CN112500148A - Preparation method of high-coercivity strontium ferrite magnetic material - Google Patents
Preparation method of high-coercivity strontium ferrite magnetic material Download PDFInfo
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- CN112500148A CN112500148A CN202011352051.2A CN202011352051A CN112500148A CN 112500148 A CN112500148 A CN 112500148A CN 202011352051 A CN202011352051 A CN 202011352051A CN 112500148 A CN112500148 A CN 112500148A
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- carboxymethyl starch
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- ferrite magnetic
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 40
- 239000000696 magnetic material Substances 0.000 title claims abstract description 35
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 33
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical class O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000002002 slurry Substances 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000000654 additive Substances 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 17
- 230000000996 additive effect Effects 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 10
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 239000005995 Aluminium silicate Substances 0.000 claims description 57
- 235000012211 aluminium silicate Nutrition 0.000 claims description 57
- 229920002472 Starch Polymers 0.000 claims description 51
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 51
- 235000019698 starch Nutrition 0.000 claims description 51
- 239000008107 starch Substances 0.000 claims description 51
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000012065 filter cake Substances 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- 238000009830 intercalation Methods 0.000 claims description 14
- 230000002687 intercalation Effects 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 7
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Inorganic materials [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 238000001179 sorption measurement Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of a high-coercivity strontium ferrite magnetic material, which comprises the following steps: s1, weighing Fe2O3Powder, SrCO3Uniformly mixing the powder to obtain a premix; s2, uniformly mixing the premix and the modified kaolin additive, and then adding water for ball milling to obtain primary slurry; s3, drying the primary slurry, pre-burning at 1300-1320 ℃, cooling and crushing to obtain a primary pre-burned material; s4, adding water into the primary pre-sintered material and carrying out ball milling to obtain secondary slurry; s5, carrying out wet pressing magnetic field forming on the secondary slurry to obtain a blank; s6, sintering the blank at 1240-1260 ℃, and cooling to obtain the product. The strontium ferrite magnetic material prepared by the invention has high coercivity and high remanence performance, and is a permanent magnetic material with excellent performance.
Description
Technical Field
The invention relates to the technical field of ferrite magnetic materials, in particular to a preparation method of a high-coercivity strontium ferrite magnetic material.
Background
The permanent magnetic material is a magnetic body which can still keep a magnetic field outwards after a magnetization field is removed, can be applied to the fields of computers, communication, electrical electronics, energy power and the like, and has irreplaceable functions as a core material of various magnetic energy devices. The ferrite permanent magnet material has the advantages of rich raw material sources, low cost, stable chemical property, good abrasion resistance, higher coercive force, larger saturation magnetization and good magnetocrystalline anisotropy, and is the most widely applied permanent magnet material at present. With the continuous development of the technology, higher and higher requirements are also put forward on the performance of the permanent magnetic material. In order to meet the trend of miniaturization, high precision and large capacity of devices, it is necessary to improve the coercive force of a ferrite magnetic material and to have high remanence.
At present, the method for improving the coercive force of the permanent magnetic ferrite is mainly to add alumina, chromic oxide and kaolin as additives singly or in a mixing way in the ball milling process of the ferrite. A certain amount of addition is usually required for the purpose of significantly increasing the coercive force, but as the content of these additives increases, the nonmagnetic phase increases, resulting in a decrease in remanence. Therefore, for ferrite magnetic materials, how to combine high coercivity and high remanence becomes a key and difficult point for developing new materials.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of a high-coercivity strontium ferrite magnetic material.
The invention provides a preparation method of a high-coercivity strontium ferrite magnetic material, which comprises the following steps:
s1, according to the mol ratio (5.9-6.1): 1 weighing Fe2O3Powder, SrCO3Uniformly mixing the powder to obtain a premix;
s2, mixing the premix and the modified kaolin additive according to the mass ratio of 100: (0.5-0.8), uniformly mixing, adding water, and ball-milling to obtain primary slurry;
s3, drying the primary slurry, pre-burning at 1300-1320 ℃, cooling and crushing to obtain a primary pre-burned material;
s4, adding water into the primary pre-sintered material and performing ball milling to obtain secondary slurry;
s5, carrying out wet pressing magnetic field forming on the secondary slurry to obtain a blank;
s6, sintering the blank at 1240-1260 ℃, and cooling to obtain the high-coercivity strontium ferrite magnetic material;
preparation of the modified kaolin additiveThe preparation method comprises the following steps: firstly, carboxymethyl starch is used as an intercalation agent to carry out intercalation modification on kaolin to obtain carboxymethyl starch intercalation kaolin, and then Cr is added3+、Al3+Loading on the carboxymethyl starch intercalated kaolin to obtain the carboxymethyl starch intercalated kaolin.
Preferably, the method for preparing the modified kaolin additive comprises the following steps:
(1) uniformly dispersing kaolin in dimethyl sulfoxide, stirring and reacting at 70-90 ℃ for 20-30h, then filtering, dispersing the obtained filter cake in water, adding carboxymethyl starch, stirring and reacting at 70-90 ℃ for 10-15h, filtering again, washing and drying the obtained filter cake to obtain carboxymethyl starch intercalated kaolin;
(2) mixing Cr (NO)3)3、Al(NO3)3Fully dissolving in water, adding the carboxymethyl starch intercalated kaolin for oscillation adsorption, filtering, and drying the obtained filter cake to obtain the carboxymethyl starch intercalated kaolin.
Preferably, in the step (1), the mass ratio of the kaolin to the carboxymethyl starch is (4-6): 1, the ratio of kaolin to dimethyl sulfoxide is 1 g: (5-20) mL.
Preferably, in the step (2), the carboxymethyl starch intercalated kaolin is mixed with Cr (NO)3)3The mass ratio of (A) to (B) is 100: (10-15), carboxymethyl starch intercalated Kaolin with Al (NO)3)3The mass ratio of (A) to (B) is 100: (5-10).
Preferably, in the step (2), the conditions for oscillating adsorption are as follows: at 40-50 deg.C, pH 6-6.5, and time 3-5 h.
Preferably, in the step S3, the burn-in time is 7-9 h; in the step S6, the sintering time is 3-5 h.
Preferably, in the step S2, the ball milling is performed until the particle size is 1 to 1.5 μm, and in the step S4, the ball milling is performed until the particle size is 0.8 to 1 μm.
A strontium ferrite magnetic material with high coercivity is prepared by the preparation method.
The invention has the following beneficial effects:
the invention firstly uses carboxymethyl starch as an intercalating agent to carry out intercalation modification on kaolinTo obtain carboxymethyl starch intercalated kaolin, and then adding Cr3+、Al3+The carboxymethyl starch intercalation kaolin is loaded on the carboxymethyl starch intercalation kaolin, is used as an additive and is added into a strontium ferrite material in the ball milling process. The intercalation modification of the carboxymethyl starch can ensure that the kaolin is subjected to interlayer peeling and is more uniformly dispersed in the strontium ferrite slurry, and the carboxymethyl starch has a certain dispersing effect and can further improve the dispersing effect of the kaolin; moreover, because the kaolin is in a stripping state and has a better bonding interface with the strontium ferrite slurry, the dispersity and the bonding property of the kaolin doped in the slurry are improved, so that uniform eutectic can be generated on the surface of the crystal grain under the condition of reducing the addition amount, the crystal grain is refined better, and the intrinsic coercive force is improved; trace amount of Cr3+、Al3+The magnetic powder is uniformly loaded on carboxymethyl starch intercalated kaolin through adsorption, can participate in solid phase reaction to a certain extent, enters a permanent magnetic ferrite lattice, and also has the functions of inhibiting the growth of crystal grains and reducing the coercive force. Because the content of the additive is relatively low and the content of the nonmagnetic phase in the magnet is also correspondingly low, the strontium ferrite permanent magnet material prepared by the invention can have high remanence (Br) and high coercivity (Hcj) and has excellent magnetic property.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a high-coercivity strontium ferrite magnetic material comprises the following steps:
s1, according to the mol ratio (5.9-6.1): 1 weighing Fe2O3Powder, SrCO3Uniformly mixing the powder to obtain a premix;
s2, mixing the premix and the modified kaolin additive according to the mass ratio of 100: (0.5-0.8), uniformly mixing, adding water, and ball-milling to obtain primary slurry;
s3, drying the primary slurry, pre-burning at 1300-1320 ℃, cooling and crushing to obtain a primary pre-burned material;
s4, adding water into the primary pre-sintered material and performing ball milling to obtain secondary slurry;
s5, carrying out wet pressing magnetic field forming on the secondary slurry to obtain a blank;
s6, sintering the blank at 1240-1260 ℃, and cooling to obtain the high-coercivity strontium ferrite magnetic material;
the preparation method of the modified kaolin additive comprises the following steps: firstly, carboxymethyl starch is used as an intercalation agent to carry out intercalation modification on kaolin to obtain carboxymethyl starch intercalation kaolin, and then Cr is added3+、Al3+Loading on the carboxymethyl starch intercalated kaolin to obtain the carboxymethyl starch intercalated kaolin.
Example 2
A preparation method of a high-coercivity strontium ferrite magnetic material comprises the following steps:
s1, mixing the raw materials in a molar ratio of 6.05: 1 weighing Fe2O3Powder, SrCO3Uniformly mixing the powder to obtain a premix;
s2, mixing the premix and the modified kaolin additive according to the mass ratio of 100: 0.65, adding water, and ball-milling until the granularity is 1-1.5 mu m to obtain primary slurry;
s3, drying the primary slurry, pre-burning for 8 hours at 1310 ℃, cooling and crushing to obtain a primary pre-burned material;
s4, adding water into the primary pre-sintered material, and ball-milling until the particle size is 0.8-1 mu m to obtain secondary slurry;
s5, carrying out wet pressing magnetic field forming on the secondary slurry to obtain a blank;
s6, sintering the blank at 1255 ℃ for 4h, and cooling to obtain the high-coercivity strontium ferrite magnetic material;
the preparation method of the modified kaolin additive comprises the following steps:
(1) uniformly dispersing kaolin in dimethyl sulfoxide, stirring and reacting for 25 hours at 80 ℃, then filtering, dispersing the obtained filter cake in water, adding carboxymethyl starch, stirring and reacting for 12 hours at 80 ℃, filtering again, washing and drying the obtained filter cake to obtain carboxymethyl starch intercalated kaolin, wherein the mass ratio of the kaolin to the carboxymethyl starch is 5: 1, the ratio of kaolin to dimethyl sulfoxide is 1 g: 15 mL;
(2) mixing Cr (NO)3)3、Al(NO3)3Fully dissolving in water, adding the carboxymethyl starch intercalated kaolin, oscillating and adsorbing for 4 hours at 45 ℃ under the condition that the pH value is 6.2, filtering, and drying the obtained filter cake to obtain the carboxymethyl starch intercalated kaolin and Cr (NO)3)3The mass ratio of (A) to (B) is 100: 12, inserting carboxymethyl starch into kaolin and Al (NO)3)3The mass ratio of (A) to (B) is 100: 8.
example 3
A preparation method of a high-coercivity strontium ferrite magnetic material comprises the following steps:
s1, and the molar ratio is 5.9: 1 weighing Fe2O3Powder, SrCO3Uniformly mixing the powder to obtain a premix;
s2, mixing the premix and the modified kaolin additive according to the mass ratio of 100: 0.5, mixing uniformly, adding water, and ball-milling until the granularity is 1-1.5 mu m to obtain primary slurry;
s3, drying the primary slurry, pre-burning for 9 hours at 1300 ℃, cooling and crushing to obtain a primary pre-burned material;
s4, adding water into the primary pre-sintered material, and ball-milling until the particle size is 0.8-1 mu m to obtain secondary slurry;
s5, carrying out wet pressing magnetic field forming on the secondary slurry to obtain a blank;
s6, sintering the blank at 1240 ℃ for 5h, and cooling to obtain the high-coercivity strontium ferrite magnetic material;
the preparation method of the modified kaolin additive comprises the following steps:
(1) uniformly dispersing kaolin in dimethyl sulfoxide, stirring and reacting for 30 hours at 70 ℃, then filtering, dispersing the obtained filter cake in water, adding carboxymethyl starch, stirring and reacting for 15 hours at 70 ℃, filtering again, washing and drying the obtained filter cake to obtain carboxymethyl starch intercalated kaolin, wherein the mass ratio of the kaolin to the carboxymethyl starch is 4: 1, the ratio of kaolin to dimethyl sulfoxide is 1 g: 5 mL;
(2) mixing Cr (NO)3)3、Al(NO3)3Fully dissolving in water, adding the carboxymethyl starch intercalated kaolin, oscillating and adsorbing for 5h at 40 ℃ under the condition that the pH value is 6, filtering, and drying the obtained filter cake to obtain the carboxymethyl starch intercalated kaolin and Cr (NO)3)3The mass ratio of (A) to (B) is 100: 10, intercalation of carboxymethyl starch with Al (NO)3)3The mass ratio of (A) to (B) is 100: 5.
example 4
A preparation method of a high-coercivity strontium ferrite magnetic material comprises the following steps:
s1, mixing the raw materials in a molar ratio of 6.1: 1 weighing Fe2O3Powder, SrCO3Uniformly mixing the powder to obtain a premix;
s2, mixing the premix and the modified kaolin additive according to the mass ratio of 100: 0.8, mixing uniformly, adding water, and ball-milling until the granularity is 1-1.5 mu m to obtain primary slurry;
s3, drying the primary slurry, pre-burning for 7 hours at 1320 ℃, cooling and crushing to obtain a primary pre-burned material;
s4, adding water into the primary pre-sintered material, and ball-milling until the particle size is 0.8-1 mu m to obtain secondary slurry;
s5, carrying out wet pressing magnetic field forming on the secondary slurry to obtain a blank;
s6, sintering the blank at 1260 ℃ for 3h, and cooling to obtain the high-coercivity strontium ferrite magnetic material;
the preparation method of the modified kaolin additive comprises the following steps:
(1) uniformly dispersing kaolin in dimethyl sulfoxide, stirring and reacting for 20 hours at 90 ℃, then filtering, dispersing the obtained filter cake in water, adding carboxymethyl starch, stirring and reacting for 10 hours at 90 ℃, filtering again, washing and drying the obtained filter cake to obtain carboxymethyl starch intercalated kaolin, wherein the mass ratio of the kaolin to the carboxymethyl starch is 6: 1, the ratio of kaolin to dimethyl sulfoxide is 1 g: 20 mL;
(2) mixing Cr (NO)3)3、Al(NO3)3Fully dissolving in water, adding the carboxymethyl starch intercalated kaolin, oscillating and adsorbing for 3h at 50 ℃ under the condition that the pH value is 6.5, filtering, and drying the obtained filter cake to obtain the carboxymethyl starch intercalated kaolin and Cr (NO)3)3The mass ratio of (A) to (B) is 100: 15, carboxymethyl starch intercalated Kaolin with Al (NO)3)3The mass ratio of (A) to (B) is 100: 10.
the magnetic properties of the strontium ferrite magnetic materials prepared in examples 2 to 4 were measured using a permanent magnet automatic measuring instrument, and the results are shown in table 1.
TABLE 1 magnetic Properties of strontium ferrite magnetic materials
| Example 2 | Example 3 | Example 4 | |
| Br(mT) | 421 | 424 | 412 |
| Hcj(KA/m) | 325 | 320 | 328 |
As can be seen from table 1, the strontium ferrite magnetic material of the present invention not only has high coercivity, but also can maintain high remanence performance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A preparation method of a high-coercivity strontium ferrite magnetic material is characterized by comprising the following steps:
s1, according to the mol ratio (5.9-6.1): 1 weighing Fe2O3Powder, SrCO3Uniformly mixing the powder to obtain a premix;
s2, mixing the premix and the modified kaolin additive according to the mass ratio of 100: (0.5-0.8), uniformly mixing, adding water, and ball-milling to obtain primary slurry;
s3, drying the primary slurry, pre-burning at 1300-1320 ℃, cooling and crushing to obtain a primary pre-burned material;
s4, adding water into the primary pre-sintered material and performing ball milling to obtain secondary slurry;
s5, carrying out wet pressing magnetic field forming on the secondary slurry to obtain a blank;
s6, sintering the blank at 1240-1260 ℃, and cooling to obtain the high-coercivity strontium ferrite magnetic material;
the preparation method of the modified kaolin additive comprises the following steps: firstly, carboxymethyl starch is used as an intercalation agent to carry out intercalation modification on kaolin to obtain carboxymethyl starch intercalation kaolin, and then Cr is added3+、Al3+Loading on the carboxymethyl starch intercalated kaolin to obtain the carboxymethyl starch intercalated kaolin.
2. The method for preparing a high coercivity strontium ferrite magnetic material according to claim 1, wherein the modified kaolin additive is prepared by the steps of:
(1) uniformly dispersing kaolin in dimethyl sulfoxide, stirring and reacting at 70-90 ℃ for 20-30h, then filtering, dispersing the obtained filter cake in water, adding carboxymethyl starch, stirring and reacting at 70-90 ℃ for 10-15h, filtering again, washing and drying the obtained filter cake to obtain carboxymethyl starch intercalated kaolin;
(2) mixing Cr (NO)3)3、Al(NO3)3Fully dissolving in water, adding the carboxymethyl starch intercalated kaolin for oscillation adsorption, filtering, and drying the obtained filter cake to obtain the carboxymethyl starch intercalated kaolin.
3. The method for preparing a high coercive force strontium ferrite magnetic material according to claim 2, wherein in the step (1), the mass ratio of kaolin to carboxymethyl starch is (4-6): 1, the ratio of kaolin to dimethyl sulfoxide is 1 g: (5-20) mL.
4. The method for preparing a high coercivity strontium ferrite magnetic material according to claim 2 or 3, wherein in step (2), carboxymethyl starch intercalated kaolin and Cr (NO) are added3)3The mass ratio of (A) to (B) is 100: (10-15), carboxymethyl starch intercalated Kaolin with Al (NO)3)3The mass ratio of (A) to (B) is 100: (5-10).
5. The method for preparing a high coercivity strontium ferrite magnetic material according to any one of claims 2 to 4, wherein in step (2), the oscillation adsorption conditions are as follows: at 40-50 deg.C, pH 6-6.5, and time 3-5 h.
6. The method for preparing a high coercive force strontium ferrite magnetic material according to any one of claims 1 to 5, wherein in the step S3, the pre-sintering time is 7 to 9 hours; in the step S6, the sintering time is 3-5 h.
7. The method for preparing a high coercivity strontium ferrite magnetic material according to any one of claims 1 to 6, wherein the step S2 is ball milled to a particle size of 1-1.5 μm, and the step S4 is ball milled to a particle size of 0.8-1 μm.
8. A high coercivity strontium ferrite magnetic material, obtainable by the process of any one of claims 1 to 7.
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