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CN104036907A - Method for preparing soft magnetic metal composite via warm compaction - Google Patents

Method for preparing soft magnetic metal composite via warm compaction Download PDF

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CN104036907A
CN104036907A CN201410246527.2A CN201410246527A CN104036907A CN 104036907 A CN104036907 A CN 104036907A CN 201410246527 A CN201410246527 A CN 201410246527A CN 104036907 A CN104036907 A CN 104036907A
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soft magnetic
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magnetic metal
passivation
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严密
白国华
吴琛
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Zhejiang University ZJU
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Abstract

本发明公开了一种温压成型制备金属软磁复合材料的方法。1)将钝化剂和溶剂混合起来得到钝化液,将钝化液和磁性金属粉末混合,搅拌,烘干,得到钝化粉,2)将粘结剂溶解在溶剂中配成粘结剂溶液,将粘结剂溶液和钝化粉混合,搅拌均匀,烘干,得到绝缘包覆的金属软磁粉,3)将上述绝缘包覆的金属软磁粉和润滑剂混合均匀,装入模具中,温压成型。本发明的优点是利用温压成型法制备金属软磁复合材料在成型过程中就可以实现粘结的固化,可以将压制和固化两道工序合并为温压一道工序,简化工艺,显著降低压制压力,所得金属软磁复合材料具有电阻率高,饱和磁通密度高,矫顽力低的特点,在金属软磁粉芯的制备中有广阔的应用前景。The invention discloses a method for preparing metal soft magnetic composite materials by warm pressing. 1) Mix passivation agent and solvent to get passivation solution, mix passivation solution and magnetic metal powder, stir, dry to get passivation powder, 2) Dissolve binder in solvent to make binder Solution, mix the binder solution and passivation powder, stir evenly, and dry to obtain the insulating-coated metal soft magnetic powder. 3) Mix the above-mentioned insulating-coated metal soft magnetic powder and lubricant evenly, and put it into the mold. Warm compression molding. The advantage of the present invention is that the metal soft magnetic composite material prepared by the warm pressing molding method can realize bonding and curing during the molding process, and the two processes of pressing and curing can be combined into one warm pressing process, which simplifies the process and significantly reduces the pressing pressure The obtained metal soft magnetic composite material has the characteristics of high resistivity, high saturation magnetic flux density and low coercive force, and has broad application prospects in the preparation of metal soft magnetic powder cores.

Description

一种温压成型制备金属软磁复合材料的方法A method for preparing metal soft magnetic composite materials by warm pressing

技术领域technical field

本发明涉及一种温压成型制备金属软磁复合材料的方法,属于电子元器件新材料新工艺领域。The invention relates to a method for preparing metal soft magnetic composite materials by warm pressing, and belongs to the field of new materials and new technologies for electronic components.

背景技术Background technique

温压成型法是将混合粉末在封闭钢模中预热,然后进行加压成型,由于压制的温度介于通常的室温和热压温度之间,因而被称之为温压。温压工艺可以用较低的压制压力获得较高的压坯密度和强度,在高强度铁基零件,粘结钕铁硼磁体等领域存在广泛应用。The warm pressing method is to preheat the mixed powder in a closed steel mold, and then perform press molding. Since the pressing temperature is between the usual room temperature and the hot pressing temperature, it is called warm pressing. The warm pressing process can obtain higher green compact density and strength with lower pressing pressure, and is widely used in high-strength iron-based parts, bonded NdFeB magnets and other fields.

随着电子技术的发展,节能降耗对于电子器件来说愈发重要,想方设法降低高频下的损耗具有重大意义。传统硅钢片在高频下损耗太大,限制了其高频应用,于是将磁性粉末进行钝化、绝缘包覆、压制成型后得到的金属软磁复合材料可以有效的解决高频下的损耗问题。金属软磁复合材料的主要特征是磁性金属粉末由绝缘介质包覆,电阻率比传统金属软磁材料高,饱和磁通密度比铁氧体软磁材料高,应用频率更广。在电力电子领域,金属软磁复合材料模压制成的磁粉芯被广泛的用于制作变压器、滤波器、互感器等电子元件。With the development of electronic technology, energy saving and consumption reduction are becoming more and more important for electronic devices, and it is of great significance to find ways to reduce the loss at high frequencies. Traditional silicon steel sheets have too much loss at high frequencies, which limits their high-frequency applications. Therefore, the metal soft magnetic composite material obtained by passivating the magnetic powder, insulating coating, and pressing can effectively solve the loss problem at high frequencies. . The main feature of the metal soft magnetic composite material is that the magnetic metal powder is covered by an insulating medium, the resistivity is higher than that of the traditional metal soft magnetic material, the saturation magnetic flux density is higher than that of the ferrite soft magnetic material, and the application frequency is wider. In the field of power electronics, magnetic powder cores made of metal soft magnetic composite materials are widely used to make electronic components such as transformers, filters, and transformers.

但是由于绝缘包覆,磁性金属颗粒间距增大,使得磁性金属粉末在压制,固化处理后,坯体的密度会降低,进而导致机械强度降低。而且由于压制成型引入的内应力使得材料的磁性能恶化,需要增加去应力退火工工艺,使生产过程复杂化。因此开发一种能够提高金属软磁复合材料成型密度的材料制备方法十分有必要。However, due to the insulation coating, the distance between the magnetic metal particles increases, so that the density of the green body will decrease after the magnetic metal powder is pressed and solidified, resulting in a decrease in mechanical strength. Moreover, due to the internal stress introduced by pressing and forming, the magnetic properties of the material deteriorate, and it is necessary to increase the stress relief annealing process, which complicates the production process. Therefore, it is necessary to develop a material preparation method that can increase the molding density of metal soft magnetic composites.

发明内容Contents of the invention

本发明的目的是提供一种温压成型制备金属软磁复合材料的方法。The object of the present invention is to provide a method for preparing metal soft magnetic composite materials by warm pressing.

温压成型制备金属软磁复合材料的方法包括如下步骤:The method for preparing metal soft magnetic composite material by warm pressing comprises the following steps:

1)粉料钝化1) Powder passivation

将溶剂和钝化剂配成钝化液,将颗粒尺寸为0.1~250μm的金属软磁粉混合,加入钝化液,搅拌0.1~2h,放入烘箱钝化,钝化温度为40~100℃,钝化时间为0.1~4h,得到钝化粉;Make a passivation solution with a solvent and a passivator, mix the metal soft magnetic powder with a particle size of 0.1-250 μm, add the passivation solution, stir for 0.1-2 hours, put it into an oven for passivation, and passivate at a temperature of 40-100°C. The passivation time is 0.1-4h, and the passivation powder is obtained;

2)绝缘包覆2) Insulation coating

将粘结剂溶解在有机溶剂中,得到粘结剂溶液,在钝化粉中加入粘结剂溶液,搅拌0.1~2h,放入烘箱烘干,烘烤温度为40~100℃,烘烤时间为0.1~4h,得到绝缘包覆的金属软磁粉;Dissolve the binder in an organic solvent to obtain a binder solution, add the binder solution to the passivation powder, stir for 0.1-2 hours, put it in an oven for drying, the baking temperature is 40-100°C, and the baking time is for 0.1 to 4 hours to obtain insulating-coated metal soft magnetic powder;

3)温压成型3) Warm compression molding

将润滑剂加入绝缘包覆的金属软磁粉中搅拌均匀,装入成型模具中,对模腔内的金属软磁粉进行加热并保温,加热温度为60~150℃,使得在压制过程中,粘结剂发生固化,采用600~1200Mpa的压力将粉末压制成型,保压5~30min,脱模,得到样品。Add the lubricant to the insulating coated metal soft magnetic powder and stir evenly, put it into the forming mold, heat the metal soft magnetic powder in the mold cavity and keep it warm. The heating temperature is 60-150°C, so that the bonding The agent is solidified, and the powder is pressed into shape with a pressure of 600-1200Mpa, kept under pressure for 5-30 minutes, and demolded to obtain a sample.

所述的金属软磁粉为还原铁粉、羰基铁粉、铁硅铝合金粉末、铁镍合金粉末、铁镍钼合金粉末、铁硅硼非晶粉末、铁硅合金粉末或铁硅镍合金粉末。所述的溶剂为去离子水、乙醇、甲乙酮、丙酮、丁酮或乙酸乙酯。所述的钝化剂为双氧水、高锰酸钾、磷酸或铬酸。所述的钝化液中钝化剂的质量分数为0.1~5%。所述的钝化液与金属软磁粉的质量比为0.01:1~1:1。所述的粘结剂为环氧树脂、酚醛树脂、聚乙烯醇、聚乙烯醇缩丁醛或玻璃粉,粘结剂溶液中粘结剂的质量分数为5~50%。所述的粘结剂溶液与金属粉末的质量比为0.01:1~1:1。The metal soft magnetic powder is reduced iron powder, carbonyl iron powder, iron-silicon-aluminum alloy powder, iron-nickel alloy powder, iron-nickel-molybdenum alloy powder, iron-silicon-boron amorphous powder, iron-silicon alloy powder or iron-silicon-nickel alloy powder. The solvent is deionized water, ethanol, methyl ethyl ketone, acetone, butanone or ethyl acetate. The passivating agent is hydrogen peroxide, potassium permanganate, phosphoric acid or chromic acid. The mass fraction of the passivating agent in the passivating solution is 0.1-5%. The mass ratio of the passivation solution to the metal soft magnetic powder is 0.01:1˜1:1. The binder is epoxy resin, phenolic resin, polyvinyl alcohol, polyvinyl butyral or glass powder, and the mass fraction of the binder in the binder solution is 5-50%. The mass ratio of the binder solution to the metal powder is 0.01:1˜1:1.

所述的润滑剂为硬脂酸锌、硬脂酸钡、酰酸基蜡、硬脂酸锂或六方BN,润滑剂含量为绝缘包覆的金属软磁粉质量的0.1~1%。所述的模具形状是长方体、圆柱体、椭圆柱体或者他们的组合体。The lubricant is zinc stearate, barium stearate, acyl wax, lithium stearate or hexagonal BN, and the content of the lubricant is 0.1-1% of the mass of the insulating-coated metal soft magnetic powder. The shape of the mold is cuboid, cylinder, ellipse cylinder or their combination.

本发明与现有技术相比具有以下优点:Compared with the prior art, the present invention has the following advantages:

1)通过温压成型,可以制备出具有高压制密度,高机械强度的金属软磁复合材料;1) Metal soft magnetic composite materials with high compaction density and high mechanical strength can be prepared by warm pressing;

2)通过温压成型控制压制时的温度,可以将传统压制成型法制备金属软磁复合材料的压制工序和固化工序简化为一道工序,生产过程简单,效率高;2) By controlling the temperature during pressing by warm pressing, the pressing process and curing process of the metal soft magnetic composite material prepared by the traditional pressing forming method can be simplified into one process, the production process is simple and the efficiency is high;

3)制备的金属软磁复合材料具有高饱和磁通密度,低矫顽力,低损耗,高电阻率的特点。3) The prepared metal soft magnetic composite material has the characteristics of high saturation magnetic flux density, low coercive force, low loss and high resistivity.

具体实施方式Detailed ways

本发明的金属软磁复合材料制备方法是将磁性金属粉末在钝化液中钝化后,与粘结剂溶液混合,搅拌均匀,烘干,绝缘包覆后加入润滑剂进行温压成型。此种金属软磁复合材料具有高的饱和磁通密度,高的电阻率,高的密度和优异的机械强度。The preparation method of the metal soft magnetic composite material of the present invention is to passivate the magnetic metal powder in a passivation solution, mix it with a binder solution, stir evenly, dry it, add a lubricant after insulation coating, and carry out warm pressing molding. The metal soft magnetic composite material has high saturation magnetic flux density, high resistivity, high density and excellent mechanical strength.

温压成型制备金属软磁复合材料的方法包括如下步骤:The method for preparing metal soft magnetic composite material by warm pressing comprises the following steps:

1)粉料钝化1) Powder passivation

将溶剂和钝化剂配成钝化液,将颗粒尺寸为0.1~250μm的金属软磁粉混合,加入钝化液,搅拌0.1~2h,放入烘箱钝化,钝化温度为40~100℃,钝化时间为0.1~4h,得到钝化粉;Make a passivation solution with a solvent and a passivator, mix the metal soft magnetic powder with a particle size of 0.1-250 μm, add the passivation solution, stir for 0.1-2 hours, put it into an oven for passivation, and passivate at a temperature of 40-100°C. The passivation time is 0.1-4h, and the passivation powder is obtained;

2)绝缘包覆2) Insulation coating

将粘结剂溶解在有机溶剂中,得到粘结剂溶液,在钝化粉中加入粘结剂溶液,搅拌0.1~2h,放入烘箱烘干,烘烤温度为40~100℃,烘烤时间为0.1~4h,得到绝缘包覆的金属软磁粉;Dissolve the binder in an organic solvent to obtain a binder solution, add the binder solution to the passivation powder, stir for 0.1-2 hours, put it in an oven for drying, the baking temperature is 40-100°C, and the baking time is for 0.1 to 4 hours to obtain insulating-coated metal soft magnetic powder;

3)温压成型3) Warm compression molding

将润滑剂加入绝缘包覆的金属软磁粉中搅拌均匀,装入成型模具中,对模腔内的金属软磁粉进行加热并保温,加热温度为60~150℃,使得在压制过程中,粘结剂发生固化,采用600~1200Mpa的压力将粉末压制成型,保压5~30min,脱模,得到样品。Add the lubricant to the insulating coated metal soft magnetic powder and stir evenly, put it into the forming mold, heat the metal soft magnetic powder in the mold cavity and keep it warm. The heating temperature is 60-150°C, so that the bonding The agent is solidified, and the powder is pressed into shape with a pressure of 600-1200Mpa, kept under pressure for 5-30 minutes, and demolded to obtain a sample.

所述的金属软磁粉为还原铁粉、羰基铁粉、铁硅铝合金粉末、铁镍合金粉末、铁镍钼合金粉末、铁硅硼非晶粉末、铁硅合金粉末或铁硅镍合金粉末。所述的溶剂为去离子水、乙醇、甲乙酮、丙酮、丁酮或乙酸乙酯。所述的钝化剂为双氧水、高锰酸钾、磷酸或铬酸。所述的钝化液中钝化剂的质量分数为0.1%~5%。所述的钝化液与金属软磁粉的质量比为0.01:1~1:1。所述的粘结剂为环氧树脂、酚醛树脂、聚乙烯醇、聚乙烯醇缩丁醛或玻璃粉,粘结剂溶液中粘结剂的质量分数为5%~50%。所述的粘结剂溶液与金属粉末的质量比为0.01:1~1:1。The metal soft magnetic powder is reduced iron powder, carbonyl iron powder, iron-silicon-aluminum alloy powder, iron-nickel alloy powder, iron-nickel-molybdenum alloy powder, iron-silicon-boron amorphous powder, iron-silicon alloy powder or iron-silicon-nickel alloy powder. The solvent is deionized water, ethanol, methyl ethyl ketone, acetone, butanone or ethyl acetate. The passivating agent is hydrogen peroxide, potassium permanganate, phosphoric acid or chromic acid. The mass fraction of the passivating agent in the passivating solution is 0.1%-5%. The mass ratio of the passivation solution to the metal soft magnetic powder is 0.01:1˜1:1. The binder is epoxy resin, phenolic resin, polyvinyl alcohol, polyvinyl butyral or glass powder, and the mass fraction of the binder in the binder solution is 5% to 50%. The mass ratio of the binder solution to the metal powder is 0.01:1˜1:1.

所述的润滑剂为硬脂酸锌、硬脂酸钡、酰酸基蜡、硬脂酸锂或六方BN,润滑剂含量为绝缘包覆的金属软磁粉质量的0.1%~1%。所述的模具形状是长方体、圆柱体、椭圆柱体或者他们的组合体。The lubricant is zinc stearate, barium stearate, acyl wax, lithium stearate or hexagonal BN, and the content of the lubricant is 0.1%-1% of the mass of the insulating coated metal soft magnetic powder. The shape of the mold is cuboid, cylinder, ellipse cylinder or their combination.

通过本发明可以制备出高成型密度,饱和磁通密度,低矫顽力,高电阻率,低损耗,优异机械强度金属软磁复合材料。The invention can prepare metal soft magnetic composite materials with high molding density, saturated magnetic flux density, low coercive force, high resistivity, low loss and excellent mechanical strength.

下面结合具体实例对本发明做进一步说明,但本发明并不仅仅局限于以下实施例。The present invention will be further described below in conjunction with specific examples, but the present invention is not limited only to the following examples.

实施例1:Example 1:

1)将磷酸和丙酮配成质量分数为0.6%的钝化液,按3:1:1的质量比取粒径分别为150μm、75μm、45μm的还原铁粉和钝化液按照质量比为1:0.1的比例进行钝化,在搅拌机中搅拌0.5h,放入烘箱钝化,钝化温度为70℃,钝化时间为1h,得到钝化粉;1) Phosphoric acid and acetone are made into a passivation solution with a mass fraction of 0.6%, and the reduced iron powder and the passivation solution with a mass ratio of 150 μm, 75 μm, and 45 μm are taken according to a mass ratio of 3:1:1. : passivation at a ratio of 0.1, stirred in a mixer for 0.5h, put into an oven for passivation, the passivation temperature is 70°C, the passivation time is 1h, and passivation powder is obtained;

2)将环氧树脂和乙醇配成环氧树脂质量分数为10%的粘结剂溶液,将粘结剂溶液和钝化粉按照质量比为0.1:1的比例混合,搅拌机搅拌0.5h,搅拌均匀,在80℃烘箱中烘烤2h,烘干,得到绝缘包覆的金属软磁粉待用。2) Mix epoxy resin and ethanol into a binder solution with a mass fraction of epoxy resin of 10%, mix the binder solution and passivation powder according to the mass ratio of 0.1:1, stir with a mixer for 0.5h, and stir Evenly, bake in an oven at 80°C for 2 hours, and dry to obtain insulating-coated metal soft magnetic powder for use.

3)将润滑剂硬脂酸锌按照质量分数0.3%加入绝缘包覆的金属软磁粉中搅拌均匀,装入成型模具中,对模腔内的磁粉进行加热并保温,加热温度为100℃,采用800Mpa的压力将粉末压制成型,保压10min,脱模,得到样品。3) Add the lubricant zinc stearate into the insulation-coated metal soft magnetic powder according to the mass fraction of 0.3%, stir evenly, put it into the forming mold, heat and keep the magnetic powder in the mold cavity at a heating temperature of 100°C, and use The pressure of 800Mpa is used to compress the powder, keep the pressure for 10min, and demould to obtain the sample.

制备出的样品组织致密,孔隙率低,密度为7.2g/cm3,断裂拉力为37kg,将样品进行软磁性能和电学性能测试,结果如下:饱和磁通密度Bs=1.5T,矫顽力Hc=130A/m,电阻率ρ=1.3×105Ω·cm,损耗为330mW/cm3/(50KHz/0.05T),样品的机械性能,磁学和电学性能优异。The prepared sample has a compact structure, low porosity, a density of 7.2g/cm 3 , and a breaking force of 37kg. The soft magnetic and electrical properties of the sample were tested, and the results are as follows: saturation magnetic flux density Bs = 1.5T, coercive force Hc=130A/m, resistivity ρ=1.3×10 5 Ω·cm, loss 330mW/cm 3 /(50KHz/0.05T), and the sample has excellent mechanical, magnetic and electrical properties.

实施例2:Example 2:

1)将磷酸和乙醇配成质量分数为0.1%的钝化液,按3:2:1的质量比取粒径分别为150μm、75μm、45μm的铁镍合金粉末和钝化液按照质量比为1:0.01的比例进行钝化,在搅拌机中搅拌0.1h,放入烘箱钝化,钝化温度为40℃,钝化时间为4h,得到钝化粉。1) Phosphoric acid and ethanol are made into a passivation solution with a mass fraction of 0.1%, and the iron-nickel alloy powder and the passivation solution with a particle size of 150 μm, 75 μm, and 45 μm are taken according to a mass ratio of 3:2:1. The ratio of 1:0.01 was passivated, stirred in a mixer for 0.1h, put into an oven for passivation, the passivation temperature was 40°C, and the passivation time was 4h to obtain passivation powder.

2)将环氧树脂和丙酮配成环氧树脂质量分数为50%的粘结剂溶液,将粘结剂溶液和钝化粉按照质量比为1:1的比例混合,搅拌机搅拌2h,搅拌均匀,在40℃烘箱中烘烤4h,烘干,得到绝缘包覆的金属软磁粉待用。2) Mix epoxy resin and acetone into a binder solution with a mass fraction of epoxy resin of 50%, mix the binder solution and passivation powder according to the mass ratio of 1:1, stir with a mixer for 2 hours, and stir evenly , baked in an oven at 40° C. for 4 hours, and dried to obtain insulating-coated metal soft magnetic powder for use.

3)将润滑剂硬脂酸锌按照质量分数0.1%加入绝缘包覆的金属软磁粉中搅拌均匀,装入成型模具中,对模腔内的磁粉进行加热并保温,加热温度为60℃,采用1200Mpa的压力将粉末压制成型,保压5min脱模,得到样品。3) Add the lubricant zinc stearate into the insulating-coated metal soft magnetic powder according to the mass fraction of 0.1%, stir evenly, put it into the forming mold, heat and keep the magnetic powder in the mold cavity at a heating temperature of 60°C, and use The powder was pressed into shape under a pressure of 1200Mpa, and the pressure was kept for 5 minutes to demould to obtain a sample.

制备出的样品组织致密,孔隙率低,密度为8g/cm3,断裂拉力为43kg,将样品进行软磁性能和电学性能测试,结果如下:饱和磁通密度Bs=1.6T,矫顽力Hc=150A/m,电阻率ρ=3.7×105Ω·cm,损耗为120mW/cm3/(50KHz/0.05T),样品的机械性能,磁学和电学性能优异。The prepared sample has a compact structure, low porosity, a density of 8g/cm 3 , and a breaking force of 43kg. The soft magnetic and electrical properties of the sample were tested, and the results are as follows: saturation magnetic flux density Bs = 1.6T, coercive force Hc =150A/m, resistivity ρ=3.7×10 5 Ω·cm, and loss of 120mW/cm 3 /(50KHz/0.05T), the mechanical, magnetic and electrical properties of the sample are excellent.

实施例3:Example 3:

1)将磷酸和丙酮配成质量分数为5%的钝化液,按3:2:1的质量比取粒径分别为250μm、75μm、45μm的铁硅铝合金粉末和钝化液按照质量比为1:1的比例进行钝化,在搅拌机中搅拌2h,放入烘箱钝化,钝化温度为100℃,钝化时间为0.1h,得到钝化粉。1) Phosphoric acid and acetone are made into a passivation solution with a mass fraction of 5%, and the particle diameters are 250 μm, 75 μm, 45 μm and the passivation solution according to the mass ratio of 3:2:1. Passivate at a ratio of 1:1, stir in a mixer for 2 hours, put into an oven for passivation, the passivation temperature is 100°C, and the passivation time is 0.1h to obtain passivation powder.

2)将酚醛树脂和乙醇配成环氧树脂质量分数为5%的粘结剂溶液,将粘结剂溶液和钝化粉按照质量比为0.01:1的比例混合,搅拌机搅拌0.1h,搅拌均匀,在100℃烘箱中烘烤0.1h,烘干,得到绝缘包覆的金属软磁粉待用。2) Mix phenolic resin and ethanol into a binder solution with a mass fraction of epoxy resin of 5%, mix the binder solution and passivation powder according to the mass ratio of 0.01:1, stir with a mixer for 0.1h, and stir evenly , baked in an oven at 100° C. for 0.1 h, and dried to obtain insulating-coated metal soft magnetic powder for use.

3)将润滑剂硬脂酸钡按照质量分数1%加入绝缘包覆的金属软磁粉中搅拌均匀,装入成型模具中,对模腔内的磁粉进行加热并保温,加热温度为150℃,采用600Mpa的压力将粉末压制成型,保压30min脱模,得到样品。3) Add the lubricant barium stearate into the insulation-coated metal soft magnetic powder according to the mass fraction of 1%, stir evenly, put it into the forming mold, heat and keep the magnetic powder in the mold cavity at a heating temperature of 150°C, and use The powder was pressed into shape under a pressure of 600 MPa, and the pressure was maintained for 30 minutes to demould, and a sample was obtained.

制备出的样品组织致密,孔隙率低,密度为6.3g/cm3,断裂拉力为32kg,将样品进行软磁性能和电学性能测试,结果如下:饱和磁通密度Bs=1.1T,矫顽力Hc=35A/m,电阻率ρ=6.3×106Ω·cm,损耗为120mW/cm3/(50KHz/0.05T),样品的机械性能,磁学和电学性能优异。The prepared sample has a compact structure, low porosity, a density of 6.3g/cm 3 , and a breaking force of 32kg. The soft magnetic and electrical properties of the sample were tested, and the results are as follows: saturation magnetic flux density Bs = 1.1T, coercive force Hc=35A/m, resistivity ρ=6.3×10 6 Ω·cm, loss 120mW/cm 3 /(50KHz/0.05T), the sample has excellent mechanical, magnetic and electrical properties.

实施例4:Example 4:

1)将磷酸和丙酮配成质量分数为0.8%的钝化液,按3:1:1的质量比取粒径分别为150μm、75μm、0.1μm的铁硅硼非晶粉和钝化液按照质量比为1:0.08的比例进行钝化,在搅拌机中搅拌0.5h,放入烘箱钝化,钝化温度为80℃,钝化时间为1.5h,得到钝化粉。1) Phosphoric acid and acetone are made into a passivation solution with a mass fraction of 0.8%, and the iron-silicon-boron amorphous powder and the passivation solution with a particle size of 150 μm, 75 μm, and 0.1 μm are selected according to a mass ratio of 3:1:1. The mass ratio was 1:0.08 for passivation, stirred in a mixer for 0.5h, put into an oven for passivation, the passivation temperature was 80°C, and the passivation time was 1.5h to obtain passivation powder.

2)将酚醛树脂和乙醇配成环氧树脂质量分数为10%的粘结剂溶液,将粘结剂溶液和钝化粉按照质量比为0.1:1的比例混合,搅拌机搅拌0.5h,搅拌均匀,在80℃烘箱中烘烤2h,烘干,得到绝缘包覆的金属软磁粉待用。2) Mix phenolic resin and ethanol into a binder solution with a mass fraction of epoxy resin of 10%, mix the binder solution and passivation powder at a mass ratio of 0.1:1, stir with a mixer for 0.5h, and stir evenly , baked in an oven at 80° C. for 2 hours, and dried to obtain insulating-coated metal soft magnetic powder for use.

3)将六方BN按照质量分数0.3%加入绝缘包覆的金属软磁粉中搅拌均匀,装入成型模具中,对模腔内的磁粉进行加热并保温,加热温度为170℃,采用900Mpa的压力将粉末压制成型,保压20min脱模,得到样品。3) Add hexagonal BN into the insulation-coated metal soft magnetic powder according to the mass fraction of 0.3%, stir evenly, put it into the forming mold, heat and keep the magnetic powder in the mold cavity, the heating temperature is 170°C, and the pressure is 900Mpa. The powder was pressed and molded, and the pressure was maintained for 20 minutes to demould, and the sample was obtained.

制备出的样品组织致密,孔隙率低,密度为6.1g/cm3,断裂拉力为30kg,将样品进行软磁性能和电学性能测试,结果如下:饱和磁通密度Bs=1.0T,矫顽力Hc=5A/m,电阻率ρ=8.5×106Ω·cm,损耗为30mW/cm3/(50KHz/0.05T),样品的机械性能,磁学和电学性能优异。The prepared sample has a dense structure, low porosity, a density of 6.1g/cm 3 , and a breaking force of 30kg. The soft magnetic and electrical properties of the sample were tested, and the results are as follows: saturation magnetic flux density Bs = 1.0T, coercive force Hc=5A/m, resistivity ρ=8.5×10 6 Ω·cm, loss 30mW/cm 3 /(50KHz/0.05T), the sample has excellent mechanical, magnetic and electrical properties.

Claims (9)

1. warm compaction molding is prepared a method for soft magnetic metal composite material, it is characterized in that comprising the steps:
1) powder passivation
Solvent and passivator are made into passivating solution, and the soft magnetic metal powder that is 0.1~250 μ m by particle size mixes, and adds passivating solution, stirs 0.1~2h, puts into baking oven passivation, and passivation temperature is 40~100 ℃, and passivation time is 0.1~4h, obtains passivating powder;
2) insulating wrapped
Binding agent is dissolved in organic solvent, obtains binder solution, add binder solution in passivating powder, stir 0.1~2h, put into oven for drying, baking temperature is 40~100 ℃, and baking time is 0.1~4h, obtains the soft magnetic metal powder of insulating wrapped;
3) warm compaction molding
Lubricant is added in the soft magnetic metal powder of insulating wrapped and stir, pack in mould, soft magnetic metal powder in die cavity is heated and is incubated, heating-up temperature is 60~150 ℃, makes in pressing process, and binding agent occurs to solidify, adopt the pressure of 600~1200Mpa by powder pressing forming, pressurize 5~30min, the demoulding, obtains sample.
2. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described soft magnetic metal powder is reduced iron powder, carbonyl iron dust, sendust powder, Fe-Ni Alloy Powder, iron nickel-molybdenum alloy powder, ferrum-silicon-boron amorphous powder, ferro-silicium powder or iron silicon nickel alloy powder.
3. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described solvent is deionized water, ethanol, methylethylketone, acetone, butanone or ethyl acetate.
4. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described passivator is hydrogen peroxide, potassium permanganate, phosphoric acid or chromic acid.
5. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that the mass fraction of passivator in described passivating solution is 0.1~5%.
6. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described passivating solution and the mass ratio of soft magnetic metal powder are 0.01:1~1:1.
7. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described binding agent is epoxy resin, phenolic resins, polyvinyl alcohol, polyvinyl butyral resin or glass dust, in binder solution, the mass fraction of binding agent is 5~50%.
8. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described binder solution and the mass ratio of metal dust are 0.01:1~1:1.
9. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described lubricant is zinc stearate, barium stearate, acyl acidic group wax, lithium stearate or six side BN, 0.1~1% of the soft magnetic metal opaque amount that lubricant content is insulating wrapped.
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CN113724958A (en) * 2021-08-31 2021-11-30 安徽工业大学 Preparation method for producing iron-based soft magnetic iron core based on reduced iron powder alloying
CN113724958B (en) * 2021-08-31 2024-04-16 安徽工业大学 Preparation method for producing iron-based soft magnetic iron core based on reduced iron powder alloying
CN113990646A (en) * 2021-10-28 2022-01-28 山东恒瑞磁电科技有限公司 Preparation method of integrally formed inductor
CN113990646B (en) * 2021-10-28 2025-01-03 山东恒瑞磁电股份有限公司 A method for preparing an integrally formed inductor
CN114974873A (en) * 2022-06-21 2022-08-30 苏州锦鳞电子科技有限公司 Soft magnetic composite material, preparation method thereof and molded inductor
CN115475935A (en) * 2022-10-27 2022-12-16 广东金泓新材料有限公司 Preparation method of iron-based soft magnetic composite powder and iron-based soft magnetic composite powder
CN115475935B (en) * 2022-10-27 2023-08-22 广东金泓新材料有限公司 Preparation method of iron-based soft magnetic composite powder and iron-based soft magnetic composite powder
CN115762947A (en) * 2022-11-24 2023-03-07 深圳市铂科新材料股份有限公司 Insulation coating method of soft magnetic powder and application thereof
CN116598085A (en) * 2023-05-09 2023-08-15 东北大学 Preparation method of a high-frequency wide-temperature low-coercivity iron-based soft magnetic composite material
CN119381107A (en) * 2024-12-30 2025-01-28 浙江天通电子信息材料研究院有限公司 Nanocrystalline magnetic powder core and preparation method thereof
CN120299851A (en) * 2025-06-11 2025-07-11 浙江东睦科达磁电有限公司 A MHz-level low-loss sendust magnetic powder core and its preparation method

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