 0.005Pa, according to the mode of heating of 5 DEG C/min, make the temperature around freezing of a furnace reach 1090 DEG C, keep 4h, then make Nd-Fe-Bo permanent magnet material body vacuum be 0.005Pa in freezing of a furnace, naturally cooling to temperature T1 is 350 DEG C, namely carries out sintering circuit.
2, opposing connection freezing of a furnace is heated to 880 DEG C again, keeps 3h, and opposing connection freezing of a furnace keeps low speed continuous coo1ing, is adjusted to the power of 1/3 of normal value, is cooled to temperature T2 to be 150 DEG C, is the first aging sequence by the peak power frequency control blower fan power of fan that is 25KW.
3, opposing connection freezing of a furnace is heated to 490 DEG C again, keep 4h, opposing connection freezing of a furnace keeps low speed continuous coo1ing, is adjusted to the power of 1/3 of normal value by the peak power frequency control blower fan power of fan that is 25KW, be cooled to temperature T3 to be 100 DEG C, be the second aging sequence.
The present invention has lower feature:
1, owing to designing the cooling of air-cooled continuity, do not re-use discontinuous air-cooled, more accurate to distinguished and admirable control, maintain the identical speed of cooling of Nd-Fe-Bo permanent magnet material body, therefore avoid the generation occurring cracking phenomena.
2, owing to devising frequency control blower fan, parameters is easy to operate, and control accuracy is high.
Above-described embodiment is a kind of way of realization of the method for the sintering aging technique for producing iron B permanent magnetic material provided by the present invention; according to other distortion of scheme provided by the present invention; the composition increased or reduce wherein or step; or the present invention is used for other the technical field close with the present invention, all belongs to protection scope of the present invention.
Claims (1)
1. one kind for producing the sintering aging technique of Nd-Fe-Bo permanent magnet material; It is characterized in that: the steps include: that Nd-Fe-Bo permanent magnet material body in freezing of a furnace is configured such that in the mode of carrying out aging sequence cooling and with the air quantity of low wind speed, Nd-Fe-Bo permanent magnet material body to be cooled continuously;
(1) the Nd-Fe-Bo permanent magnet material pressed compact body being, 120mm ╳ 100mm ╳ 50mm specification is placed in freezing of a furnace, use vavuum pump, the vacuum around freezing of a furnace is made to be 0.005Pa, according to the mode of heating of 5 DEG C/min, make the temperature around freezing of a furnace reach 1090 DEG C, keep 4h, then make Nd-Fe-Bo permanent magnet material body vacuum be 0.005Pa in freezing of a furnace, naturally cooling to temperature T1 is 350 DEG C, namely carries out sintering circuit;
(2), opposing connection freezing of a furnace is heated to 880 DEG C again, keeping 3h, is the power that the frequency control blower fan power of fan of 25KW is adjusted to 1/3 of normal value by peak power, and opposing connection freezing of a furnace keeps low speed air-cooled continuously, be cooled to temperature T2 to be 150 DEG C, be the first aging sequence;
(3), opposing connection freezing of a furnace is heated to 490 DEG C again, keeping 4h, is the power that the frequency control blower fan power of fan of 25KW is adjusted to 1/3 of normal value by peak power, and opposing connection freezing of a furnace keeps low speed air-cooled continuously, be cooled to temperature T3 to be 100 DEG C, be the second aging sequence.
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| CN103962555B (en) * | 2014-04-04 | 2017-02-15 | 江苏金石稀土有限公司 | Method for sintering cylindrical or annular sintered NdFeB with height ≤ 30 mm |
| CN104576020A (en) * | 2014-11-26 | 2015-04-29 | 宁波宏垒磁业有限公司 | NdFeB magnet sintering method |
| CN108242306A (en) * | 2017-12-12 | 2018-07-03 | 浙江东阳东磁稀土有限公司 | A kind of novel sintered cooling technique of Sintered NdFeB magnet |
| CN110106334B (en) * | 2018-02-01 | 2021-06-22 | 福建省长汀金龙稀土有限公司 | Device and method for continuously performing grain boundary diffusion and heat treatment |
| CN108907203A (en) * | 2018-05-21 | 2018-11-30 | 中国计量大学 | A kind of heat treatment method improving neodymium iron boron blank intrinsic coercivity consistency |
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Effective date of registration: 20160622 Address after: 311 No. three industrial road, Feicheng hi tech Industrial Development Zone, Shandong 271600, China Patentee after: The aluminum Shandong Yinuowei strong magnetic material limited company Address before: 271602 No. three industrial road, hi tech Development Zone, Tai'an, Shandong, Feicheng 311 Patentee before: Shandong Yinuowei Strong Magnet Material Co., Ltd. |
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Address after: 271600 No. three industrial road, hi tech Development Zone, Tai'an, Shandong, Feicheng 311 Patentee after: Sinochem (Shandong) magnetic materials Co., Ltd Address before: 311 No. three industrial road, Feicheng hi tech Industrial Development Zone, Shandong 271600, China Patentee before: CHINALCO SHANDONG INOVE STRONG MAGNET MARTERIAL Co.,Ltd. |