WO2012151714A1 - Nicuzn ferrite material with high magnetic conductivity - Google Patents

Nicuzn ferrite material with high magnetic conductivity Download PDF

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WO2012151714A1
WO2012151714A1 PCT/CN2011/000805 CN2011000805W WO2012151714A1 WO 2012151714 A1 WO2012151714 A1 WO 2012151714A1 CN 2011000805 W CN2011000805 W CN 2011000805W WO 2012151714 A1 WO2012151714 A1 WO 2012151714A1
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ferrite material
ferrite
sintering
cuo
sintered
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PCT/CN2011/000805
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French (fr)
Chinese (zh)
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陆明岳
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临沂中瑞电子有限公司
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Priority to PCT/CN2011/000805 priority Critical patent/WO2012151714A1/en
Publication of WO2012151714A1 publication Critical patent/WO2012151714A1/en

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    • 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
    • C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
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    • 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
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Definitions

  • the invention relates to a high magnetic permeability NiCuZn ferrite material and a preparation method thereof. Background technique
  • chip inductors there are two types of chip inductors, one is a laminated chip inductor, and the other is a wound chip inductor.
  • Each of these two chip inductors has its outstanding advantages: The size of the laminated chip inductor can be made smaller, but due to the structure, the inductance cannot be made large, and the rated DC current allowed to pass is limited; Wire-wound chip inductors can make the inductor larger, and allow the rated DC current to pass larger, but it is difficult to make the size smaller. Therefore, the two chip inductors have different applications in different occasions, and the two complement each other and are indispensable.
  • the conventional high magnetic permeability NiZn ferrite has a high sintering temperature and is difficult to increase the sintered density, so that the product strength is also poor, and it is difficult to use the wound chip inductor application field.
  • NiCuZn ferrite material formed by introducing an appropriate amount of Cu in the NiZn ferrite material to replace part of Ni can not only significantly improve the sintering characteristics of the material, but also the magnetic permeability and bulk density of the material within a certain range. The strength has certain adjustment and improvement effects.
  • the NiCuZn ferrite material for the wound chip inductor was prepared by the oxide method.
  • the best way is to use the oxide method, optimize the material formulation, select more suitable trace elements and determine the optimal addition amount, determine the optimal sintering process parameters through a large number of process experiments, and thus obtain a higher magnetic permeability.
  • An object of the present invention is to provide a high magnetic permeability NiCuZn ferrite material for use in a wound chip inductor and a method of fabricating the same.
  • the invention provides a high magnetic permeability NiCuZn ferrite material, characterized in that: the material comprises a main component and an auxiliary component, and the main component is calculated as oxide content: Fe 2 0 3 is 47.5 ⁇ 49.8 mol%, ZnO It is 30 to 40 mol%, CuO is 5 to 15 mol%, and the balance is NiO; the auxiliary component includes K 2 C0 3 , Si0 2 , W0 3 , and the content of the auxiliary component is: K 2 C0 3 : 0.15 to 0.85 wt % , Si0 2 : 0.03 to 0.25 wt %, W0 3 : 0.15 to 0.35 wt %.
  • the NiCuZn ferrite material prepared by the invention is characterized in that it can be sintered at 1000 ° C or lower, and the obtained material has an initial magnetic permeability of up to 3350 at 25 ° C under the test conditions of 100 kHz and 0.25 mT.
  • the specific loss factor is less than 3.5 X 10" 6 , and the specific loss factor under the test conditions of 500 kHz and 0.25 mT is less than 12.6 X 10 - 6.
  • the relevant auxiliary components used in the present invention such as: K 2 C0 3 , Si0 2 , Wo 3, etc., the price is relatively low, which can greatly reduce the production cost.
  • a high magnetic permeability NiCuZn ferrite material preparation method steps are:
  • Raw materials are mixed and calcined: 47.5 to 49.8 mol% mol% of Fe 2 O 3 , 30 to 40 mol% mol% of ZnO, 5 to 15 mol% of CuO, and the remainder is NiO as a raw material, mixed and ground to 1.0. -3.0 ⁇ m, pre-fired after drying;
  • K 2 C0 3 0.15 to 0.85 wt %
  • Si0 2 0.03 to 0.25 wt %
  • W0 3 0.15 to 0.35 wt %.
  • the raw material is first sanded and spray-dried and granulated.
  • the weighed raw materials are placed in a sand mill, and equal weight of deionized water is added beforehand for sanding for about 0.5 hours.
  • About 10 is added to the raw material slurry.
  • the %PVA solution (concentration of about 10%) was subjected to spray drying granulation.
  • the spray-dried granulated powder is pre-fired through a rotary kiln at a calcination temperature of 750 to 800 °C.
  • Secondary sanding and spray drying granulation process :
  • the ferrite pre-sintered material and the auxiliary component are placed in a sand mill, and an equal weight of deionized water is added in advance, and sanded for 1 to 2 hours, so that the average particle size of the pre-sintered material is less than 1.0 ⁇ m; Approximately 10% PVA solution (concentration of about 10%) was added to the body slurry, and subjected to secondary spray drying granulation.
  • the ferrite blank is placed in a furnace for sintering at a sintering temperature of 950 to 1000 ° C, and the sintering time is particularly 10-20 hours, and the temperature is maintained for 3 to 5 hours.
  • the NiCuZn ferrite material prepared by the invention has uniform grain size, clear grain boundary, complete crystal grain and excellent high frequency characteristic; high density and mechanical strength, suitable for winding type chip
  • the invention replaces part of NiO with CuO, and at the same time adds some trace elements, such as: K 2 C0 3 , Si0 2 , W0 3 , so that the sintering temperature is greatly reduced, and the high magnetic permeability NiCuZn ferrite material prepared by the invention can be used in ⁇ Sintered below, which greatly improves the high-frequency electromagnetic properties of the material, improves the sintered density of the material, greatly improves the mechanical strength of the material, and satisfies the manufacturing process requirements of the wound-type chip inductor.
  • the obtained material is at 25 ° C. initial permeability of greater than 3350, than the loss factor under test conditions of less than 100kHz and 0.25mT 3.5 X 10_ 6, a loss factor than under the test conditions of less than 500kHz and 0.25mT 12.6 X 10- 6.
  • the auxiliary components used in the present invention such as K 2 C0 3 , Si0 2 , W0 3 , etc., are relatively inexpensive, which can greatly reduce the production cost, and at the same time, since the ferrite can be sintered at a lower temperature, it can be greatly save energy. detailed description
  • the invention provides a low-temperature sintering high magnetic permeability NiCuZn ferrite material and a preparation method thereof.
  • the optimum sintering process parameters were determined through a large number of experiments, so that the calcination temperature was lower than 800 ° C, and the sintering temperature was lower than 1000 ° C, which greatly improved.
  • the high-frequency electromagnetic properties of the material improve the sintering density of the material and improve the mechanical strength of the material, satisfying the manufacturing process requirements of the wound-type chip inductor, and on the other hand, saving energy and greatly reducing the manufacturing cost.
  • the initial magnetic permeability of the material at 25 ° C is as high as 3350, and the specific loss factor is less than 3.5 X ⁇ ⁇ under the test conditions of 100 kHz and 0.25 mT.
  • the specific loss factor is less than 12.6 X 10_ 6 under the test conditions of 500 kHz and 0.25 mT. .
  • a high magnetic permeability NiCuZn ferrite material is produced, and the selected raw materials are industrially pure Fe 2 O 3 , ZnO, NiO and CuO. Weigh all kinds of raw materials according to the formula for wet grinding, and the grinding equipment is sand mill. In the wet grinding process, add equal mass of deionized water and sand for about 0.5 hours to make the raw materials mix well.
  • the temperature range during calcination is 750 ⁇ 800°C. Since the main formula is Cu-rich formula, CuO can form CuFe204 at around 700 °C with Fe 2 0 3 , which makes the tip stone ferrite form at a very low temperature. This is very advantageous for promoting the subsequent sintering reaction and can effectively lower the sintering temperature.
  • the invention adopts a very effective combination of trace elements and uses K 2 C0 3 as a fluxing agent, which can effectively lower the sintering temperature, lower the sintering temperature below the crucible, and promote the effective growth of ferrite grains, so that the ferrite
  • the material has an initial permeability greater than 3350.
  • K 2 C0 3 due to the significant effect of K 2 C0 3 on promoting the liquid phase sintering of ferrite, it is easy to promote iron.
  • the oxygen crystal grains grow abnormally. Therefore, when K 2 C0 3 is added alone, the high frequency performance of the ferrite material is poor, and the specific loss coefficient is greater than 250 X 10-6 under the test conditions of 500 kHz and 0.25 mT.
  • the invention has found through a large number of experiments that W0 3 can effectively control the abnormal growth of ferrite grains, because W0 3 has a high melting point, and the radius of the W atom is large, and it is difficult to enter the inside of the ferrite grains. Thereby, abnormal growth of ferrite grains due to the addition of K 2 C0 3 can be effectively prevented. After adding Si0 2 , the high frequency electromagnetic properties of the material can be effectively improved.
  • auxiliary components K 2 C0 3 , Si0 2 , and W0 3 By the combination test of the addition amounts of the auxiliary components K 2 C0 3 , Si0 2 , and W0 3 , it was found that the auxiliary components were added in the following amounts: K 2 C0 3 : 0.15 to 0.85 wt %, Si0 2 : 0.03 to 0.25 wt %, When W0 3 : 0.15 to 0.35 wt%, excellent electromagnetic properties can be obtained.
  • the material can be sintered below 1000 ,, the obtained material has an initial permeability of more than 3350 at 25 ° C, and the specific loss factor under test conditions of 100 kHz and 0.25 mT is less than 3.5 X 10_ 6 , tested at 500 kHz and 0.25 mT. ratio of loss coefficient under conditions of less than 12.6 X 10- 6.
  • the invention obtains a good microstructure by adding W0 3 , the grain size of the ferrite material is uniform, the grain boundary is clear, the crystal grain is complete, the high frequency characteristic is excellent, and the ferrite density and mechanical strength are obviously improved, satisfying the winding. Manufacturing process requirements for wire chip inductors.
  • the high magnetic permeability NiCuZn ferrite material prepared by the invention and the preparation process are as follows:
  • the raw materials of the high magnetic permeability low-temperature sintered NiCuZn ferrite material provided by the present invention are industrially pure Fe 2 O 3 , ZnO, NiO and CuO.
  • the main composition and content of the ferrite material are calculated as oxides: Fe 2 0 3 is 47.5 to 49.8 mol%, ZnO is 30 to 40 mol%, and CuO is 5 to 15 mol%;
  • Pre-burning The primary spray granulated powder is pre-fired through a rotary kiln, and the calcination temperature is 750 to 800 °C.
  • auxiliary components The content of the auxiliary components is respectively K 2 C0 3 : 0.15 to 0.85 wt %, Si0 2 : 0.03 to 0.25 wt %, W0 3 : 0.15 to 0.35 wt% with respect to the total amount of the main components. %.
  • Secondary spray drying granulation Approximately 10% PVA solution (concentration of about 10%) is added to the ferrite slurry, and subjected to secondary spray drying granulation.
  • Sintering The ferrite blank is placed in a furnace for sintering, the sintering temperature is 950 ⁇ 1000 ° C, the sintering time is 10-20 hours, and the temperature is kept for 3 to 5 hours. Sintering is carried out in air without the need for a protective atmosphere.
  • the sintering equipment can be a box furnace, a bell furnace or a fully automatic pusher kiln.
  • NiCuZn ferrite material prepared by the process of the present invention can be realized in the sintered 100CTC the range, the initial permeability of greater than 3350, than the loss factor under test conditions of less than 100kHz and 0.25mT 3.5 X 10- 6, at 500kHz And the ratio of loss coefficient at 0.25mT test conditions of less than 12.6 X 10- 6.
  • the invention provides a high magnetic permeability NiCuZn ferrite material and a preparation method thereof.
  • the high-frequency electromagnetic properties of the material improve the sintering density of the material and improve the mechanical strength of the material, satisfy the manufacturing process requirements of the wound-type chip inductor, and on the other hand save energy and greatly reduce the manufacturing cost.
  • the following are specific examples to further illustrate the effects of the present invention.
  • the raw materials of the low-temperature sintered NiCuZn ferrite material are selected as industrial pure Fe 2 O 3 , ZnO, NiO, CuO.
  • the spray-dried granulated powder was pre-fired through a rotary kiln at a pre-firing temperature of 750 °C.
  • the ferrite pre-sintered material and the auxiliary component are placed in a sand mill, and an equal weight of deionized water is added in advance and sanded for 2 hours to make the average particle size of the pre-sintered material less than 1.0 ⁇ m;
  • the secondary spray-dried granulated ferrite powder is pressed into a ferrite-like ring blank.
  • the ferrite blank was placed in a box furnace for sintering at a temperature of 960 ° C for 3 hours, and sintering was carried out in the air without a protective atmosphere, and the furnace was cooled to room temperature.
  • Table 1 Test results of magnetic properties and density of sintered samples:
  • the raw materials of the low-temperature sintered NiCuZn ferrite material are selected as industrial pure Fe 2 O 3 , ZnO, NiO and CuO.
  • Fe 2 0 3 , ZnO, CuO and NiO were weighed according to Fe 2 0 3 of 48 mol%, ZnO of 35 mol%, CuO of 5 mol%, and NiO of 12 mol%.
  • the spray-dried granulated powder was pre-fired through a rotary kiln at a pre-firing temperature of 760 °C.
  • the secondary spray-dried granulated ferrite powder is pressed into a ferrite-like ring blank.
  • the raw materials of the low-temperature sintered NiCuZn ferrite material are selected as industrial pure Fe 2 O 3 , ZnO, NiO and CuO.
  • the spray-dried granulated powder was pre-fired through a rotary kiln at a calcination temperature of 780 °C.
  • the secondary spray-dried granulated ferrite powder is pressed into a ferrite-like ring blank.
  • the ferrite blank was placed in a box furnace for sintering at a temperature of 990 ° C for 3 hours, and sintering was carried out in the air without a protective atmosphere, and the furnace was cooled to room temperature.

Abstract

A NiCuZn ferrite material with high magnetic conductivity and the preparation method thereof. The ferrite material comprises Fe2O3, ZnO, CuO and NiO as main components, and auxiliary components. The main components comprise 47.5-49.8mol% of Fe2O3, 30-40mol% of ZnO, 5-15mol% of CuO, and balance of NiO. The auxiliary components comprise 0.15-0.85wt% of K2CO3, 0.03-0.25wt% of SiO2 and 0.15-0.35wt% of WO3 based on the total amount of the main components. By the addition of auxiliary components, the sintering temperature of the NiCuZn ferrite material with high magnetic conductivity is significantly lowered compared to the conventional way, and the material can be sintered at the temperature of 1000℃ below. On the one hand, not only the high-frequency electromagnetic properties of the material are significantly improved, but also the sintered density and mechanical strength are enhanced, and the higher magnetic conductivity is obtained, on the other hand energy is saved and production cost is reduced significantly. The NiCuZn ferrite material has a initial permeability of ≥3350 at 25℃, a loss coefficient of ＜3.5×10-6 under the testing condition of 100kHz, 0.25mT, and a loss coefficient of ＜12.6×10-6 under the testing condition of 500kHz, 0.25mT.

Description

一种高磁导率 NiCuZn铁氧体材料 技术领域  High magnetic permeability NiCuZn ferrite material technical field
本发明涉及一种高磁导率 NiCuZn铁氧体材料及其制备方法。 背景技术  The invention relates to a high magnetic permeability NiCuZn ferrite material and a preparation method thereof. Background technique
现代电子技术的不断进步， 要求电子设备不断向小型化、 轻量化、 薄型化方向发展， 另 外为适应现代通讯、 网络技术、 计算机、 视听设备、 电子办公设备、 汽车电子***、 军用及 航空航天电子以及电磁兼容 (EMC)的需要，作为三大无源器件之一的片式电感器也获得了较 大的发展。  The continuous advancement of modern electronic technology requires electronic devices to continue to be smaller, lighter, and thinner. In addition, it is suitable for modern communication, network technology, computers, audio-visual equipment, electronic office equipment, automotive electronic systems, military and aerospace electronics. As well as the need for electromagnetic compatibility (EMC), chip inductors, one of the three major passive components, have also achieved significant development.
从结构上来说， 片式电感器有两种， 一是叠层片式电感器， 另一种是绕线式片式电感器。 这两种片式电感器各有其突出的优点： 叠层片式电感器尺寸可以做得更小， 但由于结构的原 因， 电感量不能做得很大， 而且允许通过的额定直流电流有限； 绕线式片式电感器则可以将 电感做得较大， 而且允许通过的额定直流电流可以较大， 但尺寸做得更小有困难。 因此， 这 两种片式电感器在不同的场合有不同的应用， 两者相互补充， 缺一不可。  Structurally speaking, there are two types of chip inductors, one is a laminated chip inductor, and the other is a wound chip inductor. Each of these two chip inductors has its outstanding advantages: The size of the laminated chip inductor can be made smaller, but due to the structure, the inductance cannot be made large, and the rated DC current allowed to pass is limited; Wire-wound chip inductors can make the inductor larger, and allow the rated DC current to pass larger, but it is difficult to make the size smaller. Therefore, the two chip inductors have different applications in different occasions, and the two complement each other and are indispensable.
传统的高磁导率 NiZn铁氧体， 由于烧结温度高， 且烧结密度难以提高， 因此， 产品强度 也较差， 难以用到绕线式片式电感器应用领域。  The conventional high magnetic permeability NiZn ferrite has a high sintering temperature and is difficult to increase the sintered density, so that the product strength is also poor, and it is difficult to use the wound chip inductor application field.
通过在 NiZn铁氧体材料中引入适量的 Cu取代部分 Ni而形成的 NiCuZn铁氧体材料，不 仅可以显著改善材料的烧结特性， 而且在一定的范围内还对材料的磁导率、体密度及强度都 有一定的调整和改善作用。 国外最早开发了利用氧化物法制备用于绕线式片式电感器的 NiCuZn铁氧体材料。  The NiCuZn ferrite material formed by introducing an appropriate amount of Cu in the NiZn ferrite material to replace part of Ni can not only significantly improve the sintering characteristics of the material, but also the magnetic permeability and bulk density of the material within a certain range. The strength has certain adjustment and improvement effects. The NiCuZn ferrite material for the wound chip inductor was prepared by the oxide method.
早期用于绕线式片式电感器的 NiCuZn铁氧体材料， 尽管与传统 NiZn材料相比， 烧结温 度己降低到 1150°C左右， 但在高频及机械强度方面仍然不能满足新型绕线式片式电感器进 一步向小型化方向的发展需求。 为此， 必须在配方及烧结工艺上作进一步改进。  The early NiCuZn ferrite material used for wound-type chip inductors, although the sintering temperature has been reduced to about 1150 °C compared with the conventional NiZn material, it still cannot meet the new winding type in terms of high frequency and mechanical strength. Chip inductors are further demanding in the direction of miniaturization. To this end, further improvements must be made in the formulation and sintering process.
为了降低烧结温度， 改善材料的性能， 目前主要采取的措施主要有以下几类：  In order to reduce the sintering temperature and improve the performance of the material, the main measures currently taken are as follows:
1、 采取或发明新的制备方法取代原有的氧化物法。 例如共沉淀法、 溶胶凝胶法、 溶胶- 凝胶自蔓延燃烧法、 水热法和自蔓延法等。 虽然这些方法都各自有其特点， 也在一定程度上 克服了氧化物法的一些缺陷，但制造成本过高，另外工艺控制及稳定性方面与氧化物法相比， 还是存在着许多的不足， 技术也不够成熟， 对环境还有一定程度的污染。  1. Take or invent a new preparation method to replace the original oxide method. For example, coprecipitation method, sol-gel method, sol-gel self-propagating combustion method, hydrothermal method, and self-propagation method. Although these methods have their own characteristics, they have overcome some defects of the oxide method to a certain extent, but the manufacturing cost is too high, and there are still many shortcomings in the process control and stability compared with the oxide method. It is also not mature enough to have a certain degree of pollution to the environment.
2、 添加助熔剂。 在以往的制造方法或发明中， 通常添加 Bi203、 V205、 Mo03、 In203以 及其他有关氧化物的组合作为助熔剂， 虽然对于降低烧结温度有一定的效果，但随着助熔剂 的添加， 材料的损耗增大， 使得产品的性能下降； 另外， 由于这些氧化物的价格很高， 大大 增加了生产成本； 因此， 必须寻找更为合适的微量添加元素。 3、 调整工艺， 细化粉料。 将粉料的平均粒度减小到亚微米或纳米级别， 增加了颗粒的比 表面积， 提高了粉料的活性， 但是单纯的减小粒度， 将对设备提出更高的要求， 不利于成本 的下降， 而且单纯通过调整工艺减小粒度也有一定的限度， 不能够无限的减小粒度， 当粒度 下降到一定程度后， 容易重新团聚。 2. Add flux. In the conventional production method or invention, a combination of Bi 2 O 3 , V 2 0 5 , Mo 0 3 , In 2 0 3 and other related oxides is usually added as a flux, and although it has a certain effect on lowering the sintering temperature, With the addition of flux, the loss of materials increases, and the performance of the product decreases. In addition, because of the high price of these oxides, the production cost is greatly increased; therefore, it is necessary to find a more suitable trace additive element. 3. Adjust the process and refine the powder. Reducing the average particle size of the powder to the sub-micron or nano-scale increases the specific surface area of the particles and increases the activity of the powder. However, simply reducing the particle size will place higher demands on the equipment, which is not conducive to cost reduction. Moreover, there is a certain limit to reducing the particle size simply by adjusting the process, and it is not possible to reduce the particle size indefinitely. When the particle size drops to a certain extent, it is easy to re-agglomerate.
因此， 最好的办法还是采用氧化物法， 通过优化材料配方， 选择更为合适的微量元素并 确定其最佳加入量，通过大量工艺实验确定最佳烧结工艺参数， 从而获得具有较高磁导率的 低温烧结 NiCuZn铁氧体材料。 发明内容  Therefore, the best way is to use the oxide method, optimize the material formulation, select more suitable trace elements and determine the optimal addition amount, determine the optimal sintering process parameters through a large number of process experiments, and thus obtain a higher magnetic permeability. The rate of low temperature sintering of NiCuZn ferrite materials. Summary of the invention
本发明的目的是提供一种应用于绕线式片式电感器的高磁导率 NiCuZn铁氧体材料及其 制备方法。  SUMMARY OF THE INVENTION An object of the present invention is to provide a high magnetic permeability NiCuZn ferrite material for use in a wound chip inductor and a method of fabricating the same.
本发明提供的一种高磁导率 NiCuZn铁氧体材料， 其特征是： 该材料包括主成分以及辅 助成分， 主成分以氧化物含量计算为： Fe203为 47.5〜49.8mol%、 ZnO为 30〜40mol%、 CuO 为 5〜15mol%， 余为 NiO; 所述辅助成分包括 K2C03、 Si02、 W03， 辅助成分的含量分别是： K2C03 ： 0.15〜0.85wt %、 Si02: 0.03〜0.25wt %、 W03: 0.15〜0.35wt %。 The invention provides a high magnetic permeability NiCuZn ferrite material, characterized in that: the material comprises a main component and an auxiliary component, and the main component is calculated as oxide content: Fe 2 0 3 is 47.5~49.8 mol%, ZnO It is 30 to 40 mol%, CuO is 5 to 15 mol%, and the balance is NiO; the auxiliary component includes K 2 C0 3 , Si0 2 , W0 3 , and the content of the auxiliary component is: K 2 C0 3 : 0.15 to 0.85 wt % , Si0 2 : 0.03 to 0.25 wt %, W0 3 : 0.15 to 0.35 wt %.
本发明制备的 NiCuZn铁氧体材料， 其特征是： 可以在 1000°C以下烧结而成， 获得的材 料在 25 °C下的起始磁导率高达 3350， 在 100kHz和 0.25mT的测试条件下的比损耗系数小于 3.5 X 10"6, 在 500kHz和 0.25mT的测试条件下的比损耗系数小于 12.6 X 10—6。 本发明所采用 的有关辅助成分， 如： K2C03、 Si02、 wo3等， 价格较为低廉， 这可以大大降低生产成本。 The NiCuZn ferrite material prepared by the invention is characterized in that it can be sintered at 1000 ° C or lower, and the obtained material has an initial magnetic permeability of up to 3350 at 25 ° C under the test conditions of 100 kHz and 0.25 mT. The specific loss factor is less than 3.5 X 10" 6 , and the specific loss factor under the test conditions of 500 kHz and 0.25 mT is less than 12.6 X 10 - 6. The relevant auxiliary components used in the present invention, such as: K 2 C0 3 , Si0 2 , Wo 3, etc., the price is relatively low, which can greatly reduce the production cost.
一种高磁导率 NiCuZn铁氧体材料制备方法的步骤为：  A high magnetic permeability NiCuZn ferrite material preparation method steps are:
( 1 ) 原材料混合并预烧： 取 47.5〜49.8mol%mol%的 Fe203、 30〜40mol%mol%的 ZnO、 5〜15mol%的 CuO， 余为 NiO作为原材料， 混合并研磨至 1.0-3.0 μ m， 烘干后进行预烧；(1) Raw materials are mixed and calcined: 47.5 to 49.8 mol% mol% of Fe 2 O 3 , 30 to 40 mol% mol% of ZnO, 5 to 15 mol% of CuO, and the remainder is NiO as a raw material, mixed and ground to 1.0. -3.0 μ m, pre-fired after drying;
(2)对预烧料进行辅助成分的添加： 采用 K2C03、 Si02、 W03作为添加剂， (2) Adding an auxiliary component to the pre-sintered material: using K 2 C0 3 , Si0 2 , W0 3 as an additive,
其中： K2C03 ： 0.15〜0.85wt %、 Si02: 0.03〜0.25wt %、 W03: 0.15〜0.35wt %。 Wherein: K 2 C0 3 : 0.15 to 0.85 wt %, Si0 2 : 0.03 to 0.25 wt %, W0 3 : 0.15 to 0.35 wt %.
(3 )砂磨或球磨： 将铁氧体预烧料及上述微量元素放入砂磨或球磨机进行研磨， 使预烧 料的平均粒度小于 1.0 μ ιη;  (3) sanding or ball milling: the ferrite pre-sintered material and the above-mentioned trace elements are ground in a sanding or ball mill to make the average particle size of the pre-sintered material less than 1.0 μm;
(4)干燥造粒并成型：将料浆进行喷雾干燥造粒，并将铁氧体粉粒料压制成铁氧体毛坯； (4) Dry granulation and molding: the slurry is spray-dried and granulated, and the ferrite powder pellet is pressed into a ferrite blank;
(5 ) 烧结： 将铁氧体毛坯放入炉内烧结， 烧结温度为 950〜1000°C， 烧结时间为 10-20 小时， 保温 3〜5小时。 (5) Sintering: The ferrite blank is placed in a furnace for sintering, the sintering temperature is 950~1000 ° C, the sintering time is 10-20 hours, and the temperature is kept for 3 to 5 hours.
具体的原材料混合和预烧工艺：  Specific raw material mixing and pre-burning processes:
原材料先进行一次砂磨并喷雾干燥造粒， 将称量好的原材料放入砂磨机中， 并在事前加 入等重量的去离子水， 砂磨 0.5 小时左右； 在原材料料浆中加入约 10%PVA溶液 （浓度为 10%左右）， 进行一次喷雾干燥造粒。 然后， 将一次喷雾干燥造粒粉料通过回转窑进行预烧， 预烧温度为 750〜800°C。 二次砂磨及喷雾干燥造粒工艺： The raw material is first sanded and spray-dried and granulated. The weighed raw materials are placed in a sand mill, and equal weight of deionized water is added beforehand for sanding for about 0.5 hours. About 10 is added to the raw material slurry. The %PVA solution (concentration of about 10%) was subjected to spray drying granulation. Then, the spray-dried granulated powder is pre-fired through a rotary kiln at a calcination temperature of 750 to 800 °C. Secondary sanding and spray drying granulation process:
将铁氧体预烧料及上述辅助成分放入砂磨机中， 并在事先加入等重量的去离子水， 砂磨 1〜2小时， 使预烧料的平均粒度小于 1.0 μ ιη; 在铁氧体料浆中加入约 10%PVA溶液 （浓度 为 10%左右）， 进行二次喷雾干燥造粒。  The ferrite pre-sintered material and the auxiliary component are placed in a sand mill, and an equal weight of deionized water is added in advance, and sanded for 1 to 2 hours, so that the average particle size of the pre-sintered material is less than 1.0 μm; Approximately 10% PVA solution (concentration of about 10%) was added to the body slurry, and subjected to secondary spray drying granulation.
成型与烧结工艺：  Forming and sintering process:
将铁氧体毛坯放入炉内烧结， 烧结温度为 950〜1000°C， 烧结时间尤其为 10-20小时， 保 温 3〜5小时。  The ferrite blank is placed in a furnace for sintering at a sintering temperature of 950 to 1000 ° C, and the sintering time is particularly 10-20 hours, and the temperature is maintained for 3 to 5 hours.
本发明的有益效果是： 利用本发明制备的 NiCuZn铁氧体材料晶粒尺寸均匀， 晶界清楚， 晶粒完整， 高频特性优良； 密度及机械强度较高， 适宜用于绕线式片式电感器的制造。 本发 明使用 CuO替代了部分 NiO， 同时添加一些微量元素， 例如： K2C03、 Si02、 W03， 使烧结 温度大大降低， 本发明制备的高磁导率 NiCuZn铁氧体材料可以在 ΙΟΟΟΌ以下烧结而成， 从 而大大改善材料的高频电磁性能， 又提高材料的烧结密度， 大大提高材料的机械强度， 满足 绕线式片式电感器的制造工艺要求,获得的材料在 25°C下的起始磁导率大于 3350，在 100kHz 和 0.25mT的测试条件下的比损耗系数小于 3.5 X 10_6，在 500kHz和 0.25mT的测试条件下的 比损耗系数小于 12.6 X 10— 6。 本发明所采用的有关辅助成分如： K2C03、 Si02、 W03等， 价 格较为低廉， 这可以大大降低生产成本,同时由于铁氧体可以在更低的温度下烧结， 因而可 以大大节省能源。 具体实施方式 The beneficial effects of the invention are as follows: the NiCuZn ferrite material prepared by the invention has uniform grain size, clear grain boundary, complete crystal grain and excellent high frequency characteristic; high density and mechanical strength, suitable for winding type chip The manufacture of inductors. The invention replaces part of NiO with CuO, and at the same time adds some trace elements, such as: K 2 C0 3 , Si0 2 , W0 3 , so that the sintering temperature is greatly reduced, and the high magnetic permeability NiCuZn ferrite material prepared by the invention can be used in ΙΟΟΟΌ Sintered below, which greatly improves the high-frequency electromagnetic properties of the material, improves the sintered density of the material, greatly improves the mechanical strength of the material, and satisfies the manufacturing process requirements of the wound-type chip inductor. The obtained material is at 25 ° C. initial permeability of greater than 3350, than the loss factor under test conditions of less than 100kHz and 0.25mT 3.5 X 10_ 6, a loss factor than under the test conditions of less than 500kHz and 0.25mT 12.6 X 10- 6. The auxiliary components used in the present invention, such as K 2 C0 3 , Si0 2 , W0 3 , etc., are relatively inexpensive, which can greatly reduce the production cost, and at the same time, since the ferrite can be sintered at a lower temperature, it can be greatly save energy. detailed description
以下， 说明本发明的实施方式。  Hereinafter, embodiments of the present invention will be described.
本发明提供了一种低温烧结高磁导率 NiCuZn铁氧体材料及其制备方法。 通过优化材料 配方，选择合适的辅助成分，并确定其最佳加入量，通过大量实验确定了最佳烧结工艺参数， 使预烧温度低于 800°C， 烧结温度低于 1000°C， 大大改善材料的高频电磁性能， 提高了材料 的烧结密度， 并提高了材料的机械强度， 满足了绕线式片式电感器的制造工艺要求， 另一方 面又节省能源，大大降低了生产制造成本。材料在 25°C下的起始磁导率高达 3350，在 100kHz 和 0.25mT的测试条件下的比损耗系数小于 3.5 X ΙθΛ在 500kHz和 0.25mT的测试条件下的 比损耗系数小于 12.6 X 10_6。 The invention provides a low-temperature sintering high magnetic permeability NiCuZn ferrite material and a preparation method thereof. By optimizing the material formulation, selecting the appropriate auxiliary components, and determining the optimum addition amount, the optimum sintering process parameters were determined through a large number of experiments, so that the calcination temperature was lower than 800 ° C, and the sintering temperature was lower than 1000 ° C, which greatly improved. The high-frequency electromagnetic properties of the material improve the sintering density of the material and improve the mechanical strength of the material, satisfying the manufacturing process requirements of the wound-type chip inductor, and on the other hand, saving energy and greatly reducing the manufacturing cost. The initial magnetic permeability of the material at 25 ° C is as high as 3350, and the specific loss factor is less than 3.5 X Ι θ under the test conditions of 100 kHz and 0.25 mT. The specific loss factor is less than 12.6 X 10_ 6 under the test conditions of 500 kHz and 0.25 mT. .
制造高磁导率 NiCuZn铁氧体材料， 所选择的原材料采用工业纯的 Fe203、 ZnO、 NiO和 CuO。 按照配方称取各种原材料进行湿磨， 混磨设备选用砂磨机。 在湿磨过程中， 加入等质 量的去离子水， 砂磨 0.5小时左右， 使得原材料充分混合均匀。 A high magnetic permeability NiCuZn ferrite material is produced, and the selected raw materials are industrially pure Fe 2 O 3 , ZnO, NiO and CuO. Weigh all kinds of raw materials according to the formula for wet grinding, and the grinding equipment is sand mill. In the wet grinding process, add equal mass of deionized water and sand for about 0.5 hours to make the raw materials mix well.
预烧时的温度范围为 750〜800°C， 由于主配方为富 Cu配方， CuO能够与 Fe203在 700 °C附近形成 CuFe204， 使得尖品石铁氧体能够在很低的温度形成， 这对于促进后续的烧结 反应是非常有利的， 并能够有效的降低烧结温度。 The temperature range during calcination is 750~800°C. Since the main formula is Cu-rich formula, CuO can form CuFe204 at around 700 °C with Fe 2 0 3 , which makes the tip stone ferrite form at a very low temperature. This is very advantageous for promoting the subsequent sintering reaction and can effectively lower the sintering temperature.
本发明采用了非常有效的微量元素添加组合， 采用 K2C03作为助熔剂， 能够有效的降低 烧结温度， 使得烧结温度降低到 ΙΟΟΟΌ以下， 并促进铁氧体晶粒有效生长， 使铁氧体材料 的初始磁导率大于 3350。 但由于 K2C03对促进铁氧体液相烧结的显著作用， 很容易促使铁 氧体晶粒异常生长， 因此， 当单独添加 K2C03时， 铁氧体材料的高频性能较差， 在 500kHz 和 0.25mT的测试条件下的比损耗系数大于 250 X 10-6。 The invention adopts a very effective combination of trace elements and uses K 2 C0 3 as a fluxing agent, which can effectively lower the sintering temperature, lower the sintering temperature below the crucible, and promote the effective growth of ferrite grains, so that the ferrite The material has an initial permeability greater than 3350. However, due to the significant effect of K 2 C0 3 on promoting the liquid phase sintering of ferrite, it is easy to promote iron. The oxygen crystal grains grow abnormally. Therefore, when K 2 C0 3 is added alone, the high frequency performance of the ferrite material is poor, and the specific loss coefficient is greater than 250 X 10-6 under the test conditions of 500 kHz and 0.25 mT.
为了获得优良的高频性能， 有必要引入某些氧化物， 来控制晶粒的异常生长。 本发明通 过大量的试验发现， W03能够有效控制铁氧体晶粒的异常生长， 这是由于 W03具有很高的 熔点， 同时 W原子半径较大， 很难进入铁氧体晶粒内部， 从而能够有效阻止因 K2C03的加 入所引起的铁氧体晶粒的异常生长。 加入 Si02后， 可以有效改善材料的高频电磁性能。 通 过对辅助成分 K2C03、 Si02、 W03的加入量的组合试验， 发现辅助成分的加入量分别是： K2C03 ： 0.15〜0.85wt %、 Si02: 0.03〜0.25wt %、 W03: 0.15〜0.35wt %时， 能够获得优良 的电磁性能。 材料可以在 1000Ό以下烧结， 获得的材料在 25°C下的起始磁导率大于 3350， 在 100kHz和 0.25mT的测试条件下的比损耗系数小于 3.5 X 10_6， 在 500kHz和 0.25mT的测 试条件下的比损耗系数小于 12.6 X 10—6。 In order to obtain excellent high frequency performance, it is necessary to introduce certain oxides to control the abnormal growth of crystal grains. The invention has found through a large number of experiments that W0 3 can effectively control the abnormal growth of ferrite grains, because W0 3 has a high melting point, and the radius of the W atom is large, and it is difficult to enter the inside of the ferrite grains. Thereby, abnormal growth of ferrite grains due to the addition of K 2 C0 3 can be effectively prevented. After adding Si0 2 , the high frequency electromagnetic properties of the material can be effectively improved. By the combination test of the addition amounts of the auxiliary components K 2 C0 3 , Si0 2 , and W0 3 , it was found that the auxiliary components were added in the following amounts: K 2 C0 3 : 0.15 to 0.85 wt %, Si0 2 : 0.03 to 0.25 wt %, When W0 3 : 0.15 to 0.35 wt%, excellent electromagnetic properties can be obtained. The material can be sintered below 1000 ,, the obtained material has an initial permeability of more than 3350 at 25 ° C, and the specific loss factor under test conditions of 100 kHz and 0.25 mT is less than 3.5 X 10_ 6 , tested at 500 kHz and 0.25 mT. ratio of loss coefficient under conditions of less than 12.6 X 10- 6.
本发明通过添加 W03获得了良好的显微结构， 铁氧体材料晶粒尺寸均匀， 晶界清楚， 晶 粒完整， 高频特性优良， 同时铁氧体密度及机械强度明显提高， 满足了绕线式片式电感器的 制造工艺要求。 The invention obtains a good microstructure by adding W0 3 , the grain size of the ferrite material is uniform, the grain boundary is clear, the crystal grain is complete, the high frequency characteristic is excellent, and the ferrite density and mechanical strength are obviously improved, satisfying the winding. Manufacturing process requirements for wire chip inductors.
本发明制备的高磁导率 NiCuZn铁氧体材料及制备过程具体说明如下：  The high magnetic permeability NiCuZn ferrite material prepared by the invention and the preparation process are as follows:
1、 原材料的选择和主配方设计： 本发明提供的高磁导率低温烧结的 NiCuZn铁氧体材料 的原材料， 选择工业纯的 Fe203、 ZnO、 NiO和 CuO。 铁氧体材料的主要组成及含量以氧化 物计算为： Fe203为 47.5〜49.8mol%、 ZnO为 30〜40mol%、 CuO为 5〜15mol%; 1. Selection of raw materials and main formula design: The raw materials of the high magnetic permeability low-temperature sintered NiCuZn ferrite material provided by the present invention are industrially pure Fe 2 O 3 , ZnO, NiO and CuO. The main composition and content of the ferrite material are calculated as oxides: Fe 2 0 3 is 47.5 to 49.8 mol%, ZnO is 30 to 40 mol%, and CuO is 5 to 15 mol%;
( 1 ) 原材料混合： 按照配方称取相应的原材料。  (1) Mixing raw materials: Weigh the corresponding raw materials according to the formula.
(2)一次砂磨： 将称量好的原材料放入砂磨机中， 并在事前加入等重量的去离子水， 砂 磨 0.5小时左右； 平均粒度一般控制在 1.0-3.0 μ ηι。  (2) One sanding: Put the weighed raw materials into the sander and add equal weight of deionized water beforehand for sanding for about 0.5 hours; the average particle size is generally controlled at 1.0-3.0 μ ηι.
(3 ) 一次喷雾干燥造粒： 在原材料料浆中加入约 10%PVA溶液 （浓度为 10%左右）， 进行一次喷雾干燥造粒。  (3) One spray drying granulation: Add about 10% PVA solution (concentration: about 10%) to the raw material slurry, and perform spray drying granulation.
(4) 预烧： 将一次喷雾造粒粉料通过回转窑进行预烧， 预烧温度为 750〜800°C。  (4) Pre-burning: The primary spray granulated powder is pre-fired through a rotary kiln, and the calcination temperature is 750 to 800 °C.
(5)辅助成分的添加： 相对所述主成分总量， 辅助成分的含量分别是： K2C03 ： 0.15〜 0.85wt %、 Si02: 0.03〜0.25wt %、 W03: 0.15〜0.35wt %。 (5) Addition of auxiliary components: The content of the auxiliary components is respectively K 2 C0 3 : 0.15 to 0.85 wt %, Si0 2 : 0.03 to 0.25 wt %, W0 3 : 0.15 to 0.35 wt% with respect to the total amount of the main components. %.
(6)二次砂磨： 将铁氧体预烧料及上述杂质放入砂磨机中， 并在事先加入等重量的去离 子水， 砂磨 2小时， 使预烧料的平均粒度小于 Ι μ ηι;  (6) Secondary sanding: Put the ferrite pre-sintered material and the above-mentioned impurities into the sand mill, and add an equal weight of deionized water in advance, sanding for 2 hours, so that the average particle size of the pre-sintered material is less than Ι μ Ηι;
(7) 二次喷雾干燥造粒： 在铁氧体料浆中加入约 10%PVA溶液 （浓度为 10%左右）， 进 行二次喷雾干燥造粒。  (7) Secondary spray drying granulation: Approximately 10% PVA solution (concentration of about 10%) is added to the ferrite slurry, and subjected to secondary spray drying granulation.
(8) 成型： 对二次喷雾干燥造粒铁氧体粉料进行压制成铁氧体毛坯。  (8) Molding: The secondary spray-dried granulated ferrite powder is pressed into a ferrite blank.
(9) 烧结： 将铁氧体毛坯放入炉内烧结， 烧结温度为 950〜1000°C， 烧结时间为 10-20 小时， 保温 3〜5小时。 烧结在空气中进行， 无需保护气氛， 烧结设备可以是箱式炉、 钟罩 炉或者是全自动推板窑。  (9) Sintering: The ferrite blank is placed in a furnace for sintering, the sintering temperature is 950~1000 ° C, the sintering time is 10-20 hours, and the temperature is kept for 3 to 5 hours. Sintering is carried out in air without the need for a protective atmosphere. The sintering equipment can be a box furnace, a bell furnace or a fully automatic pusher kiln.
通过本发明方法制备的 NiCuZn铁氧体材料能够实现在 100CTC以下范围内烧结， 起始磁 导率大于 3350，在 100kHz和 0.25mT的测试条件下的比损耗系数小于 3.5 X 10—6，在 500kHz 和 0.25mT的测试条件下的比损耗系数小于 12.6 X 10—6。 本发明提供了一种高磁导率 NiCuZn 铁氧体材料及其制备方法。通过优化材料配方，选择合适的辅助成分，并确定其最佳加入量， 通过大量实验确定了最佳烧结工艺参数， 使预烧温度低于 800°C， 烧结温度低于 1000°C， 大 大改善材料的高频电磁性能， 提高了材料的烧结密度， 并提高了材料的机械强度， 满足了绕 线式片式电感器的制造工艺要求， 另一方面又节省能源， 大大降低了生产制造成本。 以下是 具体实施例以进一步说明本发明的效果。 NiCuZn ferrite material prepared by the process of the present invention can be realized in the sintered 100CTC the range, the initial permeability of greater than 3350, than the loss factor under test conditions of less than 100kHz and 0.25mT 3.5 X 10- 6, at 500kHz And the ratio of loss coefficient at 0.25mT test conditions of less than 12.6 X 10- 6. The invention provides a high magnetic permeability NiCuZn ferrite material and a preparation method thereof. By optimizing the material formulation, selecting the appropriate auxiliary components, and determining the optimum addition amount, the optimum sintering process parameters were determined through a large number of experiments, so that the calcination temperature was lower than 800 ° C, and the sintering temperature was lower than 1000 ° C, which greatly improved. The high-frequency electromagnetic properties of the material improve the sintering density of the material and improve the mechanical strength of the material, satisfy the manufacturing process requirements of the wound-type chip inductor, and on the other hand save energy and greatly reduce the manufacturing cost. The following are specific examples to further illustrate the effects of the present invention.
实施例 1 :  Example 1
( 1 )原材料的选择：提供的低温烧结的 NiCuZn铁氧体材料的原材料选择工业纯的 Fe203、 ZnO、 NiO、 CuO。 (1) Selection of raw materials: The raw materials of the low-temperature sintered NiCuZn ferrite material are selected as industrial pure Fe 2 O 3 , ZnO, NiO, CuO.
(2)成分设计与称料：按照主成分 Fe203为 49.0mol%、ZnO为 31mol%、CuO为 12mol%、 NiO为 8mol%， 称取相应重量的 Fe203、 ZnO、 CuO和 NiO。 (2) Composition design and weighing: According to the main component Fe 2 0 3 is 49.0 mol%, ZnO is 31 mol%, CuO is 12 mol%, NiO is 8 mol%, and the corresponding weights of Fe 2 O 3 , ZnO, CuO and NiO.
(3 ) 原材料的混合： 将称好的原材料放入砂磨机中， 加入等重量的去离子水， 砂磨 0.5 小时。  (3) Mixing of raw materials: Put the weighed raw materials into a sand mill, add equal weight of deionized water, and sand for 0.5 hours.
(4) 一次喷雾干燥造粒：  (4) One spray drying granulation:
在原材料料浆中加入约 10%PVA溶液 （浓度为 10%左右）， 进行一次喷雾干燥造粒。 Approximately 10% PVA solution (concentration of about 10%) was added to the raw material slurry, and spray drying granulation was carried out once.
(5 ) 预烧： (5) Pre-burning:
将一次喷雾干燥造粒粉料通过回转窑进行预烧， 预烧温度为 750°C。  The spray-dried granulated powder was pre-fired through a rotary kiln at a pre-firing temperature of 750 °C.
(6)辅助成分添加：  (6) Addition of auxiliary ingredients:
K2C03 ： 0.25 wt %, Si02: 0.15wt %、 W03: 0.15wt %。 K 2 C0 3 : 0.25 wt %, Si0 2 : 0.15 wt %, W0 3 : 0.15 wt %.
( 7) 二次砂磨：  (7) Secondary sanding:
将铁氧体预烧料及上述辅助成分放入砂磨机中， 并在事先加入等重量的去离子水， 砂磨 2小时， 使预烧料的平均粒度小于 1.0 μ m;  The ferrite pre-sintered material and the auxiliary component are placed in a sand mill, and an equal weight of deionized water is added in advance and sanded for 2 hours to make the average particle size of the pre-sintered material less than 1.0 μm;
( 8 ) 二次喷雾干燥造粒：  (8) Secondary spray drying granulation:
在铁氧体料浆中加入约 10%PVA溶液 （浓度为 10%左右）， 进行二次喷雾干燥造粒。 Approximately 10% PVA solution (concentration of about 10%) was added to the ferrite slurry, and subjected to secondary spray drying granulation.
(9) 成型： (9) Forming:
对二次喷雾干燥造粒铁氧体粉料进行压制成铁氧体样环毛坯。  The secondary spray-dried granulated ferrite powder is pressed into a ferrite-like ring blank.
( 10) 烧结：  (10) Sintering:
将铁氧体毛坯放入箱式炉内烧结， 烧结温度为 960°C， 保温 3小时， 烧结在空气中进行， 无需保护气氛， 随炉冷却到室温。  The ferrite blank was placed in a box furnace for sintering at a temperature of 960 ° C for 3 hours, and sintering was carried out in the air without a protective atmosphere, and the furnace was cooled to room temperature.
制备好的样环的磁性能测试在 HP4284A 阻抗分析仪上进行， 样品的密度采用浮力法测 量。 样品的磁性能和密度测试结果如表 1所示：  The magnetic properties of the prepared sample loops were tested on an HP4284A impedance analyzer and the density of the samples was measured by buoyancy. The magnetic properties and density test results of the samples are shown in Table 1:
表 1 : 烧结样品的磁性能和密度的测试结果:  Table 1: Test results of magnetic properties and density of sintered samples:
初始磁导率 比损耗系数 (Ταη δ / μ ί) 编号 密度 （Kg/m3 ) 测试频率 ( ΙΟΚΗζ) Initial permeability ratio loss factor (Ταη δ / μ ί ) Number density (Kg/m3 ) Test frequency ( ΙΟΚΗζ)
ΙΟΟΚΗζ 500KHz 样品 1 5.33 3355 3.5 X 10"6 12.6 X 10"6 实施例 2: ΙΟΟΚΗζ 500KHz Sample 1 5.33 3355 3.5 X 10" 6 12.6 X 10" 6 Example 2:
( 1 )材料的选择： 提供的低温烧结的 NiCuZn铁氧体材料的原材料选择工业纯的 Fe203、 ZnO、 NiO和 CuO。 (1) Material selection: The raw materials of the low-temperature sintered NiCuZn ferrite material are selected as industrial pure Fe 2 O 3 , ZnO, NiO and CuO.
(2) 成分设计与称料： 按照 Fe203为 48mol%、 ZnO为 35mol%、 CuO为 5mol%、 NiO 为 12mol%称取相应重量的 Fe203、 ZnO、 CuO和 NiO。 (2) Composition design and weighing: Fe 2 0 3 , ZnO, CuO and NiO were weighed according to Fe 2 0 3 of 48 mol%, ZnO of 35 mol%, CuO of 5 mol%, and NiO of 12 mol%.
(3 ) 原材料的混合： 将称好的原材料放入砂磨机中， 加入等重量的去离子水， 砂磨 0.5 小时。  (3) Mixing of raw materials: Put the weighed raw materials into a sand mill, add equal weight of deionized water, and sand for 0.5 hours.
(4) 一次喷雾干燥造粒：  (4) One spray drying granulation:
在原材料料浆中加入约 10%PVA溶液 （浓度为 10%左右）， 进行一次喷雾干燥造粒。 Approximately 10% PVA solution (concentration of about 10%) was added to the raw material slurry, and spray drying granulation was carried out once.
( 5 ) 预烧： (5) Pre-burning:
将一次喷雾干燥造粒粉料通过回转窑进行预烧， 预烧温度为 760°C。  The spray-dried granulated powder was pre-fired through a rotary kiln at a pre-firing temperature of 760 °C.
(6)辅助成分添加：  (6) Addition of auxiliary ingredients:
K2C03 ： 0.80wt %、 Si02: 0.25wt %、 W03: 0.35wt %。 K 2 C0 3 : 0.80 wt %, Si0 2 : 0.25 wt %, W0 3 : 0.35 wt %.
(7) 二次砂磨：  (7) Secondary sanding:
将铁氧体预烧料及上述杂质放入砂磨机中， 并在事先加入等重量的去离子水， 砂磨 1.5 小时， 使预烧料的平均粒度小于 1.0 m;  Putting the ferrite pre-sintered material and the above impurities into a sand mill, and adding an equal weight of deionized water in advance, sanding for 1.5 hours, so that the average particle size of the pre-sintered material is less than 1.0 m;
( 8 ) 二次喷雾干燥造粒：  (8) Secondary spray drying granulation:
在铁氧体料浆中加入约 10%PVA溶液 （浓度为 10%左右）， 进行二次喷雾干燥造粒。 Approximately 10% PVA solution (concentration of about 10%) was added to the ferrite slurry, and subjected to secondary spray drying granulation.
(9) 成型： (9) Forming:
对二次喷雾干燥造粒铁氧体粉料进行压制成铁氧体样环毛坯。  The secondary spray-dried granulated ferrite powder is pressed into a ferrite-like ring blank.
( 10) 烧结： - 将铁氧体毛坯放入箱式炉内烧结， 烧结温度为 980°C， 保温 3小时， 烧结在空气中进行， 无需保护气氛， 随炉冷却到室温。  (10) Sintering: - The ferrite blank is placed in a box furnace for sintering at a temperature of 980 ° C for 3 hours. Sintering is carried out in air without a protective atmosphere and is cooled to room temperature with the furnace.
制备好的样环的磁性能测试在 HP4284A 阴抗分析仪上进行， 样品的密度采用浮力法测 量。 样品的磁性能和密度测试结果如表 2所示：  The magnetic properties of the prepared sample loops were tested on a HP4284A negative impedance analyzer and the density of the samples was measured by buoyancy. The magnetic properties and density test results of the samples are shown in Table 2:
表 2: 烧结样品的磁性能和密度的测试结果：  Table 2: Test results of magnetic properties and density of sintered samples:
Figure imgf000008_0001
实施例 3 :
Figure imgf000008_0001
Example 3 :
( 1 )材料的选择： 提供的低温烧结的 NiCuZn铁氧体材料的原材料选择工业纯的 Fe203、 ZnO、 NiO和 CuO。 (1) Material selection: The raw materials of the low-temperature sintered NiCuZn ferrite material are selected as industrial pure Fe 2 O 3 , ZnO, NiO and CuO.
(2)成分设计与称料：按照配方 Fe203为 48.5mol%、 ZnO为 32mol%、 CuO为 5.5mol%、 NiO为 14mol%， 称取相应重量的 Fe203、 ZnO、 CuO和 NiO。 (3 ) 原材料的混合： 将称好的原材料放入砂磨机中， 加入等重量的去离子水， 砂磨 0.5 小时。 (2) Composition design and weighing: according to the formulation Fe 2 0 3 is 48.5 mol%, ZnO is 32 mol%, CuO is 5.5 mol%, NiO is 14 mol%, and the corresponding weights of Fe 2 O 3 , ZnO, CuO and NiO. (3) Mixing of raw materials: Put the weighed raw materials into a sand mill, add equal weight of deionized water, and sand for 0.5 hours.
(4) 一次喷雾干燥造粒：  (4) One spray drying granulation:
在原材料料浆中加入约 10%PVA溶液 （浓度为 10%左右）， 进行一次喷雾干燥造粒。 Approximately 10% PVA solution (concentration of about 10%) was added to the raw material slurry, and spray drying granulation was carried out once.
(5 ) 预烧： (5) Pre-burning:
将一次喷雾干燥造粒粉料通过回转窑进行预烧， 预烧温度为 780°C。  The spray-dried granulated powder was pre-fired through a rotary kiln at a calcination temperature of 780 °C.
(6)辅助成分添加：  (6) Addition of auxiliary ingredients:
K2C03 ： 0.40wt %、 Si02: 0.20wt %、 W03: 0.30wt % K 2 C0 3 : 0.40 wt %, Si0 2 : 0.20 wt %, W0 3 : 0.30 wt %
(7) 二次砂磨：  (7) Secondary sanding:
将铁氧体预烧料及上述杂质放入砂磨机中， 并在事先加入等重量的去离子水， 砂磨 2.0 小时， 使预烧料的平均粒度小于 1.0 μ ηι;  Putting the ferrite pre-sintered material and the above impurities into a sand mill, and adding an equal weight of deionized water in advance, sanding for 2.0 hours, so that the average particle size of the pre-sintered material is less than 1.0 μ ηι;
(8) 二次喷雾干燥造粒：  (8) Secondary spray drying granulation:
在铁氧体料浆中加入约 10%PVA溶液 （浓度为 10%左右）， 进行二次喷雾干燥造粒。 Approximately 10% PVA solution (concentration of about 10%) was added to the ferrite slurry, and subjected to secondary spray drying granulation.
(9) 成型： (9) Forming:
对二次喷雾干燥造粒铁氧体粉料进行压制成铁氧体样环毛坯。  The secondary spray-dried granulated ferrite powder is pressed into a ferrite-like ring blank.
( 10) 烧结：  (10) Sintering:
将铁氧体毛坯放入箱式炉内烧结， 烧结温度为 990°C， 保温 3小时， 烧结在空气中进行， 无需保护气氛， 随炉冷却到室温。  The ferrite blank was placed in a box furnace for sintering at a temperature of 990 ° C for 3 hours, and sintering was carried out in the air without a protective atmosphere, and the furnace was cooled to room temperature.
制备好的样环的磁性能测试在 HP4284A 阴抗分析仪上进行， 样品的密度采用浮力法测 量。 样品的磁性能和密度测试结果如表 3所示： 表 3 : 烧结样品的磁性能和密度的测试结果:  The magnetic properties of the prepared sample loops were tested on a HP4284A negative impedance analyzer and the density of the samples was measured by buoyancy. The magnetic properties and density test results of the samples are shown in Table 3: Table 3: Test results of magnetic properties and density of sintered samples:
Figure imgf000009_0001
Figure imgf000009_0001

Claims

1、 一种高磁导率 NiCuZn铁氧体材料， 其特征在于： 该铁氧体材料包括主成分 Fe203、 ZnO、 CuO、 NiO及辅助成分， 主成分包含换算为（摩尔比） Fe203为 47.5〜49.8mol%、 ZnO 为 30〜40mol%、 CuO为 5〜15mol%， 余为 NiO; 所述辅助成分包括 K2C03、 Si02、 W03， 相对所述主成分总量， K2C03、 Si02、 \¥03的总含量为0.33^ %〜1.45\^ %； 1. A high magnetic permeability NiCuZn ferrite material, characterized in that: the ferrite material comprises a main component Fe 2 O 3 , ZnO, CuO, NiO and an auxiliary component, and the main component comprises a conversion (molar ratio) of Fe. 2 0 3 is 47.5 to 49.8 mol%, ZnO is 30 to 40 mol%, CuO is 5 to 15 mol%, and the balance is NiO; the auxiliary component includes K 2 C0 3 , Si0 2 , W0 3 , relative to the total principal component The total content of K 2 C0 3 , Si0 2 , and \¥0 3 is 0.33^%~1.45\^%;
本发明制备的 NiCuZn铁氧体材料， 其特征在于： 该材料可以在 1000Ό以下烧结而成， 获得的材料在 25°C下的起始磁导率大于 3350， 在 100kHz和 0.25mT的测试条件下的比损耗 系数小于 3.5 X 10-6， 在 500kHz和 0.25mT的测试条件下的比损耗系数小于 12.6 X 10-6。  The NiCuZn ferrite material prepared by the invention is characterized in that: the material can be sintered under 1000 ,, and the obtained material has an initial permeability at 25 ° C of more than 3350, under the test conditions of 100 kHz and 0.25 mT. The specific loss factor is less than 3.5 X 10-6, and the specific loss factor is less than 12.6 X 10-6 under the test conditions of 500 kHz and 0.25 mT.
2、 根据权利要求 1所述的一种高磁导率 NiCuZn铁氧体材料， 其特征在于： 所述辅助成 分相对于主成分的含量， 分别是： K2C03 ： 0.15〜0.85wt %、 Si02: 0.03〜0.25wt %、 W03: 0.15〜0.35wt %。 2. The high magnetic permeability NiCuZn ferrite material according to claim 1, wherein: the content of the auxiliary component relative to the main component is: K 2 C0 3 : 0.15 to 0.85 wt %, Si0 2 : 0.03 to 0.25 wt%, W0 3 : 0.15 to 0.35 wt%.
PCT/CN2011/000805 2011-05-09 2011-05-09 Nicuzn ferrite material with high magnetic conductivity WO2012151714A1 (en)

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CN103693949A (en) * 2013-11-19 2014-04-02 横店集团东磁股份有限公司 Soft magnetic NiCuZn ferrite material with characteristics of wide temperature range, low temperature coefficient, high frequency and low loss, and preparation method thereof
CN109400142A (en) * 2018-10-30 2019-03-01 歌尔股份有限公司 A kind of preparation method of nickel-copper-zinc ferrite material
CN109422531A (en) * 2017-08-25 2019-03-05 仝丹丹 A kind of ferritic preparation method of nickel tungsten
CN111128515A (en) * 2020-01-04 2020-05-08 深圳感通科技有限公司 Magnetic core, common mode inductor containing magnetic core and preparation process of common mode inductor

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Publication number Priority date Publication date Assignee Title
CN103693949A (en) * 2013-11-19 2014-04-02 横店集团东磁股份有限公司 Soft magnetic NiCuZn ferrite material with characteristics of wide temperature range, low temperature coefficient, high frequency and low loss, and preparation method thereof
CN109422531A (en) * 2017-08-25 2019-03-05 仝丹丹 A kind of ferritic preparation method of nickel tungsten
CN109400142A (en) * 2018-10-30 2019-03-01 歌尔股份有限公司 A kind of preparation method of nickel-copper-zinc ferrite material
CN109400142B (en) * 2018-10-30 2022-05-06 歌尔微电子股份有限公司 Preparation method of nickel-copper-zinc ferrite material
CN111128515A (en) * 2020-01-04 2020-05-08 深圳感通科技有限公司 Magnetic core, common mode inductor containing magnetic core and preparation process of common mode inductor
CN111128515B (en) * 2020-01-04 2021-06-01 深圳感通科技有限公司 Magnetic core, common mode inductor containing magnetic core and preparation process of common mode inductor

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