JP5094780B2 - Dust core - Google Patents

Description

  The present invention relates to a dust core.

  In recent years, electric vehicles have attracted attention from the viewpoint of environmental problems. An electric vehicle includes a rotating electric machine (motor) as a power source and a smoothing transformer (reactor) as an output of an inverter circuit, and improvement in the efficiency of these components is required.

  The magnetic cores used in these parts are required to have low iron loss and high magnetic flux density, and their magnetic properties do not deteriorate even in the region from low frequency to high frequency.

  The iron loss includes an eddy current loss that is closely related to the specific resistance of the magnetic core, and a hysteresis loss that is affected by distortion in the iron powder resulting from the process of iron powder production and the subsequent process history.

The iron loss W can be represented by the sum of the eddy current loss We and the hysteresis loss Wh as in the following formula (1). Here, f is the frequency, Bm is the excitation magnetic flux density, ρ is the specific resistance, t is the thickness of the material, and k ₁ and k ₂ are coefficients.

W = We + Wh = (k ₁ Bm ² t ² / ρ) f ² + k ₂ Bm ^1.6 f (1)
From the above formula (1), since the eddy current loss We increases in proportion to the square of the frequency f, it is indispensable to suppress the eddy current loss We especially in order not to deteriorate the magnetic characteristics at high frequencies. In order to suppress the generation of eddy currents in the dust core, it is necessary to optimize the size of the magnet powder to be used, and to use a dust core that has been compression-molded with the insulation film formed on the surface of each magnet powder. There is.

  When insulation is insufficient in such a dust core, the specific resistance ρ decreases and the eddy current loss We increases. On the other hand, when the insulating film is thickened to increase the insulation, the volume ratio occupied by the soft magnetic powder contained in the magnetic core decreases, and the magnetic flux density decreases.

  In addition, if compression molding of soft magnetic powder is performed at a high pressure in order to improve magnetic flux density and the density of soft magnetic powder is increased, distortion of soft magnetic powder during molding cannot be avoided and hysteresis loss Wh increases. As a result, it is difficult to suppress the iron loss W. In particular, in the low frequency region, since the eddy current loss We is small, the influence of the hysteresis loss Wh in the iron loss W becomes large.

  Until now, with respect to such problems, by applying an insulating coat (insulating coating) to the surface of iron or an alloy powder containing iron as a main component (hereinafter also referred to as magnetic powder or iron powder) A method has been proposed that secures insulation of the core, increases the specific resistance of the entire magnetic core, and reduces macro eddy current loss. As for the reduction of hysteresis loss, it is effective to increase the iron powder particle size, apparently dilute the magnetic deterioration factors such as oxidation of the particle surface, and to remove distortion during compression molding by heat treatment. It is also known that.

Regarding the heat treatment, the insulating coat on the surface of the iron powder is destroyed, and the magnetic core specific resistance is lowered to increase the eddy current loss. Therefore, the phosphate coat iron powder is 500 to 550 ° C, and the fluoride coat is 600 to 700 ° C. There is a limit of 600 to 900 ° C. with SiO ₂ coating.

  Here, if only the specific resistance is considered, there is an advantage that the ferrite core has a specific resistance exceeding 1 to 10 Ω · cm. On the other hand, the operating magnetic flux density can be increased by increasing the density of the dust core. An operating magnetic flux density of 1.5 to 1.6 T can be obtained if the density is increased to 95% with respect to about 0.5 T (Tesla) of the ferrite core.

  In order to increase the iron powder density, it is effective to mix a salt called metal soap, such as zinc stearate and lithium stearate, into the iron powder during compression molding, and mold together. Thereby, while preventing destruction of the insulating film due to rubbing between the iron powders, rotation of the iron powder is facilitated, and a high-density molded body can be obtained at a low pressure.

  However, the added lubricant is decomposed in the heat treatment to remove the powder and forms a mixture containing carbon, oxygen and nitrogen and a metal oxide when forming the dust core. Here, this mixture is referred to as a heat-modified product.

  When this heat-denatured product is generated, there is a problem that the mechanical strength of the powder magnetic core is greatly reduced. This has been considered to require improvement in applications for automobiles that require reliability and home appliances that require long-term stable operation.

  As a means for increasing the mechanical strength of the dust core, there is a binder addition. This is accomplished by adding a thermosetting resin such as a silicon resin to iron powder and functioning as a binder by a strain relief heat treatment. However, since resin does not have lubricity, mold lubrication in which a lubricant is applied to a compression mold is necessary. For this reason, there is a difficulty in increasing the magnetic core density, and high temperature heat treatment at 600 ° C. or higher has a difficulty in binder decomposition.

Patent Document 1 discloses that a magnetic powder having a heat-resistant insulating film and a powder core of a powder magnetic core having a high specific resistance and a low iron loss are provided with iron powder or iron as a main component. Magnetic powder having an insulating film (silica (SiO ₂ ) insulating film) formed using a treatment liquid containing at least one selected from alkoxysilane and derivatives thereof and alcohol and water on the surface of the alloy powder A density of 7.5 g / cm ³ or more, an average particle size of the magnetic powder of 30 to 200 μm, and an average thickness of the insulating film of 1 to 700 nm, A dust core having a specific resistance of 1000 μΩ · cm or more is disclosed.

  In Patent Document 2, in a powder magnetic core of an electric device formed using a magnetic powder for a powder magnetic core having an electric insulating layer on the surface, the electric insulating layer includes a lone electron pair that suppresses the formation of iron oxide. It is formed by mixing an antirust agent composed of an organic compound containing at least one of nitrogen or sulfur and an insulating layer forming treatment liquid containing a phosphate chemical conversion treatment liquid into the magnetic powder and drying at a predetermined temperature. A dust core is disclosed which is characterized in that

  Patent Document 3 discloses a magnetic powder composed of a powder composed mainly of an iron element whose surface is covered with an insulating coating, wherein the powder is a spherical powder or a powder whose surface is flattened. Discloses a magnetic powder characterized by being a coating of rare earth fluoride, alkali metal fluoride, or alkaline earth metal fluoride, and a dust core using the magnetic powder.

  Patent Document 4 discloses a method for producing an iron-based powder mixture in which particles of auxiliary raw materials are fixed to the surface of iron-based powder particles with a binder, and the iron-based powder and the auxiliary raw materials at a temperature below the melting point of the binder. And then spraying the melt of the binder onto the resulting mixture to fix the particles of the auxiliary raw material on the surface of the iron-based powder particles, and a method for producing the iron-based powder mixture is disclosed. Has been.

JP 2007-129154 A JP-A-10-154613 JP 2008-016670 A JP 2007-2111275 A

  An object of the present invention is to provide a dust core having a high magnetic flux density, low iron loss, and high mechanical strength.

  The dust core of the present invention is a dust core containing magnetic powder, fluoride particles, and a heat-modified product of a lubricant, and the magnetic powder has an oxide layer and / or an insulating layer on its surface. And having the fluoride particles and the heat-modified product between the adjacent magnetic powders, the adjacent oxide layer or insulating layer having a portion bonded via the fluoride particles. It is characterized by that.

  According to the present invention, it is possible to obtain a dust core having high density, high resistance, excellent magnetic properties, and high mechanical strength.

It is the graph which showed by comparison the extraction pressure by the kind of coating material of magnetic powder at the time of shape | molding a ring sample without adding a lubricant. It is a graph which shows the three-point bending strength by the presence or absence of a lubricant. It is a cross-sectional SEM photograph which shows the structure between the iron powder which comprises the powder magnetic core of the Example by this invention. It is a schematic cross section which shows the structure between the iron powder which comprises the powder magnetic core of the Example by this invention. It is a graph which shows the relationship between the bending strength of the powder magnetic core molded object of the Example by this invention, and magnesium fluoride addition amount. It is a graph which shows the relationship between the bending strength of the powder magnetic core molded object of the Example by this invention, and heat processing temperature. It is a graph which shows the relationship between the specific resistance of the powder magnetic core of the Example by this invention, and heat processing temperature.

  The present invention relates to a powder magnetic core manufactured by compression-molding magnetic powder containing an iron element, and more particularly to a powder magnetic core suitable for use in electric parts such as a rotating electric machine (including a motor) and a reactor. .

  As a result of our study, among the insulating coatings of silica, phosphate and fluoride described in Patent Documents 1 to 3, the insulating coating of fluoride is different from other insulating coatings and has no lubricant. It has also been found that there is little damage to the mold during compression molding.

FIG. 1 is a graph showing stress (extraction pressure) when a ring sample is molded without adding a lubricant and then the sample is detached from the mold. The dimensions of the ring sample are an outer diameter of 50 mm, an inner diameter of 40 mm, and a thickness of 5 mm. There are three types of coating materials (main components of the coating layer): magnesium fluoride (MgF ₂ ), phosphate, and silica (SiO ₂ ).

  From this figure, it can be seen that the iron powder coated with fluoride has a much lower extraction pressure than other coating materials, that is, fluoride has a lubricating ability. However, even a fluoride coat requires a lubricant because it requires 40 MPa or less for production compression protection.

  On the other hand, the use of a lubricant causes a significant decrease in the dust core strength.

  FIG. 2 shows the difference in three-point bending strength depending on the presence or absence of zinc stearate (lubricant) in iron powder having a fluoride coat (fluoride coating). Fig.2 (a) is a side view which shows typically the test piece of a 3 point | piece bending strength test, a fulcrum, and a power point. FIG. 2 (b) shows the test results.

  In FIG. 2A, the dimensions of the test piece (dust core) are 55 mm wide, 10 mm high, and 5 mm thick. The distance between the two fulcrums supporting the lower part of the test piece is 40 mm, and a force point for applying a downward force is provided at the upper center of the test piece.

  From this figure, it can be seen that the addition of lubricant causes a significant decrease in bending strength.

  This is because the lubricant (heat-modified product of the lubricant) denatured by heat treatment is present between the fluoride coatings of adjacent iron powders, which prevents the fluoride from being sintered. This is thought to be due to a significant decrease in strength.

  In order to reduce damage to the compression mold during molding, the dust core needs to be molded by mixing and adding metal soap powder such as zinc stearate to the magnetic powder. However, this lubricant has room for improvement in that it is carbonized during the heat treatment necessary for the dust core and becomes a low-strength heat-modified layer.

  An object of the present invention is to provide a dust core having a high density, a high resistance value, an excellent magnetic property, and a high strength.

  In the present invention, the structure of the heat-denatured layer is devised to increase the strength of the dust core.

  The dust core of the present invention is a dust core produced by using iron or an iron-based alloy magnetic powder, compression-molding the magnetic powder with a lubricant, and performing heat treatment. The magnetic powder has a natural oxide layer on the alloy interface formed at the time of powder generation and / or an interface layer including an insulating layer, and the adjacent magnetic powder is crosslinked by fluoride particles contained in the interface layer. It has a (bonded) portion, and the interface layer has a structure including a heat-modified product of the lubricant (organic material).

  Here, the magnetic powder is mainly iron or an alloy containing iron as a main component, but includes an alloy in which the ratio of cobalt or nickel is higher than that of iron.

  The features of the present invention will be described below.

  The present invention intends to obtain a dust core having excellent lubrication performance and high mechanical strength by using a mixture of zinc stearate and magnesium fluoride powder as a lubricant.

  Patent Document 4 discloses a configuration in which zinc stearate as a binder (adhesive) and calcium fluoride for improving the machinability of a sintered body are mixed with an iron-based powder, and the mixing amount of this calcium fluoride. Is 0.5 to 5% by weight based on the mass of the iron-based powder mixture. It is said. However, in Patent Document 4, there is no description regarding providing an insulating coating (insulating layer) on the surface of the iron-based powder and bonding (sintering) the insulating coating via calcium fluoride. There is no description about increasing the mechanical strength by mixing calcium fluoride particles.

  From the results of our studies, it has been found that the effect of improving the mechanical strength cannot be obtained with the above-mentioned mixed amount of calcium fluoride.

  As will be described later, the addition amount of magnesium fluoride is desirably 2 to 40% by weight (weight percent) based on the weight (addition amount) of the magnesium fluoride and lubricant mixture (lubricant mixture) before heat treatment. That is, since the addition amount of the lubricant based on the weight before the heat treatment of the mixture of the magnetic powder, the magnesium fluoride and the lubricant is 0.1 to 0.5% by weight, the addition amount of the magnesium fluoride Is 0.002 to 0.2% by weight (also referred to as 0.002 to 0.2% on a weight basis) based on the weight of the mixture of magnetic powder, magnesium fluoride and lubricant before heat treatment. desirable.

  Moreover, in order to improve the strength of the powder magnetic core, it is necessary to perform heat treatment at 600 to 800 ° C.

  Hereinafter, the present invention will be described using examples.

  In this example, iron powder having a magnesium fluoride film formed on the surface was used as the magnetic powder, and zinc stearate was used as the lubricant. As fluoride particles, magnesium fluoride particles were used.

  A treatment liquid for forming an insulating coating (insulating layer) on the surface of the iron powder was prepared by the following procedure.

  (1) 4 g of magnesium acetate was introduced into 100 mL of water and completely dissolved using a shaker or an ultrasonic stirrer.

(2) Hydrofluoric acid diluted to 10% was gradually added in an amount equivalent to the chemical reaction that produces magnesium fluoride (MgF ₂ ).

(3) it was stirred for 1 hour or longer using an ultrasonic stirrer to a solution of MgF ₂ was formed of gelatinous precipitates.

  (4) 4000-6000 r. p. m. After centrifuging at the number of revolutions, the supernatant was removed and approximately the same amount of methanol was added.

(5) A methanol solution containing gelled MgF ₂ was stirred to make a complete suspension, and then stirred for 1 hour or more using an ultrasonic stirrer.

  (6) The above operations (4) and (5) were repeated 3 to 10 times until no anion such as acetate ion or nitrate ion was detected.

(7) Finally, a MgF ₂ treatment solution (MgF ₂ concentration was 1 g / 4 mL), which was a sol-like methanol-based solution, was obtained.

A ball mill treatment was performed on 400 g of the iron powder, and then a magnesium fluoride film was formed on the surface of the iron powder using the above-described treatment liquid, and each 50 g was separated. Each iron powder especially, iron powder (magnetic powder) and 0.3 weight percent based on the weight before the thermal treatment of the mixture of zinc stearate (lubricant) of zinc stearate (% by weight) powder, and stearic Add 1 to 80% by weight of magnesium fluoride (average particle size 0.5μm) based on the weight of the mixture of zinc oxide and magnesium fluoride before heat treatment, and put into a mixer to knead each for 30 minutes It was.

20 g of the mixed iron powder obtained by this kneading was sampled and press-molded by applying a pressure of 12 t / cm ² to a rectangular parallelepiped sample having a 55 × 10 mm cross section. The finished thickness is approximately 5 mm.

  This sample was heat treated in vacuum at 600 ° C. for 0.5 hours to remove strain.

  FIG. 3 is a cross-sectional SEM photograph showing the structure between the iron powders constituting the dust core of the example according to the present invention.

In the figure, there is a fluoride coat layer (MgF ₂ coating) on the surface of the iron powder on both the upper and lower sides, and there is a lubricant altered layer (also referred to as a heat-modified product of the lubricant) in the gap. Then, it contains MgF ₂ particles on a part of the gap.

  FIG. 4 is a schematic cross-sectional view showing the structure between iron powders constituting the powder magnetic core of the example according to the present invention.

In the figure, there are fluoride coat layers (MgF ₂ coatings) on the surfaces of the left and right iron powders, and there are lubricant alteration layers (also referred to as heat-modified products of lubricants) in the gaps. Then, it contains MgF ₂ particles on a part of the gap.

The MgF ₂ particles located in the center of this figure are in close contact with and bonded (sintered) to the fluoride coat layers on both sides. Thereby, while maintaining the electrical insulation state between iron powder, the mechanical strength of a dust core is improved.

  Using this sample, a three-point bending test shown in FIG.

  FIG. 5 is a graph showing the relationship between the bending strength and the magnesium fluoride addition amount of the powder magnetic core molded body of the example according to the present invention. The horizontal axis indicates the amount of magnesium fluoride added (wt% (wt%)) in the mixture of magnesium fluoride and lubricant (lubricant mixture), and the vertical axis indicates the bending strength.

  When the addition amount of magnesium fluoride was 0, the bending strength was very low at 6 MPa, but the strength increased with the increase in addition amount, and a maximum strength of 37 MPa was obtained at an addition amount of 10% by weight. Furthermore, when the addition amount was increased, the strength was lowered, and when the amount was increased to 80% by weight, the strength was 5 MPa.

  From this figure, it can be seen that the addition amount of magnesium fluoride in the lubricant mixture is desirably 2 to 40% by weight.

  In this embodiment, an example in which the insulating coating (insulating layer) is formed of magnesium fluoride is shown, but the present invention is not limited to this, and alkaline earth metal fluoride or rare earth metal fluoride may be used. Good.

  In the present embodiment, the example in which the fluoride particles are magnesium fluoride particles is shown, but the present invention is not limited to this, and particles such as alkaline earth metal fluorides or rare earth metal fluorides are used. May be.

  In the present embodiment, the example in which the lubricant is zinc stearate has been shown, but the lubricant is not limited to this, and salts of alkaline earth metals such as magnesium, calcium, strontium, barium (metal stearate) Salt) or a metal salt (stearic acid metal salt) such as lithium, iron, cobalt, nickel, titanium, vanadium, or copper. Also, fatty acid salts (fatty acid metal salts) such as caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, palmitoleic acid, oleic acid, linoleic acid, and linolenic acid may be used. Furthermore, salts such as alkyl sulfates, alkylbenzene sulfates, alkyl phosphates, and alkylbenzene phosphates may be used.

  The fatty acid metal salt is preferably a stearic acid metal salt, and the stearic acid metal salt is preferably zinc stearate or lithium stearate.

After 300 g of iron powder was ball milled, a magnesium fluoride film was formed on the surface of the iron powder using the treatment liquid described in Example 1, and 50 g was separated. Each especially the iron powder, iron powder (magnetic powder) and 0.3% by weight of powder of zinc stearate based on the weight before the thermal treatment of the mixture of zinc stearate (lubricant), and zinc stearate and hydrofluoric Based on the weight of the magnesium halide mixture before heat treatment, 10% by weight of magnesium fluoride having an average particle size of 0.5 μm was added, and the mixture was put into a mixer and kneaded for 30 minutes.

20 g of the mixed iron powder obtained by this kneading was sampled and press-molded by applying a pressure of 12 t / cm ² to a rectangular parallelepiped sample having a 55 × 10 mm cross section. The finished thickness is approximately 5 mm.

  This sample was heat-treated in a vacuum at 500 to 1000 ° C. for 0.5 hours to remove strain.

  Using this sample, a three-point bending test shown in FIG.

  FIG. 6 is a graph showing the relationship between the bending strength and the heat treatment temperature of the powder magnetic core molded body of the example according to the present invention.

  From this figure, it can be seen that the higher the heat treatment temperature, the higher the bending strength. When the heat treatment temperature is 500 ° C., the bending strength is low, but when the heat treatment temperature is 600 ° C., the bending strength increases. Furthermore, it turns out that it increases rapidly at 900 degreeC. That is, it is understood that a heat treatment temperature of 600 ° C. or higher is desirable.

  FIG. 7 is a graph showing the relationship between the specific resistance of the dust core of the example according to the present invention and the heat treatment temperature.

  From this figure, it can be seen that the specific resistance of the dust core decreases as the heat treatment temperature increases, and falls below the measurement limit at 900 to 1000 ° C. This is considered to be because the magnesium fluoride of the coating broke and the sintering of the iron powder proceeded at 900 ° C. or higher.

  Therefore, it can be seen from this figure that the heat treatment temperature is desirably 800 ° C. or lower.

  6 and 7 that the heat treatment temperature of 600 to 800 ° C. is desirable.

Claims (10)

And magnetic powder, a dust core comprising a fluoride particles, and a heat denaturation of the lubricant, the magnetic powder has an insulating layer formed of a fluoride on the surface thereof, Aitonaru the insulation having said fluoride particles and the heat denaturation was between layers, dust core, wherein the insulating layer Ru Neighboring is characterized by having a moiety linked through the fluoride particles.   2. The dust core according to claim 1, wherein the insulating layer contains an alkaline earth metal fluoride or a rare earth metal fluoride.   The dust core according to claim 1 or 2, wherein the fluoride particles include an alkaline earth metal fluoride or a rare earth metal fluoride.   The dust core according to any one of claims 1 to 3, wherein the lubricant contains a stearic acid metal salt.   The dust core according to claim 4, wherein the metal stearate includes zinc stearate or lithium stearate.   The dust core according to any one of claims 1 to 5, wherein the fluoride particles include magnesium fluoride.   The amount of the fluoride particles added is 0.002 to 0.2% based on the weight before heat treatment of the mixture of the magnetic powder, the fluoride particles, and the lubricant. The dust core according to any one of the above. The dust core according to claim 7, wherein a heat treatment temperature of the mixture is 600 to 800 ° C. A reactor using the dust core according to any one of claims 1 to 8 . A rotary electric machine using the dust core according to any one of claims 1 to 8 .

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