JPH0143719B2 - - Google Patents

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Publication number
JPH0143719B2
JPH0143719B2 JP59053230A JP5323084A JPH0143719B2 JP H0143719 B2 JPH0143719 B2 JP H0143719B2 JP 59053230 A JP59053230 A JP 59053230A JP 5323084 A JP5323084 A JP 5323084A JP H0143719 B2 JPH0143719 B2 JP H0143719B2
Authority
JP
Japan
Prior art keywords
ferrite
single crystal
polycrystalline
crystal
producing
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.)
Expired
Application number
JP59053230A
Other languages
Japanese (ja)
Other versions
JPS60195096A (en
Inventor
Haruo Tomita
Katsuaki Myake
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.)
NGK Insulators Ltd
Original Assignee
NGK Insulators Ltd
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 NGK Insulators Ltd filed Critical NGK Insulators Ltd
Priority to JP59053230A priority Critical patent/JPS60195096A/en
Publication of JPS60195096A publication Critical patent/JPS60195096A/en
Publication of JPH0143719B2 publication Critical patent/JPH0143719B2/ja
Granted legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B1/00—Single-crystal growth directly from the solid state
    • C30B1/02—Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/24—Complex oxides with formula AMeO3, wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. ortho ferrites

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Description

【発明の詳細な説明】[Detailed description of the invention]

本発明は、VTR磁気ヘツド等に用いられる単
結晶フエライトの製造法に関するものであり、さ
らに詳しくは、多結晶フエライト単結晶フエライ
トとを接触後加熱することにより、単結晶フエラ
イトを多結晶フエライト方向に結晶成長させて単
結晶フエライトを育成するフエライト単結晶の製
造法に関するものである。 従来、単結晶フエライトの製造法としては原料
を溶融点以上の高温で溶融した液相より単結晶を
育成するブリツヂマン法が知られている。しかし
ながら溶融した液相より単結晶を育生するブリツ
ヂマン法は、1600℃以上の高温を必要とするた
め、特に酸化亜鉛のような高温において極めて飛
散しやすい原料を使用する単結晶フエライトの製
造の場合には、製品中の組成変動が生じ易くまた
原料の溶融に使用する容器等から不純物が混入し
易いので、得られる単結晶の結晶性が一様でない
欠点があつた。さらにブリツヂマン法は高価で複
雑かつ大型の製造装置を必要とし、また製造の際
の加熱条件、種単結晶の生成条件等を正確に制御
することが困難であるので、量産性に乏しく、従
つて得られる単結晶フエライト製品が高価となる
等の問題点があつた。 上述した不具合を解消するため、本願人は特開
昭56−155100号において、固相反応によるフエラ
イト単結晶の製造法を提案した。しかしながら、
この方法では、母多結晶材と種単結晶とを鏡面研
磨仕上げした後、接合しているが、研磨後の接合
面の研削傷痕は任意な方向であつた。このような
傷痕を任意に形成させた接合体を加熱すると、研
削傷痕により加工歪が緩和される時点で微少な変
形を生じ、密着接合面が離脱し多結晶体の単結晶
化が阻害される欠点があつた。 本発明の目的は上述した不具合を解消して、研
磨時における研磨方向を一定にして密着接合面の
離脱を最小とすることにより、収率良く安価に単
結晶フエライトを得る製造法を提供しようとする
ものである。 さらに他の目的は、寸法が大きい単結晶フエラ
イトの製造法を提供しようとするものである。 本発明は多結晶フエライトと単結晶フエライト
とを接触後加熱するとにより、単結晶フエライト
を多結晶フエライト方向に結晶成長させて単結晶
フエライトを育成するフエライト単結晶の製造法
において、多結晶フエライトおよび単結晶フエラ
イトの接合面をそれぞれ鏡面に研磨するととも
に、少なくとも単結晶フエライトの鏡面研磨面の
研磨方向をそろえて実施することを特徴とするも
のである。 以下、本発明を図面を参照して詳細に説明す
る。 第1図A〜Cは本発明の製造方法の一実施例を
説明するための斜視図で、Mn−Znフエライトを
使用し形状が直方体の例を示している。まず第1
図Aに示すように、Mn−Znよりなる多結晶フエ
ライト2および同材質よりなる種単結晶フエライ
ト1,3を準備する。この多結晶フエライトとし
ては、酸化鉄の原料にスピネル構造を有する酸化
鉄またはスピネル構造の履歴を有する酸化鉄ある
いはそれらの混合物より成る酸化鉄を用いて製造
した多結晶フエライトを用いる必要がある。ま
た、多結晶フエライトと単結晶フエライトの熱膨
張係数の差は±10×10-7以下が望ましい。 上述したフエライトの組成としては好ましくは Fe2O3 45−55モル% MnO 20−40モル% ZnO 5−30モル% でさらに好ましくは Fe2O3 50−55モル% MnO 30−33モル% ZnO 15−20モル% であるが、他の組成でも本発明を適用する効果は
ある。 次に多結晶フエライト2と単結晶フエライト
1,3との接合面を、ダイヤモンド砥粒を使用し
て、好ましくは表面粗さを0.5ミクロン以下、平
坦度を0.5ミクロン以下になるように鏡面研磨す
る。このとき重要なのは、研磨方向を一定方向に
する点にある。例えば、直方体形状では直方体の
長辺方向に研磨方向をそろえることが望ましい。 次に、上述したように鏡面研磨した多結晶フエ
ライト2および単結晶フエライト1,3の接合面
に有機酸および無機酸を介在させて、第1図Bに
示すように両研磨面を密着する。両研磨面を密着
した接合体は、多結晶フエライトの不連続な結晶
粒子成長の起こる温度未満の温度、すなわち上述
した組成のフエライトでは約1330−1350℃で加熱
される。その結果、単結晶フエライト1,3を多
結晶フエライト2方向に結晶成長させ、多結晶フ
エライトを殆ど全て単結晶フエライトに転換し
た、大きい単結晶フエライト4を第1図Cに示す
ように得ることができる。 以下実施例について説明する。 実施例 マグネタイト(Fe3O4)を経由して製造した酸
化鉄で、不純物SiO2 0.005%、TiO20.005%、
CaO0.005%、Na2O0.005%を含むものと、純度
99.9%の酸化マンガンおよび酸化亜鉛を原料とし
て、その組成がMnO28モル%、ZnO19.5モル%、
Fe2O352.5モル%となるように混合した調合物を、
仮焼、粉砕、成形ののち、平衡酸素分圧下で、
1320℃4時間焼成してMn−Zn多結晶フエライト
を得た。 一方、その多結晶フエライトと、ほぼ同一の組
成を有する、高圧ブリツヂマン法で製造された単
結晶フエライトを用意し、この両方のフエライト
より、それぞれ10×30×5mmと、10×30×0.5mm
の直方体形状(板)を切り出し、それぞれの接合
面を、ダイヤモンド砥粒(2〜4μ)でスズ盤上
で、条痕(極わずかの研磨キズ)がランダムにな
るよう研磨したもの(試料D)、堅型平面研削盤
にて、試料の長辺方向に45゜の角度方向になるよ
う研磨したもの(試料C)、短辺方向に平行にな
るよう研磨したもの(試料B)、および長辺方向
に研磨したもの(試料A)を準備した。なお、こ
れらの鏡面研磨面はいずれも表面粗さRmax0.1
〜0.5ミクロン、平坦度0.3〜0.5ミクロンであつ
た。 そして多結晶フエライト板と単結晶フエライト
板の鏡面研磨面に、6NのHNO3を塗布し、密着
させた後にこれを純N2ガス雰囲気中に於て、
1150℃、30分間加熱し、引続き、O2濃度5%の
N2ガス雰囲気中に於て、1340℃、3時間保持し、
固相反応を起させ、単結晶フエライトを多結晶フ
エライト方向に結晶成長させ、多結晶フエライト
全体を単結晶化した。 結果は第1表に示すとおりである。
The present invention relates to a method for manufacturing single crystal ferrite used in VTR magnetic heads, etc., and more specifically, by heating the single crystal ferrite after contacting the polycrystal ferrite with the single crystal ferrite, the single crystal ferrite is directed in the direction of the polycrystal ferrite. The present invention relates to a method for producing a ferrite single crystal by growing the crystal to grow a single crystal ferrite. BACKGROUND ART Conventionally, as a method for producing single crystal ferrite, the Bridgeman method is known in which a single crystal is grown from a liquid phase obtained by melting a raw material at a high temperature above its melting point. However, the Bridgmann method, which grows single crystals from a molten liquid phase, requires high temperatures of over 1,600°C, which makes it particularly difficult to manufacture single-crystal ferrite using raw materials such as zinc oxide, which are extremely prone to scattering at high temperatures. However, since the composition of the product tends to fluctuate and impurities are easily mixed in from the container used to melt the raw materials, the obtained single crystal has the disadvantage that the crystallinity of the obtained single crystal is not uniform. Furthermore, the Bridzman method requires expensive, complicated, and large manufacturing equipment, and it is difficult to accurately control the heating conditions and seed single crystal formation conditions during manufacturing, so it is difficult to mass-produce. There were problems such as the resulting single crystal ferrite product being expensive. In order to solve the above-mentioned problems, the applicant proposed in Japanese Patent Application Laid-Open No. 155100/1983 a method for producing ferrite single crystals by solid phase reaction. however,
In this method, the mother polycrystalline material and the seed single crystal are mirror-polished and then bonded together, but the grinding scars on the bonded surfaces after polishing were in arbitrary directions. When a bonded body with such scratches arbitrarily formed is heated, a slight deformation occurs when the processing strain is alleviated by the grinding scars, the closely bonded surface separates, and the single crystallization of the polycrystalline body is inhibited. There were flaws. The purpose of the present invention is to eliminate the above-mentioned problems and provide a manufacturing method for obtaining single crystal ferrite at a high yield and at low cost by keeping the polishing direction constant during polishing and minimizing separation of the closely bonded surfaces. It is something to do. Yet another object is to provide a method for producing large-sized single-crystal ferrite. The present invention relates to a method for producing a ferrite single crystal in which single crystal ferrite is grown by heating the polycrystalline ferrite and single crystal ferrite in the direction of the polycrystalline ferrite by heating the polycrystalline ferrite and the single crystal ferrite. The joint surfaces of the crystal ferrites are each polished to a mirror surface, and at least the mirror polished surfaces of the single crystal ferrites are polished in the same direction. Hereinafter, the present invention will be explained in detail with reference to the drawings. FIGS. 1A to 1C are perspective views for explaining an embodiment of the manufacturing method of the present invention, and show an example in which Mn--Zn ferrite is used and the shape is a rectangular parallelepiped. First of all
As shown in Figure A, a polycrystalline ferrite 2 made of Mn-Zn and seed single-crystalline ferrites 1 and 3 made of the same material are prepared. As the polycrystalline ferrite, it is necessary to use a polycrystalline ferrite manufactured using iron oxide having a spinel structure, iron oxide having a spinel structure history, or a mixture thereof as a raw material for iron oxide. Further, the difference in thermal expansion coefficient between polycrystalline ferrite and single crystal ferrite is preferably ±10×10 -7 or less. The composition of the above-mentioned ferrite is preferably Fe 2 O 3 45-55 mol% MnO 20-40 mol% ZnO 5-30 mol%, more preferably Fe 2 O 3 50-55 mol% MnO 30-33 mol% ZnO Although the amount is 15-20 mol%, the present invention can be applied to other compositions as well. Next, the joint surface between the polycrystalline ferrite 2 and the single crystal ferrites 1 and 3 is mirror-polished using diamond abrasive grains so that the surface roughness is preferably 0.5 microns or less and the flatness is preferably 0.5 microns or less. . What is important at this time is to keep the polishing direction constant. For example, in the case of a rectangular parallelepiped shape, it is desirable to align the polishing direction in the long side direction of the rectangular parallelepiped. Next, an organic acid and an inorganic acid are interposed between the joint surfaces of polycrystalline ferrite 2 and single crystal ferrites 1 and 3, which have been mirror-polished as described above, to bring the polished surfaces into close contact as shown in FIG. 1B. The bonded body with both polished surfaces in close contact is heated to a temperature below the temperature at which discontinuous grain growth of polycrystalline ferrite occurs, ie, about 1330-1350° C. for ferrite having the composition described above. As a result, by growing the single crystal ferrites 1 and 3 in the direction of the polycrystalline ferrite 2, it was possible to obtain a large single crystal ferrite 4 in which almost all of the polycrystalline ferrite was converted to single crystal ferrite, as shown in FIG. 1C. can. Examples will be described below. Example Iron oxide produced via magnetite (Fe 3 O 4 ), with impurities SiO 2 0.005%, TiO 2 0.005%,
Contains 0.005% CaO, 0.005% Na2O , and purity
Using 99.9% manganese oxide and zinc oxide as raw materials, the composition is MnO28 mol%, ZnO 19.5 mol%,
A mixture of 52.5 mol% Fe 2 O 3 was prepared.
After calcination, crushing, and molding, under equilibrium oxygen partial pressure,
It was fired at 1320°C for 4 hours to obtain Mn-Zn polycrystalline ferrite. On the other hand, a single crystal ferrite manufactured by the high-pressure Bridgman method, which has almost the same composition as the polycrystalline ferrite, was prepared, and from both ferrites, 10 x 30 x 5 mm and 10 x 30 x 0.5 mm, respectively, were prepared.
A rectangular parallelepiped (plate) was cut out, and the joint surfaces of each were polished on a tin disk with diamond abrasive grains (2 to 4μ) so that the streaks (extremely slight polishing scratches) were random (Sample D). , with a rigid surface grinder, the sample was ground at a 45° angle to the long side (sample C), the sample was ground parallel to the short side (sample B), and the long side A specimen polished in the same direction (sample A) was prepared. All of these mirror polished surfaces have a surface roughness of Rmax0.1.
~0.5 micron, flatness 0.3-0.5 micron. Then, 6N HNO 3 was applied to the mirror-polished surfaces of the polycrystalline ferrite plate and the single-crystal ferrite plate, and after adhesion, this was placed in a pure N 2 gas atmosphere.
Heated at 1150℃ for 30 minutes, then heated at 5% O2 concentration.
Maintained at 1340℃ for 3 hours in N2 gas atmosphere,
A solid phase reaction was caused to cause crystal growth of the single crystal ferrite in the direction of the polycrystalline ferrite, and the entire polycrystalline ferrite was made into a single crystal. The results are shown in Table 1.

【表】 研磨加工の際には、加工後表面に加工歪が残留
することは避けられないが、残留歪と研磨方向と
は密接な関係があり、研磨方向を一定に揃えるこ
とは、加工歪に生じるねじれ、そりなどの現象を
最小限に抑えることができ、特に長辺方向に揃え
ることが最も効果的である。 第2図A〜Dは研磨方向による接合体の加熱後
の変形を示す斜視図であり、第2図A〜Dはそれ
ぞれ上述した実施例の試料A〜Dに対応してい
る。 以上詳細に説明したところから明らかなよう
に、本発明のフエライト単結晶の製造法によれ
ば、接合面の研磨方向を一定にそろえて加熱して
いるため、加熱後の接合面の離脱がなく、そのた
め品質の良い単結晶フエライトが収率よく得られ
る。また寸法が大きい単結晶フエライトが容易に
得られる。さらに、従来例で必要な平坦度の検査
が不必要なため、製造工程の数を減らすことがで
き、製造法の簡略化が達成できる。 本発明はVTR用の磁気ヘツドフエライト、各
種の磁気ヘツド、ノイズの少ない磁気ヘツド用フ
エライトに使用できる単結晶フエライトを従来法
と比較して安価かつ容易に作成できるため、工業
上極めて有用な単結晶フエライトの製造法であ
る。
[Table] During polishing, it is unavoidable that machining strain remains on the surface after machining, but there is a close relationship between residual strain and the polishing direction. It is possible to minimize phenomena such as twisting and warping that occur on the board, and it is most effective to align them in the long side direction. 2A to 2D are perspective views showing deformation of the bonded body after heating according to the polishing direction, and FIGS. 2A to 2D correspond to samples A to D of the above-described embodiment, respectively. As is clear from the detailed explanation above, according to the method for producing a ferrite single crystal of the present invention, since the polishing direction of the bonded surfaces is aligned and heated, there is no separation of the bonded surfaces after heating. Therefore, high quality single crystal ferrite can be obtained in good yield. Furthermore, large-sized single crystal ferrite can be easily obtained. Furthermore, since the flatness inspection required in the conventional example is unnecessary, the number of manufacturing steps can be reduced and the manufacturing method can be simplified. The present invention makes it possible to produce single crystal ferrite that can be used for magnetic head ferrite for VTRs, various magnetic heads, and magnetic head ferrite with low noise at a lower cost and easier than conventional methods, making it an industrially extremely useful single crystal. This is a method for producing ferrite.

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

第1図A〜Cは本発明の製造方法の一実施例を
説明するための斜視図、第2図A〜Dは研磨方向
による接合体の加熱後の変形を示す斜視図であ
る。 1,3……単結晶体、2……多結晶体。
1A to 1C are perspective views for explaining an embodiment of the manufacturing method of the present invention, and FIGS. 2A to 2D are perspective views showing deformation of the joined body after heating depending on the polishing direction. 1, 3...single crystal, 2...polycrystal.

Claims (1)

【特許請求の範囲】 1 多結晶フエライトと単結晶フエライトとを接
触後加熱することにより、単結晶フエライトを多
結晶フエライト方向に結晶成長させて単結晶フエ
ライトを育成するフエライト単結晶の製造法にお
いて、多結晶フエライトおよび単結晶フエライト
の接合面をそれぞれ鏡面に研磨するとともに、少
なくとも単結晶フエライトの鏡面研磨面の研磨方
向を一定方向にそろえて実施することを特徴とす
るフエライト単結晶の製造法。 2 多結晶フエライトおよび単結晶フエライトと
も直方体形状とし、研磨方向を直方体の長辺方向
と平行とした特許請求の範囲第1項記載のフエラ
イト単結晶の製造法。 3 鏡面研磨面の研磨粗さを0.5ミクロン以下で
かつ平坦度を0.5ミクロン以下とした特許請求の
範囲第1項または第2項記載のフエライト単結晶
の製造法。 4 多結晶フエライトおよび単結晶フエライトが
Mn−Znフエライトである特許請求の範囲第1
項、第2項または第3項記載のフエライト単結晶
の製造法。
[Scope of Claims] 1. A method for producing a ferrite single crystal in which polycrystalline ferrite and single-crystal ferrite are brought into contact and then heated to grow single-crystal ferrite in the direction of polycrystalline ferrite to grow single-crystal ferrite, A method for producing a ferrite single crystal, which comprises polishing the joint surfaces of polycrystalline ferrite and single-crystal ferrite to a mirror surface, and aligning the polishing direction of at least the mirror-polished surfaces of the single-crystal ferrite in a fixed direction. 2. The method for producing a ferrite single crystal according to claim 1, wherein both the polycrystalline ferrite and the single crystal ferrite have a rectangular parallelepiped shape, and the polishing direction is parallel to the long side direction of the rectangular parallelepiped. 3. The method for producing a ferrite single crystal according to claim 1 or 2, wherein the mirror-polished surface has a polishing roughness of 0.5 microns or less and a flatness of 0.5 microns or less. 4 Polycrystalline ferrite and single crystal ferrite
Claim 1 which is Mn-Zn ferrite
2. A method for producing a ferrite single crystal according to item 2, item 3, or item 3.
JP59053230A 1984-03-19 1984-03-19 Production of ferrite single crystal Granted JPS60195096A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59053230A JPS60195096A (en) 1984-03-19 1984-03-19 Production of ferrite single crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59053230A JPS60195096A (en) 1984-03-19 1984-03-19 Production of ferrite single crystal

Publications (2)

Publication Number Publication Date
JPS60195096A JPS60195096A (en) 1985-10-03
JPH0143719B2 true JPH0143719B2 (en) 1989-09-22

Family

ID=12937016

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59053230A Granted JPS60195096A (en) 1984-03-19 1984-03-19 Production of ferrite single crystal

Country Status (1)

Country Link
JP (1) JPS60195096A (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62216987A (en) * 1986-03-17 1987-09-24 Ngk Insulators Ltd Production of single crystal ferrite
US6048394A (en) * 1997-08-14 2000-04-11 Competitive Technologies Of Pa, Inc. Method for growing single crystals from polycrystalline precursors

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Publication number Publication date
JPS60195096A (en) 1985-10-03

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