CN102992752B - Method for preparing manganese-zinc (MnZn) soft magnetic ferrite - Google Patents

Abstract

The invention discloses a method for preparing a manganese-zinc (MnZn) soft magnetic ferrite, which comprises the following steps of: preparing a main ingredient, preparing an auxiliary ingredient, pre-sintering, mixing the main ingredient and the auxiliary ingredient, ball-milling twice, shaping and sintering to obtain the MnZn soft magnetic ferrite. According to the method for preparing the MnZn soft magnetic ferrite, modified nano-powder and ZrO2 ingredients are added to function as a bridge to join various raw materials, so the raw material distribution is better, the density is high, the grain boundary resistivity is high, the porosity is low, and the crystalline grain is large and uniform; the formula of the raw materials is reasonably improved, so the magnetic core has a higher resistivity after being sintered; and the method for preparing the MnZn soft magnetic ferrite greatly improves power loss, frequency characteristic, Curie temperature and other indexes.

Description

A kind of preparation method of manganese zinc (Mn-Zn) soft magnetic ferrite material

Technical field

The present invention relates to a kind of preparation method of manganese zinc (Mn-Zn) soft magnetic ferrite material.

Background technology

High resistivity ferromagnetic oxide powder, magnetic core are to realize in the electronic equipments such as program control communication, digital technology, network communication colour TV, being used as the products such as inductor, filter, pulse transformer and making its miniaturization, the requisite electronic material of lightweight, improve constantly the resistivity in magnetic material, it is the pursuit of being engaged in these professional engineers and technicians and production firm always, and the performance index of material are as all unsatisfactory in loss, frequency characteristic, Curie temperature etc.

Summary of the invention

In order to alleviate shortcomings and deficiencies of the prior art, the object of the present invention is to provide a kind of preparation method of manganese zinc (Mn-Zn) soft magnetic ferrite material.

The present invention adopts following technical scheme to achieve these goals:

The preparation method of manganese zinc (Mn-Zn) soft magnetic ferrite material, comprises the following steps:

(1) join major ingredient: be Fe in molar ratio ₂o ₃50.8-51.5mol, MnO 20.5-22.5mol, ZnO 26-27.5mol, nickel powder 0.2-0.35mol, iron powder 0.18-0.22mol prepare burden;

(2) join auxiliary material: the modified Nano carbon, the ZrO2 of 0.01-0.02%, the CaCO of 0.013-0.018wt% that are equivalent to major ingredient 0.009-0.011wt% ₃, 0.024-0.028wt% SiO ₂, 0.05-0.06wt% SnO ₂lanthana with 0.03-0.05wt%; Described modified Nano carbon is prepared by the following method:

A, trees ashes are soaked after 2-3 hour with the sodium hydroxide solution of 10-15%;

B, use 10-15% hydrochloric acid solution soak 2-3 hour;

C, washing repeatedly with deionized water, is neutral to trees ashes, dries;

D, be ground to 0.8-1.2 μ m powder, obtain modification trees ashes;

E, in nano-sized carbon, add and be equivalent to the modification trees ashes obtained above of its weight 3-5%, the nano silicon of 2-3%, be fully mixed to get;

The preparation method of described ZrO2 is as follows: attapulgite is put into high speed mixer and stir 3-5min, with a small amount of ethanol dissolved dilution NDZ-311 titanate coupling agent, the consumption of NDZ-311 titanate coupling agent is the 1-2% of attapulgite weight, add in high speed mixer with Sprayable, discharging after stirring 18-25min, ovendry power is broken into powder;

(3) pre-burning: the major ingredient that step (1) is prepared adds water and carries out ball milling 50-60 minute a time with dispersant, then spraying is dry, carries out pre-burning, and calcined temperature is 850-900 DEG C, and the pre-burning time is 1-2 hour;

(4) major ingredient, auxiliary material mix and secondary ball milling: pre-burning major ingredient is added to the auxiliary material of removing outside modified Nano powder, ZrO2, add water and dispersant to carry out secondary ball milling 1-1.5 hour, spraying is dried, built in 180-200 order pellet;

(5) moulding: secondary ball abrasive material is mixed with modified Nano powder, ZrO2,12800-14200 rev/min, high speed dispersion 2-2.5 hour, is then pressed into base;

(6) sintering: put the moulded blank after above-mentioned moulding into sintering furnace, in the blanket of nitrogen of 0.08%-0.1% oxygen volume content, be first warming up to 680-710 DEG C with 150-165 DEG C/h of speed, insulation 1-2 hour; In the blanket of nitrogen of 0.8%-1% oxygen volume content, while being warming up to 860-900 DEG C with 128-132 DEG C/h of speed, insulation 0.5-1 hour; In the blanket of nitrogen of 3%-5% oxygen volume content, then be warming up to 1250-1300 DEG C with 75-85 DEG C/h of speed, the sintered heat insulating time is 2.5-2.8 hour; After sintering, in the blanket of nitrogen of 0.08%-0.1% oxygen volume content, after cooling, obtain MnZn magnetic ferrite magnetic core.

Beneficial effect of the present invention:

1, the present invention is by adding modified Nano powder, ZrO2 composition, can be used as the bridge combination between different material, use feed distribution is better, density is high, grain boundary resistance rate is high, the porosity is low, crystal grain is large and even, rational modification composition of raw materials, after magnetic core is fired, there is higher resistivity;

2, there is higher DC superposition characteristic, solve the loose problem of magnetic core surface texture, thereby the raising of product mechanical strength, resistivity rising, loss are reduced;

3, the index such as power loss, frequency characteristic, Curie temperature all has greatly improved.

Embodiment

Embodiment 1: the preparation method of manganese zinc (Mn-Zn) soft magnetic ferrite material, comprises the following steps:

(1) join major ingredient: be Fe in molar ratio ₂o ₃51.2mol, MnO 21.5mol, ZnO 26.8mol, nickel powder 0.3mol, iron powder 0.2mol prepare burden;

(2) join auxiliary material: the modified Nano carbon, 0.015% ZrO2, the CaCO of 0.015wt% that are equivalent to major ingredient 0.01wt% ₃, 0.026wt% SiO ₂, 0.055wt% SnO ₂lanthana with 0.04wt%; Described modified Nano carbon is prepared by the following method:

A, trees ashes are soaked after 2-3 hour with 12% sodium hydroxide solution;

B, with 12% hydrochloric acid solution soak 2-3 hour;

C, washing repeatedly with deionized water, is neutral to trees ashes, dries;

D, be ground to 0.8-1.2 μ m powder, obtain modification trees ashes;

E, in nano-sized carbon, add and be equivalent to the modification trees ashes obtained above of its weight 4%, 2.5% nano silicon, be fully mixed to get;

The preparation method of described ZrO2 is as follows: attapulgite is put into high speed mixer and stir 3-5min, with a small amount of ethanol dissolved dilution NDZ-311 titanate coupling agent, the consumption of NDZ-311 titanate coupling agent is 1.5% of attapulgite weight, add in high speed mixer with Sprayable, discharging after stirring 18-25min, ovendry power is broken into powder;

(3) pre-burning: the major ingredient that step (1) is prepared adds water and carries out ball milling 55 minutes with dispersant, and then spraying is dry, carries out pre-burning, and calcined temperature is 875 DEG C, and the pre-burning time is 1-2 hour;

(4) major ingredient, auxiliary material mix and secondary ball milling: pre-burning major ingredient is added to the auxiliary material of removing outside modified Nano powder, ZrO2, add water and dispersant to carry out secondary ball milling 1-1.5 hour, spraying is dried, built in 180 order pellets;

(5) moulding: secondary ball abrasive material is mixed with modified Nano powder, ZrO2, and 13500 revs/min, high speed dispersion 2-2.5 hour, is then pressed into base;

(6) sintering: put the moulded blank after above-mentioned moulding into sintering furnace, in the blanket of nitrogen of 0.08%-0.1% oxygen volume content, be first warming up to 695 DEG C with 158 DEG C/h of speed, be incubated 1.5 hours; In the blanket of nitrogen of 0.8%-1% oxygen volume content, while being warming up to 880 DEG C with 130 DEG C/h of speed, be incubated 0.8 hour; In the blanket of nitrogen of 3%-5% oxygen volume content, then be warming up to 1280 DEG C with 80 DEG C/h of speed, the sintered heat insulating time is 2.5 hours; After sintering, in the blanket of nitrogen of 0.08%-0.1% oxygen volume content, after cooling, obtain MnZn magnetic ferrite magnetic core.

The performance data of the magnetic ferrite magnetic core making by above-described embodiment:

Claims (1)

1. a preparation method for manganese zinc (Mn-Zn) soft magnetic ferrite material, is characterized in that comprising the following steps:

(1) join major ingredient: be Fe in molar ratio ₂o ₃50.8-51.5mol, MnO 20.5-22.5mol, ZnO 26-27.5mol, nickel powder 0.2-0.35mol, iron powder 0.18-0.22mol prepare burden;

(2) join auxiliary material: be equivalent to the modified Nano carbon of major ingredient 0.009-0.011wt%, the ZrO of 0.01-0.02wt% ₂, 0.013-0.018wt% CaCO ₃, 0.024-0.028wt% SiO ₂, 0.05-0.06wt% SnO ₂lanthana with 0.03-0.05wt%; Described modified Nano carbon is prepared by the following method:

A, trees ashes are soaked after 2-3 hour with the sodium hydroxide solution of 10-15%;

B, use 10-15% hydrochloric acid solution soak 2-3 hour;

C, washing repeatedly with deionized water, is neutral to trees ashes, dries;

D, be ground to 0.8-1.2 μ m powder, obtain modification trees ashes;

E, in nano-sized carbon, add and be equivalent to the modification trees ashes obtained above of its weight 3-5%, the nano silicon of 2-3%, be fully mixed to get;

(3) pre-burning: the major ingredient that step (1) is prepared adds water and carries out ball milling 50-60 minute a time with dispersant, then spraying is dry, carries out pre-burning, and calcined temperature is 850-900 DEG C, and the pre-burning time is 1-2 hour;

(4) major ingredient, auxiliary material mix and secondary ball milling: pre-burning major ingredient is added and removes modified Nano carbon, ZrO ₂outside auxiliary material, add water and dispersant to carry out secondary ball milling 1-1.5 hour, spraying is dried, makes 180-200 order pellet;

(5) moulding: by secondary ball abrasive material and modified Nano carbon, ZrO ₂powder mixes, 12800-14200 rev/min, and high speed dispersion 2-2.5 hour, is then pressed into base;

(6) sintering: put the moulded blank after above-mentioned moulding into sintering furnace, in the blanket of nitrogen of 0.08%-0.1% oxygen volume content, be first warming up to 680-710 DEG C with 150-165 DEG C/h of speed, insulation 1-2 hour; In the blanket of nitrogen of 0.8%-1% oxygen volume content, while being warming up to 860-900 DEG C with 128-132 DEG C/h of speed, insulation 0.5-1 hour; In the blanket of nitrogen of 3%-5% oxygen volume content, then be warming up to 1250-1300 DEG C with 75-85 DEG C/h of speed, the sintered heat insulating time is 2.5-2.8 hour; After sintering, in the blanket of nitrogen of 0.08%-0.1% oxygen volume content, after cooling, obtain MnZn magnetic ferrite magnetic core.