KR0144614B1 - Preparation method for single crystal of manganese-zing ferrite - Google Patents

Preparation method for single crystal of manganese-zing ferrite

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Publication number
KR0144614B1
KR0144614B1 KR1019950008151A KR19950008151A KR0144614B1 KR 0144614 B1 KR0144614 B1 KR 0144614B1 KR 1019950008151 A KR1019950008151 A KR 1019950008151A KR 19950008151 A KR19950008151 A KR 19950008151A KR 0144614 B1 KR0144614 B1 KR 0144614B1
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South Korea
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single crystal
manganese
platinum
raw material
initial raw
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KR1019950008151A
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Korean (ko)
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KR960037874A (en
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임병묵
마재용
이병우
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이형도
삼성전기주식회사
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    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003—Heating or cooling of the melt or the crystallised material
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/006—Controlling or regulating
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/007—Mechanisms for moving either the charge or the heater
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/14—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method characterised by the seed, e.g. its crystallographic orientation
    • 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

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

Abstract

본 발명은 VTR 헤드에 사용되는 망간-아연 페라이트 단결정의 제조방법에 관한 것으로, 단결정 초기원료의 성장시점에 백금도가니 내에 백금관을 용액과 접하지 않도록 위치시키므로서 단결정의 초반부위에서의 가용부분이 크고 수율 또한 우수한 망간-아연 페라이트 단결정의 제조방법을 제공하고자 하는데 그 목적이 있다.The present invention relates to a method for producing a manganese-zinc ferrite single crystal used in a VTR head. It is an object of the present invention to provide a method for producing a manganese-zinc ferrite single crystal excellent in yield.

상기한 목적달성을 위한 본 발명은 종결정과 초기원료를 백금도가니에 넣어 로의 저부에 위치시키고 로의 온도를 단결정의 용융온도까지 높인 후, 백금도가니를 상승시켜 종결정과 초기원료를 용융시킨 다음, 다시 하강시켜 초기원료를 성장시키고, 추가원료를 투입하여 조성을 조절하면서 망간-아연 페라이트 단결정을 제조하는 방법에 있어서, 상기 초기원료의 성장시작 시점에 백금도가니의 내경보다 작은 직경의 백금관을 용액과 접촉되지 않도록 상면에 근접 위치시켜 초기원료의 성장종료시까지 유지하는 것을 표함하여 이루어지는 망간-아연 페라이트 단결정의 제조방법을 제공함을 그 요지로 한다.In order to achieve the above object, the present invention places seed crystals and initial raw materials in a platinum crucible, places them at the bottom of the furnace, raises the temperature of the furnace to the melting temperature of single crystals, and then raises the platinum crucible to melt the seed crystals and initial raw materials, In the method of manufacturing a manganese-zinc ferrite single crystal while lowering again to grow an initial raw material, and adding an additional raw material to adjust the composition, at the start of the initial raw material growth of a platinum tube with a diameter smaller than the inner diameter of the platinum crucible It is an object of the present invention to provide a method for producing a manganese-zinc ferrite single crystal, which is placed close to the upper surface so as not to be contacted and maintained until the end of growth of the initial raw material.

Description

망간-아연 페라이트 단결정의 제조방법Process for preparing manganese-zinc ferrite single crystal

제1도는 종래의 방법이 적용된 망간-아연 페라이트 단결정 제조장치의 개략도1 is a schematic diagram of a manganese-zinc ferrite single crystal manufacturing apparatus to which a conventional method is applied.

제2도는 본 발명의 방법이 적용된 망간-아연 페라이트 단결정 제조장치의 개략도2 is a schematic view of a manganese-zinc ferrite single crystal manufacturing apparatus to which the method of the present invention is applied.

*도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings

1 : 발열체 2 : 노심관1: heating element 2: core tube

3 : 백금도가니 4 : 성장된 단결정3: platinum crucible 4: grown single crystal

5 : 용액 6 : 백금관5: solution 6: platinum tube

본 발명은 VTR 헤드에 사용되는 Mn-Zn 페라이트 단결정의 제조방법에 관한 것으로, 보다 상세하게는 단결정의 초기성장시 결정내에 백금의 혼입을 최소화하여 단결정의 초반부위에서, 가용부분이 크고 수율 또한 우수한 망간-아연 페라이트 단결정을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a Mn-Zn ferrite single crystal used in a VTR head, and more particularly, to minimize the incorporation of platinum in the crystal during the initial growth of the single crystal, to minimize the incorporation of platinum in the early stage of the single crystal, the manganese has a large yield and excellent yield Zinc ferrite single crystals.

일반적으로 망간-아연 페라이트 단결정은 높은 초기투자율등의 자기적 특성외에 내마모성, 내열성, 내식성 및 가공성이 우수한 특성을 갖고 있으므로 주로 VTR 헤드,HDD용 슬라이더(Slider),캠코더용 헤드등의 용도로 사용되며, 이러한 용도들중 VTR 헤드용으로 사용되기 위해서는 특히 높은 초기투자율 및 가공성이 우수해야 하는 특성이 요구된다.In general, manganese-zinc ferrite single crystals have excellent wear resistance, heat resistance, corrosion resistance and processability in addition to magnetic properties such as high initial permeability, so they are mainly used for VTR heads, sliders for HDDs, and heads for camcorders. In order to be used for the VTR head, among these applications, particularly high initial permeability and workability are required.

VTR 헤드용으로 사용되는 망간-아연 페라이트 단결정의 제조는 대부분 연속공급 성장식 브릿지만법(Bridgmantechnique)을 채택하고 있다.The manufacture of manganese-zinc ferrite single crystals used for VTR heads mostly employs the continuous feed growth Bridgmantechnique.

이러한 브릿지만법은 초기원료를 종결정과 함께 백금도가니에 채워 로내에 장입하여 로의 저부에 위치시킨 후, 로의 온도를 단결정의 용융 온도이상으로 승온시키고 로의 저부에 위치한 백금도가니를 상승시켜 초기원료 및 종결정의 일부를 용융시킨 다음, 다시 백금도가니를 하강시키면서 서냉하여 초기원료를 성장시킨 후에 추가원료를 투입하여 조성조절을 하면서 계속 성장시켜 단결정을 제조한다.This bridgeman method fills a platinum crucible with seed crystals, loads it into a furnace, places it in the bottom of the furnace, raises the temperature of the furnace above the melting temperature of the single crystal, and raises the platinum crucible located at the bottom of the furnace. After melting some of the seed crystals, the platinum crucible is lowered and cooled slowly to grow the initial raw material, and then the additional raw material is added to continue the growth while adjusting the composition to prepare a single crystal.

이때, 초기원료의 성장이 장시간 고온에서 진행되고, 또한 제1도에서와 같이 초기원료의 성장시에는 백금도가니(3), 용액(5) 및 공기가 서로 접촉하고 있어 열전달이 좋지 않으므로 용액(5)은 잠열을 그대로 가지고 있다.At this time, the growth of the initial raw material proceeds at a high temperature for a long time, and as shown in FIG. 1, the platinum crucible (3), the solution (5) and the air are in contact with each other when the initial raw material is grown, so that the heat transfer is poor. ) Has latent heat.

따라서, 초기원료의 성장도중에 백금도가니(3), 용액(5) 및 공기의 계면에서 잠열에 의해 백금이 입자화되어 성장되는 단결정(4)내로 혼입된다. 이와같이 단결정의 성장시에 백금입자들이 혼입되게 되면 블록(Block) 제조시 불량의 원인이 되고 VTR 헤드로 가공시에도 칩핑(chipping)등의 원인제공이 되므로, 백금혼입을 줄이는 것이 필요하다.Therefore, during the growth of the initial raw material, platinum is incorporated into the single crystal 4 in which platinum is granulated and grown by latent heat at the interface between the platinum crucible 3, the solution 5 and the air. As such, when platinum particles are mixed during the growth of a single crystal, it becomes a cause of defects in manufacturing a block and provides a cause of chipping during machining with a VTR head. Therefore, it is necessary to reduce platinum mixing.

이에, 본 발명자는 상기와 같은 초기원료의 성장시 백금입자의 혼입을 최소화하기 위하여 연구와 실험을 행하고 그 결과에 근거하여 본 발명을 제아하게 된 것으로, 본 발명은 단결정 초기 원료의 성장시작 시점에 백금 도가니내에 백금관을 용액과 접하지 않도록 위치시킴으로서 단결정의 초반부위에서의 가용부분이 크고 수율 또한 우수한 망간-아연 페라이트 단결정을 제조하는 방법을 제공하고자 하는데, 그 목적이 있다.Thus, the present inventors conducted research and experiments to minimize the incorporation of platinum particles in the growth of the initial raw materials as described above, and the present invention is based on the results. It is an object of the present invention to provide a method for producing a manganese-zinc ferrite single crystal having a large soluble portion at an early portion of the single crystal and having a high yield by placing the platinum tube in a platinum crucible so as not to contact the solution.

이하, 본 발명을 설명한다.Hereinafter, the present invention will be described.

본 발명은 종결정과 초기원료를 백금도가니에 넣어 로의 저부에 위치시키고 로의 온도를 단결정의 용융온도까지 높인 후, 백금도가니를 상승시켜 종결정과 초기원료를 용융시킨 다음, 다시 하강시켜 초기원료를 성장시키고, 추가원료를 투입하여 조성을 조절하면서 망간-아연 페라이트 단결정을 제조하는 방법에 있어서, 상기 초기 원료의 성장 시작 시점에 백금도가니의 내경보다 작은 직경의 백금관을 용액과 접촉되지 않도록 상면에 근접 위치시켜 초기 원료의 성장종료시까지 유지하는 것을 포함하여 이루어지는 망간-아연 페라이트 단결정의 제조방법에 관한 것이다.In the present invention, seed crystals and initial raw materials are placed in a platinum crucible, placed at the bottom of the furnace, and the temperature of the furnace is increased to the melting temperature of the single crystal, the platinum crucible is raised to melt the seed crystals and the initial raw material, and then the raw material is lowered again. In the method of manufacturing a manganese-zinc ferrite single crystal while growing, and adding an additional raw material to adjust the composition, at the start of the growth of the initial raw material close to the upper surface of the platinum tube of diameter smaller than the inner diameter of the platinum crucible so as not to contact the solution A method for producing a manganese-zinc ferrite single crystal comprising positioning and maintaining until the end of growth of the initial raw material.

이하, 본 발명을 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail.

상기한 목적을 달성하기 위하여 본 발명에서는 단결정의 초기원료 성장시 제2도에서와 같이 용액(5)의 상부에 백금도가니(3)의 내경보다 작은 직경의 백금관(6)을 용액(5)과 접하지 않도록 위치시킴이 바람직한데, 그 이유는 다음과 같다.In order to achieve the above object, in the present invention, a platinum tube 6 having a diameter smaller than the inner diameter of the platinum crucible 3 is disposed on the upper portion of the solution 5 as shown in FIG. It is preferable to position it so that it does not come in contact with it, for the following reason.

상기 백금관(6)이 용액(5)과 접하게 되면 백금입자가 용액(5)에 혼입되어 용액(5)에 악영향을 끼칠 우려가 있기 때문이다.This is because when the platinum tube 6 comes into contact with the solution 5, the platinum particles may enter the solution 5 and adversely affect the solution 5.

또한, 본 발명에서는 상기와 같이 용액(5)의 상면에 근접 설치하는 백금관(6)의 직경을 20-25㎜로 함이 보다 바람직한데, 그 이유는 다음과 같다. 백금관(6)의 직경이 20㎜이하일 경우에는 백금도가니(3) 내의 잠열을 외부로 배출하기에는 충분치 못하므로 백금관(6)의 직경이 20㎜이상이 바람직하나, 25㎜이상일 경우에는 백금도가니(3)의 내벽과의 간격이 좁아 백금도가니(3) 및 백금관(6)의 상승 하강시 백금도가니(3) 내벽에 접촉되어 백금관(6)이 백금도가니(3)에 부착되는 것과 같은 조업사고 발생의 우려가 있기 때문이다.Moreover, in this invention, as for the diameter of the platinum tube 6 installed close to the upper surface of the solution 5 as mentioned above, it is more preferable that it is 20-25 mm, The reason is as follows. When the diameter of the platinum tube 6 is 20 mm or less, it is not sufficient to discharge latent heat in the platinum crucible 3 to the outside. Therefore, the diameter of the platinum tube 6 is preferably 20 mm or more. The gap between the inner wall of (3) and the inner wall of the platinum crucible (3) and the platinum pipe (6) is in contact with the inner surface of the platinum crucible (3) so that the platinum pipe (6) is attached to the platinum crucible (3). This is because there is a risk of operation accidents.

이하,본 발명의 망간-아연 페라이트 단결정을 제조하는 방법을 첨부된 도면 제2도를 참고하여 상세히 설명한다.Hereinafter, a method for preparing a manganese-zinc ferrite single crystal of the present invention will be described in detail with reference to FIG. 2.

먼저 종결정과 초기원료를 채운 백금도가니(3)를 로의 저부에 위치시킨 후, 로의 온도를 단결정 용해온도 이상으로 승온시키고 백금도가니(3)를 상승시켜 종결정과 초기원료를 용융시킨 다음, 다시 백금도가니(3)를 서서히 하강시켜 초기원료를 성장시킨다. 이때, 초기원료의 성장이 시작되는 시점에 백금관(6)을 용액(5)의 상면과 접하지 않으면서 최대한 근접되게 위치시켜 잠열을 외부로 배출시킨다.First, place a platinum crucible (3) filled with seed crystals and an initial raw material at the bottom of the furnace. Then, raise the temperature of the furnace above the single crystal melting temperature and raise the platinum crucible (3) to melt the seed crystal and the initial raw material. The platinum crucible (3) is slowly lowered to grow an initial raw material. At this time, when the growth of the initial raw material is started, the platinum tube 6 is placed as close as possible without contacting the upper surface of the solution 5 to discharge latent heat to the outside.

이와같이 하여 초기원료의 성장이 완료되면 백금관(6)을 치우고 추가원료를 투입하여 조성조절을 하면서 단결정을 성장시킨다.In this way, when the growth of the initial raw material is completed, the platinum tube (6) is removed and additional raw materials are added to adjust the composition to grow single crystals.

상술한 바와같이, 본 발명은 망간-아연 페라이트 단결정의 제조시 백금관을 사용하여 외부로의 잠열의 배출을 원활히 하므로서, 초기원료성장시에 백금의 혼입을 최소화할 수 있어 결정의 초반부위에서의 가용부분이 크고 수율 또한 우수한 망간-아연 페라이트 단결정을 제조할 수 있는 효과가 있다.As described above, the present invention facilitates the release of latent heat to the outside by using a platinum tube in the production of manganese-zinc ferrite single crystal, thereby minimizing the incorporation of platinum during the initial raw material growth, so that it is available at the early stage of crystallization. There is an effect that can produce a manganese-zinc ferrite single crystal having a large portion and excellent yield.

Claims (2)

종결정과 초기원료를 백금도가니에 넣어 로의 저부에 위치시키고 로의 온도를 단결정의 용융온도까지 높인 후, 백금도가니를 상승시켜 종결정과 초기원료를 용융시킨 다음, 다시 하강시켜 초기 원료를 성장시키고, 추가 원료를 투입하여 조성을 조절하면서 망간-아연 페라이트 단결정을 제조하는 방법에 있어서, 상기 초기원료의 성장시작 시점에 백금도가니의 내경보다 작은 직경의 백금관을 용액과 접촉되지 않도록 상면에 근접 위치시켜 초기 원료의 성장종료시까지 유지하는 것을 포함하여 이루어짐을 특징으로 하는 망간-아연 페라이트 단결정의 제조방법Place seed crystals and initial raw materials into platinum crucibles and place them at the bottom of the furnace, raise the temperature of the furnace to the melting temperature of single crystals, raise the platinum crucible to melt seed crystals and initial raw materials, and then lower them to grow initial raw materials, In the method of manufacturing a manganese-zinc ferrite single crystal while adjusting the composition by adding an additional raw material, at the start of the growth of the initial raw material by placing a platinum tube with a diameter smaller than the inner diameter of the platinum crucible close to the upper surface so as not to contact the solution Method for producing a manganese-zinc ferrite single crystal characterized in that it comprises until the end of growth of the raw material 제1항에 있어서, 상기 백금관의 직경은 20-25㎜인 것을 특징으로 하는 망간-아연 페라이트 단결정의 제조방법The method of manufacturing a manganese-zinc ferrite single crystal according to claim 1, wherein the platinum tube has a diameter of 20-25 mm.
KR1019950008151A 1995-04-07 1995-04-07 Preparation method for single crystal of manganese-zing ferrite KR0144614B1 (en)

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Publication number Priority date Publication date Assignee Title
KR20170024370A (en) 2015-08-25 2017-03-07 농업회사법인 주식회사 생생초 Lactic acid fermentation broth containing GABA method of producing components using the mushroom extract

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20170024370A (en) 2015-08-25 2017-03-07 농업회사법인 주식회사 생생초 Lactic acid fermentation broth containing GABA method of producing components using the mushroom extract

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