CN112661501B - NiZn ferrite material for high-frequency power conversion and preparation method thereof - Google Patents
NiZn ferrite material for high-frequency power conversion and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of electronic materials, and provides a NiZn ferrite material for high-frequency power conversion, wherein the main material of the NiZn ferrite material comprises the following components: 10.1-18.2mol% NiO, 33.2-53.1mol% Fe 2 O 3 18.2 to 30.5mol% of ZnO, the balance being CuO; the additive comprises the following components in percentage by weight: 0.01-0.20wt% of CaCO 3 、0.05‑0.25wt％SiO 2 0.05-0.30wt% CuO and 0.01-0.18wt% V 2 O 5 . The invention also provides a preparation method of the NiZn ferrite material, which comprises the following steps of (1) preparing a formula in a certain proportion; (2) primary ball milling; (3) pre-burning; (4) adding additives; (5) secondary ball milling; (6) forming; and (7) sintering. The NiZn ferrite material for high-frequency power conversion has the characteristics of high magnetic conductivity, high saturation magnetic induction intensity and high Curie temperature.
Description
Technical Field
The invention relates to the technical field of electronic materials, in particular to a NiZn ferrite material for high-frequency power conversion and a preparation method thereof.
Background
The rapid development of the electronic information industry requires the development of various electronic devices in the directions of high frequency, miniaturization, and integration. With improvements in the performance of transformers, inductors, chokes and other electromagnetic components, miniaturization of various electronic devices has advanced significantly. However, with the emergence of ultra-light and ultra-thin devices (such as notebook computers, LEDs, LCDs, PDPs, PDAs, etc.), higher demands are made for further miniaturization of components, and such ultra-light and ultra-thin devices require miniaturized DC-DC converters, filter inductors, signal amplification power inductors, and the like. The current commonly adopted miniaturization scheme is to encapsulate the wound magnetic core and then put the encapsulated wound magnetic core into an electronic device to realize the expected functions of the equipment. In recent years, high-frequency MnZn power ferrite materials have been widely used for mini DC-DC converters, inductors, and the like, but have two disadvantages per se. On one hand, the high-frequency MnZn power ferrite is limited by the bottleneck of the working frequency, can only stably work under 3MHz, and is limited by the working frequency; on the other hand, the MnZn ferrite has low resistivity, can be used by post-treatment process links such as coating or paint dipping and the like, and has the phenomenon of sparking discharge when used at high frequency. However, the NiZn ferrite material can just make up for the above deficiencies, and NiZn ferrite has high frequency stability of magnetic permeability and high resistivity (about 106 Ω · m), and can be directly wound into a coil without any post-treatment processes such as coating or paint dipping, etc., so as to avoid high-frequency sparking discharge of electronic devices, and provide important guarantee for further realizing miniaturization of electronic equipment and high-density installation of electronic devices. Due to the obvious advantages, the power supply has great business opportunity for further realizing high frequency, small size and light weight in the updating of the switching power supply and the like in an ultra-light and ultra-thin electronic system. In recent years, due to international higher requirements for high-density planar installation of electronic systems and electromagnetic interference and electromagnetic compatibility, electronic information products and household electrical appliance products are required to reach high power density and international and domestic electromagnetic compatibility standards, so that the requirement for the NiZn ferrite material applied to the electronic information products and the household electrical appliance products is higher and higher, and research and development of the NiZn ferrite for high-frequency power conversion has become a research and industrialization hotspot of the current magnetic material industry.
In recent years, significant companies and research and development organizations in foreign developed countries have paid much attention to the research and development of NiZn ferrite materials for high frequency power conversion, such as TDK, FDK, hitachi, sony, young Hwa in korea, philips in europe, epos, thomson, GE in the united states, ferroxcube, etc., and new materials are continuously introduced to the development needs of the electronic information industry, wherein the new materials are typically YN202 materials developed by Young Hwa in korea, and the performance characteristics thereof are as follows: mu i =1300 +/-20%, bs =360mT, tc =160 ℃, which is the current high density mounting electronic equipment, especially the plane display (important material in LED, LCD, PDP, etc.), domestic companies such as Zhejiang east magnet, tiantong electron, guangdong east sunlight, nanjing Jin Ning, etc. are also tracking and researching NiZn ferrite material adapting to the change of the demand, but the current NiZn ferrite material at home and abroad has the following main problems that 1) when the magnetic conductivity of the material reaches more than 1500, the saturation magnetic induction intensity Bs is about 250mT, the Curie temperature Tc is about 100 ℃, and the application occasion requirements of large current and high density mounting (the heat dissipation condition is limited) can not be met; 2) If the saturation induction density Bs is increased to 380mT and the Curie temperature Tc is about 170 ℃, the magnetic permeability of the material is reduced to below 800, and the requirement of miniaturization of electronic equipment (especially a flat display system) cannot be met.
Therefore, the development of the NiZn ferrite for high-frequency power conversion with the magnetic conductivity mu i of more than or equal to 1600, the room temperature saturation magnetic induction Bs of more than or equal to 380mT and the Curie temperature Tc of more than or equal to 200 ℃ is urgently needed in China, so that the current carrying capacity of an electronic system is improved, the power density is improved, the miniaturization is realized, and the reliability of the electronic system is improved. Publication number CN111205075a discloses a nickel-zinc ferrite material and a preparation method thereof, although the magnetic permeability is improved to a certain extent, the room temperature saturation magnetic induction and the curie temperature are still not high enough.
Content of application
The invention aims to provide a NiZn ferrite material for high-frequency power conversion and a preparation method thereof, which have the characteristics of high magnetic conductivity, high saturation magnetic induction intensity and high Curie temperature.
The embodiment of the invention is realized by the following technical scheme: the main body material of the NiZn ferrite material for high-frequency power conversion comprises: 10.1-18.2mol% NiO, 33.2-53.1mol% Fe 2 O 3 18.2-30.5mol% ZnO, the balance CuO; the additive comprises the following components in percentage by weight of the main material：0.01-0.20wt％CaCO 3 、0.05-0.25wt％SiO 2 0.05-0.30wt% CuO and 0.01-0.18wt% V 2 O 5 。
Further, the main body material of the NiZn ferrite material of the present invention includes: 12-1imol of NiO, 45-53mol% of Fe 2 O 3 20-25mol% ZnO, and the balance CuO; the additive comprises the following components in percentage by weight of the main material: 0.1-0.15wt.% CaCO 3 、0.1-0.2wt％SiO 2 0.1-0.2wt% of CuO and 0.1-0.15wt% of V 2 O 5 。
Preferably, the principal material of the NiZn ferrite material of the present invention includes: 14.6mol% NiO, 52.2mol% Fe 2 O 3 21.5mol% ZnO, 11.7mol% CuO; the additive comprises the following components in percentage by weight: 0.1wt% of CaCO 3 、0.1wt％SiO 2 0.25wt% CuO and 0.05wt% V 2 O 5 。
The preparation method of the NiZn ferrite material for high-frequency power conversion comprises the following preparation steps:
s1, formula: preparing the main body material according to the proportion;
s2, primary ball milling;
s3, pre-burning;
s4, additive: adding additives according to the mixture ratio;
s5, secondary ball milling;
s6, forming;
and S7, sintering.
Further, the primary ball milling in the step S2 is to uniformly mix the powder in the step S1 in a ball mill, and the grinding time is 0.5-3.5 hours.
Further, the pre-sintering in the step S3 is to dry the ball-milling material obtained in the step S2 and pre-sinter the ball-milling material in a furnace at 750-950 ℃ for 0.5-1.5 hours.
Further, the secondary ball milling in the step S5 is to ball mill the powder obtained in the step S4 in a ball mill for 2.5 to 5.5 hours, and the granularity of the powder is controlled between 0.8 and 1.2 mu m.
Further, the molding in step S6 is to dry the powder obtained in step S5, add 8-10wt% of PVA for granulation, and press-mold on a press.
Further, the sintering in step S7 is to sinter the blank obtained in step S6 in a microwave sintering furnace, and keep the temperature at 900-1050 ℃ for 1.5-2.5 hours. Further, in step S6, 9wt% of PVA was added.
Aiming at the requirements of the NiZn ferrite material for high-frequency power conversion at home and abroad at present, the invention provides the NiZn ferrite material for high-frequency power conversion and the preparation method thereof, and the guiding idea is as follows: ion occupancy mechanism, magnetic domain theory, exchange mechanism. Firstly, high-purity NiO and Fe are optimized 2 O 3 ZnO and CuO are used as raw materials, the ion occupying situation and the exchange action mechanism of the NiZn ferrite material for high-frequency power conversion are deeply analyzed, and the occupying distribution and the bond length and bond angle on the magnetic crystal position are regulated and controlled; secondly, according to the fluxing/crystal-resisting interaction mechanism of different additives to the NiZn ferrite material for high-frequency power conversion, caCO is adopted 3 、SiO 2 、CuO、V 2 O 5 Regulating and controlling the grain boundary/grain characteristics of the NiZn ferrite material for high-frequency power conversion by the additives; and finally, preparing the NiZn ferrite material for high-frequency power conversion, which has the characteristics of high magnetic conductivity, high saturation magnetic induction and high Curie temperature, by combining a sintering process of high-density uniform crystal grains on the premise of optimizing the preparation process of the formula, the additive and the powder.
The technical scheme of the embodiment of the invention at least has the following advantages and beneficial effects: by using CaCO in the invention 3 、SiO 2 、CuO、V 2 O 5 And regulating and controlling the grain boundary/grain characteristics of the NiZn ferrite material for high-frequency power conversion by the additives, thereby preparing the NiZn ferrite material for high-frequency power conversion with the characteristics of high magnetic conductivity, high saturation magnetic induction and high Curie temperature.
Detailed Description
Example 1
The preparation method of the NiZn ferrite material for high-frequency power conversion in the embodiment comprises the following steps:
s1, formula: the main material was changed to 10.1mol% of NiO and 33.2mol% of Fe 2 O 3 、18.2mol％ZnO，38.5mol％CuO；
S2, primary ball milling: uniformly mixing the powder obtained in the step S1 in a ball mill for 0.5 hour;
s3, pre-burning: drying the ball milling material obtained in the step S2, and respectively presintering in a furnace at 750 ℃ for 0.5 hour;
s4, additive: adding the following additives into the powder obtained in the step S3 according to the weight ratio of the powder to the main material: 0.01wt% of CaCO 3 、0.05wt％SiO 2 0.05wt% of CuO and 0.01wt% of V 2 O 5 ；
S5, secondary ball milling: ball-milling the powder obtained in the step S4 in a ball mill for 2.5 hours, wherein the granularity of the powder is controlled to be 0.8-1.0 mu m;
s6, forming: drying the powder obtained in the step S5, adding 8wt% of PVA for granulation, and performing compression molding on the powder on a press;
s7, sintering: and (5) sintering the blank obtained in the step (S6) in a microwave sintering furnace, and preserving heat for 1.5 hours at 900 ℃.
Example 2
The preparation method of the NiZn ferrite material for high-frequency power conversion in the embodiment comprises the following steps:
s1, formula: 18.2mol% of NiO and 51.1mol% of Fe as the host material 2 O 3 、30.5mol％ZnO，0.2mol％CuO；
S2, primary ball milling: uniformly mixing the powder obtained in the step S1 in a ball mill for 3.5 hours;
s3, pre-burning: drying the ball milling material obtained in the step S2, and respectively presintering in a furnace at 950 ℃ for 1.5 hours;
s4, additive: adding the following additives into the powder obtained in the step S3 according to the weight ratio of the powder to the main material: 0.20wt% of CaCO 3 、0.25wt％SiO 2 0.30wt% CuO and 0.18wt% V 2 O 5 ；
S5, secondary ball milling: ball-milling the powder obtained in the step S4 in a ball mill for 5.5 hours, wherein the granularity of the powder is controlled to be 1.0-1.2 mu m;
s6, forming: drying the powder obtained in the step S5, adding 1wt% PVA for granulation, and pressing and molding on a press;
s7, sintering: and (5) sintering the blank obtained in the step (S6) in a microwave sintering furnace, and preserving heat for 2.5 hours at 1050 ℃.
Example 3
The preparation method of the NiZn ferrite material for high-frequency power conversion in the embodiment comprises the following steps:
s1, formula: the main material was taken to be 14.6mol% NiO, 52.2mol% Fe 2 O 3 、21.5mol％ZnO，11.7mol％CuO；
S2, primary ball milling: uniformly mixing the powder obtained in the step S1 in a ball mill for 1.2 hours;
s3, pre-burning: drying the ball milling material obtained in the step S2, and respectively presintering in a furnace at 915 ℃ for 1.5 hours;
s4, additive: adding the following additives into the powder obtained in the step S3 according to the weight ratio of the main materials: 0.04wt% of CaCO 3 、0.16wt％SiO 2 0.19wt% CuO and 0.11wt% V 2 O 5 ；
S5, secondary ball milling: ball-milling the powder obtained in the step S4 in a ball mill for 3.5 hours, wherein the granularity of the powder is controlled to be 0.8-1.2 mu m;
s6, forming: drying the powder obtained in the step S5, adding 9wt% of PVA for granulation, and pressing and molding on a press;
s7, sintering: and (5) sintering the blank obtained in the step (S6) in a microwave sintering furnace, and keeping the temperature at 1020 ℃ for 2 hours.
Example 4
The preparation method of the NiZn ferrite material for high-frequency power conversion in the embodiment comprises the following steps:
s1, formula: the bulk material was 14.6mol% NiO, 52.2mol% Fe 2 O 3 、21.5mol％ZnO，11.7mol％CuO；
S2, primary ball milling: uniformly mixing the powder obtained in the step S1 in a ball mill for 1.2 hours;
s3, pre-burning: drying the ball milling material obtained in the step S2, and respectively presintering in a furnace at 915 ℃ for 1.5 hours;
s4, additive: adding the following additives into the powder obtained in the step S3 according to the weight ratio of the powder to the main material: 0.06wt% of CaCO 3 、0.14wt％SiO 2 0.21wt% CuO and 0.09wt% V 2 O 5 ；
S5, secondary ball milling: ball-milling the powder obtained in the step S4 in a ball mill for 3.5 hours, wherein the granularity of the powder is controlled to be 0.8-1.2 mu m;
s6, forming: drying the powder obtained in the step S5, adding 9wt% of PVA for granulation, and pressing and molding on a press;
s7, sintering: and (5) sintering the blank obtained in the step (S6) in a microwave sintering furnace, and keeping the temperature at 1020 ℃ for 2 hours.
Example 5
The preparation method of the NiZn ferrite material for high-frequency power conversion in the embodiment comprises the following steps:
s1, formula: the bulk material was 14.6mol% NiO, 52.2mol% Fe 2 O 3 、21.5mol％ZnO，11.7mol％CuO；
S2, primary ball milling: uniformly mixing the powder obtained in the step S1 in a ball mill for 1.2 hours;
s3, pre-burning: drying the ball milling material obtained in the step S2, and respectively presintering in a furnace at 915 ℃ for 1.5 hours;
s4, additive: adding the following additives into the powder obtained in the step S3 according to the weight ratio of the powder to the main material: 0.08wt.% CaCO 3 、0.12wt％SiO 2 0.23wt% CuO and 0.07wt% V 2 O 5 ；
S5, secondary ball milling: ball-milling the powder obtained in the step S4 in a ball mill for 3.5 hours, wherein the granularity of the powder is controlled to be 0.8-1.2 mu m;
s6, forming: drying the powder obtained in the step S5, adding 9wt% of PVA for granulation, and pressing and molding on a press;
s7, sintering: and (5) sintering the blank obtained in the step (S6) in a microwave sintering furnace, and keeping the temperature at 1020 ℃ for 2 hours.
Example 6
The preparation method of the NiZn ferrite material for high-frequency power conversion comprises the following steps:
s1, formula: the main material was taken to be 14.6mol% NiO, 52.2mol% Fe 2 O 3 、21.5mol％ZnO，11.7mol％CuO；
S2, primary ball milling: uniformly mixing the powder obtained in the step S1 in a ball mill for 1.2 hours;
s3, pre-burning: drying the ball milling material obtained in the step S2, and respectively presintering in a furnace at 915 ℃ for 1.5 hours;
s4, additive: adding the following additives into the powder obtained in the step S3 according to the weight ratio of the powder to the main material: 0.1wt% of CaCO 3 、0.10wt％SiO 2 0.25wt% CuO and 0.05wt% V 2 O 5 ；
S5, secondary ball milling: ball-milling the powder obtained in the step S4 in a ball mill for 3.5 hours, wherein the granularity of the powder is controlled to be 0.8-1.2 mu m;
s6, forming: drying the powder obtained in the step S5, adding 9wt% of PVA for granulation, and pressing and molding on a press;
s7, sintering: and (5) sintering the blank obtained in the step (S6) in a microwave sintering furnace, and keeping the temperature at 1020 ℃ for 2 hours.
Comparative examples 1 to 4
Comparative examples 1 to 4 are different from example 6 in the main components and additives, and the rest of the process is completely the same.
TABLE 1 Main and additive formulations for comparative examples 1-4
The test results of examples 3 to 6 and comparative examples 1 to 4 are shown in the following table 2:
TABLE 2 permeability, room temperature magnetic induction and Curie temperature results for examples 3-6, comparative examples 1-4
| μ i (@10kHz,25℃) | B s (@25℃) | T c (℃) | |
| Example 3 | 1625 | 382 | 200 |
| Example 4 | 1681 | 389 | 202 |
| Example 5 | 1715 | 392 | 202 |
| Example 6 | 1782 | 395 | 204 |
| Comparative example 1 | 2213 | 329 | 112 |
| Comparative example 2 | 2103 | 319 | 109 |
| Comparative example 3 | 2169 | 336 | 118 |
| Comparative example 4 | 2269 | 326 | 116 |
As can be seen from the data in Table 2, the NiZn ferrite material for high frequency power conversion and the preparation method thereof of the invention have the magnetic permeability>1600. Magnetic induction at room temperature B s >380mT, curie temperature T c >At 200 ℃. Compared with the comparative example, the magnetic permeability is lower, but the magnetic induction intensity at room temperature and the Curie temperature are obviously improved. The method has good application prospect in the aspects of improving the current carrying capacity of the electronic system, improving the power density, realizing miniaturization and improving the reliability of the electronic system.
The present invention has been described in terms of the preferred embodiment, and it is not intended to be limited to the embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A NiZn ferrite material for high-frequency power conversion is characterized by comprising a main body material and an additive; the host material includes: 10.1-18.2mol% NiO, 33.2-53.1mol% Fe 2 O 3 18.2 to 30.5mol% of ZnO, the balance being CuO;
the additive comprises the following components in percentage by weight of the main body material: 0.01-0.20wt% ofaCO 3 、0.05-0.25wt％SiO 2 0.05-0.30wt% CuO and 0.01-0.18wt% V 2 O 5 。
2. The NiZn ferrite material for high frequency power conversion according to claim 1, wherein the host material comprises: 12-16980% NiO, 45-53mol% Fe 2 O 3 20-25mol% ZnO, and the balance CuO;
the additive comprises the following components in percentage by weight: 0.1-0.15wt.% CaCO 3 、0.1-0.2wt％SiO 2 0.1-0.2wt% of CuO and 0.1-0.15wt% of V 2 O 5 。
3. The NiZn ferrite material for high frequency power conversion according to claim 1, wherein the host material comprises: 14.6mol% NiO, 52.2mol% Fe 2 O 3 、21.5mol％ZnO、11.7mol％CuO；
The additive comprises the following components in percentage by weight of the main body material: 0.1wt% of CaCO 3 、0.1wt％SiO 2 0.25wt% CuO and 0.05wt% V 2 O 5 。
4. A method for preparing a NiZn ferrite material for high frequency power conversion in accordance with any of claims 1-3, characterized by comprising the steps of:
s1, formula: preparing the main body material according to the proportion;
s2, primary ball milling;
s3, pre-burning;
s4, additive: adding additives according to the mixture ratio;
s5, performing secondary ball milling;
s6, forming;
and S7, sintering.
5. The method for preparing a NiZn ferrite material for high frequency power conversion according to claim 4, wherein the primary ball milling in step S2 is to mix the powder in step S1 uniformly in a ball mill for 0.5 to 3.5 hours.
6. The method for preparing a NiZn ferrite material for high frequency power conversion according to claim 4, wherein the pre-sintering in step S3 is to bake the ball-milled material obtained in step S2 and pre-sinter the ball-milled material in a furnace at 750-950 ℃ for 0.5-1.5 hours.
7. The method for preparing a NiZn ferrite material for high frequency power conversion according to claim 4, wherein the secondary ball milling in step S5 is to ball mill the powder obtained in step S4 in a ball mill for 2.5-5.5 hours, and the particle size of the powder is controlled to be 0.8-1.2 μm.
8. The method of claim 4, wherein the step S6 of forming is performed by drying the powder obtained in step S5, adding 8-10wt% PVA for granulation, and press-forming on a press.
9. The method for preparing a NiZn ferrite material for high frequency power conversion as claimed in claim 4, wherein the sintering in step S7 is carried out by sintering the blank obtained in step S6 in a microwave sintering furnace and maintaining the temperature at 900-1050 ℃ for 1.5-2.5 hours.
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| CN116283265A (en) * | 2023-04-14 | 2023-06-23 | 电子科技大学 | Low-temperature sintered NiCuZn power ferrite and preparation method thereof |
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