CN103310936A - Low-loss Fe-based nanocrystalline soft magnetic powder core and manufacturing method thereof - Google Patents

Abstract

The invention discloses a low-loss Fe-based nanocrystalline soft magnetic powder core and a manufacturing method thereof. The ingredient of the alloy powder core forming the powder core is FeaSibBcCudMeYf, wherein M refers to C, P, Cr or Mn, the subscripts a, b, c, d, e, f represent corresponding atomic percent of alloying elements, and the following formulas are met: a is not less than 70 and not more than 90, b is not less than 2 and not more than 15, c is not less than 4 and not more than 13, d is not less than 0.4 and not more than 3, e is not less than 2 and not more than 8, f is less than 0 and not more than 5, and besides, the total percent of a, b, c, d, e and f equals to 100. The prepared magnetic powder core has smaller eddy-current loss, the preparation technology is simple, the formation is easy, the environmental protection is facilitated, and a certain cost advantage is guaranteed.

Description

A kind of low-loss Fe-based nanocrystalline magnetic powder core and preparation method thereof

technical field

The invention relates to the field of magnetic materials, in particular to a low-loss Fe-based nanocrystalline magnetic powder core and a preparation method thereof.

Background technique

Soft magnetic powder cores are widely used in electronic information, electrical engineering and medium and high frequency fields. With the development of the electronic industry, the requirements for the miniaturization of electronic products are getting higher and higher. In recent decades, in order to meet the development of the electronics industry, researchers from various countries have used different methods to prepare various soft magnetic powder cores with different magnetic properties. These magnetic powder cores are widely used in filters, frequency modulation choke coils and switching power supplies.

In 1921, Arnold and G.W.Elmen of the Westinghouse Company of the United States first pressed electrolytic iron powder into a magnetic powder core. They mainly used this magnetic powder core as a load inductance in telephone lines. Two years later, they developed a high magnetic permeability. Permalloy, and made it into a magnetic powder core in 1927, because of its good advantages, it was quickly industrialized, and it was widely used in the 1950s. In 1932, Japanese Masumoto and Hiroshi Yamamoto invented sendust. Since the invention was in Sendai, sendust is also called Sendust. However, it was not until the early 1980s that Sendust magnetic powder cores were successfully developed and gradually realized industrialization. In 1940, V.E.Legg and F.J.Given of Bell Laboratories in the United States developed an iron-nickel-molybdenum alloy magnetic powder core, which is composed of 81% nickel, 17% iron and 2% molybdenum. Because it contains about 2% molybdenum, the magnetic permeability and resistivity are greatly improved, and it has good time stability, small temperature coefficient, low loss and other advantages, and has attracted high attention since then. In the 1960s, the guidance and control part of the American MK-46II torpedo used this magnetic core extensively.

People have done a lot of work to make electronic devices adapt to the working environment of different frequency bands, so that they have high frequency, low loss, high Q value and other characteristics. At present, iron-nickel-molybdenum alloy magnetic powder cores occupy a major share in the high-end market, but their application has been limited due to the high cost of iron-nickel-molybdenum magnetic powder cores. In recent years, Fe-based nanocrystalline-amorphous soft magnetic powder cores have attracted much attention due to their low cost, simple preparation process, and excellent performance, and are expected to replace some uses of iron-nickel-molybdenum magnetic powder cores.

Contents of the invention

The purpose of the invention is to overcome the deficiencies of the prior art and provide a low-loss Fe-based nanocrystalline magnetic powder core and a preparation method thereof.

The composition of the low-loss Fe-based nanocrystalline magnetic powder core is: Fe _a Si _b B _c Cu _{d Me} Y _f , where M is C, P, Cr or Mn, subscripts a, b, c, d, e, f Indicates the atomic percentage of the corresponding alloying element, meeting the following conditions: 70≤a≤90, 2≤b≤15, 4≤c≤13, 0.4≤d≤3, 2≤e≤8, 0<f≤5; and a +b+c+d+e+f=100.

The steps of the preparation method of the low-loss Fe-based nanocrystalline magnetic powder core are as follows:

(1) After the Fe _a Si _b B _c Cu _d M _e Y _f amorphous ribbon is kept at 420 ° C for 1 h in a vacuum annealing furnace, it is mechanically crushed, where M is C, P, Cr or Mn, The subscripts a, b, c, d, e, and f represent the atomic percentages of the corresponding alloy elements, and satisfy the following conditions: 70≤a≤90,2≤b≤15,4≤c≤13,0.4≤d≤3,2 ≤e≤8,0<f≤5; and a+b+c+d+e+f=100;

(2) Fe _a Si _b B _c Cu _d M _e Y _f amorphous thin strips are mechanically crushed, and placed in a planetary ball mill for ball milling, the ball-to-material ratio is 5:1, the ball milling time is 4 hours, and the speed is 260r/min. Add ethanol to prevent oxidation, dry and sieve to obtain Fe _a Si _b B _c Cu _{d Me} Y _f magnetic powder with different particle sizes;

(3) Mix Fe _a Si _b B _c Cu _{d Me} Y _f magnetic powders of different meshes, among which Fe _a Si _b B _c Cu _d Me _{Y f} magnetic powders of -100 mesh to +200 mesh account for 15% of the total mass %, -200 mesh ~ +300 mesh Fe _a Si _b B _c Cu _{d Me} Y _f magnetic powder accounts for 70% of the total mass, -300 mesh ~ +400 mesh Fe _a Si _b B _c Cu _d Me _{Y f} magnetic powder accounts for 10% of the total mass, -400 mesh Fe _a Si _b B _c Cu _{d Me} Y _f magnetic powder accounts for 5% of the total mass, after passivation treatment with 0.4wt% phosphoric acid aqueous solution, and 0.5wt% organic binder Mix well and press into magnetic powder core under 1.80GPa pressure;

(4) Place the pressed magnetic powder core in a vacuum annealing furnace at 500° C. for 1 hour to obtain a Fe-based nanocrystalline magnetic powder core.

The organic binder is epoxy resin or silicone resin.

The invention has the advantages that the low-loss Fe-based nanocrystalline magnetic powder core with excellent soft magnetic properties can be obtained through the method, and the process is simple, easy to shape, beneficial to environmental protection, and has certain cost advantages.

Detailed ways

The composition of the low-loss Fe-based nanocrystalline magnetic powder core is: Fe _a Si _b B _c Cu _{d Me} Y _f , where M is C, P, Cr or Mn, subscripts a, b, c, d, e, f Indicates the atomic percentage of the corresponding alloying element, meeting the following conditions: 70≤a≤90, 2≤b≤15, 4≤c≤13, 0.4≤d≤3, 2≤e≤8, 0<f≤5; and a +b+c+d+e+f=100.

Example 1

(1) Mechanically crush the Fe ₇₀ Si ₁₅ B ₄ Cu _0.4 M ₈ Y _2.6 amorphous ribbon in a vacuum annealing furnace at 420°C for 1 hour;

(2) Fe ₇₀ Si ₁₅ B ₄ Cu _0.4 M ₈ Y _2.6 Amorphous strips were mechanically crushed, then placed in a planetary ball mill for ball milling with a ball-to-material ratio of 5:1, ball milling time of 4 hours, and a rotational speed of 260r/min. Add ethanol to prevent oxidation, dry and sieve to obtain Fe ₇₀ Si ₁₅ B ₄ Cu _0.4 M ₈ Y _2.6 magnetic powder with different particle sizes;

(3) Mix Fe ₇₀ Si ₁₅ B ₄ Cu _0.4 M ₈ Y _2.6 magnetic powders of different meshes, among which Fe ₇₀ Si ₁₅ B ₄ Cu _0.4 M ₈ Y _2.6 magnetic powders of -100 mesh to +200 mesh account for 15% of the total mass %, -200 mesh to +300 mesh Fe ₇₀ Si ₁₅ B ₄ Cu _0.4 M ₈ Y _2.6 magnetic powder accounts for 70% of the total mass, -300 mesh to +400 mesh Fe ₇₀ Si ₁₅ B ₄ Cu _0.4 M ₈ Y _2.6 magnetic powder accounts for 10% of the total mass, -400 mesh Fe ₇₀ Si ₁₅ B ₄ Cu _0.4 M ₈ Y _2.6 magnetic powder accounts for 5% of the total mass, after passivation treatment with 0.4wt% phosphoric acid aqueous solution, bonded with 0.5wt% epoxy resin The binder is fully mixed and pressed under a pressure of 1.80GPa to form a ring-shaped blank; the outer diameter of the magnetic ring is 22.90mm, the inner diameter is 14.20mm, and the height is 7.60mm.

(4) Place the pressed magnetic powder core in a vacuum annealing furnace at 500° C. for 1 hour to obtain a Fe-based nanocrystalline magnetic powder core.

After testing, the relevant electromagnetic parameters of the target product are shown in Table 1:

Example 2

(1) After the Fe ₉₀ Si ₂ B ₄ Cu ₁ P ₂ Y ₁ amorphous thin strip was kept at 420°C for 1 h in a vacuum annealing furnace, it was mechanically crushed;

(2) After the Fe ₉₀ Si ₂ B ₄ Cu ₁ P ₂ Y ₁ amorphous strip is mechanically crushed, it is placed in a planetary ball mill for ball milling, the ball-to-material ratio is 5:1, the ball milling time is 4 hours, and the speed is 260r/min. Add ethanol to prevent oxidation, dry and sieve to obtain Fe ₉₀ Si ₂ B ₄ Cu ₁ P ₂ Y ₁ magnetic powder with different particle sizes;

(3) Mix Fe ₉₀ Si ₂ B ₄ Cu ₁ P ₂ Y ₁ magnetic powders of different meshes, among which Fe ₉₀ Si ₂ B ₄ Cu ₁ P ₂ Y ₁ magnetic powders of -100 mesh to +200 mesh account for 15% of the total mass %, -200 mesh to +300 mesh Fe ₉₀ Si ₂ B ₄ Cu ₁ P ₂ Y ₁ magnetic powder accounts for 70% of the total mass, -300 mesh to +400 mesh Fe ₉₀ Si ₂ B ₄ Cu ₁ P ₂ Y ₁ magnetic powder accounts for 10% of the total mass, -400 mesh Fe ₉₀ Si ₂ B ₄ Cu ₁ P ₂ Y ₁ magnetic powder accounts for 5% of the total mass, after passivation treatment with 0.4wt% phosphoric acid aqueous solution, and 0.5wt% silicone resin The binder is fully mixed and pressed into a magnetic powder core under a pressure of 1.80GPa;

(4) Place the pressed magnetic powder core in a vacuum annealing furnace at 500° C. for 1 hour to obtain a Fe-based nanocrystalline magnetic powder core.

After testing, the relevant electromagnetic parameters of the target product are shown in Table 2:

Example 3

(1) Mechanically crush the Fe ₆₀ Si ₁₁ B ₁₃ Cu ₃ Cr ₈ Y ₅ amorphous thin ribbon at 420°C for 1 hour in a vacuum annealing furnace;

(2) After the Fe ₆₀ Si ₁₁ B ₁₃ Cu ₃ Cr ₈ Y ₅ amorphous strip is mechanically crushed, it is placed in a planetary ball mill for ball milling, the ball-to-material ratio is 5:1, the ball milling time is 4 hours, and the speed is 260r/min. Add ethanol to prevent oxidation, dry and sieve to obtain Fe ₆₀ Si ₁₁ B ₁₃ Cu ₃ Cr ₈ Y ₅ magnetic powder with different particle sizes;

(3) Mix Fe ₆₀ Si ₁₁ B ₁₃ Cu ₃ Cr ₈ Y ₅ magnetic powders of different meshes, among which Fe ₆₀ Si ₁₁ B ₁₃ Cu ₃ Cr ₈ Y ₅ magnetic powders of -100 mesh to +200 mesh account for 15% of the total mass %, -200 mesh to +300 mesh Fe ₆₀ Si ₁₁ B ₁₃ Cu ₃ Cr ₈ Y ₅ magnetic powder accounts for 70% of the total mass, -300 mesh to +400 mesh Fe ₆₀ Si ₁₁ B ₁₃ Cu ₃ Cr ₈ Y ₅ magnetic powder accounts for 10% of the total mass, -400 mesh Fe ₆₀ Si ₁₁ B ₁₃ Cu ₃ Cr ₈ Y ₅ magnetic powder accounts for 5% of the total mass, after passivation treatment with 0.4wt% phosphoric acid aqueous solution, bonded with 0.5wt% epoxy resin The binder is fully mixed and pressed into a magnetic powder core under a pressure of 1.80GPa;

(4) Place the pressed magnetic powder core in a vacuum annealing furnace at 500° C. for 1 hour to obtain a Fe-based nanocrystalline magnetic powder core.

After testing, the relevant electromagnetic parameters of the target product are shown in Table 3:

Example 4

(1) After the Fe ₇₄ Si ₆ B ₆ Cu ₃ Mn ₆ Y ₅ amorphous thin strip was kept at 420°C for 1 hour in a vacuum annealing furnace, it was mechanically crushed;

(2) After the Fe ₇₄ Si ₆ B ₆ Cu ₃ Mn ₆ Y ₅ amorphous strip is mechanically crushed, it is placed in a planetary ball mill for ball milling, the ball-to-material ratio is 5:1, the ball milling time is 4 hours, and the speed is 260r/min. Add ethanol to prevent oxidation, dry and sieve to obtain Fe ₇₄ Si ₆ B ₆ Cu ₃ Mn ₆ Y ₅ magnetic powder with different particle sizes;

(3) Mix Fe ₇₄ Si ₆ B ₆ Cu ₃ Mn ₆ Y ₅ magnetic powders of different meshes, among which Fe ₇₄ Si ₆ B ₆ Cu ₃ Mn ₆ Y ₅ magnetic powders of -100 mesh to +200 mesh account for 15% of the total mass %, -200 mesh to +300 mesh Fe ₇₄ Si ₆ B ₆ Cu ₃ Mn ₆ Y ₅ magnetic powder accounts for 70% of the total mass, -300 mesh to +400 mesh Fe ₇₄ Si ₆ B ₆ Cu ₃ Mn ₆ Y ₅ magnetic powder accounts for 10% of the total mass, -400 mesh Fe ₇₄ Si ₆ B ₆ Cu ₃ Mn ₆ Y ₅ magnetic powder accounts for 5% of the total mass, after passivation treatment with 0.4wt% phosphoric acid aqueous solution, and 0.5wt% silicone resin The binder is fully mixed and pressed into a magnetic powder core under a pressure of 1.80GPa;

(4) Place the pressed magnetic powder core in a vacuum annealing furnace at 500° C. for 1 hour to obtain a Fe-based nanocrystalline magnetic powder core.

After testing, the relevant electromagnetic parameters of the target product are shown in Table 4:

Claims (3)

1. a low-loss Fe base nanometer crystal powder core is characterized in that it consists of: Fe _aSi _bB _cCu _dM _eY _f, M is C, P, Cr or Mn in the formula, subscript a, b, c, d, e, f represent the atomic percent of respective alloy element, meet the following conditions: 70≤a≤90,2≤b≤15,4≤c≤13,0.4≤d≤3,2≤e≤8,0＜f≤5; And a+b+c+d+e+f=100.

2. the preparation method of a low-loss Fe base nanometer crystal powder core is characterized in that its step is as follows:

(1) with Fe _aSi _bB _cCu _dM _eY _fAmorphous thin ribbon in vacuum annealing furnace in 420 ℃ the insulation 1h after, it is carried out Mechanical Crushing, M is C, P, Cr or Mn in the formula, subscript a, b, c, d, e, f represent the atomic percent of respective alloy element, meet the following conditions: 70≤a≤90,2≤b≤15,4≤c≤13,0.4≤d≤3,2≤e≤8,0＜f≤5; And a+b+c+d+e+f=100;

(2) Fe _aSi _bB _cCu _dM _eY _fAfter the amorphous thin ribbon Mechanical Crushing, place the planetary ball mill ball milling, ratio of grinding media to material is 5:1, and Ball-milling Time is 4h, and rotating speed is 260r/min, and adds the anti-oxidation of ethanol, the dry Fe that obtains the variable grain degree by screening _aSi _bB _cCu _dM _eY _fMagnetic;

(3) with the Fe of different meshes _aSi _bB _cCu _dM _eY _fMagnetic mixes, wherein-100 order ~+200 purpose Fe _aSi _bB _cCu _dM _eY _fMagnetic accounts for 15% ,-200 orders of gross mass ~+300 purpose Fe _aSi _bB _cCu _dM _eY _fMagnetic accounts for 70% ,-300 orders of gross mass ~+400 purpose Fe _aSi _bB _cCu _dM _eY _fMagnetic accounts for 10% ,-400 purpose Fe of gross mass _aSi _bB _cCu _dM _eY _fMagnetic accounts for 5% of gross mass, through after the phosphate aqueous solution Passivation Treatment of 0.4wt%, fully mixes with the binding agent of 0.5wt%, and be pressed into powder core under 1.80GPa pressure;

(4) powder core that suppresses is placed 500 ℃ of insulations of vacuum annealing furnace 1h, obtain Fe base nanometer crystal powder core.

3. the preparation method of a kind of low-loss Fe base nanometer crystal powder core according to claim 2 is characterized in that described binding agent is epoxy resin or silicone resin.