Embodiment
The present invention will be described in more detail.
Result as further investigation, if the inventor finds following alloy composite and selects as the soft magnetic metallic glass powder with excellent economic benefit, then can obtain to have the powder that excellent magnetic matter and glass form performance: as (Fe, Co, Ni)-(Al, Si, C, the P)-B-MM ' of the basic alloy of FeSiBMM ' (M=is selected from least a among Zr, Nb, Ta, Hf, Mo, Ti, V, Cr and the W, at least a among Zn, Sn and the R (wherein R is at least a element that is selected from the rare earth metal that comprises Y) of M '=be selected from).The inventor also finds if by making powder carry out oxidation or insulation coating, use die head etc. powder to be formed molding then and obtain powder core by suitable method of moulding, then this powder core is a kind of high magnetic permeability powder core that shows at wide band excellent magnetic permeability and the excellent properties that never obtained, thereby can low-cost prepare a kind of high frequency magnetic core that is made of the soft magnetic material with high saturation magnetic flux metric density and high specific resistance.In addition, find that inductance element by providing high frequency magnetic core with at least one turn coil to obtain is cheap and have before the high-performance that never has.
The inventor also finds, by limiting the granularity of forming the soft magnetic metallic glass powder that general formula represents by above-mentioned, this powder core is in the core loss aspect of performance excellence of high frequency.In addition, find that inductance element by providing high frequency magnetic core with at least one turn coil to obtain is cheap and have before the high-performance that never has.Also find to obtain to be suitable for the inductance element that the big electric current of high frequency is used by forming with the state compacting that forms internal structure so that coil is imbedded in the magnet.
In order to increase the ratio resistance of molding, molded alloy powder before can carry out oxidizing thermal treatment in atmospheric air.In order to form the high density molded body, can under the temperature that is not less than as the softening point of the resin of adhesive, continue molded.In order to realize the high density of molding, molded can in the sub-cooled liquid temperature scope of alloy powder, carrying out.
Specifically, the soft magnetic metallic glass powder has the alloy composition that following general formula is represented: (Fe
1-a-bNi
aCo
b)
100-x-y-z(M
1-pM '
p)
xT
yB
z(wherein, 0≤a≤0.30,0≤b≤0.50,0≤a+b≤0.50,0≤p≤0.5,1 atom %≤x≤5 atom %, 1 atom %≤y≤12 atom %, 12 atom %≤z≤25 atom %, the atom % of 22 atom %≤(x+y+z)≤32, M is selected from least a among Zr, Nb, Ta, Hf, Mo, Ti, V, Cr and the W, and M ' is for being selected from least a among Zn, Sn and the R (wherein R is at least a element that is selected from the rare earth metal that comprises Y), and T is selected from least a among Al, Si, C and the P).This molding obtains by the mixture of molded soft magnetic metallic glass powder and scheduled volume adhesive, and described scheduled volume is the mass ratio with respect to the soft magnetic metallic glass powder.
To the alloy composition of soft magnetic metallic glass powder be described herein.Fe as key component is the element that helps magnetic, and is for obtaining the indispensable element of high saturation magnetic flux metric density.Part Fe can be replaced by Ni and/or Co, and the ratio of each or total amount is 0~0.5.This replacement component has improves the effect that glass forms performance.Herein, the replacement ratio of Ni is 0~0.3.Especially, the Co expection has the effect that improves saturation flux density simultaneously.In whole alloy powder, the total amount of Fe and substituted element (one or more) is being not less than 68 atom % and is being not more than in the scope of 78 atom %.This be because, if this content is not 68 atom % or bigger, then saturation flux density is too low, practicality loss is if this content is greater than 78 atom %, then because crystallization causes the magnetic permeability and the core loss reduction of magnetic core.
Element M is to improve glass to form the required transition metal of performance, and it is at least a element of selecting from Zr, Nb, Ta, Hf, Mo, Ti, V, Cr and W.The content of element M is for being not less than 1 atom % and being not more than 5 atom %.This be because if content less than 1 atom %, the remarkable deterioration of then forming of glass decreased performance, and magnetic permeability and core loss, if this content surpasses 5 atom %, then saturation flux density reduces, and practicality loses.Replace the element M of 0~0.5 ratio by Zn, Sn, R (R is at least a element that is selected from the rare earth metal that comprises Y), then form the ratio that can increase Fe, Co, Ni under the situation of performance, so that can improve saturation flux density at deterioration glass not.
Si and B are the necessary element of preparation soft magnetic metallic glass powder.Si content is being not less than 1 atom % and is being not more than in the scope of 12 atom %.B content is being not less than 12 atom % and is being not more than in the scope of 25 atom %.If this be because if Si content less than 1 atom % or greater than 12 atom % or B content less than 12 atom % or greater than 25 atom %, then glass forms performance and reduces, and can not prepare stable soft magnetism glass powder.Herein, Si can use Al, P and C to replace.The total amount of Al, P and C is not more than 0.5 quality %, because surpass above-mentioned scope, and the serious deterioration of then amorphous formation, the therefore character that can not obtain to be scheduled to.
The soft magnetic metallic glass powder is by water atomization or gas atomization preparation.Preferably at least 50% granularity is for being not less than 10 μ m.Especially, water atomization is thought low cost and is prepared the method for alloy powder in a large number.Can prepare powder by this method very large advantage is arranged on commercial Application.Yet if traditional amorphous compositions, 10 μ m or bigger alloy powder be crystallization, makes the remarkable deterioration of magnetic property.As a result, productive rate seriously descends, thereby has hindered commercial Application.On the other hand, if granularity is 150 μ m or littler, soft magnetic metallic glass powder then according to the present invention is easy to vitrifying (amorphization).Therefore, productive rate height.Therefore from cost consideration, soft magnetic metallic glass powder of the present invention has very big advantage.In addition, preparing in the alloy powder, on powder surface, forming suitable oxide coated film by water atomization.Therefore, by resin being mixed with alloy powder and, being easy to obtain to have the magnetic core of high specific resistance with the molded formation molding of mixture.
In in the alloy powder of the alloy powder of water atomization preparation and gas atomization preparation any,, then form more excellent oxidation thing coated film if carry out under the temperature of heat treatment alloy powder crystallization temperature of using He in the atmospheric air not being higher than.At this moment, can improve the ratio resistance of magnetic core, so that reduce the core loss of magnetic core.
On the other hand, for the inductance element of intending being used for frequency applications, can having very by use, the metal dust of small grain size reduces the vortex flow loss.Yet for alloy composition well known in the art, if average diameter is 30 μ m or littler, the powder oxidation is remarkable in preparation process.Therefore, in powder, be difficult to obtain pre-determined characteristics by common water atomization plant preparation.Yet the metal glass powder has excellent alloy corrosion resistance, so this metal glass powder is advantageous, even because powder is very little, also can be easier to prepare the powder that oxygen content reduces and have excellent properties.
Then, be described as the method for type molding.Basically, 10% quality is than adhesive such as the silicones and the soft magnetic metallic glass powder of content.Use die head or, can obtain molding by casting.This molding is as high frequency magnetic core, and it has 50% or bigger powder filling rate example, 1.6 * 10
4Have 0.5T or bigger magnetic density in the application in A/m magnetic field, and have 1 * 10
4The ratio resistance of cm.Herein, the content of binding agent is 10% or littler mass ratio.This be because, if this content surpasses 10%, then saturation flux density becomes and is equal to or less than ferritic saturation flux density, magnetic core loses practicality.Molding can be by mixing soft magnetic metallic glass powder and adhesive, and use die head this mixture of compression forming and obtain, in the mass ratio of soft magnetic metallic glass powder, the amount of adhesive is 5% or littler mass ratio.In this case, molding has 70% or bigger powder filling rate example, uses 1.6 * 10
4Have 0.75T or bigger magnetic density during A/m magnetic field, and have 1 Ω cm or bigger ratio resistance.When magnetic density is 0.75T or bigger and be 1 Ω m or when bigger than resistance, to compare with sendust core, the more excellent and practicality of its performance is further improved.In addition, molding can be by mixing soft magnetic metallic glass powder and adhesive, and under the temperature conditions that is not higher than the adhesive softening point, use die head this mixture of compression forming and obtain, in the mass ratio of soft magnetic metallic glass powder, the amount of adhesive is 3% or littler mass ratio.In this case, molding has 80% or bigger powder filling rate example, uses 1.6 * 10
4Have 0.9T or bigger magnetic density during A/m magnetic field, and have 0.1 Ω cm or bigger ratio resistance.When magnetic density is 0.9T or bigger and be 0.1 Ω m or when bigger than resistance, to compare with commercially available any powder core at present, the more excellent and practicality of its performance is further improved.In addition, molding can be by mixing soft magnetic metallic glass powder and adhesive, and in the sub-cooled liquid temperature scope of soft magnetic metallic glass powder this mixture of compression forming and obtaining, in the mass ratio of soft magnetic metallic glass powder, the amount of adhesive is 1% or littler mass ratio.In this case, molding has 90% or bigger powder filling rate example, uses 1.6 * 10
4Have 1.0T or bigger magnetic density during A/m magnetic field, and have 0.01 Ω cm or bigger ratio resistance.When magnetic density is 1.0T or bigger and be 0.01 Ω m or when bigger than resistance, magnetic density is substantially equal to comprise the magnetic density of the layers of magnetic core of amorphous metal and high silicon steel plate in the application region.Yet the molding of Huo Deing has little hysteresis loss and high ratio resistance herein, so core loss character is very excellent.Like this, further improve as the practicality of magnetic core.
In addition, after the moulding, can under the temperature conditions that is not higher than as the heat treated Curie point of strain relief, heat-treat as the molding of high frequency magnetic core.In this case, core loss further reduces, and further improves as the usability of magnetic core.Here, for keeping interparticle insulating properties, need to comprise SiO in the part intermediate materials between the alloy powder particle at least
2(as selection, all intermediate materials can all be SiO
2).
If desired after forming the gap on the part magnetic circuit, if, then can prepare the product that in the highfield, shows high magnetic permeability and have excellent properties by equipping above-mentioned inductance element with high frequency magnetic core preparation of at least one turn coil.
Fig. 1 is the external perspective view that high frequency magnetic core 1 basic structure according to an embodiment of the invention is shown.Fig. 1 illustrates the state that the high frequency magnetic core 1 that uses above-mentioned soft magnetic metallic glass powder forms annular plate.
Fig. 2 is the external perspective view that has the inductance element that the high frequency magnetic core 1 of coil obtains by equipment.The coil 3 that Fig. 2 illustrates pre-fixing turn has the state that lead-in wire is pulled out the inductance element 101 of part 3a and 3b around high frequency magnetic core 1 winding as annular plate with preparation.
Fig. 3 illustrates the external perspective view of high frequency magnetic core 1 basic structure according to another embodiment of the invention.Fig. 3 illustrates the high frequency magnetic core 1 that uses above-mentioned soft magnetic metallic glass powder and forms annular plate, and forms the state in gap (gap) 2 on the part magnetic circuit.Gap 2 is that the blank that is filled with insulating material is gone or the interval.As insulating material, suitable have a thermal endurance insulating trip.
Fig. 4 has coil 3 and has the external perspective view of inductance element 101 of high frequency magnetic core 1 preparation in gap 2 by equipment.Fig. 4 illustrates the coil 3 that twines pre-fixing turn around the high frequency magnetic core 1 as the annular plate with gap 2 and has the state that lead-in wire is pulled out the inductance element 102 of part 3a and 3b with preparation.
If the mixture by molded soft magnetic metallic glass powder with above-mentioned metal glass composition and adhesive forms powder core, then this powder core shows and have low-down loss character when high frequency, and the excellent properties that never obtained before having, described soft magnetic metallic glass powder has 45 μ m or littler maximum particle size on granularity, have 30 μ m or littler average diameter, and in the mass ratio of soft magnetic metallic glass powder, the content of described adhesive is 10% or littler mass ratio.Have the powder core of coil by equipment, obtain inductance element with excellent Q character.In addition, the magnet that has embedding coil wherein by press forming can obtain to be applicable to the inductance element of big high-frequency current to form complete structure.
The reason that limits particle size will be described in detail herein.If maximum particle size surpasses 45 μ m on granularity, then in the Q of high-frequency region character deterioration.In addition, if average diameter is not 30 μ m or littler, then 500kHz or higher on Q character can not surpass 40.In addition, if average diameter is not 20 μ m or littler, then 1MHz or higher on the Q value can not be 50 or bigger just.The advantage of metal glass powder is because the ratio resistance of alloy self is 2~10 times of traditional material, even thereby under same particle sizes Q character also high.If identical Q character is abundant, then spendable particle size range broadens, so that has reduced the powder production cost.
Fig. 5 is the external perspective view of the high frequency inductance element basic structure of another embodiment according to the present invention.With reference to figure 5, long plate shape material (bar material) 5 that is formed by above-mentioned soft magnetic metallic glass powder twines with the in-plane (horizontal direction in the drawings) of plate, forms winding coil 7.This winding coil is embedded in the magnet 8, and described magnet 8 contains the mixture of Magnaglo and adhesive.In this case, carry out compression molding, to obtain overall structure as inductance element 103.The winding coil 7 of board-like material 7 has the part that protrudes from the opposite both ends of the surface of magnet 8 as pigtail splice.The whole surface of the winding part of board-like material 5 all is mounted with insulating coating 6.
Now, in conjunction with the several embodiment of production technology and inductance elements that comparing embodiment is described high frequency magnetic core of the present invention and this high frequency magnetic core of use of comprising.
(embodiment 1~36, comparing embodiment 1~13)
At first, as the powder preparation step, weighing comprises that the simple metal element material of Fe, Si, B, Nb and replacement element is to obtain predetermined composition.By using these materials, various soft-magnetic alloy powders prepare by normally used water atomization.Here to notice that mischmetal(l) (mishmetal) is the mixture of rare earth metal.Using 30%La, 50%Ce, 15%Nd and surplus herein, is the mixture of other one or more rare earth elements.
Then, as the molding preparation process, various alloy powders are divided into the alloy powder with 45um or littler powder size.Subsequently, sneak into 5% mass ratio as the organic siliconresin of adhesive.Then, by using band groove and outer dia φ
Outward=27mm, inside diameter φ
InThe die head of=14mm is by in room-temperature applications 14.7 * 10
8The pressure of Pa and form various moldings makes the molding height equal 5mm.
In addition, various moldings carry out resin solidification.Subsequently, measure the weight and the size of various moldings.Then, provide the coil of the suitable number of turns to prepare various inductance elements (having shape shown in Figure 2).
Then, for each different sample of inductance element, use the LCR meter to obtain magnetic permeability from the inductance value of 100kHz.In addition, by using dc magnetic energy determinator, when using 1.6 * 10
4During the magnetic field of A/m, measure saturation flux density.In addition, the upper and lower surface of each magnetic core is all polished, and carries out X-ray diffraction (XRD) and measure to observe phase.The gained result is table 1 illustrate.
Table 1 illustrates the ratio of components of sample.In addition, if the XRD figure case that obtains by XRD determining only is found to be the broad peak of glassy phase feature then is judged as glassy phase, if the spike owing to crystallization can be observed with broad peak, then be judged as (glass+crystallization) phase, if do not have the broad peak value to observe spike then be judged as crystalline phase.Have the composition sample of glassy phase for those, confirm that as the glass transition temperature of the hot assay determination of DSC and crystallization temperature the sub-cooled liquid temperature range delta Tx for all samples is 30K or higher.Measure the ratio resistance of molding (magnetic core) by the two ends DC measurement.As a result, confirm that all samples shows the excellence that is not less than 1 Ω cm and compares resistance.
The temperature increase rate of DSC is 40K/min.Find out from embodiment 1~3 and comparing embodiment 1 and 2, can infer,, then can obtain to have the magnetic core of glassy phase if Nb content is 3~6%.Yet, find at Nb content to be that magnetic density is low to moderate 0.75T or littler in 6% the comparing embodiment 2.From embodiment 4~10 and comparing embodiment 3~6, can think if Si content be 1 or bigger, B content be 25 or littler, Fe content be 68~78, then can obtain to have the magnetic core of glassy phase.From embodiment 11~16 and comparing embodiment 7 and 8, can think with Ni, Co instead of part Fe, even Nb content is 1%, also can obtain the metal glass powder.Yet, surpass 0.3 if find the replacement amount of Ni, and the replacement amount of Co surpasses 0.5, the effect of the magnetic density that can not be improved (comparing with embodiment 1).Shown in embodiment 17~20, think that also Ni and Co can make up adding, and use Ta, Mo to replace Nb can obtain similar effect.
From embodiment 21~24 and comparing embodiment 9 and 10, can think if the amount of Nb is 1%, then can not form glassy phase with high magnetic permeability, and if this content surpasses 2% or bigger, then can form glassy phase.In addition, can think,, then can not form glassy phase if still replace ratio to surpass 0.5 by replacing Nb can improve saturation flux density with Zn.
Table 1
| Alloy composition | 1.6 * 10
4Magnetic flux density/T during A/m
| Magnetic permeability at 100kHz | The XDR measurement result |
Comparing embodiment
1 | Fe
74Si
4B
20Nb
2 | 0.92/T | 22 | Crystalline phase |
Embodiment 1 | Fe
73Si
4B
20Nb
3 | 0.87 | 31 | Glassy phase |
Embodiment 2 | Fe
72Si
4B
20Nb
4 | 0.82 | 33 | Glassy phase |
Embodiment 3 | Fe
71Si
4B
20Nb
5 | 0.77 | 35 | Glassy phase |
Comparing embodiment
2 | Fe
70Si
4B
20Nb
6 | 0.72 | 37 | Glassy phase |
Comparing embodiment
3 | Fe
77Si
0B
20Nb
3 | 0.98 | 19 | Crystalline phase |
Embodiment 4 | Fe
76Si
1B
20Nb
3 | 0.95 | 30 | Glassy phase |
Embodiment 5 | Fe
75Si
2B
20Nb
3 | 0.93 | 32 | Glassy phase |
Embodiment 6 | Fe
73Si
4B
20Nb
3 | 0.87 | 34 | Glassy phase |
Embodiment 7 | Fe
68Si
9B
20Nb
3 | 0.76 | 36 | Glassy phase |
Comparing embodiment
4 | Fe
67Si
10B
20Nb
3 | 0.70 | 21 | Crystalline phase |
Comparing embodiment
5 | Fe
79Si
4B
14Nb
3 | 0.95 | 20 | Crystalline phase |
Embodiment 8 | Fe
78Si
4B
15Nb
3 | 0.94 | 33 | Glassy phase |
Embodiment 9 | Fe
73Si
4B
20Nb
3 | 0.87 | 35 | Glassy phase |
Embodiment 10 | Fe
68Si
4B
25Nb
3 | 0.80 | 37 | Glassy phase |
Comparing embodiment
6 | Fe
67Si
4B
26Nb
3 | 0.79 | 23 | Crystalline phase |
Embodiment 11 | (Fe
0.9Ni
0.1Co
0)
75Si
4B
20Nb
1 | 0.92 | 32 | Glassy phase |
Embodiment 12 | (Fe
0.8Ni
0.2Co
0)
75Si
4B
20Nb
1 | 0.87 | 34 | Glassy phase |
Embodiment 13 | (Fe
0.7Ni
0.3Co
0)
75Si
4B
20Nb
1 | 0.82 | 36 | Glassy phase |
Comparing embodiment
7 | (Fe
0.6Ni
0.4Co
0)
75Si
4B
20Nb
1 | 0.77 | 38 | Glassy phase |
Embodiment 14 | (Fe
0.9Ni
0Co
0.1)
75Si
4B
20Nb
1 | 0.92 | 31 | Glassy phase |
Embodiment 15 | (Fe
0.8Ni
0Co
0.2)
75Si
4B
20Nb
1 | 0.95 | 33 | Glassy phase |
Embodiment 16 | (Fe
0.7Ni
0Co
0.5)
75Si
4B
20Nb
1 | 0.88 | 35 | Glassy phase |
Comparing embodiment
8 | (Fe
0.6Ni
0Co
0.6)
75Si
4B
20Nb
1 | 0.85 | 37 | Glassy phase |
Embodiment 17 | (Fe
0.7Ni
0.1Co
0.2)
75Si
4B
20Nb
1 | 0.88 | 34 | Glassy phase |
Embodiment 18 | (Fe
0.7Ni
0.1Co
0.2)
74Si
4B
20Nb
2 | 0.84 | 36 | Glassy phase |
Embodiment 19 | (Fe
0.7Ni
0.1Co
0.2)
74Si
4B
20Ta
2 | 0.84 | 34 | Glassy phase |
Embodiment 20 | (Fe
0.7Ni
0.1Co
0.2)
74Si
4B
20Mo
2 | 0.84 | 35 | Glassy phase |
Table 2
| Alloy composition | 1.6 * 10
4Magnetic flux density/T during A/m
| Magnetic permeability at 100kHz | XRD determining result |
Comparing embodiment
9 | Fe
75Si
7B
17Nb
1 | 0.91 | 18 | Crystalline phase |
Embodiment 21 | Fe
74Si
7B
17Nb
2 | 0.87 | 35 | Glassy phase |
Embodiment 22 | Fe
73Si
7B
17Nb
3 | 0.82 | 37 | Glassy phase |
Embodiment 23 | Fe
73Si
7B
17Nb
2Zn
1 | 0.84 | 37 | Glassy phase |
Embodiment 24 | Fe
73Si
7B
17Nb
1.5Zn
1.5 | 0.85 | 35 | Glassy phase |
Comparing embodiment
10 | Fe
73Si
7B
17Nb
1Zn
2 | 0.86 | 19 | Crystalline phase |
Comparing embodiment
11 | Fe
75Si
7B
17Nb
0Zn
1 | 0.93 | 17 | Crystalline phase |
Embodiment 25 | Fe
74Si
7B
17Nb
1Zn
1 | 0.89 | 33 | Glassy phase |
Embodiment 26 | Fe
71Si
7B
17Nb
4Zn
1 | 0.75 | 37 | Glassy phase |
Comparing embodiment
12 | Fe
70Si
7B
17Nb
5Zn
1 | 0.68 | 35 | Glassy phase |
Embodiment 27 | Fe
73Si
7B
17Nb
2Sn
1 | 0.81 | 35 | Glassy phase |
Embodiment 28 | Fe
73.5Si
7B
17Nb
2 (misch metal)
0.5 | 0.85 | 35 | Glassy phase |
Embodiment 29 | (Fe
0.9Ni
0.1Co
0)
74Si
7B
17Nb
1Zn
1 | 0.87 | 34 | Glassy phase |
Embodiment 30 | (Fe
0.8Ni
0Co
0.2)
74Si
7B
17Nb
1Zn
1 | 0.89 | 32 | Glassy phase |
Embodiment 31 | (Fe
0.7Ni
0.1Co
0.2)
74Si
7B
17Nb
1Zn
1 | 0.88 | 33 | Glassy phase |
Embodiment 32 | (Fe
0.7Ni
0.1Co
0.2)
73Si
7B
17Ta
2Zn
1 | 0.78 | 32 | Glassy phase |
Embodiment 33 | (Fe
0.7Ni
0.1Co
0.2)
73Si
7B
17Mo
2Zn
1 | 0.76 | 34 | Glassy phase |
Embodiment 34 | (Fe
73Si
12B
12Nb
2)+ (Al
0.05C
0.05P
0.05)wt%
| 0.86 | 33 | Glassy phase |
Embodiment 35 | (Fe
73Si
9B
14Nb
3)+ (Al
0.1C
0.1P
0.1)wt%
| 0.81 | 35 | Glassy phase |
Embodiment 36 | (Fe
73Si
9B
14Nb
3)+ (Al
0.3C
0.1P
0.1)wt%
| 0.80 | 33 | Glassy phase |
Comparing embodiment
13 | (Fe
73Si
9B
14Nb
3)+ (Al
0.2C
0.2P
0.2)wt%
| 0.80 | 15 | Crystalline phase |
As for the total amount of Zn and Nb, from embodiment 25 and 26 and comparing embodiment 11 and 12 can infer 5% or be suitable more for a short time.Can infer from embodiment 27 and 28,, can obtain similar effect if add Sn or mischmetal(l) replacement Zn.Can infer from embodiment 29~31, be replaced by Ni or Co and these two kinds of elements can make up adding, then can obtain similar effect as fruit part Fe.Shown in embodiment 32 and 33,, then can obtain type effect if Ta or Mo are used to replace Nb.Shown in embodiment 34~36 and comparing embodiment 13, can add Al, C and P.Yet,, form the remarkable variation of ability of impalpable structure if total amount surpasses 0.5 quality %.
(embodiment 37)
Has (Fe by the water atomization preparation
0.8Ni
0Co
0.2)
75Si
4B
20Nb
1The alloy powder of forming.The powder of Huo Deing is divided into the powder with 75 μ m or smaller szie like this.Carry out XRD determining, determined broad peak as the glassy phase feature.Then, carry out DSC heat and analyze, thereby determine that Δ Tx is 35K with mensuration glass transition temperature and crystallization temperature.Then, this powder is at atmospheric air and be lower than 450 ℃ of heat treatments 0.5 hour of glass transition temperature, thereby forms oxide on powder surface.Then, this powder and 10%, 5%, 2.5%, 1% and 0.5% silicones mix.By using the die head of φ 27 * φ 14, these powder in room temperature, be higher than carry out under 550 ℃ of these three kinds of conditions in 150 ℃ of the resin softening temperature and the sub-cooled liquid temperature scope at this metal glass powder molded.Magnetic density and the direct current of measure powder filling rate example, measuring by dc magnetic matter compare resistance.The gained result is table 3 illustrate.
Table 3
Sample number into spectrum | Resin content (%) | Molding temperature | Powder filling rate (%) | 1.6 * 10
4Magnetic flux density/T during A/m
| Than resistance Ω cm |
1 | 0.5 | Room temperature | 69.0 | 0.92 | ≥100 |
2 | 1 | ″ | 69.9 | 0.93 | ≥100 |
3 | 2.5 | ″ | 70.8 | 0.94 | ≥100 |
4 | 5 | ″ | 70.3 | 0.94 | ≥100 |
5 | 10 | ″ | 52.0 | 0.66 | ≥104 |
6 | 0.5 | 150℃ | 80.8 | 1.10 | 5 |
7 | 1 | ″ | 81.5 | 1.11 | 10 |
8 | 2.5 | ″ | 82.2 | 1.12 | 15 |
9 | 5 | ″ | 70.8 | 0.94 | ≥100 |
10 | 10 | ″ | 52.5 | 0.67 | ≥104 |
11 | 0.5 | 550℃ | 95.5 | 1.33 | 0.1 |
12 | 1 | ″ | 92.5 | 1.28 | 0.5 |
13 | 2.5 | ″ | 82.7 | 1.13 | 10 |
14 | 5 | ″ | 71.2 | 0.95 | ≥100 |
15 | 10 | ″ | 52.2 | 0.67 | ≥104 |
As seen from Table 3, when the content of adhesive surpasses 5%, compare with the ratio resistance of FERRITE CORE, it has up to 〉=10 than resistance
4Value.Even also do not obtain special-effect, be enough therefore in the room temperature mold pressing because molding temperature raises.Secondly, when the amount of adhesive equals 5%, obtain, and be enough in the room temperature mold pressing up to 1 Ω cm or higher ratio resistance.Secondly, can infer, when binder content equaled 2.5%, if carry out mold pressing at 150 ℃, then powder filling rate example was significantly improved, the magnetic density height, and obtain 0.1 Ω cm or higher ratio resistance.Secondly, can infer, when the content of adhesive was 1% and 0.5%, if carry out mold pressing at 550 ℃, then powder filling rate example was significantly improved, the saturation flux density height, and obtain 0.01 Ω cm or higher ratio resistance.
(embodiment 38)
In embodiment 38, has Fe by the water atomization preparation
73Si
7B
17Nb
2Zn
1The alloy powder of forming.Subsequently, the powder that obtains like this is divided into and has the 75 μ m or the powder of small grain size more.Then, carry out XRD determining to determine broad peak as the glassy phase feature.In addition, carry out DSC heat and analyze, thereby determine that vitrifying initial temperature range delta Tx is 35K with mensuration glass transition temperature and crystallization temperature.Then, this powder keeps also heat treatment 0.5 hour at atmospheric air and 450 ℃ of temperature conditions that are lower than glass transition temperature, to form oxide on powder surface.
Then, the silicones as adhesive of this powder and 10%, 5%, 2.5%, 1% and 0.5% mass ratio mixes.Has outer dia φ by use
Outward=27mm * inside diameter φ
InThe band groove die head of=14mm, these powder three kinds of condition of different temperatures promptly in room temperature, be higher than under 150 ℃ of the resin softening temperature and 550 ℃ of these three kinds of conditions, by using 11.8 * 10 in the sub-cooled liquid temperature scope of this soft magnetic metallic glass powder
8Pa pressure carries out molded, makes highly to equal 5mm.Like this, prepare various moldings.
Then, the molding that obtains like this carries out resin solidification.Subsequently, measure the weight and the size of each molding.Then, twine the coil of the suitable number of turns to prepare various inductance elements (having shape shown in Figure 2).
Then, for each different sample (numbering 1~15) of inductance element, measure powder filling rate example %, pass through the magnetic density of dc magnetic matter measurement (1.6 * 10
4A/m) and direct current than resistance Ω cm.The gained result is table 4 illustrate.
Table 4
Sample number into spectrum | Resin content (%) | Molding temperature | Powder filling rate (%) | 1.6 * 10
4Magnetic flux density/T during A/M
| Than resistance Ω cm |
1 | 0.5 | Room temperature | 68.9 | 0.83 | ≥100 |
2 | 1 | Room temperature | 69.7 | 0.84 | ≥100 |
3 | 2.5 | Room temperature | 70.5 | 0.85 | ≥100 |
4 | 5 | Room temperature | 70.1 | 0.84 | ≥100 |
5 | 10 | Room temperature | 51.5 | 0.56 | ≥104 |
6 | 0.5 | 150℃ | 80.7 | 1.02 | 5 |
7 | 1 | 150℃ | 81.3 | 1.03 | 10 |
8 | 2.5 | 150℃ | 81.9 | 1.04 | 15 |
9 | 5 | 150℃ | 70.6 | 0.85 | ≥100 |
10 | 10 | 150℃ | 52.0 | 0.58 | ≥10E
4 |
11 | 0.5 | 550℃ | 95.4 | 1.21 | 0.1 |
12 | 1 | 550℃ | 92.2 | 1.17 | 0.5 |
13 | 2.5 | 550℃ | 82.4 | 1.05 | 10 |
14 | 5 | 550℃ | 71.0 | 0.85 | ≥100 |
15 | 10 | 550℃ | 51.7 | 0.57 | ≥10
4 |
As shown in table 4, when the content (resin content) of adhesive surpasses 5%, to compare with the ratio resistance of FERRITE CORE, it has up to 〉=10 than resistance
4Value.Can infer, even molding temperature raises, can not obtain special effect, the molded condition about room temperature is enough.In addition, can infer, when resin content equals 5%, obtain up to 1 Ω cm or higher ratio resistance, and molded in room temperature be enough.In addition, can infer, when resin content equaled 2.5%, if carry out moldedly at 150 ℃, then powder filling rate example was significantly improved, the magnetic density height, and obtain 0.1 Ω cm or higher ratio resistance.In addition, can infer, when the content of adhesive was 1% and 0.5%, if carry out mold pressing at 550 ℃, then powder filling rate example was significantly improved, the saturation flux density height, and obtain 0.01 Ω cm or higher ratio resistance.
(embodiment 39)
Use sample number into spectrum 12 among the embodiment 37, with various core material comparative measurements inductive.In addition, the magnetic core by using the preparation of identical alloy powder and identical production technology blanket of nitrogen and 500 ℃ of heat treatment 0.5 hour to obtain another sample.The inductive nature of this sample also is illustrated.For making the inductance value standardization, the gained magnetic permeability is used for comparison.The core material that is compared is sendust (Sendust), 6.5% silicon steel and iron-based amorphous metal.
Table 5
The sample name | 1.6 * 10
4Magnetic flux density/T during A/M
| Than resistance Ω cm | Magnetic permeability | Core loss 20kHz 0.1T |
The present invention | 1.28 | 0.5 | 150 | 50/mW/cc |
The present invention's (heat treatment) | 1.29 | 0.4 | 200 | 30 |
The MnZn ferrite | 0.55 | ≥10
4 | 100
* | 10 |
Sendust | 0.65 | 100 | 80 | 100 |
6.5% silicon steel | 1.0 | 100μ | 100
* | 250 |
Fe-base amorphous metal | 1.3 | 150μ | 100
* | 400 |
Annotate)
*On the part magnetic circuit, embed gapped.
Find out that from last table 5 inductance element of the present invention has the magnetic density that equates with the inductance element magnetic density of using amorphous metal, and show than the low core loss character of inductance element core loss character of using sendust.Therefore inductance element of the present invention can be as very excellent inductance element.Confirm that in the inductance element that uses heat treated magnetic core, magnetic permeability and core loss further improve.
(embodiment 40)
In embodiment 40, by using the material preparation inductance element of sample number into spectrum 12 correspondences among the embodiment 38.In addition, by using identical alloy powder and identical production technology, and prepared another inductance element in 0.5 hour 500 ℃ of blanket of nitrogen heat treatments.In addition, be relatively, prepare inductance element (comprising the structure that on the part magnetic circuit, has the gap as shown in Figure 4) as core material by using sendust (Sendust), 6.5% silicon steel and iron-based amorphous metal respectively.For those inductance elements, measure the magnetic density of measuring by dc magnetic matter (1.6 * 10
4A/m), direct current than resistance Ω cm, be used for standardized magnetic permeability of inductance value and core loss (20kHz 0.1T).Result shown in the acquisition table 6.
Table 6
The sample name | 1.6 * 10
4Magnetic flux density/T during A/M
| Than resistance Ω cm | Magnetic permeability | Core loss 20kHz 0.1T |
The present invention | 1.21 | 0.5 | 160 | 50/mW/cc |
The present invention's (heat treatment) | 1.23 | 0.4 | 220 | 25 |
The MnZn ferrite | 0.55 | ≥104 | 100
* | 9 |
Sendust | 0.65 | 100 | 80 | 100 |
6.5% silicon steel | 1.0 | 100μ | 100
* | 250 |
Fe-base amorphous metal | 1.3 | 150μ | 100
* | 400 |
As seen from Table 6, inductance element of the present invention has the magnetic density that equates with the magnetic density of using Fe base amorphous metal as the inductance element of magnetic core, and shows than using sendust as the low core loss of the core loss of the inductance element of magnetic core.Therefore inductance element of the present invention has very excellent character.Confirm that in the inductance element that uses heat treated magnetic core, magnetic permeability and core loss further improve, and obtain more excellent performance.
(embodiment 41)
In embodiment 41, has Fe by the water atomization preparation
73Si
7B
17Nb
3The alloy powder of forming.The powder that obtains is divided into and has the 45 μ m or the powder of small grain size more subsequently.Then, carry out the XRD test to determine broad peak as the glassy phase feature.In addition, carry out DSC heat and analyze, thereby determine that sub-cooled liquid temperature range delta Tx is 35K with mensuration glass transition temperature and crystallization temperature.Then, obtain by water atomization and powder with following alloy composition is filtered into 20um or littler powder by the standard sieve.These powder are with the mixed shown in the table 7.
In addition, use the powder that obtains like this, mix with the silicones as adhesive of 1.5% quality than content.Has outer dia φ by use
Outward=27mm * inside diameter φ
InThe band groove die head of=14mm, these powder use 11.8 * 10 in room temperature
8Pa pressure carries out molded, so that highly equal 5mm.Like this, prepare different types of molding.After molded, in 500 ℃ Ar atmosphere, heat-treat.
Then, the various moldings that obtain like this carry out resin solidification.Subsequently, measure the weight and the size of each molding.Then, twine the coil of the suitable number of turns to prepare various inductance elements (having shape shown in Figure 2).
Then, for each different sample of inductance element, measure powder filling rate example %, magnetic permeability and core loss (20kHz 0.1T).Result shown in the acquisition table 7.
Table 7
Sample number into spectrum | Alloy composition | Add powder than (quality %) | Powder filling rate (volume %) | Magnetic permeability at 100kHz | Core loss 20kHz 0.1T |
Comparing embodiment | - | - | 71.5 | 35 | 25kW/m
3 |
The present invention | 1 | 3%SiFe | 5 | 72.1 | 37 | 30 |
2 | ″ | 10 | 72.7 | 39 | 40 |
3 | ″ | 20 | 73.3 | 40 | 60 |
4 | ″ | 30 | 74 | 41 | 70 |
5 | ″ | 40 | 74.5 | 42 | 80 |
6 | ″ | 50 | 75.0 | 44 | 90 |
7 | ″ | 60 | 75.2 | 44 | 200 |
8 | Sendust | 30 | 72.7 | 38 | 80 |
9 | The Mo permalloy | 30 | 75.0 | 43 | 85 |
10 | Pure iron powder | 30 | 76.5 | 48 | 95 |
As seen from Table 7, thereby inductance element of the present invention improves happy powder filling rate example by the littler soft magnetic powder of granularity is added in the metal glass powder, thereby has improved magnetic permeability.On the other hand,, then improve deleterious if institute's addition surpasses 50%, and the remarkable deterioration of core loss.Therefore, can infer, addition is preferably 50% or littler.
(embodiment 42)
In embodiment 42, has Fe by the water atomization preparation
73Si
7B
17Nb
3The alloy powder of forming.By changing various working conditions, prepare powder with length-width ratio shown in the table 8.The powder that obtains is divided into and has the 45 μ m or the powder of small grain size more subsequently.Then, carry out the XRD test to determine broad peak as the glassy phase feature.
In addition, carry out DSC heat and analyze, thereby determine that sub-cooled liquid temperature range delta Tx is 35K with mensuration glass transition temperature and crystallization temperature.
In addition, use the powder that obtains like this, mix with the silicones as adhesive of 3.0% quality than content.Has outer dia φ by use
Outward=27mm * inside diameter φ
InThe band groove die head of=14mm, these powder use 14.7 * 10 in room temperature
8Pa pressure carries out molded, so that highly equal 5mm.Like this, prepare different types of molding.After molded, in 500 ℃ Ar atmosphere, heat-treat.
Then, the various moldings that obtain like this carry out resin solidification.Subsequently, measure the weight and the size of each molding.Then, twine the coil of the suitable number of turns to prepare various inductance elements (having shape shown in Figure 2).
Then, for each different sample of inductance element, measure powder filling rate example % and magnetic permeability.Result shown in the acquisition table 8.
Table 8
Sample number into spectrum | Length-width ratio | Powder filling rate (volume %) | Magnetic permeability when 100KHz |
Comparing embodiment | 1.1 | 68 | 26 |
The present invention | 1 | 1.6 | 67 | 32 |
2 | 2.1 | 65 | 42 |
3 | 2.5 | 63 | 52 |
4 | 2.9 | 60 | 62 |
5 | 3.3 | 52 | 59 |
As shown in table 8, inductance element of the present invention improves magnetic permeability by the length-width ratio that increases the metal glass powder.On the other hand, if length-width ratio surpasses 3.0, then under the influence that the powder filling rate reduces, magnetic permeability reduces.Therefore, can infer, the length-width ratio of powder is preferably 3 or littler.
(embodiment 43)
At first, as the powder preparation step, weighing is usually used in the material of commercial Application, to obtain FeSi
9B
14Nb
3Composition.Use this material, by hydraulic atomized preparation median particle magnetically soft alloy micro powder inequality.
Secondly, as the molding preparation process, the alloy powder of Huo Deing filters to obtain the powder shown in the table 9 by the variety classes standard screen like this.Subsequently, the silicones as adhesive mixes with the amount of 3% mass ratio.Then, use the die head of 10mm * 10mm, with every kind of powder with have outer dia φ
Outward=8, inside diameter φ
InThe coil of=4mm and 2mm height carries out molded and arranges, so that the coil after molded is arranged in the accurate magnetic core of molding, by using 4.9 * 10 in room temperature
8The pressure of Pa is so that highly be 5mm.Like this, just formed molding.Then, carry out resin solidification at 150 ℃.As for sample number 5, also pass through the another kind of sample of this inductance element of heat treatment preparation in 0.5 hour in 500 ℃ blanket of nitrogen.
Then, for each different sample of inductance element, use the LCR meter to measure inductance and resistance at different frequency.Draw from mensuration, inductance value can obtain Q peak frequency and Q peak value when 1MHz.The result that obtains table 9 illustrate.
Then, for the same sample of inductance element, the evaluation kit that is used for typical DC/DC transducer is measured energy conversion efficiency.The gained result is as follows.Condition determination is 12V input, 5V output, 300kHz driving frequency and 1A output current.
Table 9
Sample number into spectrum | Mesh particle diameter μ m | Average diameter (D50) μ m | At the L of 1MHz (μ H) | Q peak frequency | The Q peak value | Energy conversion efficiency |
Comparing embodiment |
1 | 45 | 34 | 0.59 | 300kHz | 30 | 79.5% |
1 | | 29 | 0.62 | 600kHz | 42 | 83.0 |
2 | | 24 | 0.65 | 800kHz | 45 | 83.5 |
3 | | 19 | 0.68 | 1.5MHz | 60 | 85.0 |
4 | | 16 | 0.66 | 2.5MHz | 65 | 85.2 |
5 | | 11 | 0.64 | 3.5MHz | 75 | 85.5 |
5 (heat treatments) | | | 0.72 | 3.0MHz | 80 | 87.1 |
Comparing embodiment 2 | 63 | 28 | 0.67 | 400kHz | 35 | 79.8 |
As seen from Table 9, in inductance element of the present invention, when the mesh particle diameter is that 45 μ m or littler and average diameter are 30 μ m or more hour, Q peak frequency is 500kHz or bigger, and the Q peak value is 40 or bigger.Simultaneously, energy conversion efficiency is very excellent, is 80% or bigger.When the mesh particle diameter is that 45 μ m or littler and average diameter are 20 μ m or more hour, Q peak frequency is 1MHz or bigger, and the Q peak value is 50 or bigger.Simultaneously, energy conversion efficiency is very excellent, is 85% or bigger.In addition, can infer,, can further improve transformation efficiency by this inductance element of heat treatment.
As mentioned above, in high frequency magnetic core according to the present invention, selected to have the soft magnetic metallic glass powder of excellent economic benefit, thereby define following alloy composition: (Fe, Co, Ni)-(Al, Si, C, P)-(M is selected from least a among Zr, Nb, Ta, Hf, Mo, Ti, V, Cr and the W to B-MM ', and M ' is for being selected from least a among Zn, Sn and the R (wherein R is at least a element that is selected from the rare earth metal that comprises Y).This makes and can obtain to have excellent magnetic energy and glass formation performance.By this way, preparation powder core.Thereby, obtain the high magnetic permeability powder core that shows excellent magnetic permeability character and never know at wide frequency ranges.Therefore, can produce soft magnetic material high frequency magnetic core economically with high saturation magnetic flux metric density and high specific resistance.In addition, obtain to comprise high frequency magnetic core and at least one circle inductance element around the coil of this high frequency magnetic core, it is a kind of economic and high performance product that never obtained.Therefore, the present invention is very useful in commercial Application.
In the present invention, if use on granularity, have 45 μ m or littler maximum particle size and have 30 μ m or littler, better be the metal glass powder of 20 μ m or littler average diameter, the powder core that then obtains when high frequency, to have very low-loss character.Comprise that high frequency magnetic core and at least one circle have excellent Q performance around the inductance element of the coil of this high frequency magnetic core, so that can improve the energy efficiency of supply.Therefore, the present invention is very useful in commercial Application.
In addition, in the present invention, on granularity, have 45 μ m or littler maximum particle size and have 30 μ m or littler, better be 20 μ m or littler average diameter the metal glass powder be embedded in coil in the magnet and carry out compression molding to form complete structure.In this case, except that excellent magnetic core performance, passed the metal magnet by radiation from the heat that the electric current that flows through coil produces as the metal glass phase character.By thermal-radiating synergy, can obtain the inductance element that rated current increases for identical shaped.
High frequency magnetic core according to the present invention has the soft magnetic metallic glass material of high saturation magnetic flux metric density and high specific resistance by use and obtains economically.In addition, have inductance element that the magnetic core of coil obtains by equipment and have in my innocent life excellent magnetic energy at high frequency band.Therefore, can prepare the high magnetic permeability powder core of with low cost and excellent performance in my innocent life, and the inductance element as the energy feed element of various electronic installations can be provided, such as choking-winding and transformer.
Use the high frequency magnetic core that obtains by molded powder in the present invention, can prepare the high-performance inductance element on high frequency with small granularity.In addition, in the high frequency magnetic core that obtains by molded small granularity powder, the coil that is embedded in the magnet is carried out compression molding to form overall structure.Therefore, can preparation size little and be applicable to the inductance element of big electric current.