CN102992752A - 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 that being used as the products such as inducer, wave filter, pulse transformer in the electronicss such as program control communication, digital technique, network communication colour TV makes its miniaturization, the requisite electronic material of lightweight, improve constantly the resistivity in the magneticsubstance, it is the pursuit of being engaged in these professional engineering technical personnel and production firm always, and the performance index of material are all unsatisfactory such as loss, frequency response 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 may further comprise the steps:

(1) joins major ingredient: be in molar ratio Fe 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 ₂Lanthanum trioxide with 0.03-0.05wt%; Described modified Nano carbon prepares by the following method:

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

B, usefulness 10-15% hydrochloric acid soln soaked 2-3 hour;

C, with deionized water wash repeatedly is neutral to the trees ashes, oven dry;

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%, fully be mixed to get;

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

(3) pre-burning: the major ingredient that step (1) is prepared adds water and dispersion agent carried out one time ball milling 50-60 minute, and then spraying drying is carried out pre-burning, and calcined temperature is 850-900 ℃, and the pre-burning time is 1-2 hour;

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

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

(6) sintering: put the moulded blank after the above-mentioned moulding into sintering oven, in the nitrogen atmosphere of the long-pending content of 0.08%-0.1% oxysome, be warming up to 680-710 ℃ with 150-165 ℃ of/hour speed first, be incubated 1-2 hour; In the nitrogen atmosphere of the long-pending content of 0.8%-1% oxysome, when being warming up to 860-900 ℃ with 128-132 ℃ of/hour speed, be incubated 0.5-1 hour; In the nitrogen atmosphere of the long-pending content of 3%-5% oxysome, be warming up to 1250-1300 ℃ with 75-85 ℃ of/hour speed again, the sintered heat insulating time is 2.5-2.8 hour; In the nitrogen atmosphere of the long-pending content of 0.08%-0.1% oxysome, namely get the MnZn magnetic ferrite magnetic core after the cooling behind the sintering.

Beneficial effect of the present invention:

1, the present invention is by adding modified Nano powder, ZrO2 composition, can be used as the bridge keying action between the different material, the use feed distribution is better, density is high, the grain boundary resistance rate high, void content is low, crystal grain is large and even, the rational modification composition of raw materials, so that after magnetic core fires, have higher resistivity;

2, have higher dc superposition characteristic, solve the loose problem of magnetic core surface tissue, the product physical strength improves, resistivity rises, loss reduces thereby make;

3, the indexs such as power loss, frequency response characteristic, Curie temperature all have greatly improved.

Embodiment

Embodiment 1: the preparation method of manganese zinc (Mn-Zn) soft magnetic ferrite material may further comprise the steps:

(1) joins major ingredient: be in molar ratio Fe 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 ₂Lanthanum trioxide with 0.04wt%; Described modified Nano carbon prepares by the following method:

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

B, soaked 2-3 hour with 12% hydrochloric acid soln;

C, with deionized water wash repeatedly is neutral to the trees ashes, oven dry;

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, fully be mixed to get;

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

(3) pre-burning: the major ingredient that step (1) is prepared adds water and dispersion agent and carried out ball milling 55 minutes, and then spraying drying is carried out pre-burning, and calcined temperature is 875 ℃, and the pre-burning time is 1-2 hour;

(4) major ingredient, auxiliary material mix and secondary ball milling: the pre-burning major ingredient is added the auxiliary material of removing outside modified Nano powder, the ZrO2, add entry and dispersion agent and carried out secondary ball milling 1-1.5 hour, spraying drying, built in 180 order pellets;

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

(6) sintering: put the moulded blank after the above-mentioned moulding into sintering oven, in the nitrogen atmosphere of the long-pending content of 0.08%-0.1% oxysome, be warming up to 695 ℃ with 158 ℃ of/hour speed first, be incubated 1.5 hours; In the nitrogen atmosphere of the long-pending content of 0.8%-1% oxysome, when being warming up to 880 ℃ with 130 ℃ of/hour speed, be incubated 0.8 hour; In the nitrogen atmosphere of the long-pending content of 3%-5% oxysome, be warming up to 1280 ℃ with 80 ℃ of/hour speed again, the sintered heat insulating time is 2.5 hours; In the nitrogen atmosphere of the long-pending content of 0.08%-0.1% oxysome, namely get the MnZn magnetic ferrite magnetic core after the cooling behind the sintering.

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

Claims (1)

1. the preparation method of a manganese zinc (Mn-Zn) soft magnetic ferrite material is characterized in that may further comprise the steps:

(1) joins major ingredient: be in molar ratio Fe 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 ₂Lanthanum trioxide with 0.03-0.05wt%; Described modified Nano carbon prepares by the following method:

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

B, usefulness 10-15% hydrochloric acid soln soaked 2-3 hour;

C, with deionized water wash repeatedly is neutral to the trees ashes, oven dry;

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%, fully be mixed to get;

(3) pre-burning: the major ingredient that step (1) is prepared adds water and dispersion agent carried out one time ball milling 50-60 minute, and then spraying drying is carried out pre-burning, and calcined temperature is 850-900 ℃, and the pre-burning time is 1-2 hour;

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

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

(6) sintering: put the moulded blank after the above-mentioned moulding into sintering oven, in the nitrogen atmosphere of the long-pending content of 0.08%-0.1% oxysome, be warming up to 680-710 ℃ with 150-165 ℃ of/hour speed first, be incubated 1-2 hour; In the nitrogen atmosphere of the long-pending content of 0.8%-1% oxysome, when being warming up to 860-900 ℃ with 128-132 ℃ of/hour speed, be incubated 0.5-1 hour; In the nitrogen atmosphere of the long-pending content of 3%-5% oxysome, be warming up to 1250-1300 ℃ with 75-85 ℃ of/hour speed again, the sintered heat insulating time is 2.5-2.8 hour; In the nitrogen atmosphere of the long-pending content of 0.08%-0.1% oxysome, namely get the MnZn magnetic ferrite magnetic core after the cooling behind the sintering.