CN114656253B - Preparation method of ferrite material with ultrahigh quality factor and ultralow power loss - Google Patents
Preparation method of ferrite material with ultrahigh quality factor and ultralow power loss Download PDFInfo
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Abstract
The invention provides a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss, which comprises the following steps: step S1: grinding to micron level, stoving, pre-sintering the cooled main material, taking out and hotMixing with adjuvants, and keeping the temperature for 20-30min; step S2: placing the mixture into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material; and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding and granulating; and step S4: pressing the material into a standard ring; step S5: sintering the standard ring to form the ferrite material with ultrahigh quality factor and ultralow power loss through a sintering and forming process of heating sintering-shaping-heat treatment; wherein the main materials are as follows: fe 2 O 3 70-75 parts of Mn 3 O 4 20-25 parts of ZnO, 3-8 parts of ZnO, and the auxiliary materials are as follows: co 2 O 3 0.3-0.5 part of ZrO 2 0.001-0.002 parts of Nb 2 O 5 0.001-0.003 portion; the secondary auxiliary materials are as follows: 0.001-0.003 part of short glass fiber and 0.003-0.005 part of superfine heavy calcium. The invention provides a preparation method of a ferrite material with good high-temperature performance, ultrahigh quality factor and ultralow power loss.
Description
Technical Field
The invention relates to the technical field of soft magnetic ferrite cores, in particular to a preparation method of a ferrite material with ultrahigh quality factor and ultralow power loss.
Background
The ferrite material is available in the 20 th century, the 60 th century, and various scientists begin to research the wet method for preparing Mn-Zn ferrite, the ferrite material and the magnetic core are put into industrial production, and the application field of the ferrite material is continuously expanded in the 90 th century along with the appearance of the ferrite nano material. The ferrite material is still the mainstream product used in the current application field due to good high-frequency property, simple manufacturing process and low production cost. The ferrite material is developed, and the performance of the ferrite material is towards high frequency, high quality factor and low power loss direction on the basis of the prior art; the volume is developing towards miniaturization, flaking and surface mounting, with ever-increasing demands in the field of application. Therefore, in order to seize the technology and market high points, the research and development of new ferrite materials and magnetic cores and new products are very important for colleges, research institutions and enterprises in China. Particularly, the research is fiercely and competitively researched in the novel application fields of new energy automobiles (such as automobile wireless charging piles, vehicle-mounted chargers, DC/DC converters and the like), solar photovoltaic power generation (such as direct current EMI filters, energy storage inductors, isolation transformers and the like) and wireless chargers (such as Ni-Zn ferrite thin magnetic sheets, mn-Zn ferrite thin magnetic sheets, flexible ferrite magnetic sheets and the like)!
Soft magnetic ferrites are often divided into three different types: high permeability ferrites, power ferrites, and anti-electromagnetic interference ferrites. The ferrite with high magnetic permeability has high requirement on initial magnetic permeability, for manganese-zinc ferrite, usually more than 5000, and the products which are already put into use in industry can reach 13000-15000 (models such as TDK-EPCOS: T66, T46, H5C3 and the like), but when the initial magnetic permeability is too high, the Curie temperature and the temperature stability of the magnetic permeability are deteriorated, and the ferrite with too high magnetic permeability can not enter into practical industrial application; for high permeability nickel zinc ferrites, the initial permeability is typically above 2000. The power ferrite is the most widely used ferrite with the largest yield at present, is mainly used in the power transmission process, and is expected to have lower power consumption at higher frequency and improve the power transmission efficiency, and ideal loss can be reduced along with temperature rise, so that after components generate heat due to working reasons, the reduction of the ferrite power loss can enable the components to work at a stable temperature.
Therefore, a preparation method of a ferrite material with good high-temperature performance, ultra-high quality factor and ultra-low power loss needs to be researched.
Disclosure of Invention
The invention aims to provide a preparation method of a ferrite material with good high-temperature performance, ultrahigh quality factor and ultralow power loss.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.5-1.0h, taking out, and mixing with the auxiliary material while the main material is hot and keeping the temperature for 20-30min;
step S2: placing the mixed main material and auxiliary material into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 8-10 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8-8.5 MPa;
step S5: sintering the standard ring to form the ferrite material with ultrahigh quality factor and ultralow power loss through a sintering and forming process of heating sintering-shaping-heat treatment;
wherein the main materials are as follows: 70-75 parts of Fe2O3, 20-25 parts of Mn3O4 and 3-8 parts of ZnO, and the auxiliary materials are as follows: 0.3-0.5 part of Co2O3, 0.001-0.002 part of ZrO2 and 0.001-0.003 part of Nb2O 5;
the secondary auxiliary materials are as follows: 0.001-0.003 part of short glass fiber and 0.003-0.005 part of superfine heavy calcium.
As a further improvement of the invention, the hot temperature in step S1 is from 500 to 700 ℃.
As a further improvement of the present invention, the sintering and forming in step S6 includes the following steps:
(1) And (3) sintering: heating the pressed material to sinter for 0.8-1.5h under the condition that the oxygen content is 5-5.5%;
(2) Shaping: heating the primarily sintered material to 1250-1300 ℃, and keeping the temperature for 1.5-4h in a negative pressure environment;
(3) And (3) heat treatment: heating the material to 1200-1250 ℃ at the speed of 1.0-3.0 ℃/min, and keeping the temperature for 1-1.5h to obtain the ferrite material with ultrahigh quality factor and ultralow power loss.
As a further improvement of the invention, the oxygen content in step (2) is 3.5-3.9%.
As a further improvement of the invention, the negative pressure environment pressure in the step (2) shaping is 0.05-0.07MPa.
As a further improvement of the invention, the oxygen content in step (3) is 3.0-5.5%.
The beneficial effects of the invention are:
1. the invention mainly adopts a specific formula and combines a corresponding process to prepare the soft magnetic ferrite material with high Bs value, good high-temperature performance and especially low power loss, has simple preparation process and simple and convenient operation, and is suitable for industrial production of enterprises.
2. The invention mixes the main material and the auxiliary material after sintering under the condition of 500-700 ℃ while the main material and the auxiliary material are hot, so as to lead Zr in the auxiliary material 4+ 、Nb 5+ Uniformly enter the interior of the ferrite to form Zr 4+ -Fe 2+ 、Nb 5+ -Fe 2+ The electron pair promotes the generation of positive ion vacancy in the mixed material, becomes Schottky defect in the subsequent sintering and forming process, increases the diffusion rate of ions and promotes the solid phase reaction rate, zr 4+ The crystal grains are enriched at the crystal boundary to block the growth of the crystal grains and form uniform crystal grains, so that the crystal grains are refined, the loss of the material is reduced, and the quality factor of the material is improved.
3. In the sintering and forming process of the preparation method, the glass fiber is arranged in the secondary auxiliary material, so that a viscous state can be formed at high temperature, the air holes of the material can be filled, the density of the material is improved, the saturation magnetic flux density of the material is improved, the gas in the material which is initially heated in the first stage is driven to escape from the material under the condition of micro negative pressure, the porosity of the material is reduced, and the high saturation magnetic flux density of the subsequent material is further improved.
4. According to the invention, a heat treatment process is also arranged after the shaping, and the heat treatment process similar to a metal releases stress suddenly generated by cooling in the material, so that the stress uniformity of the material is effectively improved, the internal structure of the material is further refined, the loss of the material is reduced, and the quality factor value of the material is effectively improved.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. It should be apparent that the described embodiments are only some 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 of the present invention without inventive step, shall fall within the scope of protection of the present invention.
1. Examples of the embodiments
Example 1
Preparation method of ferrite material with ultrahigh quality factor and ultralow power lossThe material comprises main materials, auxiliary materials and secondary auxiliary materials, wherein the main materials are as follows: fe 2 O 3 70 parts of Mn 3 O 4 20 parts of ZnO, 3 parts of auxiliary materials: co 2 O 3 0.3 part of ZrO 2 0.001 part of Nb 2 O 5 0.001 part; the secondary auxiliary materials are as follows: 0.001 part of glass short fiber and 0.003 part of superfine heavy calcium;
the preparation method comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.5h, taking out, and mixing with the auxiliary material while hot at 500 ℃ for 20min;
step S2: placing the mixed main material and auxiliary material into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 8 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8 MPa;
step S5: then the sintering and forming process of heating sintering-shaping-heat treatment is carried out as follows:
(1) And (3) sintering: heating the pressed material to sinter for 0.8h under the condition that the oxygen content is 5%;
(2) Shaping: heating the primarily sintered material to 1250 ℃, and keeping the temperature for 1.5h in a negative pressure environment with the oxygen content of 3.5% and the pressure of 0.05 MPa;
(3) And (3) heat treatment: heating the material to 1200 ℃ at the speed of 1.0 ℃/min, keeping the temperature for 1h under the condition that the oxygen content is 3.0 percent, preparing a standard ring sample of the ferrite material with the outer diameter of 25 multiplied by the inner diameter of 15 multiplied by the height of 7.5, and carrying out magnetic performance test on the sample, wherein the results are shown in the following table 1:
TABLE 1 test results of various properties of the sample (HC 44Q), comparison results with the TDK PC44 material properties
Example 2
The invention relates to a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss, which comprises the following raw materials of main materials, auxiliary materials and secondary auxiliary materials, wherein the main materials are as follows: fe 2 O 3 75 parts of Mn 3 O 4 25 parts of ZnO, 8 parts of ZnO, and the auxiliary materials are: co 2 O 3 -0.5 part, zrO 2 0.002 part of Nb 2 O 5 0.003 part of a mixture; the secondary auxiliary materials are as follows: 0.003 part of short glass fiber and 0.005 part of superfine heavy calcium;
the preparation method comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 1.0h, taking out, and mixing with the auxiliary material while the main material is hot at 700 ℃ for heat preservation for 30min;
step S2: placing the mixed main material and auxiliary materials into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 10 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8.5 MPa;
step S5: then the sintering and forming process of heating sintering-shaping-heat treatment is carried out as follows:
(1) And (3) sintering: heating the pressed material to sinter for 1.5h under the condition that the oxygen content is 5.5 percent;
(2) Shaping: heating the primarily sintered material to 1300 ℃, and keeping the temperature for 4 hours in a negative pressure environment with the oxygen content of 3.9% and the pressure of 0.07 MPa;
(3) And (3) heat treatment: heating the material to 1250 ℃ at the speed of 3.0 ℃/min, keeping the temperature for 1.5h under the condition that the oxygen content is 5.5%, preparing a standard ring sample of the ferrite material with the ultra-high quality factor and the ultra-low power loss, wherein the outer diameter of the standard ring sample is 25 multiplied by the inner diameter of the standard ring sample is 15 multiplied by the height of the standard ring sample is 7.5, and performing a magnetic property test on the sample, wherein the results are shown in the following table 2:
TABLE 2 test results of various properties of the sample (HC 44Q), comparison results with TDK PC44 material properties
Example 3
The invention relates to a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss, which comprises the following raw materials of main materials, auxiliary materials and secondary auxiliary materials, wherein the main materials are as follows: fe 2 O 3 72 parts of Mn 3 O 4 22 parts of ZnO, 5 parts of auxiliary materials: co 2 O 3 0.4 part of ZrO 2 0.0016 part and Nb 2 O 5 0.002 part; the secondary auxiliary materials are as follows: 0.002 parts of short glass fiber and 0.004 parts of superfine heavy calcium;
the preparation method comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.8h, taking out, and mixing with the auxiliary material while the main material is hot at 600 ℃ for heat preservation for 25min;
step S2: placing the mixed main material and auxiliary materials into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 9 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8.3 MPa;
step S5: then the sintering and forming process of heating sintering-shaping-heat treatment is carried out as follows:
(1) And (3) sintering: heating the pressed material to sinter for 1.2h under the condition that the oxygen content is 5.2%;
(2) Shaping: heating the primarily sintered material to 1280 ℃, and keeping the temperature for 2 hours in a negative pressure environment with the oxygen content of 3.7% and the pressure of 0.08 MPa;
(3) And (3) heat treatment: heating the material to 1220 ℃ at the speed of 2.0 ℃/min, keeping the temperature for 1.2h under the condition that the oxygen content is 4.5%, preparing a standard ring sample of the ferrite material with the outer diameter of 25 multiplied by the inner diameter of 15 multiplied by the height of 7.5 and the ultrahigh quality factor and the ultralow power loss, and testing the magnetic performance of the sample, wherein the results are shown in the following table 3:
TABLE 3 test results of each performance of the sample (HC 44Q) and the results of comparing the performance of the material with that of TDK PC44
Example 4
The invention relates to a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss, which comprises the following raw materials of main materials, auxiliary materials and secondary auxiliary materials, wherein the main materials are as follows: fe 2 O 3 72 parts of Mn 3 O 4 22 parts of ZnO, 5 parts of auxiliary materials: co 2 O 3 0.4 part of ZrO 2 0.0016 part and Nb 2 O 5 0.002 part; the secondary auxiliary materials are as follows: 0.002 parts of glass short fiber and 0.004 parts of superfine heavy calcium;
the preparation method comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.8h, taking out, cooling to room temperature, and blending with the auxiliary material for 25min;
step S2: placing the mixed main material and auxiliary materials into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 9 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8.3 MPa;
step S5: then the sintering and forming process of heating sintering-shaping-heat treatment is carried out as follows:
(1) And (3) sintering: heating the pressed material to sinter for 1.2h under the condition of oxygen content of 5.2%;
(2) Shaping: heating the primarily sintered material to 1280 ℃, and keeping the temperature for 2 hours in a negative pressure environment with the oxygen content of 3.7% and the pressure of 0.08 MPa;
(3) And (3) heat treatment: heating the material to 1220 ℃ at the speed of 2.0 ℃/min, keeping the temperature for 1.2h under the condition that the oxygen content is 4.5%, preparing a standard ring sample of the ferrite material with the ultra-high quality factor and the ultra-low power loss, wherein the outer diameter of the standard ring sample is 25 multiplied by the inner diameter of the standard ring sample is 15 multiplied by the height of the standard ring sample is 7.5, and performing a magnetic property test on the sample, wherein the results are shown in the following table 4:
TABLE 4 test results of various properties of the sample (HC 44Q), comparison results with the TDK PC44 material properties
Example 5
The invention relates to a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss, which comprises the following raw materials of main materials, auxiliary materials and secondary auxiliary materials, wherein the main materials are as follows: fe 2 O 3 72 parts of Mn 3 O 4 22 parts of ZnO, 5 parts of auxiliary materials: co 2 O 3 0.4 part; the secondary auxiliary materials are as follows: 0.002 parts of glass short fiber and 0.004 parts of superfine heavy calcium;
the preparation method comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.8h, taking out, and mixing with the auxiliary material while the main material is hot at 600 ℃ for heat preservation for 25min;
step S2: placing the mixed main material and auxiliary materials into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 9 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8.3 MPa;
step S5: then the sintering and forming process of heating sintering-shaping-heat treatment is carried out as follows:
(1) And (3) sintering: heating the pressed material to sinter for 1.2h under the condition that the oxygen content is 5.2%;
(2) Shaping: heating the primarily sintered material to 1280 ℃, and keeping the temperature for 2 hours in a negative pressure environment with the oxygen content of 3.7% and the pressure of 0.08 MPa;
(3) And (3) heat treatment: heating the material to 1220 ℃ at the speed of 2.0 ℃/min, keeping the temperature for 1.2h under the condition that the oxygen content is 4.5 percent, and obtaining a standard ring sample of the ferrite material with the ultra-high quality factor and the ultra-low power loss, wherein the outer diameter of the standard ring sample is 25 multiplied by the inner diameter of the standard ring sample is 15 multiplied by the height of the standard ring sample is 7.5, and the sample is subjected to a magnetic performance test, and the results are shown in the following table 5:
TABLE 5 test results of various properties of the sample (HC 44Q), comparison results with the TDK PC44 material properties
Example 6
The invention relates to a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss, which comprises the following raw materials of main materials, auxiliary materials and secondary auxiliary materials, wherein the main materials are as follows: fe 2 O 3 72 parts of Mn 3 O 4 22 parts and ZnO 5 parts, and the auxiliary materials are: co 2 O 3 0.4 part; the secondary auxiliary materials are as follows: 0.002 parts of glass short fiber and 0.004 parts of superfine heavy calcium;
the preparation method comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.8h, taking out, cooling to room temperature, and blending with the auxiliary material for 25min;
step S2: placing the mixed main material and auxiliary materials into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 9 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8.3 MPa;
step S5: then the sintering and forming process of heating sintering-shaping-heat treatment is carried out as follows:
(1) And (3) sintering: heating the pressed material to sinter for 1.2h under the condition that the oxygen content is 5.2%;
(2) Shaping: heating the primarily sintered material to 1280 ℃, and keeping the temperature for 2 hours in a negative pressure environment with the oxygen content of 3.7% and the pressure of 0.08 MPa;
(3) And (3) heat treatment: heating the material to 1220 ℃ at the speed of 2.0 ℃/min, keeping the temperature for 1.2h under the condition that the oxygen content is 4.5%, preparing a standard ring sample of the ferrite material with the ultra-high quality factor and the ultra-low power loss, wherein the outer diameter of the standard ring sample is 25 multiplied by the inner diameter of the standard ring sample is 15 multiplied by the height of the standard ring sample is 7.5, and performing a magnetic property test on the sample, wherein the results are shown in the following table 6:
TABLE 6 test results of various properties of the sample (HC 44Q), the comparison result with the TDK PC44 material property
Example 7
The invention relates to a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss, which comprises the following raw materials of main materials, auxiliary materials and secondary auxiliary materials, wherein the main materials are as follows: fe 2 O 3 72 parts of Mn 3 O 4 22 parts of ZnO, 5 parts of auxiliary materials: co 2 O 3 0.4 part of ZrO 2 0.0016 part and Nb 2 O 5 0.002 parts of (B); the secondary auxiliary materials are as follows: 0.004 portion of superfine heavy calcium;
the preparation method comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.8h, taking out, and mixing with the auxiliary material while the main material is hot at 600 ℃ for heat preservation for 25min;
step S2: placing the mixed main material and auxiliary materials into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 9 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8.3 MPa;
step S5: and then the sintering and forming process of heating sintering-shaping-heat treatment is carried out as follows:
(1) And (3) sintering: heating the pressed material to sinter for 1.2h under the condition that the oxygen content is 5.2%;
(2) Shaping: heating the primarily sintered material to 1280 ℃, and keeping the temperature for 2 hours in a negative pressure environment with the oxygen content of 3.7% and the pressure of 0.08 MPa;
(3) And (3) heat treatment: heating the material to 1220 ℃ at the speed of 2.0 ℃/min, keeping the temperature for 1.2h under the condition that the oxygen content is 4.5%, preparing a standard ring sample of the ferrite material with the outer diameter of 25 multiplied by the inner diameter of 15 multiplied by the height of 7.5 and the ultrahigh quality factor and the ultralow power loss, and testing the magnetic properties of the sample, wherein the results are shown in the following table 7:
TABLE 7 results of various property tests of the sample (HC 44Q), comparison with TDK PC44 material property
Example 8
The invention relates to a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss, which comprises the following raw materials of main materials, auxiliary materials and secondary auxiliary materials, wherein the main materials are as follows: fe 2 O 3 72 parts of Mn 3 O 4 22 parts and ZnO 5 parts, and the auxiliary materials are: co 2 O 3 0.4 part of ZrO 2 0.0016 part and Nb 2 O 5 0.002 part; the secondary auxiliary materials are as follows: 0.002 parts of short glass fiber and 0.004 parts of superfine heavy calcium;
the preparation method comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.8h, taking out, and mixing with the auxiliary material while the main material is hot at 600 ℃ for heat preservation for 25min;
step S2: placing the mixed main material and auxiliary materials into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 9 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8.3 MPa;
step S5: then the sintering and forming process of heating sintering-shaping-heat treatment is carried out as follows:
(1) And (3) sintering: heating the pressed material to sinter for 1.2h under the condition that the oxygen content is 5.2%;
(2) Shaping: the primarily sintered material is heated to 1280 ℃, the temperature is kept for 2h under the negative pressure environment with the oxygen content of 3.7 percent and the pressure of 0.08MPa, the ferrite material standard ring sample with the outer diameter of 25 multiplied by the inner diameter of 15 multiplied by the height of 7.5 and the ultra-low power loss is prepared by cooling, the sample is subjected to the magnetic performance test, and the result is shown in the following table 8:
TABLE 8 test results of each property of the sample (HC 44Q), the comparison result with the TDK PC44 material property
Example 9
The invention relates to a preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss, which comprises the following raw materials of main materials, auxiliary materials and secondary auxiliary materials, wherein the main materials are as follows: fe 2 O 3 72 parts of Mn 3 O 4 22 parts and ZnO 5 parts, and the auxiliary materials are: co 2 O 3 0.4 part; the secondary auxiliary materials are as follows: 0.004 portion of superfine heavy calcium;
the preparation method comprises the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.8h, taking out, cooling to room temperature, and blending with the auxiliary material for 25min;
step S2: placing the mixed main material and auxiliary materials into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 9 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, and pressing the material into a standard ring under the pressure of 8.3 MPa;
step S5: then the sintering and forming process of heating sintering-shaping-heat treatment is carried out as follows:
(1) And (3) sintering: heating the pressed material to sinter for 1.2h under the condition of oxygen content of 5.2%;
(2) Shaping: the primarily sintered material is heated to 1280 ℃, the temperature is kept for 2 hours in a negative pressure environment with the oxygen content of 3.7 percent and the pressure of 0.08MPa, the sample is cooled to obtain a standard ring sample of the ferrite material with the ultra-high quality factor and the ultra-low power loss, the outer diameter of the standard ring sample is 25 multiplied by the inner diameter of the standard ring sample is 15 multiplied by 7.5, the sample is subjected to a magnetic performance test, and the results are shown in the following table 9:
TABLE 9 test results of various properties of the sample (HC 44Q), comparison results with the TDK PC44 material properties
The principles and embodiments of the present invention are explained herein using specific examples, which are set forth only to help understand the method and its core ideas of the present invention. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (4)
1. A preparation method of a ferrite material with ultra-high quality factor and ultra-low power loss is characterized by comprising the following steps:
step S1: grinding the main material in a ball mill to micron level, drying, pre-sintering the cooled main material for 0.5-1.0h, taking out, and mixing with the auxiliary material while the main material is hot and keeping the temperature for 20-30min;
step S2: placing the mixed main material and auxiliary material into a ball mill for secondary ball milling, and drying to obtain a pre-sintered main material;
and step S3: putting the pre-sintered main material and the ground secondary auxiliary material into a ball mill for grinding, drying after grinding, and adding 8-10 parts of PVA glue for granulation;
and step S4: then adding zinc polyesterate, pressing the material into a standard ring under the pressure of 8-8.5 MPa;
step S5: sintering the standard ring to form the ferrite material with ultrahigh quality factor and ultralow power loss through a sintering and forming process of heating sintering-shaping-heat treatment;
wherein the main materials are as follows: fe 2 O 3 70-75 parts of Mn 3 O 4 20-25 parts of ZnO, 3-8 parts of ZnO, and the auxiliary materials are as follows: co 2 O 3 0.3-0.5 part of ZrO 2 0.001-0.002 parts of Nb 2 O 5 0.001-0.003 part of;
the secondary auxiliary materials are as follows: 0.001-0.003 part of short glass fiber and 0.003-0.005 part of superfine heavy calcium;
the hot temperature in the step S1 is 500-700 ℃;
the sintering and forming in the step S5 comprises the following steps:
(1) And (3) sintering: heating the pressed material to sinter for 0.8-1.5h under the condition that the oxygen content is 5-5.5%;
(2) Shaping: heating the primarily sintered material to 1250-1300 ℃, and keeping the temperature for 1.5-4h in a negative pressure environment;
(3) And (3) heat treatment: heating the material to 1200-1250 ℃ at the speed of 1.0-3.0 ℃/min, and keeping the temperature for 1-1.5h to obtain the ferrite material with ultrahigh quality factor and ultralow power loss.
2. The method for preparing an ultra-high quality factor and ultra-low power loss ferrite material according to claim 1, wherein the oxygen content in the sintering and molding step (2) is 3.5-3.9%.
3. The method for preparing a ferrite material with ultra-high quality factor and ultra-low power loss as claimed in claim 1, wherein the negative pressure environment pressure in the step (2) of sintering and forming is 0.05-0.07MPa.
4. The method for preparing a ferrite material with ultra-high quality factor and ultra-low power loss as claimed in claim 1, wherein the oxygen content in the sintering and forming step (3) is 3.0-5.5%.
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