WO2011093489A1 - 電子部品の製造方法 - Google Patents
電子部品の製造方法 Download PDFInfo
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- WO2011093489A1 WO2011093489A1 PCT/JP2011/051889 JP2011051889W WO2011093489A1 WO 2011093489 A1 WO2011093489 A1 WO 2011093489A1 JP 2011051889 W JP2011051889 W JP 2011051889W WO 2011093489 A1 WO2011093489 A1 WO 2011093489A1
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- Prior art keywords
- oxygen
- magnetic
- heat treatment
- firing
- temperature
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 73
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000001301 oxygen Substances 0.000 claims abstract description 72
- 239000004020 conductor Substances 0.000 claims abstract description 55
- 239000012298 atmosphere Substances 0.000 claims abstract description 54
- 238000010304 firing Methods 0.000 claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 claims description 22
- 238000005498 polishing Methods 0.000 claims description 11
- 239000000696 magnetic material Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 abstract 1
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 30
- 229910000859 α-Fe Inorganic materials 0.000 description 19
- 239000000919 ceramic Substances 0.000 description 14
- 238000007747 plating Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000002788 crimping Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000002966 varnish Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- QELJHCBNGDEXLD-UHFFFAOYSA-N nickel zinc Chemical compound [Ni].[Zn] QELJHCBNGDEXLD-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
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- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
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- H01F17/0006—Printed inductances
- H01F17/0013—Printed inductances with stacked layers
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- H01F27/28—Coils; Windings; Conductive connections
- H01F27/29—Terminals; Tapping arrangements for signal inductances
- H01F27/292—Surface mounted devices
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
- C04B2235/6584—Oxygen containing atmosphere, e.g. with changing oxygen pressures at an oxygen percentage below that of air
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- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T29/4902—Electromagnet, transformer or inductor
- Y10T29/49075—Electromagnet, transformer or inductor including permanent magnet or core
Definitions
- the present invention relates to a method of manufacturing an electronic component, and more particularly, to a method of manufacturing an electronic component including a magnetic body portion and an internal conductor portion disposed in the magnetic body portion.
- ferrite element As an electronic component (ferrite element) including a magnetic body portion (ferrite) and an inner conductor portion disposed in the magnetic body portion, 0.3 part by weight of PbO component with respect to 100 parts by weight of nickel-zinc based ferrite
- a ferrite element formed by arranging an internal conductor (copper conductor) inside a magnetic body (ferrite base) added at a ratio of 5.0 parts by weight or less and integrally firing (patent) See claim 1 of Document 1).
- the PbO component is 0.3 parts by weight or more and 5.0 parts by weight or less
- the B 2 O 3 component is 0.03 parts by weight or more and 1.5 parts by weight or less
- the SiO 2 component is 0.03 parts by weight or more and 1.5 parts by weight or less.
- a low melting point component such as PbO, B 2 O 3 , or SiO 2 is added in order to lower the firing temperature of the ferrite matrix, and Cu constituting the internal conductor in a nitrogen atmosphere. Firing is carried out at a temperature of 950 to 1030 ° C., which is lower than the melting point.
- Patent Document 1 an ferrite matrix (ferrite porcelain) and an internal conductor (Cu) are simultaneously fired in a nitrogen atmosphere, but an Ellingham diagram (not shown) showing the equilibrium oxygen partial pressure of the oxide.
- Cu and Fe 2 O 3 coexist at a high temperature of 800 ° C. or higher. It is known that the region does not exist. That is, at a temperature of 800 ° C. or higher, when firing is performed with an oxygen partial pressure set in an oxidizing atmosphere that maintains the state of Fe 2 O 3 , Cu is also oxidized to produce Cu 2 O.
- Fe 2 O 3 is reduced to produce Fe 3 O 4 .
- the ferrite matrix (ferrite porcelain) and the inner conductor (Cu) when simultaneously firing the ferrite matrix (ferrite porcelain) and the inner conductor (Cu), if the firing is performed under an oxygen partial pressure such that the ferrite is not reduced, the Cu constituting the inner conductor is oxidized and functions as an inner conductor. If it is fired under conditions that maintain the metal state without oxidation of Cu, there is a risk that the ferrite will be reduced and the function as a magnetic material may not be fulfilled sufficiently.
- Patent Document 1 Although ferrite and Cu are simultaneously fired in a nitrogen atmosphere, since there is no region where Cu and Fe 2 O 3 coexist, firing is performed in a reducing atmosphere in which Cu is not oxidized. Then, since the ferrite is reduced, there is a problem that the specific resistance ⁇ is lowered. For this reason, there is a possibility that high characteristics and reliability required for the electronic component cannot be realized.
- the present invention solves the above problems, and suppresses and prevents the oxidation of Cu constituting the internal conductor portion in the firing step, and includes a magnetic material containing NiO, ZnO, Fe 2 O 3 and the like in the firing step. Even when reduction occurs in the part (for example, reduction of Fe 2 O 3 to Fe 3 O 4 , etc.), the magnetic part is subsequently oxidized to ensure the original characteristics, thereby providing good characteristics.
- Another object of the present invention is to provide an electronic component manufacturing method that can efficiently manufacture highly reliable electronic components.
- a method for manufacturing an electronic component of the present invention includes: A magnetic part containing at least NiO, ZnO, and Fe 2 O 3 ; and an internal conductor mainly composed of Cu, which is disposed in the magnetic part and partly drawn to the surface of the magnetic part.
- a method for manufacturing an electronic component comprising: An unfired laminated body in which an unfired internal conductor material that becomes the internal conductor portion after firing is disposed in an unfired magnetic material that becomes the magnetic body portion after firing, is obtained as an equilibrium oxygen partial pressure of Cu—Cu 2 O.
- the oxygen-containing atmosphere heat treatment step is characterized in that the temperature drop in the temperature lowering process is stopped at a predetermined temperature and held for a predetermined time.
- the heat treatment temperature in the oxygen-containing atmosphere heat treatment step is preferably 900 ° C. or lower.
- the surface of the inner conductor portion drawn to the surface of the magnetic body portion is polished by polishing the surface of the fired laminated body obtained through the oxygen-containing atmosphere heat treatment step.
- An oxide film removing step for removing the oxide film is further provided.
- the method for producing an electronic component of the present invention comprises a non-fired laminated body in which an unfired internal conductor material that becomes an internal conductor part after firing is disposed in an unfired magnetic material that becomes a magnetic part after firing.
- a firing step of firing in an oxygen concentration atmosphere below the equilibrium oxygen partial pressure of Cu 2 O, and a fired laminated body fired in the firing step in an atmosphere having an oxygen concentration of 0.01% or more in the subsequent temperature lowering process And heat treatment in an oxygen-containing atmosphere heat treatment step, so that it is possible to perform the firing while preventing the Cu constituting the internal conductor portion from being oxidized in the firing step, and the magnetic body in the firing step.
- the firing step as "Cu-Cu 2 O oxygen concentration atmosphere under equilibrium oxygen partial pressure of the" in (main baking step), the equilibrium oxygen concentration in the Cu-Cu 2 O, Cu- Cu 2 O It is desirable to apply an oxygen concentration condition in the range of 1/100 (10 ⁇ 2 times) the equilibrium oxygen concentration.
- the reduced magnetic part is reliably oxidized.
- the magnetic body the original characteristics (for example, to increase the value of the reduced specific resistance reduced to a desired value).
- the heat treatment temperature in the oxygen-containing atmosphere heat treatment step is set to a temperature of 900 ° C. or lower, thereby suppressing the oxidation of Cu constituting the internal conductor portion, and the magnetic body. It is possible to oxidize the part, and the present invention can be further improved.
- the effect of heat treatment in an oxygen-containing atmosphere is affected by the oxygen concentration in the heat treatment atmosphere, the time for performing the heat treatment, and the like.
- the heat treatment temperature in the oxygen-containing atmosphere heat treatment step depends on the oxygen concentration in the atmosphere and the heat treatment. It is desirable to set it in consideration of time.
- the inner conductor It is possible to reliably connect the portion and the external electrode, and it is preferable because a more reliable electronic component can be reliably manufactured.
- laminated coil components as shown in FIGS. 2 and 3 were produced by the method according to the example of the present invention.
- the laminated coil component 1 is provided on both ends of a laminated body (magnetic body portion) 11 a that includes a spiral coil L in which an internal conductor portion 5 a is interlayer-connected.
- the coil L has a structure including a pair of external electrodes 21 and 22 arranged to be electrically connected to both end portions L1 and L2 of the coil L.
- the electronic component to which the present invention can be applied is not limited to the laminated coil component as shown in FIGS. 2 and 3, and the present invention can be applied to various types including an internal conductor portion and a magnetic body portion.
- the present invention can be widely applied to the manufacture of electronic parts. Hereinafter, the manufacturing method will be described.
- this blended magnetic material was wet-mixed for 20 hours with a ball mill using zirconia-based media (zirconia balls) as pulverization / mixing media to obtain a slurry.
- This slurry was dried with a dryer and calcined at 750 ° C. for 2 hours to obtain a calcined product.
- This calcined product was wet pulverized with a ball mill for 20 hours, and after completion of the pulverization, a predetermined amount of a binder was added and mixed to obtain a ceramic slurry.
- the ceramic slurry thus obtained was formed into a sheet shape by a doctor blade method to obtain, for example, a ceramic green sheet (magnetic ceramic green sheet) having a thickness of 25 ⁇ m.
- a Cu paste (unfired internal conductor material) made of Cu powder, varnish, and solvent is magnetically bonded. Screen printing was performed on the surface of the body ceramic green sheet to form a predetermined coil conductor pattern (unfired inner conductor material) and an interlayer connection via-hole conductor.
- the magnetic ceramic green sheet for the exterior part for forming the exterior part is formed without forming a coil conductor pattern or an interlayer connection via-hole conductor. Used as is.
- FIG. 1 is an exploded perspective view of one green laminate 11 obtained by cutting. In this embodiment, the number of turns of the coil L is 9.5 turns.
- the oxygen partial pressure is controlled by adjusting the mixing ratio of the mixed gas of N 2 —H 2 —H 2 O to control the oxygen partial pressure derived from oxygen generated by the decomposition of H 2 O. Firing was carried out at a Cu—Cu 2 O equilibrium oxygen partial pressure (6.6 ⁇ 10 ⁇ 2 Pa at 1000 ° C.) or less. Specifically, firing was performed with an oxygen partial pressure in the range of 6.6 ⁇ 10 ⁇ 2 Pa to 6.6 ⁇ 10 ⁇ 3 Pa.
- both end portions of the coil L formed by connecting the coil conductors (inner conductor portions) 5a, which are disposed inside the fired laminated body 11a, are connected to each other.
- a laminated coil component 1 having a pair of conducting external electrodes 21 and 22 (see FIG. 2) was produced.
- the sample under the condition 1 in Table 1 prepared without passing through a heat treatment in an oxygen-containing atmosphere (oxygen-containing atmosphere heat treatment) in the temperature lowering process after the holding at the top temperature was completed (
- oxygen-containing atmosphere heat treatment oxygen-containing atmosphere heat treatment
- the impedance value was low, and the maximum value was about 300 ⁇ in the vicinity of 70 MHz. This is because Fe 2 O 3 constituting the magnetic part is reduced to Fe 3 O 4 in the firing step, and the characteristics are deteriorated.
- the obtained impedance value is shown in FIG. As shown, it was confirmed that the maximum value was as high as about 590 ⁇ at 100 to 200 MHz.
- the present invention is not limited to the above-described embodiment, and specific conditions of the oxygen-containing atmosphere in the oxygen-containing atmosphere heat treatment step performed in the temperature lowering process after the holding at the top temperature is completed, Various applications and modifications can be made within the scope of the invention with respect to the starting temperature, the holding temperature and the holding time when holding at a constant temperature.
- the surface of the laminate (baked laminate) obtained through the oxygen-containing atmosphere heat treatment step is polished to remove the oxide film on the end surface of the coil drawn out to the surface of the laminate.
- a barrel polishing method is used as the method, there are no particular restrictions on the specific method and conditions of barrel polishing. It is also possible to use a known method such as sand blasting other than barrel polishing.
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Abstract
Description
少なくともNiO、ZnO、Fe2O3を含む磁性体部と、前記磁性体部内に配設され、一部が前記磁性体部の表面に引き出された、Cuを主成分とする内部導体部とを具備する電子部品の製造方法であって、
焼成後に前記磁性体部となる未焼成磁性体材料中に、焼成後に前記内部導体部となる未焼成内部導体材料が配設された未焼成積層体を、Cu-Cu2Oの平衡酸素分圧以下の酸素濃度雰囲気中で焼成する焼成工程と、
前記焼成工程で焼成された焼成済積層体を、その後の降温過程で、酸素濃度が0.01%以上の雰囲気中で熱処理する含酸素雰囲気熱処理工程と
を有することを特徴としている。
その結果、特性が良好で信頼性の高い電子部品を効率よく製造することが可能になる。
なお、本発明においては、焼成工程(本焼成工程)における「Cu-Cu2Oの平衡酸素分圧以下の酸素濃度雰囲気」として、Cu-Cu2Oの平衡酸素濃度から、Cu-Cu2Oの平衡酸素濃度の1/100(10-2倍)の範囲の酸素濃度条件を適用することが望ましい。これは、焼成工程(本焼成工程)における雰囲気中の酸素濃度が、Cu-Cu2Oの平衡酸素濃度を超えるとCuの酸化が起こり、その1/100を下回ると上記熱処理を行うことによる比抵抗の回復が十分ではなくなる傾向があることによる。
なお、含酸素雰囲気熱処理の効果は、熱処理雰囲気中の酸素濃度や、熱処理を施す時間などに影響されるので、実際には、含酸素雰囲気熱処理工程における熱処理温度は、雰囲気中の酸素濃度や熱処理時間などを考慮して定めることが望ましい。
この積層型コイル部品1は、図2,3に示すように、内部導体部5aが層間接続されてなる螺旋状のコイルLを内部に備えた積層体(磁性体部)11aの両端側に、コイルLの両端部L1,L2と導通するように配設された一対の外部電極21,22を備えた構造を有している。なお、本発明を適用することが可能な電子部品は、図2,3に示すような積層型コイル部品に限られるものではなく、本発明は、内部導体部と磁性体部とを備えた種々の電子部品を製造する場合に広く適用することが可能である。
以下、その製造方法について説明を行う。
まず、Fe2O3粉末と、ZnO粉末と、NiO粉末と、CuO粉末とを用意した。
そして、Fe2O3粉末、ZnO粉末、NiO粉末、およびCuO粉末を
Fe2O3 49.0mol%
ZnO 30.0mol%
NiO 20.0mol%
CuO 1.0mol%
の割合で秤量し、配合磁性体原料を得た。
図1に示すように、コイル用導体(未焼成内部導体材料)5を有する磁性体セラミックグリーンシート(未焼成磁性体材料)2、コイル用導体を有しない外層用の磁性体セラミックグリーンシート(外装用の未焼成磁性体材料)2(2a)を、所定の順序で積層した。
なお、この実施例では、コイルLのターン数は9.5ターンとした。
また、コイル用導体パターンを有しない磁性体セラミックグリーンシートを複数枚積層し、上記(2)の場合と同じく60℃の温度で100MPaの圧力で圧着することにより、コイル用導体パターンを全く有しない圧着ブロックを作製した。この圧着ブロックを円板状に打ち抜き、厚み1mm、直径10mmの円板試料を作製した。
上述のようにして作製した未焼成積層体、および未焼成の円板試料を、所定の酸素濃度雰囲気中において、所定の温度で熱処理し、十分に脱脂(脱バインダー)した。なお、脱脂時の酸素濃度は、内部導体であるCuが酸化しない雰囲気を選定した。
脱脂後の積層体、および円板試料を、N2-H2-H2Oの混合ガスを流動させ、酸素分圧を制御した焼成炉に入れ、3℃/分の昇温速度でトップ温度(1000℃)まで昇温し、2~4時間保持して、積層体および円板試料を焼結させた。
次に、トップ温度での保持が終了した段階で、3℃/分の降温速度で温度を降下させた。
そして、表1に示すように、温度が900~600℃になった段階で、焼成炉に投入するガスをN2-O2混合ガス、またはエアに変更し、室温まで降温速度3℃/分で温度を低下させ、焼成した積層体、および円板試料を取り出した(表1の条件2~8)。
次に、上記(6)の工程(含酸素雰囲気熱処理工程)を経て得られた焼成済みの積層体を、それぞれ500個ずつ、純水300mlを加えて、約φ1mmのジルコニア質のメディア(ジルコニアボール)とともに、バレル研磨機用のポット(容量1000ml)に入れ、該ポットを所定の回転数で所定時間回転させることにより、焼成済みの積層体をバレル研磨した。
なお、このバレル研磨は、上記(6)の含酸素雰囲気熱処理工程を経て得られる積層体(焼成済積層体)の表面を研磨して、積層体の表面に引き出されたコイル(内部導体部)Lの端部表面に形成された酸化膜を除去するために行われるものである。
次に、バレル研磨を行った後の積層体(焼成済積層体)の両端部に、Ag粉と、ガラスフリットと、ワニスと、溶剤とからなる外部電極形成用の導電ペーストを塗布して乾燥させた後、所定の酸素分圧雰囲気中で、750℃の温度条件下に焼き付けを行い、外部電極本体となる焼付電極を形成した。それから、この焼付電極に周知の方法により電解めっきを施して、焼付電極の表面にニッケルめっき膜、スズめっき膜を順次形成することにより、図2,3に示すように、焼成済積層体(磁性体部)11aの両端側に、コイルLの両端部L1,L2と導通する一対の外部電極21,22を形成した。
(a)インピーダンスカーブ
上述のようにして作製した積層コイル部品について、アジレント・テクノロジー社製のインピーダンスアナライザ(型番HP4291A)を用いて、インピーダンスカーブを測定した。表1の条件1,7および9の試料について測定したインピーダンスカーブを図4,5および6に示す。
また、積層体の表面に、一方の外部電極側から他方の外部電極側に向かってめっき膜に伸びが発生しているものを、めっき伸びが発生しているとして×と判定した。このようにして調べためっき伸びの発生の有無の判定結果を表1に合わせて示す。
一方、含酸素雰囲気熱処理工程を経て製造された、表1の条件2~13の試料では、めっき伸びの発生は認められなかった。
また、磁性体部の比抵抗を測定するため、上述のようにして作製した円板試料の両主面に、Agからなる電極を形成して、比抵抗測定用の試料とした。
そして、この円板試料の両主面の電極間に50Vの直流電界を印加して、絶縁抵抗(IR)を測定し、試料寸法から比抵抗を算出した。算出した比抵抗の値を表1に合わせて示す。
また、他の条件(条件2~13)の場合、めっき伸びの発生は認められていないが、これは、焼成工程で還元された磁性体部が、含酸素雰囲気熱処理工程で酸化されて比抵抗が高くなり、めっきが伸びにくくなったことによるものである。
2 磁性体セラミックグリーンシート
2a 外層用の磁性体セラミックグリーンシート
5 コイル用導体(未焼成内部導体材料)
5a 内部導体部(焼成済内部導体材料)
6 コイル内蔵積層部
7 外層部
10 層間接続用ビアホール導体
11 未焼成積層体
11a 焼成済積層体
21,22 一対の外部電極
L コイル
L1,L2 コイルLの両端部
Claims (4)
- 少なくともNiO、ZnO、Fe2O3を含む磁性体部と、前記磁性体部内に配設され、一部が前記磁性体部の表面に引き出された、Cuを主成分とする内部導体部とを具備する電子部品の製造方法であって、
焼成後に前記磁性体部となる未焼成磁性体材料中に、焼成後に前記内部導体部となる未焼成内部導体材料が配設された未焼成積層体を、Cu-Cu2Oの平衡酸素分圧以下の酸素濃度雰囲気中で焼成する焼成工程と、
前記焼成工程で焼成された焼成済積層体を、その後の降温過程で、酸素濃度が0.01%以上の雰囲気中で熱処理する含酸素雰囲気熱処理工程と
を有することを特徴とする電子部品の製造方法。 - 前記含酸素雰囲気熱処理工程が、前記降温過程における温度の降下を、所定の温度で停止させ、該温度を所定時間保持することにより行われることを特徴とする請求項1記載の電子部品の製造方法。
- 前記含酸素雰囲気熱処理工程における熱処理温度が、900℃以下の温度であることを特徴とする請求項1または2記載の電子部品の製造方法。
- 前記含酸素雰囲気熱処理工程を経て得られる焼成済積層体の表面を研磨して、前記磁性体部の表面に引き出された前記内部導体部の表面の酸化膜を除去する酸化膜除去工程をさらに備えていることを特徴とする請求項1~3のいずれかに記載の電子部品の製造方法。
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WO2013031842A1 (ja) * | 2011-09-02 | 2013-03-07 | 株式会社 村田製作所 | フェライト磁器組成物、セラミック電子部品、及びセラミック電子部品の製造方法 |
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KR101417333B1 (ko) * | 2011-09-02 | 2014-07-08 | 가부시키가이샤 무라타 세이사쿠쇼 | 페라이트 자기 조성물, 세라믹 전자 부품 및 세라믹 전자 부품의 제조 방법 |
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US9230722B2 (en) | 2011-09-02 | 2016-01-05 | Murata Manufacturing Co., Ltd. | Ferrite ceramic composition, ceramic electronic component, and process for producing ceramic electronic component |
US9245680B2 (en) | 2011-09-02 | 2016-01-26 | Murata Manufacturing Co., Ltd. | Common mode choke coil and method for manufacturing the same |
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JP2014120574A (ja) * | 2012-12-14 | 2014-06-30 | Murata Mfg Co Ltd | 多層基板 |
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JP5382144B2 (ja) | 2014-01-08 |
US20120297610A1 (en) | 2012-11-29 |
JPWO2011093489A1 (ja) | 2013-06-06 |
US8590123B2 (en) | 2013-11-26 |
CN102741956B (zh) | 2014-08-20 |
CN102741956A (zh) | 2012-10-17 |
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