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CN-121974674-A - Manufacturing method of high-frequency manganese zinc ferrite material

CN121974674ACN 121974674 ACN121974674 ACN 121974674ACN-121974674-A

Abstract

The invention discloses a manufacturing method of a high-frequency manganese zinc ferrite material, and belongs to the technical field of ferrite soft magnetic materials. The manufacturing method comprises the steps of S1, primary batching, S2, primary ball milling, S3, primary sintering to obtain primary sintering powder, S4, secondary ball milling, namely adding an additive into the primary sintering powder, ball milling to obtain secondary ball milling powder, S5, granulating, namely adding a polyvinyl alcohol aqueous solution into the secondary ball milling powder, pre-pressing, grinding and sieving to obtain granules, S6, forming the granules into magnetic rings with T25 multiplied by 15 multiplied by 7.5 by compression, S7, secondary sintering, namely sintering the magnetic rings to obtain a sintered body, S8, aging, namely heating the sintered body to 300-500 ℃ from normal temperature for 60-180 min, preserving heat for 1-5 h, and cooling to normal temperature after 60-180 min to obtain the manganese zinc ferrite. The invention realizes low loss under high frequency condition, increases the use requirement of manganese zinc ferrite high frequency 2MHZ, and promotes the updating requirement of server power supply.

Inventors

  • YU JINGJING
  • GAO HONGLIANG
  • HUANG YOUDONG
  • LIU SHIHAO

Assignees

  • 安徽龙磁金属科技有限公司

Dates

Publication Date
20260505
Application Date
20251231

Claims (10)

  1. 1. A method for manufacturing a high-frequency manganese zinc ferrite material, comprising the steps of: S1, weighing main components for one time; S2, ball milling is carried out for the first time; s3, sintering for the first time to obtain primary sintering powder; S4, performing secondary ball milling, namely adding an additive into the primary sintering powder, and performing ball milling to obtain secondary ball milling powder; s5, granulating, namely adding a polyvinyl alcohol aqueous solution into the secondary ball milling powder, pre-pressing, grinding and sieving to obtain granules; S6, forming, namely pressing the particles into magnetic rings with T25 multiplied by 15 multiplied by 7.5; S7, sintering the magnetic ring for the second time to obtain a sintered body; And S8, aging, namely heating the sintered body to 300-500 ℃ from normal temperature for 60-180 min, preserving heat for 1-5 h, and cooling to normal temperature after 60-180 min to obtain the manganese-zinc ferrite.
  2. 2. The method for manufacturing a high-frequency manganese-zinc-ferrite material according to claim 1, wherein in the step S1, the main component is composed of 53.6-54.25 mol% of Fe 2 O 3 , 3.90-4.77 mol% of ZnO, and the balance of MnO.
  3. 3. The method for manufacturing the high-frequency manganese zinc ferrite material according to claim 1, wherein in the step S2, the specific step of primary ball milling is that the main component is put into a ball mill, ball milling is carried out for 0.5-3 hours, and primary ball milling powder is obtained after the obtained slurry is dried.
  4. 4. The method for manufacturing the high-frequency manganese zinc ferrite material according to claim 1, wherein in the step S3, the specific step of primary sintering is to heat the primary ball milling powder to 800-1000 ℃ at the speed of 200-300 ℃ per hour under the air atmosphere, keep the temperature for 1-3 hours, and cool the primary ball milling powder along with a furnace to obtain the primary sintering powder.
  5. 5. The method for manufacturing a high-frequency manganese-zinc-ferrite material according to claim 1, wherein in step S4, the additive comprises the following raw materials ：CaCO 3 ：0.03～0.09wt%、Nb 2 O 5 ：0.02～0.06wt%、SiO 2 ：0.006～0.012wt%、V 2 O 5 ：0.03～0.06wt%、Co 2 O 3 ：0.3～0.9wt%、ZrO 2 ：0.02～0.06wt%、Ta 2 O 5 ：0.003～0.015wt%.
  6. 6. The method for manufacturing a high-frequency manganese-zinc-ferrite material according to claim 1, wherein in the step S4, the ball milling time is 1 to 5 hours.
  7. 7. The method for manufacturing a high-frequency manganese-zinc ferrite material according to claim 1, wherein in the step S5, the addition amount of the polyvinyl alcohol aqueous solution is 8-10 wt% of the total weight of the powder after the secondary ball milling.
  8. 8. The method for producing a high-frequency manganese-zinc-ferrite material according to claim 1, wherein in step S5, the concentration of the aqueous polyvinyl alcohol solution is 8wt% to 10wt%.
  9. 9. The method for manufacturing the high-frequency manganese-zinc ferrite material according to claim 1, wherein in the step S7, the magnetic ring is sintered in a bell jar furnace by adopting a mode of balancing oxygen partial pressure, the temperature is raised from normal temperature to 950-1170 ℃ for 1-6 h, the temperature is kept at the highest temperature for 8-14 h, the oxygen partial pressure control range in the sintering atmosphere is 0.5% -4%, the temperature is lowered after the heat preservation is finished, the temperature is lowered from the highest sintering temperature to 500 ℃ for 10-20 h, and the temperature is lowered from 500 ℃ to 100 ℃ for 10-20 h, so that the sintered body is obtained.
  10. 10. The method of manufacturing a high frequency manganese zinc ferrite material according to claim 9, wherein the temperature reduction stage maintains an equilibrium partial pressure of oxygen matching the corresponding temperature before 950 ℃, and after 950 ℃, the oxygen concentration is reduced to 0, and the product is continuously cooled to normal temperature under nitrogen or vacuum environment.

Description

Manufacturing method of high-frequency manganese zinc ferrite material Technical Field The invention relates to the technical field of ferrite soft magnetic materials, in particular to a manufacturing method of a high-frequency manganese zinc ferrite material. Background With the development of the third generation semiconductor technology represented by gallium nitride (GaN), the server power supply is forward converted in the high frequency, flattening and integration directions, and the variable frequency working mode puts higher requirements on the soft magnetic ferrite material, so that the low-loss characteristic is required to be kept in a high frequency band of 2MHz or more so as to adapt to the higher transmission power requirement, and the server power supply is promoted to be updated. The high-frequency low-loss material with the frequency of 2MHz and above can be produced in an attempt by only a few manufacturers, and the low-loss material with the frequency range of 3MHz-5MHz is a difficult problem to be solved in industry. The core reasons of the existing material for overhigh loss in a high-frequency band include that eddy current loss and residual loss are increased due to larger grain size, a sintering process is imperfect, a sintering atmosphere and a temperature curve are difficult to accurately control by a conventional kiln, excessive growth of grains and stress of a sintered body are easy to cause, high-frequency loss is further deteriorated, the cooperative optimization of a formula and the sintering process is insufficient, and the loss is effectively reduced through the combination of component regulation and process improvement. The existing solution has obvious limitation, although the adjustment can be carried out by optimizing high-frequency powder and trying a sintering process, the traditional sintering method, such as a common kiln, unreasonable heating and cooling rate and heat preservation time, can not realize the balance of grain refinement and high-density sintering, and still is difficult to meet the core requirement of customers on high frequency and low loss. Therefore, developing a high-frequency low-loss Mn-Zn ferrite material which is suitable for frequency bands of 2MHz and above and has reasonable formula and special sintering process becomes a key for solving the bottleneck of high-frequency development of a server power supply. Disclosure of Invention The invention provides a manufacturing method of a high-frequency manganese zinc ferrite material, which can solve the problems that the traditional sintering method in the prior art cannot realize the balance of grain refinement and high-density sintering and still cannot meet the core requirement of customers on high frequency and low loss. The aim of the invention can be achieved by the following technical scheme: a manufacturing method of a high-frequency manganese zinc ferrite material comprises the following steps: S1, weighing main components for one time; S2, ball milling is carried out for the first time; s3, sintering for the first time to obtain primary sintering powder; S4, performing secondary ball milling, namely adding an additive into the primary sintering powder, and performing ball milling to obtain secondary ball milling powder; s5, granulating, namely adding a polyvinyl alcohol aqueous solution into the secondary ball milling powder, pre-pressing, grinding and sieving to obtain granules; S6, forming, namely pressing the particles into magnetic rings with T25 multiplied by 15 multiplied by 7.5; S7, sintering the magnetic ring for the second time to obtain a sintered body; And S8, aging, namely heating the sintered body to 300-500 ℃ from normal temperature for 60-180 min, preserving heat for 1-5 h, and cooling to normal temperature after 60-180 min to obtain the manganese-zinc ferrite. In the step S1, the main component comprises 53.6-54.25mol% of Fe 2O3, 3.90-4.77 mol% of ZnO and the balance of MnO. In the step S2, the specific step of primary ball milling is that the main components are put into a ball mill, ball milling is carried out for 0.5-3 hours, and primary ball milling powder is obtained after the obtained slurry is dried. In the step S3, the primary sintering is carried out by heating primary ball milling powder to 800-1000 ℃ at the speed of 200-300 ℃ per hour under air atmosphere, preserving heat for 1-3 h, and cooling along with a furnace to obtain primary sintering powder. Further, in step S4, the additive comprises the following raw materials ：CaCO3：0.03～0.09wt%、Nb2O5：0.02～0.06wt%、SiO2：0.006～0.012wt%、V2O5：0.03～0.06wt%、Co2O3：0.3～0.9wt%、ZrO2：0.02～0.06wt%、Ta2O5：0.003～0.015wt%. Further, in the step S4, the ball milling time is 1-5 hours. Further, in the step S5, the adding amount of the polyvinyl alcohol aqueous solution is 8-10wt% of the total weight of the powder after secondary ball milling, wherein the concentration of the polyvinyl alcohol aqueous solution is 8-10wt%. In step S7,