CN115368125A - Manganese-zinc soft magnetic ferrite material with high breaking strength and manufacturing method thereof - Google Patents
Manganese-zinc soft magnetic ferrite material with high breaking strength and manufacturing method thereof Download PDFInfo
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Abstract
The invention develops a high-breaking-strength manganese-zinc soft magnetic ferrite material and a manufacturing method thereof, and the manganese-zinc soft magnetic ferrite material is sintered for 2 times, the binding force of the manganese-zinc soft magnetic ferrite is improved by a polyvinyl alcohol aqueous solution and a modified starch aqueous solution, and the adhesion of the modified starch is improved by high-temperature and high-pressure water vapor in a sintering section, so that the effect of improving the strength of the manganese-zinc soft magnetic ferrite is achieved.
Description
Technical Field
The invention relates to a preparation process of a soft magnetic ferrite material, in particular to a manganese-zinc soft magnetic ferrite material with high breaking strength and a manufacturing method thereof.
Background
The soft magnetic ferrite material is Fe 2 O 3 The ferrimagnetic oxide as the main component is produced by a powder metallurgy method. The method comprises the following steps of Mn-Zn, cu-Zn, ni-Zn and the like, wherein the Mn-Zn ferrite material has the largest yield and the largest dosage, and the Mn-Zn ferrite material has low resistivity of 1-10 ohm/mAnd is generally used at a frequency of 100kHZ or less.
With the rapid upgrade and update of electronic products, the miniaturization, the compaction caused by high packaging density and the like have become the development trend of electronic products, which inevitably requires that the fit clearance between a magnetic core and a coil framework is smaller and smaller, the structure is more compact, the stress of the magnetic core on the coil framework is larger and larger, and the soft magnetic ferrite material has the defect of brittleness in physical characteristics as the ceramic material, so how to ensure that the product has better strength after miniaturization, so as to ensure the performance stability and the service life of the product under various complex environments, and the anti-beating and anti-collision capabilities in the processes of transportation, installation and the like are the problems which must be solved under the trend of the miniaturization and the compaction of the electronic products.
Disclosure of Invention
The invention develops a high-breaking-strength manganese-zinc soft magnetic ferrite material and a manufacturing method thereof, and the manganese-zinc soft magnetic ferrite material is sintered for 2 times, the binding force of the manganese-zinc soft magnetic ferrite is improved by a polyvinyl alcohol aqueous solution and a modified starch aqueous solution, and the adhesion of the modified starch is improved by high-temperature and high-pressure water vapor in a sintering section, so that the effect of improving the strength of the manganese-zinc soft magnetic ferrite is achieved.
A manufacturing method of a high flexural strength manganese-zinc soft magnetic ferrite material comprises the following specific steps:
(1) Primary burdening: the mole fraction of the massage is Fe 2 O 3 :65-70 parts, mnO:25-28 parts of ZnO:18-20 parts of materials are mixed;
(2) Primary ball milling: uniformly mixing the raw materials weighed in the step (1), adding a polyvinyl alcohol aqueous solution with the mass of 10-15wt% of the powder, carrying out high-speed ball milling at 8000-10000rpm for 40-60min, and carrying out spray drying to obtain granular powder A;
(3) Pre-burning: putting the granular powder A prepared in the step (2) in N 2 Heating to 500-550 deg.C in atmosphere, maintaining for 1-2h, and adding 1-3% oxygen in volume 2 Heating to 900-930 deg.C in atmosphere, maintaining for 1-2h, and adding N 2 Cooling in the atmosphere to prepare a pre-sintered material;
(4) Secondary burdening: weighing V which is 1.0-1.5wt% of the pre-sintering material 2 O 3 0.5 to 1.0 weight percent of CuO and 0.5 to 0.8 weight percent of CaCO 3 0.03 to 0.05wt% of Nb 2 O 5 0.02-0.05wt% MoO;
(5) Secondary ball milling: uniformly mixing the raw materials weighed in the step (4) with the pre-sintering material prepared in the step (3), adding a modified starch aqueous solution with the mass of 20-30% of the powder, carrying out high-speed ball milling at 8000-10000rpm for 20-30min, and carrying out spray drying to obtain granular powder B;
(6) And (3) pressing and forming: adding the granular powder B obtained in the step (5) into a forming die, and pressing and forming by using a full-automatic dry press;
(7) And (3) sintering: firstly, introducing high-temperature high-pressure steam, and preserving heat for 2-3h; then in N 2 Heating to 500-550 ℃ under the atmosphere, keeping the temperature for 1-2h, continuing heating to 900-950 ℃, and keeping the temperature for 1-2h; then 3-5% oxygen volume content of N 2 Heating to 1250-1300 deg.C in atmosphere, keeping the temperature for 4-6h, and finally adding N 2 And cooling in the atmosphere to prepare the MnZn soft magnetic ferrite material.
Further, the preparation method of the polyvinyl alcohol aqueous solution in the step (2) comprises the following steps:
heating purified water to 85-90 ℃, then adding polyethylene glycol accounting for 2% of the mass of the purified water and sodium lignosulfonate accounting for 0.5%, stirring and dissolving uniformly, adding PVA17-88 accounting for 8% of the mass of the purified water, stirring and dissolving, and cooling to room temperature to obtain the polyvinyl alcohol aqueous solution.
Further, the polyethylene glycol is PEG-2000.
Further, the preparation method of the modified starch aqueous solution in the step (5) comprises the following steps:
heating purified water to 65-75 ℃, then adding waxy corn amylopectin with the mass of 0.1-0.3% of that of the purified water, then adding potassium permanganate with the mass of 0.3-0.5% of that of the purified water, stirring until the mixture is uniformly gelatinized, then cooling, cooling to-5-0 ℃ by using an ice salt bath, dropwise adding benzenesulfonyl chloride with the volume of 1-3% of that of the purified water, reacting for 3-5h, and then performing freeze drying and ethanol washing to obtain modified starch; and dissolving the modified starch in warm water 200 times the mass of the modified starch to prepare a modified starch aqueous solution.
Further, the high-temperature and high-pressure water vapor in the step (7) is water vapor with the pressure of 1.5MPa and the temperature of 200 ℃.
The invention has the advantages that: according to the invention, the strength of the manganese-zinc soft magnetic ferrite can be effectively improved through 2 times of sintering; meanwhile, the binding force of the manganese-zinc soft magnetic ferrite is improved through the polyvinyl alcohol aqueous solution and the modified starch aqueous solution, so that the effect of improving the strength of the manganese-zinc soft magnetic ferrite is achieved; meanwhile, the adhesion of the modified starch is improved by high-temperature and high-pressure steam in the sintering section, so that the strength of the manganese-zinc soft magnetic ferrite can be effectively improved.
Drawings
FIG. 1 is a schematic diagram of the EE magnetic core strength test of the invention.
Detailed Description
Example 1
A manufacturing method of a high flexural strength manganese-zinc soft magnetic ferrite material comprises the following specific steps:
(1) Primary material preparation: the mole fraction of the massage is Fe 2 O 3 :65 parts, mnO:28 parts and ZnO: 18. proportioning;
(2) Primary ball milling: uniformly mixing the raw materials weighed in the step (1), adding a polyvinyl alcohol aqueous solution with the mass of 10wt% of the powder, carrying out high-speed ball milling at 10000rpm for 40min, and carrying out spray drying to obtain granular powder A;
(3) Pre-burning: putting the granular powder A prepared in the step (2) in N 2 Heating to 500 deg.C in atmosphere, keeping the temperature for 2h, and adding 1% oxygen in volume 2 Heating to 930 deg.C in atmosphere, maintaining for 1h, and finally maintaining in N 2 Cooling in the atmosphere to prepare a pre-sintered material;
(4) Secondary burdening: weighing V corresponding to 1.0wt% of the pre-sintering material 2 O 3 1.0wt% of CuO, 0.5wt% of CaCO 3 0.03wt% of Nb 2 O 5 0.02wt% MoO;
(5) Secondary ball milling: uniformly mixing the raw materials weighed in the step (4) with the pre-sintering material prepared in the step (3), adding a modified starch aqueous solution with the mass of 20% of that of the powder, performing high-speed ball milling at 10000rpm for 20min, and performing spray drying to obtain granular powder B;
(6) And (3) pressing and forming: adding the granular powder B obtained in the step (5) into a forming die, and pressing and forming by using a full-automatic dry press;
(7) And (3) sintering: firstly, introducing high-temperature high-pressure steam with the pressure of 1.5MPa and the temperature of 200 ℃, and preserving heat for 2 hours; then in N 2 Heating to 500 ℃ in the atmosphere, keeping the temperature for 2h, then continuing heating to 900 ℃, and keeping the temperature for 2h; then N with 3% volume content of oxygen 2 Raising the temperature to 1250 ℃ under the atmosphere, preserving the heat for 6 hours, and finally, adding N 2 And cooling in the atmosphere to prepare the MnZn soft magnetic ferrite material.
The preparation method of the polyvinyl alcohol aqueous solution in the step (2) comprises the following steps:
heating purified water to 85 ℃, adding PEG-2000 accounting for 2% of the mass of the purified water and sodium lignosulfonate accounting for 0.5%, stirring and dissolving uniformly, adding PVA17-88 accounting for 8% of the mass of the purified water, stirring and dissolving, and cooling to room temperature to obtain the polyvinyl alcohol aqueous solution.
The preparation method of the modified starch aqueous solution in the step (5) comprises the following steps:
heating purified water to 65 ℃, adding waxy corn amylopectin with the mass of 0.1% of that of the purified water, adding potassium permanganate with the mass of 0.3% of that of the purified water, stirring until the mixture is uniformly gelatinized, cooling to-5 ℃ by using an ice salt bath, dropwise adding benzenesulfonyl chloride with the volume of 1% of that of the purified water, reacting for 3 hours, and performing freeze drying and ethanol washing to obtain modified starch; the modified starch prepared above is dissolved in warm water 200 times the mass of the starch to prepare a modified starch aqueous solution.
Example 2
A manufacturing method of a high flexural strength manganese-zinc soft magnetic ferrite material comprises the following specific steps:
(1) Primary burdening: the mole fraction of the massage is Fe 2 O 3 :66 parts and MnO:26 parts and ZnO: 18. proportioning;
(2) Primary ball milling: uniformly mixing the raw materials weighed in the step (1), adding a polyvinyl alcohol aqueous solution with the weight of 12wt% of the powder, carrying out high-speed ball milling at 10000rpm for 60min, and carrying out spray drying to obtain granular powder A;
(3) Pre-burning: putting the granular powder A prepared in the step (2) in N 2 Heating to 520 ℃ in the atmosphere, preserving the heat for 2h, and then adding 2% oxygen volume content of N 2 Heating to 910 deg.C under atmosphere, keeping the temperature for 2h, and finally adding N 2 Cooling in the atmosphere to prepare a pre-sintered material;
(4) Secondary burdening: weighing V corresponding to 1.2wt% of the pre-sintering material 2 O 3 0.6wt% of CuO, 0.5wt% of CaCO 3 0.04wt% of Nb 2 O 5 0.03wt% MoO;
(5) Secondary ball milling: uniformly mixing the raw materials weighed in the step (4) with the pre-sintering material prepared in the step (3), adding a modified starch aqueous solution with the powder mass of 22%, performing high-speed ball milling at 10000rpm for 30min, and performing spray drying to obtain granular powder B;
(6) And (3) compression molding: adding the granular powder B obtained in the step (5) into a forming die, and pressing and forming by using a full-automatic dry press;
(7) And (3) sintering: firstly, introducing high-temperature and high-pressure steam with the pressure of 1.5MPa and the temperature of 200 ℃, and preserving heat for 3 hours; then in N 2 Heating to 520 ℃ under the atmosphere, keeping the temperature for 2h, then continuing heating to 910 ℃, and keeping the temperature for 2h; then N with 4 percent of oxygen volume content 2 Heating to 1300 ℃ under the atmosphere, preserving the heat for 5 hours, and finally, adding N 2 And cooling in the atmosphere to prepare the MnZn soft magnetic ferrite material.
The preparation method of the polyvinyl alcohol aqueous solution in the step (2) comprises the following steps:
heating purified water to 90 ℃, adding PEG-2000 accounting for 2% of the mass of the purified water and sodium lignosulfonate accounting for 0.5%, stirring and dissolving uniformly, adding PVA17-88 accounting for 8% of the mass of the purified water, stirring and dissolving, and cooling to room temperature to obtain the polyvinyl alcohol aqueous solution.
The preparation method of the modified starch aqueous solution in the step (5) comprises the following steps:
heating purified water to 70 ℃, adding waxy corn amylopectin accounting for 0.2 percent of the mass of the purified water, adding potassium permanganate accounting for 0.4 percent of the mass of the purified water, stirring until the mixture is uniformly gelatinized, cooling to-5 ℃ by using an ice salt bath, dropwise adding benzenesulfonyl chloride accounting for 2 percent of the volume of the purified water, reacting for 4 hours, and performing freeze drying and ethanol washing to obtain modified starch; and dissolving the modified starch in warm water 200 times the mass of the modified starch to prepare a modified starch aqueous solution.
Example 3
A manufacturing method of a high flexural strength manganese-zinc soft magnetic ferrite material comprises the following specific steps:
(1) Primary material preparation: the mole fraction of the massage is Fe 2 O 3 :70 parts, mnO:25 parts of ZnO: 20. proportioning;
(2) Primary ball milling: uniformly mixing the raw materials weighed in the step (1), adding a polyvinyl alcohol aqueous solution with the powder mass of 15wt%, performing high-speed ball milling at 8000rpm for 60min, and performing spray drying to obtain granular powder A;
(3) Pre-burning: putting the granular powder A prepared in the step (2) in N 2 Heating to 550 deg.C in atmosphere, maintaining for 1h, and adding 3% oxygen volume content N 2 Heating to 900 deg.C under atmosphere, maintaining for 2 hr, and adding N 2 Cooling in the atmosphere to prepare a pre-sintered material;
(4) Secondary burdening: weighing V corresponding to 1.5wt% of the pre-sintering material 2 O 3 0.5wt% of CuO, 0.8wt% of CaCO 3 0.05wt% of Nb 2 O 5 0.05wt% MoO;
(5) Secondary ball milling: uniformly mixing the raw materials weighed in the step (4) with the pre-sintering material prepared in the step (3), adding a modified starch aqueous solution with the powder mass of 30%, performing high-speed ball milling at 8000rpm for 30min, and performing spray drying to obtain granular powder B;
(6) And (3) pressing and forming: adding the granular powder B obtained in the step (5) into a forming die, and pressing and forming by using a full-automatic dry press;
(7) And (3) sintering: firstly, introducing high-temperature and high-pressure steam with the pressure of 1.5MPa and the temperature of 200 ℃, and preserving heat for 3 hours; then in N 2 Heating to 550 ℃ under the atmosphere, keeping the temperature for 1h, then continuing heating to 950 ℃ and keeping the temperature for 1h; then N with 5% volume content of oxygen 2 Heating to 1300 deg.C under atmosphere, keeping the temperature for 4h, and finally adding N 2 And cooling in the atmosphere to prepare the MnZn soft magnetic ferrite material.
The preparation method of the polyvinyl alcohol aqueous solution in the step (2) comprises the following steps:
heating purified water to 90 ℃, adding PEG-2000 accounting for 2% of the mass of the purified water and sodium lignosulfonate accounting for 0.5%, stirring and dissolving uniformly, adding PVA17-88 accounting for 8% of the mass of the purified water, stirring and dissolving, and cooling to room temperature to obtain the polyvinyl alcohol aqueous solution.
The preparation method of the modified starch aqueous solution in the step (5) comprises the following steps:
heating purified water to 75 ℃, adding waxy corn amylopectin with the mass of 0.3% of that of the purified water, adding potassium permanganate with the mass of 0.5% of that of the purified water, stirring until the mixture is uniformly gelatinized, cooling to 0 ℃ by using an ice salt bath, dropwise adding benzenesulfonyl chloride with the volume of 3% of that of the purified water, reacting for 5 hours, and performing freeze drying and ethanol washing to obtain modified starch; the modified starch prepared above is dissolved in warm water 200 times the mass of the starch to prepare a modified starch aqueous solution.
Comparative example 1
A method for manufacturing a Mn-Zn soft magnetic ferrite material comprises the steps of mixing powder materials with the same proportion as that in example 2 all at one time, then adding a polyvinyl alcohol aqueous solution and a modified starch aqueous solution with the same proportion and using amount as that in example 2, and sintering according to the same sintering process as that in example 2 to obtain the MnZn soft magnetic ferrite material.
Comparative example 2
A method for manufacturing a manganese-zinc soft magnetic ferrite material, wherein PEG-2000 is not added into a polyvinyl alcohol aqueous solution, and the rest processes are the same as those of the embodiment 2.
Comparative example 3
A method for manufacturing a manganese-zinc soft magnetic ferrite material is provided, wherein sodium lignosulphonate is not added into a polyvinyl alcohol aqueous solution in the manufacturing method, and the rest processes are the same as those in the embodiment 2.
Comparative example 4
A method for preparing manganese-zinc soft magnetic ferrite material, wherein sodium lignosulphonate is replaced by sodium dodecyl sulfate with the same mass in polyvinyl alcohol aqueous solution, and the rest process is the same as that of the embodiment 2.
Comparative example 5
In the preparation method, the waxy corn amylopectin is replaced by the corn amylose with the same quality in the modified starch aqueous solution, and the rest processes are the same as the process in the embodiment 2.
Comparative example 6
A method for manufacturing a manganese-zinc soft magnetic ferrite material is characterized in that potassium permanganate is not added into a modified starch aqueous solution, and the rest processes are the same as those in the embodiment 2.
Comparative example 7
A preparation method of a manganese-zinc soft magnetic ferrite material is provided, wherein benzene sulfonyl chloride is not added into modified starch aqueous solution in the preparation method, and the rest processes are the same as those in the embodiment 2.
Comparative example 8
A method for manufacturing a manganese-zinc soft magnetic ferrite material is provided, wherein high-temperature and high-pressure water vapor is not introduced into a sintering section in the step (7), and the rest processes are the same as those of the embodiment 2.
EE magnetic cores with the same specification are prepared according to the above examples and comparative examples, 10 magnetic cores are respectively selected, the mechanical strength is tested according to the attached drawings of the specification, the average value is taken, and the test result is as follows:
the magnetic cores obtained in the above examples and comparative examples have AL in the range of 5050-5200nH/N 2 The properties are very close but the mechanical strength is very different, as shown in the table above, with a curie temperature between 210 and 220 ℃.
And finally: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (5)
1. A manufacturing method of a high flexural strength manganese zinc soft magnetic ferrite material is characterized in that: the manufacturing method specifically comprises the following steps:
(1) Primary burdening: the mole fraction of the massage is Fe 2 O 3 :65-70 parts, mnO:25-28 parts of ZnO:18-20 parts of raw materials are mixed;
(2) Primary ball milling: uniformly mixing the raw materials weighed in the step (1), adding a polyvinyl alcohol aqueous solution with the mass of 10-15wt% of the powder, carrying out high-speed ball milling at 8000-10000rpm for 40-60min, and carrying out spray drying to obtain granular powder A;
(3) Pre-burning: putting the granular powder A prepared in the step (2) in N 2 Heating to 500-550 deg.C in atmosphere, maintaining for 1-2h, and adding 1-3% oxygen in volume 2 Heating to 900-930 deg.C in atmosphere, maintaining for 1-2h, and adding N 2 Cooling in the atmosphere to prepare a pre-sintered material;
(4) Secondary burdening: weighing V which is 1.0-1.5wt% of the pre-sintering material 2 O 3 0.5 to 1.0 weight percent of CuO and 0.5 to 0.8 weight percent of CaCO 3 0.03-0.05wt% of Nb 2 O 5 0.02-0.05wt% of MoO;
(5) Secondary ball milling: uniformly mixing the raw materials weighed in the step (4) with the pre-sintering material prepared in the step (3), adding a modified starch aqueous solution with the mass of 20-30% of the powder, carrying out high-speed ball milling at 8000-10000rpm for 20-30min, and carrying out spray drying to obtain granular powder B;
(6) And (3) compression molding: adding the granular powder B obtained in the step (5) into a forming die, and pressing and forming by using a full-automatic dry press;
(7) And (3) sintering: firstly, introducing high-temperature and high-pressure steam, and preserving heat for 2-3h; then in N 2 Heating to 500-550 ℃ under the atmosphere, keeping the temperature for 1-2h, continuing heating to 900-950 ℃, and keeping the temperature for 1-2h; then 3-5% oxygen volume content of N 2 Heating to 1250-1300 deg.C in atmosphere, keeping the temperature for 4-6h, and finally adding N 2 And cooling in the atmosphere to prepare the MnZn soft magnetic ferrite material.
2. The method for manufacturing a high flexural strength manganese-zinc soft magnetic ferrite material according to claim 1, characterized in that: the preparation method of the polyvinyl alcohol aqueous solution in the step (2) comprises the following steps:
heating purified water to 85-90 ℃, then adding polyethylene glycol accounting for 2% of the mass of the purified water and sodium lignosulfonate accounting for 0.5%, stirring and dissolving uniformly, adding PVA17-88 accounting for 8% of the mass of the purified water, stirring and dissolving, and cooling to room temperature to obtain the polyvinyl alcohol aqueous solution.
3. The method for manufacturing a high flexural strength manganese-zinc soft magnetic ferrite material according to claim 2, characterized in that: the polyethylene glycol is PEG-2000.
4. The method for manufacturing a high flexural strength manganese-zinc soft magnetic ferrite material according to claim 1, characterized in that: the preparation method of the modified starch aqueous solution in the step (5) comprises the following steps:
heating purified water to 65-75 ℃, adding waxy corn amylopectin with the mass of 0.1-0.3% of that of the purified water, adding potassium permanganate with the mass of 0.3-0.5% of that of the purified water, stirring until the mixture is uniformly gelatinized, cooling to-5-0 ℃ by using an ice salt bath, dropwise adding benzenesulfonyl chloride with the volume of 1-3% of that of the purified water, reacting for 3-5h, and performing freeze drying and ethanol washing to obtain modified starch; the modified starch prepared above is dissolved in warm water 200 times the mass of the starch to prepare a modified starch aqueous solution.
5. The method for manufacturing a high flexural strength manganese-zinc soft magnetic ferrite material according to claim 1, characterized in that: and (7) the high-temperature and high-pressure water vapor is water vapor with the pressure of 1.5MPa and the temperature of 200 ℃.
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