JPH0465032B2 - - Google Patents
Info
- Publication number
- JPH0465032B2 JPH0465032B2 JP16372784A JP16372784A JPH0465032B2 JP H0465032 B2 JPH0465032 B2 JP H0465032B2 JP 16372784 A JP16372784 A JP 16372784A JP 16372784 A JP16372784 A JP 16372784A JP H0465032 B2 JPH0465032 B2 JP H0465032B2
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- solidified
- single crystal
- layer
- composition
- 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
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- 239000000203 mixture Substances 0.000 claims description 33
- 239000013078 crystal Substances 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- 239000011701 zinc Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000011572 manganese Substances 0.000 claims description 10
- 229910000859 α-Fe Inorganic materials 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 2
- 230000015271 coagulation Effects 0.000 claims 1
- 238000005345 coagulation Methods 0.000 claims 1
- 238000005204 segregation Methods 0.000 description 11
- 239000007789 gas Substances 0.000 description 10
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 10
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 235000014692 zinc oxide Nutrition 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- WMVRXDZNYVJBAH-UHFFFAOYSA-N dioxoiron Chemical compound O=[Fe]=O WMVRXDZNYVJBAH-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
（産業上の技術分野）
本発明はMn・Znフエライト単結晶の製造方
法、特にはVTR磁気ヘツドやフロツピイデイス
ク用磁気ヘツドなどに用いられる磁気特性にすぐ
れたMn・Znフエライト単結晶の製造方法に関す
るものである。
（従来の技術）
Mn・Znフエライト単結晶はVTR磁気ヘツド
やフロツピイデイスク用磁気ヘツドとして実用化
されているが、これは鉄、マンガン、亜鉛の酸化
物からなる仮焼原料を白金ルツボ中で均一に溶融
し、温度勾配中を移動させて、先端部から凝固さ
せて単結晶化するといういわゆるブリツジマン法
で製造されている。しかしこの方法には亜鉛の蒸
発や凝固過程における偏析などのために単結晶体
が上下で組成の異なるものとなり、磁気特性にバ
ラツキが生じるという欠点がある。また、単結晶
の育成中に凝固した分だけの原料を連続的に補給
して組成偏析を是正するという方法もあるが、こ
れには単結晶の歩留りが下がるし、装置が大がか
りのものとなるという技術的、経済的な不利があ
る。
（発明の構成）
本発明はこのような不利を解決したMn・Znフ
エライト単結晶の製造方法に関するものであり、
これは鉄、マンガン、亜鉛の酸化物からなる組成
の異なる少なくとも２種の焼成原料を、ルツボ中
に各原料組成物が層状になるように仮凝固させた
のち、この凝固体層にガス抜き穴を設け、これを
ルツボの先端部から徐々に溶融し、凝固させて単
結晶化することを特徴とするものである。
これを説明すると、本発明者らは組成偏析がな
く、したがつて磁気特性のバラツキの少ない
Mn・Znフエライト単結晶体の製造方法について
種々検討した結果、従来法における単結晶体の育
成方向における偏析を補償するような複数の仮焼
組成体を準備してこれらを順次堆積した凝固体を
作り、これを順次溶融すれば組成偏析のない単結
晶体を得ることができるということを見出し、こ
の実施方法についてさらに研究を進め、少なくと
も２種の組成の異なる仮焼原料組成物を準備して
これらをルツボ中にそれらが層状になるように順
次溶融凝固させたのち、この仮凝固体にガス抜き
穴（望ましくは凝固体層の２分の１以上の深さの
穴）を設けて順次再溶融すれば組成偏析の非常に
少ない単結晶を容易にかつ確実に得ることができ
るということを確認して本発明を完成させた。
本発明のMn・Znフエライト単結晶を作るため
の素原料は公知のものであり、これは鉄、マンガ
ン、亜鉛の酸化物の混合物とされるが、これは二
三酸化鉄（Fe2O3）を50〜65モル％、酸化マンガ
ン（MnO）を20〜35モル％、酸化亜鉛が15〜30
モル％の組成となるように配合したものとすれば
よい。この組成物は本発明の方法においては単結
晶育成中における組成偏析を解決するために組成
の異なる少なくとも２種、好ましくは３〜５種の
組成物とする必要があるが、この場合この偏析に
よつて減少する鉄、亜鉛分を順次増加させ、マン
ガンを減少させるようにすればよく、例えばこれ
を３種の組成物とする場合にはFe2O3を53.0、
54.5、56.0モル％、MnOを29.0、25.25、21.5モル
％、ZnOを18.0、20.25、22.5モル％のように変化
させたものとすればよい。
なお、ブリツジマン法によつて育成したMn・
Znフエライト単結晶の場合、その組成偏析は最
初に凝固する下部先端から中央部にかけてゆるや
かであるが、中央部から最後に凝固する上部にか
けて激しくなる。そこで、２種以上の仮焼組成物
を順次ルツボ内に集積させる場合には、最初ルツ
ボの底に堆積させる第１組成物の量を全体の約1/
２くらいとし、第２、第３の組成物の量を組成偏
析の勾配に対応させて調節するのがよい。これら
はまず第１の組成物をルツボ内に入れて溶融し仮
凝固させたのち、ついで第２の組成物を入れて第
１の組成物の凝固物を境界部分以外は溶解しない
ようにして溶解してから凝固させて順次凝固物と
して堆積させて各層の混融物が生じないようにす
ることがよい。
つぎにこのようにして得られた少なくとも２種
の原料組成物の仮凝固体層は、溶融、再凝固で単
結晶化されるのであるが、これは溶解時に還元作
用によるO2のようなガスが発生し、このガスが
ルツボ内に充満するとその内圧によつてルツボが
破壊されたり、溶融物が吹き出したりする可能性
があるので、これにはガス抜きのため穴を形成し
ておくことが必要である。このガス抜き穴は仮凝
固体の中心部にドリルなどで設けるようにすれば
よいが、これは単結晶育成時の条件として溶融部
が仮凝固体の長さの1/3くらいが最も適当とされ
るということから仮凝固体の長さの1/2以上の深
さとすることが望ましい。
本発明の方法はこのようにガス抜き穴を設けた
仮凝固体をルツボ中で順次溶融し、凝固させて単
結晶化するのであるが、この溶融はルツボの下の
先端部から徐々に行なうことがよく、これによれ
ば第１層の溶融、再凝固後に行なわれる第１層と
第２層との混融凝固、第２層と第３層の混融凝固
による単結晶体はその仮凝固体層が組成偏析を補
償する組成とされているので、第１層の凝固で得
られたものと同一組成のものとして得られるとい
う有利性が与えられる。
つぎに本発明の実施例をあげる。
実施例
酸化鉄（Fe2O3）、酸化マンガン（MnO）、酸
化亜鉛（ZnO）とからなる第１表に示したような
Ａ、Ｂ、Ｃの３種のフエライト組成物を準備し、
Ａ組成物400ｇ、Ｂ組成物250ｇ、Ｃ組成物150ｇ
を白金ルツボ中に順次装入し、ブリツジマン炉中
で順次溶融し、仮凝固させて、白金ルツボ中に
Ａ、Ｂ、C3層からなる高さ13cmの仮凝固体層を
形成させた。
ついで、この仮凝固体を炉中で放冷し、室温に
まで冷却してから、ダイヤモンドドリルで３mm
φ、深さ10cmの穴を作り、ルツボごと超音波洗浄
器で洗浄した。
つぎに、ルツボの下部先端がブリツジマン炉の
温度分布の最高点になるようにルツボを設置し、
酸化を防ぐための炉内に窒素を流しながら80℃／
時のスピードで炉を昇温させ、温度が1650℃にな
つた時点で昇温を止め、還元によるFeOの発生を
抑えるために窒素ガスを止め炉内に酸素を流して
1650℃で１時間保持したのち、ルツボを回転させ
ながら５mm／時のスピードでルツボを降下させ
た。
ついで、炉内での酸化を防ぐために窒素ガスを
流しながら150〜200℃／時のスピードで炉を室温
にまで冷却し、このようにして得たインゴツトの
先端部を切断除去したのちフツ酸でエツチングし
て単結晶化を確認したのち、得られた長さ11cmの
インゴツトから２cmごとに厚さ0.5mmのウエーハ
を切出し、化学分析したところ、その組成偏析に
ついて第２表に示したとおりの結果が得られた。
なお、比較のため上記のような３種の組成物を
使用せず、これをＡ組成物800ｇのみとした以外
は同様にして処理して得たMn・Znフエライト単
結晶ウエーハの化学分析値は第２表に併記したと
おりであり、また上記においてガス抜き穴を設け
ずに単結晶の育成をしたときにはガス爆発によつ
てルツボが破壊された。
(Industrial Technical Field) The present invention relates to a method for manufacturing Mn/Zn ferrite single crystals, and in particular to manufacturing Mn/Zn ferrite single crystals with excellent magnetic properties used in VTR magnetic heads, floppy disk magnetic heads, etc. It is about the method. (Prior art) Mn/Zn ferrite single crystals have been put into practical use as magnetic heads for VTR magnetic heads and floppy disks, but in this case, calcined raw materials consisting of oxides of iron, manganese, and zinc are placed in a platinum crucible. It is manufactured using the so-called Bridgeman method, in which it is uniformly melted at a temperature gradient, then solidified from the tip to form a single crystal. However, this method has the disadvantage that the upper and lower parts of the single crystal have different compositions due to zinc evaporation and segregation during the solidification process, resulting in variations in magnetic properties. Another method is to correct the compositional segregation by continuously replenishing the amount of raw material that has solidified during single crystal growth, but this reduces the yield of single crystals and requires large-scale equipment. There are technical and economic disadvantages. (Structure of the Invention) The present invention relates to a method for manufacturing Mn/Zn ferrite single crystal that solves the above disadvantages.
In this method, at least two types of firing raw materials with different compositions, consisting of oxides of iron, manganese, and zinc, are temporarily solidified in a crucible so that each raw material composition forms a layer, and then gas vent holes are formed in this solidified layer. It is characterized in that it is gradually melted from the tip of the crucible and solidified to form a single crystal. To explain this, the present inventors found that there is no compositional segregation, and therefore there is little variation in magnetic properties.
As a result of various studies on manufacturing methods for Mn/Zn ferrite single crystals, we have prepared multiple calcined compositions that compensate for the segregation in the growth direction of single crystals in the conventional method, and created a solidified body by sequentially depositing these compositions. We discovered that it is possible to obtain a single crystal with no compositional segregation by sequentially melting it, and further research on this method led to the preparation of at least two types of calcined raw material compositions with different compositions. After sequentially melting and solidifying these so that they form a layer in a crucible, a gas vent hole (preferably a hole at least half the depth of the solidified material layer) is provided in this temporary solidified material and the material is sequentially re-melted. The present invention was completed by confirming that by melting, a single crystal with very little compositional segregation can be easily and reliably obtained. The raw material for making the Mn/Zn ferrite single crystal of the present invention is a known one, and is said to be a mixture of iron, manganese, and zinc oxides, but this is made from iron dioxide (Fe 2 O 3 ) 50-65 mol%, manganese oxide (MnO) 20-35 mol%, zinc oxide 15-30
What is necessary is just to mix|blend so that it may become the composition of mol%. In the method of the present invention, this composition needs to be composed of at least two different compositions, preferably three to five different compositions, in order to solve compositional segregation during single crystal growth. Therefore, the iron and zinc content, which decreases as a result, can be increased sequentially, and the manganese content can be decreased. For example, when making a composition of three types, Fe 2 O 3 is 53.0, Fe 2 O 3 is 53.0,
54.5, 56.0 mol%, MnO 29.0, 25.25, 21.5 mol%, and ZnO 18.0, 20.25, 22.5 mol%. In addition, Mn・
In the case of Zn ferrite single crystals, the compositional segregation is gradual from the lower tip where it solidifies first to the center, but becomes more severe from the center to the top where it solidifies last. Therefore, when two or more types of calcined compositions are sequentially accumulated in a crucible, the amount of the first composition deposited on the bottom of the crucible is reduced to about 1/2 of the total amount.
It is preferable that the amount of the second and third components be adjusted in accordance with the gradient of composition segregation. First, the first composition is placed in a crucible, melted, and temporarily solidified, and then the second composition is placed in the crucible and the solidified product of the first composition is melted in such a way that the solidified product of the first composition is not melted except at the boundary. It is preferable to solidify the mixture and then deposit it as a solidified product in order to prevent the formation of mixed melts in each layer. Next, the temporarily solidified layer of the at least two raw material compositions obtained in this way is melted and resolidified to form a single crystal, but this is because gases such as O 2 are released by the reducing action during melting. If gas is generated and the crucible is filled with this gas, the crucible may be destroyed or the melt may blow out due to the internal pressure, so it is recommended to form a hole in the crucible to vent the gas. is necessary. This gas vent hole can be made in the center of the temporary solidified body using a drill or the like, but the most suitable condition for this when growing a single crystal is that the molten zone is about 1/3 of the length of the temporary solidified body. Therefore, it is desirable that the depth be at least 1/2 of the length of the temporary solidified body. In the method of the present invention, the temporary solidified body provided with gas vent holes is sequentially melted in a crucible and solidified to form a single crystal, but this melting is performed gradually from the bottom tip of the crucible. According to this, the single crystal is temporarily solidified by the melting of the first layer, the mixing and solidification of the first and second layers, and the mixing and solidification of the second and third layers after melting and resolidification of the first layer. Since the body layer is of a composition that compensates for compositional segregation, it has the advantage of being obtained with the same composition as that obtained by solidification of the first layer. Next, examples of the present invention will be given. Example Three types of ferrite compositions A, B, and C as shown in Table 1, consisting of iron oxide (Fe 2 O 3 ), manganese oxide (MnO), and zinc oxide (ZnO), were prepared,
A composition 400g, B composition 250g, C composition 150g
were sequentially charged into a platinum crucible, sequentially melted in a Bridgeman furnace, and temporarily solidified to form a 13 cm high temporarily solidified layer consisting of three layers A, B, and C in the platinum crucible. Next, this temporary solidified body is allowed to cool in a furnace, cooled to room temperature, and then drilled with a diamond drill to a diameter of 3 mm.
A hole of φ and depth of 10 cm was made, and the crucible was cleaned with an ultrasonic cleaner. Next, set up the crucible so that the bottom tip of the crucible is at the highest point of the temperature distribution in the Bridgmann furnace.
Heat to 80℃/while flowing nitrogen into the furnace to prevent oxidation.
The temperature was raised in the furnace at a speed of 1,650℃, and the temperature increase was stopped when the temperature reached 1650℃. In order to suppress the generation of FeO due to reduction, nitrogen gas was stopped and oxygen was allowed to flow into the furnace.
After holding at 1650° C. for 1 hour, the crucible was lowered at a speed of 5 mm/hour while rotating the crucible. Next, the furnace was cooled to room temperature at a rate of 150 to 200°C/hour while flowing nitrogen gas to prevent oxidation in the furnace, and the tips of the ingots thus obtained were cut and removed, and then treated with hydrofluoric acid. After etching and confirming single crystallization, 0.5 mm thick wafers were cut out every 2 cm from the resulting 11 cm long ingot and chemically analyzed, and the compositional segregation results are shown in Table 2. was gotten. For comparison, the chemical analysis values of a Mn/Zn ferrite single crystal wafer obtained by processing in the same manner except that only 800 g of composition A was used instead of using the above three types of compositions are as follows. As shown in Table 2, when a single crystal was grown without providing a gas vent hole in the above example, the crucible was destroyed by a gas explosion.
【表】【table】
Claims (1)
異なる少なくとも２種の焼成原料を、ルツボ中に
各原料組成物が層状になるように仮凝固させたの
ち、この凝固体層にガス抜き穴を設け、これをル
ツボの先端部から徐々に溶融し、凝固させて単結
晶化することを特徴とするMn・Znフエライト単
結晶の製造方法。 ２ ガス抜き穴を凝固体層の長さの少なくとも1/
２以上の深さとする特許請求の範囲第１項記載の
方法。[Claims] 1. At least two types of firing raw materials having different compositions consisting of oxides of iron, manganese, and zinc are temporarily solidified so that each raw material composition is layered in a crucible, and then this solidified product is A method for manufacturing Mn/Zn ferrite single crystal, which is characterized by providing a gas vent hole in the layer, gradually melting the layer from the tip of the crucible, and solidifying it to form a single crystal. 2 The gas vent hole should be at least 1/1/2 of the length of the coagulation layer.
The method according to claim 1, wherein the depth is two or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16372784A JPS6140894A (en) | 1984-08-03 | 1984-08-03 | Manufacturing method of Mn/Zn ferrite single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16372784A JPS6140894A (en) | 1984-08-03 | 1984-08-03 | Manufacturing method of Mn/Zn ferrite single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6140894A JPS6140894A (en) | 1986-02-27 |
| JPH0465032B2 true JPH0465032B2 (en) | 1992-10-16 |
Family
ID=15779514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16372784A Granted JPS6140894A (en) | 1984-08-03 | 1984-08-03 | Manufacturing method of Mn/Zn ferrite single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6140894A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4539535B2 (en) * | 2005-11-09 | 2010-09-08 | 三菱マテリアル株式会社 | Method for producing langate single crystal |
| JP4539588B2 (en) * | 2006-03-13 | 2010-09-08 | 三菱マテリアル株式会社 | Method for producing LTGA single crystal |
-
1984
- 1984-08-03 JP JP16372784A patent/JPS6140894A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6140894A (en) | 1986-02-27 |
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