CN110835261B - Preparation method of high-resistivity soft magnetic ferrite material - Google Patents
Preparation method of high-resistivity soft magnetic ferrite material Download PDFInfo
- Publication number
- CN110835261B CN110835261B CN201911041600.1A CN201911041600A CN110835261B CN 110835261 B CN110835261 B CN 110835261B CN 201911041600 A CN201911041600 A CN 201911041600A CN 110835261 B CN110835261 B CN 110835261B
- Authority
- CN
- China
- Prior art keywords
- mixture
- sintering
- finally
- preparing
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/64—Burning or sintering processes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
-
- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Magnetic Ceramics (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention discloses a preparation method of a high-resistivity soft magnetic ferrite material, which comprises the following steps: step one, preparing a sintering aid: grinding the glass powder through 120-160 meshes, mixing the glass powder with the alkaline earth metal carbonate according to the weight ratio of 2:3, adding the mixture into an ethanol solvent, stirring the mixture at the rotating speed of 100-200r/min for 30-40min, finally carrying out ultrasonic treatment for 10-20min, and finally centrifuging and drying the mixture to obtain the sintering aid. In the sintering process of the material, the calcium carbonate is decomposed to promote the matrix to generate pores, the glass powder is in a flowing state at high temperature and permeates into the matrix after being pressed under high pressure, so that a glass resistance layer is formed in the matrix, and the resistance layer can not be achieved by a simple spraying process.
Description
Technical Field
The invention relates to the technical field of soft magnetic ferrite materials, in particular to a preparation method of a high-resistivity soft magnetic ferrite material.
Background
With the development of science and technology and the progress of society, people continuously and deeply research high-performance materials, and the soft magnetic ferrite is produced by a powder metallurgy method by using a ferrimagnetic oxide taking ferric oxide as a main component. The ferrite material comprises Mn-Zn, Cu-Zn, Ni-Zn and the like, wherein the Mn-Zn ferrite has the largest yield and dosage, and the soft magnetic ferrite has the characteristics of low loss factor, high magnetic conductivity, high impedance/frequency. The high-frequency power supply is widely applied to common mode filters, saturated inductors, current transformers, leakage protectors, insulating transformers and signal and pulse transformers, and is multipurpose on broadband transformers and EMI. The power ferrite has high saturation magnetic induction.
Since the soft magnetic material is made of a metal material, although the properties such as magnetic permeability are good, the resistivity is poor, and the prior chinese patent publication No. CN109694245A discloses a high-resistivity soft magnetic ferrite core and a processing method thereof. The high-resistivity soft magnetic ferrite core is characterized in that: the raw materials comprise the following components in parts by weight: 53-56 parts of ferric oxide, 6-11 parts of zinc oxide, 27-31 parts of manganese oxide, 3-5 parts of copper hydroxide, 2.5-3.6 parts of nickel sesquioxide, 0.9-1.3 parts of sodium polyacrylate, 0.4-0.7 part of silica sol, 0.7-1.1 part of polyvinyl alcohol, 1.2-1.6 parts of polyamide resin, 0.7-1.3 parts of sodium silicate and 3-7 parts of deionized water.
Disclosure of Invention
The invention aims to provide a preparation method of a high-resistivity soft magnetic ferrite material, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a high-resistivity soft magnetic ferrite material comprises the following steps:
step one, preparing a sintering aid: grinding glass powder through 120-160 meshes, mixing the glass powder with alkaline earth metal carbonate according to the weight ratio of 2:3, adding the mixture into an ethanol solvent, stirring the mixture at the rotating speed of 100-200r/min for 30-40min, finally performing ultrasonic treatment for 10-20min, and finally centrifuging and drying the mixture to obtain a sintering aid;
step two, preparing the electric resistance agent: mixing ceramic powder according to a weight ratio of 1:2, then sending the mixture into a ball mill for ball milling, sieving with a 200-mesh sieve, then sending the mixture and a compatibilization modified liquid into a high-temperature high-pressure reaction kettle together, reacting for 45-55min at a pressure of 110 ℃ and 5MPa, after the reaction is finished, centrifuging and drying to obtain an electric resistance agent, wherein the preparation method of the compatibilization modified liquid comprises the steps of grinding Re rare earth powder and sieving with a 100-mesh sieve, then adding the Re rare earth powder into a sodium alginate solution for ultrasonic dispersion for 20-30min, then centrifuging and drying, adding the obtained product into an ionic liquid, and continuously stirring for 20-30min at a rotating speed of 250r/min of 210-;
step three, preparing a base material: adding iron oxide, zinc oxide and manganese oxide into a smelting furnace according to the weight ratio of 7:2:1, smelting for 20-30min until the raw materials are completely molten, then adding the electric resistance agent prepared in the step two and accounting for 15% of the total weight of the iron oxide, continuing to smelt for 10-20min, and finally preserving heat for later use;
step four, preparing a base layer: cooling and molding the base material obtained in the step three, then sending the base material and the sintering aid into a mold for sintering, and cooling and molding after sintering;
step five: thermal homogenization of the base layer: and (3) performing thermal homogenization treatment on the base layer obtained in the fourth step, ending the thermal homogenization treatment, and finally obtaining the high-resistivity soft magnetic ferrite material, wherein the thermal homogenization treatment firstly heats the temperature to 350 ℃ for 320 plus materials at the speed of 1-3 ℃/min, then anneals to 260 ℃, preserves the temperature for 25min, finally tempers to 550 ℃ for 450 plus materials at the speed of 5 ℃/min, keeps the temperature for 15-25min, and finally recovers to the room temperature under the natural condition.
Preferably, the alkaline earth metal carbonate in step one is calcium carbonate.
Preferably, the smelting process of the step three-smelting furnace is also accompanied by a pulse magnetic field, the pulse magnetic induction intensity of the pulse magnetic field is 3.5T, and the pulse number is 25.
Preferably, the sintering in the fourth step is firstly sintering at 600 ℃ for 20-30min, applying pressure of 2-5MPa in the sintering process, keeping the pressure for 10min, then raising the temperature to 1100 ℃ at the speed of 5 ℃/min, sintering for 30-40min, applying pressure of 6-10MPa, and keeping the pressure for 15 min.
Preferably, the thermal homogenization treatment is to raise the temperature to 335 ℃ at the speed of 2 ℃/min, then anneal to 260 ℃, preserve heat for 25min, finally temper to 500 ℃ at the speed of 5 ℃/min, continue to preserve heat for 20min, and finally recover to room temperature under natural conditions.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the process of sintering the material, the calcium carbonate decomposition of the sintering aid can promote the matrix to generate pores, the glass powder is in a flowing state at high temperature and permeates into the matrix after high-pressure pressing treatment, so that a glass resistance layer is formed in the matrix, and the resistance layer is not achieved by a simple spraying process. Firstly heating the material to 335 ℃ at the speed of 2 ℃/min, then annealing, preserving heat, tempering and preserving heat, and finally cooling to room temperature under natural conditions.
(2) The resistance agent adopts ceramic powder as a resistance medium, can improve the compatibility and the reactivity with a matrix after being treated by a compatibilization modification liquid, has high activity of Re rare earth powder in the compatibilization modification liquid, has negative charges on the surface after being treated by a sodium alginate solution, and is treated by ionic liquid 1-butyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide, so that the compatibility of the ceramic powder and the matrix is enhanced, the problem that the performance of the existing raw materials is reduced due to difficult compatibility is solved, and the resistance of the material is greatly improved by adopting the combined effect of an electric resistance agent and a sintering aid.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the preparation method of the high-resistivity soft magnetic ferrite material comprises the following steps:
step one, preparing a sintering aid: grinding glass powder through 120 meshes, mixing the glass powder with alkaline earth metal carbonate according to the weight ratio of 2:3, adding the mixture into an ethanol solvent, stirring the mixture at the rotating speed of 100r/min for 30min, performing ultrasonic treatment for 10min, centrifuging and drying the mixture to obtain a sintering aid;
step two, preparing the electric resistance agent: mixing ceramic powder according to the weight ratio of 1:2, then sending the mixture into a ball mill for ball milling, sieving the mixture with a 200-mesh sieve, then sending the mixture and a compatibilization modified solution into a high-temperature high-pressure reaction kettle together, reacting for 45min at the pressure of 110 ℃ and 5MPa, and after the reaction is finished, centrifuging and drying the mixture to obtain an electric resistance agent;
step three, preparing a base material: adding iron oxide, zinc oxide and manganese oxide into a smelting furnace according to the weight ratio of 7:2:1, smelting for 20min until the raw materials are completely molten, then adding the electric resistance agent prepared in the step two and accounting for 15% of the total weight of the iron oxide, continuing smelting for 10min, and finally preserving heat for later use;
step four, preparing a base layer: cooling and molding the base material obtained in the step three, then sending the base material and the sintering aid into a mold for sintering, and cooling and molding after sintering;
step five: thermal homogenization of the base layer: and (4) carrying out thermal homogenization treatment on the base layer obtained in the step four, and finally obtaining the high-resistivity soft magnetic ferrite material.
The alkaline earth metal carbonate in step one of this example is calcium carbonate.
In the second step of this embodiment, the preparation method of the compatibilization modified liquid includes grinding the Re rare earth powder, sieving with a 100-mesh sieve, adding the Re rare earth powder into the sodium alginate solution, performing ultrasonic dispersion for 20min, centrifuging, drying, adding the Re rare earth powder into the ionic liquid, and continuously stirring at a rotation speed of 210r/min for 20min to obtain the compatibilization modified liquid.
The ionic liquid of this example was 1-butyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide.
The smelting process of the three-smelting furnace in the step of the embodiment is also accompanied by a pulse magnetic field, the pulse magnetic induction intensity of the pulse magnetic field is 3.5T, and the pulse number is 25.
In the fourth step of this example, the sintering is performed at 600 ℃ for 20min, a pressure of 2MPa is applied during the sintering, the pressure is maintained for 10min, then the temperature is increased to 1100 ℃ at a rate of 5 ℃/min, the sintering is performed for 30-40min, and a pressure of 6MPa is applied, and the pressure is maintained for 15 min.
In the thermal homogenization treatment of the embodiment, the temperature is firstly increased to 320 ℃ at the speed of 1 ℃/min, then the annealing is carried out to 260 ℃, the heat preservation is carried out for 25min, finally the tempering is carried out to 450 ℃ at the speed of 5 ℃/min, the heat preservation is continuously carried out for 15min, and finally the temperature is recovered to the room temperature under the natural condition.
Example 2:
the preparation method of the high-resistivity soft magnetic ferrite material comprises the following steps:
step one, preparing a sintering aid: grinding glass powder through a 160-mesh sieve, mixing the glass powder with alkaline earth metal carbonate according to a weight ratio of 2:3, adding the mixture into an ethanol solvent, stirring the mixture at a rotating speed of 200r/min for 40min, performing ultrasonic treatment for 20min, centrifuging and drying the mixture to obtain a sintering aid;
step two, preparing the electric resistance agent: mixing ceramic powder according to the weight ratio of 1:2, then sending the mixture into a ball mill for ball milling, sieving the mixture with a 200-mesh sieve, then sending the mixture and a compatibilization modification solution into a high-temperature high-pressure reaction kettle together, reacting for 55min at the temperature of 110 ℃ and the pressure of 5MPa, and after the reaction is finished, centrifuging and drying the mixture to obtain a resistance agent;
step three, preparing a base material: adding iron oxide, zinc oxide and manganese oxide into a smelting furnace according to the weight ratio of 7:2:1, smelting for 30min until the raw materials are completely molten, then adding the electric resistance agent prepared in the step two and accounting for 15% of the total weight of the iron oxide, continuing smelting for 20min, and finally preserving heat for later use;
step four, preparing a base layer: cooling and molding the base material obtained in the step three, then sending the base material and the sintering aid into a mold for sintering, and cooling and molding after sintering;
step five: thermal homogenization of the base layer: and (4) carrying out thermal homogenization treatment on the base layer obtained in the step four, and finally obtaining the high-resistivity soft magnetic ferrite material.
The alkaline earth metal carbonate in step one of this example is calcium carbonate.
In the second step of this embodiment, the preparation method of the compatibilization modified liquid includes grinding the Re rare earth powder, sieving with a 100-mesh sieve, adding the ground Re rare earth powder into the sodium alginate solution, performing ultrasonic dispersion for 30min, centrifuging, drying, and adding the obtained product into the ionic liquid to continue stirring for 30min at a rotation speed of 250r/min, thereby obtaining the compatibilization modified liquid.
The ionic liquid of this example was 1-butyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide.
The smelting process of the three-smelting furnace in the step of the embodiment is also accompanied by a pulse magnetic field, the pulse magnetic induction intensity of the pulse magnetic field is 3.5T, and the pulse number is 25.
In the fourth step of this example, the sintering is performed at 600 ℃ for 30min, a pressure of 5MPa is applied during the sintering, the pressure is maintained for 10min, then the temperature is increased to 1100 ℃ at a rate of 5 ℃/min, the sintering is performed for 40min, and a pressure of 10MPa is applied, and the pressure is maintained for 15 min.
In the thermal homogenization treatment of the embodiment, the temperature is firstly increased to 350 ℃ at the speed of 3 ℃/min, then the annealing is carried out to 260 ℃, the heat preservation is carried out for 25min, finally the tempering is carried out to 550 ℃ at the speed of 5 ℃/min, the heat preservation is continuously carried out for 25min, and finally the temperature is recovered to the room temperature under the natural condition.
Example 3:
the preparation method of the high-resistivity soft magnetic ferrite material comprises the following steps:
step one, preparing a sintering aid: grinding glass powder through 140 meshes, mixing the glass powder with alkaline earth metal carbonate according to the weight ratio of 2:3, adding the mixture into an ethanol solvent, stirring the mixture at the rotating speed of 150r/min for 35min, performing ultrasonic treatment for 15min, centrifuging and drying the mixture to obtain a sintering aid;
step two, preparing the electric resistance agent: mixing ceramic powder according to the weight ratio of 1:2, then sending the mixture into a ball mill for ball milling, sieving the mixture with a 200-mesh sieve, then sending the mixture and a compatibilization modification solution into a high-temperature high-pressure reaction kettle together, reacting for 50min at the temperature of 110 ℃ and the pressure of 5MPa, and after the reaction is finished, centrifuging and drying the mixture to obtain a resistance agent;
step three, preparing a base material: adding iron oxide, zinc oxide and manganese oxide into a smelting furnace according to the weight ratio of 7:2:1, smelting for 25min until the raw materials are completely molten, then adding the electric resistance agent prepared in the step two and accounting for 15% of the total weight of the iron oxide, continuing smelting for 15min, and finally preserving heat for later use;
step four, preparing a base layer: cooling and molding the base material obtained in the step three, then sending the base material and the sintering aid into a mold for sintering, and cooling and molding after sintering;
step five: thermal homogenization of the base layer: and (4) carrying out thermal homogenization treatment on the base layer obtained in the step four, and finally obtaining the high-resistivity soft magnetic ferrite material.
The alkaline earth metal carbonate in step one of this example is calcium carbonate.
In the second step of this embodiment, the preparation method of the compatibilization modified liquid includes grinding the Re rare earth powder, sieving with a 100-mesh sieve, adding the ground Re rare earth powder into the sodium alginate solution, performing ultrasonic dispersion for 25min, centrifuging, drying, and adding the obtained product into the ionic liquid to continue stirring at a rotation speed of 230r/min for 25min, thereby obtaining the compatibilization modified liquid.
The ionic liquid of this example was 1-butyl-3-methylimidazolium bis (trifluoromethanesulfonyl) imide.
The smelting process of the three-smelting furnace in the step of the embodiment is also accompanied by a pulse magnetic field, the pulse magnetic induction intensity of the pulse magnetic field is 3.5T, and the pulse number is 25.
In the fourth step of this example, sintering is performed at 600 ℃ for 25min, a pressure of 3.5MPa is applied during sintering, the pressure is maintained for 10min, then the temperature is increased to 1100 ℃ at a rate of 5 ℃/min, sintering is performed for 35min, and a pressure of 8MPa is applied, and the pressure is maintained for 15 min.
In the thermal homogenization treatment of the embodiment, the temperature is firstly increased to 335 ℃ at the speed of 2 ℃/min, then the annealing is carried out to 260 ℃, the temperature is kept for 25min, finally the tempering is carried out to 475 ℃ at the speed of 5 ℃/min, the temperature is kept for 20min, and finally the temperature is recovered to the room temperature under the natural condition.
Comparative example 1:
the materials and the preparation process are basically the same as those of the example 3, except that the ceramic powder and the glass powder are directly added into the base material after being mixed, the glass powder is not mixed by adopting a preparation method of a sintering aid, and the ceramic powder is not treated by a compatibilization modification liquid.
Comparative example 2:
the materials and preparation process were substantially the same as those of example 3, except that the thermal homogenization treatment was not used.
Comparative example 3:
basically the same materials and preparation processes as those of example 3, except that chinese patent publication No. CN109694245A discloses a high resistivity soft magnetic ferrite core and the raw materials and method of example 1 in the processing method thereof.
And (3) performance testing: the performance of examples 1-3 and comparative examples 1-3 was tested under conventional conditions, and the results are shown in Table 1
| Group of | Resistance (m omega) | Magnetic permeability | Magnetic induction intensity (T) |
| Example 1 | 45 | 91 | 0.89 |
| Example 2 | 44 | 90 | 0.88 |
| Example 3 | 46 | 93 | 0.91 |
| Comparative example 1 | 37 | 83 | 0.79 |
| Comparative example 2 | 41 | 87 | 0.82 |
| Comparative example 3 | 30 | 80 | 0.7 |
TABLE 1
As can be seen from Table 1, the resistance of the embodiment 3 of the invention is improved by 16m omega compared with the comparative example 3, the improvement rate is 53.3%, and meanwhile, the resistivity is reduced by 24.3% by adopting the method of the comparative example 1, and the magnetic conductivity and the magnetic induction intensity are both worsened.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (5)
1. A preparation method of a high-resistivity soft magnetic ferrite material is characterized by comprising the following steps:
step one, preparing a sintering aid: grinding glass powder through 120-160 meshes, mixing the glass powder with alkaline earth metal carbonate according to the weight ratio of 2:3, adding the mixture into an ethanol solvent, stirring the mixture at the rotating speed of 100-200r/min for 30-40min, finally performing ultrasonic treatment for 10-20min, and finally centrifuging and drying the mixture to obtain a sintering aid;
step two, preparing the electric resistance agent: mixing ceramic powder according to the weight ratio of 1:2, then sending the mixture into a ball mill for ball milling, sieving the mixture with a 200-mesh sieve, then sending the mixture and a compatibilization modified solution into a high-temperature high-pressure reaction kettle together, reacting for 45-55min at the pressure of 110 ℃ and 5MPa, after the reaction is finished, centrifuging and drying the mixture to obtain an electric resistance agent, wherein the preparation method of the compatibilization modified solution comprises the steps of grinding Re rare earth powder and sieving the ground Re rare earth powder with a 100-mesh sieve, then adding the Re rare earth powder into a sodium alginate solution for ultrasonic dispersion for 20-30min, then centrifuging and drying the mixture, adding the Re rare earth powder into an ionic liquid, and continuously stirring the mixture for 20-30min at the rotating speed of 250r/min of 210-;
step three, preparing a base material: adding iron oxide, zinc oxide and manganese oxide into a smelting furnace according to the weight ratio of 7:2:1, smelting for 20-30min until the raw materials are completely molten, then adding the electric resistance agent prepared in the step two and accounting for 15% of the total weight of the iron oxide, continuing to smelt for 10-20min, and finally preserving heat for later use;
step four, preparing a base layer: cooling and molding the base material obtained in the step three, then sending the base material and the sintering aid into a mold for sintering, and cooling and molding after sintering;
step five: thermal homogenization of the base layer: and (3) performing thermal homogenization treatment on the base layer obtained in the step four, ending the thermal homogenization treatment, and finally obtaining the high-resistivity soft magnetic ferrite material, wherein the thermal homogenization treatment firstly heats the temperature to 350 ℃ at the speed of 1-3 ℃/min, then anneals to 260 ℃, preserves the temperature for 25min, finally tempers to 550 ℃ at the speed of 5 ℃/min, continues to preserve the temperature for 15-25min, and finally recovers to the room temperature under natural conditions.
2. The method of claim 1, wherein the alkaline earth metal carbonate in the first step is calcium carbonate.
3. The method for preparing the high-resistivity soft magnetic ferrite material according to claim 1, wherein the smelting process of the three-smelting furnace is accompanied by a pulse magnetic field, the pulse magnetic induction intensity of the pulse magnetic field is 3.5T, and the pulse number is 25.
4. The method for preparing a high-resistivity soft magnetic ferrite material according to claim 1, wherein the sintering in the fourth step is performed for 20-30min at 600 ℃, a pressure of 2-5MPa is applied during the sintering, the pressure is maintained for 10min, then the temperature is increased to 1100 ℃ at a rate of 5 ℃/min, the sintering is performed for 30-40min, and a pressure of 6-10MPa is applied, and the pressure is maintained for 15 min.
5. The method for preparing a high-resistivity soft magnetic ferrite material according to claim 1, wherein the thermal homogenization treatment is to raise the temperature to 335 ℃ at a rate of 2 ℃/min, then anneal to 260 ℃, preserve the temperature for 25min, finally temper to 500 ℃ at a rate of 5 ℃/min, continue to preserve the temperature for 20min, and finally return to room temperature under natural conditions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911041600.1A CN110835261B (en) | 2019-10-30 | 2019-10-30 | Preparation method of high-resistivity soft magnetic ferrite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911041600.1A CN110835261B (en) | 2019-10-30 | 2019-10-30 | Preparation method of high-resistivity soft magnetic ferrite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110835261A CN110835261A (en) | 2020-02-25 |
| CN110835261B true CN110835261B (en) | 2022-07-12 |
Family
ID=69575892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911041600.1A Active CN110835261B (en) | 2019-10-30 | 2019-10-30 | Preparation method of high-resistivity soft magnetic ferrite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110835261B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111777419B (en) * | 2020-05-29 | 2022-05-31 | 天长市烁源磁电有限公司 | Sintering process of magnetic ferrite core |
| CN113336530B (en) * | 2021-06-25 | 2022-11-08 | 重庆名檀陶瓷有限公司 | Preparation method of wear-resistant glazed pottery jar |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04101401A (en) * | 1990-08-20 | 1992-04-02 | Matsushita Electric Ind Co Ltd | Ferrite magnetic body and production thereof |
| JP2003292379A (en) * | 2002-03-30 | 2003-10-15 | Maruishi Yogyo Genryo Kk | Hybrid ceramic and manufacturing method therefor |
| CN103382100A (en) * | 2013-06-26 | 2013-11-06 | 蚌埠市高华电子有限公司 | Soft-magnetic ferrite magnetic core material and preparation method thereof |
| CN103382101A (en) * | 2013-06-26 | 2013-11-06 | 蚌埠市高华电子有限公司 | Rare-earth soft-magnetic ferrite with high magnetic permeability and preparation method thereof |
| CN103396108A (en) * | 2013-06-26 | 2013-11-20 | 蚌埠市高华电子有限公司 | Soft magnetic ferrite material and preparation method thereof |
| CN105198396A (en) * | 2015-10-14 | 2015-12-30 | 广东成电华瓷电子科技有限公司 | NiCuZn ferrite material and manufacturing method thereof |
| CN105829263A (en) * | 2013-12-19 | 2016-08-03 | 株式会社村田制作所 | Glass ceramic material and layered ceramic electronic component |
| CN107021747A (en) * | 2017-05-03 | 2017-08-08 | 中国振华集团云科电子有限公司 | Microwave ferrite material and microwave-medium ceramics high temperature co-firing method |
| CN107434407A (en) * | 2016-05-26 | 2017-12-05 | 株式会社村田制作所 | Glass ceramics ferrite composition and electronic unit |
| CN109233807A (en) * | 2018-09-25 | 2019-01-18 | 云南师范大学 | A kind of rare-earth compound luminescent hydrogel material and the preparation method and application thereof |
-
2019
- 2019-10-30 CN CN201911041600.1A patent/CN110835261B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04101401A (en) * | 1990-08-20 | 1992-04-02 | Matsushita Electric Ind Co Ltd | Ferrite magnetic body and production thereof |
| JP2003292379A (en) * | 2002-03-30 | 2003-10-15 | Maruishi Yogyo Genryo Kk | Hybrid ceramic and manufacturing method therefor |
| CN103382100A (en) * | 2013-06-26 | 2013-11-06 | 蚌埠市高华电子有限公司 | Soft-magnetic ferrite magnetic core material and preparation method thereof |
| CN103382101A (en) * | 2013-06-26 | 2013-11-06 | 蚌埠市高华电子有限公司 | Rare-earth soft-magnetic ferrite with high magnetic permeability and preparation method thereof |
| CN103396108A (en) * | 2013-06-26 | 2013-11-20 | 蚌埠市高华电子有限公司 | Soft magnetic ferrite material and preparation method thereof |
| CN105829263A (en) * | 2013-12-19 | 2016-08-03 | 株式会社村田制作所 | Glass ceramic material and layered ceramic electronic component |
| CN105198396A (en) * | 2015-10-14 | 2015-12-30 | 广东成电华瓷电子科技有限公司 | NiCuZn ferrite material and manufacturing method thereof |
| CN107434407A (en) * | 2016-05-26 | 2017-12-05 | 株式会社村田制作所 | Glass ceramics ferrite composition and electronic unit |
| CN107021747A (en) * | 2017-05-03 | 2017-08-08 | 中国振华集团云科电子有限公司 | Microwave ferrite material and microwave-medium ceramics high temperature co-firing method |
| CN109233807A (en) * | 2018-09-25 | 2019-01-18 | 云南师范大学 | A kind of rare-earth compound luminescent hydrogel material and the preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110835261A (en) | 2020-02-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110835261B (en) | Preparation method of high-resistivity soft magnetic ferrite material | |
| CN108424136B (en) | MnZn power ferrite for MHz-level switching power supply and preparation method thereof | |
| CN103803963A (en) | NiCuZn ferrite material and preparation method thereof | |
| CN104078182A (en) | Iron-based soft magnetic composite magnetic powder core and preparation method thereof | |
| CN103456480A (en) | One-step heat treatment preparation process method for soft nanocrystalline magnetic powder core | |
| CN104078181A (en) | Iron-based alloy magnetic powder core adopting core-shell heterostructure and preparation method thereof | |
| CN103666364A (en) | Organic insulating binder for metal soft-magnetic composite material and method for preparing metal soft-magnetic composite material | |
| CN101913850A (en) | Preparation method of high-magnetic-conductivity low-temperature-sintering Z-shaped hexagonal ferrite material | |
| CN108395233A (en) | High-power and low-loss high frequency transformer MnZn ferrite material and preparation method | |
| CN107216135A (en) | NiCuZn ferrites magnetic sheet and preparation method | |
| CN110922179B (en) | High-permeability low-loss ferrite material and preparation method thereof | |
| CN113121217A (en) | Soft magnetic ferrite material and preparation method thereof | |
| CN110981460B (en) | Preparation method of ferrite magnetic material with high magnetic permeability | |
| CN111863424A (en) | Polyimide/inorganic oxide composite coated iron-silicon magnetic powder core and preparation method thereof | |
| CN113451039B (en) | FeSi-based water atomized Fe-Si-Cr soft magnetic powder core and preparation method thereof | |
| CN113059834B (en) | Preparation method of pearl shell-imitated electromagnetic wave absorption film | |
| CN105070452A (en) | Low-loss magnetic core material used for electric appliance | |
| CN115631940A (en) | Magnetic powder core coated with nano boron nitride-aluminum oxide composite film and preparation method thereof | |
| CN110047638B (en) | Iron-based soft magnetic composite material coated with zinc oxide insulating layer and preparation method thereof | |
| CN114050043A (en) | Preparation method of oxide-coated iron-silicon-cadmium soft magnetic composite material | |
| CN107910176A (en) | A kind of rare-earth Nd-Fe-B superfine powder recoverying and utilizing method | |
| CN103680917A (en) | Manufacturing method for nanocrystalline magnetic core for high-frequency electronic transformer | |
| CN110957123A (en) | Method for preparing iron-nickel soft magnetic powder core with magnetic conductivity of 125 | |
| CN105294094A (en) | Magnetic core material with high winding ratio and high magnetic conductivity and preparation method of magnetic core material | |
| CN106169349A (en) | A kind of stable ferrite core material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |