阅读说明：本技术 一种磁性复合材料及其制备方法 (Magnetic composite material and preparation method thereof ) 是由 张作州 于 2019-09-27 设计创作，主要内容包括：本发明公开了一种磁性复合材料及其制备方法,该复合材料由材料A、材料B混合烧制而成,材料A与材料B的重量比为100:3-6；材料A中各成分的重量百分含量为：B 1-3％,Nd 25-28％,Ni 1.8-2.2％,Ag 0.008-0.013％,Ta 0.08-0.12％,Tm 2-5％,Be 0.1-0.5％,Si 1.5-1.9％,余量为Fe；材料B由物质(Na,Ca)<Sub>0.33</Sub>(Al,Mg)<Sub>2</Sub>[Si<Sub>4</Sub>O<Sub>10</Sub>](OH)<Sub>2</Sub>·nH<Sub>2</Sub>O、物质Na<Sub>2</Sub>O·Al<Sub>2</Sub>O<Sub>3</Sub>·6SiO<Sub>2</Sub>和四氧化三铁组成,三者之间的重量比例为1:0.2-0.6:5。本发明磁性复合材料具有较高的综合磁性能。另外制备过种中材料经过适当处理,保证了材料成分、组织和性能的均匀性,保证了合金的质量。该材料制备工艺简便,制备所用原料成本较低,过程简单,生产的材料具有良好的性能,便于工业化生产,在电器行业具有良好的应用前景。(the invention discloses a magnetic composite material and a preparation method thereof, wherein the composite material is prepared by mixing and firing a material A and a material B, and the weight ratio of the material A to the material B is 100: 3-6; the material A comprises the following components in percentage by weight: 1-3% of B, 25-28% of Nd, 1.8-2.2% of Ni, 0.008-0.013% of Ag, 0.08-0.12% of Ta, 2-5% of Tm, 0.1-0.5% of Be, 1.5-1.9% of Si and the balance of Fe; material B is composed of substance (Na, Ca) 0.33 (Al,Mg) 2 [Si 4 O 10 ](OH) 2 ·nH 2 O, substance Na 2 O·Al 2 O 3 ·6SiO 2 And ferroferric oxide, wherein the weight ratio of the three components is 1:0.2-0.6: 5. The magnetic composite material of the invention has the advantages ofhigh comprehensive magnetic performance. In addition, the prepared seed material is properly treated, so that the uniformity of the components, the structure and the performance of the material is ensured, and the quality of the alloy is ensured. The material has the advantages of simple preparation process, low cost of raw materials for preparation, simple process, good performance of the produced material, convenience for industrial production and good application prospect in the electrical appliance industry.)

1. A magnetic composite material, characterized by: the material A and the material B are mixed and fired, and the weight ratio of the material A to the material B is 100: 3-6;

The material A comprises the following components in percentage by weight: 1-3% of B, 25-28% of Nd, 1.8-2.2% of Ni, 0.008-0.013% of Ag, 0.08-0.12% of Ta, 2-5% of Tm, 0.1-0.5% of Be, 1.5-1.9% of Si and the balance of Fe;

Material B is composed of substance (Na, Ca)_0.33(Al,Mg)₂[Si₄O₁₀](OH)₂·nH₂O, substance Na₂O·Al₂O₃·6SiO₂And ferroferric oxide, wherein the weight ratio of the three components is 1:0.2-0.6: 5.

2. A method of making the magnetic composite material of claim 1, comprising the steps of: uniformly mixing the material A and the material B according to the weight ratio of 100:3-6, and then placing the mixture into a mold to be molded in a magnetic field; and (3) sintering the formed green body in vacuum at 1180-1230 ℃ for 4-6h, performing primary tempering at 810-850 ℃ for 1-1.5h, and performing secondary tempering at 450-480 ℃ for 2-3.5h to obtain the magnetic composite material.

3. the method of claim 2, wherein: when the material A is prepared, the materials are prepared according to the weight percentage of B1-3%, Nd 25-28%, Ni 1.8-2.2%, Ag 0.008-0.013%, Ta 0.08-0.12%, Tm 2-5%, Be 0.1-0.5%, Si 1.5-1.9% and the balance of Fe, wherein boron takes ferroboron containing 20 wt% as a raw material, and the balance is pure substances; by utilizing a sheet casting technology, under the protection of nitrogen, alloy casting sheets with different thicknesses are obtained by adjusting the linear speed of a roller: the smelting temperature is 1530-1560 ℃, and mother alloy liquid is obtained; pouring molten mother alloy liquid on a rotary disc of a forming furnace under the protection of nitrogen to form a cast sheet, wherein the rotary linear speed of a pouring point of the rotary disc is 14-18m/s, and the casting point is castThe thickness of the sheet is 2-5 mm, and the length and width of the sheet are 5-8 mm; the cast sheet is subjected to hydrogen explosion and airflow milling to obtain powder with the average particle size of 3-6 microns: placing the cast sheet into a sealable reaction kettle, and introducing H into the reaction kettle₂After S gas is generated, heating the gas at 70-120 ℃ for 2-3h, and then taking out the gas for air cooling; then putting the processed cast sheet into a hydrogen crushing furnace with the vacuum degree of 0.08-0.11Pa and the pressure in the furnace of 0.7-1.8atm for hydrogen crushing, heating the cast sheet to 280-305 ℃, and performing hydrogen crushing for 45-55 minutes to obtain coarse powder; and then placing the coarse powder into an airflow mill, grinding the coarse powder into fine powder to obtain a material A, and grinding the material A into powder by the airflow mill at the pressure of 5-8 atm.

4. The method of claim 2, wherein: material B was prepared by mixing materials (Na, Ca)_0.33(Al,Mg)₂[Si₄O₁₀](OH)₂·nH₂O and Na as substance₂O·Al₂O₃·6SiO₂The powder of (A) is put into a ball mill for ball milling, wherein the materials (Na, Ca) in the raw materials_0.33(Al,Mg)₂[Si₄O₁₀](OH)₂·nH₂O and Na as substance₂O·Al₂O₃·6SiO₂The weight ratio of the powder is 1:0.2-0.6, and the fineness of the substance powder is 10-20 μm; in a ball mill, the mass ratio of high-aluminum grinding balls to raw materials to water is 1.5:1:0.8-1.5, the ball milling time is 12-18h, and after the ball milling is finished, the powder is baked in an oven at 200 ℃ for 1-2h to obtain inorganic material mixed powder of 3-6 mu m for later use; taking 280g of substance FeCl₃·6H₂O and substance FeSO₄·7H₂Placing O in 1000mL of deionized water to form an aqueous solution, and stirring and mixing uniformly, wherein the substance FeCl is₃·6H₂O and substance FeSO₄·7H₂The proportion of O is according to Fe^{2 +}With Fe³⁺The weight ratio of (A) to (B) is 1: 1.75; after the mixture is stirred evenly, 1000mL of deionized water is added into the mixture, the mixture is stirred for 2-5min, a certain amount of inorganic material mixed powder is added into the mixture, the mixture is stirred for 2-5min, wherein the adding amount of the inorganic material mixed powder is added according to the weight ratio of the inorganic material mixed powder to the ferroferric oxide of 1.2-1.6:5, and the amount of the ferroferric oxide is the amount of the ferroferric oxide generated in the material BThe quantity of the ferroferric oxide; heating the solution to 100-105 ℃ and preserving heat for 2-5h, taking out residues after water in the solution is discharged, putting the residues into a baking furnace, heating to 120-150 ℃ and preserving heat for 2-5h, taking out materials after cooling, and putting the materials into a ball mill for ball milling for 2-5h to obtain a material B with the particle size of 3-6 mu m.

Technical Field

The invention belongs to the technical field of composite materials, and particularly relates to a magnetic composite material and a preparation method thereof.

Background

CN201910389317.1 provides a rare earth iron boron permanent magnet material containing Al and Cu and a preparation method thereof. The preparation method comprises the following steps: providing a diffusion source, wherein the diffusion source comprises Al, Cu and rare earth compounds; and applying the diffusion source to at least part of the surface of a permanent magnet prefabricated material, and then performing diffusion treatment and tempering treatment to obtain the rare earth iron boron permanent magnet material containing Al and Cu. The rare earth iron boron permanent magnet material comprises grains with a shell structure and a grain boundary phase, Al is enriched in a neodymium-rich phase and coated on the surfaces of the grains, Cu is enriched in the neodymium-rich phase, and the content of Al and Cu elements is gradually reduced from the surface to the inside of the rare earth iron boron permanent magnet material. However, the production process is complicated and the combination property is not high.

Disclosure of Invention

The invention aims to provide a composite magnetic material aiming at the technical defects, wherein the material has small demagnetization rate at high temperature and good magnetic performance; the invention also aims to provide a preparation method of the composite magnetic material, which has simple process and low production cost and is suitable for industrial production.

The above purpose of the invention is realized by the following technical scheme:

A magnetic composite material is formed by mixing and firing a material A and a material B, wherein the weight ratio of the material A to the material B is 100: 3-6;

The material A comprises the following components in percentage by weight: 1-3% of B, 25-28% of Nd, 1.8-2.2% of Ni, 0.008-0.013% of Ag, 0.08-0.12% of Ta0.08, 2-5% of Tm, 0.1-0.5% of Be, 1.5-1.9% of Si, and the balance of Fe;

Material B is composed of substance (Na, Ca)_0.33(Al,Mg)₂[Si₄O₁₀](OH)₂·nH₂O, substance Na₂O·Al₂O₃·6SiO₂And ferroferric oxide, wherein the weight ratio of the three components is 1:0.2-0.6: 5.

The preparation method of the magnetic composite material comprises the following steps: uniformly mixing the material A and the material B according to the weight ratio of 100:3-6, and then placing the mixture into a mold to be molded in a magnetic field; and (3) sintering the formed green body in vacuum at 1180-1230 ℃ for 4-6h, performing primary tempering at 810-850 ℃ for 1-1.5h, and performing secondary tempering at 450-480 ℃ for 2-3.5h to obtain the magnetic composite material.

furthermore, when the material A is prepared, the materials A are prepared according to the weight percentage of B1-3%, Nd 25-28%, Ni 1.8-2.2%, Ag 0.008-0.013%, Ta0.08-0.12%, Tm 2-5%, Be 0.1-0.5%, Si 1.5-1.9% and the balance of Fe, wherein boron takes ferroboron containing 20 wt% as a raw material, and the balance is pure substances; by utilizing a sheet casting technology, under the protection of nitrogen, alloy casting sheets with different thicknesses are obtained by adjusting the linear speed of a roller: the smelting temperature is 1530-1560 ℃, and mother alloy liquid is obtained; pouring molten mother alloy liquid on a rotary table of a forming furnace under the protection of nitrogen to form a cast sheet, wherein the rotary linear speed of a pouring point of the rotary table is 14-18m/s, the thickness of the cast sheet is 2-5 mm, and the length and the width of the cast sheet are 5-8 mm; the cast sheet is subjected to hydrogen explosion and airflow milling to obtain powder with the average particle size of 3-6 microns: placing the cast sheet into a sealable reaction kettle, and introducing H into the reaction kettle₂After S gas is generated, heating the gas at 70-120 ℃ for 2-3h, and then taking out the gas for air cooling; then putting the processed cast sheet into a hydrogen crushing furnace with the vacuum degree of 0.08-0.11Pa and the pressure in the furnace of 0.7-1.8atm for hydrogen crushing, heating the cast sheet to 280-305 ℃, and performing hydrogen crushing for 45-55 minutes to obtain coarse powder; and then placing the coarse powder into an airflow mill, grinding the coarse powder into fine powder to obtain a material A, and grinding the material A into powder by the airflow mill at the pressure of 5-8 atm.

Further, when preparing the material B, the substance (Na, Ca)_0.33(Al,Mg)₂[Si₄O₁₀](OH)₂·nH₂O and Na as substance₂O·Al₂O₃·6SiO₂The powder of (A) is put into a ball mill for ball milling, wherein the materials (Na, Ca) in the raw materials_0.33(Al,Mg)₂[Si₄O₁₀](OH)₂·nH₂O and Na as substance₂O·Al₂O₃·6SiO₂The weight ratio of the powder is 1:0.2-0.6, and the fineness of the substance powder is 10-20 μm; in a ball mill, the mass ratio of high-aluminum grinding balls to raw materials to water is 1.5:1:0.8-1.5, the ball milling time is 12-18h, and after the ball milling is finished, the powder is baked in an oven at 200 ℃ for 1-2h to obtain inorganic material mixed powder of 3-6 mu m for later use; taking 280g of substance FeCl₃·6H₂O and substance FeSO₄·7H₂O deviceForming an aqueous solution in 1000mL of deionized water, and stirring and mixing the aqueous solution uniformly, wherein the substance FeCl is₃·6H₂O and substance FeSO₄·7H₂The proportion of O is according to Fe²⁺With Fe³⁺The weight ratio of (A) to (B) is 1: 1.75; after the mixture is stirred uniformly, 1000mL of deionized water is added into the mixture, the mixture is continuously stirred for 2-5min, a certain amount of inorganic material mixed powder is added into the mixture, the mixture is stirred for 2-5min, wherein the adding amount of the inorganic material mixed powder is added according to the weight ratio of the inorganic material mixed powder to the ferroferric oxide of 1.2-1.6:5, and the quantity of the ferroferric oxide is the quantity of the ferroferric oxide generated in the material B; heating the solution to 100-105 ℃ and preserving heat for 2-5h, taking out residues after water in the solution is discharged, putting the residues into a baking furnace, heating to 120-150 ℃ and preserving heat for 2-5h, taking out materials after cooling, and putting the materials into a ball mill for ball milling for 2-5h to obtain a material B with the particle size of 3-6 mu m.

Has the advantages that:

Material A mainly forms magnetic main phase Nd₂Fe₁₄B and sub-major phase Tm₂Fe₁₄B, strengthening the demagnetization coupling effect, so that the magnet has high coercive force and avoids the great decline of remanence, thereby obtaining higher comprehensive magnetic performance; in the sintering process, high-melting point alloy elements Ta and Ni are added, so that a new phase can be precipitated in a magnet structure; be and Ag eliminate the phenomenon of direct contact between main phase grains, effectively inhibit the growth of the main phase grains and facilitate the obtainment of finer and uniform grain structures; meanwhile, the wetting angle of the Nd-rich phase and the main phase is reduced, the growth of the main phase is inhibited, the defect density of the main phase interface is reduced, and the nucleation of the anti-magnetization domain at the interface is difficult. Si can assist B in improving the thermal stability of the main phase magnet. Si can also act with Ta and Ni, and prevents diffusion transfer of key rare earth elements in the A material in sintering.

the material B contains a low-melting-point metal oxide complex, can be uniformly distributed in a main phase grain boundary to play a pinning effect, and improves the coercive force. In addition, the magnetic material can be dispersedly distributed around the main phase grains, the organization structure of a grain boundary phase can be effectively improved, the grain boundary modification is carried out on the magnet, and the grain boundary phase is strengthened, so that the remanence of the material is improved. The material B contains magnetic substance ferroferric oxide sandwiched between metal oxide complexes, so that the intrinsic coercivity can be improved, namely, the growth of grains at grain intersection is inhibited through the formed main phase intergranular secondary phase iron-rich phase, the main phase grains are refined, and therefore the enhancement of stray fields around the grains is inhibited, and the intrinsic coercivity is further improved.

The magnetic composite material has higher comprehensive magnetic performance. In addition, the prepared seed material is properly treated, so that the uniformity of the components, the structure and the performance of the material is ensured, and the quality of the alloy is ensured. The material has the advantages of simple preparation process, low cost of raw materials for preparation, simple process, good performance of the produced material, convenience for industrial production and good application prospect in the electrical appliance industry.

Drawings

FIG. 1 is a structural view of a magnetic composite material in example 1.

Detailed Description

The following detailed description of the present invention is provided in connection with the accompanying drawings and examples, but not intended to limit the scope of the invention.