WO2023058478A1 - フェライト焼結体および積層コイル部品 - Google Patents

フェライト焼結体および積層コイル部品 Download PDF

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WO2023058478A1
WO2023058478A1 PCT/JP2022/035598 JP2022035598W WO2023058478A1 WO 2023058478 A1 WO2023058478 A1 WO 2023058478A1 JP 2022035598 W JP2022035598 W JP 2022035598W WO 2023058478 A1 WO2023058478 A1 WO 2023058478A1
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French (fr)
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一星 杉井
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Murata Manufacturing Co Ltd
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Murata Manufacturing Co Ltd
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Priority to CN202280052579.9A priority Critical patent/CN117716454A/zh
Priority to JP2023552801A priority patent/JP7537625B2/ja
Publication of WO2023058478A1 publication Critical patent/WO2023058478A1/ja
Priority to US18/426,915 priority patent/US20240212894A1/en
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Definitions

  • the present invention relates to ferrite sintered bodies and laminated coil components.
  • Patent Document 1 discloses a composite magnetic material containing a ferrite composition and zinc silicate, wherein the ferrite composition is composed of spinel ferrite and bismuth oxide present in the spinel ferrite.
  • the ratio of the weight of the bismuth oxide to the weight of the entire material is 0.025% by weight or more and 0.231% by weight or less, and the ratio of the weight of the zinc silicate to the sum of the weight of the zinc silicate and the weight of the spinel ferrite.
  • Patent Document 1 when the ratio of the weight of bismuth oxide to the weight of the entire composite magnetic material is 0.025% by weight or more and 0.231% by weight or less, the sinterability of the composite magnetic material is improved, and It is said that a high specific resistance can be secured. Furthermore, when the ratio of the weight of zinc silicate to the sum of the weight of zinc silicate and the weight of spinel ferrite is 8% by weight or more and 76% by weight or less, both high magnetic permeability and good DC superimposition characteristics can be achieved. It is
  • the present invention was made to solve the above problems, and aims to provide a ferrite sintered body that has good DC superimposition characteristics and sinterability, and that suppresses plating elongation.
  • a further object of the present invention is to provide a laminated coil component having an insulating layer made of the ferrite sintered body.
  • the ferrite sintered body of the present invention contains main components and subcomponents.
  • the above main components are 4 mol % or more and 13 mol % or less of Fe converted to Fe 2 O 3 , 47 mol % or more and 58 mol % or less of Zn converted to ZnO, and 1 mol % or more and 4 mol % of Cu converted to CuO. % or less, 2 mol % or more and 8 mol % or less of Ni in terms of NiO, and 28 mol % or more and 36 mol % or less of Si in terms of SiO 2 .
  • the secondary component is 0.8 parts by weight or more and 3 parts by weight or less in terms of Bi 2 O 3 and 0.005 parts by weight or more in terms of ZrO 2 with respect to 100 parts by weight of the main component. , 0.1 parts by weight or less.
  • the laminated coil component of the present invention includes a laminated body in which insulating layers made of the ferrite sintered body of the present invention and coil conductors are alternately laminated.
  • ferrite sintered body that has good DC superposition characteristics and sinterability, and that suppresses plating elongation. Furthermore, according to the present invention, it is possible to provide a laminated coil component having an insulating layer composed of the ferrite sintered body.
  • FIG. 1 is a perspective view schematically showing an example of the laminated coil component of the present invention.
  • FIG. 2 is an exploded plan view schematically showing an example of the internal structure of a laminate that constitutes the laminated coil component shown in FIG. 3 is a cross-sectional view schematically showing an example of a laminated coil component including the laminate shown in FIG. 2.
  • FIG. 4 is an enlarged view of the portion indicated by IV in FIG.
  • the ferrite sintered body and laminated coil component of the present invention will be described below.
  • the present invention is not limited to the following configurations, and can be appropriately modified and applied without changing the gist of the present invention. It should be noted that a combination of two or more of the individual preferred configurations of the invention described below is also the invention.
  • the ferrite sintered body of the present invention contains main components and subcomponents.
  • the main component is 4 mol% or more and 13 mol% or less of Fe converted to Fe 2 O 3 , 47 mol% or more and 58 mol% or less of Zn converted to ZnO, and 1 mol% or more to 4 mol% of Cu converted to CuO.
  • Ni is contained in an amount of 2 mol % or more and 8 mol % or less in terms of NiO
  • Si is contained in an amount of 28 mol % or more and 36 mol % or less in terms of SiO 2 .
  • the sum of Fe 2 O 3 , ZnO, CuO, NiO and SiO 2 is 100 mol %.
  • the subcomponents are 0.8 parts by weight or more and 3 parts by weight or less in terms of Bi2O3 , 0.005 parts by weight or more in terms of Zr in terms of ZrO2 , and 0 .1 part by weight or less.
  • an applied magnetic field of -10% from the initial magnetic permeability is 15,000 A/m or more, sufficiently sintered even at 920 ° C. for 3 hours, and plating elongation is suppressed. be able to.
  • the content of each element can be determined by analyzing the composition of the sintered body using inductively coupled plasma emission/mass spectroscopy (ICP-AES/MS).
  • ICP-AES/MS inductively coupled plasma emission/mass spectroscopy
  • the main components are 4 mol% or more and 9 mol% or less of Fe converted to Fe 2 O 3 , 52 mol% or more and 58 mol% or less of Zn converted to ZnO, and Cu to CuO. It is preferable to contain 1 mol % or more and 3 mol % or less in conversion, 2 mol % or more and 5 mol % or less of Ni in terms of NiO, and 31 mol % or more and 36 mol % or less of Si in terms of SiO 2 . However, the sum of Fe 2 O 3 , ZnO, CuO, NiO and SiO 2 is 100 mol %.
  • the DC bias characteristics can be further enhanced.
  • a ceramic composition having an applied magnetic field of 18000 A/m or more, which reduces the initial magnetic permeability by -10%.
  • the subcomponents further include 0.003 parts by weight or more and 0.1 parts by weight or less in terms of Mn 2 O 3 and Cr with respect to 100 parts by weight of the main component. It may be contained in an amount of 0.003 parts by weight or more and 0.1 parts by weight or less in terms of 2O3 .
  • the DC superimposition characteristics can be further enhanced.
  • the ferrite sintered body of the present invention preferably has an average crystal grain size of 0.2 ⁇ m or more and 0.8 ⁇ m or less.
  • the average crystal grain size of the ferrite sintered body means the area equivalent circle diameter (D50) at which the cumulative distribution of the area equivalent circle diameters of the crystal grains is 50% on a number basis.
  • the area equivalent circle diameter of crystal grains can be measured by observing the cross section of the ferrite sintered body using a scanning electron microscope (SEM).
  • the ferrite sintered body of the present invention preferably contains a magnetic phase containing at least Fe, Ni, Zn and Cu, and a non-magnetic phase containing at least Si and Zn.
  • the ferrite sintered body contains a non-magnetic phase, magnetic saturation is easily suppressed as described above, so the DC superimposition characteristics can be improved.
  • the magnetic phase and non-magnetic phase are distinguished as follows. First, the section of the ferrite sintered body is subjected to elemental mapping by scanning transmission electron microscope-energy dispersive X-ray analysis (STEM-EDX). The two phases can be distinguished from each other by defining a region in which Fe exists as a magnetic phase and a region in which Si exists as a non-magnetic phase.
  • STEM-EDX scanning transmission electron microscope-energy dispersive X-ray analysis
  • a laminated coil component of the present invention includes a laminated body in which insulating layers made of the ferrite sintered body of the present invention and coil conductors are alternately laminated.
  • FIG. 1 is a perspective view schematically showing an example of the laminated coil component of the present invention.
  • Laminated coil component 1 further includes external electrodes 21 and 22 provided on the outer surface of laminate 10 .
  • the number of external electrodes, the positions at which the external electrodes are provided, and the like are appropriately changed.
  • the laminate 10 has, for example, a rectangular parallelepiped shape or a substantially rectangular parallelepiped shape.
  • FIG. 1 shows a length direction L, a width direction W and a height direction T. As shown in FIG. The length direction L, width direction W, and height direction T are orthogonal to each other.
  • FIG. 2 is an exploded plan view schematically showing an example of the internal structure of the laminate that constitutes the laminated coil component shown in FIG. 3 is a cross-sectional view schematically showing an example of a laminated coil component including the laminate shown in FIG. 2.
  • FIG. 3 corresponds to a cross-sectional view along line III-III of the laminated coil component shown in FIG.
  • the laminate 10 includes insulating layers 11a, 11b, 11c, 11d, 11e, 11f, 11g and 11h, and coil conductors 12a, 12b, 12c, 12d, 12e, 12f and 12g. are stacked alternately.
  • a coil is formed by electrically connecting coil conductors 12a, 12b, 12c, 12d, 12e, 12f, and 12g through via conductors 13a, 13b, 13c, 13d, 13e, and 13f.
  • the laminated coil component 1 has a vertical winding structure in which the coil conductors are laminated in the height direction T, but a horizontal winding structure in which the coil conductors are laminated in the length direction L or the width direction W. It may have a wound structure.
  • Each of the insulating layers 11a, 11b, 11c, 11d, 11e, 11f, 11g and 11h is composed of the ferrite sintered body of the present invention.
  • the coil conductors 12a, 12b, 12c, 12d, 12e, 12f and 12g are each made of Ag or the like.
  • via conductors 13a, 13b, 13c, 13d, 13e and 13f are each made of Ag or the like.
  • the external electrode 21 includes, in order from the laminate 10 side, a base electrode 21a and a plated electrode 21b provided on the base electrode 21a.
  • the external electrode 22 includes, in order from the laminate 10 side, a base electrode 22a and a plated electrode 22b provided on the base electrode 22a.
  • the base electrodes 21a and 22a each preferably contain Ag.
  • the plating electrodes 21b and 22b may each have a single-layer structure or a multi-layer structure.
  • the plating electrode 21b has a multilayer structure, it is preferable that the plating electrode 21b includes a Ni plating electrode and a Sn plating electrode in this order from the base electrode 21a side.
  • the plating electrode 22b has a multi-layer structure, the plating electrode 22b preferably includes a Ni-plating electrode and a Sn-plating electrode in order from the base electrode 22a side.
  • FIG. 4 is an enlarged view of the portion indicated by IV in FIG.
  • the length of the plating electrode 21b extending from the tip of the base electrode 21a is preferably 30 ⁇ m or less.
  • the length of the plating electrode 21b extending from the tip of the base electrode 21a may be 0 ⁇ m or greater than 0 ⁇ m.
  • the length of the plating electrode 22b extending from the tip of the base electrode 22a is preferably 30 ⁇ m or less.
  • the length of the plating electrode 22b extending from the tip of the underlying electrode 22a may be 0 ⁇ m or greater than 0 ⁇ m.
  • a laminated coil component having an insulating layer composed of the ferrite sintered body of the present invention is preferably manufactured as follows.
  • ⁇ Magnetic material manufacturing process Fe 2 O 3 , ZnO, CuO and NiO are weighed to give a given composition.
  • This compounding raw material is placed in a ball mill together with pure water and PSZ (partially stabilized zirconia) balls, and wet-mixed and pulverized for a predetermined time (for example, 4 hours or more and 8 hours or less). After drying by evaporating water, it is calcined at a predetermined temperature (eg, 700° C. or higher and 800° C. or lower) for a predetermined time (eg, 2 hours or longer and 5 hours or shorter).
  • a magnetic material specifically Ni--Cu--Zn ferrite powder is produced.
  • the magnetic material that is calcined is preferably pulverized again so that the average particle diameter D50 is about 0.1 ⁇ m or more and 0.2 ⁇ m or less.
  • the Ni—Cu—Zn ferrite powder obtained after calcination has a Fe content of 40 mol% or more and 49.5 mol% or less in terms of Fe 2 O 3 , a Zn content of 2 mol% or more and 35 mol% or less in terms of ZnO, and Cu in terms of CuO. is preferably 6 mol % or more and 13 mol % or less, and Ni is preferably contained in an amount of 10 mol % or more and 45 mol % or less in terms of NiO.
  • the Ni--Cu--Zn ferrite powder may contain additives such as Co, Bi, Sn and Mn, inevitable impurities and the like.
  • Nonmagnetic material manufacturing process SiO 2 and ZnO are weighed to the given composition. At that time, it is preferable to blend so that the molar ratio of ZnO to SiO 2 is 1.8 or more and 2.2 or less.
  • This compounding raw material is placed in a ball mill together with pure water and PSZ balls, and wet-mixed and pulverized for a predetermined time (for example, 4 hours or more and 8 hours or less). After the moisture is evaporated and dried, the material is calcined at a predetermined temperature (eg, 1000° C. or higher and 1300° C. or lower) for a predetermined time (eg, 2 hours or longer and 5 hours or shorter). Thereby, a non-magnetic material, specifically zinc silicate powder, is produced.
  • a predetermined temperature eg, 1000° C. or higher and 1300° C. or lower
  • the non-magnetic material that is calcined is preferably pulverized again so that the average particle size D50 is about 0.1 ⁇ m or more and 0.2 ⁇ m or less.
  • SiO 2 powder having an average particle size D50 of about 0.1 ⁇ m or more and 0.2 ⁇ m or less is prepared as a non-magnetic material.
  • the average particle diameter D50 of the magnetic material and the non-magnetic material described above is the volume equivalent diameter of 50% obtained using a laser diffraction scattering particle size distribution measurement method.
  • Green sheet manufacturing process The magnetic material and non-magnetic material produced in the above steps are blended in a predetermined ratio. In addition, certain amounts of Bi 2 O 3 and ZrO 2 are added. Predetermined amounts of Mn 2 O 3 and Cr 2 O 3 are added as required. These formulations are placed in a ball mill together with PSZ media, and an organic binder such as polyvinyl butyral resin, an organic solvent such as ethanol or toluene, a plasticizer, etc. are added and mixed to prepare a slurry. . The obtained slurry is formed into a sheet having a predetermined thickness (for example, 20 ⁇ m or more and 30 ⁇ m or less) by a doctor blade method or the like. After that, a green sheet is produced by punching into a predetermined shape (for example, a rectangular shape).
  • a predetermined thickness for example, 20 ⁇ m or more and 30 ⁇ m or less
  • a via hole is formed at a predetermined location by irradiating the produced green sheet with a laser beam.
  • a conductive paste containing Ag or the like as a main component is filled in the via holes and coated on the surface of the green sheet by a screen printing method or the like.
  • a coil conductor pattern is formed on the green sheet.
  • Green sheets with coil conductor patterns and green sheets without coil conductor patterns are laminated in a predetermined order (for example, the order shown in FIG. 2).
  • a laminate block is produced by thermocompression bonding the laminated green sheets.
  • ⁇ Singulation process> If necessary, individualized chips are produced by cutting the laminate block into a predetermined size with a dicer or the like.
  • the singulated chips are fired at a predetermined temperature (eg, 900° C. or higher and 920° C. or lower) for a predetermined time (eg, 2 hours or longer and 4 hours or shorter).
  • a predetermined temperature eg, 900° C. or higher and 920° C. or lower
  • a predetermined time eg, 2 hours or longer and 4 hours or shorter.
  • the green sheet becomes an insulating layer composed of a ferrite sintered body, and the coil conductor pattern becomes a coil conductor or a via conductor.
  • the coil conductor pattern becomes a coil conductor or a via conductor.
  • the laminated body may be subjected to, for example, barrel polishing to round the corners and ridges of the laminated body.
  • a corner is a portion where three surfaces of the laminate intersect, and a ridge is a portion where two surfaces of the laminate intersect.
  • a conductive paste is applied to the end faces of the laminate from which the coil conductors are drawn out.
  • Conductive pastes include, for example, Ag and glass.
  • a predetermined temperature for example, 800° C. or higher and 820° C. or lower
  • the thickness of the underlying electrode is, for example, about 5 ⁇ m.
  • a Ni-plated electrode and a Sn-plated electrode are sequentially formed on the base electrode by electrolytic plating or the like.
  • the external electrodes are formed.
  • the size of the laminated coil component is 0.6 mm in the length direction L, 0.3 mm in the width direction W, and 0.3 mm in the height direction T, for example.
  • Example 1 (Preparation of sample) 48 mol % of Fe 2 O 3 , 10 mol % of ZnO, 28 mol % of NiO and 14 mol % of CuO were blended. This formulation was wet-mixed and pulverized, and then dried to remove moisture. The obtained dried product was calcined at a temperature of 800° C. for 2 hours. The obtained calcined material was wet pulverized until the average particle diameter D50 reached 0.2 ⁇ m. Thus, a ferrite powder was produced as a magnetic material.
  • ZnO and SiO 2 were blended at a ZnO:SiO 2 molar ratio of 2:1. This formulation was wet-mixed and pulverized, and then dried to remove moisture. The obtained dried product was calcined at a temperature of 1100° C. for 2 hours. The obtained calcined material was wet pulverized until the average particle diameter D50 reached 0.2 ⁇ m. Thus, a zinc silicate powder was produced. In addition, SiO 2 powder with an average particle size D50 of 0.2 ⁇ m was prepared. These zinc silicate powders and SiO2 powders were taken as non-magnetic materials.
  • a slurry was prepared by mixing predetermined amounts of an organic binder, an organic solvent and a plasticizer in a ball mill. The resulting slurry was formed into a sheet having a thickness of about 25 ⁇ m by a doctor blade method, and then punched into a rectangular shape to produce a green sheet.
  • a laminate block was produced by stacking and crimping a plurality of the produced green sheets.
  • a ring-shaped sample having an outer diameter of 20 mm, an inner diameter of 12 mm, and a thickness of 1.5 mm was produced by punching out the laminate block into a ring shape and firing at 920° C. for 3 hours.
  • a laminated coil component was produced according to the procedure described in ⁇ Coil Conductor Pattern Forming Process> to ⁇ External Electrode Forming Process>.
  • composition The ring-shaped samples were analyzed for composition using inductively coupled plasma emission/mass spectroscopy (ICP-AES/MS). Table 1 shows the results.
  • the average crystal grain size D50 is the area equivalent circle diameter at which the cumulative distribution of the measured area equivalent circle diameters of the crystal grains is 50% on a number basis. Table 1 shows the results.
  • the main component is 4 mol% or more and 13 mol% or less in terms of Fe as Fe 2 O 3 , 47 mol% or more and 58 mol% or less in terms of ZnO, and 1 mol% or more in terms of CuO. , 4 mol% or less, 2 mol% or more and 8 mol% or less of Ni in terms of NiO, 28 mol% or more and 36 mol% or less of Si in terms of SiO 2 , and the subcomponent is Bi per 100 parts by weight of the main component. 0.8 parts by weight or more and 3 parts by weight or less in terms of Bi 2 O 3 , and Zr in terms of ZrO 2 0.005 parts by weight or more and 0.1 parts by weight or less.
  • the magnetic permeability ⁇ ' is 1.2 or more
  • the DC superimposition characteristic is 15000 A/m or more
  • the sintering is sufficient even at 920 ° C. for 3 hours, and the plating elongation is suppressed.
  • a ferrite sintered body is obtained.
  • the main component is 4 mol% or more and 9 mol% or less of Fe converted to Fe 2 O 3 , 52 mol% or more and 58 mol% or less of Zn converted to ZnO, and 1 mol% or more to 3 mol% of Cu converted to CuO. % or less, 2 mol % or more and 5 mol % or less of Ni in terms of NiO, and 31 mol % or more and 36 mol % or less of Si in terms of SiO 2 .
  • a ferrite sintered body having a superposition characteristic of 18000 A/m or more is obtained.
  • Samples 7, 8 and 19 had poor sinterability, and were not sufficiently sintered after firing at 920°C for 3 hours.
  • Samples 21 to 27 were prepared by adding Mn and Cr to the composition of Sample 5 in Table 1, and the same evaluation as in Example 1 was performed. Table 2 shows the results.
  • the secondary component is 0.003 parts by weight or more and 0.1 parts by weight or less in terms of Mn 2 O 3 , and 0 parts by weight in terms of Cr 2 O 3 .
  • DC superimposition characteristics equal to or higher than that of Sample 5 are obtained.

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0851012A (ja) * 1994-08-05 1996-02-20 Hitachi Ferrite Ltd 酸化物磁性材料
JP2004296865A (ja) * 2003-03-27 2004-10-21 Taiyo Yuden Co Ltd 巻き線チップインダクタ用フェライトコアとその製造方法及び巻き線チップインダクタ
JP2010103266A (ja) * 2008-10-22 2010-05-06 Toda Kogyo Corp Ｎｉ−Ｚｎ−Ｃｕ系フェライト焼結体からなるインダクタンス素子
JP2016196397A (ja) * 2015-04-02 2016-11-24 Tdk株式会社 フェライト組成物および電子部品
JP2020121916A (ja) * 2019-01-29 2020-08-13 Tdk株式会社 フェライト組成物および積層電子部品
JP2020123616A (ja) * 2019-01-29 2020-08-13 Tdk株式会社 フェライト組成物および積層電子部品

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0851012A (ja) * 1994-08-05 1996-02-20 Hitachi Ferrite Ltd 酸化物磁性材料
JP2004296865A (ja) * 2003-03-27 2004-10-21 Taiyo Yuden Co Ltd 巻き線チップインダクタ用フェライトコアとその製造方法及び巻き線チップインダクタ
JP2010103266A (ja) * 2008-10-22 2010-05-06 Toda Kogyo Corp Ｎｉ−Ｚｎ−Ｃｕ系フェライト焼結体からなるインダクタンス素子
JP2016196397A (ja) * 2015-04-02 2016-11-24 Tdk株式会社 フェライト組成物および電子部品
JP2020121916A (ja) * 2019-01-29 2020-08-13 Tdk株式会社 フェライト組成物および積層電子部品
JP2020123616A (ja) * 2019-01-29 2020-08-13 Tdk株式会社 フェライト組成物および積層電子部品

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