JPH11307336A - Manufacture of soft magnetic ferrite - Google Patents

Manufacture of soft magnetic ferrite

Info

Publication number
JPH11307336A
JPH11307336A JP10122979A JP12297998A JPH11307336A JP H11307336 A JPH11307336 A JP H11307336A JP 10122979 A JP10122979 A JP 10122979A JP 12297998 A JP12297998 A JP 12297998A JP H11307336 A JPH11307336 A JP H11307336A
Authority
JP
Japan
Prior art keywords
ferrite
magnetic field
spinel
soft magnetic
type
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.)
Withdrawn
Application number
JP10122979A
Other languages
Japanese (ja)
Inventor
Nobuyuki Hiratsuka
信之 平塚
Ryoichi Aogaki
良一 青柿
Jun Nakagawa
準 中川
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 JP10122979A priority Critical patent/JPH11307336A/en
Publication of JPH11307336A publication Critical patent/JPH11307336A/en
Withdrawn legal-status Critical Current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)
  • Magnetic Ceramics (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

PROBLEM TO BE SOLVED: To improve the drop of magnetic permeability in a high frequency area, by heat-treating spinel-type ferrite containing at least nickel oxide, and containing at least one type of Co, Ba and Sr in a magnetic field. SOLUTION: At least one type of Co, Ba and Sr is added to a temporarily baked object containing at least nickel oxide and it is baked. Then, spinel-type ferrite is formed. At that time, the content of CO, Ba and Sr is reduced to CoO, BaFe12 O19 and SrFe12 O19 and about 0.1-about 10 weight % in total is obtained. Spinel-type ferrite is heat-treated in a magnetic field and a face (111) is preferentially oriented. Spinel-type ferrite contains zinc oxide. The drop of magnetic permeability in a high frequency area is improved, the use limit frequency of ferrite containing nickel is extended and the use of ferrite at about 100 MHz is realized.

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、高周波用軟磁性フ
ェライトの製造方法に関する。[0001] The present invention relates to a method for producing a soft magnetic ferrite for high frequency.

【０００２】[0002]

【従来の技術】フェライトは、渦電流損失が金属に比べ
著しく小さいため、高周波用磁心に適している。しか
し、フェライトには磁気共鳴による限界周波数（Snoek
の限界）が存在し、この限界周波数を超えると透磁率が
急激に低下すると共に損失が急激に増大して、使用不可
能となる。高周波用フェライトとしては、Ｎｉ−Ｚｎフ
ェライト等のＮｉ系スピネル型フェライトが利用される
ことが多く、特に、Ｎｉ−Ｚｎフェライトは、透磁率が
比較的高いことから多用されている。しかし、Ｎｉ−Ｚ
ｎフェライトの限界周波数は１００MHz未満であり、近
年の電気・電子機器における使用周波数の高周波化に伴
い、より高周波で使用可能とすることが望まれている。2. Description of the Related Art Ferrite is suitable for high frequency magnetic cores because eddy current loss is significantly smaller than that of metal. However, the limit frequency (Snoek
When this limit frequency is exceeded, the magnetic permeability decreases rapidly and the loss increases sharply, making it unusable. As the high-frequency ferrite, Ni-based spinel type ferrite such as Ni-Zn ferrite is often used, and in particular, Ni-Zn ferrite is frequently used because of its relatively high magnetic permeability. However, Ni-Z
The limit frequency of n-ferrite is less than 100 MHz, and it is desired to be able to use it at a higher frequency with the recent increase in the frequency used in electric and electronic devices.

【０００３】[0003]

【発明が解決しようとする課題】本発明の目的は、Ｎｉ
系スピネル型フェライトの限界周波数を向上させること
であり、特に、Ｎｉ−Ｚｎフェライトを１００MHz以上
の高周波領域で使用可能とすることである。SUMMARY OF THE INVENTION An object of the present invention is to provide Ni
The purpose is to improve the critical frequency of the spinel-type ferrite, and in particular, to make Ni-Zn ferrite usable in a high frequency region of 100 MHz or more.

【０００４】[0004]

【課題を解決するための手段】上記目的は、下記（１）
〜（５）のいずれかの構成により達成される。 （１） 少なくとも酸化ニッケルを含有し、Ｃｏ、Ｂａ
およびＳｒの少なくとも１種を含有するスピネル型フェ
ライトを、磁場中で熱処理する工程を有する軟磁性フェ
ライトの製造方法。 （２） 前記スピネル型フェライトが、Ｃｏ、Ｂａおよ
びＳｒの少なくとも１種を、それぞれＣｏＯ、ＢａＦｅ
12Ｏ19およびＳｒＦｅ12Ｏ19に換算して合計で０．１〜
１０重量％含有する上記（１）の軟磁性フェライトの製
造方法。 （３） 前記スピネル型フェライトが、少なくとも酸化
ニッケルを含有する仮焼物に、酸化コバルト、Ｂａフェ
ライトおよびＳｒフェライトの少なくとも１種を添加し
て焼成することにより製造されたものである上記（１）
または（２）の軟磁性フェライトの製造方法。 （４） 磁場中での熱処理により（１１１）面を優先的
に配向させる上記（１）〜（３）のいずれかの軟磁性フ
ェライトの製造方法。 （５） 前記スピネル型フェライトが、酸化亜鉛を含有
する上記（１）〜（４）のいずれかの軟磁性フェライト
の製造方法。The above object is achieved by the following (1).
This is achieved by any one of the above configurations (5) to (5). (1) Co, Ba containing at least nickel oxide
A method for producing a soft magnetic ferrite, comprising a step of heat-treating a spinel ferrite containing at least one of Sr and Sr in a magnetic field. (2) The spinel-type ferrite contains at least one of Co, Ba and Sr as CoO and BaFe, respectively.
Converted to 12 O 19 and SrFe 12 O 19 ,
The method for producing a soft magnetic ferrite according to the above (1) containing 10% by weight. (3) The spinel-type ferrite is produced by adding at least one of cobalt oxide, Ba ferrite, and Sr ferrite to a calcined product containing at least nickel oxide, followed by firing.
Or (2) the method for producing a soft magnetic ferrite. (4) The method for producing a soft magnetic ferrite according to any one of (1) to (3), wherein the (111) plane is preferentially oriented by heat treatment in a magnetic field. (5) The method for producing a soft magnetic ferrite according to any one of (1) to (4), wherein the spinel-type ferrite contains zinc oxide.

【０００５】[0005]

【発明の実施の形態】本発明では、少なくとも酸化ニッ
ケルを含有し、Ｃｏ、ＢａおよびＳｒの少なくとも１種
を含有するスピネル型フェライトに、磁場中で熱処理を
施す。この磁場中での熱処理により、高周波域における
透磁率の落ち込みが改善されて周波数特性が良好とな
り、例えばＮｉ−Ｚｎフェライトでは１００MHzにおい
て実用上十分な透磁率が得られる。なお、Ｎｉ−Ｚｎフ
ェライトでは、ＣｏＯの添加により磁場中熱処理なしで
も１００MHzにおいて５０前後の透磁率が得られること
もあるが、この場合、１００MHz近傍において磁気共鳴
が発生し、透磁率は不安定になるため、実用に供するこ
とはできない。これに対し本発明をＮｉ−Ｚｎフェライ
トに適用した場合、透磁率は１００MHz付近においても
ほぼ一定であるため、このような問題は生じない。DESCRIPTION OF THE PREFERRED EMBODIMENTS In the present invention, a heat treatment is performed in a magnetic field on a spinel ferrite containing at least nickel oxide and containing at least one of Co, Ba and Sr. By the heat treatment in this magnetic field, the drop in the magnetic permeability in a high-frequency range is improved and the frequency characteristics are improved. For example, in the case of Ni-Zn ferrite, a practically sufficient magnetic permeability is obtained at 100 MHz. In addition, in the case of Ni—Zn ferrite, a magnetic permeability of about 50 can be obtained at 100 MHz without heat treatment in a magnetic field by adding CoO. In this case, magnetic resonance occurs near 100 MHz and the magnetic permeability becomes unstable. Therefore, it cannot be put to practical use. On the other hand, when the present invention is applied to Ni—Zn ferrite, such a problem does not occur because the magnetic permeability is substantially constant even near 100 MHz.

【０００６】磁場中熱処理の際の具体的条件は、フェラ
イトの組成等に応じて適宜決定すればよいが、一般に、
磁場強度は好ましくは１０Oe以上、より好ましくは１kO
e以上であり、到達温度は好ましくは３００℃以上、よ
り好ましくは５００℃以上である。磁場強度が低すぎて
も、到達温度が低すぎても、磁場中熱処理による効果が
不十分となる。また、上記到達温度に保持する時間は特
に限定されず、加熱対象物のフェライト全体が均一な温
度となるように、フェライトの寸法に応じて適宜決定す
ればよいが、通常、１分間〜５時間程度とすることが好
ましい。また、冷却速度は、好ましくは３０〜２００℃
/時間、より好ましくは５０〜１００℃/時間である。本
発明の効果は、磁場を印加しながら冷却することで、フ
ェライト中の磁気イオンが熱振動しながら再配列するこ
とにより実現するので、冷却速度が速すぎると、再配列
に利用できる時間が短くなり、十分な効果が得られな
い。一方、冷却速度が遅すぎると、フェライトの熱分解
が促進されることもあり、かつ、処理に長時間を要して
効率が低下するので、好ましくない。なお、本発明にお
いて用いる磁場強度の上限は特にないが、量産に使用可
能な現在の磁場発生装置では、通常、上限は１００kOe
程度である。また、到達温度は、通常、６００℃以下で
あることが好ましい。到達温度が高すぎると、フェライ
トが熱分解され、磁気特性が劣化する可能性が高まる。
熱処理は大気中、あるいは、窒素やアルゴン等の不活性
雰囲気中で行うことが好ましい。The specific conditions for the heat treatment in a magnetic field may be appropriately determined according to the composition of the ferrite and the like.
The magnetic field strength is preferably at least 10 Oe, more preferably 1 kO
e or more, and the ultimate temperature is preferably 300 ° C. or more, more preferably 500 ° C. or more. If the magnetic field strength is too low or the temperature reached is too low, the effect of the heat treatment in the magnetic field becomes insufficient. Further, the time for maintaining the above-mentioned temperature is not particularly limited, and may be appropriately determined according to the size of the ferrite so that the entire ferrite of the object to be heated has a uniform temperature, but is usually 1 minute to 5 hours. It is preferable to set the degree. The cooling rate is preferably 30 to 200 ° C.
/ Hour, more preferably 50 to 100 ° C / hour. The effect of the present invention is realized by cooling while applying a magnetic field, whereby the magnetic ions in the ferrite are rearranged while thermally oscillating.If the cooling rate is too high, the time available for rearrangement is short. And a sufficient effect cannot be obtained. On the other hand, if the cooling rate is too slow, the thermal decomposition of ferrite may be promoted, and the treatment takes a long time to lower the efficiency, which is not preferable. Although there is no particular upper limit on the magnetic field strength used in the present invention, the upper limit is usually 100 kOe in current magnetic field generators that can be used for mass production.
It is about. In addition, the ultimate temperature is usually preferably 600 ° C. or lower. If the attained temperature is too high, ferrite is thermally decomposed and the possibility of deteriorating magnetic properties increases.
The heat treatment is preferably performed in the air or in an inert atmosphere such as nitrogen or argon.

【０００７】磁場中熱処理による透磁率の周波数特性の
改善は、一軸異方性の付与によるものと考えられる。例
えば、Ｘ線回折による分析では、磁場中熱処理によって
（１１１）面が優先配向することが確認できる。It is considered that the improvement of the frequency characteristic of the magnetic permeability by the heat treatment in a magnetic field is due to the provision of uniaxial anisotropy. For example, in the analysis by X-ray diffraction, it can be confirmed that the (111) plane is preferentially oriented by the heat treatment in the magnetic field.

【０００８】本発明のスピネル型フェライトにおいて、
Ｃｏ、ＢａおよびＳｒの含有量は、それぞれをＣｏＯ、
ＢａＦｅ12Ｏ19およびＳｒＦｅ12Ｏ19に換算して合計で
０．１〜１０重量％であることが好ましく、０．５〜８
重量％であることがより好ましい。これらの元素の含有
量が少なすぎると本発明の効果が不十分となり、含有量
が多すぎると透磁率が低下してしまう。In the spinel type ferrite of the present invention,
The contents of Co, Ba and Sr are respectively CoO,
The total amount is preferably 0.1 to 10% by weight in terms of BaFe 12 O 19 and SrFe 12 O 19 , and 0.5 to 8% by weight.
More preferably, it is% by weight. If the content of these elements is too small, the effect of the present invention will be insufficient, and if the content is too large, the magnetic permeability will decrease.

【０００９】Ｃｏ、ＢａおよびＳｒをスピネル型フェラ
イトに含有させるためには、スピネル型フェライトの製
造工程においてこれらの元素の化合物（以下、添加化合
物という）を添加する。添加化合物としては酸化物が好
ましく、特に、酸化コバルト、ＢａフェライトおよびＳ
ｒフェライトが好ましい。これらの酸化物を用いること
により、本発明の効果は著しく向上する。酸化コバルト
はＣｏＯ、ＢａフェライトはＢａＦｅ12Ｏ19、Ｓｒフェ
ライトはＳｒＦｅ12Ｏ19が化学量論組成であるが、添加
化合物の組成は化学量論組成から偏倚していてもよい。In order to include Co, Ba and Sr in the spinel ferrite, a compound of these elements (hereinafter referred to as an additive compound) is added in the process of producing the spinel ferrite. As the additive compound, an oxide is preferable, and in particular, cobalt oxide, Ba ferrite and S
r Ferrite is preferred. By using these oxides, the effects of the present invention are significantly improved. The stoichiometric composition of cobalt oxide is CoO, the Ba ferrite is BaFe 12 O 19 , and the Sr ferrite is SrFe 12 O 19, but the composition of the additive compound may deviate from the stoichiometric composition.

【００１０】本発明が適用されるスピネル型フェライト
は、少なくとも酸化ニッケルを含有するものである。こ
のようなスピネル型フェライトとしては、Ｎｉフェライ
ト、Ｎｉ−Ｚｎフェライト、Ｎｉ−Ｃｕフェライト、Ｎ
ｉ−Ｃｕ−Ｚｎフェライトなどが好ましく、これらのう
ちでは、酸化亜鉛を含有するもの、特にＮｉ−Ｚｎフェ
ライトが好ましい。本発明を適用する場合、各フェライ
トの具体的な主組成は特に限定されず、通常利用される
組成範囲から適宜選択すればよい。例えば、Ｎｉ−Ｚｎ
フェライトの主組成は、通常、酸化鉄がＦｅ2Ｏ3 換算
で４５〜５５mol％程度、酸化亜鉛がＺｎＯ換算で１０
〜３５mol％程度、酸化ニッケルがＮｉＯ換算で１５〜
３５mol％程度である。また、各フェライトには、特性
向上のために各種副成分が添加されるが、本発明におい
ても従来公知の各種副成分を含んでいてよく、また、通
常含まれる不可避的不純物を含んでいてよい。例えば、
Ｎｉ−Ｚｎフェライトにおける副成分ないし不純物とし
ては、酸化カルシウム、酸化ビスマス、酸化アルミニウ
ム、酸化ケイ素、酸化クロム等が挙げられる。The spinel-type ferrite to which the present invention is applied contains at least nickel oxide. Such spinel ferrites include Ni ferrite, Ni-Zn ferrite, Ni-Cu ferrite, and N
i-Cu-Zn ferrite and the like are preferable, and among these, those containing zinc oxide, particularly Ni-Zn ferrite, are preferable. When the present invention is applied, the specific main composition of each ferrite is not particularly limited, and may be appropriately selected from a commonly used composition range. For example, Ni-Zn
The main composition of the ferrite is usually about 45～55Mol% in iron oxide in terms of Fe 2 O 3, zinc oxide in terms of ZnO 10
~ 35mol%, nickel oxide is 15 ~
It is about 35 mol%. In addition, various subcomponents are added to each ferrite in order to improve the properties, and the present invention may also include various conventionally known subcomponents, and may also include unavoidable impurities that are usually included. . For example,
Examples of subcomponents or impurities in the Ni-Zn ferrite include calcium oxide, bismuth oxide, aluminum oxide, silicon oxide, and chromium oxide.

【００１１】本発明により製造されるスピネル型フェラ
イトの平均結晶粒径は特に限定されず、Ｃｏ、Ｂａ、Ｓ
ｒを添加しない場合と同等、例えば１〜３０μm程度で
あればよい。なお、製造条件がほぼ同じであっても、Ｃ
ｏ、Ｂａ、Ｓｒの添加により結晶粒径が影響を受けるこ
とがある。例えば、Ｎｉ−ＺｎフェライトにＣｏＯを添
加した場合、添加量が５重量％程度であると無添加の場
合よりも結晶粒径が大きくなるが、添加量が１０重量％
程度であると、添加量が５重量％の場合よりも結晶粒径
は小さくなる。このように粒成長が抑えられるのは、Ｃ
ｏＯが許容される固溶量を超えることにより、結晶粒界
に偏析しやすくなるためであると考えられる。The average crystal grain size of the spinel-type ferrite produced according to the present invention is not particularly limited, and Co, Ba, S
It may be equivalent to the case where r is not added, for example, about 1 to 30 μm. Note that even if the manufacturing conditions are almost the same,
The crystal grain size may be affected by the addition of o, Ba, and Sr. For example, when CoO is added to Ni-Zn ferrite, when the addition amount is about 5% by weight, the crystal grain size becomes larger than when it is not added, but the addition amount is 10% by weight.
When the amount is about 5%, the crystal grain size becomes smaller than when the addition amount is 5% by weight. The reason why grain growth is suppressed in this way is that C
It is considered that when oO exceeds the allowable solid solution amount, segregation at crystal grain boundaries is likely to occur.

【００１２】次に、本発明の製造方法の具体的な流れを
説明する。Next, a specific flow of the manufacturing method of the present invention will be described.

【００１３】まず、主成分原料を、焼成後に所定の組成
が得られるように混合する。主成分原料としては、例え
ばＮｉ−Ｚｎフェライトでは、通常、酸化鉄（Ｆｅ
2Ｏ3）粉末、酸化ニッケル（ＮｉＯ）粉末および酸化亜
鉛（ＺｎＯ）粉末を用いるが、これらの酸化物のほか、
焼成により酸化物となる化合物、例えば、炭酸塩、水酸
化物、硝酸塩等を用いることもできる。混合には、湿式
混合法を利用することが好ましい。First, the main component materials are mixed so as to obtain a predetermined composition after firing. As a main component material, for example, in the case of Ni—Zn ferrite, iron oxide (Fe
2 O 3 ) powder, nickel oxide (NiO) powder and zinc oxide (ZnO) powder are used. In addition to these oxides,
Compounds that become oxides by firing, such as carbonates, hydroxides, and nitrates, can also be used. It is preferable to use a wet mixing method for the mixing.

【００１４】次いで、混合した原料を仮焼する。仮焼に
際し、温度や雰囲気等の各種条件は、主組成に応じた最
適なものを選択すればよい。例えば、Ｎｉ−Ｚｎフェラ
イトでは、空気中や酸素分圧を制御した雰囲気中におい
て、８００〜１２００℃程度で、１〜１０時間程度仮焼
すればよい。Next, the mixed raw materials are calcined. In calcination, various conditions such as temperature and atmosphere may be selected to be optimal according to the main composition. For example, Ni-Zn ferrite may be calcined at about 800 to 1200 ° C. for about 1 to 10 hours in air or an atmosphere in which the oxygen partial pressure is controlled.

【００１５】次いで、仮焼物を粉砕する。この粉砕は、
湿式で行うことが好ましい。仮焼物の粉砕は、仮焼物の
平均１次粒径が、０．５〜１．５μm程度となるまで行
うことが好ましい。Next, the calcined product is pulverized. This crushing
It is preferable to carry out by a wet method. The pulverization of the calcined product is preferably performed until the average primary particle size of the calcined product becomes about 0.5 to 1.5 μm.

【００１６】本発明では、添加化合物を仮焼前に添加し
てもよいが、より高い効果を得るためには、仮焼物に添
加することが好ましい。添加化合物を仮焼後に添加する
場合、添加化合物を仮焼物に添加して両者を粉砕・混合
してもよく、仮焼物粉砕後に添加化合物を添加して、粉
砕・混合してもよい。いずれの場合も、粉砕・混合は湿
式で行うことが好ましい。なお、添加化合物は、平均粒
径が１〜１００μm程度となるまで粉砕されることが好
ましい。In the present invention, the additive compound may be added before calcining, but it is preferable to add the compound to the calcined material in order to obtain a higher effect. When the additive compound is added after calcining, the additive compound may be added to the calcined material and both may be pulverized and mixed, or the additional compound may be added after pulverizing the calcined material and pulverized and mixed. In any case, the pulverization and mixing are preferably performed by a wet method. In addition, it is preferable that the additive compound is pulverized until the average particle diameter becomes about 1 to 100 μm.

【００１７】仮焼後、所定の形状に成形し、得られた成
形体を焼成する。焼成に際しても、温度や雰囲気等の各
種条件は、主組成に応じた最適なものを選択すればよ
い。例えば、Ｎｉ−Ｚｎフェライトでは、空気中や酸素
分圧を制御した雰囲気中において、１０００〜１３５０
℃程度で、１〜１０時間程度焼成すればよい。After calcination, it is formed into a predetermined shape, and the obtained molded body is fired. In firing, various conditions such as temperature and atmosphere may be selected to be optimal according to the main composition. For example, in the case of Ni-Zn ferrite, 1000-1350 in air or an atmosphere in which the oxygen partial pressure is controlled.
What is necessary is just to bake at about ℃ for about 1 to 10 hours.

【００１８】本発明により製造される軟磁性フェライト
の用途は特に限定されないが、例えば、高周波用磁心、
マイクロ波用材料などに好適である。The use of the soft magnetic ferrite produced according to the present invention is not particularly limited.
Suitable for microwave materials and the like.

【００１９】[0019]

【実施例】主成分原料として、Ｆｅ2Ｏ3粉末、ＺｎＯ粉
末およびＮｉＯ粉末を用意し、これらを、焼成後の組成
がＮｉ0.3Ｚｎ0.7Ｆｅ2Ｏ4となるように秤量し、ボール
ミルにより１０時間湿式混合した。得られた混合物を空
気中において１１５０℃で５時間仮焼し、仮焼物をボー
ルにより２４時間湿式粉砕した。EXAMPLE An Fe 2 O 3 powder, a ZnO powder and a NiO powder were prepared as main component raw materials, and these were weighed so that the composition after sintering would be Ni 0.3 Zn 0.7 Fe 2 O 4. Wet mixed for hours. The obtained mixture was calcined in air at 1150 ° C. for 5 hours, and the calcined product was wet-pulverized with a ball for 24 hours.

【００２０】次いで、粉砕物に、添加化合物としてＣｏ
Ｏ粉末、ＢａＦｅ12Ｏ19粉末またはＳｒＦｅ12Ｏ19粉末
を添加し、ボールミルにより３時間湿式混合した。各添
加化合物の添加量を下記表１に示す。Then, Co was added to the pulverized material as an additive compound.
O powder, BaFe 12 O 19 powder or SrFe 12 O 19 powder was added and wet-mixed for 3 hours by a ball mill. Table 1 below shows the addition amounts of each additive compound.

【００２１】次いで、仮焼物と添加化合物との混合物を
湿式成形し、トロイダル状の成形体を得た。Next, the mixture of the calcined product and the additive compound was subjected to wet molding to obtain a toroidal molded body.

【００２２】次いで、成形体を、空気中において１１５
０℃で５時間焼成し、外径１８mm、内径１２mm、高さ５
mmのトロイダル状焼結体磁心サンプルを得た。Next, the molded body is placed in air for 115 minutes.
Bake at 0 ° C for 5 hours, outer diameter 18mm, inner diameter 12mm, height 5
A toroidal sintered compact magnetic core sample of mm was obtained.

【００２３】各サンプルに対し、５０MHzおよび１００M
Hzにおける初透磁率を測定した。測定には、ベクトルイ
ンピーダンスメータを用いた。次いで、各サンプルに対
し、磁場中熱処理を施した。処理は空気中で行い、磁場
強度は５０kOe、到達温度は６００℃、温度保持時間は
１時間、冷却速度は６０℃／時間とした。なお、印加し
た磁場の方向は、トロイダル状サンプルの径方向に垂直
（サンプルの軸方向）とした。この磁場中熱処理後に、
再び初透磁率を測定した。測定結果を表１に示す。For each sample, 50 MHz and 100 M
The initial permeability at Hz was measured. A vector impedance meter was used for the measurement. Next, each sample was subjected to a heat treatment in a magnetic field. The treatment was performed in air, the magnetic field strength was 50 kOe, the reached temperature was 600 ° C., the temperature holding time was 1 hour, and the cooling rate was 60 ° C./hour. The direction of the applied magnetic field was perpendicular to the radial direction of the toroidal sample (the axial direction of the sample). After this heat treatment in a magnetic field,
The initial magnetic permeability was measured again. Table 1 shows the measurement results.

【００２４】[0024]

【表１】 [Table 1]

【００２５】表１から、本発明の効果が明らかである。
すなわち、添加化合物を含まないサンプルNo.１は、磁
場中熱処理の有無によらず５０MHzにおいても実用的な
初透磁率が得られず、また、添加化合物を含むサンプル
でも磁場中熱処理なしでは１００MHzにおいて実用的な
初透磁率が得られないのに対し、添加化合物を含むサン
プルを磁場中熱処理した場合には、１００MHzにおいて
十分に高い初透磁率が得られることがわかる。なお、表
１に示す本発明サンプルは、１００MHz付近に共鳴周波
数が存在するために初透磁率が高くなったのではなく、
初透磁率は１００MHzの前後でほぼ一定であった。特
に、ＣｏＯを添加したサンプルでは、５０MHzから１０
０MHzの範囲で初透磁率の低下が小さく、磁場中熱処理
による効果が大きいことがわかる。From Table 1, the effect of the present invention is clear.
That is, in Sample No. 1 containing no additive compound, a practical initial magnetic permeability was not obtained even at 50 MHz regardless of the presence or absence of heat treatment in a magnetic field. While practical initial permeability cannot be obtained, a sufficiently high initial permeability can be obtained at 100 MHz when the sample containing the additive compound is heat-treated in a magnetic field. In addition, the sample of the present invention shown in Table 1 did not have an increased initial permeability due to the presence of a resonance frequency near 100 MHz.
The initial permeability was almost constant around 100 MHz. In particular, in the case of the sample to which CoO is added, 10 MHz to 10 MHz
It can be seen that the decrease in the initial magnetic permeability is small in the range of 0 MHz, and the effect of the heat treatment in the magnetic field is large.

【００２６】表１に示されるサンプルNo.５について、
磁場中熱処理が結晶配向に与える影響を調べるために、
Ｘ線回折による分析を行った。なお、Ｘ線は、サンプル
の上面から入射させた。サンプルNo.５のＸ線回折チャ
ートを図１に示す。図１に「横磁界」として示すチャー
トは、磁場中熱処理の際の磁場印加方向をサンプルの径
方向とした場合のものであり、「縦磁界」として示すチ
ャートは、磁場中熱処理の際の磁場印加方向をサンプル
の軸方向とした場合のものである。For sample No. 5 shown in Table 1,
To investigate the effect of heat treatment in a magnetic field on crystal orientation,
Analysis by X-ray diffraction was performed. Note that X-rays were incident from the upper surface of the sample. An X-ray diffraction chart of Sample No. 5 is shown in FIG. The chart shown as “transverse magnetic field” in FIG. 1 is a case where the magnetic field application direction during the heat treatment in the magnetic field is the radial direction of the sample, and the chart shown as “longitudinal magnetic field” is the magnetic field during the heat treatment in the magnetic field. This is a case where the application direction is the axial direction of the sample.

【００２７】図１から、縦磁界での磁場中熱処理によ
り、（１１１）面およびこれと等価な面の反射ピークが
大きくなっていることが明瞭にわかる。したがって、磁
場中熱処理により、（１１１）面が優先的に配向したこ
とがわかる。FIG. 1 clearly shows that the heat treatment in a magnetic field with a vertical magnetic field increases the reflection peaks of the (111) plane and the equivalent plane. Therefore, it is understood that the (111) plane was preferentially oriented by the heat treatment in the magnetic field.

【００２８】[0028]

【発明の効果】本発明によれば、Ｎｉ含有フェライトの
使用限界周波数が延び、特に、Ｎｉ−Ｚｎフェライトで
は、従来使用不可能であった１００MHzでの使用が可能
となる。According to the present invention, the usable limit frequency of Ni-containing ferrite is extended, and in particular, Ni-Zn ferrite can be used at 100 MHz, which has not been conventionally used.

【図面の簡単な説明】[Brief description of the drawings]

【図１】磁場中熱処理によるＮｉ−Ｚｎフェライトの結
晶配向変化を示すＸ線回折チャートである。FIG. 1 is an X-ray diffraction chart showing a change in crystal orientation of Ni—Zn ferrite by heat treatment in a magnetic field.

Claims (5)

【特許請求の範囲】[Claims] 【請求項１】 少なくとも酸化ニッケルを含有し、Ｃ
ｏ、ＢａおよびＳｒの少なくとも１種を含有するスピネ
ル型フェライトを、磁場中で熱処理する工程を有する軟
磁性フェライトの製造方法。Claims: 1. A composition comprising at least nickel oxide,
A method for producing a soft magnetic ferrite, comprising a step of heat-treating a spinel-type ferrite containing at least one of o, Ba and Sr in a magnetic field. 【請求項２】 前記スピネル型フェライトが、Ｃｏ、Ｂ
ａおよびＳｒの少なくとも１種を、それぞれＣｏＯ、Ｂ
ａＦｅ12Ｏ19およびＳｒＦｅ12Ｏ19に換算して合計で
０．１〜１０重量％含有する請求項１の軟磁性フェライ
トの製造方法。2. The method according to claim 1, wherein the spinel ferrite is Co, B
at least one of a and Sr is CoO, B
aFe 12 O 19 and SrFe 12 manufacturing method of a soft magnetic ferrite according to claim 1, in terms of O 19 containing 0.1 to 10 wt% in total. 【請求項３】 前記スピネル型フェライトが、少なくと
も酸化ニッケルを含有する仮焼物に、酸化コバルト、Ｂ
ａフェライトおよびＳｒフェライトの少なくとも１種を
添加して焼成することにより製造されたものである請求
項１または２の軟磁性フェライトの製造方法。3. A method according to claim 1, wherein the calcined material containing at least nickel oxide contains cobalt oxide,
The method for producing a soft magnetic ferrite according to claim 1 or 2, wherein the method is produced by adding at least one of a ferrite and Sr ferrite and calcining. 【請求項４】 磁場中での熱処理により（１１１）面を
優先的に配向させる請求項１〜３のいずれかの軟磁性フ
ェライトの製造方法。4. The method for producing a soft magnetic ferrite according to claim 1, wherein the (111) plane is preferentially oriented by heat treatment in a magnetic field. 【請求項５】 前記スピネル型フェライトが、酸化亜鉛
を含有する請求項１〜４のいずれかの軟磁性フェライト
の製造方法。5. The method for producing a soft magnetic ferrite according to claim 1, wherein said spinel-type ferrite contains zinc oxide.
JP10122979A 1998-04-16 1998-04-16 Manufacture of soft magnetic ferrite Withdrawn JPH11307336A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10122979A JPH11307336A (en) 1998-04-16 1998-04-16 Manufacture of soft magnetic ferrite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10122979A JPH11307336A (en) 1998-04-16 1998-04-16 Manufacture of soft magnetic ferrite

Publications (1)

Publication Number Publication Date
JPH11307336A true JPH11307336A (en) 1999-11-05

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ID=14849317

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6893581B2 (en) 2002-02-01 2005-05-17 Sanyo Electric Co., Ltd. Composite magnetic material and a method for producing the same
KR100725546B1 (en) 2006-02-22 2007-06-08 요업기술원 Magnetic material for magnetic core and the manufacturing method thereof
JP2010076989A (en) * 2008-09-26 2010-04-08 Dowa Electronics Materials Co Ltd Soft magnetic ferrite particle and method for producing the same
JP2012076955A (en) * 2010-09-30 2012-04-19 Dowa Electronics Materials Co Ltd Ferrite particle, and electrophotographic developing carrier and electrophotographic developer using the same
CN109867517A (en) * 2019-03-28 2019-06-11 天通控股股份有限公司 A kind of WPC and NFC dual-purpose high-frequency high-magnetic-permeability low-loss nickel-zinc ferrite and preparation method thereof
CN113816734A (en) * 2021-10-08 2021-12-21 横店集团东磁股份有限公司 NiCuZn ferrite material and preparation method and application thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6893581B2 (en) 2002-02-01 2005-05-17 Sanyo Electric Co., Ltd. Composite magnetic material and a method for producing the same
US7101489B2 (en) 2002-02-01 2006-09-05 Sanyo Electric Co., Ltd. Composite magnetic material and a method for producing the same
KR100725546B1 (en) 2006-02-22 2007-06-08 요업기술원 Magnetic material for magnetic core and the manufacturing method thereof
JP2010076989A (en) * 2008-09-26 2010-04-08 Dowa Electronics Materials Co Ltd Soft magnetic ferrite particle and method for producing the same
JP2012076955A (en) * 2010-09-30 2012-04-19 Dowa Electronics Materials Co Ltd Ferrite particle, and electrophotographic developing carrier and electrophotographic developer using the same
CN109867517A (en) * 2019-03-28 2019-06-11 天通控股股份有限公司 A kind of WPC and NFC dual-purpose high-frequency high-magnetic-permeability low-loss nickel-zinc ferrite and preparation method thereof
CN113816734A (en) * 2021-10-08 2021-12-21 横店集团东磁股份有限公司 NiCuZn ferrite material and preparation method and application thereof

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