High permeability manganese zinc ferrite broadband material kah150 material and preparation method thereof

Abstract

The embodiment of the application discloses high magnetic permeability manganese-zinc ferrite broadband material KAH150 material and a preparation method thereof, the material has the magnetic permeability ui in the range of 10000-15000+ / -25% under the condition of 10-200KHZ frequency; the Curie temperature Tc of the material is greater than 130 DEG C; the method comprises the following steps: obtaining raw materials according to the proportioning mode that Fe2O3 is 51.2-54.5mol%, ZnO is 19.1-22.40mol%, and the rest is MnO; the raw materials are sequentially subjected to ball milling, pre-sintering, secondary sand milling, spray granulation, blank preparation and sintering treatment, and the high magnetic permeability manganese-zinc ferrite broadband material KAH150 material is obtained. Through the combination adjustment of fixed formula and doping, the material magnetic permeability can still maintain ui >=10000 at 200KHZ, and the high-frequency performance is greatly improved.

Description

Technical Field

[0001] This invention relates to the field of electronic material preparation technology, and more specifically, to the high-permeability manganese-zinc ferrite broadband material KAH150 and its preparation method. Background Technology

[0002] For the KAH150 manganese-zinc ferrite broadband material, materials with a permeability ui of 15000 typically begin to decline at 50kHz, exhibiting poor frequency characteristics. At 200kHz, ui drops below 6000ui, resulting in poor broadband performance, failing to meet the customer's requirement of both ui=15000 and broadband characteristics. Currently, materials with a permeability ui of 15000 can only achieve a Curie temperature TC of 100℃, which cannot meet the requirements of some automotive and new energy products that require both high permeability and a high Curie temperature.

[0003] 1. With the increasing demands on electronic products, products with high permeability of manganese zinc exceeding 12000 are needed to reduce the number of turns and lower costs, while also possessing high-frequency impedance effects. Currently, products with a permeability of 15000 achieve a satisfactory level at 10kHz, but the permeability drops significantly after 100kHz, failing to meet the high-frequency characteristics requirements beyond 100kHz.

[0004] 2. Currently, materials with ui=15000 on the market can only reach a Curie temperature TC of 100-105℃, while the Curie temperature of this invention reaches 130℃ (the main component is different from existing materials).

[0005] 3. This invention achieves a permeability of over 10,000 at a frequency of 200kHz for a material with an ui=15000 by controlling the average particle size of the powder ball mill, adding trace elements, and effectively combining the sintering process.

[0006] 4. The product of this invention can enable customers to design products with fewer turns (reducing costs) and higher impedance, resulting in EMI products with higher performance and greater market competitiveness.

[0007] 1. The disadvantages of existing technology are:

[0008] 1) Currently, for products with a permeability of 15,000, although the permeability of 10kHz is at a certain level, the permeability drops below 60% after 100kHz, and even below 30% at 200kHz.

[0009] 2) Currently, products with a UI of 15000 only have a Curie temperature of 100-105 degrees Celsius, which limits their application in some fields.

[0010] The objectives of this invention are: 1) To enable customers to reduce the number of turns (lower costs) and increase impedance in their product designs, resulting in higher performance and greater market competitiveness for EMI products. 2) To address the issue of low Curie temperature (Tc) in materials with an ui=15000°C. Summary of the Invention

[0011] To address the shortcomings of current materials, this application provides a high-permeability manganese-zinc ferrite broadband material KAH150 and its preparation method, in order to solve the problem that current materials cannot meet the requirements of high Curie temperature and high permeability.

[0012] The present invention provides a high-permeability manganese-zinc ferrite broadband material KAH150, wherein the permeability ui of the material is in the range of 10000-15000±25% under the frequency condition of 10-200KHZ.

[0013] In one feasible implementation, the Curie temperature Tc of the material is greater than 130°C.

[0014] The high-permeability manganese-zinc ferrite broadband material KAH150 includes a main component and a secondary component; the main component is a mixture of Fe2O3, ZnO, and MnO, and the secondary component is a mixture of added dopants MoO3, Bi2O3, CaCO3, V2O5, CuO, TiO2, Co2O3, and WO3.

[0015] In one feasible implementation, the main components are proportioned as follows: Fe2O3 51.2%-54.5 mol%, ZnO 19.1%-22.40 mol%, and MnO 23.5%-26.7 mol%.

[0016] In one feasible implementation, the secondary components are the added dopants, namely: MoO3 0.01-0.05 wt%, Bi2O3 0.01-0.04 wt%, CaCO3 0.005-0.04 wt%, V2O5 0.01-0.04 wt%, CuO 0.02-0.05 wt%, TiO2 0.01-0.05 wt%, Co2O3 0.01-0.04 wt%, and WO3 0.01-0.05 wt%.

[0017] This invention provides another method for preparing the high-permeability manganese-zinc ferrite broadband material KAH150, comprising the following steps:

[0018] Step 1: First ball milling: Prepare the ingredients according to the ratio of the main components, add the materials and deionized water to the sand mill and then ball mill;

[0019] Step 2: Pre-firing: After drying and granulating the material from Step 1, it is placed in a pre-firing furnace for pre-firing;

[0020] Step 3: Secondary ball milling: The pre-burned material from Step 2 and the prepared by-products are mixed and added to a sand mill. Deionized water is then added for secondary sand milling. 10 minutes before the end of the secondary sand milling, an 8% PVA solution is added to obtain a secondary slurry with an average particle size of 0.80 to 0.90 μm.

[0021] Step 4: Granulation: Spray granulation of the material from step 3 to obtain 80-120 mesh granules;

[0022] Step 5: Press the above granules into T25-15-8 blanks using a press, with a blank density of 3.00-3.15 g / cm3;

[0023] Step 6: Sinter the T25-15-8 blank in a bell-shaped kiln. The sintering temperature is 1360-1440℃ and the holding time is 5-8 hours. The kiln is then cooled to 120℃ before being removed. The sample is then taken out and tested after being kept at a constant temperature of 22-27℃ for 3 hours.

[0024] In one feasible implementation, the pre-firing in step 2 is carried out at a temperature of 870–960°C for 1–3 hours.

[0025] In one feasible implementation, the sintering in step 6 is carried out at a heating rate of 1.0℃ / min in the heating range of 900 to 1150℃, with the oxygen content controlled at 0.1% to 1.0%.

[0026] In one feasible implementation, in step 6, except for the last hour when the oxygen content of the heat preservation section is 8%, the oxygen content of the remaining heat preservation section during sintering time is 20%, i.e., air sintering.

[0027] In one feasible implementation, step 6, the sintered T25-15-8 sample, has a tested density of not less than 5.0 g / cm³. 3 .

[0028] The present invention has the following beneficial effects:

[0029] (1) The high-permeability manganese-zinc ferrite broadband material KAH150 of the present invention is obtained by grinding, pressing and sintering using a unique doping combination. The main components determine the Curie temperature to reach 130℃. The appropriate doping combination promotes better liquid phase sintering and further promotes grain growth, resulting in more uniform grains, reducing grain boundary porosity and forming a high finished product density. This allows the material to maintain a permeability of over 10,000 at a high frequency of 200kHz, forming a unique and excellent new material.

[0030] (2) Ordinary high permeability materials generally contain about 5 kinds of trace elements. This invention adds a total of 8 kinds of trace elements. Through the effective combination of doping amounts, the high frequency characteristics of the material are improved. Under the frequency conditions of 10-200KHZ, the permeability ui of the material of this invention is in the range of 10000-15000±25%, which is significantly improved compared with the prior art.

[0031] (3) The material of the present invention has a median ui of 15,000 at a frequency of 10 kHz, but the permeability ui at a frequency of 200 kHz is more than twice that of traditional materials, and has a very obvious advantage in high frequency characteristics.

[0032] (4) The material of this invention enables customers to reduce the number of coil turns in EMI products and reduce costs during product design, while obtaining better high-frequency and high-impedance characteristics, making it suitable for application in the increasingly demanding automotive and new energy fields. Attached Figure Description

[0033] The accompanying drawings, which are provided to further illustrate the invention and constitute a part of this invention, are illustrative embodiments of the invention and their descriptions are used to explain this application and do not constitute an undue limitation of the invention.

[0034] In the attached diagram:

[0035] Figure 1 This is a flowchart illustrating the preparation method of KAH150, a broadband manganese-zinc ferrite material with high magnetic permeability.

[0036] Figure 2 This is a data comparison chart of Example 1 with Comparative Examples 1 and 2. Detailed Implementation

[0037] To enable those skilled in the art to better understand the technical solutions in this application, the technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of this application.

[0038] Currently, materials with a permeability ui of 15000 typically begin to decline at a frequency of 50kHz, exhibiting poor frequency characteristics. By 200kHz, ui has dropped below 6000ui, resulting in poor bandwidth characteristics. This fails to meet the customer's requirement of ui=15000 while also achieving bandwidth characteristics.

[0039] Currently, materials with a permeability ui of 15000 can only reach a Curie temperature TC of 100℃, which cannot meet the requirements of some automotive and new energy products that require both high permeability and high Curie temperature.

[0040] The present invention relates to a high-permeability manganese-zinc ferrite broadband material, KAH150, which achieves a permeability ui in the range of 10000-15000±25% at frequencies of 10-200kHz. This represents a significant improvement over existing technologies.

[0041] The material described in this invention has a Curie temperature Tc > 130℃, which is 30℃ higher than existing materials with the same temperature, meeting the requirements of automotive and new energy products.

[0042] The material of this invention includes a main component and secondary components; the main component is a mixture of Fe2O3, ZnO and MnO, and the secondary component is a mixture of added dopant materials MoO3, Bi2O3, CaCO3, V2O5, CuO, TiO2, Co2O3 and WO3.

[0043] The main components of this invention are formulated in the following proportions: Fe2O3 51.2%-54.5 mol%, ZnO 19.1%-22.40 mol%, and MnO 23.5%-26.7 mol%.

[0044] The byproducts of this invention are the added dopants, namely: MoO3 0.01-0.05 wt%, Bi2O3 0.01-0.04 wt%, CaCO3 0.005-0.04 wt%, V2O5 0.01-0.04 wt%, CuO 0.02-0.05 wt%, TiO2 0.01-0.05 wt%, Co2O3 0.01-0.04 wt%, and WO3 0.01-0.05 wt%.

[0045] The key point of this invention is the effective combination of dopant types and amounts, which results in uniform grain size within the magnetic core, reduces porosity, and forms a new material with high density and a more rational microstructure. The sintering densification process of this invention also plays a significant role in ensuring uniform crystallization within the product. The high-permeability manganese-zinc ferrite broadband material KAH150 of this invention requires densification during sintering to ensure uniform grain growth, reduce porosity, and improve microstructure.

[0046] Example 1:

[0047] like Figure 1 As shown, the preparation method of the high-permeability manganese-zinc ferrite broadband material KAH150 includes the following steps:

[0048] 1) Obtain the raw materials according to the following ratio: Fe2O3 52.34 mol%, ZnO 22.03 mol%, MnO 25.63 mol%. Then, add an appropriate amount of deionized water to the sand mill and sand mill for 45 minutes, and then perform spray granulation.

[0049] 2) Place the above spray-granulated material into a pre-firing furnace and pre-fire it at a temperature of 860℃ for 3 hours.

[0050] 3) For the pre-fired granules mentioned above, the amount of trace elements added as a secondary component, relative to the total weight of the main components, is as follows:

[0051] MoO3 is 0.02 wt%, Bi2O3 is 0.02 wt%, CaCO3 is 0.01 wt%, V2O5 is 0.015 wt%, TiO2 is 0.03 wt%, CuO is 0.02 wt%, Co2O3 is 0.015 wt%, WO3 is 0.02 wt%, and 8 trace elements are added.

[0052] 4) Place the powder containing the main and secondary components into a sand mill for secondary sand milling. The secondary sand milling time is 105 minutes, and the average particle size is controlled to be 0.80-0.85μm. 20 minutes before the end of the secondary sand milling, add a PVA solution with a percentage concentration of 8% at 10% of the powder weight. Then spray granulation is performed, and the powder is sieved through 60 mesh and 180 mesh.

[0053] 5) Press the above granules into T25-15-8 blanks, controlling the blank density to be between 3.00 and 3.10 g / cm³. 3 .

[0054] 6) Sinter the T25-15-8 blank in a bell-shaped kiln. The sintering holding temperature is 1360-1440℃ and the holding time is 5-8 hours. In the heating section, the temperature is 900-1150℃ and the heating rate is 1.0℃ / min. The oxygen content is controlled at 0.1%-1.0%. Except for the last hour when the oxygen content is 8%, the holding section is air sintering.

[0055] Comparative Example 1:

[0056] The preparation method of the high-permeability manganese-zinc ferrite broadband material KAH150 includes the following steps:

[0057] 1) Obtain the raw materials according to the following ratio: Fe2O3 52.34 mol%, ZnO 22.03 mol%, MnO 25.63 mol%. Then, add an appropriate amount of deionized water to the sand mill and sand mill for 45 minutes, and then perform spray granulation.

[0058] 2) Place the above spray-granulated material into a pre-firing furnace and pre-fire it at a temperature of 860℃ for 3 hours.

[0059] 3) For the pre-fired granules mentioned above, the amount of trace elements added as a secondary component, relative to the total weight of the main components, is as follows:

[0060] MoO3 is 0.02 wt%, Bi2O3 is 0.02 wt%, CaCO3 is 0.01 wt%, V2O5 is 0.01 wt%, TiO2 is 0.01-0.05 wt%, and 5 trace elements are added.

[0061] 4) Place the powder containing the main and secondary components into a sand mill for secondary sand milling. The secondary sand milling time is 105 minutes, and the average particle size is controlled to be 0.80-0.85μm. 20 minutes before the end of the secondary sand milling, add a PVA solution with a percentage concentration of 8% at 10% of the powder weight. Then spray granulation is performed, and the powder is sieved through 60 mesh and 180 mesh.

[0062] 5) Press the above granules into T25-15-8 blanks, controlling the blank density to be between 3.00 and 3.10 g / cm³. 3 .

[0063] 6) Sinter the T25-15-8 blank in a bell-shaped kiln. The sintering holding temperature is 1360-1440℃ and the holding time is 5-8 hours. In the heating section, the temperature is 900-1150℃ and the heating rate is 1.0℃ / min. The oxygen content is controlled at 0.1%-1.0%. Except for the last hour when the oxygen content is 8%, the holding section is air sintering.

[0064] Comparative Example 2:

[0065] The preparation method of the high-permeability manganese-zinc ferrite broadband material KAH150 includes the following steps:

[0066] 1) Obtain the raw materials according to the following ratio: Fe2O3 52.34 mol%, ZnO 22.03 mol%, MnO 25.63 mol%. Then, add an appropriate amount of deionized water to the sand mill and sand mill for 45 minutes, and then perform spray granulation.

[0067] 2) Place the above spray-granulated material into a pre-firing furnace and pre-fire it at a temperature of 860℃ for 3 hours.

[0068] 3) For the pre-fired granules mentioned above, the amount of trace elements added as a secondary component, relative to the total weight of the main components, is as follows:

[0069] MoO3 is 0.02 wt%, Bi2O3 is 0.02 wt%, CaCO3 is 0.01 wt%, V2O5 is 0.01 wt%, TiO2 is 0.02 wt%, CuO is 0.02 wt%, and 6 trace elements are added.

[0070] 4) Place the powder containing the main and secondary components into a sand mill for secondary sand milling. The secondary sand milling time is 105 minutes, and the average particle size is controlled to be 0.80-0.85μm. 20 minutes before the end of the secondary sand milling, add a PVA solution with a percentage concentration of 8% at 10% of the powder weight. Then spray granulation is performed, and the powder is sieved through 60 mesh and 180 mesh.

[0071] 5) Press the above granules into T25-15-8 blanks, controlling the blank density to be between 3.00 and 3.10 g / cm³. 3 .

[0072] 6) Sinter the T25-15-8 blank in a bell-shaped kiln. The sintering holding temperature is 1360-1440℃ and the holding time is 5-8 hours. In the heating section, the temperature is 900-1150℃ and the heating rate is 1.0℃ / min. The oxygen content is controlled at 0.1%-1.0%. Except for the last hour when the oxygen content is 8%, the holding section is air sintering.

[0073] The T25-15-8 samples from the above three schemes were kept at a constant temperature of 25 degrees Celsius for 3 hours, and then tested. The results are as follows. Figure 2 As shown.

[0074] The above results indicate that:

[0075] 1) The material of this invention has a median ui of 15,000 at a frequency of 10 kHz, but its permeability ui at a frequency of 200 kHz is more than twice that of traditional materials, and it has a very obvious advantage in high-frequency characteristics.

[0076] 2) The material of this invention uses a main component ratio with a Curie temperature of 130 degrees, which is 30 degrees higher than the current material with ui=15000 (Tc=100 degrees).

[0077] 3) The material of this invention allows customers to reduce the number of coil turns in EMI products during product design, thereby reducing costs, while obtaining better high-frequency and high-impedance characteristics, making it suitable for applications in the increasingly demanding automotive and new energy fields.

[0078] It is readily understood that, based on the several embodiments provided in this application, those skilled in the art can combine, split, or reorganize the embodiments of this application to obtain other embodiments, none of which exceed the protection scope of this application.

[0079] The above detailed embodiments further illustrate the purpose, technical solution, and beneficial effects of the embodiments of this application. It should be understood that the above are merely specific embodiments of the embodiments of this application and are not intended to limit the protection scope of the embodiments of this application. Any modifications, equivalent substitutions, improvements, etc., made on the basis of the technical solutions of the embodiments of this application should be included within the protection scope of the embodiments of this application.

Claims

1. High permeability Mn-Zn ferrite broadband material KAH150 material characterized in that, The material comprises a main component and a secondary component; the main component is a mixed material of Fe2O3, ZnO and MnO, the secondary component is a mixed material of added doping materials MoO3, Bi2O3, CaCO3, V2O5, CuO, TiO2, Co2O3 and WO3; the main component is in a proportioning mode that Fe2O3 is 51.2%-54.5mol%, ZnO is 19.1%-22.40mol% and MnO is 23.5%-26.7mol%; the secondary component is that the added doping materials are respectively MoO3 0.01-0.05wt%, Bi2O3 0.01-0.04wt%, CaCO3 0.005%-0.04wt%, V2O5 0.01-0.04wt%, CuO 0.02-0.05wt%, TiO2 0.01-0.05wt%, Co2O3 0.01-0.04wt% and WO3 0.01-0.05wt%.

2. The method of producing high permeability Mn-Zn ferrite broadband material KAH150 material according to claim 1, characterized in that, The method comprises the following steps: Step 1: primary ball milling: ingredients are proportioned according to the main component, and then the ingredients and deionized water are added into a sand mill for ball milling; Step 2: pre-burning: the ingredients of step 1 are dried and granulated, and then put into a pre-burning furnace for pre-burning; Step 3: secondary ball milling: the pre-burning ingredients of step 2 and the prepared secondary component are doped, added into a sand mill, and then deionized water is added for secondary sand milling, and a PVA solution with a percentage concentration of 8% is added 10 minutes before the end of the secondary sand milling, so as to prepare secondary slurry with an average particle size of 0.80-0.90μm; Step 4: granulation: the ingredients of step 3 are spray granulated to obtain granular ingredients with a mesh size of 80-120; Step 5: The above granules were pressed into T25-15-8 blanks by a press, blank density 3.00-3.15 g / cm 3 ; Step 6: the T25-15-8 blank is sintered in a bell jar kiln, the sintering and holding temperature is 1360-1440℃, the holding time is 5-8 hours, the kiln is cooled to 120 degrees before being lowered, and the sample is taken out and tested after being kept at a constant temperature of 22-27℃ for 3 hours.

3. The method of producing high permeability Mn-Zn ferrite broadband material KAH150 material according to claim 2, characterized in that, The pre-burning temperature of step 2 is 870-960℃, and the pre-burning time is 1-3 hours.

4. The method of producing high permeability Mn-Zn ferrite broadband material KAH150 material according to claim 2, characterized in that, The sintering of step 6 is in a heating section of 900-1150℃, and the heating rate is 1.0℃ / min, and the oxygen content is controlled to be 0.1%-1.0%.

5. The method of producing high permeability Mn-Zn ferrite broadband material KAH150 material according to claim 2, characterized in that, In the holding section of step 6, the oxygen content is 20% except for the last 1 hour, that is, air sintering.

6. The method of producing high permeability Mn-Zn ferrite broadband material KAH150 material according to claim 2, characterized in that, The step 6, the density of the sintered T25-15-8 sample is not less than 5.0 g / cm 3 .

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