CN112645704B - Preparation method of high-performance ferrite - Google Patents
Preparation method of high-performance ferrite Download PDFInfo
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- CN112645704B CN112645704B CN202011578997.0A CN202011578997A CN112645704B CN 112645704 B CN112645704 B CN 112645704B CN 202011578997 A CN202011578997 A CN 202011578997A CN 112645704 B CN112645704 B CN 112645704B
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 37
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 239000002002 slurry Substances 0.000 claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 208000005156 Dehydration Diseases 0.000 claims abstract description 14
- 230000018044 dehydration Effects 0.000 claims abstract description 14
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 14
- 238000001238 wet grinding Methods 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- 239000000654 additive Substances 0.000 claims description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- 239000011575 calcium Substances 0.000 claims description 10
- 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 10
- 239000011701 zinc Substances 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 9
- 239000012071 phase Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 5
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 5
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 5
- 229940075613 gadolinium oxide Drugs 0.000 claims description 5
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 5
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 5
- KBLRIGLPGMRISA-UHFFFAOYSA-N neodymium(3+) oxygen(2-) praseodymium(3+) Chemical compound [O-2].[Pr+3].[Nd+3].[O-2].[O-2] KBLRIGLPGMRISA-UHFFFAOYSA-N 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000003746 solid phase reaction Methods 0.000 claims description 5
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- 239000004227 calcium gluconate Substances 0.000 claims description 3
- 229960004494 calcium gluconate Drugs 0.000 claims description 3
- 235000013927 calcium gluconate Nutrition 0.000 claims description 3
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000000696 magnetic material Substances 0.000 abstract description 7
- 239000004615 ingredient Substances 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract 1
- 230000008569 process Effects 0.000 description 7
- 230000005389 magnetism Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- ROYOLNQPXVHWNE-UHFFFAOYSA-N [Co].[Ca].[La] Chemical compound [Co].[Ca].[La] ROYOLNQPXVHWNE-UHFFFAOYSA-N 0.000 description 2
- WOIHABYNKOEWFG-UHFFFAOYSA-N [Sr].[Ba] Chemical compound [Sr].[Ba] WOIHABYNKOEWFG-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical group 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 125000005619 boric acid group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
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- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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Abstract
The invention relates to the technical field of magnetic materials, and discloses a preparation method of high-performance ferrite, which comprises the following steps: the method comprises the following steps: pretreating the raw materials at high temperature; step two: weighing the ingredients and performing wet grinding and crushing; step three: performing dehydration treatment, namely dehydrating the mixed material obtained in the step two by using a horizontal centrifuge, wherein the solid content of the slurry obtained after dehydration is 67wt%; step four: pre-burning step by step; step five: crushing and ball-milling, namely, performing dry ball-milling crushing on the pre-sintered material obtained by pre-sintering step by step in the fourth step, adding a dispersing agent for secondary ball-milling, and performing ball-milling for 18 hours continuously to obtain slurry; step six: molding; step seven: sintering, heat treating the formed body in the sixth step at a temperature of 200 ℃ to remove moisture. The preparation method of the high-performance ferrite has the phase molecular formula of Sr (1‑a‑2b‑c‑d) Ca a Pr b Nd b La c Gd d Fe (2n‑x‑y) Co x Zn y O 19 The permanent magnetic ferrite has the advantages that the permanent magnetic ferrite has the performance of larger than or equal to 4550 Gs intrinsic coercive force larger than or equal to 5500 Oe by high-temperature pretreatment, wet grinding and disintegration, stepwise pre-sintering and the like of raw materials for proportioning.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a preparation method of high-performance ferrite.
Background
In the modern society, with the rapid development of the electronic industry, the demand of magnetic materials is more and more, although China is a large country for producing magnetic materials, the product size precision and the performance grade of the magnetic materials are different from those of developed countries, and as one kind of magnetic materials, the permanent magnetic ferrite is the most widely applied magnetic material at present, particularly, the high-performance permanent magnetic ferrite material is a basic functional material for the contemporary society and the development thereof, and along with the development trend of miniaturization and lightness and thinness of various electronic and electric products, the requirement on the performance of the ferrite is higher and higher.
At present, the existing strontium barium ferrite and calcium lanthanum cobalt ferrite developed at home and abroad based on an ion substitution technology are not enough to meet the increasingly high requirements of electronic product miniaturization on the magnetic properties of the permanent magnetic ferrite, and the performance that the residual magnetism is not less than 4500Gs and the intrinsic coercive force is not less than 5500 Oe can not be realized at the highest, for example, the idea that La and Co are respectively used for replacing Sr and Fe disclosed by patent CN 1335997A realizes the magnetic properties Br4500Gs and Hcj3200 Oe disclosed by patents Br 4450Gs and Hcj 4460 Oe and CN 102945718A.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of high-performance ferrite, which has Sr in a phase molecular formula (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 The method has the advantages that the performance of permanent magnetic ferrite with the residual magnetism being larger than or equal to 4550 Gs intrinsic coercive force being larger than or equal to 5500 Oe is realized through high-temperature pretreatment, wet grinding and breaking of raw materials, step-by-step pre-sintering and the like, and the problems that the existing strontium barium ferrite and calcium lanthanum cobalt ferrite researched and developed at home and abroad based on an ion substitution technology are not enough to meet the requirement of miniaturization of electronic products on the increasingly higher magnetic property of the permanent magnetic ferrite, and the performance of the residual magnetism being larger than or equal to 5500 Oe in 4500Gs cannot be realized at the highest.
(II) technical scheme
To achieve Sr in the molecular formula of phase (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 In order to match, the purpose of realizing the performance of the permanent magnetic ferrite with the remanence larger than or equal to 4550 Gs intrinsic coercive force larger than or equal to 5500 Oe is realized through high-temperature pretreatment, wet grinding and crushing, step-by-step pre-sintering and the like of raw materials, the invention provides the following technical scheme: a high-performance ferrite with Sr as its molecular formula (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 ；
Wherein: 0.3 to 0.5 of a, 0.02 to 0.1 of b, 0.2 to 0.4 of c, 0.05 to 0.15 of d, 0.2 to 0.4 of x, 0.05 to 0.2 of y and 9.5 to 11.5 of 2 n-x-y.
Preferably, the optimal range of a is 0.34-0.46, the ratio range of c/(2b + d) of b, c and d is 1.5-4.2, and the optimal range is 1.9-3.8; the optimal range of x is 0.25-0.38, and the optimal range of y is 0.08-0.17.
A preparation method of high-performance ferrite comprises the following steps:
the method comprises the following steps: high temperature pretreatment of raw materials
Keeping the raw materials of iron oxide, strontium carbonate, calcium carbonate, lanthanum oxide, cobalt oxide, praseodymium neodymium oxide, gadolinium oxide and zinc oxide at the high temperature of 300 ℃ for 1 hour respectively, then sealing and storing, and reducing the temperature of the raw materials to be below 60 ℃;
step two: ingredient weighing and wet grinding disintegrating
The preparation method comprises the following steps of mixing materials according to the molecular formula Sr (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 The mole ratio of the permanent magnetic ferrite main phase raw material after high-temperature pretreatment in the first step is weighed: wherein a is 0.3-0.5, b is 0.02-0.1, c is 0.2-0.4, d is 0.05-0.15, x is 0.2-0.4, y is 0.05-0.2, and 2n-x-y is 9.5-11.5;
carrying out wet ball milling and crushing on the proportioned raw materials, adding a primary additive into the proportioned raw materials, putting the mixed materials into a wet ball mill for carrying out wet milling and crushing, and carrying out material crushing in the ball mill: water: the ball proportion is 1;
step three: dehydration treatment
Dehydrating the mixed material obtained in the step two by using a horizontal centrifuge, wherein the solid content of slurry obtained after dehydration is 67wt%;
step four: step-by-step burn-in
Performing first-step granulation presintering on the mixed material obtained after dehydration treatment in the third step in a first rotary kiln, controlling the presintering temperature at 800-1000 ℃ and the material passing speed at 2m/h to obtain a granular material with zero scorching loss at 1000 ℃, and then performing second-step presintering in a second rotation 2 to perform solid-phase reaction, wherein the presintering temperature is controlled at 1280-1380 ℃ and the material passing speed is 5m/h;
step five: crushing ball mill
Pre-sintering materials obtained in the fourth step in steps are subjected to dry ball milling and crushing, then dispersing agents are added for secondary ball milling, and the ball milling is continued for 18 hours to obtain slurry;
step six: shaping of
Dehydrating the slurry obtained in the fifth step by using a centrifugal machine, wherein the solid content of the slurry obtained after dehydration is 73wt%, and then placing the obtained slurry in a 700KA/M magnetic field for compression molding;
step seven: sintering of
And (3) carrying out heat treatment on the formed body in the sixth step at the temperature of 200 ℃, removing water, and then sintering in the atmosphere, wherein the sintering temperature is controlled to be 1190-1260 ℃, so as to obtain the sintered permanent magnet.
Preferably, the first additive in the second step is boric acid and silica powder, and the adding proportion of the first additive is 0.2kg of boric acid and 0.4kg of silica per 100kg of raw material.
Preferably, phi 4.8mm bearing steel is used for the balls in the wet ball mill in the second step.
Preferably, the dispersant in the fifth step is added according to the following weight ratio, and the total amount of the dispersant added per 100kg of the pre-sintered material is 0.1kg.
Preferably, the dispersant in the fifth step is calcium gluconate or sorbitol.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of high-performance ferrite, which has the following beneficial effects:
1. according to the preparation method of the high-performance ferrite, the raw materials of iron oxide, strontium carbonate, calcium carbonate, lanthanum oxide, cobalt oxide, praseodymium neodymium oxide, gadolinium oxide and zinc oxide are respectively subjected to heat preservation at the high temperature of 300 ℃ for 1 hour and then are stored in a sealing manner, so that the moisture and volatile substances in the raw materials can be effectively removed, the raw material proportion is more accurate, and the formula volatility is reduced.
2. According to the preparation method of the high-performance ferrite, steel balls with the particle size phi of 4.8mm are used in a ball mill for wet grinding and disintegration by virtue of ingredient weighing, and are subjected to speed reduction grinding, so that the molecular structure of the raw material can be maintained to a large extent, the passing rate of a 200-mesh screen is controlled, uniformly dispersed slurry is obtained, and the raw material is not easy to crystallize in a pre-sintering link.
3. According to the preparation method of the high-performance ferrite, the step-by-step pre-sintering method is adopted, when the granulation pre-sintering is carried out in the first step, materials pass through the high-temperature pre-sintering stage in the second step at a low speed, so that the raw materials are fully decomposed and then undergo solid-phase reaction in the high-temperature pre-sintering stage in the second step, the influence of decomposed volatile matters of the raw materials on the solid-phase reaction is reduced, the obtained granular materials are more compact, and the improvement of performance is facilitated.
4. According to the preparation method of the high-performance ferrite, the obtained pre-sintering powder only needs to be added with a dispersing agent during secondary grinding, and the dispersing agent can improve the orientation of slurry particles during magnetic field forming, so that the slurry is easier to orient; different from the conventional ball milling process, other additives such as calcium carbonate and silicon oxide are not added for the second time but only added for the first time, so that the performance is improved.
5. The phase molecular formula of the high-performance ferrite prepared by the preparation method is concretely Sr (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 The permanent magnetic ferrite residual magnetism is not less than 4550 Gs intrinsic coercive force not less than 5500 Oe by the process of the pre-sintering material.
Drawings
FIG. 1 is a table showing the molecular formula of ferrite obtained by the method for preparing a high performance ferrite according to the present invention;
FIG. 2 is a table of magnetic properties of a method for preparing a high performance ferrite according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to FIGS. 1-2, a high performance ferrite is shown, which has a phase componentSub-formula is concretely Sr (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 ；
Wherein: 0.3 to 0.5 of a, 0.02 to 0.1 of b, 0.2 to 0.4 of c, 0.05 to 0.15 of d, 0.2 to 0.4 of x, 0.05 to 0.2 of y and 9.5 to 11.5 of 2 n-x-y.
The optimal range of a is 0.34 to 0.46, the ratio range of b, c and d, c/(2b + d), is 1.5 to 4.2, and the optimal range is 1.9 to 3.8; the optimal range of x is 0.25-0.38, and the optimal range of y is 0.08-0.17.
A preparation method of high-performance ferrite comprises the following steps:
the method comprises the following steps: high temperature pretreatment of raw materials
Keeping the raw materials of iron oxide, strontium carbonate, calcium carbonate, lanthanum oxide, cobalt oxide, praseodymium neodymium oxide, gadolinium oxide and zinc oxide at the high temperature of 300 ℃ for 1 hour respectively, then sealing and storing, and reducing the temperature of the raw materials to be below 60 ℃;
step two: ingredient weighing and wet milling and crushing
The preparation method comprises the following steps of mixing materials according to the molecular formula Sr (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 The mole ratio of the permanent magnetic ferrite main phase raw material after high-temperature pretreatment in the first step is weighed: wherein a is 0.3-0.5, b is 0.02-0.1, c is 0.2-0.4, d is 0.05-0.15, x is 0.2-0.4, y is 0.05-0.2, and 2n-x-y is 9.5-11.5;
carrying out wet ball milling and crushing on the proportioned raw materials, adding a primary additive into the proportioned raw materials, putting the mixed materials into a wet ball mill for carrying out wet milling and crushing, and carrying out material crushing in the ball mill: water: the ball proportion is 1;
step three: dehydration treatment
Dehydrating the mixed material obtained in the step two by using a horizontal centrifuge, wherein the solid content of slurry obtained after dehydration is 67wt%;
step four: step-by-step burn-in
Performing first-step granulation presintering on the mixed material obtained after dehydration treatment in the third step in a first rotary kiln, controlling the presintering temperature at 800-1000 ℃ and the material passing speed at 2m/h to obtain a granular material with zero scorching loss at 1000 ℃, and then performing second-step presintering in a second rotation 2 to perform solid-phase reaction, wherein the presintering temperature is controlled at 1280-1380 ℃ and the material passing speed is 5m/h;
step five: crushing ball mill
Pre-sintering materials obtained in the fourth step are subjected to dry ball milling and crushing, then dispersing agents are added for secondary ball milling, and the ball milling is continued for 18 hours to obtain slurry;
step six: shaping of
Dehydrating the slurry obtained in the fifth step by using a centrifugal machine, wherein the solid content of the slurry obtained after dehydration is 73wt%, and then placing the obtained slurry in a 700KA/M magnetic field for compression molding;
step seven: sintering of
And (4) performing heat treatment on the formed body in the sixth step at the temperature of 200 ℃, removing water, and then sintering in the atmosphere, wherein the sintering temperature is controlled to be 1190-1260 ℃, so as to obtain the sintered permanent magnet.
In the second step, the primary additive is boric acid and silicon micropowder, and the addition proportion of the primary additive is that 0.2kg of boric acid and 0.4kg of silicon oxide are added into every 100kg of raw materials.
And D, using phi 4.8mm bearing steel for the balls in the wet ball mill in the step II.
In the fifth step, the dispersing agent is added according to the following weight proportion, and the total amount of the dispersing agent added in each 100kg of the pre-sintered material is 0.1kg.
And the dispersant in the fifth step is calcium gluconate or sorbitol.
In summary, according to the preparation method of the high-performance ferrite, the raw materials of iron oxide, strontium carbonate, calcium carbonate, lanthanum oxide, cobalt oxide, praseodymium neodymium oxide, gadolinium oxide and zinc oxide are respectively preserved in a heat preservation mode at the high temperature of 300 ℃ for 1 hour and then are stored in a sealing mode, so that moisture and volatile substances in the raw materials can be effectively removed, the raw materials are proportioned, and the high-performance ferrite is sealedMore accurate, the formula fluctuation is reduced, bearing steel small-particle-size steel balls with the particle diameter phi of 4.8mm are used in a ball mill through ingredient weighing and wet grinding and are ground at a reduced speed, the molecular structure of raw materials can be maintained to a greater extent, the passing rate of a 200-mesh screen is controlled, and uniformly dispersed slurry is obtained, so that the raw materials are not easy to crystallize in a pre-sintering link; different from the conventional ball milling process, other additives such as calcium carbonate and silicon oxide are not added for the second time but only added for the first time, which is beneficial to improving the performance, and the phase molecular formula of the prepared high-performance ferrite is specifically Sr (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 The permanent magnetic ferrite residual magnetism is not less than 4550 Gs intrinsic coercive force not less than 5500 Oe by the process of the pre-sintering material.
It is to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A high performance ferrite characterized by: the phase molecular formula of the high-performance ferrite is specifically Sr (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 (ii) a Wherein: a is 0.3 to 0.5, b is 0.02 to 0.1, c is 0.2 to 0.4, d is 0.05 to 0.15, x is 0.2 to 0.4, y is 0.05 to 0.2, and 2n-x-y is 9.5 to 11.5;
the preparation method of the high-performance ferrite comprises the following steps:
the method comprises the following steps: performing high-temperature pretreatment on raw materials, namely respectively preserving the heat of the raw materials of iron oxide, strontium carbonate, calcium carbonate, lanthanum oxide, cobalt oxide, praseodymium neodymium oxide, gadolinium oxide and zinc oxide at the high temperature of 300 ℃ for 1 hour, then sealing and storing the raw materials, and reducing the temperature of the raw materials to be below 60 ℃;
step two: the preparation method of the material by weighing the material and wet milling and disintegrating the crushed material has the material according to the molecular formula Sr (1-a-2b-c-d) Ca a Pr b Nd b La c Gd d Fe (2n-x-y) Co x Zn y O 19 The mole ratio of the permanent magnetic ferrite main phase raw material after high-temperature pretreatment in the first step is weighed: wherein a is 0.3-0.5, b is 0.02-0.1, c is 0.2-0.4, d is 0.05-0.15, x is 0.2-0.4, y is 0.05-0.2, and 2n-x-y is 9.5-11.5; carrying out wet ball milling and crushing on the proportioned raw materials, adding a primary additive into the proportioned raw materials, putting the mixed materials into a wet ball mill for carrying out wet milling and crushing, and carrying out material crushing in the ball mill: water: the ball ratio is 1; the primary additive is specifically boric acid and silicon micropowder, and the adding proportion of the primary additive is that 0.2kg of boric acid and 0.4kg of silicon oxide are added into every 100kg of raw materials;
step three: dehydrating the mixed material obtained in the step two by using a horizontal centrifuge, wherein the solid content of the slurry obtained after dehydration is 67wt%;
step four: pre-burning step by step, performing first-step granulation pre-burning on the mixed material obtained after dehydration treatment in the third step in a first rotary kiln, controlling the pre-burning temperature to be 800-1000 ℃, and the material passing speed to be 2m/h to obtain a granular material with zero burning loss at 1000 ℃, and then performing second-step pre-burning in a second rotary kiln to perform solid phase reaction, wherein the pre-burning temperature is controlled to be 1280-1380 ℃, and the material passing speed is 5m/h;
step five: grinding and ball milling, namely, after the pre-sintered material obtained by pre-sintering step by step in the fourth step is ground by dry ball milling, adding a dispersing agent for secondary ball milling, and continuously ball milling for 18 hours to obtain slurry;
step six: carrying out dehydration treatment on the slurry obtained in the fifth step by using a centrifugal machine, wherein the solid content of the slurry obtained after dehydration is 73wt%, and then placing the obtained slurry in a 700kA/m magnetic field for compression molding;
step seven: and sintering at the temperature of 200 ℃ to carry out heat treatment on the formed body in the sixth step, removing water, and then sintering in the atmosphere, wherein the sintering temperature is controlled to be 1190-1260 ℃, so as to obtain the sintered permanent magnet.
2. A high performance ferrite as claimed in claim 1, wherein: a is 0.34-0.46, c/(2b + d) is 1.5-4.2, x is 0.25-0.38, and y is 0.08-0.17.
3. A high performance ferrite as claimed in claim 1, wherein: and D, using phi 4.8mm bearing steel for the balls in the wet ball mill in the step II.
4. A high performance ferrite as claimed in claim 1, wherein: the dispersant in the fifth step is added according to the following weight ratio, and the total amount of the dispersant added in each 100kg of the pre-sintered material is 0.1kg.
5. A high performance ferrite as claimed in claim 1, wherein: and the dispersant in the fifth step is calcium gluconate or sorbitol.
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