JP2001085216A - Oxide magnetic material, manufacture thereof chip parts, and manufacture thereof - Google Patents

Oxide magnetic material, manufacture thereof chip parts, and manufacture thereof

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Publication number
JP2001085216A
JP2001085216A JP26293599A JP26293599A JP2001085216A JP 2001085216 A JP2001085216 A JP 2001085216A JP 26293599 A JP26293599 A JP 26293599A JP 26293599 A JP26293599 A JP 26293599A JP 2001085216 A JP2001085216 A JP 2001085216A
Authority
JP
Japan
Prior art keywords
magnetic material
oxide magnetic
beads
producing
silicon nitride
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP26293599A
Other languages
Japanese (ja)
Inventor
Ko Ito
綱 伊藤
Yukio Takahashi
幸雄 高橋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
TDK Corp
Original Assignee
TDK Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by TDK Corp filed Critical TDK Corp
Priority to JP26293599A priority Critical patent/JP2001085216A/en
Priority to KR1020000047346A priority patent/KR100550684B1/en
Priority to US09/641,333 priority patent/US6485840B1/en
Priority to TW089116732A priority patent/TW475184B/en
Priority to CNB2004100485884A priority patent/CN1287395C/en
Priority to CNB001288679A priority patent/CN1192399C/en
Publication of JP2001085216A publication Critical patent/JP2001085216A/en
Priority to US10/238,727 priority patent/US7070732B2/en
Pending legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • 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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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain an oxide magnetic material which can be baked simultaneously with Ag which is used as internal conductors, keeps sinterability and magnetic permeability, and can shorten its crushing time, chip parts using the magnetic material, and methods for manufacturing the magnetic material and chip parts. SOLUTION: An oxide magnetic material contains Fe3O3, ZnO, CuO, and NiO as main ingredients and 0.001-0.011 wt.% Y2O3, 0.031-0.194 wt.% ZrO2, and 0.010-0.056 wt.% Si as accessory ingredients.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【０００１】[0001]

【発明の属する技術分野】本発明は、各種電子部品に使
用される酸化物磁性材料と、その酸化物磁性材料を用い
て構成され、高周波領域で使用されるバルク型コイル部
品や内部導体を含むインダクタ用チップ部品と、前記酸
化物磁性材料の製造方法とチップ部品の製造方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an oxide magnetic material used for various electronic components, and a bulk type coil component and an internal conductor formed using the oxide magnetic material and used in a high frequency range. The present invention relates to a chip component for an inductor, a method for producing the oxide magnetic material, and a method for producing a chip component.

【０００２】[0002]

【従来の技術】高周波領域で使用されるコイル部品等の
酸化物磁性材料として、Ｎｉ−Ｃｕ−Ｚｎ系のフェライ
トが一般に用いられる。その製造方法としては、粉末冶
金法が一般的である。この方法は、出発材料となるＦｅ
2Ｏ3、ＮｉＯ、ＣｕＯ、ＺｎＯ等の酸化物を所定の比率
となるように秤量し、その後乾式もしくは湿式にて混合
粉砕し、この混合粉末を仮焼成する。次いで、この仮焼
成物を粗粉砕し、さらに微粉砕する。湿式で粉砕を行っ
た場合は乾燥が必要となる。ここでフェライトの特性は
その組成に負うところが大きく、製造の管理の面から、
組成のずれを極めて小さくすることが必要である。ま
た、積層型コイル用の材料としては、Ａｇの融点以下の
低温で焼成する必要があり、Ｆｅ2Ｏ3、ＮｉＯ、Ｃｕ
Ｏ、ＺｎＯの０．１ｍｏｌ％レベルでの組成管理が求め
られる。特にＦｅ2Ｏ3については、フェライトの化学量
論組成（ストイキオ組成）に近づくにつれて反応性が向
上するが、これを越えると反応性が急激に劣化するた
め、フェライトの主成分の中で最も慎重な組成管理が必
要となる。2. Description of the Related Art Ni-Cu-Zn based ferrite is generally used as an oxide magnetic material for a coil component or the like used in a high frequency range. Powder metallurgy is generally used as the manufacturing method. In this method, the starting material Fe
Oxides such as 2 O 3 , NiO, CuO, and ZnO are weighed so as to have a predetermined ratio, and then mixed and pulverized in a dry or wet method, and the mixed powder is calcined. Next, the calcined product is roughly pulverized and further finely pulverized. Drying is required when wet grinding is performed. Here, the properties of ferrite largely depend on its composition, and in terms of manufacturing control,
It is necessary to minimize the composition deviation. In addition, as a material for the laminated coil, it is necessary to fire at a low temperature equal to or lower than the melting point of Ag, such as Fe 2 O 3 , NiO, Cu
It is required to control the composition of O and ZnO at a level of 0.1 mol%. In particular, with regard to Fe 2 O 3 , the reactivity increases as the stoichiometric composition (stoichiometric composition) of the ferrite is approached. However, when the stoichiometric composition is exceeded, the reactivity is rapidly deteriorated. Strict composition control is required.

【０００３】従来のＮｉ−Ｃｕ−Ｚｎフェライトは、そ
の製造工程において、ステンレス鋼ボール、アルミナボ
ール、ジルコニアボール等を媒体ビーズとして用い、混
合粉砕、仮焼成を経た材料の粗粉砕および微粉砕を行っ
てきた。バルク型コイル用材料は、通常、比表面積が
１．０〜６．０ｍ2／ｇ程度となるように仮焼成物を粉
砕しているが、積層型コイル材料はＡｇの融点以下の低
温で焼成する必要があるため、長時間の粉砕を行い、比
表面積を３．０〜１５．０ｍ2／ｇ程度まで上げること
によって粉末の低温での反応性を向上させている。[0003] Conventional Ni-Cu-Zn ferrite is manufactured by using a stainless steel ball, an alumina ball, a zirconia ball or the like as a medium bead, and performing a coarse pulverization and a fine pulverization of a material which has been mixed and pulverized, and calcined. Have been. The bulk coil material is usually obtained by pulverizing the calcined material so that the specific surface area is about 1.0 to 6.0 m 2 / g, but the laminated coil material is calcined at a low temperature equal to or lower than the melting point of Ag. Therefore, the pulverization is performed for a long time to increase the specific surface area to about 3.0 to 15.0 m 2 / g, thereby improving the reactivity of the powder at a low temperature.

【０００４】ここで、ステンレス鋼ボールはＦｅを主成
分としており、粉砕時のメカノケミカル反応により、Ｎ
ｉ−Ｃｕ−Ｚｎフェライトの主成分であるＦｅ2Ｏ3を増
加させる。そして、Ｆｅ2Ｏ3の増加はＮｉ−Ｃｕ−Ｚｎ
フェライトの組成を変化させると共に、安定した組成管
理が困難となる。すなわち秤量値で管理することができ
ない。また、その他の媒体ビーズにおいても耐摩耗性に
難点があり、これらの媒体ビーズの摩耗粉が不純物とし
て混入する虞があるという難点があった。[0004] Here, the stainless steel ball is mainly composed of Fe, and N is generated by a mechanochemical reaction during pulverization.
Fe 2 O 3 which is a main component of i-Cu-Zn ferrite is increased. And the increase of Fe 2 O 3 is Ni-Cu-Zn.
In addition to changing the ferrite composition, stable composition management becomes difficult. That is, it cannot be managed by the weighed value. Also, other medium beads have a problem in abrasion resistance, and there is a problem that abrasion powder of these medium beads may be mixed as impurities.

【０００５】また、一般の媒体ビーズは、外側の耐摩耗
性に比較し、内部のそれは低く、製造を重ねていく上で
摩耗により生じた粉体の混入量の違いによる組成のずれ
が発生し、安定した組成が得られない。そして長時間に
わたる粉砕は混入量の増加を招き、焼成物の特性劣化を
招くことになる。すなわち、不純物として混入した摩耗
粉はＮｉ−Ｃｕ−Ｚｎフェライトの焼結性を劣化させ、
理論密度近傍の焼結体密度および透磁率を得るための焼
成温度が高温となり、製造コストの増加、製品の安定性
の低下を招き、さらにＡｇの融点以下での焼成が困難に
なる。[0005] In addition, general media beads have a lower inner abrasion resistance than the outer abrasion resistance, and a composition deviation occurs due to a difference in the amount of powder mixed in due to abrasion during repeated production. And a stable composition cannot be obtained. Further, pulverization over a long period of time causes an increase in the amount of mixing, which leads to deterioration of characteristics of the fired product. That is, the wear powder mixed as an impurity deteriorates the sinterability of the Ni-Cu-Zn ferrite,
The sintering temperature for obtaining the sintered body density and the magnetic permeability near the theoretical density becomes high, which leads to an increase in the production cost and a decrease in the stability of the product, and it becomes difficult to sinter at or below the melting point of Ag.

【０００６】粉砕時の摩耗粉の混入を低減することを目
的として、特許第２７０８１６０号公報においては、媒
体ビーズとして、耐摩耗性の大きな安定化ジルコニア
（ＦＳＺ）や部分安定化ジルコニア（ＰＳＺ）からなる
ボールを媒体ビーズとしてＭｎ−Ｚｎ系フェライトの粉
砕に用いることが記載されている。該公報記載の方法
は、直径が０．５〜３．０ｍｍのジルコニアボールを媒
体ビーズとして微粉砕工程に使用することにより、不純
物の混入を極力防止し、主成分に対して０．０２重量％
程度以下に混入量の抑制する方法である。また、この方
法により、従来の１２００℃以上という仮焼温度に対
し、約１００℃から２００℃低温（すなわち１０００℃
程度）で焼結させても理論密度近傍の焼結体が得られ、
工業的には焼成温度が下がり、製造コストの低減が可能
であるとしている。For the purpose of reducing the mixing of wear powder at the time of pulverization, Japanese Patent No. 2708160 discloses a medium bead made of stabilized zirconia (FSZ) or partially stabilized zirconia (PSZ) having high wear resistance. It is described that the resulting balls are used as media beads for pulverizing Mn-Zn ferrite. The method described in this publication uses a zirconia ball having a diameter of 0.5 to 3.0 mm as a medium bead in the fine pulverization step, thereby preventing contamination of impurities as much as possible, and using 0.02% by weight of the main component.
This is a method of suppressing the amount of contamination to less than the extent. In addition, this method reduces the calcining temperature from 1200 ° C. or higher to about 100 ° C. to 200 ° C. lower (that is, 1000 ° C.).
), A sintered body near the theoretical density can be obtained,
Industrially, the firing temperature is lowered, and it is possible to reduce the manufacturing cost.

【０００７】また、特開平７−１３３１５０号公報に
は、機械的強度が高い磁性材料の提供を目的として、Ｎ
ｉ−Ｃｕ−Ｚｎフェライトの材料の主成分に対し、０．
０１〜３．０重量％のＺｒＯ2を混入して１１００℃で
１．５時間焼成した例が開示されている。[0007] Japanese Patent Application Laid-Open No. Hei 7-133150 discloses a magnetic material having a high mechanical strength.
With respect to the main component of the material of i-Cu-Zn ferrite, 0.1% is used.
There is disclosed an example in which ZrO 2 of from 0.1 to 3.0% by weight is mixed and calcined at 1100 ° C. for 1.5 hours.

【０００８】[0008]

【発明が解決しようとする課題】しかし、前記特許第２
７０８１６０号公報記載の製造方法に記載された１００
０℃程度の焼成温度は焼成コストを低減できる温度では
なく、また融点が約９６０℃であるＡｇとの同時焼成は
不可能である。また、特開平７−１３３１５０号公報記
載のように、１１００℃ではさらにＡｇとの同時焼成は
不可能である。However, the above-mentioned patent No. 2
No. 100 described in the production method described in JP-A-708160.
The firing temperature of about 0 ° C. is not a temperature at which the firing cost can be reduced, and simultaneous firing with Ag having a melting point of about 960 ° C. is impossible. Further, as described in JP-A-7-133150, simultaneous calcination with Ag cannot be performed at 1100 ° C.

【０００９】また、特許第２７０８１６０号公報記載の
製造方法では、媒体ビーズの摩耗による不純物の材料へ
の混入を低く抑えるため、媒体ビーズに直径の小さいも
のを使用し、例えば１９６時間という長い時間をかけて
仮焼成物を粉砕しているので、ボール効率（材料処理量
／ボール重量）、すなわち粉砕効率が悪いという問題点
もある。In the manufacturing method described in Japanese Patent No. 2708160, a medium bead having a small diameter is used in order to suppress contamination of impurities due to abrasion of the medium bead with a material, and a long time such as 196 hours is used. Since the calcined product is pulverized over time, there is also a problem that the ball efficiency (material processing amount / ball weight), that is, the pulverization efficiency is poor.

【００１０】本発明は、上記問題点に鑑み、低温焼成が
可能であって、焼結性や透磁率と保持し、粉砕時間が短
縮できる酸化物磁性材料とこれを用いたチップ部品と前
記酸化物磁性材料の製造方法とチップ部品の製造方法を
提供することを目的とする。In view of the above problems, the present invention provides an oxide magnetic material which can be fired at a low temperature, maintains sinterability and magnetic permeability, and shortens the pulverization time, and a chip component using the same. It is an object of the present invention to provide a method for manufacturing a magnetic material and a method for manufacturing a chip component.

【００１１】[0011]

【課題を解決するための手段】請求項１の酸化物磁性材
料は、Ｆｅ２Ｏ３、ＺｎＯ、ＣｕＯおよびＮｉＯを主成
分とし、この主成分に、全体量に対する含有量が０．０
０１〜０．０１１重量％となるＹ２Ｏ３を含み、かつ
０．０３〜０．１９４重量％となるＺｒＯ２を含み、か
つ０．０１０〜０．０５６重量％となるＳｉ（Ｓｉの酸
化物である場合を含む）を含むことを特徴とする。The oxide magnetic material according to the first aspect contains Fe 2 O 3 , ZnO, CuO and NiO as main components, and the main component has a content of 0.0 to the total amount.
Si (Oxidation of Si) containing 0.01 to 0.011% by weight of Y 2 O 3 and containing 0.03 to 0.194% by weight of ZrO 2 and 0.010 to 0.056% by weight (Including the case where the object is an object).

【００１２】なお、透磁率、焼結体密度等の特性に影響
を与えない程度であれば、不純物としてＰ、Ａｌ、Ｂ、
Ｍｎ、Ｍｇ、Ｃｏ、Ｂａ、Ｓｒ、Ｂｉ、Ｐｂ、Ｗ、Ｖ、
Ｍｏ等を含有してもよい。また、主成分の組成は、所定
値以上の透磁率を得る上で、好ましくは、Ｆｅ２Ｏ３
４０〜５１ｍｏｌ％、ＺｎＯ １〜３４ｍｏｌ％、Ｃｕ
Ｏ １〜３０ｍｏｌ％、残部ＮｉＯである。さらに好ま
しくはＦｅ２Ｏ３ ４６〜５０ｍｏｌ％、ＺｎＯ ３２
〜３４ｍｏｌ％、ＣｕＯ ９〜１１ｍｏｌ％、ＮｉＯ
８〜１１ｍｏｌ％である。If the properties such as the magnetic permeability and the density of the sintered body are not affected, P, Al, B,
Mn, Mg, Co, Ba, Sr, Bi, Pb, W, V,
Mo or the like may be contained. The composition of the main component is preferably Fe 2 O 3 in order to obtain a magnetic permeability equal to or higher than a predetermined value.
40-51 mol%, ZnO 1-34 mol%, Cu
O 1 to 30 mol%, with the balance being NiO. More preferably, 46-50 mol% of Fe 2 O 3 , ZnO 32
~ 34mol%, CuO 9-11 mol%, NiO
8 to 11 mol%.

【００１３】Ｙ2Ｏ3を含む部分安定化ジルコニアボール
（ＰＳＺ）を用い、仮焼成後の粉体を粉砕する場合、部
分安定化ジルコニアボールはＹ2Ｏ3を約３ｍｏｌ％含む
ものが硬度、破壊強靱値が最も優れていることが分かっ
ており（内田老鶴園発行、強靱ジルコニア−タフなセラ
ミックス、著者堀三郎）、粉砕された粉体の平均粒径が
０．１〜１．０μｍ程度の粒度のものを得ようとする
と、Ｙ2Ｏ3が０．００１重量％未満、ＺｒＯ2が０．０
３１重量％未満、Ｓｉが０．０１０重量％未満の組成の
ものであれば、攪拌速度を遅くし、長い時間をかけて粉
砕する必要が生じるが、これらの重量％以上になれば、
ボール直径や攪拌速度にもよるが、粉砕効率が上り、よ
り短時間で粉砕可能である。一方、Ｙ2Ｏ3が０．０１１
重量％、ＺｒＯ2が０．１９４重量％、Ｓｉが０．０５
６重量％を越えると、Ａｇとの同時焼成が可能な９２０
℃において、物理的強度において問題が生じないと言わ
れている５．０ｇ／ｃｍ3以上の見かけ密度が得にくく
なり、見かけ密度を確保するため、焼成温度を高くせざ
るを得なくなる。また、Ｙ２Ｏ３が０．０１１重量％、
ＺｒＯ２が０．１９４重量％、Ｓｉが０．０５６重量％
を越えると、透磁率の劣化も見られる。[0013] When partially sintered zirconia balls (PSZ) containing Y 2 O 3 are used to pulverize the powder after calcination, the partially stabilized zirconia balls containing about 3 mol% of Y 2 O 3 have a hardness of It is known that the fracture toughness value is the best (published by Uchida Rokakuen, tough zirconia-tough ceramics, author Saburo Hori), and the average particle size of the pulverized powder is about 0.1 to 1.0 μm an attempt to obtain those granularity, Y 2 O 3 is less than 0.001 wt%, ZrO 2 0.0
If the composition is less than 31% by weight and Si is less than 0.010% by weight, it is necessary to reduce the stirring speed and pulverize over a long period of time.
Although it depends on the ball diameter and the stirring speed, the crushing efficiency is increased, and crushing can be performed in a shorter time. On the other hand, when Y 2 O 3 is 0.011
Wt%, ZrO 2 is 0.194 wt%, Si 0.05
If it exceeds 6% by weight, it is possible to simultaneously fire with Ag 920
At ℃, it is difficult to obtain an apparent density of 5.0 g / cm 3 or more, which is said to cause no problem in physical strength, and it is necessary to raise the firing temperature to secure the apparent density. 0.012% by weight of Y 2 O 3 ;
0.194% by weight of ZrO 2 and 0.056% by weight of Si
When it exceeds, the permeability is also deteriorated.

【００１４】請求項２のチップ部品は、請求項１の酸化
物磁性材料の焼結体を用い、バルク型コイル部品として
構成されていることを特徴とする。According to a second aspect of the present invention, there is provided a chip component comprising a sintered body of the oxide magnetic material according to the first aspect and configured as a bulk type coil component.

【００１５】請求項２のチップ部品は、請求項１の酸化
物磁性材料を用いて構成されるため、焼成温度が低く、
廉価に提供でき、強度や透磁率の面においても高温焼成
のものとそれほど遜色がない。Since the chip component of the second aspect is formed using the oxide magnetic material of the first aspect, the firing temperature is low.
It can be provided at low cost, and is not inferior to the one fired at high temperature in terms of strength and magnetic permeability.

【００１６】請求項３のチップ部品は、請求項１の酸化
物磁性材料の焼結体を用い、かつ焼結体内に導電体層を
有して積層型コイル部品または積層型コイル部品を一部
に含んで構成されていることを特徴とする。According to a third aspect of the present invention, there is provided a chip component comprising a sintered body of the oxide magnetic material according to the first aspect and having a conductor layer in the sintered body to partially form a laminated coil component or a laminated coil component. Characterized by being included.

【００１７】請求項４のチップ部品は、請求項３におい
て、内部導体がＡｇまたはＡｇとＰｄの合金を主成分と
することを特徴とする。According to a fourth aspect of the present invention, in the third aspect, the internal conductor is mainly composed of Ag or an alloy of Ag and Pd.

【００１８】請求項３、４のチップ部品においては、請
求項１の酸化物磁性材料を用いて構成されるため、請求
項２のチップ部品と同様の強度、透磁率が得られ、Ａｇ
やＡｇ−Ｐｄの合金との同時焼成が可能である。Since the chip parts of the third and fourth aspects are formed using the oxide magnetic material of the first aspect, the same strength and magnetic permeability as those of the chip parts of the second aspect can be obtained, and Ag can be obtained.
And Ag-Pd alloy can be co-fired.

【００１９】請求項５は、請求項１の酸化物磁性材料を
製造する方法であって、原料の混合粉砕時および仮焼成
を経た材料の粉砕時に湿式内部循環式のメディア撹拌型
ミルを用い、媒体ビーズとして部分安定化ジルコニアと
窒化珪素を使用し、媒体ビースの摩滅により、酸化物磁
性材料内に、全体量に対する含有量が０．００１〜０．
０１１重量％となるＹ２Ｏ３を含み、かつ０．０３〜
０．１９４重量％となるＺｒＯ２を含み、かつ０．０１
０〜０．０５６重量％となるＳｉを含有させることを特
徴とする。A fifth aspect of the present invention relates to a method for producing the oxide magnetic material according to the first aspect, wherein a wet internal circulation type media stirring type mill is used at the time of mixing and pulverizing the raw materials and at the time of pulverizing the material having undergone calcination. Partially stabilized zirconia and silicon nitride are used as the medium beads, and the content of the total amount in the oxide magnetic material is 0.001 to 0.
0.11% by weight of Y 2 O 3 , and
Containing 0.194% by weight of ZrO 2 and 0.01
It is characterized by containing 0 to 0.056% by weight of Si.

【００２０】このように、部分安定化ジルコニアボール
と窒化珪素ボールを利用して仮焼成後の材料の粉砕を行
うことにより、従来のステンレス鋼ボール等を用いる場
合のような組成管理の困難の問題を解消することができ
る。また、粉砕工程を利用してＹ2Ｏ3、ＺｒＯ2および
Ｓｉの混入を行うので、材料混入のための秤量や混合の
工程が不要になる。As described above, since the material after the preliminary firing is crushed by using the partially stabilized zirconia balls and the silicon nitride balls, the problem of difficulty in composition control as in the case of using conventional stainless steel balls or the like is obtained. Can be eliminated. In addition, since Y 2 O 3 , ZrO 2 and Si are mixed by using a pulverizing step, a weighing and mixing step for mixing the materials becomes unnecessary.

【００２１】請求項６の酸化物磁性材料を製造する方法
は、請求項５において、部分安定化ジルコニアビーズお
よび窒化珪素ビーズの全体量に対し、窒化珪素ビーズ
が、体積比で２０％〜９９％であることを特徴とする。According to a sixth aspect of the present invention, in the method for producing an oxide magnetic material according to the fifth aspect, the silicon nitride beads have a volume ratio of 20% to 99% with respect to the total amount of the partially stabilized zirconia beads and the silicon nitride beads. It is characterized by being.

【００２２】部分安定化ジルコニアビーズと窒化珪素ビ
ーズの比率をこの比率に設定することにより、部分安定
化ジルコニアビーズのみを用いて粉砕した場合と比較し
ても、部分安定化ジルコニアビーズの主成分であるＺｒ
Ｏ2とＹ2Ｏ3の摩耗による混入量の制御が一層容易とな
る。By setting the ratio between the partially stabilized zirconia beads and the silicon nitride beads to this ratio, the ratio of the main components of the partially stabilized zirconia beads to that of the pulverization using only the partially stabilized zirconia beads can be improved. A certain Zr
It becomes easier to control the amount of O 2 and Y 2 O 3 mixed due to wear.

【００２３】請求項７は、請求項５または６の酸化物磁
性材料の製造方法であって、媒体ビーズとしてその直径
が０．２〜５ｍｍのものを使用することを特徴とする。A seventh aspect of the present invention is the method for producing an oxide magnetic material according to the fifth or sixth aspect, wherein medium beads having a diameter of 0.2 to 5 mm are used.

【００２４】媒体ビーズの直径が０．２ｍｍ未満である
と、粉砕効率が低下し、５ｍｍを越えると得られる粉末
の微細化を十分行うことができず、理論密度近傍の焼結
体密度を得るための焼成温度が高くなり、また、透磁率
の劣化を招くことになる。If the diameter of the medium beads is less than 0.2 mm, the pulverization efficiency is lowered, and if it exceeds 5 mm, the obtained powder cannot be sufficiently refined and a sintered body density close to the theoretical density is obtained. Temperature increases, and the magnetic permeability deteriorates.

【００２５】請求項８は、請求項５から７までの酸化物
磁性材料の製造方法であって、媒体ビーズの撹拌速度を
２．０〜８．０ｍ／ｓとすることを特徴とする。An eighth aspect of the present invention is the method for producing an oxide magnetic material according to the fifth to seventh aspects, wherein the stirring speed of the medium beads is set to 2.0 to 8.0 m / s.

【００２６】媒体ビーズの攪拌速度が２．０ｍ／ｓに満
たない速度では、所望の比表面積まで粉砕処理を行うた
めの時間が長時間となり、材料の製造に係るリードタイ
ムを考慮すると適正とはいえない。一方、８．０ｍ／ｓ
を越えると媒体ビーズの摩耗量が増大し、理論密度近傍
の焼結体密度および所望の透磁率を得るための焼成温度
が高温となり、製造コストの増加、製品の安定性の低減
を招き、さらにＡｇの融点以下での焼成は困難となる。If the stirring speed of the medium beads is less than 2.0 m / s, it takes a long time to perform the pulverizing treatment to a desired specific surface area, and it is not appropriate in consideration of the lead time for the production of the material. I can't say. On the other hand, 8.0 m / s
Exceeding the above results in an increase in the amount of wear of the medium beads, the firing temperature for obtaining a sintered body density near the theoretical density and a desired magnetic permeability becomes high, leading to an increase in manufacturing costs and a reduction in product stability, and It becomes difficult to bake below the melting point of Ag.

【００２７】請求項９は、請求項５から８までのいずれ
かの酸化物磁性材料の製造方法であって、仮焼成を経た
材料から粉砕により比表面積が６．０〜１５．０ｍ2／
ｇのものを粉体を得ることを特徴とする。A ninth aspect of the present invention is the method for producing an oxide magnetic material according to any one of the fifth to eighth aspects, wherein the specific surface area is 6.0 to 15.0 m 2 / g by pulverizing the calcined material.
g is obtained as a powder.

【００２８】比表面積が６．０ｍ／ｇ未満であると、理
論密度近傍の焼結体密度を得るための焼成温度が高温に
なり、また、透磁率の劣化を招くこととなる。また、１
５．０ｍ2／ｇ以上とするには粉砕時間が長くなる。If the specific surface area is less than 6.0 m / g, the sintering temperature for obtaining a sintered body density near the theoretical density becomes high, and the magnetic permeability is deteriorated. Also, 1
To make it 5.0 m 2 / g or more, the pulverization time becomes long.

【００２９】請求項１０は、請求項３または４のチップ
部品の製造方法であって、媒体ビーズにより粉砕した酸
化物磁性材料と内部導体とを成形して９１０〜９２０℃
で焼成することを特徴とする。A tenth aspect of the present invention is the method of manufacturing a chip component according to the third or fourth aspect, wherein the oxide magnetic material pulverized by the medium beads and the inner conductor are formed at 910 to 920 ° C.
Characterized by firing.

【００３０】焼成温度が９１０℃未満であると、焼結不
足になり、９２０℃を越えるとフェライト中に電極材料
が拡散してチップの電磁気的特性を著しく悪化させる。
なお、焼成時間は５分から３時間程度である。If the firing temperature is lower than 910 ° C., the sintering becomes insufficient. If the firing temperature is higher than 920 ° C., the electrode material is diffused into the ferrite and the electromagnetic properties of the chip are remarkably deteriorated.
The firing time is about 5 minutes to 3 hours.

【００３１】[0031]

【発明の実施の形態】本発明によるバルク型コイル部品
または積層型コイル部品あるいはその他の電子部品用酸
化物磁性材料は、Ｆｅ2Ｏ3、ＺｎＯ、ＮｉＯ、ＣｕＯを
主成分とするフェライト材料であり、必要な場合には前
記したＰ、Ａｌ、Ｂ、Ｍｎ、Ｍｇ、Ｃｏ、Ｂａ、Ｓｒ、
Ｂｉ、Ｐｂ、Ｗ、Ｖ、Ｍｏ等の微量添加物を秤量して加
え、さらに副成分として、媒体ビーズである部分安定化
ジルコニアボールおよび窒化珪素ビーズの摩耗により混
入したＺｒＯ2、Ｙ2Ｏ3およびＳｉを含有するものであ
る。そして、原料の混合粉砕時および仮焼成後の材料の
粉砕時における媒体ビーズの粒度、攪拌速度、攪拌時間
を調整することにより、媒体ビーズの混入の量を調整
し、焼成温度の高温化を必要とせず、Ａｇの融点以下で
の焼成を可能とするものである。BEST MODE FOR CARRYING OUT THE INVENTION An oxide magnetic material for a bulk type coil component, a laminated type coil component or other electronic components according to the present invention is a ferrite material containing Fe 2 O 3 , ZnO, NiO and CuO as main components. If necessary, P, Al, B, Mn, Mg, Co, Ba, Sr,
A trace amount of additives such as Bi, Pb, W, V, and Mo are weighed and added, and ZrO 2 and Y 2 O 3 mixed as a result of abrasion of partially stabilized zirconia balls and silicon nitride beads as medium beads. And Si. Then, by adjusting the particle size, stirring speed, and stirring time of the medium beads at the time of mixing and pulverizing the raw materials and at the time of pulverizing the material after the preliminary firing, it is necessary to adjust the amount of the mixed medium beads and to increase the firing temperature. However, it is possible to perform calcination at a temperature equal to or lower than the melting point of Ag.

【００３２】前記のように秤量された材料は、湿式内部
循環式のメディア攪拌型ミルを用い、媒体ビーズとし
て、部分安定化ジルコニアボールと窒化珪素ボールを用
い、混合粉砕する。その後、仮焼成し、湿式内部循環式
のメディア攪拌型ミルを用い、媒体ビーズとして、部分
安定化ジルコニアボールを用い、粉砕することにより、
酸化物磁性材料を得る。The materials weighed as described above are mixed and pulverized by using a media stirring type mill of a wet internal circulation type, using partially stabilized zirconia balls and silicon nitride balls as medium beads. After that, by calcining, using a wet internal circulation type media stirring type mill, using partially stabilized zirconia balls as media beads, by crushing,
Obtain an oxide magnetic material.

【００３３】バルク型コイル用のコアは、上記のように
して製造した酸化物磁性材料にバインダーを加え、造粒
した後に所定の形状に成形、加工し、空気中で９００〜
１３００℃程度で焼成して作る。なお、このコアは、焼
成後に加工してもよい。そして、このコアに、Ａｕ、Ａ
ｇ、Ｃｕ、Ｆｅ、Ｐｔ、Ｓｎ、Ｎｉ、Ｐｂ、Ａｌ、Ｃｏ
またはこれらの合金からなるワイヤを巻いて作製する。The core for the bulk type coil is formed by adding a binder to the oxide magnetic material produced as described above, granulating the resultant, shaping it into a predetermined shape, and processing it in air at 900 to 900 μm.
It is made by firing at about 1300 ° C. This core may be processed after firing. And in this core, Au, A
g, Cu, Fe, Pt, Sn, Ni, Pb, Al, Co
Alternatively, it is produced by winding a wire made of these alloys.

【００３４】一方、積層型コイルは、通常、酸化物磁性
材料からなる磁性体層ペーストと内部導電体層とを厚膜
技術（印刷法やドクターブレード法）により積層し一体
化した後、焼成し、得られた焼結体表面に外部電極用ペ
ーストを印刷し、焼き付けすることにより製造される。
内部導電体用ペーストは、通常、導電性素子とバインダ
ーと溶剤とを含有する。導電性素子の材質は、インダク
タの品質係数Ｑが向上するという理由から、Ａｇまたは
Ａｇ−Ｐｄ合金が好適である。焼成条件や焼成雰囲気は
磁性体や導電性素子の材質等に応じて適宜決定すればよ
いが、焼成温度は好ましくは８００〜９５０℃、より好
ましくは９１０〜９２０℃程度である。On the other hand, a laminated coil is usually formed by laminating and integrating a magnetic layer paste composed of an oxide magnetic material and an internal conductor layer by a thick film technique (printing method or doctor blade method) and then firing. The paste is manufactured by printing and baking a paste for an external electrode on the surface of the obtained sintered body.
The paste for an internal conductor usually contains a conductive element, a binder, and a solvent. The material of the conductive element is preferably Ag or an Ag-Pd alloy because the quality factor Q of the inductor is improved. The firing conditions and firing atmosphere may be appropriately determined according to the material of the magnetic material or the conductive element, but the firing temperature is preferably 800 to 950 ° C, more preferably about 910 to 920 ° C.

【００３５】[0035]

【実施例】（秤量および粉砕）Ｎｉ−Ｃｕ−Ｚｎフェラ
イトの主成分として、ＮｉＯ ８．７ｍｏｌ％、ＣｕＯ
１０．０ｍｏｌ％、ＺｎＯ ３２．０ｍｏｌ％、Ｆｅ
2Ｏ3 ４９．３ｍｏｌ％なる組成のものを媒体ビーズと
して直径３ｍｍの部分安定化ジルコニア（ＰＳＺ）と窒
化珪素ビーズを用い、湿式内部循環方式のメディア撹拌
型ミルにより、表１に示す媒体ビーズの比率により湿式
で混合し、乾燥した後８００℃にて仮焼成した。次にこ
の仮焼成物を媒体ビーズであるＰＳＺを用い、表１に示
すように、再び湿式内部循環方式のメデイア撹拌型ミル
により湿式で仮焼成物の濃度を３３％とし、表１の左端
の欄に示すように、撹拌速度、粉砕時間、ボール直径を
パラメータとして変化させ、微粉砕した。Example (weighing and pulverization) As a main component of Ni-Cu-Zn ferrite, 8.7 mol% of NiO, CuO
10.0 mol%, ZnO 32.0 mol%, Fe
The media beads having a composition of 49.3 mol% of 2 O 3 were used as media beads, and partially stabilized zirconia (PSZ) having a diameter of 3 mm and silicon nitride beads were used. The mixture was wet-mixed according to the ratio, dried, and then calcined at 800 ° C. Next, as shown in Table 1, this calcined product was wet-adjusted to a concentration of 33% by a wet internal circulation type media stirring type mill using PSZ which is a medium bead. As shown in the column, the mixture was finely pulverized while changing the stirring speed, the pulverization time, and the ball diameter as parameters.

【００３６】すなわちサンプル１〜９は媒体ビーズの比
率を体積比としてＰＳＺ：５０％、窒化珪素：５０％、
また、媒体ビーズの直径を３ｍｍとし、材料の平均粒径
が０．５μｍ、すなわち比表面積が８ｍ2／ｇとなるよ
うに、撹拌速度を１ｍ／ｓ、２．０ｍ／ｓ、４．０ｍ／
ｓ、４．３ｍ／ｓ、５．０ｍ／ｓ、６．０ｍ／ｓ、７．
０ｍ／ｓ、８．０ｍ／ｓ、１０ｍ／ｓと変化させ、各撹
拌速度に対し、粉砕時間を９３時間、８２時間、５５時
間、４５時間、４０時間、２８時間、２０時間、１２時
間、２。５時間と変化させた。そしてこれらをサンプル
１〜９として、いずれも、平均粒径が０．５μｍ、比表
面積が８ｍ2／ｇの粉体を得た。That is, in Samples 1 to 9, PSZ: 50%, silicon nitride: 50%, and
Further, the stirring speed was set to 1 m / s, 2.0 m / s, and 4.0 m / s so that the diameter of the medium beads was 3 mm and the average particle size of the material was 0.5 μm, that is, the specific surface area was 8 m 2 / g.
s, 4.3 m / s, 5.0 m / s, 6.0 m / s, 7.
0 m / s, 8.0 m / s, and 10 m / s. For each stirring speed, the pulverization time was 93 hours, 82 hours, 55 hours, 45 hours, 40 hours, 28 hours, 20 hours, 12 hours, It was changed to 2.5 hours. Using these as Samples 1 to 9, powders having an average particle diameter of 0.5 μm and a specific surface area of 8 m 2 / g were obtained.

【００３７】また、サンプル１０〜１３は、ボール直径
を３ｍｍ、撹拌速度を４ｍ／ｓとし、粉砕時間を１時
間、１．５時間、１１５時間、１３４時間に変化させ、
平均粒径が２．２μｍ、１．８μｍ、０．３μｍ、０．
２μｍ、比表面積が１．８ｍ2／ｇ、２．２ｍ2／ｇ、１
５ｍ2／ｇ、１７ｍ2／ｇの粉体を得たものである。For samples 10 to 13, the ball diameter was 3 mm, the stirring speed was 4 m / s, and the pulverization time was changed to 1, 1.5, 115, and 134 hours.
The average particle size is 2.2 μm, 1.8 μm, 0.3 μm, and 0.1 μm.
2μm, specific surface area of 1.8m 2 /g,2.2m 2 / g, 1
Powders of 5 m 2 / g and 17 m 2 / g were obtained.

【００３８】また、サンプル１４〜１６は、撹拌速度を
４ｍ／ｓ、粉砕時間を５５時間と一定にし、ボール直径
を０．２ｍｍ、５ｍｍ、１２ｍｍに変化させて、それぞ
れ平均粒径が０．６μｍ、０．７μｍ、１．５μｍ、比
表面積がそれぞれ７ｍ2／ｇ、６ｍ2／ｇ、３ｍ2／ｇの
粉体を得たものである。In Samples 14 to 16, the stirring speed was 4 m / s, the grinding time was constant at 55 hours, the ball diameter was changed to 0.2 mm, 5 mm and 12 mm, and the average particle diameter was 0.6 μm. , 0.7 μm, 1.5 μm, and powders having specific surface areas of 7 m 2 / g, 6 m 2 / g, and 3 m 2 / g, respectively.

【００３９】また、サンプル１７〜１９は、撹拌速度を
４ｍ／ｓ、粉砕時間を５５時間、ボール直径を３ｍｍと
一定にし、媒体ビーズとして用いたＰＳＺと窒化珪素の
比率を体積比でＰＳＺ：窒化珪素＝２０：８０、ＰＳ
Ｚ：窒化珪素＝８０：２０、ＰＳＺ：窒化珪素＝９９：
１と変化させ、それぞれ平均粒径が０．７μｍ、０．４
５μｍ、０．４５μｍ、比表面積がそれぞれ６ｍ２／
ｇ、９ｍ２／ｇ、９ｍ２／ｇの粉体を得たものである。In Samples 17 to 19, the stirring speed was 4 m / s, the grinding time was 55 hours, the ball diameter was constant at 3 mm, and the ratio of PSZ used as medium beads to silicon nitride was PSZ: nitride by volume ratio. Silicon = 20: 80, PS
Z: silicon nitride = 80: 20, PSZ: silicon nitride = 99:
1, and the average particle size is 0.7 μm and 0.4, respectively.
5 μm, 0.45 μm, each having a specific surface area of 6 m 2 /
g, 9 m 2 / g, and 9 m 2 / g powder.

【００４０】また、比較のため、従来例として、サンプ
ル２０〜２２について試験を行った。サンプル２０は、
主成分が、ＮｉＯ ９．５ｍｏｌ％、ＣｕＯ １０．５
ｍｏｌ％、ＺｎＯ ３４．０ｍｏｌ％、Ｆｅ2Ｏ3 ４
６．０ｍｏｌ％のものを用い、粉砕機として前記湿式内
部循環式メディア撹拌型ミルを用い、ボールとして直径
が３ｍｍ、材質がステンレス鋼のものを用い、前記サン
プル１〜９と同じ平均粒径０．５μｍ、比表面積８ｍ2
／ｇが得られるように、撹拌速度、粉砕時間を設定した
ものである。For comparison, samples 20 to 22 were tested as conventional examples. Sample 20 is
The main components are NiO 9.5 mol%, CuO 10.5
mol%, ZnO 34.0 mol%, Fe 2 O 3 4
6.0 mol%, a wet internal circulation type media stirring type mill as a pulverizer, a ball having a diameter of 3 mm and a material of stainless steel, and the same average particle diameter of 0 as the samples 1 to 9 were used. 0.5 μm, specific surface area 8 m 2
/ G is obtained by setting the stirring speed and the pulverization time.

【００４１】サンプル２１は、サンプル１〜１８で使用
した主成分の材料を用い、粉砕機として前記湿式内部循
環式メディア撹拌型ミルを用い、ボールとして直径が３
ｍｍ、材質がチタニアのものを用い、前記サンプル１〜
９と同じ平均粒径０．５μｍ、比表面積８ｍ2／ｇが得
られるように、撹拌速度、粉砕時間を設定したものであ
る。Sample 21 was made of the material of the main component used in Samples 1 to 18, the wet internal circulation type media stirring type mill was used as a pulverizer, and the ball was 3 mm in diameter.
mm, the material is made of titania, the samples 1 to
The stirring speed and the pulverizing time were set so that the same average particle size of 0.5 μm and the specific surface area of 8 m 2 / g as in Example 9 were obtained.

【００４２】サンプル２２は、主成分が、ＮｉＯ ９．
５ｍｏｌ％、ＣｕＯ １０．５ｍｏｌ％、ＺｎＯ ３
４．０ｍｏｌ％、Ｆｅ2Ｏ3 ４６．０ｍｏｌ％のものを
用い、粉砕機としてボールミルを用い、ボールとして直
径が３ｍｍ、材質がステンレス鋼のものを用い、平均粒
径０．３μｍ、比表面積１２ｍ2／ｇのものを得たもの
である。The sample 22 was composed mainly of NiO 9.
5 mol%, CuO 10.5 mol%, ZnO 3
4.0 mol%, 46.0 mol% of Fe 2 O 3 , a ball mill as a pulverizer, a ball having a diameter of 3 mm, a material of stainless steel, an average particle diameter of 0.3 μm, and a specific surface area of 12 m 2 / g was obtained.

【００４３】なお、表２に示した材料中の不純物とその
混入量および表３に示す製造後の主成分の定量分析は蛍
光Ｘ線分析法により測定した。また、比表面積は（株）
島津製作所製流動式比表面積自動測定装置、フローソー
プ２３００型でＢＥＴ一点法により測定した。また、平
均粒径は、ハネウェル（ＨＯＮＥＷＥＬＬ）社製マイク
ロトラックＨＲＡ９３２０−Ｘ１００型でレーザー回折
・散乱法により測定した。The impurities in the materials shown in Table 2 and the amounts of the impurities mixed therein and the quantitative analysis of the main components after production shown in Table 3 were measured by X-ray fluorescence analysis. The specific surface area is
It was measured by a BET one-point method using a flow soap type 2300 automatic measuring apparatus made by Shimadzu Corporation. The average particle size was measured by a laser diffraction / scattering method using Microtrack HRA9320-X100 manufactured by Honeywell.

【００４４】（透磁率および焼結体密度測定のための試
料作製）前記サンプル１〜２２に示した材料にバインダ
ーとしてＰＶＡ１２４の３％水溶液を１０重量部加えて
造粒し、後述の測定条件により所定の形状に成形し、空
気中で８７０℃、８８０℃、９１０℃、９２０℃、９４
０℃、１０００℃、１１００℃で２時間焼成して作製し
た。(Preparation of Samples for Measuring Magnetic Permeability and Sintered Body Density) 10% by weight of a 3% aqueous solution of PVA124 was added as a binder to the materials shown in Samples 1 to 22 and granulated. It is molded into a predetermined shape and 870 ° C, 880 ° C, 910 ° C, 920 ° C, 94
It was produced by firing at 0 ° C., 1000 ° C., and 1100 ° C. for 2 hours.

【００４５】（評価）コアの材料としての評価は、所望
の比表面積とするまでの粉砕時間と、媒体ビーズの摩耗
による混入と思われる不純物の確認と、主成分であるＦ
ｅ2Ｏ3、ＺｎＯ、ＣｕＯ、ＮｉＯの組成のずれと、表４
に示す初透磁率と、表５に示す見かけ密度とを評価する
ことにより行った。初透磁率の測定は、外径１８ｍｍ、
内径１０ｍｍ、高さ３．１ｍｍのトロイダル型となるよ
うに成形し、空気中で所定温度にて焼成し、ワイヤーを
２０回巻いて実際にコイルを作製し、インピーダンスア
ナライザ（ヒューレットパッカード社製４２９１Ａ）に
より、磁界を０．４Ａ／ｍ印加し、１００ｋＨｚのイン
ダクタンスを測定し、形状から得られた定数から算出し
てこれを求めた。(Evaluation) Evaluation of the material of the core includes grinding time until a desired specific surface area is obtained, confirmation of impurities considered to be mixed in due to abrasion of the medium beads, and F as a main component.
Table 4 shows the deviation of the composition of e 2 O 3 , ZnO, CuO, and NiO.
And the apparent density shown in Table 5 were evaluated. The measurement of the initial magnetic permeability is 18 mm in outer diameter,
It is formed into a toroidal shape having an inner diameter of 10 mm and a height of 3.1 mm, fired in air at a predetermined temperature, wound a wire 20 times to actually produce a coil, and an impedance analyzer (4291A manufactured by Hewlett-Packard Company). , A magnetic field of 0.4 A / m was applied, the inductance at 100 kHz was measured, and the inductance was calculated from the constant obtained from the shape.

【００４６】見かけ密度は、焼結体の寸法から体積を求
め、その質量を体積で除算して求めた。ここで、見かけ
密度は、焼結体の焼結性の良し悪しを見るためのもので
ある。見かけ密度が低いことにより、焼結体内部の空孔
が多くなり、素子化した場合において、高い温湿度での
使用により、この空孔が原因となり、ショート不良等の
信頼性に影響を及ぼしたり、物理的強度が脆弱となると
いう問題が生じる。このような問題が生じない見かけ密
度は、一般にＮｉ−Ｃｕ−Ｚｎフェライトの理論密度
（５．３〜５．５ｇ／ｃｍ3）の９５％以上となる５．
０ｇ／ｃｍ3以上である。The apparent density was determined by calculating the volume from the dimensions of the sintered body and dividing the mass by the volume. Here, the apparent density is used to check whether the sinterability of the sintered body is good or bad. Since the apparent density is low, the number of pores inside the sintered body increases, and when the element is manufactured, when used at high temperature and humidity, these pores cause the reliability of short-circuit failure and the like. This causes a problem that the physical strength becomes weak. The apparent density at which such a problem does not occur is generally 95% or more of the theoretical density (5.3 to 5.5 g / cm 3 ) of Ni—Cu—Zn ferrite.
0 g / cm 3 or more.

【００４７】[0047]

【表１】 [Table 1]

【００４８】[0048]

【表２】 [Table 2]

【００４９】（評価結果） ［不純物の混入］表１において、サンプル１〜９のよう
に、所望の比表面積を８ｍ2／ｇとしたとき、撹拌速度
が増加するにつれ、粉砕時間が短時間になることから、
撹拌速度の増加が粉砕効率を向上させることが分かる。
ただし、この撹拌速度の増加は媒体ビーズの摩耗量を増
加させる。表２に示すように、ＰＳＺおよび窒化珪素に
ついては、その主成分であるＺｒＯ2とＹ2Ｏ3とＳｉが
混入するが、他の成分の混入は認められない。(Evaluation Results) [Contamination of Impurities] In Table 1, when the desired specific surface area was 8 m 2 / g as in Samples 1 to 9, as the stirring speed increased, the pulverization time was shortened. From becoming
It can be seen that increasing the stirring speed improves the grinding efficiency.
However, this increase in the stirring speed increases the abrasion amount of the medium beads. As shown in Table 2, the main components of PSZ and silicon nitride are mixed with ZrO 2 , Y 2 O 3 and Si, but no other components are mixed.

【００５０】一方、従来例であるサンプル２０、２１に
おいては、ボール直径と撹拌速度が同じであるサンプル
５の場合と粉砕時間とボールの摩耗量を比較すると、サ
ンプル２０、すなわちステンレス鋼の場合、ＰＳＺ：窒
化珪素＝５０：５０の場合より粉砕時間が短縮され、粉
砕効率は非常に高いが、摩耗量はＰＳＺ：窒化珪素＝５
０：５０の場合に比較して約２０倍と非常に多量であ
る。また、サンプル２１、すなわちチタニアの場合もＰ
ＳＺ：窒化珪素＝５０：５０に比較して約８．２倍の摩
耗量がある。On the other hand, in the conventional samples 20 and 21, when the grinding time and the wear amount of the ball are compared with the case of the sample 5 having the same ball diameter and the stirring speed, the sample 20, that is, the stainless steel, The grinding time is shorter than in the case of PSZ: silicon nitride = 50: 50, the grinding efficiency is very high, but the wear amount is PSZ: silicon nitride = 5.
Compared with the case of 0:50, it is about 20 times, which is a very large amount. Also, in the case of sample 21, that is, titania, P
There is about 8.2 times as much wear as SZ: silicon nitride = 50: 50.

【００５１】［不純物の混入による材料組成のずれ］表
３は主成分であるＦｅ2Ｏ3、ＺｎＯ、ＣｕＯ、ＮｉＯの
秤量から混合粉砕、仮焼成、微粉砕を経た材料の組成の
ずれを示す。これは主成分である前記各酸化物の定量分
析の結果である。表３から分かるように、サンプル２
０、２２のようにステンレス鋼を媒体ビーズに用いた場
合、秤量から完成までのＦｅ2Ｏ3のずれが大きく、Ｎｉ
−Ｃｕ−Ｚｎフェライトにおいて、最も慎重な管理が要
求されるＦｅ2Ｏ3の組成が秤量から完成までに３ｍｏｌ
％以上増加する。また、ステンレス鋼は内部と外部の硬
度に違いがあるため、媒体ビーズの使用が長期にわたる
と、Ｆｅ2Ｏ3の混入量にも違いが生じるため、組成管理
が困難になることが分かる。[Difference in Material Composition Due to Incorporation of Impurities] Table 3 shows the deviation in the composition of the material obtained by weighing the main components Fe 2 O 3 , ZnO, CuO, and NiO, followed by mixing and pulverization, calcination, and fine pulverization. . This is the result of quantitative analysis of each of the oxides as the main components. As can be seen from Table 3, sample 2
When stainless steel is used for the medium beads as in 0 and 22, the deviation of Fe 2 O 3 from weighing to completion is large, and
In -cu-Zn ferrite, the composition of Fe 2 O 3 the most careful management is required to 3mol to complete the weighing
% Or more. Further, it can be seen that since stainless steel has a difference in hardness between the inside and the outside, if the medium beads are used for a long period of time, the mixing amount of Fe 2 O 3 will also differ, and it will be understood that the composition control becomes difficult.

【００５２】［粉砕時間と比表面積との関係］また、サ
ンプル１０〜１３から分かるように、粉砕時間を長時間
とすることにより、比表面積を増加させることができる
ことが分かる。[Relationship Between Pulverization Time and Specific Surface Area] As can be seen from Samples 10 to 13, it can be seen that the specific surface area can be increased by increasing the pulverization time.

【００５３】[0053]

【表３】 [Table 3]

【００５４】［ボール直径と比表面積との関係］また、
撹拌速度と粉砕時間を一定としたサンプル３、１４、１
５、１６に示すように、同じ撹拌速度で同じ粉砕時間粉
砕した場合、ボール直径が３ｍｍの場合が得られる粉体
の比表面積が最も大きく、粉砕効率が高いことが分か
る。一般にボール直径が小さくなるにつれて、粉砕効率
が大きくなることが知られているが、ただしそれは、粗
粉砕工程を経た場合であって、十分粗粉砕を行わない実
施例においては、ボール直径が３ｍｍの場合が最も粉砕
効率が高いことが分かる。なお、サンプル２２のように
ボールミルを使用した場合、１９２時間の長時間の粉砕
により、比表面積を１２ｍ2／ｇとすることが可能とな
る。しかしこれは、湿式内部循環式のメディア撹拌型ミ
ルで撹拌速度を４ｍ／ｓとしたときのサンプル１２と比
較しても、倍以上の粉砕時間を要する。しかも、サンプ
ル２２の場合、比表面積も小さく、ボールミルの粉砕効
率が低いことが分かる。[Relationship between ball diameter and specific surface area]
Samples 3, 14, 1 with constant stirring speed and grinding time
As shown in FIGS. 5 and 16, it can be seen that when pulverization is performed at the same stirring speed for the same pulverization time, the specific surface area of the powder obtained when the ball diameter is 3 mm is the largest and the pulverization efficiency is high. It is generally known that as the ball diameter decreases, the grinding efficiency increases. However, this is the case where the ball has undergone the coarse grinding step, and in the example where the coarse grinding is not sufficiently performed, the ball diameter is 3 mm. It can be seen that the case has the highest grinding efficiency. When a ball mill is used as in Sample 22, the specific surface area can be made 12 m 2 / g by pulverizing for 192 hours. However, this requires twice or more the pulverization time as compared with Sample 12 when the stirring speed is 4 m / s in a wet internal circulation type media stirring type mill. In addition, in the case of the sample 22, the specific surface area is small, and it is understood that the pulverizing efficiency of the ball mill is low.

【００５５】［初透磁率、見かけ密度について］表４に
示す初透磁率は、表５に示す見かけ密度と関連のあるこ
とが分かる。すなわち比較的低い透磁率しか得られない
サンプル９〜１１、１６、２１においては、見かけ密度
も低くなる。サンプル１〜９において、ボール直径３ｍ
ｍのＰＳＺと窒化珪素を媒体ビーズとして、湿式内部循
環式のメディア撹拌型ミルを用い、比表面積が８ｍ2／
ｇとなるように撹拌速度を変化させたが、撹拌速度を大
きくすると透磁率と焼結体密度は双方とも劣化した。こ
れはＰＳＺの成分であるＺｒＯ2とＹ2Ｏ3の混合量およ
び窒化珪素によるＳｉの混入量の増加が、特性の劣化に
寄与しているものである。ただし焼成温度が１１００℃
とするとその差は小さく、ほぼ同等と考えられるが、９
４０℃以下では大きくなる。[Regarding Initial Permeability and Apparent Density] It can be seen that the initial permeability shown in Table 4 is related to the apparent density shown in Table 5. That is, in samples 9 to 11, 16, and 21 in which only a relatively low magnetic permeability can be obtained, the apparent density is low. In samples 1 to 9, the ball diameter is 3m
m of PSZ and silicon nitride as media beads, using a wet internal circulation type media stirring type mill, and a specific surface area of 8 m 2 /
The stirring speed was changed so as to obtain g, but when the stirring speed was increased, both the magnetic permeability and the sintered body density were deteriorated. This is because the increase in the amount of mixture of ZrO 2 and Y 2 O 3 which are the components of PSZ and the amount of Si mixed in by silicon nitride contributes to the deterioration of the characteristics. However, firing temperature is 1100 ° C
Then, the difference is small and considered to be almost equal.
If the temperature is lower than 40 ° C., it becomes large.

【００５６】また、この特性は従来の条件であるサンプ
ル２２と比較すると、撹拌速度が６ｍ／ｓ、ＺｒＯ2の
混入量が０．１１１重量％、Ｙ2Ｏ3が０．００６重量
％、Ｓｉが０．０２７重量％を越えると劣化することが
分かる。これを越えない範囲では従来と比較して極めて
良好な特性が得られる。また、９２０℃での焼成、すな
わちＡｇの融点以下での焼成が可能となる。ただし、こ
の値を越えても、ＺｒＯ2の混入量が０．１９４重量
％、Ｙ2Ｏ3が０．０１１重量％、Ｓｉが０。０５６重量
％を越えない範囲であれば、サンプル８に示すように、
９２０℃において、５ｇ／ｃｍ3以上の見かけ密度が得
られた。Further, as compared with the sample 22, which is a conventional condition, the stirring speed is 6 m / s, the mixing amount of ZrO 2 is 0.111% by weight, Y 2 O 3 is 0.006% by weight, It can be seen that when the content exceeds 0.027% by weight, it deteriorates. Within a range not exceeding this, extremely excellent characteristics can be obtained as compared with conventional ones. In addition, firing at 920 ° C., that is, firing at a temperature equal to or lower than the melting point of Ag, becomes possible. However, even if this value is exceeded, if the amount of ZrO 2 does not exceed 0.194% by weight, Y 2 O 3 does not exceed 0.011% by weight, and Si does not exceed 0.056% by weight, sample 8 is used. As shown,
At 920 ° C., an apparent density of 5 g / cm 3 or more was obtained.

【００５７】［撹拌速度について］見かけ密度５．０ｇ
／ｃｍ3以上が、Ａｇとの同時焼成に好適な９２０℃以
下の焼結により得られるサンプルは、サンプル１〜８、
サンプル１２〜１５、サンプル１７〜１９、サンプル２
０、２２である。サンプル９の場合、撹拌速度が１０ｍ
／ｓであり、この場合は、平均粒径、比表面積がサンプ
ル１〜８と同じであっても、ＺｒＯ2、Ｙ2Ｏ3、Ｓｉの
混入量が多過ぎるため、９４０℃であっても５．０ｇ／
ｃｍ3以上の見かけ密度を得ることができない。また、
サンプル１の場合、撹拌速度が１ｍ／ｓであり、比表面
積が８．０ｍ2／ｇとなるまでに９３時間の長時間を要
するので好ましくない。このようなことから、好適な撹
拌速度は２．０〜８．０ｍ／ｓである。[Agitating speed] Apparent density 5.0 g
/ Cm 3 or more is a sample obtained by sintering at 920 ° C. or less suitable for co-firing with Ag,
Sample 12-15, Sample 17-19, Sample 2
0 and 22. In the case of sample 9, the stirring speed is 10 m
In this case, even if the average particle diameter and the specific surface area are the same as those of Samples 1 to 8, even if the temperature is 940 ° C. because the amount of ZrO 2 , Y 2 O 3 , and Si mixed is too large. 5.0 g /
It is not possible to obtain an apparent density of more than cm 3 . Also,
In the case of the sample 1, the stirring speed is 1 m / s, and it takes 93 hours for the specific surface area to reach 8.0 m 2 / g, which is not preferable. For this reason, a suitable stirring speed is 2.0 to 8.0 m / s.

【００５８】[0058]

【表４】 [Table 4]

【００５９】［比表面積について］得られる粉体の比表
面積が２．５ｍ2／ｇであるサンプル１１や３ｍ2／ｇで
あるサンプル１６の場合には、９２０℃において、５ｇ
／ｃｍ3以上の見かけ密度が得られない。比表面積が６
ｍ2／ｇとなるサンプル１５においては、５．０ｇ／ｃ
ｍ3以上の見かけ密度が得られる。[Specific Surface Area] In the case of Sample 11 having a specific surface area of 2.5 m 2 / g or Sample 16 having a specific surface area of 3 m 2 / g, 5 g at 920 ° C.
/ Cm 3 or higher. Specific surface area is 6
In sample 15, which has an m 2 / g of 5.0 g / c
An apparent density of at least m 3 is obtained.

【００６０】一方、サンプル１２のように、比表面積が
１５ｍ2／ｇであれば、見かけ密度として５．０ｇ／ｃ
ｍ3以上の値が得られる。サンプル１２の場合、粉砕時
間が１１５時間と長くなっているが、これは撹拌速度を
大とすることにより、短縮することができる。On the other hand, when the specific surface area is 15 m 2 / g as in Sample 12, the apparent density is 5.0 g / c.
A value of at least m 3 is obtained. In the case of Sample 12, the grinding time is as long as 115 hours, but this can be reduced by increasing the stirring speed.

【００６１】[0061]

【表５】 [Table 5]

【００６２】［ボール直径について］サンプル３、１４
〜１６は撹拌速度、粉砕時間を一定にし、媒体ビーズと
して使用したボール直径を変更し、湿式内部循環式のメ
ディア撹拌型ミルを用いて粉砕を行ったものであるが、
サンプル３、１４、１５のように、直径が０．２〜５ｍ
ｍの範囲では５ｇ／ｃｍ3以上の見かけ密度が９２０℃
以上での焼成で得られる。[About Ball Diameter] Samples 3 and 14
１６16 are agitation speed, crushing time is fixed, the ball diameter used as the medium beads is changed, and crushing is performed using a wet internal circulation type media stirring type mill,
0.2 to 5 m in diameter as in samples 3, 14, 15
m, the apparent density of 5 g / cm 3 or more is 920 ° C.
Obtained by the above firing.

【００６３】［ＰＳＺビーズと窒化珪素ビーズの比率に
ついて］サンプル３、１７〜１９は、ボール直径、撹拌
速度、粉砕時間を一定にし、媒体ビーズとして使用した
ＰＳＺと窒化珪素の体積比率を変更し、湿式内部循環式
のメディア撹拌型ミルを用いて粉砕を行ったものである
が、ＰＳＺ：窒化珪素＝２０：８０〜９９：１の範囲に
おいて、５ｇ／ｃｍ３以上の見かけ密度が９２０℃以上
の焼成温度で得られる。[Regarding the Ratio of PSZ Beads to Silicon Nitride Beads] In Samples 3, 17 to 19, the ball diameter, the stirring speed, and the pulverizing time were kept constant, and the volume ratio of PSZ and silicon nitride used as the medium beads was changed. The pulverization was carried out using a wet internal circulation type media stirring type mill. In the range of PSZ: silicon nitride = 20: 80 to 99: 1, the apparent density of 5 g / cm 3 or more was 920 ° C. or more. Obtained at the firing temperature.

【００６４】［焼成温度について］Ａｇの融点９６０℃
より低い９４０℃以下であれば、Ａｇとの同時焼成が可
能である。従って焼成温度は８０〜９４０℃であり、さ
らに好ましくは９１０〜９２０℃である。[Baking temperature] Melting point of Ag: 960 ° C.
If the temperature is lower than 940 ° C. or lower, simultaneous firing with Ag is possible. Therefore, the firing temperature is from 80 to 940 ° C, more preferably from 910 to 920 ° C.

【００６５】なお、サンプル２１のチタニアボール使用
の場合、５ｇ／ｃｍ3の焼結体密度を得るには１１００
℃以上の焼成温度が必要である。In the case of using the titania balls of Sample 21, 1100 is required to obtain a sintered body density of 5 g / cm 3.
A firing temperature of at least ℃ is required.

【００６６】［特許第２７０８１６０号公報記載の方法
との比較］該公報に記載の方法では、媒体ビーズ摩耗に
よるＺｒＯ2の混入量を０．０２重量％程度に抑えるた
め、１９６時間という長時間をかけてゆっくりと粉砕し
ている。本発明は、Ａｇとの同時焼成を目標として、９
２０℃程度の焼成でも５ｇ／ｃｍ3以上の見かけ密度が
得られる範囲でＺｒＯ2、Ｙ2Ｏ3の混入量をサンプル７
のようにそれぞれ０．０３重量％、０．００１重量％以
上に、また、窒化珪素ビーズも併用してそのＳｉの混入
量をサンプル１８のように０．００１重量％以上に上
げ、これにより撹拌速度を上げて粉砕効率を上げること
を可能としているのである。[Comparison with the method described in Japanese Patent No. 2708160] In the method described in this publication, a long time of 196 hours is used in order to suppress the amount of ZrO 2 mixed due to abrasion of the medium beads to about 0.02% by weight. It is slowly crushed. The present invention aims at co-firing with Ag,
Sample 7 determines the amount of ZrO 2 and Y 2 O 3 mixed within a range where an apparent density of 5 g / cm 3 or more can be obtained even when firing at about 20 ° C.
The amount of Si mixed therein was increased to at least 0.03% by weight and 0.001% by weight, respectively, as described above, and the amount of Si mixed therein was increased to at least 0.001% by weight, as in Sample 18, using silicon nitride beads. It is possible to increase the grinding efficiency by increasing the speed.

【００６７】[0067]

【発明の効果】請求項１の酸化物磁性材料によれば、Ｐ
ＳＺと窒化珪素を用いてＮｉ−Ｃｕ−Ｚｎに前記混入量
のＹ2Ｏ3、ＺｒＯ2およびＳｉを含ませることにより、
Ａｇとの同時焼成が可能な温度において焼成可能で、焼
成により５．０ｇ／ｃｍ3以上の見かけ密度で透磁率の
面においても需要に応じることのできる焼結体を得るこ
とができる。また、Ｙ2Ｏ3、ＺｒＯ2およびＳｉの量を
前記範囲に設定することにより、短い粉砕時間で酸化物
磁性材料を得ることができ、製造コストを低減できる。According to the oxide magnetic material of the first aspect, P
By using SZ and silicon nitride to include the above-mentioned mixed amounts of Y 2 O 3 , ZrO 2 and Si in Ni—Cu—Zn,
It is possible to obtain a sintered body which can be fired at a temperature at which simultaneous firing with Ag is possible, and which can meet the demand in terms of magnetic permeability at an apparent density of 5.0 g / cm 3 or more by firing. Further, by setting the amounts of Y 2 O 3 , ZrO 2 and Si within the above range, an oxide magnetic material can be obtained in a short pulverization time, and the production cost can be reduced.

【００６８】請求項２、３のチップ部品は、請求項１の
酸化物磁性材料の焼結体を用い、バルク型コイル部品、
あるいは積層型コイル部品が構成されるので、強度や透
磁率の面においても高温焼成のものとそれほど遜色がな
いコイル部品が得られる。A chip component according to claims 2 and 3 uses a sintered body of the oxide magnetic material according to claim 1 and is a bulk type coil component.
Alternatively, since a laminated coil component is formed, it is possible to obtain a coil component that is not inferior in strength and permeability to that of high-temperature firing.

【００６９】請求項４のチップ部品は、請求項３におい
て、内部導体がＡｇまたはＡｇとＰｄの合金を主成分と
するので、Ｑの高いコイル部品が得られる。According to a fourth aspect of the present invention, since the internal conductor is mainly composed of Ag or an alloy of Ag and Pd, a coil component having a high Q can be obtained.

【００７０】請求項５、６の酸化物磁性材料を製造する
方法によれば、ＰＳＺボール、窒化珪素ボールを利用し
て仮焼成後の材料の粉砕を行うことにより、従来のステ
ンレス、鋼ボール等を用いる場合のような組成管理の困
難の問題を解消することができる。また、粉砕工程を利
用してＹ2Ｏ3、、ＺｒＯ2およびＳｉの混入を行うので、
材料混入のための秤量や混合の工程が不要になる。ま
た、特許第２７０８１６０号公報に記載のように、粉砕
時の媒体ビーズからの混入量を低く抑える場合に比較
し、撹拌速度を上げ、粉砕時間を短縮して製造コストを
安価にすることができる。According to the method for producing an oxide magnetic material according to claims 5 and 6, the material after calcination is crushed by using a PSZ ball or a silicon nitride ball to obtain a conventional stainless steel, steel ball or the like. Can solve the problem of difficulty in composition management as in the case of using a. In addition, since Y 2 O 3 , ZrO 2 and Si are mixed using a pulverizing process,
There is no need for a weighing or mixing process for mixing the materials. Also, as compared with the case where the mixing amount from the medium beads during pulverization is suppressed low as described in Japanese Patent No. 2708160, the stirring speed can be increased, the pulverization time can be shortened, and the production cost can be reduced. .

【００７１】請求項７ないし９の酸化物磁性材料の製造
方法によれば、媒体ビーズ直径、媒体ビーズの撹拌速
度、仮焼成を経た粉砕物の比面積をそれぞれ前記各範囲
に設定するため、粉砕効率が低下や、焼結体密度および
透磁率の劣化をきたすことなく、酸化物磁性材料を得る
ことができる。According to the method for manufacturing an oxide magnetic material of claims 7 to 9, since the diameter of the medium beads, the stirring speed of the medium beads, and the specific area of the pulverized material after the calcination are respectively set in the respective ranges, An oxide magnetic material can be obtained without lowering the efficiency or lowering the sintered body density and the magnetic permeability.

【００７２】請求項１０のチップ部品の製造方法によれ
ば、媒体ビーズにより粉砕した酸化物磁性材料と内部導
体とを成形して９１０〜９２０℃で焼成するため、焼結
不足になったり、フェライト中に電極材料が拡散するこ
とを防ぎ、電磁気的特性の劣化を防止することができ
る。According to the tenth aspect of the present invention, the oxide magnetic material pulverized by the medium beads and the internal conductor are formed and fired at 910 to 920 ° C., resulting in insufficient sintering or ferrite. It is possible to prevent the electrode material from diffusing therein, and to prevent deterioration of the electromagnetic characteristics.

─────────────────────────────────────────────────────
────────────────────────────────────────────────── ───

【手続補正書】[Procedure amendment]

【提出日】平成１１年１１月８日（１９９９．１１．
８）[Submission date] November 8, 1999 (1999.11.
8)

【手続補正１】[Procedure amendment 1]

【補正対象書類名】明細書[Document name to be amended] Statement

【補正対象項目名】００４８[Correction target item name] 0048

【補正方法】変更[Correction method] Change

【補正内容】[Correction contents]

【００４８】[0048]

【表２】 [Table 2]

【手続補正２】[Procedure amendment 2]

【補正対象書類名】明細書[Document name to be amended] Statement

【補正対象項目名】００５０[Correction target item name] 0050

【補正方法】変更[Correction method] Change

【補正内容】[Correction contents]

【００５０】一方、従来例であるサンプル２０、２１に
おいては、ボール直径と撹拌速度が同じであるサンプル
５の場合と粉砕時間とボールの摩耗量を比較すると、サ
ンプル２０、すなわちステンレス鋼の場合、ＰＳＺ：窒
化珪素＝５０：５０の場合より粉砕時間が短縮され、粉
砕効率は非常に高いが、摩耗量はＰＳＺ：窒化珪素＝５
０：５０の場合に比較して約７３倍と非常に多量であ
る。また、サンプル２１、すなわちチタニアの場合もＰ
ＳＺ：窒化珪素＝５０：５０に比較して約８．２倍の摩
耗量がある。On the other hand, in the conventional samples 20 and 21, when the grinding time and the wear amount of the ball are compared with the case of the sample 5 having the same ball diameter and the stirring speed, the sample 20, that is, the stainless steel, The grinding time is shorter than in the case of PSZ: silicon nitride = 50: 50, the grinding efficiency is very high, but the wear amount is PSZ: silicon nitride = 5.
Compared with the case of 0:50, the amount is about 73 times, which is a very large amount. Also, in the case of sample 21, that is, titania, P
There is about 8.2 times as much wear as SZ: silicon nitride = 50: 50.

【手続補正３】[Procedure amendment 3]

【補正対象書類名】明細書[Document name to be amended] Statement

【補正対象項目名】００５３[Correction target item name] 0053

【補正方法】変更[Correction method] Change

【補正内容】[Correction contents]

【００５３】[0053]

【表３】 [Table 3]

Claims (10)

【特許請求の範囲】[Claims] 【請求項１】Ｆｅ2Ｏ3、ＺｎＯ、ＣｕＯおよびＮｉＯを
主成分とし、この主成分に、全体量に対する含有量が
０．００１〜０．０１１重量％となるＹ2Ｏ3を含み、か
つ０．０３１〜０．１９４重量％となるＺｒＯ2を含
み、かつ０．０１０〜０．０５６重量％となるＳｉを含
むことを特徴とする酸化物磁性材料。[Claim 1] as the main component Fe 2 O 3, ZnO, CuO and NiO, this main component, comprises Y 2 O 3 to the content to the total amount becomes 0.001 to 0.011 wt%, and oxide magnetic material comprising a 0.031 to 0.194 contain by weight percent comprising ZrO 2, and a 0.010 to 0.056 wt% Si. 【請求項２】請求項１の酸化物磁性材料の焼結体を用
い、バルク型コイル部品として構成されていることを特
徴とするチップ部品。2. A chip component comprising a sintered body of the oxide magnetic material according to claim 1 and configured as a bulk type coil component. 【請求項３】請求項１の酸化物磁性材料の焼結体を用
い、かつ焼結体内に導電体層を有して積層型コイル部品
または積層型コイル部品を一部に含んで構成されている
ことを特徴とするチップ部品。3. A laminated coil component or a laminated coil component partially comprising a sintered body of the oxide magnetic material according to claim 1 and having a conductor layer in the sintered body. A chip component characterized by the following. 【請求項４】請求項３において、内部導体がＡｇまたは
ＡｇとＰｄの合金を主成分とすることを特徴とするチッ
プ部品。4. The chip component according to claim 3, wherein the inner conductor is mainly composed of Ag or an alloy of Ag and Pd. 【請求項５】請求項１の酸化物磁性材料を製造する方法
であって、 原料の混合粉砕時および仮焼成を経た材料の粉砕時に湿
式内部循環式のメディア撹拌型ミルを用い、媒体ビーズ
として部分安定化ジルコニアと窒化珪素を使用し、 媒体ビースの摩滅により、酸化物磁性材料内に、全体量
に対する含有量が０．００１〜０．０１１重量％となる
Ｙ2Ｏ3を含み、かつ０．０３〜０．１９４重量％となる
ＺｒＯ2を含み、かつ０．０１０〜０．０５６重量％と
なるＳｉを含有させることを特徴とする酸化物磁性材料
の製造方法。5. A method for producing an oxide magnetic material according to claim 1, wherein a media stirring type mill of a wet internal circulation type is used as a medium bead at the time of mixing and pulverizing a raw material and at the time of pulverizing a material having undergone calcining. moiety using stabilized zirconia and silicon nitride, comprising the attrition media beads, the oxide within the magnetic material, a Y 2 O 3 to the content to the total amount becomes 0.001 to 0.011 wt%, and 0 .03～0.194 comprises by weight percent comprising ZrO 2, and method for producing an oxide magnetic material, characterized by the inclusion of Si as the 0.010 to 0.056 wt%. 【請求項６】請求項５において、 部分安定化ジルコニアビーズおよび窒化珪素ビーズの全
体量に対し、窒化珪素ビーズが、体積比で２０％〜９９
％であることを特徴とする酸化物磁性材料の製造方法。6. The method according to claim 5, wherein the silicon nitride beads have a volume ratio of 20% to 99% based on the total amount of the partially stabilized zirconia beads and silicon nitride beads.
% Of the oxide magnetic material. 【請求項７】請求項５または６の酸化物磁性材料の製造
方法であって、 媒体ビーズとしてその直径が０．２〜５ｍｍのものを使
用することを特徴とする酸化物磁性材料の製造方法。7. The method for producing an oxide magnetic material according to claim 5, wherein the medium beads having a diameter of 0.2 to 5 mm are used. . 【請求項８】請求項５から７までのいずれかの酸化物磁
性材料の製造方法であって、 媒体ビーズの撹拌速度を２．０〜８．０ｍ／ｓとするこ
とを特徴とする酸化物磁性材料の製造方法。8. The method for producing an oxide magnetic material according to claim 5, wherein the stirring speed of the medium beads is 2.0 to 8.0 m / s. Manufacturing method of magnetic material. 【請求項９】請求項５から８までのいずれかの酸化物磁
性材料の製造方法であって、 仮焼成を経た材料から粉砕により比表面積が６．０〜１
５．０ｍ2／ｇの粉体を得ることを特徴とする酸化物磁
性材料の製造方法。9. The method for producing an oxide magnetic material according to claim 5, wherein the specific surface area of the material having undergone calcination is 6.0 to 1 by pulverization.
A method for producing an oxide magnetic material, wherein a powder of 5.0 m 2 / g is obtained. 【請求項１０】請求項３または４のチップ部品の製造方
法であって、 媒体ビーズにより粉砕した酸化物磁性材料と内部導体と
を成形して９１０〜９２０℃で焼成することを特徴とす
るチップ部品の製造方法。10. The method for manufacturing a chip component according to claim 3, wherein the oxide magnetic material pulverized by the medium beads and the internal conductor are formed and fired at 910 to 920 ° C. The method of manufacturing the part.
JP26293599A 1999-08-19 1999-09-17 Oxide magnetic material, manufacture thereof chip parts, and manufacture thereof Pending JP2001085216A (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
JP26293599A JP2001085216A (en) 1999-09-17 1999-09-17 Oxide magnetic material, manufacture thereof chip parts, and manufacture thereof
KR1020000047346A KR100550684B1 (en) 1999-08-19 2000-08-17 Oxide magnetic material and chip part
US09/641,333 US6485840B1 (en) 1999-08-19 2000-08-18 Oxide magnetic material and chip part
TW089116732A TW475184B (en) 1999-08-19 2000-08-18 Oxide magnetic material and chip part
CNB2004100485884A CN1287395C (en) 1999-08-19 2000-08-18 Oxide magnetic material and chip part
CNB001288679A CN1192399C (en) 1999-08-19 2000-08-18 Oxide magnetic material and chip
US10/238,727 US7070732B2 (en) 1999-08-19 2002-09-11 Method for producing an oxide magnetic material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP26293599A JP2001085216A (en) 1999-09-17 1999-09-17 Oxide magnetic material, manufacture thereof chip parts, and manufacture thereof

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Publication Number Publication Date
JP2001085216A true JP2001085216A (en) 2001-03-30

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Country Link
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6852245B2 (en) 2001-04-27 2005-02-08 Tdk Corporation Process for producing granules for being molded into ferrite, granules for being molded into ferrite, green body and sintered body
JP2011096977A (en) * 2009-11-02 2011-05-12 Tdk Corp Ferrite composition, ferrite core, and electronic component
JP2012099662A (en) * 2010-11-02 2012-05-24 Tdk Corp Ferrite composition, ferrite core, and electronic component
JP2012124216A (en) * 2010-12-06 2012-06-28 Tdk Corp Ferrite composition, ferrite core and electronic component

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6852245B2 (en) 2001-04-27 2005-02-08 Tdk Corporation Process for producing granules for being molded into ferrite, granules for being molded into ferrite, green body and sintered body
JP2011096977A (en) * 2009-11-02 2011-05-12 Tdk Corp Ferrite composition, ferrite core, and electronic component
JP2012099662A (en) * 2010-11-02 2012-05-24 Tdk Corp Ferrite composition, ferrite core, and electronic component
JP2012124216A (en) * 2010-12-06 2012-06-28 Tdk Corp Ferrite composition, ferrite core and electronic component

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