CN105384434B - A kind of manufacture method of dry-pressing permanent-magnet ferrite - Google Patents
A kind of manufacture method of dry-pressing permanent-magnet ferrite Download PDFInfo
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Abstract
The invention discloses a kind of manufacture method of dry-pressing permanent-magnet ferrite.Its concrete operation step is as follows：Preburning material is chosen, by ball milling after some required additives of quality proportioning addition；Untill slurry after ball milling is stored in into drying；Magnetic drying after add 0~0.6% calcium stearate, 0.8~1.2% alcohol camphor solution, 0~0.4% talcum powder, it is to be mixed stir after broken up with high speed dispersor；By magnetic in 60~90 DEG C of tempering；It is molded in more than 8000Oe magnetic fields, obtains high 1.2~2cm formed body；First by base substrate 350~400 DEG C be incubated 1~3 hour, after 1150~1350 DEG C be incubated 0.1~3 hour；Grinding, clean, detection.The beneficial effects of the invention are as follows：On the one hand carry out process modification increase lonneal technique and cause magnetic particle diameter topography optimization, be advantageous to improve the degree of orientation and then improve magnetic property；On the other hand by the improvement of additive in prilling, be advantageous to compressing and then improve yield rate.
Description
Technical field
The present invention relates to magnetic material correlative technology field, refers in particular to a kind of manufacture method of dry-pressing permanent-magnet ferrite.
Background technology
M type permanent-magnet ferrites are a kind of oxides with ferrimagnetism, have good magnetic property, and cost performance protrudes,
It is widely used in the fields such as an electric notor, sensor, office equipment, automobile motor, Medical Devices.M type permanent-magnet ferrite molecules
Formula can be expressed as AFe12O19, in the industrial production, magnetic oriented moulding has wet method and dry method.Compared with wet method pressing under magnetic field,
Drymagnetic shaping has the advantages that efficiency high, shrinkage factor be small, product size is easily controlled；High-performance drymagnetic shaping permanent magnetism
Ferrite sintered body be mainly used to make it is various be generally difficult to using the Wet-pressing molding of routine come such as size that produces it is smaller,
Thin, complex-shaped and various extremely radial oriented magnetic devices.These magnetic devices are widely used in water pump, automobile and micro- spy
On motor.
Compared with wet moulding, dry pressing, which prepares permanent-magnet ferrite, also obvious inferior position, because not being situated between particle
Matter, which relaxes, causes that the drymagnetic shaping degree of orientation is not high and blank easily ftractures after high temperature sintering, because above reason causes
The popularization that dry pressing prepares permanent-magnet ferrite is subject to certain restrictions.Domestic most manufacturers are general when preparing dry-pressing magnet at present
The additive such as binding agent and lubricant is all added to improve magnetic property and ratio of briquetting, common binding agent have sodium chloroacetate, paraffin,
Camphor, polyvinyl alcohol, polysaccharide, polypropylene lipid etc., lubricant have stearic acid, and industrial production typically uses camphor alcohol molten
Liquid coordinates calcium stearate to use.
The content of the invention
The present invention is above-mentioned in order to overcome the shortcomings of to exist in the prior art, there is provided one kind improves magnetic property and yield rate
Dry-pressing permanent-magnet ferrite manufacture method.
To achieve these goals, the present invention uses following technical scheme：
A kind of manufacture method of dry-pressing permanent-magnet ferrite, concrete operation step are as follows：
(1) ball milling：Preburning material is chosen, by ball milling after some required additives of quality proportioning addition；
(2) dry：Untill slurry after ball milling is stored in into drying；
(3) it is granulated：Magnetic drying after add 0~0.6% calcium stearate, 0.8~1.2% alcohol camphor solution, 0~
0.4% talcum powder, it is to be mixed stir after broken up with high speed dispersor；
(4) lonneal：By magnetic in 60~90 DEG C of tempering；
(5) it is molded：It is molded in more than 8000Oe magnetic fields, obtains high 1.2~2cm formed body；
(6) sinter：First by base substrate 350~400 DEG C be incubated 1~3 hour, after 1150~1350 DEG C be incubated 0.1~3
Hour；
(7) post-process：Grinding, clean, detection.
The present inventor, which studies, finds that the reason for magnetic powder particle surface has stress and air gap after high speed is scattered causes magnetic
Powder fills uneven influence orientation in mold cavity, and blank has bright crackle or dark cracks influence yield rate after shaping.
One aspect of the present invention carries out process modification increase lonneal technique and causes magnetic particle diameter topography optimization, is advantageous to improve the degree of orientation
And then improve magnetic property；On the other hand by the improvement of additive in prilling, be advantageous to compressing and then improve finished product
Rate.
Preferably, in step (1), Ball-milling Time is 5~20 hours, and rotating speed is 30~70r/min, obtains particle
Average-size is 1.0~1.5 μm.Change magnetic powder particle pattern by controlling rotational speed of ball-mill so that magnetic is easy to magnetic field orientating.
Preferably, in step (2), untill slurry is stored in drying at 110~150 DEG C.
Preferably, in step (4), tempering time is 0.5~1.5 hour.In order to remove calcium stearate.
Preferably, in step (5), typed pressure is 3~10MPa.Solve the problems, such as dry-pressing magnet crackle, improve magnetic
The yield rate of body.
Preferably, in step (7), after grinding and cleaning, magnet is incubated 24 hours at 23 DEG C.Improve magnet
Magnetic property, while the precision of detection can be ensured.
The beneficial effects of the invention are as follows：On the one hand carry out process modification increase lonneal technique and cause magnetic particle diameter pattern
Optimization, be advantageous to improve the degree of orientation and then improve magnetic property；On the other hand by the improvement of additive in prilling, be advantageous to
Compressing and then raising yield rate.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1：
Y38 Preburning materials on the market are chosen, carry out ball milling by some required additives of quality proportioning addition, the time is 15 small
When, rotating speed 30r/min.Untill the slurry that above-mentioned steps obtain is stored in into drying at 110 DEG C, the average-size of particle is
1.2 μm or so.0.4% calcium stearate is added after magnetic is dried, 1.2% alcohol camphor solution (camphor: alcohol=1: 1), is treated
Broken up after well mixed with high speed disintegrator.Magnetic is put into mould in 8000Oe magnetic fields to be molded, briquetting pressure 4MPa, obtained
To a diameter of 5cm of formed body, high 1.6cm.Base substrate is incubated 3 hours to remove calcium stearate at 350 DEG C, then 1150
DEG C insulation 3 hours, obtain ferrite sintered magnet.After grinding and cleaning, magnet is incubated 24 hours at 23 DEG C, then measured
Magnetic property obtains Br=4061Gs, Hcb=3221Oe, Hcj=3567Oe, (BH) max=4.05MGoe.
Comparative example 1：
Y38 Preburning materials on the market are chosen, carry out ball milling by some required additives of quality proportioning addition, the time is 15 small
When, rotating speed 70r/min.Untill the slurry that above-mentioned steps obtain is stored in into drying at 110 DEG C, the average-size of particle is
1.1 μm or so.0.4% calcium stearate, 1.2% alcohol camphor solution are added after magnetic is dried, it is to be mixed uniformly rear with a high speed
Pulverizer is broken up.Magnetic is put into mould in 8000Oe magnetic fields to be molded, briquetting pressure 4MPa, obtains a diameter of of formed body
5cm, high 1.6cm.Base substrate is incubated 3 hours to remove calcium stearate at 350 DEG C, then 3 hours is incubated at 1150 DEG C, obtains
Ferrite sintered magnet.After grinding cleaning, magnet is incubated 24 hours at 23 DEG C, magnetic property is then measured and obtains Br=
3923Gs, Hcb=3350Oe, Hcj=3836Oe, (BH) max=3.85MGoe.
The magnetic property of the embodiment 1 of table 1 and the magnet of comparative example 1
Table 1 is the magnetic property of embodiment 1 and the gained magnet of comparative example 1.As shown in Table 1, rotational speed of ball-mill is that 30r/min is made
Standby magnet remanent magnetism is higher than the magnet that rotating speed is prepared by 70r/min.By observing magnetic powder particle pattern, when rotating speed is
Magnetic powder particle pattern obtained by 30r/min is intended to spherical, and the magnetic powder particle pattern obtained by rotating speed is 70r/min is piece
Shape, and size distribution is uneven.Magnetic is spherical in shape in dry-pressing magnetic field is easier to magnetic field orientating, and the mobility of magnetic is more preferable, fills out
Fill density evenly.
Embodiment 2：
Y38 Preburning materials on the market are chosen, carry out ball milling by some required additives of quality proportioning addition, the time is 12 small
When, rotating speed 50r/min.Untill the slurry that above-mentioned steps obtain is stored in into drying at 110 DEG C, the average-size of particle is
1.2 μm or so.0.5% calcium stearate, 1.0% alcohol camphor solution, 0.2% talcum powder are added after magnetic is dried, it is to be mixed
Broken up after uniformly with high speed disintegrator.Magnetic is put into mould in 8000Oe magnetic fields to be molded, briquetting pressure 5MPa, obtained into
A diameter of 5cm of body, high 1.5cm.Base substrate is incubated 1 hour to remove calcium stearate at 400 DEG C, then in 1350 DEG C of guarantors
Temperature 0.1 hour, obtains ferrite sintered magnet.After grinding and cleaning, magnet is incubated 24 hours at 23 DEG C, then measures magnetic
Performance obtains Br=4103Gs, Hcb=3245Oe, Hcj=3612Oe, (BH) max=4.09MGoe.
Comparative example 2：
Y38 Preburning materials on the market are chosen, carry out ball milling by some required additives of quality proportioning addition, the time is 12 small
When, rotating speed 50r/min.Untill the slurry that above-mentioned steps obtain is stored in into drying at 110 DEG C, the average-size of particle is
1.2 μm or so.0.5% calcium stearate, 1.0% alcohol camphor solution are added after magnetic is dried, it is to be mixed uniformly rear with a high speed
Pulverizer is broken up.Magnetic is put into mould in 8000Oe magnetic fields to be molded, briquetting pressure 5MPa, obtains a diameter of of formed body
5cm, high 1.5cm.Base substrate is incubated 1 hour to remove calcium stearate at 400 DEG C, then 0.1 hour is incubated at 1350 DEG C, obtains
To ferrite sintered magnet.After grinding cleaning, magnet is incubated 24 hours at 23 DEG C, magnetic property is then measured and obtains Br=
4037Gs, Hcb=3210Oe, Hcj=3600Oe, (BH) max=3.95MGoe.
The magnetic property of the embodiment 2 of table 2 and the magnet of comparative example 2
Table 2 is the magnetic property of embodiment 2 and the gained magnet of comparative example 2.As shown in Table 2,0.2% talcum powder of addition contributes to
Remanent magnetism improves and shaping qualification rate improves.Talcum powder can reduce the friction between dry powder as dispersant, play the effect of buffering
Fruit contributes to magnetic field orientating and improves ratio of briquetting.
Embodiment 3：
Y38 Preburning materials on the market are chosen, carry out ball milling by some required additives of quality proportioning addition, the time is 5 small
When, rotating speed 70r/min.Untill the slurry that above-mentioned steps obtain is stored in into drying at 110 DEG C, the average-size of particle is
1.0 μm or so.0.6% calcium stearate, 1.2% alcohol camphor solution, 0.2% talcum powder are added after magnetic is dried, it is to be mixed
Broken up after uniformly with high speed disintegrator.By magnetic after 80 DEG C are tempered 1 hour, it is put into mould and is molded in 8000Oe magnetic fields, into
Type pressure is 8MPa, obtains a diameter of 5cm of formed body, high 1.3cm.Base substrate is incubated 2 hours with except destearinizing at 370 DEG C
Sour calcium, 1 hour then is incubated at 1200 DEG C, obtains ferrite sintered magnet.After grinding and cleaning, by magnet in 23 DEG C of insulations
24 hours, then measure magnetic property and obtain Br=4205Gs, Hcb=3506Oe, Hcj=4024Oe, (BH) max=
4.30MGoe。
Comparative example 3：
Y38 Preburning materials on the market are chosen, carry out ball milling by some required additives of quality proportioning addition, the time is 5 small
When, rotating speed 70r/min.Untill the slurry that above-mentioned steps obtain is stored in into drying at 110 DEG C, the average-size of particle is
1.0 μm or so.0.6% calcium stearate, 1.2% alcohol camphor solution, 0.2% talcum powder are added after magnetic is dried, it is to be mixed
Broken up after uniformly with high speed disintegrator.By magnetic：It is put into mould to be molded in 8000Oe magnetic fields, briquetting pressure 8MPa, obtains
A diameter of 5cm of formed body, high 1.3cm.Base substrate is incubated 2 hours to remove calcium stearate at 370 DEG C, then at 1200 DEG C
Insulation 1 hour, obtains ferrite sintered magnet.After grinding and cleaning, magnet is incubated 24 hours at 23 DEG C, then measures magnetic
Performance obtains Br=4112Gs, Hcb=3354Oe, Hcj=3635Oe, (BH) max=4.08MGoe.
The magnetic property of the embodiment 3 of table 3 and the magnet of comparative example 3
Table 3 is the magnetic property of embodiment 3 and the gained magnet of comparative example 3.As shown in Table 3, magnetic after granulation is subjected to low temperature
Tempering contributes to remanent magnetism to improve and be molded qualification rate raising.Due to magnetic surface after magnetic is scattered with additive mixing high speed machine
It there are gas attachment and stress be present, magnetic poor fluidity in mold cavity is caused during pressing under magnetic field, it is made
Standby green density is uneven, and inconsistent easily formation crackle is shunk during sintering.Lonneal is carried out to the magnetic
Air gap and stress can be removed therefore the mobility of magnetic can be improved, prepared dry-pressing magnet density is uniform, is molded qualification rate
It is high.
Claims (5)
1. a kind of manufacture method of dry-pressing permanent-magnet ferrite, it is characterized in that, concrete operation step is as follows：
(1) ball milling：Preburning material is chosen, by ball milling after some required additives of quality proportioning addition；
(2) dry：Untill slurry after ball milling is stored in into drying；
(3) it is granulated：0~0.6% calcium stearate, 0.8~1.2% alcohol camphor solution, 0.2~0.4% are added after magnetic drying
Talcum powder, it is to be mixed stir after broken up with high speed dispersor；
(4) lonneal：By magnetic in 60~90 DEG C of tempering；Tempering time is 0.5~1.5 hour；
(5) it is molded：It is molded in more than 8000Oe magnetic fields, obtains high 1.2~2cm formed body；
(6) sinter：Base substrate is first incubated 1~3 hour at 350~400 DEG C, after it is 0.1~3 small in 1150~1350 DEG C of insulations
When；
(7) post-process：Grinding, clean, detection.
2. a kind of manufacture method of dry-pressing permanent-magnet ferrite according to claim 1, it is characterized in that, in step (1), ball
Consume time as 5~20 hours, rotating speed is 30~70r/min, and the average-size for obtaining particle is 1.0~1.5 μm.
3. a kind of manufacture method of dry-pressing permanent-magnet ferrite according to claim 1, it is characterized in that, in step (2), material
Untill slurry is stored in drying at 110~150 DEG C.
4. a kind of manufacture method of dry-pressing permanent-magnet ferrite according to claim 1, it is characterized in that, in step (5), into
Type pressure is 3~10MPa.
5. a kind of manufacture method of dry-pressing permanent-magnet ferrite according to claim 1, it is characterized in that, in step (7), mill
After cutting and cleaning, magnet is incubated 24 hours at 23 DEG C.
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| CN106278223A (en) * | 2016-08-04 | 2017-01-04 | 安徽虹泰磁电有限公司 | Permanent-magnet ferrite dry-pressing multistage magnet ring processing technology |
| CN106866131A (en) * | 2017-02-23 | 2017-06-20 | 海安县巨力磁材有限责任公司 | A kind of preparation method of high-performance permanent-magnet ferrite |
| CN110342923A (en) * | 2019-06-17 | 2019-10-18 | 横店集团东磁股份有限公司 | A kind of dry-pressing opposite sex ferrite fines preparation method and dry-pressing opposite sex permanent-magnet ferrite improving the degree of orientation and performance |
| CN110143821A (en) * | 2019-06-24 | 2019-08-20 | 海安南京大学高新技术研究院 | The production method that adhesive is used in the molding of dry-pressing opposite sex permanent-magnet ferrite |
| CN110483071A (en) * | 2019-08-22 | 2019-11-22 | 江门江益磁材有限公司 | A kind of dry-pressing permanent-magnet ferrite and its manufacturing method |
| CN114890783A (en) * | 2022-05-13 | 2022-08-12 | 武穴东磁磁材有限公司 | Production method of permanent magnetic ferrite pre-sintered material |
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| US4440713A (en) * | 1982-09-30 | 1984-04-03 | International Business Machines Corp. | Process for making fine magnetic ferrite powder and dense ferrite blocks |
| JP3181560B2 (en) * | 1998-10-23 | 2001-07-03 | ティーディーケイ株式会社 | Ferrite oxide magnetic material |
| CN104261811B (en) * | 2014-04-15 | 2015-10-21 | 横店集团东磁股份有限公司 | A kind of high-performance permanent-magnet ferrite and manufacture method thereof |
| CN104496458A (en) * | 2014-09-22 | 2015-04-08 | 横店集团东磁股份有限公司 | Manufacturing method of dry-pressed anisotropic ferrite magnetic powder |
| CN105023686A (en) * | 2015-07-27 | 2015-11-04 | 合肥凯士新材料贸易有限公司 | High-magnetism neodymium-iron-boron bonded permanent magnet containing talc powder |
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Effective date of registration: 20190710 Address after: 435414 Shifo Temple Industrial Park, Wuxue City, Huanggang City, Hubei Province Patentee after: Wuxuedong Magnets Co., Ltd. Address before: 322118 Hengdian industrial district, Dongyang City, Jinhua, Zhejiang Patentee before: Dongci Co., Ltd. of Hengdian Group Corp. |