CN112898006A - Preparation process of permanent magnetic ferrite ball milling mixing material - Google Patents
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- 238000000498 ball milling Methods 0.000 title claims abstract description 65
- 239000000463 material Substances 0.000 title claims abstract description 56
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 36
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 30
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000654 additive Substances 0.000 claims abstract description 22
- 230000000996 additive effect Effects 0.000 claims abstract description 22
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004227 calcium gluconate Substances 0.000 claims abstract description 10
- 229960004494 calcium gluconate Drugs 0.000 claims abstract description 10
- 235000013927 calcium gluconate Nutrition 0.000 claims abstract description 10
- 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 abstract description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 229910000831 Steel Inorganic materials 0.000 claims description 14
- 239000010959 steel Substances 0.000 claims description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- 239000002245 particle Substances 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 4
- 230000005389 magnetism Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- 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
- C04B35/2683—Other ferrites containing alkaline earth metals or lead
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
Abstract
The invention discloses a preparation process of a permanent magnetic ferrite ball milling mixed material, which comprises the following steps: mixing iron oxide red and barium carbonate according to the mass ratio of 4:1, adding an additive after mixing, and then pre-sintering in a kiln to form a permanent magnetic ferrite pre-sintering material; adding the permanent magnetic ferrite pre-sintering material into zirconia balls and water, and mixing in a ball mill for 3-5 h; and transferring the ball-milled materials into a second-stage ball mill by using compressed air for ball milling. The preparation method is simple and easy to implement, the production cost is low, the addition of the calcium gluconate is beneficial to improving the particle size distribution of slurry in the ball milling process, and simultaneously, the orientation of particles in the forming stage is improved, so that the residual magnetism and the intrinsic coercive force of the material are improved. The added chromium powder has the fluxing function and can effectively reduce the sintering temperature. The grading ball milling mode can reduce the probability and the mixing amount of iron impurities, and different ball milling speeds are adopted, so that the particle size distribution tends to be just too distributed, and the magnetism of the permanent magnetic ferrite is effectively improved.
Description
Technical Field
The invention belongs to the technical field of permanent magnet materials, and particularly relates to a preparation process of a ball-milling mixed material of a permanent magnet ferrite.
Background
The permanent magnetic ferrite is also called hard magnetic ferrite, has the characteristic of continuously keeping constant magnetic field or magnetic moment after magnetization, is an important magnetic material, and can be widely applied to various application fields such as automobile direct current motors, starting motors, inductors, audio converters, separators and the like. With the development of science and technology, more equipment is required to be more miniaturized, lightweight, energy-saving and high-efficiency, and the permanent magnetic ferrite is used as an important permanent magnetic material in a plurality of equipment and puts more rigorous requirements on the performance of the permanent magnetic ferrite.
The conventional permanent magnetic ferrite ball-milling mixing preparation process is complex in production process, difficult to produce in large batch, high in production cost and technically innovative on the basis of the conventional technology.
Disclosure of Invention
The invention aims to provide a preparation process of a permanent magnetic ferrite ball milling mixed material.
In order to achieve the purpose, the invention provides the following technical scheme: a permanent magnetic ferrite ball milling mixing process comprises the following steps: step one, mixing iron oxide red and barium carbonate according to a mass ratio of 4:1, adding an additive after mixing, and then pre-sintering in a kiln to form a permanent magnetic ferrite pre-sintering material;
secondly, adding the permanent magnetic ferrite pre-sintering material into zirconia balls and water to a ball mill for mixing, wherein the ball milling time is 3-5 hours; wherein the weight ratio of the permanent magnetic ferrite pre-sintering material to the water to the zirconia balls is (0.8-1): (1.3-1.5): (10-12);
step three, transferring the materials ball-milled in the step two into a second-stage ball mill by using compressed air for ball milling, and adding steel balls and water into the materials, wherein the materials are as follows: steel ball: the proportion of water is (0.8-1): (1.2-1.5): (13-15).
Preferably, the addition amount of the additive is 3-5% of the mass of the iron oxide red.
Preferably, the additive comprises the following raw materials in percentage by weight based on 100 percent of the additive: 20-30% of calcium carbonate, 20-40% of silicon dioxide, 30-45% of metal chromium powder and 20-45% of calcium gluconate.
Further preferably, the additive is 100% and comprises the following raw materials in percentage by weight: 25% of calcium carbonate, 20% of silicon dioxide, 30% of metal chromium powder and 25% of calcium gluconate.
Preferably, the conditions for pre-burning in the kiln in the first step are as follows: pre-sintering at 1200-1300 ℃ for 40-80 minutes;
preferably: the diameter of the zirconia ball is 5-8 mm, and the diameter of the steel ball is 3-6 mm.
Preferably, the ball milling process in the third step is divided into three stages: in the first stage, the rotating speed is kept between 60rpm and 85rpm, and ball milling is carried out for 2 to 3 hours; in the second stage, the rotating speed is kept between 35rpm and 65rpm, and ball milling is carried out for 5 to 6 hours; and in the third stage, the rotation speed is kept between 25rpm and 55rpm, and ball milling is carried out for 5 to 6 hours to complete the ball milling.
Compared with the prior art, the invention has the following beneficial effects: the preparation method is simple and easy to implement, the production cost is low, the addition of the calcium gluconate is beneficial to improving the particle size distribution of slurry in the ball milling process, and simultaneously, the orientation of particles in the forming stage is improved, so that the residual magnetism and the intrinsic coercive force of the material are improved. The added chromium powder has the fluxing function and can effectively reduce the sintering temperature. The adoption of the graded ball milling mode can reduce the mixing probability and the mixing amount of iron impurities, and the adoption of different ball milling speeds leads the particle size distribution to tend to be just too distributed, thereby effectively improving the magnetism of the permanent magnetic ferrite.
Description of the drawings:
FIG. 1 is a schematic diagram of the preparation process of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely in the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Example 1:
a permanent magnetic ferrite ball milling mixing process comprises the following steps: step one, mixing iron oxide red and barium carbonate according to a mass ratio of 4:1, adding an additive after mixing, and then pre-sintering in a kiln to form a permanent magnetic ferrite pre-sintering material; the pre-sintering conditions are as follows: presintering at 1200 ℃ for 40 minutes; the addition amount of the additive is 3% of the mass of the iron oxide red; the additive is 100 percent and comprises the following raw materials in percentage by weight: 20% of calcium carbonate, 20% of silicon dioxide, 30% of metal chromium powder and 30% of calcium gluconate.
Secondly, adding the permanent magnetic ferrite pre-sintering material into zirconia balls and water to a ball mill for mixing, wherein the ball milling time is 3 hours; wherein the weight ratio of the permanent magnetic ferrite pre-sintering material to the water to the zirconia balls is 0.8: 1.3: 10;
step three, transferring the materials ball-milled in the step two into a second-stage ball mill by using compressed air for ball milling, and adding steel balls and water into the materials, wherein the materials are as follows: steel ball: the ratio of water is 0.8: 1.2: 13; the ball milling process in the third step is divided into three stages: in the first stage, the rotating speed is kept at 60rpm, and ball milling is carried out for 2 hours; in the second stage, the rotating speed is kept at 35rpm, and ball milling is carried out for 5 hours; and in the third stage, the rotation speed is kept at 25rpm, and ball milling is carried out for 5 hours to complete the ball milling.
Example 2:
a permanent magnetic ferrite ball milling mixing process comprises the following steps: step one, mixing iron oxide red and barium carbonate according to a mass ratio of 4:1, adding an additive after mixing, and then pre-sintering in a kiln to form a permanent magnetic ferrite pre-sintering material; the pre-sintering conditions are as follows: presintering for 80 minutes at 1300 ℃; the addition amount of the additive is 5% of the mass of the iron oxide red; the additive is 100 percent and comprises the following raw materials in percentage by weight: 30% of calcium carbonate, 40% of silicon dioxide, 45% of metal chromium powder and 45% of calcium gluconate.
Secondly, adding the permanent magnetic ferrite pre-sintering material into zirconia balls and water to a ball mill for mixing, wherein the ball milling time is 5 hours; wherein the weight ratio of the permanent magnetic ferrite pre-sintering material to the water to the zirconia balls is 1: 1.5: 12;
step three, transferring the materials ball-milled in the step two into a second-stage ball mill by using compressed air for ball milling, and adding steel balls and water into the materials, wherein the materials are as follows: steel ball: the proportion of water is 1: 1.2: 13; the ball milling process in the third step is divided into three stages: in the first stage, the rotating speed is kept at 85rpm, and ball milling is carried out for 3 hours; in the second stage, the rotating speed is kept at 65rpm, and ball milling is carried out for 6 hours; and in the third stage, the rotating speed is kept at 55rpm, and ball milling is carried out for 6 hours to complete the ball milling.
Example 3:
a permanent magnetic ferrite ball milling mixing process comprises the following steps: step one, mixing iron oxide red and barium carbonate according to a mass ratio of 4:1, adding an additive after mixing, and then pre-sintering in a kiln to form a permanent magnetic ferrite pre-sintering material; the pre-sintering conditions are as follows: presintering for 60 minutes at 1250 ℃; the addition amount of the additive is 4% of the mass of the iron oxide red; the additive is 100 percent and comprises the following raw materials in percentage by weight: 25% of calcium carbonate, 25% of silicon dioxide, 30% of metal chromium powder and 20% of calcium gluconate.
Secondly, adding the permanent magnetic ferrite pre-sintering material into zirconia balls and water to a ball mill for mixing, wherein the ball milling time is 4 hours; wherein the weight ratio of the permanent magnetic ferrite pre-sintering material to the water to the zirconia balls is 1: 1.4: 11;
step three, transferring the materials ball-milled in the step two into a second-stage ball mill by using compressed air for ball milling, and adding steel balls and water into the materials, wherein the materials are as follows: steel ball: the proportion of water is 1: 1.3: 14; the ball milling process in the third step is divided into three stages: in the first stage, the rotation speed is kept at 70rpm, and ball milling is carried out for 2.5 hours; in the second stage, the rotating speed is kept at 50rpm, and the ball milling is carried out for 5.5 hours; and in the third stage, the rotation speed is kept at 55rpm, and the ball milling is finished for 5.5 hours.
Comparative example: a permanent magnetic ferrite ball milling mixing process comprises the following steps: step one, mixing iron oxide red and barium carbonate according to a mass ratio of 4:1, adding an additive after mixing, and then pre-sintering in a kiln to form a permanent magnetic ferrite pre-sintering material; the pre-sintering conditions are as follows: presintering for 60 minutes at 1250 ℃; the addition amount of the additive is 4% of the mass of the iron oxide red; the additive is 100 percent and comprises the following raw materials in percentage by weight: 25% of calcium carbonate, 25% of silicon dioxide, 30% of metal chromium powder and 20% of calcium gluconate.
Secondly, adding the permanent magnetic ferrite pre-sintering material into zirconia balls and water to a ball mill for mixing, wherein the ball milling time is 4 hours; wherein the weight ratio of the permanent magnetic ferrite pre-sintering material to the water to the zirconia balls is 1: 1.4: 11;
step three, transferring the materials ball-milled in the step two into a second-stage ball mill by using compressed air for ball milling, and adding steel balls and water into the materials, wherein the materials are as follows: steel ball: the proportion of water is 1: 1.5: 15; keeping the rotating speed at 55rpm, and performing ball milling for 5-6 hours to finish the ball milling.
The ball-milling materials prepared in examples 1 to 3 and comparative example were pressure-molded under the same conditions, sintered to prepare ferrite beads having a diameter of 20mm, and magnetic property test was performed thereon, and the test results are shown in Table 1
TABLE 1
| Item | Example 1 | Example 2 | Example 3 | Comparative example |
| Br(mT) | 429 | 426 | 420 | 389 |
| Hcb(kA/m) | 295 | 290 | 286 | 267 |
| Hcj(kA/m) | 332 | 321 | 318 | 290 |
Therefore, it can be seen that the magnetic performance of the permanent magnetic ferrite material prepared by the permanent magnetic ferrite ball milling and mixing process of the embodiments 1 to 3 is better.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that 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 (7)
1. A preparation process of a permanent magnetic ferrite ball milling mixed material is characterized by comprising the following steps: the specific process comprises the following steps: step one, mixing iron oxide red and barium carbonate according to a mass ratio of 4:1, adding an additive after mixing, and then pre-sintering in a kiln to form a permanent magnetic ferrite pre-sintering material;
secondly, adding the permanent magnetic ferrite pre-sintering material into zirconia balls and water to a ball mill for mixing, wherein the ball milling time is 3-5 hours; wherein the weight ratio of the permanent magnetic ferrite pre-sintering material to the water to the zirconia balls is (0.8-1): (1.3-1.5): (10-12);
step three, transferring the materials ball-milled in the step two into a second-stage ball mill by using compressed air for ball milling, and adding steel balls and water into the materials, wherein the materials are as follows: steel ball: the proportion of water is (0.8-1): (1.2-1.5): (13-15).
2. The preparation process of the permanent magnet ferrite ball milling mixed material according to claim 1, characterized in that: the addition amount of the additive is 3-5% of the mass of the iron oxide red.
3. The preparation process of the permanent magnet ferrite ball milling mixed material according to claim 1, characterized in that: the additive is 100 percent and comprises the following raw materials in percentage by weight: 20-30% of calcium carbonate, 20-40% of silicon dioxide, 30-45% of metal chromium powder and 20-45% of calcium gluconate.
4. The preparation process of the permanent magnet ferrite ball milling mixed material according to claim 1, characterized in that: the additive is 100 percent and comprises the following raw materials in percentage by weight: 25% of calcium carbonate, 20% of silicon dioxide, 30% of metal chromium powder and 25% of calcium gluconate.
5. The preparation process of the permanent magnet ferrite ball milling mixed material according to claim 1, characterized in that: the pre-sintering conditions in the kiln in the first step are as follows: pre-sintering at 1200-1300 ℃ for 40-80 minutes.
6. The preparation process of the permanent magnet ferrite ball milling mixed material according to claim 1, characterized in that: the diameter of the zirconia ball is 5-8 mm, and the diameter of the steel ball is 3-6 mm.
7. The preparation process of the permanent magnet ferrite ball milling mixed material according to claim 1, characterized in that: the ball milling process in the third step is divided into three stages: in the first stage, the rotating speed is kept between 60rpm and 85rpm, and ball milling is carried out for 2 to 3 hours; in the second stage, the rotating speed is kept between 35rpm and 65rpm, and ball milling is carried out for 5 to 6 hours; and in the third stage, the rotation speed is kept between 25rpm and 55rpm, and ball milling is carried out for 5 to 6 hours to complete the ball milling.
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| CN102329128A (en) * | 2011-06-11 | 2012-01-25 | 宜宾职业技术学院 | Hard calcium ferrite and manufacturing method thereof |
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