CN103887054B - Large scale Nd-Fe-B magnet steel preparation method - Google Patents
Large scale Nd-Fe-B magnet steel preparation method Download PDFInfo
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- CN103887054B CN103887054B CN201210554681.7A CN201210554681A CN103887054B CN 103887054 B CN103887054 B CN 103887054B CN 201210554681 A CN201210554681 A CN 201210554681A CN 103887054 B CN103887054 B CN 103887054B
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Abstract
A kind of preparation method of large scale Nd-Fe-B magnet steel, the one-level tempering temperature rise period have employed ladder-elevating temperature technique and adds 140 –, 180 DEG C of insulation platforms, strictly control programming rate, make large scale magnet steel thermally equivalent in temperature-rise period, reduce the internal stress that bulk magnet steel produced in the temperature rise period, after tempering terminates, sintering briquette is cooled to set point of temperature 50 – 70 DEG C to come out of the stove, reaches when not extending life cycle of the product, reduce large scale Nd-Fe-B magnet steel crack number when not increasing production cost, improve the object of qualification rate.
Description
Technical field
The present invention relates to a kind of preparation method of permanent magnet material, particularly relate to the preparation method improving large scale Nd-Fe-B magnet steel qualification rate.
Background technology
At present, known Nd-Fe-Bo permanent magnet material sintering tempering process, it comprises the following steps: and pressed compact enters stove → vacuumize → heat up → high temperature sintering → sintering briquette comes out of the stove → and sintering briquette enters stove → mono-second annealing → cooling and comes out of the stove.Recent years, along with the output of Nd-Fe-Bo permanent magnet material increases sharply, the application of the aspect such as wind power generation, elevator motor, ore dressing facilitates the production of large scale Nd-Fe-B magnet steel.The alloy that sintered Nd-Fe-B permanent magnetic material is is matrix with Nd2Fe14B intermetallic compound, intermetallic compound has complicated crystal structure, slide coefficient is few, tensile strength is low, when crystalline material by High-temperature cooling to low temperature time, very large internal stress can be produced between crystal, cause magnet to occur crackle and cracking, make its product because of appearance yield reduction about 20% – 30%.And existing production technology carries out the preparation of large scale Nd-Fe-B magnet steel by adjustment sintering temperature rise period technique, prolongation heating-up time on the basis of stock size product sintering process, carry out the preparation of large scale Nd-Fe-B magnet steel in this way, though conforming product rate increases but can not ensure, simultaneously because the production cycle of product is long, cause production cost too high, and affect the delivery time of order.
Summary of the invention
The object of the invention is to solve the problem that the said goods qualification rate is low and life cycle of the product is long, a kind of preparation method improving large scale Nd-Fe-B magnet steel qualification rate is provided, when not extending production cycle, the increase production cost of product, by changing mode and the tempering process curve of code material, reduce crack number, thus improve large scale Nd-Fe-B magnet steel qualification rate.
The invention provides a kind of volume and be greater than 200cm
3large scale Nd-Fe-B magnet steel preparation method, comprise following processing step:
1) will treat that the large scale Nd-Fe-B magnet steel code of tempering is expected into stove;
2) ladder-elevating temperature, keeps when in-furnace temperature is warming up to 140-180 DEG C, after 30-50 minute, continuing in-furnace temperature to be warming up to one-level temperature 940 DEG C;
3) one-level tempering complete after, by large scale Nd-Fe-B magnet steel through cooling, second annealing, be cooled to 50-70 DEG C and come out of the stove.
Wherein, described step 2) in ladder heating step be specially:
In-furnace temperature is made to be warming up to 140-180 DEG C by 50-70 DEG C in 30-60 minute;
In 30-50 minute, furnace temperature is warming up to 360-440 DEG C by 140-180 DEG C;
Be warming up to the one-level temperature 940 DEG C of NdFeB material by 360-440 DEG C in 90-110 minute.
Programming rate described in this process is per minutely be less than 10 DEG C.
Heating steps described in this process is evacuated to higher than starting heating during 0.5pa for being carried out by sintering furnace.
Wherein, the step of described step 3) is specially:
After one-level tempering completes, in-furnace temperature is cooled to 50-70 DEG C, stops cooling;
After stopping cooling, be heated to second annealing temperature 480-640 DEG C by again vacuumizing in stove higher than starting during 0.5pa;
After second annealing completes, in-furnace temperature is cooled to 50-70 DEG C and comes out of the stove.
Cooling step described in this process adopts air-cooled, water-cooled and/or oil cooling.
The present invention significantly can improve the conforming product rate of large scale Nd-Fe-B magnet steel when not extending the production cycle of product, increase production cost.
The one-level tempering temperature rise period have employed ladder-elevating temperature technique and adds 140 –, 180 DEG C of insulation platforms, strictly control programming rate, make large scale magnet steel thermally equivalent in temperature-rise period, reduce the internal stress that bulk magnet steel produced in the temperature rise period, after tempering terminates, sintering briquette is cooled to set point of temperature 50 – 70 DEG C to come out of the stove, cool too fast internal stress after avoiding that bulk magnet steel Yin Wendu is too high and coming out of the stove to increase and cause product to occur crackle and cracking, improve the qualification rate of product.
Embodiment
Below in conjunction with embodiment, the technical solution used in the present invention is further described.
Embodiment 1: arrange shaping 800 blocks of sintering briquettes to be of a size of the pressed compact of 104.5*61.5*25.9 specification, enters same stove sintering, after having sintered, sintering briquette is divided into two equal portions, is arranged in the tempering at twice of same stove.
First time uses normal process tempering, specific operation process is as follows: the product piled up is entered stove, sintering furnace is vacuumized, when vacuum degree is higher than starting heating during 0.5pa, make in-furnace temperature be warming up to one-level temperature by 70 DEG C with 90 minutes, keep 240 minutes in one-level temperature, air-cooled to 100 DEG C through 90 minutes, air-cooledly after second annealing again to come out of the stove to 70 DEG C, be called experiment 1;
Second time uses new technology tempering, and specific operation process is as follows: the product piled up is entered stove, and the first step vacuumizes sintering furnace; Second step, when vacuum degree is higher than starting heating during 0.5pa, made in-furnace temperature be warming up to 140 DEG C by 70 DEG C with 30 minutes, and keeping 30 minutes; 3rd step was warming up to 440 DEG C with 50 minutes by 140 DEG C, vacuum degree is higher than 0.5pa simultaneously, 4th step was warming up to one-level temperature with 90 ' minute by 440 DEG C, and from second step, be heated to the 4th step-up to one-level temperature, sintering furnace vacuum degree is higher than 0.5pa; Programming rate will control to be less than less than 10 DEG C per minute, and large scale Nd-Fe-B magnet steel to 70 DEG C come out of the stove (must ensure that tapping temperature reaches regulation and requires), is called experiment 2 through one-level tempering → air-cooled → intensification → second annealing → air-cooled;
Two stove sintering briquettes are through overgroundly to cut, after go-on-go, and test to outward appearance, assay sees the following form:
| Experiment numbers | Enter stove quantity (block) | Crack number (block) | Ratio (%) |
| 1 | 400 | 89 | 22.25 |
| 2 | 400 | 11 | 2.75 |
Embodiment 2: arrange shaping 800 blocks of sintering briquettes to be of a size of the pressed compact of 110*50.5*22.5 specification, enters same stove sintering, divides and sintering briquette is divided into two equal portions, be arranged in the tempering at twice of same stove after having sintered.
First time uses normal process tempering, specific operation process is as follows: the product piled up is entered stove, sintering furnace is vacuumized, when vacuum degree is higher than starting heating during 0.5pa, make in-furnace temperature be warming up to one-level temperature by 70 DEG C with 90 minutes, keep 240 minutes in one-level temperature, air-cooled to 100 DEG C through 90 minutes, air-cooledly after second annealing again to come out of the stove to 70 DEG C, be called experiment 1;
Second time uses new technology tempering, and specific operation process is as follows: the product piled up is entered stove, and the first step vacuumizes sintering furnace; Second step, when vacuum degree is higher than starting heating during 0.5pa, made in-furnace temperature be warming up to 160 DEG C by 60 DEG C with 45 minutes, and keeping 40 minutes; 3rd step was warming up to 400 DEG C with 40 minutes by 160 DEG C, vacuum degree is higher than 0.5pa simultaneously, 4th step was warming up to one-level temperature with 100 ' minute by 400 DEG C, and from second step, be heated to the 4th step-up to one-level temperature, sintering furnace vacuum degree is higher than 0.5pa; Programming rate will control to be less than less than 10 DEG C per minute, and large scale Nd-Fe-B magnet steel to 60 DEG C come out of the stove (must ensure that tapping temperature reaches regulation and requires), is called experiment 2 through one-level tempering → air-cooled → intensification → second annealing → air-cooled;
Two stove sintering briquettes are through overgroundly to cut, after go-on-go, and test to outward appearance, assay sees the following form:
| Experiment numbers | Enter stove quantity (block) | Crack number (block) | Ratio (%) |
| 1 | 400 | 92 | 23.00 |
| 2 | 400 | 9 | 2.25 |
Embodiment 3: arrange shaping 800 blocks of sintering briquettes to be of a size of the pressed compact of 119.5*69.9*21.8 specification, enters same stove sintering, divides and sintering briquette is divided into two equal portions, be arranged in the tempering at twice of same stove after having sintered.
First time uses normal process tempering, specific operation process is as follows: the product piled up is entered stove, sintering furnace is vacuumized, when vacuum degree is higher than starting heating during 0.5pa, make in-furnace temperature be warming up to one-level temperature by 70 DEG C with 90 minutes, keep 240 minutes in one-level temperature, air-cooled to 100 DEG C through 90 minutes, air-cooledly after second annealing again to come out of the stove to 70 DEG C, be called experiment 1;
Second time uses new technology tempering, and specific operation process is as follows: the product piled up is entered stove, and the first step vacuumizes sintering furnace; Second step, when vacuum degree is higher than starting heating during 0.5pa, made in-furnace temperature be warming up to 180 DEG C by 50 DEG C with 60 minutes, and keeping 50 minutes; 3rd step was warming up to 360 DEG C with 30 minutes by 180 DEG C, vacuum degree is higher than 0.5pa simultaneously, 4th step was warming up to one-level temperature with 110 ' minute by 360 DEG C, and from second step, be heated to the 4th step-up to one-level temperature, sintering furnace vacuum degree is higher than 0.5pa; Programming rate will control to be less than less than 10 DEG C per minute, and large scale Nd-Fe-B magnet steel to 50 DEG C come out of the stove (must ensure that tapping temperature reaches regulation and requires), is called experiment 2 through one-level tempering → air-cooled → intensification → second annealing → air-cooled;
Two stove sintering briquettes are through overgroundly to cut, after go-on-go, and test to outward appearance, assay sees the following form:
| Experiment numbers | Enter stove quantity (block) | Crack number (block) | Ratio (%) |
| 1 | 400 | 95 | 23.75 |
| 2 | 400 | 14 | 3.50 |
By three Experimental comparison, after adopting new technology, crackle ratio significantly reduces.
Crackle is the crack that material produces under effect of stress, and adopt the method for range estimation to detect, criterion of acceptability is product surface flawless.
Claims (5)
1. a preparation method for large scale Nd-Fe-B magnet steel, is characterized in that, comprises following processing step:
1) will treat that the large scale Nd-Fe-B magnet steel code of tempering is expected into stove;
2) ladder-elevating temperature, keeps when in-furnace temperature is warming up to 140-180 DEG C, after 30-50 minute, continuing in-furnace temperature to be warming up to one-level temperature 940 DEG C;
3) one-level tempering complete after, by large scale Nd-Fe-B magnet steel through cooling, second annealing, be cooled to 50-70 DEG C and come out of the stove;
Wherein, described step 2) in ladder heating step be specially:
A) in-furnace temperature is made to be warming up to 140-180 DEG C by 50-70 DEG C in 30-60 minute;
B) in 30-50 minute, furnace temperature is warming up to 360-440 DEG C by 140-180 DEG C;
C) the one-level temperature 940 DEG C of NdFeB material is warming up in 90-110 minute by 360-440 DEG C.
2. the preparation method of large scale Nd-Fe-B magnet steel according to claim 1, wherein, described programming rate is per minutely be less than 10 DEG C.
3. the preparation method of large scale Nd-Fe-B magnet steel according to claim 1, wherein, described step heating steps a) is evacuated to higher than starting heating during 0.5pa for being carried out by sintering furnace.
4. the preparation method of large scale Nd-Fe-B magnet steel according to claim 1, wherein, described step 3) step be specially:
I. after one-level tempering completes, in-furnace temperature is cooled to 50-70 DEG C, stops cooling;
Ii is heated to second annealing temperature 480-640 DEG C by vacuumizing in stove higher than starting during 0.5pa after stopping cooling;
Iii., after second annealing completes, in-furnace temperature is cooled to 50-70 DEG C and comes out of the stove.
5. the preparation method of large scale Nd-Fe-B magnet steel according to claim 4, wherein, described cooling step adopts air-cooled, water-cooled and/or oil cooling.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1570155A (en) * | 2004-04-29 | 2005-01-26 | 山西汇镪磁性材料制作有限公司 | Sintered Nd Iron boron permanent magnet tempering process |
| CN101364464A (en) * | 2008-06-14 | 2009-02-11 | 烟台首钢磁性材料股份有限公司 | Large-size corrosion resisting neodymium iron boron permanent magnetic material and manufacturing process thereof |
| CN101619381A (en) * | 2009-07-30 | 2010-01-06 | 浙江升华强磁材料有限公司 | Tempering method for sintering Nd-Fe-B permanent magnet |
| CN102031350A (en) * | 2010-11-02 | 2011-04-27 | 徐州金石彭源稀土材料厂 | Sintered neodymium iron boron tempering process |
| CN102211192A (en) * | 2011-06-09 | 2011-10-12 | 天津一阳磁性材料有限责任公司 | Method for preparing high-performance neodymium iron boron by using secondary recycled materials |
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| JP5209349B2 (en) * | 2008-03-13 | 2013-06-12 | インターメタリックス株式会社 | Manufacturing method of NdFeB sintered magnet |
| CN101792327A (en) * | 2010-02-09 | 2010-08-04 | 武汉理工大学 | Preparation method of alumina oxide matrix porous ceramic material |
| CN102360909B (en) * | 2011-06-16 | 2014-03-19 | 安徽大地熊新材料股份有限公司 | Preparation method for neodymium iron boron magnet |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1570155A (en) * | 2004-04-29 | 2005-01-26 | 山西汇镪磁性材料制作有限公司 | Sintered Nd Iron boron permanent magnet tempering process |
| CN101364464A (en) * | 2008-06-14 | 2009-02-11 | 烟台首钢磁性材料股份有限公司 | Large-size corrosion resisting neodymium iron boron permanent magnetic material and manufacturing process thereof |
| CN101619381A (en) * | 2009-07-30 | 2010-01-06 | 浙江升华强磁材料有限公司 | Tempering method for sintering Nd-Fe-B permanent magnet |
| CN102031350A (en) * | 2010-11-02 | 2011-04-27 | 徐州金石彭源稀土材料厂 | Sintered neodymium iron boron tempering process |
| CN102211192A (en) * | 2011-06-09 | 2011-10-12 | 天津一阳磁性材料有限责任公司 | Method for preparing high-performance neodymium iron boron by using secondary recycled materials |
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Denomination of invention: Preparation method of large-sized neodymium iron boron magnetic steel Effective date of registration: 20230717 Granted publication date: 20160330 Pledgee: China CITIC Bank Co.,Ltd. Taiyuan Branch Pledgor: SINO MAGNETICS TECHNOLOGY Co.,Ltd. Registration number: Y2023140000039 |