CN110372362A - A kind of preparation method and permanent-magnet ferrite material of permanent-magnet ferrite material - Google Patents
A kind of preparation method and permanent-magnet ferrite material of permanent-magnet ferrite material Download PDFInfo
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Abstract
The present invention relates to permanent-magnet ferrite material fields, disclose the preparation method and permanent-magnet ferrite material of a kind of permanent-magnet ferrite material.The preparation method is the following steps are included: press SrOnFe2O3, n is the calculated strontium carbonate of 5.9-6.1, iron powder quality, and adds boric acid and silica, carries out wet ball grinding and obtains slurry, dries；The slurry of drying obtains permanent ferrite prefiring material by the cylindric green compact of precompressed, sintering, and calcium gluconate vibration is added by vibrating ball-mill, obtains coarse powder, CaCO is added3, SiO2, SrCO3, glucose, boric acid, obtain mixed powder carry out fine grinding obtain fines slurry, after press Wet-pressing molding obtains magnetic cake blank, sintering obtain permanent-magnet ferrite material.Method of the invention improves fine grinding effect using the steel ball of three kinds of different sizes by secondary addition common calcium carbonate, silica, strontium carbonate, boric acid and glucose, to reduce Ball-milling Time, reduces production cost.
Description
Technical field
The present invention relates to permanent-magnet ferrite material field, be specifically related to a kind of permanent-magnet ferrite material preparation method and
Permanent-magnet ferrite material.
Background technique
Since last century the fifties find permanent-magnet ferrite, kind, production method and production technology have obtained non-
Often big development, experienced from isotropic magnet to anisotropy magnet, from barium ferrite to strontium ferrite, from dry-pressing formed
It is crossed over to important technicals such as Wet-pressing moldings.
High-performance permanent-magnet ferrite Preburning material is substantially using iron oxide red as raw material at present, and production cost is relatively
Greatly, and in ball-milling technology the steel ball of single specification or the steel ball grinding material of two kinds of specifications are substantially used, ball milling effect is poor, the time
It is long, it is at high cost.Such as the patent application of the preparation method of entitled permanent ferrite magnetic shoe for DC electric motor
CN200910095298.8 is logical by a small amount of rare earth of secondary addition common calcium carbonate, silica, aluminium oxide etc. or addition
The steel ball level-one fine grinding for crossing ∮ 6- ∮ 8mm, to complete the production of ferrimagnet；A kind of entitled permanent magnetic ferrite magnet
The patent application CN201610694955.0 of production method pass through the common calcium carbonate of secondary addition, silica, aluminium oxide
Deng by second level fine grinding technology, to complete the production of ferrimagnet.
Summary of the invention
The purpose of the invention is to overcome the shortcomings of above-mentioned background technique, a kind of system of permanent-magnet ferrite material is provided
Preparation Method and permanent-magnet ferrite material, this method with cheap iron scale after ball milling is processed into iron powder directly with strontium carbonate, add
Agent is added sufficiently to generate hexagonal ferrite prefiring material by the solid phase reaction under high temperature.Wherein ball-milling technology uses three kinds of specifications
Steel ball carry out fine grinding, more traditional ball-milling technology is guaranteeing that Ball-milling Time can decline 1- similar in slurry partial size in situation
2 two hours, so as to reduce production cost, have many advantages, such as that production cost is low, performance is high.
To achieve the object of the present invention, permanent-magnet ferrite material of the present invention preparation method the following steps are included:
(1) SrOnFe is pressed2O3, n is the calculated strontium carbonate of 5.9-6.1, iron powder quality, and adds boric acid and titanium dioxide
Silicon obtains mixed powder A；
(2) the resulting mixed powder A of step (1) is subjected to wet ball grinding and obtains slurry；
(3) the resulting slurry of step (2) is dried；
(4) it by the slurry of step (3) drying by the cylindric green compact of precompressed, then is sintered, obtains its solid phase reaction
Permanent ferrite prefiring material；
(5) by step (4) resulting permanent ferrite prefiring material, calcium gluconate vibration is added by vibrating ball-mill, is obtained
Coarse powder；
(6) CaCO is added in step (5) resulting coarse powder3, SiO2, SrCO3, glucose, boric acid, obtain mixed powder B into
Row fine grinding obtains fines slurry；
(7) by the resulting fines slurry of step (6) after press Wet-pressing molding obtains magnetic cake blank, sintering obtains permanent-magnet ferrite
Material.
Further, SrOnFe is based in the step (1)2O3Quality addition 0.1-0.3% boric acid and 0.1-
0.3% silica；Preferably, the iron powder is the iron powder that iron scale passes through that ball milling is processed into.
Further, in the step (2) mixed powder the A ∮ 4 of 5:3:2, ∮ 6, ∮ 8mm in proportion steel ball, material: ball: water
Than for 1:(1.3~1.6): (11~15) carry out wet ball grinding.
Further, the wet ball grinding time is 3.5-5 hours in the step (2), and the granularity for obtaining slurry is 0.95 μm.
Further, slurry is dried at 115~125 DEG C in the step (3).
Further, sintering is to keep the temperature 2.5~3.5 hours at 1300-1350 DEG C in the step (4).
Further, in the step (5) additional amount of calcium gluconate be permanent ferrite prefiring material quality 0.2-
0.4%.
Further, vibration 2-4 minutes in the step (5), 3.5-5.5 μm of coarse powder is obtained.
Further, the CaCO of meal quality 0.8-1.2% is added in the step (6)3, meal quality 0.1-0.3%
SiO2, the SrCO of meal quality 0.2-0.4%3, the glucose of meal quality 0.1-0.3%, meal quality 0.1-0.3%'s
Boric acid.
Further, steel ball of the mixed powder B by the ∮ 4 of 5:3:2, ∮ 6, ∮ 8mm in proportion in the step (6), material:
Ball: water is than being about 1:(1.5~1.7): (14~16) carry out fine grinding 9~13 hours, obtain 0.9 μm of fines slurry.
Preferably, the resulting fines of step (6) is starched into the press in forming magnetic field for 8000Gs in the step (7), it is wet
After molded magnetic cake blank, it is 1220-1250 DEG C of roller bed type electrical kiln single layer sintering by sintering temperature, obtains permanent-magnet ferrite
Magnet.Such single layer Fast Sintering, is easy to dumping, to obtain performance more preferably permanent-magnet ferrite material.
Compared with prior art, advantages of the present invention is mainly to pass through the common calcium carbonate of secondary addition, silica, carbon
Sour strontium, boric acid and glucose are made powder more contact steel ball in fine grinding, are improved using the steel ball of three kinds of different sizes
Fine grinding effect reduces production cost to reduce Ball-milling Time, is suitable for automobile, family with the magnetic shoe that this Preburning material produces
Electrical appliance, on the motor of the industries such as industrial automation.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.Additional aspect and advantage of the invention will be set forth in part in the description, partially will be under
Become obvious in the description in face, or practice through the invention is recognized.It is only used to explain this hair it should be appreciated that being described below
It is bright, it is not intended to limit the present invention.
Term "comprising" used herein, " comprising ", " having ", " containing " or its any other deformation, it is intended that covering
Non-exclusionism includes.For example, composition, step, method, product or device comprising listed elements are not necessarily limited to those and want
Element, but may include not expressly listed other elements or such composition, step, method, product or device it is intrinsic
Element.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range is intended to include its end
Value and all integers and score in the range.
Moreover, technical characteristic involved in each embodiment of the present invention as long as they do not conflict with each other can
To be combined with each other.
Embodiment 1
(1) SrOnFe is pressed2O3, n is 5.95 77.1 grams of calculated strontium carbonates, 500 grams of iron powder, 1.15 grams of boric acid, dioxy
1.73 grams of SiClx.
(2) by (1) resulting powder by the steel ball of the ∮ 4 of 5:3:2, ∮ 6, ∮ 8mm in proportion, material: ball: water is than about 1:
1.5:13 carries out wet ball grinding 4 hours, obtains 0.95 μm of granularity of slurry.
(3) (2) resulting slurry is dried at 120 DEG C.
(4) by (3) resulting powder by the cylindric green compact of precompressed, then 1330 DEG C of heat preservations is carried out and are sintered within 3 hours, keep it solid
Phase reaction obtains permanent ferrite prefiring material.
(5) it by (4) resulting permanent-magnet ferrite material, is added 0.3% calcium gluconate vibration 3 minutes, is obtained by vibrating ball-mill
To 4.1 μm of coarse powder.
(6) by 500 grams of (5) resulting coarse powder, 5 grams of CaCO are added3, 1 gram of SiO2, 1.5 grams of SrCO3, 1 gram of glucose, 1 gram
Boric acid, by the steel ball of the ∮ 4 of 5:3:2 in proportion, ∮ 6, ∮ 8mm, material: ball: water carries out fine grinding 11 hours than about 1:1.6:15,
0.9 μm of fines slurry is obtained,
(7) (6) resulting fines slurry in the press that forming magnetic field is 8000Gs, after Wet-pressing molding obtains magnetic cake blank, is led to
Burning junction temperature is 1240 DEG C of roller bed type electrical kiln single layer Fast Sinterings, is easy to dumping, to obtain performance more preferably permanent magnet oxygen
Body magnet.
Embodiment 2
(1) by 5.95 77.1 grams of the calculated strontium carbonate of molar ratio, 500 grams of iron powder, 1.15 grams of boric acid, silica
1.73 gram.
(2) by (1) resulting powder by the steel ball of the ∮ 4 of 5:3:2, ∮ 6, ∮ 8mm in proportion, material: ball: water is than about 1:
1.5:13 carries out wet ball grinding 4 hours, obtains 0.95 μm of granularity of slurry.
(3) (2) resulting slurry is dried at 120 DEG C.
(4) by (3) resulting powder by the cylindric green compact of precompressed, then 1330 DEG C of heat preservations is carried out and are sintered within 2.5 hours, make it
Solid phase reaction obtains permanent ferrite prefiring material.
(5) it by (4) resulting permanent-magnet ferrite material, is added 0.3% calcium gluconate vibration 3 minutes, is obtained by vibrating ball-mill
To 4.3 μm of coarse powder.
(6) by 500 grams of (5) resulting coarse powder, 4 grams of CaCO are added3, 1 gram of SiO2, 2 grams of SrCO3, 1 gram of glucose, 1 gram of boron
Acid, by the steel ball of the ∮ 4 of 5:3:2 in proportion, ∮ 6, ∮ 8mm, material: ball: water is carried out fine grinding 12 hours, is obtained than being about 1:1.6:15
It is starched to 0.88 μm of fines,
(7) (6) resulting fines slurry in the press that forming magnetic field is 8000Gs, after Wet-pressing molding obtains magnetic cake blank, is led to
Burning junction temperature is 1240 DEG C of roller bed type electrical kiln single layer Fast Sinterings, is easy to dumping, to obtain performance more preferably permanent magnet oxygen
Body magnet.
Comparative example
(1) by 5.95 77.1 grams of the calculated strontium carbonate of molar ratio, 500 grams of iron powder, 1.15 grams of boric acid, silica
1.73 gram.
(2) by (1) resulting powder by the steel ball of ∮ 6mm in proportion, material: ball: water carries out wet than being about 1:1.5:13
Method ball milling 5 hours, obtain 0.98 μm of granularity of slurry.
(3) (2) resulting slurry is dried at 120 DEG C.
(4) by (3) resulting powder by the cylindric green compact of precompressed, then 1330 DEG C of heat preservations is carried out and are sintered within 3 hours, keep it solid
Phase reaction obtains permanent ferrite prefiring material.
(5) it by (4) resulting permanent-magnet ferrite material, is added 0.3% calcium gluconate vibration 3 minutes, is obtained by vibrating ball-mill
To 4.0 μm of coarse powder.
(6) by 500 grams of (5) resulting coarse powder, 5 grams of CaCO are added3, 1 gram of SiO2, 1.5 grams of SrCO3, 1 gram of boric acid passes through ∮
The steel ball of 6mm, material: ball: water carries out fine grinding 14 hours than about 1:1.6:15, obtains 0.9 μm of fines slurry,
(7) (6) resulting fines slurry in the press that forming magnetic field is 8000Gs, after Wet-pressing molding obtains magnetic cake blank, is led to
Burning junction temperature is that 1240 DEG C of roller bed type electrical kiln single layer Fast Sinterings obtain permanent magnetic ferrite magnet.
Effect example
Permanent magnetic ferrite magnet made from the various embodiments described above is sampled by magnetic performance testing method as defined in GB/T 3217
Test, the results are shown in Table 1:
Permanent magnetic ferrite magnet the performance test results made from each embodiment of table 1
| Embodiment | Br(Gs) | Hcb(Oe) | Hcj(Oe) | (BH)max(MGOe) |
| 1 | 4293 | 3286 | 3399 | 4.439 |
| 2 | 4301 | 3315 | 3428 | 4.436 |
| 3 | 4256 | 3201 | 3283 | 4.423 |
The unit of above-mentioned test item is explained as follows:
Gs: Gauss, 1T=10kGs；Oe: oersted, 1kOe=79.6kA/m；MGOe: million is high difficult to understand, 1MGOe=
7.96kJ/m3。
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of permanent-magnet ferrite material, which is characterized in that the preparation method comprises the following steps:
(1) SrOnFe is pressed2O3, n is the calculated strontium carbonate of 5.9-6.1, iron powder quality, and adds boric acid and silica, is obtained
Mixed powder A；
(2) the resulting mixed powder A of step (1) is subjected to wet ball grinding and obtains slurry；
(3) the resulting slurry of step (2) is dried；
(4) it by the slurry of step (3) drying by the cylindric green compact of precompressed, then is sintered, its solid phase reaction is made to obtain permanent magnetism
Ferrite prefiring material；
(5) by step (4) resulting permanent ferrite prefiring material, calcium gluconate vibration is added by vibrating ball-mill, obtains coarse powder；
(6) CaCO is added in step (5) resulting coarse powder3, SiO2, SrCO3, glucose, boric acid, obtain mixed powder B carry out it is thin
Mill obtains fines slurry；
(7) by the resulting fines slurry of step (6) after press Wet-pressing molding obtains magnetic cake blank, sintering obtains permanent-magnet ferrite material
Material.
2. the preparation method of permanent-magnet ferrite material according to claim 1, which is characterized in that base in the step (1)
In SrOnFe2O3Quality addition 0.1-0.3% boric acid and 0.1-0.3% silica；Preferably, the iron powder is
Iron scale passes through the iron powder that ball milling is processed into.
3. the preparation method of permanent-magnet ferrite material according to claim 1, which is characterized in that mixed in the step (2)
Close the steel ball of powder the A ∮ 4 of 5:3:2, ∮ 6, ∮ 8mm in proportion, material: ball: water ratio is 1:(1.3~1.6): (11~15) carry out wet
Method ball milling.
4. the preparation method of permanent-magnet ferrite material according to claim 1, which is characterized in that wet in the step (2)
Method Ball-milling Time is 3.5-5 hours, and the granularity for obtaining slurry is 0.95 μm.
5. the preparation method of permanent-magnet ferrite material according to claim 1, which is characterized in that material in the step (3)
Slurry is dried at 115~125 DEG C.
6. the preparation method of permanent-magnet ferrite material according to claim 1, which is characterized in that burnt in the step (4)
Knot is to keep the temperature 2.5~3.5 hours at 1300-1350 DEG C.
7. the preparation method of permanent-magnet ferrite material according to claim 1, which is characterized in that Portugal in the step (5)
The additional amount of grape Calciofon is the 0.2-0.4% of permanent ferrite prefiring material quality；Preferably, vibration 2-4 in the step (5)
Minute, obtain 3.5-5.5 μm of coarse powder.
8. the preparation method of permanent-magnet ferrite material according to claim 1, which is characterized in that add in the step (6)
Enter the CaCO of meal quality 0.8-1.2%3, the SiO of meal quality 0.1-0.3%2, the SrCO of meal quality 0.2-0.4%3, slightly
The glucose of silty amount 0.1-0.3%, the boric acid of meal quality 0.1-0.3%.
9. the preparation method of permanent-magnet ferrite material according to claim 1, which is characterized in that mixed in the step (6)
Powder material B is closed by the steel ball of the ∮ 4 of 5:3:2, ∮ 6, ∮ 8mm in proportion, material: ball: water is than being about 1:(1.5~1.7): (14~16),
It carries out fine grinding 9~13 hours, obtains 0.9 μm of fines slurry；Preferably, the resulting fines of step (6) is starched in the step (7)
It is 1220-1250 DEG C of roller bed type by sintering temperature after Wet-pressing molding obtains magnetic cake blank in the press that forming magnetic field is 8000Gs
The sintering of electrical kiln single layer, obtains permanent magnetic ferrite magnet.
10. a kind of permanent-magnet ferrite material, which is characterized in that the permanent-magnet ferrite material is any using claim 1-9
Item the method preparation gained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910636082.1A CN110372362A (en) | 2019-07-15 | 2019-07-15 | A kind of preparation method and permanent-magnet ferrite material of permanent-magnet ferrite material |
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Cited By (7)
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| CN111099889A (en) * | 2019-12-27 | 2020-05-05 | 湖南航天磁电有限责任公司 | Method for improving magnetic property of permanent magnetic ferrite |
| CN111704452A (en) * | 2020-05-22 | 2020-09-25 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite material and preparation method thereof |
| CN112876231A (en) * | 2021-03-09 | 2021-06-01 | 中南大学 | Preparation method of permanent magnetic ferrite and permanent magnetic ferrite |
| CN114031385A (en) * | 2021-10-22 | 2022-02-11 | 浙江安特磁材股份有限公司 | Method for preparing permanent magnetic ferrite material from high-chlorine iron oxide red |
| CN115180939A (en) * | 2022-08-02 | 2022-10-14 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite magnet and preparation method thereof |
| CN115650716A (en) * | 2022-11-02 | 2023-01-31 | 安徽龙磁科技股份有限公司 | Preparation method of permanent magnetic ferrite wet-pressing magnetic shoe |
| CN115724655A (en) * | 2021-08-25 | 2023-03-03 | 横店集团东磁股份有限公司 | Method for preparing high-performance permanent magnetic ferrite material from low-purity iron oxide red |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111099889A (en) * | 2019-12-27 | 2020-05-05 | 湖南航天磁电有限责任公司 | Method for improving magnetic property of permanent magnetic ferrite |
| CN111704452A (en) * | 2020-05-22 | 2020-09-25 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite material and preparation method thereof |
| CN112876231A (en) * | 2021-03-09 | 2021-06-01 | 中南大学 | Preparation method of permanent magnetic ferrite and permanent magnetic ferrite |
| CN115724655A (en) * | 2021-08-25 | 2023-03-03 | 横店集团东磁股份有限公司 | Method for preparing high-performance permanent magnetic ferrite material from low-purity iron oxide red |
| CN114031385A (en) * | 2021-10-22 | 2022-02-11 | 浙江安特磁材股份有限公司 | Method for preparing permanent magnetic ferrite material from high-chlorine iron oxide red |
| CN115180939A (en) * | 2022-08-02 | 2022-10-14 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite magnet and preparation method thereof |
| CN115650716A (en) * | 2022-11-02 | 2023-01-31 | 安徽龙磁科技股份有限公司 | Preparation method of permanent magnetic ferrite wet-pressing magnetic shoe |
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