WO2015106568A1

WO2015106568A1 - Preparation process for mnzn soft ferrite having ultra-low value loss and high uq

Info

Publication number: WO2015106568A1
Application number: PCT/CN2014/085174
Authority: WO
Inventors: 李想; 张志宏
Original assignee: 四川省德阳博益磁性材料有限公司
Priority date: 2014-01-14
Filing date: 2014-08-26
Publication date: 2015-07-23
Also published as: CN103771850B; CN103771850A

Abstract

A preparation process for a MnZn soft ferrite material having an ultra-low value loss and a high uQ. The manufacturing process is: (1) powder: (1.1) powder formulation; (1.2) powder moisture content technology; (2) spray granulation; (3) pre-sintering; (4) mixing grinding granulation; (5) forming; (6) sintering; (7) detection; (8) vacuum coating. The uQ product is increased from the current industry and market level of around six hundred and fifty thousand to around one million, thereby enabling the MnZn soft ferrite material to have superior performance.

Description

Ultra low value loss high uQ-MnZn soft ferrite preparation process Technical Field:

The invention relates to an ultra-low value loss high uQ-MnZn soft ferrite material property and a preparation method thereof, and belongs to the high-end technical field of soft ferrite materials.

Background technique:

Soft ferrites are widely used in many fields such as household appliances, network communications, automotive electronics, and aerospace military defense. In recent years, its application fields have continued to deepen, and the demand for the performance of soft ferrites has been increasing and increasing.

High-uQ materials and high-Bs materials, which were originally used for low magnetic flux density (weak current) and high magnetic flux density (strong current), have overlapped and merged with each other, and new materials have been developed that combine all the characteristics including high-u materials. Suitable for both IT electronics and power electronics. Its main features are two high, two low, two width, namely high Bs, high DC superposition; low loss, low harmonic distortion; wide frequency, wide temperature.

As shown in FIG. 1, the prior art production process is:

(1) Formulation of materials: Confirm the purity, particle size and particle shape, specific surface area, uniformity, powder accumulation characteristics, impurity content and type, moisture content of raw materials, etc., and adjust and control by heat treatment and vibration ball milling. The impurities and the particle size and distribution of the raw and auxiliary materials control the specific surface area and the solid phase reaction activity of the raw materials.

(2)—Secondary ball mill: Adopt rolling ball mill, ball mill medium is steel ball, process conditions according to weight ratio steel ball: Raw material: Deionized water = 3: 1: 1 control, ball milling time 4~7 hours.

(3) Pre-burning: Select 800-950 °C pre-burning temperature, holding time 5-7 hours.

(4) Secondary ball milling: The process conditions are based on the weight ratio as a reference to make the steel ball: Raw material: Deionized water = 4: 1: 0. 5~0. 8 control, sanding time 2-3 hours.

(5) Granulation: Ensure that the particles have good sphericity, uniform particle size distribution and good particle flow. (6) Molding: Mold press molding, controlling the pressure and product density and single weight during molding.

(7) Sham burn: Increase product density.

(8) Sintering: Sintering the pressed core for 20-24 hours, the sintering temperature is controlled at

In the range of 1360-1400 °C, to ensure the comprehensive performance of the product.

(9) Detection: Test the magnetic properties of the product such as characteristics and inductance values.

(10) Coating: Coating on the surface of the core to increase the insulation properties of the core surface. Disadvantages of the prior art: It is impossible to achieve a comprehensive uQ of MnZn soft ferrite materials of more than 800,000, and the process is cumbersome, and energy saving and emission reduction effects are not achieved in terms of energy consumption.

Summary of the invention:

In view of the above problems, the technical problem to be solved by the present invention is to provide an ultra-low value loss high uQ-MnZn soft ferrite material property and a preparation process thereof.

The ultra-low value loss high uQ-MnZn soft ferrite material property and preparation process thereof are as follows:

(1), powder:

(1. 1), powder formula: In addition to the detection of the purity, particle size and particle shape of the raw materials, a database of raw and auxiliary materials is established on the proportion formulation of the materials to determine the purity, particle size, specific surface area, uniformity of the raw materials, The accumulation characteristics, impurity content and type, moisture content of the powder, establish a raw material testing and inspection system, establish testing methods and standards, and adjust and control the impurity and particle size of the raw and auxiliary materials by heat treatment and vibration ball milling. Distribution, control specific surface area and raw material solid phase reaction activity, so as to prepare high uQ materials for different product requirements of different customers;

(1. 2), powder moisture content technology: The advanced equipment is used to control and study the water content through the principle of high pressure atomization to achieve a reasonable range of water content;

(2), spray granulation: using spray drying granulation process, the particle size is more uniform, the consistency is better, the powder particle size can be controlled within the range of 3 - 5 μ ηι; (3), pre-burning: using 800 ° C -820 ° C pre-burning temperature, holding time is 4-5 hours;

(4), mixed grinding granulation: after the spray granulation for pre-burning, another granulation process;

(5), forming: a special mold press forming, controlling the water content of the incoming material, the pressure and the product density and the weight of the press molding, satisfying the molding density of 3. 0 - 3. 5 g / cm ³ ;

(6), sintering: The entire cycle of sintering is 20-22 hours. 5小时; The sintering temperature is controlled in the range of 1100 - 1150 ° C, the time is 2. 5-3. 5 hours;

(7), detection: Test the magnetic properties of the product such as characteristics, inductance value, positive and negative temperature (_25 °C - +125 °C) impact;

(002), vacuum coating: using vacuum vapor deposition coating technology to develop, the product can withstand voltage breakdown can reach 1800V, up to 3000V; the thickness of the coating layer is strictly controlled at 0. 002mm.

The beneficial effects of the invention are as follows: the uQ product of the MnZn soft ferrite material is increased to about 1 million, thereby making the material performance superior, better satisfying all the requirements of the customer, and being widely used in various industries to reduce the cost.

BRIEF DESCRIPTION OF THE DRAWINGS:

For ease of description, the present invention is described in detail by the following detailed description and drawings. Figure 1 is a flow chart of the production process in the background art;

2 is a flow chart of the fabrication of the present invention.

detailed description:

The present invention will be described below by way of specific embodiments shown in the accompanying drawings. However, it should be understood that the description is only illustrative, and is not intended to limit the scope of the invention. In addition, descriptions of well-known structures and techniques are omitted in the following description in order to avoid unnecessarily obscuring the inventive concept.

As shown in FIG. 2, the specific technical solution adopts the following technical solutions: Its production process is:

(1), powder: (1. 1), powder formula: In addition to the detection of the purity, particle size and particle shape of the raw materials, a database of raw and auxiliary materials is established on the proportion formulation of the materials to determine the purity, particle size, specific surface area, uniformity of the raw materials, The accumulation characteristics, impurity content and type, moisture content of the powder, establish a raw material testing and inspection system, establish testing methods and standards, and adjust and control the impurity and particle size of the raw and auxiliary materials by heat treatment and vibration ball milling. Distribution, control of specific surface area and raw material solid phase reaction activity, so as to prepare high uQ materials for different product requirements of different customers.

In the current raw material ratio database, from the influence of the crystal structure, grain growth, compactness and ultimate macroscopic magnetic properties of soft ferrite materials, some existing ingredients and formulas are as follows:

(1. 2), powder moisture content technology: Moisture content is one of the key control points of the product. If the moisture is too heavy, it will cause the product to stick during the press molding process, resulting in a decrease in density and difficulty in molding; 8%。 The moisture content of the product needs to be maintained at 0. 8%. The content, therefore, the control of moisture and its uniform water content is essential.

The advanced equipment is used to control and study the water content through the high-pressure atomization principle, to achieve a reasonable range of water content, improve the high performance of the material, and achieve the purpose of obtaining excellent high-uQ materials.

(2), spray granulation: using spray drying granulation process, the particle size is more uniform, consistent More preferably, the particle size of the powder can be controlled within the range of 3 - 5 μm; the particle has good sphericity, uniform particle size distribution, good particle flowability, and is advantageous for product densification.

(3), pre-burning: using 800 ° C -820 ° C pre-burning temperature, holding time 4-5 hours, increase the density, so that the solid phase reaction is complete, which is conducive to improve the electromagnetic properties of the sample.

(4) Mixing and granulating: After the granulation is carried out for pre-burning, a granulation process is carried out, which not only ensures the mixing effect of the powder but also reduces the energy.

(5), molding: special mold press molding, control the water content of the incoming material, pressure and product density and single weight during press molding, meet the molding density of 3. 0 - 3. 5 g / cm3, good consistency, for the next One step of sintering to lay the foundation.

(6) Sintering: Using the most advanced bell-type sintering equipment in the world, improving the sintering atmosphere and process, optimizing the sintering temperature, and exploring the influence of sintering conditions on grain size, uniformity, phase structure and phase composition, sintering temperature , the relationship between time and electromagnetic properties of ferrite materials.

The entire cycle of sintering is 20-22 hours. The sintering temperature is controlled in the range of 1100-1150 °C, and the time is guaranteed to be about 3 hours, so as to improve the consistency and stability of the product and ensure the comprehensive performance of the product. The review reduced the sintering time of the product by 20% and reduced production costs.

(7), Detection: Test the magnetic properties of the product such as characteristics, inductance value, positive and negative temperature (_25 °C - +125 °C) impact.

(8), vacuum coating: The use of advanced vacuum vapor deposition coating technology to develop, the product's withstand voltage breakdown can reach more than 1800V, up to 3000V or more. The thickness of the coating layer is strictly controlled to 0. 002mm, avoiding the use of an insulating layer that is too thin to cause the material to lose its protection. Excessive thickness also causes the insulation layer to rupture during the winding process, has no insulation effect, or affects the size problem used by the customer.

The specific embodiment will increase the uQ product from about 650,000 in the current industry and market to about 1 million, so that the performance of the MnZn soft ferrite material is superior, and the high uQ-MnZn material can better satisfy the high-end communication. , satellite navigation, anti-electromagnetic interference, electromagnetic In technologies such as capacitive technology, missile guidance, enemy and enemy identification, and electronic countermeasures, all the requirements of customers are met, thereby reducing costs.

The specific embodiment breaks the situation that the uQ product of the high-stability, low-loss and high-loss uQ material of the soft ferrite is about 600,000, and the uQ product is increased to about 1 million, thereby making the material performance superior and satisfying all the requirements of the customer. More widely used in various industries, especially in high-end communications or aerospace, defense technology, the requirements for soft ferrite materials, reduce the dependence on the import of such high-performance materials, promote industrial development and network filters and transformers, etc. Component costs are reduced.

The basic principles and main features of the present invention and the advantages of the present invention are shown and described above. It should be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, and that the present invention is only described in the foregoing embodiments and the description of the present invention, without departing from the spirit and scope of the invention. Various changes and modifications are intended to fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and their equivalents.

Claims

claims

1. The preparation process of ultra-low value and high loss uQ-MnZn soft magnetic ferrite is characterized by: Its production process is as follows:

(1), Powder:

(1. 1) Powder formula: In addition to testing and confirming the purity, particle size and particle shape of raw materials, a raw and auxiliary material database is established to determine the purity, particle size, specific surface area, uniformity, and Powder accumulation characteristics, impurity content and type, moisture content and other indicators, establish a raw material testing and inspection system, establish testing and inspection methods and standards, adjust and control the impurity content and particle size of raw and auxiliary materials through heat treatment and vibration ball milling, etc. Distribution, control the specific surface area and solid phase reactivity of raw materials, thereby formulating high uQ materials according to different product requirements put forward by different customers;

(1. 2) Powder moisture content technology: Use advanced equipment to control and research the moisture content through the principle of high-pressure atomization to achieve a reasonable range of moisture content;

(2) Spray granulation: Using the spray drying granulation process, the particle size is more uniform and the consistency is better. The size of the powder particles can be controlled within the range of 3-5 μm;

(3) Pre-burning: Use a pre-burning temperature of 800°C-820°C, and a holding time of 4-5 hours;

(4) Mixing and granulation: After spray granulation and pre-calcination, perform the granulation process again;

(5) Molding: Press and mold with a special mold to control the moisture content of the incoming material, the pressure during molding, the density and unit weight of the product, and meet the molding density of 3. 0-3. 5 g/cm ³ ;

(6) Sintering: The entire sintering cycle takes 20-22 hours. The sintering temperature is controlled within the range of 1100-1150°C, and the sintering time is 2.5-3.5 hours;

(7) Testing: Test the product’s characteristics, inductance value, positive and negative temperature (_25°C- +125°C) impact and other magnetic properties;

(8) Vacuum coating: Developed using vacuum vapor deposition coating technology, the product's voltage breakdown resistance can reach 1800V, up to 3000V; the thickness of the coating layer must be strictly controlled. Control at 0. 002mm.