CN115745589A - Preparation method of ferrite - Google Patents
Preparation method of ferrite Download PDFInfo
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- CN115745589A CN115745589A CN202211294694.5A CN202211294694A CN115745589A CN 115745589 A CN115745589 A CN 115745589A CN 202211294694 A CN202211294694 A CN 202211294694A CN 115745589 A CN115745589 A CN 115745589A
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- ferrite
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- polyoxyethylene ether
- presintering
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002002 slurry Substances 0.000 claims abstract description 67
- 238000000227 grinding Methods 0.000 claims abstract description 50
- 239000004094 surface-active agent Substances 0.000 claims abstract description 44
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 37
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011268 mixed slurry Substances 0.000 claims abstract description 25
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000007670 refining Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 12
- 238000004945 emulsification Methods 0.000 claims description 34
- 230000000694 effects Effects 0.000 claims description 30
- 239000003607 modifier Substances 0.000 claims description 15
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 11
- 239000000839 emulsion Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 37
- 230000001804 emulsifying effect Effects 0.000 abstract description 3
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 26
- 239000002245 particle Substances 0.000 description 13
- 239000000654 additive Substances 0.000 description 10
- 238000007792 addition Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 238000000498 ball milling Methods 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000006247 magnetic powder Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Soft Magnetic Materials (AREA)
- Magnetic Ceramics (AREA)
Abstract
The invention relates to a preparation method of ferrite, which belongs to the technical field of magnetic materials and comprises the following steps: (1) The SrCO is prepared according to the mass percentage 3 ：8％‑12％，CaCO 3 ：0.5％‑3％,La 2 O 3 :1% -3%, nonionic polyoxyethylene ether fluorocarbon surfactant: 0.001% -0.01% of Fe 2 O 3 (ii) a (2) Adding the raw materials into medium water for mixing to prepare mixed slurry; (3) Refining and dispersing the mixed slurry to obtain emulsified slurry; (4) Dehydrating the emulsified slurry, presintering and then crushing to prepare presintering powder; (5) The pre-sintered powder material IIPerforming secondary fine grinding to prepare fine ground paste; (6) Pressing the fine ground slurry into a green body and sintering to obtain the ferrite. By adding the nonionic polyoxyethylene ether fluorocarbon surfactant, the emulsifying effect of the emulsifying pump in the subsequent process is enhanced, the magnetic property of the material is improved, and the magnetic property of the material is more stable.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to a preparation method of ferrite.
Background
The permanent magnetic ferrite is one of the most widely used magnetic materials at present, is a basic functional material in the contemporary society and the development thereof, and the preparation processes of the permanent magnetic ferrite basic pre-sintering material are mainly divided into two processes, namely a wet process ferrite pre-sintering material preparation process and a dry process ferrite pre-sintering material preparation process. From the perspective of improving the magnetic performance, the product obtained by the wet-process ferrite pre-sintering material preparation process has the highest magnetic performance, and the main reason is that the material refining and homogenizing effect in the wet-process ferrite pre-sintering material preparation process is the best, so that the hexagonal ferrite pre-sintering material can be fully generated by solid-phase reaction.
In the traditional wet ferrite pre-sintering material preparation process, the most widely applied thinning and homogenizing equipment is various ball mills or sand mills, the equipment has large floor area, a plurality of pipelines and high energy consumption, in the equipment, the general grinding medium is various bearing steel balls or alloy steel balls, the average abrasion loss of the steel balls in one grinding process is 5 to 10 kg per ton of material, and the abraded objects of the steel balls are mixed into the material, so that the performance of the product is inevitably reduced or unstable, particularly the product with high-grade performance requirements has stricter requirements on the components of the material. In addition, the traditional wet ball milling or sanding is adopted, the viscosity of slurry is increased after grinding and refining, the slurry residue on a grinding medium is difficult to clean, partial residue enters the next grinding process, the particle size dispersion of the slurry is large, particles with uniform particle sizes are difficult to obtain, the uniformity of the sizes of the sintered crystal particles is difficult to guarantee, and the stability of the magnetic performance of the material is influenced.
Disclosure of Invention
In order to solve the technical problems mentioned in the background art, the invention provides a preparation method of ferrite.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of ferrite comprises the following steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：8％-12％，
CaCO 3 ：0.5％-3％,
La 2 O 3 ：1％-3％，
activity modifier: 0.001 to 0.01 percent of,
the balance being Fe 2 O 3 ；
Wherein the activity modifier is a nonionic polyoxyethylene ether fluorocarbon surfactant;
(2) Adding the raw materials in the step (1) into medium water for mixing to prepare mixed slurry;
(3) Refining and dispersing the mixed slurry prepared in the step (2) through an emulsification pump to obtain emulsified slurry;
(4) Dehydrating the emulsified slurry prepared in the step (3), presintering in a high-temperature presintering furnace, and crushing to prepare presintering powder;
(5) Secondarily and finely grinding the pre-sintered powder prepared in the step (4) to prepare fine ground paste;
(6) And (5) pressing the fine ground slurry prepared in the step (5) into a green body through a forming press, and sintering to obtain the ferrite.
The activity modifier is a nonionic polyoxyethylene ether fluorocarbon surfactant, and by utilizing the excellent water solubility and good solubilization, wetting and softening properties of the surfactant, the surface tension of a system is greatly reduced, the mutual solubility and diffusion capacity among raw materials is increased, the damage of a post-process emulsification pump to a material molecular structure is reduced, and the emulsification effect of the post-process emulsification pump is enhanced; the nonionic polyoxyethylene ether fluorocarbon surfactant has high surface activity and stability, has more excellent performance than the common surfactant, can be added and used at an extremely low content to achieve the effect, and reduces the use cost.
Further, the temperature of the medium water in the step (2) is 40-60 ℃, and the temperature of the medium water is set to be not higher than 60 ℃ in consideration of the optimum effect of the activity improving agent and cost factors.
Further, the emulsification pump in the step (3) is a bipolar combined emulsification pump which is formed by connecting two single-stage six-layer horizontal emulsification pumps in series so as to directly complete the conveying, dispersing and crushing of the mixed slurry, achieve the effects of refining, homogenizing, dispersing and emulsifying and form a stable emulsion state.
Furthermore, the stator-rotor spacing range of the single-stage six-layer horizontal emulsion pump is 0.2-0.5mm, and the frequency conversion adjusting rotating speed range is 1200-2000rpm.
Further, the pre-sintering temperature range of the high-temperature pre-sintering furnace in the step (4) is 1100-1380 ℃.
Further, the secondary fine grinding procedure in the step (5) is carried out according to the mass percentageCaco by adding 0.2-1.6% 3 ，0.1％-0.6％SiO 2 ，0.1％-0.6％H 3 BO 3 ，2％-5％La 2 O 3 ，0.6％-2.5％Co 2 O 3 And 0.001% -0.005% of active modifier, the active modifier is nonionic polyoxyethylene ether fluorocarbon surfactant, utilize its dispersibility, water-solubility, reduce the reunion between the magnetic powder, utilize its detergency, make the grinding equipment of secondary fine grinding very easy to wash, reduce the residue of the supplies on the grinding medium after grinding, reduce the discreteness of the particle size, obtain the particle of the homogeneous size, guarantee the uniformity of grain size after sintering, thus make the magnetic property of the material more stable.
Further, the sintering temperature in the step (6) is 1180-1270 ℃.
The invention has the beneficial effects that:
1. the raw materials are refined and homogenized by using the bipolar combined emulsification pump, the traditional grinding equipment is replaced, the process floor area is reduced, the pipeline is simplified, the energy consumption is reduced, basically no loss object enters in the refining and homogenizing process, the stability of the material components is ensured, and the magnetic performance of the material is more stable;
2. by adding the activity modifier nonionic polyoxyethylene ether fluorocarbon surfactant, the surface tension of a raw material system is greatly reduced, the mutual solubility and the diffusion capacity among raw materials are increased, the damage of an emulsification pump to a material molecular structure is reduced, the emulsification effect of the emulsification pump in the post-process is enhanced, the problems of blockage of the emulsification pump and the like caused by the thinning viscosity increase of slurry are avoided, the thinning and homogenizing effect is improved, the solid phase reaction is more fully carried out during the high-temperature sintering of the material, and the magnetic performance of the material is improved;
3. the activity modifier nonionic polyoxyethylene ether fluorocarbon surfactant is added during secondary fine grinding, so that secondary fine grinding equipment is easy to clean, residues of materials on a grinding medium after grinding are reduced, the dispersion of particle size is reduced, particles with uniform particle size are obtained, the consistency of the size of the sintered crystal particles is ensured, and the magnetic performance of the material is more stable;
4. the selected activity modifier nonionic polyoxyethylene ether fluorocarbon surfactant has high surface activity and stability, has more excellent performance than common surfactants, can be added in an extremely low content to achieve the use effect, reduces the use cost and simultaneously reduces the influence on the material performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious 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
The embodiment provides a preparation method of ferrite, which comprises the following specific steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：9.5％，CaCO 3 ：1.2％,La 2 O 3 :2.6%, nonionic polyoxyethylene ether fluorocarbon surfactant: 0.004%, and the balance of Fe 2 O 3 ；
(2) Adding the raw materials into medium water for mixing to prepare mixed slurry; wherein the temperature of the medium water is controlled to be 45-50 ℃;
(3) Refining and dispersing the mixed slurry through a bipolar combined type emulsification pump to obtain emulsified slurry; wherein the stator-rotor spacing of the emulsification pump is 0.3mm, and the variable frequency adjustment rotating speed is 1400rpm;
(4) Dehydrating the emulsified slurry, presintering the dehydrated emulsified slurry in a high-temperature presintering furnace at 1350 ℃, and crushing the dehydrated emulsified slurry to prepare presintering powder;
(5) And performing secondary fine grinding on the pre-sintered powder, wherein the additives accounting for the mass percent of the pre-sintered powder are added in the secondary fine grinding as follows: 1.2% of CaCO 3 ，0.4％SiO 2 ,0.2％H 3 BO 3 ,3.5％La 2 O 3 ,1.2％Co 2 O 3 And 0.003% of nonionic polyoxyethylene ether fluorocarbon surfactant to prepare fine grinding slurry;
(6) Pressing the fine ground slurry into a green body by a forming press, and sintering at 1240 ℃ to obtain the ferrite.
Example 2
The embodiment provides a preparation method of ferrite, which comprises the following specific steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：10.2％，CaCO 3 ：1.8％,La 2 O 3 :1.9%, nonionic polyoxyethylene ether fluorocarbon surfactant: 0.006% and the balance of Fe 2 O 3 ；
(2) Adding the raw materials into medium water for mixing to prepare mixed slurry; wherein the temperature of the medium water is controlled at 46-52 ℃;
(3) Refining and dispersing the mixed slurry through a bipolar combined type emulsification pump to obtain emulsified slurry; wherein the stator-rotor spacing of the emulsion pump is 0.2mm, and the variable frequency regulating rotating speed is 1600rpm;
(4) Dehydrating the emulsified slurry, presintering the dehydrated emulsified slurry in a high-temperature presintering furnace at 1340 ℃, and then crushing the dehydrated emulsified slurry to prepare presintering powder;
(5) And carrying out secondary fine grinding on the pre-sintered powder, wherein the additives accounting for the mass percent of the pre-sintered powder are added in the secondary fine grinding as follows: 0.9% of CaCO 3 ，0.3％SiO 2 ,0.25％H 3 BO 3 ,3.2％La 2 O 3 ,1.3％Co 2 O 3 And 0.002% of nonionic polyoxyethylene ether fluorocarbon surfactant to prepare fine grinding slurry;
(6) Pressing the fine ground slurry into a green body by a forming press, and sintering at 1230 ℃ to obtain the ferrite.
Example 3
The embodiment provides a preparation method of ferrite, which comprises the following specific steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：11％，CaCO 3 ：2.1％,La 2 O 3 :1.5%, nonionic polyoxyethylene ether fluorocarbon surfactant: 0.009%, and the balance of Fe 2 O 3 ；
(2) Adding the raw materials into medium water and mixing to prepare mixed slurry; wherein the temperature of the medium water is controlled at 44-51 ℃;
(3) Refining and dispersing the mixed slurry through a bipolar combined type emulsification pump to obtain emulsified slurry; wherein, the stator-rotor distance of the emulsification pump is 0.4mm, and the variable frequency regulating rotating speed is 1200rpm;
(4) Dehydrating the emulsified slurry, presintering the dehydrated emulsified slurry in a high-temperature presintering furnace at 1360 ℃, and then crushing the dehydrated emulsified slurry to prepare presintering powder;
(5) And performing secondary fine grinding on the pre-sintered powder, wherein the additives accounting for the mass percent of the pre-sintered powder are added in the secondary fine grinding as follows: 0.6% of CaCO 3 ，0.25％SiO 2 ,0.15％H 3 BO 3 ,3.8％La 2 O 3 ,1.45％Co 2 O 3 And 0.005% nonionic polyoxyethylene ether fluorocarbon surfactant to prepare fine abrasive slurry;
(6) Pressing the fine ground slurry into a green body by a forming press, and sintering at 1200 ℃ to obtain the ferrite.
Example 4
The embodiment provides a preparation method of ferrite, which comprises the following specific steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：8.7％，CaCO 3 ：2.4％,La 2 O 3 :1.7%, nonionic polyoxyethylene ether fluorocarbon surfactant: 0.005% and the balance of Fe 2 O 3 ；
(2) Adding the raw materials into medium water and mixing to prepare mixed slurry; wherein the temperature of the medium water is controlled at 50-55 ℃;
(3) Refining and dispersing the mixed slurry through a bipolar combined type emulsification pump to obtain emulsified slurry; wherein the stator-rotor spacing of the emulsification pump is 0.5mm, and the variable frequency adjusting rotating speed is 1700rpm;
(4) Dehydrating the emulsified slurry, presintering the dehydrated emulsified slurry in a high-temperature presintering furnace at 1300 ℃, and then crushing the dehydrated emulsified slurry to prepare presintering powder;
(5) The pre-sintering powder is finely ground for the second time and finely ground for the second timeThe additive accounting for the mass percentage of the pre-sintering powder is added as follows: 0.5% of CaCO 3 ，0.45％SiO 2 ,0.1％H 3 BO 3 ,2.5％La 2 O 3 ,1.0％Co 2 O 3 And 0.004% nonionic polyoxyethylene ether fluorocarbon surfactant to prepare fine grinding slurry;
(6) Pressing the fine ground slurry into a green body by a forming press, and sintering at 1210 ℃ to obtain the ferrite.
Comparative example 1
The comparative example provides a preparation method of ferrite, which comprises the following specific steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：9.5％，CaCO 3 ：1.2％,La 2 O 3 :2.6 percent, and the balance of Fe 2 O 3 ；
(2) Adding the raw materials into medium water for mixing to prepare mixed slurry; wherein the temperature of the medium water is controlled at 45-50 ℃;
(3) Refining and dispersing the mixed slurry through a bipolar combined type emulsification pump to obtain emulsified slurry; wherein the stator-rotor spacing of the emulsification pump is 0.3mm, and the variable frequency adjustment rotating speed is 1400rpm;
(4) Dehydrating the emulsified slurry, presintering the dehydrated emulsified slurry in a high-temperature presintering furnace at 1350 ℃, and crushing the dehydrated emulsified slurry to prepare presintering powder;
(5) And carrying out secondary fine grinding on the pre-sintered powder, wherein the additives accounting for the mass percent of the pre-sintered powder are added in the secondary fine grinding as follows: 1.2% of CaCO 3 ，0.4％SiO 2 ,0.2％H 3 BO 3 ,3.5％La 2 O 3 ,1.2％Co 2 O 3 And 0.003% of nonionic polyoxyethylene ether fluorocarbon surfactant to prepare fine grinding slurry;
(6) Pressing the fine ground slurry into a green body by a forming press, and sintering at 1240 ℃ to obtain the ferrite.
Comparative example 1 differs from example 1 in that: in the step (1), the addition of nonionic polyoxyethylene ether fluorocarbon surfactant is omitted.
Comparative example 2
The comparative example provides a preparation method of ferrite, which comprises the following specific steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：9.5％，CaCO 3 ：1.2％,La 2 O 3 :2.6%, nonionic polyoxyethylene ether fluorocarbon surfactant: 0.004%, and the balance of Fe 2 O 3 ；
(2) Adding the raw materials into medium water for mixing to prepare mixed slurry; wherein the temperature of the medium water is controlled at 32-38 ℃;
(3) Refining and dispersing the mixed slurry through a bipolar combined type emulsification pump to obtain emulsified slurry; wherein the stator-rotor spacing of the emulsification pump is 0.3mm, and the variable frequency adjustment rotating speed is 1400rpm;
(4) Dehydrating the emulsified slurry, presintering the dehydrated emulsified slurry in a high-temperature presintering furnace at 1350 ℃, and crushing the dehydrated emulsified slurry to prepare presintering powder;
(5) And performing secondary fine grinding on the pre-sintered powder, wherein the additives accounting for the mass percent of the pre-sintered powder are added in the secondary fine grinding as follows: 1.2% of CaCO 3 ，0.4％SiO 2 ,0.2％H 3 BO 3 ,3.5％La 2 O 3 ,1.2％Co 2 O 3 And 0.003% of nonionic polyoxyethylene ether fluorocarbon surfactant to prepare fine grinding slurry;
(6) Pressing the fine ground slurry into a green body by a forming press, and sintering at 1240 ℃ to obtain the ferrite.
Comparative example 2 differs from example 1 in that: the temperature of the medium water in the step (2) is controlled to be 32-38 ℃.
Comparative example 3
The comparative example provides a preparation method of ferrite, which comprises the following specific steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：10.2％，CaCO 3 ：1.8％,La 2 O 3 :1.9%, nonionic polyoxyethylene ether fluorocarbon surfactant: 0.006% and the balance of Fe 2 O 3 ；
(2) Adding the raw materials into medium water for mixing to prepare mixed slurry; wherein the temperature of the medium water is controlled at 46-52 ℃;
(3) Refining and dispersing the mixed slurry through a ball mill to obtain emulsified slurry;
(4) Dehydrating the emulsified slurry, presintering the dehydrated emulsified slurry in a high-temperature presintering furnace at 1340 ℃, and then crushing the dehydrated emulsified slurry to prepare presintering powder;
(5) And carrying out secondary fine grinding on the pre-sintered powder, wherein the additives accounting for the mass percent of the pre-sintered powder are added in the secondary fine grinding as follows: 0.9% of CaCO 3 ，0.3％SiO 2 ,0.25％H 3 BO 3 ,3.2％La 2 O 3 ,1.3％Co 2 O 3 And 0.002% of nonionic polyoxyethylene ether fluorocarbon surfactant to prepare fine grinding slurry;
(6) Pressing the fine ground slurry into a green body by a forming press, and sintering at 1230 ℃ to obtain the ferrite.
Comparative example 3 differs from example 2 in that: and (3) grinding by using a conventional ball milling process in the step (2).
Comparative example 4
The comparative example provides a preparation method of ferrite, which comprises the following specific steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：11％，CaCO 3 ：2.1％,La 2 O 3 :1.5%, nonionic polyoxyethylene ether fluorocarbon surfactant: 0.009%, the balance being Fe 2 O 3 ；
(2) Adding the raw materials into medium water for mixing to prepare mixed slurry; wherein the temperature of the medium water is controlled at 44-51 ℃;
(3) Refining and dispersing the mixed slurry through a bipolar combined type emulsification pump to obtain emulsified slurry; wherein the stator-rotor spacing of the emulsification pump is 0.4mm, and the variable frequency adjustment rotating speed is 1200rpm;
(4) Dehydrating the emulsified slurry, presintering the dehydrated emulsified slurry in a high-temperature presintering furnace at 1360 ℃, and then crushing the dehydrated emulsified slurry to prepare presintering powder;
(5) The pre-sintering powder is finely ground for the second time, and the pre-sintering powder is added in the fine grinding for the second timeThe additives of the burnt powder material in percentage by mass are as follows: 0.6% of CaCO 3 ，0.25％SiO 2 ,0.15％H 3 BO 3 ,3.8％La 2 O 3 ,1.45％Co 2 O 3 And 0.005% nonionic polyoxyethylene ether fluorocarbon surfactant to prepare fine grinding slurry;
(6) Pressing the fine ground slurry into a green body by a forming press, and sintering at 1200 ℃ to obtain the ferrite.
Comparative example 4 differs from example 3 in that: in the step (5), the addition of the nonionic polyoxyethylene ether fluorocarbon surfactant is omitted.
Comparative example 5
The comparative example provides a preparation method of ferrite, which comprises the following specific steps:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：8.7％，CaCO 3 ：2.4％,La 2 O 3 :1.7%, phosphate type general surfactant: 0.005% and the balance of Fe 2 O 3 ；
(2) Adding the raw materials into medium water for mixing to prepare mixed slurry; wherein the temperature of the medium water is controlled at 50-55 ℃;
(3) Refining and dispersing the mixed slurry through a bipolar combined type emulsification pump to obtain emulsified slurry; wherein, the stator-rotor distance of the emulsification pump is 0.5mm, and the variable frequency regulating rotating speed is 1700rpm;
(4) Dehydrating the emulsified slurry, presintering in a high-temperature presintering furnace at 1300 ℃, and crushing to prepare presintering powder;
(5) And performing secondary fine grinding on the pre-sintered powder, wherein the additives accounting for the mass percent of the pre-sintered powder are added in the secondary fine grinding as follows: 0.5% of CaCO 3 ，0.45％SiO 2 ,0.1％H 3 BO 3 ,2.5％La 2 O 3 ,1.0％Co 2 O 3 And 0.004% nonionic polyoxyethylene ether fluorocarbon surfactant to prepare fine grinding slurry;
(6) Pressing the fine ground slurry into a green body by a forming press, and sintering at 1210 ℃ to obtain the ferrite.
Comparative example 5 differs from example 4 in that: replacing the nonionic polyoxyethylene ether fluorocarbon surfactant in the step (1) with a phosphate type common surfactant.
The ferrite products obtained in examples 1 to 4 and comparative examples 1 to 5 were tested for residual magnetism (Br), magnetic coercive force (Hcb), intrinsic coercive force (Hcj) and magnetic energy product (BH), and the test results are shown in Table 1.
TABLE 1
| Br(Gs) | Hcb(Oe) | Hcj(Oe) | (BH)max(MGOe) | |
| Example 1 | 4345 | 4078 | 4867 | 4.642 |
| Example 2 | 4360 | 4057 | 4728 | 4.653 |
| Example 3 | 4382 | 4090 | 4829 | 4.691 |
| Example 4 | 4431 | 4124 | 4962 | 4.782 |
| Comparative example 1 | 4219 | 3957 | 4512 | 4.341 |
| Comparative example 2 | 4302 | 4021 | 4679 | 4.474 |
| Comparative example 3 | 4342 | 4038 | 4781 | 4.642 |
| Comparative example 4 | 4349 | 4058 | 4712 | 4.651 |
| Comparative example 5 | 4242 | 3981 | 4639 | 4.382 |
Conclusion analysis:
the difference between the comparative example 1 and the example 1 is that the addition of the nonionic polyoxyethylene ether fluorocarbon surfactant is omitted in the step (1), the nonionic polyoxyethylene ether fluorocarbon surfactant can greatly reduce the surface tension of a raw material system, increase the mutual solubility and the diffusion capacity among raw materials, improve the refining and homogenizing effects and reduce the viscosity of slurry, and from the data result, the performance of each parameter in a finished product after the omission is greatly reduced relative to that in the example 1;
the difference between the comparative example 2 and the example 1 is that the temperature of the medium water in the step (2) is controlled to be 32-38 ℃, the non-ionic polyoxyethylene ether fluorocarbon surfactant selected by the invention has the phenomenon of liquid phase separation under the condition of lower temperature, the activity is lower, the effect is poorer, and the data result shows that each parameter in the finished product has the performance reduction relative to the example 1;
the difference between the comparative example 3 and the example 2 is that the conventional ball milling process is used for grinding in the step (2), and when the conventional ball milling process is used for grinding, grinding medium abradants enter the slurry to influence the material components and further influence the material performance, and from the data result, each parameter in the finished product of the conventional process is reduced relative to the performance of the example 2;
the difference between the comparative example 4 and the example 3 is that the addition of the nonionic polyoxyethylene ether fluorocarbon surfactant is omitted in the secondary fine grinding in the step (4), the material on the grinding medium after grinding has more residues, the dispersion of the particle size is large, the particle size is not uniform, the uniformity of the grain size after sintering is poor, the magnetic performance of the material is reduced or unstable, and the data result shows that each parameter in the finished product is reduced relative to the performance of the example 3;
the difference between the comparative example 5 and the example 4 is that the nonionic polyoxyethylene ether fluorocarbon surfactant in the step (1) is replaced by a phosphate type common surfactant, and a common surfactant additive is selected, so that the activity of the raw material is increased to a small extent, the surface tension between systems cannot be greatly reduced, the viscosity of the emulsified slurry is high, the dispersion homogenization effect is reduced, the magnetic performance of the material is reduced or unstable, and the performance of each parameter in the finished product is greatly reduced compared with that in the example 4.
In conclusion, the active modifier nonionic polyoxyethylene ether fluorocarbon surfactant is added into the raw materials and the secondary fine grinding, so that the surface tension of a raw material system is greatly reduced, the mutual solubility and the diffusion capacity of the raw materials are improved, the damage of an emulsification pump to a material molecular structure is reduced, the emulsification effect of the emulsification pump in the subsequent process is enhanced, the refining homogenization effect is improved, the dispersion of particle size is reduced, the solid phase reaction is more fully performed during high-temperature sintering of the material, and the magnetic performance of a finished material is greatly improved.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The preparation method of the ferrite is characterized by comprising the following steps of:
(1) The raw materials are as follows according to the mass percentage:
SrCO 3 ：8％-12％，
CaCO 3 ：0.5％-3％,
La 2 O 3 ：1％-3％，
activity modifier: 0.001 to 0.01 percent of,
the balance being Fe 2 O 3 ；
Wherein the activity modifier is a nonionic polyoxyethylene ether fluorocarbon surfactant;
(2) Adding the raw materials in the step (1) into medium water for mixing to prepare mixed slurry;
(3) Refining and dispersing the mixed slurry prepared in the step (2) through an emulsification pump to obtain emulsified slurry;
(4) Dehydrating the emulsified slurry prepared in the step (3), presintering in a high-temperature presintering furnace, and crushing to prepare presintering powder;
(5) Secondarily and finely grinding the pre-sintered powder prepared in the step (4) to prepare fine ground paste;
(6) And (6) pressing the fine ground paste prepared in the step (5) into a green body through a forming press, and sintering to obtain the ferrite.
2. The preparation method of the ferrite according to claim 1, wherein the raw materials in the step (1) are as follows by mass percent:
SrCO 3 ：8.5％-11.5％，
CaCO 3 ：0.5％-2.5％,
La 2 O 3 ：1.5％-3％，
activity modifier: 0.002% -0.009%,
the balance being Fe 2 O 3 ；
Wherein the activity modifier is nonionic polyoxyethylene ether fluorocarbon surfactant.
3. The method for preparing ferrite as claimed in claim 1, wherein the temperature of the medium water in the step (2) is 40-60 ℃.
4. The method as claimed in claim 1, wherein the emulsification pump in step (3) is a bipolar combination emulsification pump consisting of two single-stage six-layer horizontal emulsification pumps connected in series.
5. The method for preparing ferrite according to claim 4, wherein the stator-rotor spacing range of the single-stage six-layer horizontal emulsion pump is 0.2-0.5mm, and the frequency conversion regulation rotating speed range is 1200-2000rpm.
6. The method as claimed in claim 1, wherein the pre-firing temperature of the high temperature pre-firing furnace in the step (4) is in a range of 1100 to 1380 ℃.
7. The method as claimed in claim 1, wherein the secondary fine grinding in step (5) is carried out by adding 0.2% -1.6% by mass of CaCO 3 ，0.1％-0.6％SiO 2 ，0.1％-0.6％H 3 BO 3 ，2％-5％La 2 O 3 ，0.6％-2.5％Co 2 O 3 And 0.001% -0.005% of activity modifier, wherein the activity modifier is nonionic polyoxyethylene ether fluorocarbon surfactant.
8. The method as claimed in claim 6, wherein the sintering temperature in step (6) is 1180-1270 ℃.
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