CN1988066A - High performance permanent magnetic ferrite magnetic powder and its preparing method - Google Patents
High performance permanent magnetic ferrite magnetic powder and its preparing method Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000006247 magnetic powder Substances 0.000 title claims description 24
- 230000005291 magnetic effect Effects 0.000 claims abstract description 35
- 239000000126 substance Substances 0.000 claims abstract description 20
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 229910052788 barium Inorganic materials 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 30
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 17
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 16
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- 230000001902 propagating effect Effects 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229960004643 cupric oxide Drugs 0.000 claims description 8
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 8
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 3
- 206010013786 Dry skin Diseases 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 15
- 238000002360 preparation method Methods 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 2
- 230000005389 magnetism Effects 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000000137 annealing Methods 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 3
- 208000035126 Facies Diseases 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 150000003437 strontium Chemical class 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Hard Magnetic Materials (AREA)
Abstract
This invention relates to a high performance magnet ferrite powder and a method of preparation, in which, the chemical composition of the powder is Al-xLaxFe12-yCuyO19, and A is Sr or Ba or their combination of any proportions, x is 0.05-0.4, y is 0.05-0.4. This invention does not apply rare strategic metal Co but cheap La-Cu joint dopent to control the chemical components of ferrite to get the powder of high remanence, high eigen coercive force and high magnetic energy product.
Description
(1) technical field
The present invention relates to a kind of high performance permanent magnetic ferrite magnetic powder and preparation method thereof.
(2) background technology
Nineteen fifty-two, the proposition chemical compositions such as J.J.Went of Philips company are SrO6 (Fe
2O
3) oxide magnet material, structure is the Magnetoplumbate-type hexad ferrite, claims M type hexad ferrite again.From that time, because low, the easy maturation of technology of cost of its abundant raw materials, average price and unit magnetic energy product, there is not problem of oxidation again, in many applications such as automotive direct current machine, starter motor, small air gap magetic indicator joint, Audio-Frequency Transformer, separator, holding devices, oxide magnet material is desirable first-selected permanent magnetic material.
In M type permanent-magnet ferrite magnet, demanding remanent magnetism, high HCJ and high magnetic energy product.At M type hexad ferrite manufacture view, Japan has realized three " 4 " already, be that remanent magnetism surpasses 4KGs, HCJ surpasses 4KOe, magnetic energy product above 4MGOe, at present, though shift to China gradually in the ferrite production base, permanent magnetic material NdFeB of new generation impacts also very big to Ferrite Material,, with Japanese TDK company is the world-renowned ferrite production producer of representative, but never abandons and loosens high-performance permanent-magnet ferrite (magnetic energy product surpasses 4.5MGOe) Products Development research.And the magnetic energy product of domestic present main flow ferrite product is still near 4MGOe, and high performance ferrite product is very few for number.Because each ferrimagnet manufacturing enterprise has carried out permanently effective research to technological factors such as orientation, density, now, the space of improving magnet performance by improvement orientation and density is very small, and the intrinsic magnetic property of magnetic (especially concerning bonded permanent magnet) is the key factor of decision final magnet performance, therefore, explore and study the novel preparation technology of high-performance M type ferrite magnetic, the structure of improving present high-end ferrite product is constituted, important scientific and technical innovation meaning is arranged.
A main path that improves M type permanent-magnet ferrite performance is to carry out doping vario-property.At present, be the high-end ferrite production producer of representative with Japanese TDK, the high-end ferrimagnet of being produced is all finished by doping vario-property.Such as bibliographical information, it is Sr that people such as Tenaud have obtained component
1-xLa
xFe
12-xCo
xO
19Ferrimagnet, under abundant orientation situation, when x=0.2, its remanent magnetism is 427mT, H
CjBe 353KA/m, when x=0.4, its remanent magnetism is 438mT, H
CjBe 273KA/m; Robot systems such as field mouth benevolence have been studied La, Zn and have been united replacement Sr
2+And Fe
3+, found that, for Sr
1-xLa
xFe
12-xZn
xO
19System, when x=0.3, saturation magnetization is higher by 4% than unsubstituted strontium ferrite, anisotropy constant K
1Suitable with M type barium ferrite, adopt special flouring technology and cooperate high density and highfield orientation can obtain: B
r=0.46T, H
Cb=203KA/m, H
Cj=207KA/m, (BH)
Max=41KJ/m
3, wherein, the Br value is very near the μ of SrM
0M
sTheoretical value (0.465T), maximum magnetic energy product and theoretical value (41.4KJ/m
3) also very nearly the same.People such as Taguchi then by strict control technology, have obtained Br at 0.452-0.459T, H
CjFerrimagnet between 194-223KA/m.
From top research as can be seen, by doping Co permanent-magnet ferrite being carried out modification is a main path that obtains high HCJ, as TDK Corp. at Chinese patents (application number: adopted Co, Ni, Zn to come permanent-magnet ferrite is carried out doping vario-property to improve its coercive force or maximum magnetic energy product 200510006196.6).And Hitachi Metal Co., Ltd. is at its patent (application number: also mention 99800254.2), do not adding the HCJ that obtains under the situation of Co usually below 300KA/m, and under the situation of adding 100at% Elements C o, the maximum HCJ of acquisition can reach 358KA/m.Because Co is a kind of important strategic metallic element, make the cost of permanent magnetic ferrite magnetic powder than higher with adding Co.
(3) summary of the invention
The object of the invention is to provide a kind of lower-cost new permanent magnetic ferrite magnetic powder, has high remanent magnetism, HCJ and maximum magnetic energy product.For realizing the object of the invention, the technical solution used in the present invention is:
A kind of high performance permanent magnetic ferrite magnetic powder, the chemical composition of described magnetic are A
1-xLa
xFe
12-yCu
yO
19, wherein A is the combination of Sr or Ba or their arbitrary proportions, and x is 0.05~0.4, and y is 0.05~0.4; Preferred x is 0.15~0.3, and y is 0.15~0.3.
Described A is for recommending the combination of Sr and Ba arbitrary proportion.
Through ball milling 3-6h, the meso-position radius granularity is controlled at 0.8-2 μ m to synthetic ferrite powder in high speed ball mill, and at 900-1000 ℃ of annealing 1-3h, the magnetic that is obtained is measured its remanent magnetism more than 0.218T under non-oriented situation, and maximum magnetic energy product is at 8KJ/m
3More than, HCJ is more than 300KA/m.
Especially at x=0.15-0.35, under the situation of y=0.15-0.35, the remanent magnetism of the strontium ferrite of acquisition under non-oriented situation can reach more than the 0.23T, and maximum magnetic energy product is at 10KJ/m
3Near, HCJ surpasses 310KA/m (being up to 341KA/m).
The preparation method of high performance permanent magnetic ferrite magnetic powder of the present invention is as follows: with the raw material iron powder, iron oxide, oxidant, strontium carbonate or brium carbonate, lanthana, cupric oxide mixes, 100-110 ℃ of drying removed moisture, material is evenly distributed in the self propagating high temperature reaction vessel, through lighting, cause whole system generation self propagating high temperature synthetic reaction, product is through broken, coarse crushing, fine grinding, granularity is controlled at 0.8-2 μ m, wash with water, dry, make described high performance permanent magnetic ferrite magnetic powder, sodium chlorate, iron powder, iron oxide, strontium carbonate (or brium carbonate or both sums), the ratio of the amount of substance of lanthana and cupric oxide is 1: 2.15-2.5: 3.5-3.85: 0.5-0.6: 0.025-0.2: 0.05-0.4.
The feed intake ratio of amount of substance of preferred raw material is: the ratio of the amount of substance of sodium chlorate, iron powder, iron oxide, strontium carbonate, lanthana and cupric oxide is 1: 2.15: 3.8: 0.5: 0.15: 0.3.
The preparation method of further described high performance permanent magnetic ferrite magnetic powder: with prescription proportion raw material evenly mixed 1h in mixer, be placed on then in the drying box in 100 ℃ of dry 4h, material is evenly distributed in the self propagating high temperature synthesising container then, through igniting, cause whole system generation self propagating high temperature synthetic reaction, reacted material is through broken back ball milling 6h in ball mill, granularity is controlled at 0.8-2 μ m, washes with water, dry 8h promptly gets described high performance permanent magnetic ferrite magnetic powder in drying box then.
Concrete, as with raw material, comprise that reduced iron powder, iron oxide, oxidant, strontium carbonate (or brium carbonate), lanthana, cupric oxide mix to come that synthetic to satisfy chemical formula be Sr
1-xLa
xFe
12-yCu
yO
19The permanent-magnet ferrite powder, wherein, the ratio of the amount of substance of sodium chlorate, iron powder, iron oxide, strontium carbonate (or brium carbonate or both sums), lanthana and cupric oxide is 1: 2.15-2.5: 3.5-3.85: 0.5-0.6: 0.025-0.2: 0.05-0.4.Adopt the self propagating high temperature synthetic method to synthesize desired ferrite powder, detailed process is: with the material mixed 1-3h in mixer for preparing, make each material fully mixed, dry 1-4h in drying box then, baking temperature 100-110 ℃, to remove the moisture that mixed material adsorbs in air, material is evenly distributed in the self propagating high temperature reaction vessel then, through lighting, cause whole system generation self propagating high temperature synthetic reaction, reacted material is through broken, coarse crushing, fine grinding, granularity is controlled at 0.8-2 μ m, washes with water to remove accessory substance NaCl wherein, drying, thus the final products high performance permanent magnetic ferrite magnetic powder obtained.
Because the powder magnetic energy measurement adopts the mode of bonded permanent magnet mark piece to carry out, therefore, before measuring, dried magnetic need be at 900-1000 ℃ of annealing 1-3h.
The present invention compared with prior art, its beneficial effect is embodied in: the present invention adopts a kind of new permanent-magnet ferrite prescription, do not adopt rare strategy metal Co, and adopt the relatively low La-Cu associating doped and substituted of cost to control ferritic chemical composition, thereby obtain the permanent-magnet ferrite powder of a kind of high remanent magnetism, high intrinsic coercive force and high energy product, compare with composition with traditional high performance ferrite powder manufacturing process, cost reduces greatly.
(4) description of drawings:
Fig. 1 has shown that embodiment 8 makes the XRD facies analysis result of sample.
Fig. 2 has shown that embodiment 8 makes the microscopic appearance of sample.
(5) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1~10
With certain proportion raw material (summation is 1Kg, and the concrete prescription of each material is as shown in table 1) evenly mixed 1h in mixer.Be placed on then in the drying box in 100 ℃ of dry 4h, to remove the moisture that in air, adsorbs, material is evenly distributed in the self propagating high temperature synthesising container then, through igniting, cause whole system generation self propagating high temperature synthetic reaction, reacted material is through broken back ball milling 6h in ball mill, granularity is controlled at 0.8-2 μ m, wash with water, dry 8h in drying box obtains desired finished product high performance permanent magnetic ferrite magnetic powder then.
In order to measure the magnetic property of permanent magnetic ferrite magnetic powder (abbreviation magnetic), with the dried magnetic of ball milling in Muffle furnace in 1000 ℃ of annealing 1h, utilize its phase composition of XRD analysis then.A certain proportion of ferrite powder is mixed with binding agent, be prepared into the mark piece of Ф 10 * 10mm, measuring the magnetic property of this mark piece under non-oriented situation on the permanent magnetic material analyzer,, obtaining the magnetic property of non-oriented ferromagnetic oxide powder according to ferrite powder shared ratio in the mark piece.Because with its linear variation of proportion in the mark piece, therefore, listed Hcj value is not the HCJ that contains the mark piece that directly records under the magnetic 80wt% situation to the HCJ Hcj of ferromagnetic oxide powder in the table 2.
Table 1 Sr
1-xLa
xFe
12-yCu
yO
19Input amount (the unit: g) of each raw material in the sample
Embodiment | NaClO 3 | Fe | Fe 2O 3 | SrCO 3 | La 2O 3 | CuO |
1 | 114.8 (1) | 129.5 (2.15) | 663.0 (3.85) | 79.6 (0.5) | 8.8 (0.025) | 4.3 (0.05) |
2 | 113.3 (1) | 127.8 (2.15) | 654.5 (3.85) | 78.6 (0.5) | 17.3 (0.05) | 8.5 (0.1) |
3 | 111.9 (1) | 126.2 (2.15) | 646.1 (3.85) | 77.6 (0.5) | 25.7 (0.075) | 12.5 (0.15) |
4 | 110.5 (1) | 124.6 (2.15) | 638.0 (3.85) | 76.6 (0.5) | 33.8 (0.1) | 16.5 (0.2) |
5 | 107.7 (1) | 121.6 (2.15) | 622.3 (3.85) | 74.7 (0.5) | 49.5 (0.15) | 24.2 (0.3) |
6 | 105.2 (1) | 118.6 (2.15) | 607.4 (3.85) | 72.9 (0.5) | 64.4 (0.2) | 31.4 (0.4) |
7 | 110.2 (1) | 144.5 (2.5) | 578.4 (3.5) | 91.7 (0.6) | 50.6 (0.15) | 24.7 (0.3) |
8 | 107.7 (1) | 130.0 (2.3) | 614.0 (3.8) | 74.7 (0.5) | 49.5 (0.15) | 24.1 (0.3) |
9 | 111.4 (1) | 125.7 (2.15) | 643.7 (3.85) | 77.3 (0.5) | 8.5 (0.025) | 33.3 (0.4) |
10 | 108.1 (1) | 122.0 (2.15) | 624.6 (3.85) | 75.0 (0.5) | 66.2 (0.2) | 4.04 (0.05) |
Annotate: numerical value is when being 1mol with sodium chlorate in the bracket, accordingly the amount of substance of each raw material.
The magnetic property and the XRD facies analysis result of each embodiment sample of experiment acquisition are as shown in table 2, and the XRD diffraction pattern of the sample that obtains among the embodiment 8 as shown in Figure 1.
The magnetic property of the SLC sample of table 2 doping La-Cu
Embodiment | B r(T) | H cb (KA/m) | H cj (KA/m) | (BH) max (KJ/m 3) | XRD result |
1 | 0.218 | 151 | 341 | 8.80 | The M phase |
2 | 0.234 | 159 | 338 | 9.06 | The M phase |
3 | 0.241 | 163 | 338 | 9.99 | The M phase |
4 | 0.235 | 159 | 312 | 9.33 | The M phase |
5 | 0.243 | 164 | 311 | 10.03 | The M phase |
6 | 0.222 | 148 | 303 | 8.15 | The M phase |
7 | 0.243 | 158 | 301 | 8.38 | The M phase |
8 | 0.245 | 166 | 318 | 10.09 | The M phase |
9 | 0.222 | 142 | 305 | 8.12 | The M phase |
10 | 0.216 | 139 | 301 | 8.02 | The M phase |
As can be seen from Table 2, in whole formula range, the sample that is obtained is M type permanent-magnet ferrite (SrFe
12O
19), according to the original ingredient ratio, chemical composition meets Sr as can be known
1-xLa
xFe
12-yCu
yO
19Non-oriented sample all has higher remanent magnetism and very high HCJ, wherein the remanent magnetism distribution is at 0.218-0.243T, HCJ be distributed in 301-341KA/m, especially the sample to obtaining among the embodiment 1, its HCJ is up to 341KA/m, the highest HCJ (its value is 358KA/m) of the interpolation 100at%Co element that the approaching patent in the past of this numerical value is reported, consider that this magnetic has added the binding agent of 20wt% when measuring, therefore, the HCJ of simple magnetic can be higher.And to embodiment 3 samples, it not only has very high HCJ (338KA/m), and has higher remanent magnetism (0.241mT), and under non-oriented situation, these data have surpassed the theoretical remanent magnetization value of the strontium ferrite that do not mix.Owing to do not contain strategic Elements C o in the chemical composition of this magnetic, therefore,, have bigger advance than the permanent-magnet ferrite of Co doping vario-property.
Use the present invention, the sample of acquisition has microscopic appearance preferably, the microscopic appearance that wherein obtains sample among the embodiment 3 as shown in the figure, as can be seen, the grain growth of strontium ferrite is grown complete from accompanying drawing 2, this also is its reason with higher HCJ.
Embodiment 11~20
According to the process identical with embodiment 1~10, preparation Ba
1-xLa
xFe
12-yCu
yO
19Standard sample and carry out the test of magnetic property.Each embodiment specifically fills a prescription as table 3 (the raw material summation is 1Kg), and it is as shown in table 4 that each embodiment makes the properties of product test result.
Table 3 Ba
1-xLa
xFe
12-yCu
yO
19Input amount (the unit: g) of each raw material in the sample
Embodiment | NaClO 3 | Fe | Fe 2O 3 | BaCO 3 | La 2O 3 | CuO |
11 | 113.5 (1) | 128.1 (2.15) | 655.8 (3.85) | 89.6 (0.5) | 8.7 (0.025) | 4.2 (0.05) |
12 | 112.1 (1) | 126.5 (2.15) | 647.5 (3.85) | 88.5 (0.5) | 17.2 (0.05) | 8.4 (0.1) |
13 | 110.7 (1) | 124.9 (2.15) | 639.3 (3.85) | 87.3 (0.5) | 25.4 (0.075) | 12.4 (0.15) |
14 | 109.3 (1) | 123.3 (2.15) | 631.3 (3.85) | 86.3 (0.5) | 33.5 (0.1) | 16.3 (0.2) |
15 | 106.6 (1) | 120.3 (2.15) | 616.0 (3.85) | 84.2 (0.5) | 48.9 (0.15) | 23.9 (0.3) |
16 | 104.1 (1) | 117.5 (2.15) | 601.4 (3.85) | 82.2 (0.5) | 63.7 (0.2) | 31.1 (0.4) |
17 | 108.8 (1) | 142.7 (2.5) | 571.2 (3.5) | 103.0 (0.6) | 49.9 (0.15) | 24.4 (0.3) |
18 | 106.6 (1) | 128.7 (2.3) | 607.8 (3.8) | 84.1 (0.5) | 48.9 (0.15) | 23.9 (0.3) |
19 | 110.3 (1) | 124.4 (2.15) | 636.9 (3.85) | 87.0 (0.5) | 8.4 (0.025) | 32.9 (0.4) |
20 | 107.0 (1) | 120.7 (2.15) | 618.2 (3.85) | 84.5 (0.5) | 65.5 (0.2) | 4.0 (0.05) |
Annotate: numerical value is when being 1mol with sodium chlorate in the bracket, accordingly the amount of substance of each raw material.
Table 4 Ba
1-xLa
xFe
12-yCu
yO
19The magnetic property of sample
Embodiment | B r(T) | H cb(KA/m) | H cj(KA/m) | (BH) max(KJ/m 3) | XRD result |
11 | 0.222 | 155 | 327 | 8.68 | The M phase |
12 | 0.238 | 157 | 324 | 9.04 | The M phase |
13 | 0.243 | 160 | 325 | 9.89 | The M phase |
14 | 0.238 | 153 | 300 | 9.12 | The M phase |
15 | 0.245 | 162 | 305 | 9.98 | The M phase |
16 | 0.223 | 151 | 301 | 8.02 | The M phase |
17 | 0.245 | 158 | 298 | 8.32 | The M phase |
18 | 0.245 | 162 | 315 | 10.01 | The M phase |
19 | 0.223 | 142 | 302 | 8.11 | The M phase |
20 | 0.218 | 140 | 299 | 8.01 | The M phase |
Embodiment 21~27
According to the process identical with embodiment 1~10, and preparation (Sr, Ba)
1-xLa
xFe
12-yCu
yO
19Standard sample and carry out the test of magnetic property.The concrete prescription of each embodiment sees Table 5 (the raw material summation is 1Kg), and the properties of product test result that each embodiment makes is as shown in table 6.
Table 5 (Sr, Ba)
1-xLa
xFe
12-yCu
yO
19Each raw material input amount (unit: g) in the sample
Embodiment | NaClO 3 | Fe | Fe 2O 3 | SrCO 3 | BaCO 3 | La 2O 3 | CuO |
21 | 106.7 (1) | 120.4 (2.15) | 616.6 (3.85) | 7.4 (0.05) | 75.8 (0.45) | 49.0 (0.15) | 23.9 (0.3) |
22 | 106.9 (1) | 120.6 (2.15) | 617.3 (3.85) | 14.8 (0.1) | 67.5 (0.4) | 49.1 (0.15) | 24.0 (0.3) |
23 | 107.1 (1) | 120.8 (2.15) | 618.5 (3.85) | 29.7 (0.2) | 50.7 (0.3) | 49.2 (0.15) | 24.0 (0.3) |
24 | 107.5 (1) | 121.3 (2.15) | 621.1 (3.85) | 59.7 (0.4) | 17.0 (0.1) | 49.4 (0.15) | 24.1 (0.3) |
25 | 107.6 (1) | 121.4 (2.15) | 621.7 (3.85) | 67.2 (0.45) | 8.5 (0.05) | 49.4 (0.15) | 24.1 (0.3) |
26 | 119.3 (1) | 156.5 (2.5) | 626.6 (3.5) | 74.5 (0.45) | 9.4 (0.05) | 9.1 (0.025) | 4.5 (0.05) |
27 | 108.1 (1) | 141.8 (2.5) | 567.5 (3.5) | 7.5 (0.05) | 76.8 (0.45) | 66.2 (0.2) | 32.3 (0.4) |
Annotate: numerical value is when being 1mol with sodium chlorate in the bracket, accordingly the amount of substance of each raw material.
Table 6 (Sr, Ba)
1-xLa
xFe
12-yCu
yO
19The magnetic property of sample
Embodiment | B r(T) | H cb(KA/m) | H cj(KA/m) | (BH) max(KJ/m 3) | XRD result |
21 | 0.247 | 162 | 300 | 9.96 | The M phase |
22 | 0.246 | 165 | 303 | 9.99 | The M phase |
23 | 0.243 | 163 | 306 | 9.97 | The M phase |
24 | 0.244 | 163 | 308 | 9.99 | The M phase |
25 | 0.244 | 165 | 309 | 10.01 | The M phase |
26 | 0.237 | 156 | 302 | 9.01 | The M phase |
27 | 0.235 | 153 | 299 | 8.98 | The M phase |
From top embodiment as can be seen, among the preparation method described in the invention, the sample that obtains all has higher remanent magnetism, higher intrinsic coercive force and high magnetic energy product, simultaneously the XRD testing result shows that all the powder of acquisition is single M type hexad ferrite, and La-Cu enters ferritic lattice position, and to have constituted chemical composition be A
1-xLa
xFe
12-yCu
yO
19High performance permanent magnetic ferrite magnetic powder.
Claims (8)
1, a kind of high performance permanent magnetic ferrite magnetic powder, the chemical composition that it is characterized in that described magnetic is A
1-xLa
xFe
12-yCu
yO
19, wherein A is the combination of Sr or Ba or their arbitrary proportions, and x is 0.05~0.4, and y is 0.05~0.4.
2, high performance permanent magnetic ferrite magnetic powder as claimed in claim 1 is characterized in that: described x is 0.15~0.3, and y is 0.15~0.3.
3, high performance permanent magnetic ferrite magnetic powder as claimed in claim 2 is characterized in that: described x is 0.3, and y is 0.3.
4, high performance permanent magnetic ferrite magnetic powder as claimed in claim 1 is characterized in that: described A is Sr or Ba.
5, high performance permanent magnetic ferrite magnetic powder as claimed in claim 4 is characterized in that: described A is the combination of the arbitrary proportion of Sr and Ba.
6, the method for preparing high performance permanent magnetic ferrite magnetic powder as claimed in claim 1, it is characterized in that described method is with sodium chlorate, the raw material iron powder, iron oxide, strontium carbonate is or/and brium carbonate, lanthana, cupric oxide mixes, 100~110 ℃ of dryings are removed moisture, material is evenly distributed in the self propagating high temperature reaction vessel, through lighting, cause whole system generation self propagating high temperature synthetic reaction, product is through broken, coarse crushing, fine grinding, granularity is controlled at 0.8-2 μ m, wash with water, dry, make described high performance permanent magnetic ferrite magnetic powder, described sodium chlorate, iron powder, iron oxide, strontium carbonate or brium carbonate or both sums, the ratio of the amount of substance of lanthana and cupric oxide is 1: 2.15-2.5: 3.5-3.85: 0.5-0.6: 0.025-0.2: 0.05-0.4.
7, the method for high performance permanent magnetic ferrite magnetic powder as claimed in claim 6 is characterized in that described method: the ratio of the amount of substance of sodium chlorate, iron powder, iron oxide, strontium carbonate, lanthana and cupric oxide is 1: 2.15: 3.8: 0.5: 0.15: 0.3.
8, the method for high performance permanent magnetic ferrite magnetic powder as claimed in claim 6, it is characterized in that described method: with prescription proportion raw material evenly mixed 1h in mixer, be placed on then in the drying box in 100 ℃ of dry 4h, material is evenly distributed in the self propagating high temperature synthesising container then, through igniting, cause whole system generation self propagating high temperature synthetic reaction, reacted material is through broken back ball milling 6h in ball mill, granularity is controlled at 0.8-2 μ m, washes with water, dry 8h promptly gets described high performance permanent magnetic ferrite magnetic powder in drying box then.
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