JPH0561238B2 - - Google Patents
Info
- Publication number
- JPH0561238B2 JPH0561238B2 JP4045887A JP4045887A JPH0561238B2 JP H0561238 B2 JPH0561238 B2 JP H0561238B2 JP 4045887 A JP4045887 A JP 4045887A JP 4045887 A JP4045887 A JP 4045887A JP H0561238 B2 JPH0561238 B2 JP H0561238B2
- Authority
- JP
- Japan
- Prior art keywords
- ferrite
- single crystal
- crystal
- polycrystalline
- pressure
- 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 - Lifetime
Links
- 239000013078 crystal Substances 0.000 claims description 74
- 229910000859 α-Fe Inorganic materials 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 230000002159 abnormal effect Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000003746 solid phase reaction Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002223 garnet Substances 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 1
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 235000006748 manganese carbonate Nutrition 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 229940093474 manganese carbonate Drugs 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
（産業上の利用分野）
本発明は、固相反応による多結晶の均一な単結
晶化に関するもので、特に多結晶体を単結晶化す
るのに必要な種単結晶を多結晶体に貼り付ける方
法に関するものである。
（従来の技術）
従来の、単結晶の製造法として、例えば本出願
人は先に特開昭55−162496号公報において、固相
反応法による単結晶製造法を開示した。この製造
法では、種となる単結晶体と多結晶体との各接合
面を鏡面研磨した後、塩酸、硝酸等の強酸を接合
面に介在させて接合し、多結晶体の不連続粒成長
温度未満の温度で徐々に加熱して多結晶体を単結
晶化していた。
このときの接合方法としては、鏡面研磨された
多結晶体の研磨面に種単結晶を酸を介して接触さ
せ、ピンセツト等で種単結晶を多結晶体に擦り合
わせ、一定時間保持して接合していた。
（発明が解決しようとする問題点）
しかしながら、従来の単結晶法の単結晶化すべ
き多結晶は例えば27×５×８mmの寸法であつた
が、この寸法により大きな多結晶体を単結晶化し
ようとすると、多結晶体全体が均一な単結晶にな
りにくく、種単結晶の貼り付け不良等に起因する
多結晶体の異常成長が認められる場合があつた。
そのため、単結晶の収率が低いとき共に大きな単
結晶が得られない欠点があつた。
第２図ａ，ｂはそれぞれ典型的な不良例を示す
斜視図で、１は種単結晶、２は多結晶体、３はバ
ツクダミー、４は異常結晶成長部、５は生成され
た単結晶部を示している。なお、第２図ａは種単
結晶の貼付が不十分のために異常結晶成長が発生
し、第２図ｂは多結晶体２の材料が悪いために発
生する異常結晶成長を示している。
本発明の目的は、上述した不具合を解消して、
種貼付不良等に起因する結晶の異常成長を防止し
て、収率よく大きな単結晶を得ることができる単
結晶の製造法を提供しようとするものである。
（問題点を解決するための手段）
本発明の単結晶フエライトの製造法は、多結晶
フエライトと単結晶フエライトの接合面を鏡面研
磨し、その鏡面間に酸を介在させて接合し、多結
晶フエライトの不連続粒成長温度未満の温度で加
熱して、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得る単結
晶フエライトの製造法において、前記結晶成長の
ための加熱を行う前に、前記多結晶フエライトと
単結晶フエライトとの接合体を、加熱温度：100
〜300℃、加圧圧力：0.1〜250Kg／cm2の条件で接
合熱処理をすることを特徴とするものである。
（作用）
種となる単結晶の厚さは２mm程度までが好まし
いが、その厚さに比較して面積が大きいため、加
工技術上の困難性から多少湾曲している。例えば
種単結晶0.5mmに対し1μｍ程度湾曲している。こ
の単結晶と多結晶を酸介在させて接着することに
より接合面でフエライトと酸が反応し、フエライ
ト成分の塩例えば硝酸鉄、塩化鉄その他の化合物
が生成する。この化合物層を乾燥させて単結晶と
多結晶体とを固着するため、この単結晶および多
結晶体の接合体を一定の圧力で加圧しながら加熱
することにより、接合面の化合物層もほぼ均一に
薄く乾燥される。この化合物層の厚さは加圧する
圧力で定まるが、この圧力が0.1Kg／cm2〜250Kg／
cm2である必要がある。加圧圧力が0.1Kg／cm2以下
であると、加熱中に化合物層の熱膨張による単結
晶の持ち上げが生じ、そのため冷却時に単結晶が
剥がれる。また加圧圧力が250Kg／cm2以上である
と、加熱中に化合物層がほとんど流れ出てしま
い、その冷却時に単結晶が元の湾曲形状に回復し
ようとする力に抗することができなく、単結晶が
剥れる。また、フエライトは脆性材料であり、前
記圧力以上になると圧力に抗しきれず、種単結晶
が破壊する可能性がある。実際の製造工程におい
て、比較的簡単な装置にて実施できるとともに、
製造コストも廉価となるため、加圧圧力を５〜45
Kg／cm2とするのが良い。
また、加熱温度は100℃〜300℃である必要があ
る。加熱温度が100℃以下であると、接合面に介
在するフエライト成分の塩、例えば硝酸鉄、塩化
鉄、その他の化合物が分解（蒸発）せず、単結晶
成長時の焼成中に単結晶が剥がれ、多結晶体が単
結晶化しなくなる。また、加熱温度が300℃以上
であると、フエライトが酸化するため雰囲気コン
トロールが必要となり、さらにスペーサ等の材質
が限定されるため、コストが高くなる。実際の製
造において、生産コストおよび製造設備等を考慮
して、加熱温度を140℃〜200℃とするのが良い。
そのため本発明では適切な圧力で均一に加圧しつ
つ、一定時間加熱することにより、種単結晶と多
結晶体とを緊密に固着することができ、したがつ
て、種付不良その他に起因する異方性結晶の発生
を防止し、良好な単結晶を得ることができる。
さらにまた、この接着工程での加圧により、前
述したように接合面の化合物層をほぼ均一に薄く
するが、この薄い化合物層は後の固相反応の際の
加熱中に前記フエライト成分の塩が分解されて薄
い酸化物層となり、この薄い酸化物層が目的とす
る固相反応を促進する作用がある。
（実施例）
以下に、本発明の実施例を詳細に説明する。
本発明の単結晶の製造法は、多結晶体であれば
どのような組成のものにでも適用できるが、実際
に好適に使用されるものとしては以下のような組
成があげられる。
フエライト MnO 20〜40モル％
ZnO ５〜３モル％
Fe2O3 残（好ましくは48〜60モル％）
フエライト NiO 15〜40モル％
ZnO 15〜40モル％
Fe2O3 残（好ましくは45〜55モル％）
ガーネツト：ガーネツトには3Y2O3・
5Fe2O3と3Y2O3・5Al2O3とがあり何れも本発
明の方法で製造可能である。その配合割合は
Y2O3：Fe2O3＝３：５又はY2O3：Al2O3＝
３：５である。
スピネル：スピネルはMgO・Al2O3の組成で
あり、配合割合はMgO：Al2O3＝１：１であ
る。
かかる組成の多結晶ブロツクを準備する。この
ブロツクは従来ブロツクに比して、接合面積にお
いて約６倍、体積において約10倍も大きなブロツ
クである。次にこの多結晶体ブロツクの接合面を
ダイヤモンド砥粒で鏡面研摩する。一方では、種
単結晶として、前記多結晶体の接合面と同一表面
積を有する同一組成の単結晶を用意し、同様にそ
の接合面を鏡面研摩する。
その後、種単結晶および多結晶ブロツクの接合
面に、塩酸、硝酸などの強酸を滴下し、ピンセツ
トにより種単結晶を多結晶体に擦り合わせて、単
結晶と多結晶体とを接合した。このときに、多結
晶体の、単結晶体と接合される表面とは反対側の
表面に、ダミー材を貼り付ける。この貼り付け
も、多結晶体およびダミー材の両接合面を鏡面研
摩後強酸を介して行われる。その後貼り付けられ
たダミー材を多結晶体に擦り合わせて接合する。
次に、上述のようにして得られた接合体を、本
発明により加圧治具を用いて圧力0.1Kg／cm2〜250
Kg／cm2で加圧しつつ、温度100℃〜300℃の雰囲気
中で0.1時間以上保持して、接合面を緊密に固着
する。
その後、従来の固相反応法により、この接合体
を、多結晶体の不連続な結晶粒子成長が起こる温
度より低い温度で加熱して、多結晶体全体を単結
晶化する。
以上が本発明の方法の概略である。
次に本発明の方法の要件である種単結晶を多結
晶体に接合する圧力、時間および温度を変化させ
た場合について検討する。
これに使用される多結晶体としては、純度99.9
％の炭酸マンガンを焙焼して得られた酸化マンガ
ンと、純度99.9％の酸化亜鉛および酸化第二鉄と
を原料とし、その組成がMnO＝32モル％、ZnO
＝16モル％、Fe2O3＝52モル％である調合物を成
形し、酸素分圧下で1320℃、４時間焼成してマン
ガン亜鉛フエライト多結晶体を用意する。単結晶
には、上記フエライト多結晶体とほぼ同一組成を
有する高圧ブリツジマン法で製造されたフエライ
ト単結晶を用意する。このフエライト多結晶体と
フエライト単結晶体とから、27×32×13mmのブロ
ツクおよび27×32×0.5mmの板を夫々切り出し、
それぞれの接合面をダイヤモンド砥粒を用いて研
摩した。その後、その接合面に6Nの塩酸を塗布
し、多結晶フエライトブロツクと単結晶フエライ
ト板とを重ね合わせて、擦り合わせた。
このフエライト接合体に対して、次頁の第１表
に示される諸条件にて種単結晶の多結晶体への固
着を行つた。
固着後、フエライト多結晶体の不連続な結晶粒
子成長の起こる1360℃未満の温度である1350℃で
15時間保持し、固相反応を生起させて単結晶体を
得た。
この結果を歩留（％）で第１表に示す。
(Industrial Application Field) The present invention relates to the uniform single crystallization of polycrystals by solid phase reaction, and in particular, the invention relates to the uniform single crystallization of polycrystals by pasting seed single crystals necessary for single crystallizing polycrystals onto polycrystals. It is about the method. (Prior Art) As a conventional method for producing a single crystal, for example, the present applicant previously disclosed a method for producing a single crystal using a solid phase reaction method in Japanese Patent Application Laid-open No. 162496/1983. In this manufacturing method, each bonding surface between a single crystalline material and a polycrystalline material is polished to a mirror surface, and then strong acids such as hydrochloric acid or nitric acid are interposed between the bonding surfaces to bond them, resulting in discontinuous grain growth of the polycrystalline material. Polycrystals were turned into single crystals by gradually heating at a temperature below that temperature. The bonding method at this time is to bring the seed single crystal into contact with the polished surface of the mirror-polished polycrystal through acid, rub the seed single crystal against the polycrystal using tweezers, hold for a certain period of time, and bond. Was. (Problem to be solved by the invention) However, the size of the polycrystal to be single-crystalized using the conventional single-crystal method is, for example, 27 x 5 x 8 mm. In this case, it was difficult for the entire polycrystalline body to become a uniform single crystal, and abnormal growth of the polycrystalline body was sometimes observed due to poor attachment of the seed single crystal.
Therefore, there was a drawback that large single crystals could not be obtained when the yield of single crystals was low. Figures 2a and 2b are perspective views showing typical defective examples, respectively, in which 1 is a seed single crystal, 2 is a polycrystalline body, 3 is a back dummy, 4 is an abnormal crystal growth part, and 5 is a generated single crystal part. It shows. Note that FIG. 2a shows abnormal crystal growth that occurs due to insufficient attachment of the seed single crystal, and FIG. 2b shows abnormal crystal growth that occurs because the material of the polycrystalline body 2 is poor. The purpose of the present invention is to solve the above-mentioned problems,
The object of the present invention is to provide a method for producing a single crystal that can prevent abnormal growth of crystals due to poor seed attachment, etc., and can obtain large single crystals with good yield. (Means for Solving the Problems) The method for producing single crystal ferrite of the present invention involves mirror-polishing the bonding surfaces of polycrystalline ferrite and single crystal ferrite, and bonding the polycrystalline ferrite with an acid interposed between the mirror surfaces. In a method for producing single-crystal ferrite in which single-crystal ferrite is grown in the direction of polycrystalline ferrite by heating at a temperature lower than the discontinuous grain growth temperature of ferrite, the heating for crystal growth is performed. Before heating the bonded body of polycrystalline ferrite and single crystal ferrite to a temperature of 100
The bonding heat treatment is performed under conditions of ~300°C and pressure: 0.1~250Kg/ cm2 . (Function) The thickness of the seed single crystal is preferably up to about 2 mm, but since the area is large compared to the thickness, it is somewhat curved due to processing technology difficulties. For example, the seed single crystal is curved by about 1 μm for 0.5 mm. When this single crystal and polycrystal are bonded together with an acid intervening, the ferrite and acid react at the joint surface, and salts of the ferrite component, such as iron nitrate, iron chloride, and other compounds, are produced. In order to dry this compound layer and fix the single crystal and polycrystal, the bonded body of the single crystal and polycrystal is heated while being pressurized with a constant pressure, so that the compound layer on the bonded surface is almost uniform. dried thinly. The thickness of this compound layer is determined by the pressure applied, and this pressure is 0.1Kg/cm 2 to 250Kg/
Must be cm2 . If the applied pressure is 0.1 Kg/cm 2 or less, the single crystal will be lifted up due to thermal expansion of the compound layer during heating, and therefore the single crystal will peel off during cooling. Furthermore, if the applied pressure is 250 Kg/ cm2 or more, most of the compound layer will flow out during heating, and the single crystal will not be able to resist the force that tries to recover its original curved shape when it is cooled. Crystals peel off. Further, ferrite is a brittle material, and if the pressure exceeds the above-mentioned pressure, it will not be able to withstand the pressure, and the seed single crystal may break. In the actual manufacturing process, it can be carried out using relatively simple equipment, and
The manufacturing cost is also low, so the pressure is 5 to 45.
It is best to set it to Kg/cm 2 . Moreover, the heating temperature needs to be 100°C to 300°C. If the heating temperature is below 100℃, the salts of ferrite components such as iron nitrate, iron chloride, and other compounds present on the joint surface will not decompose (evaporate), and the single crystal will peel off during firing during single crystal growth. , the polycrystalline body no longer becomes a single crystal. Furthermore, if the heating temperature is 300° C. or higher, the ferrite will oxidize, making it necessary to control the atmosphere, and furthermore, the materials of the spacer etc. will be limited, which will increase the cost. In actual production, the heating temperature is preferably set at 140°C to 200°C in consideration of production costs, manufacturing equipment, etc.
Therefore, in the present invention, the seed single crystal and the polycrystalline body can be tightly fixed by uniformly pressurizing with an appropriate pressure and heating for a certain period of time. It is possible to prevent the generation of oriented crystals and obtain good single crystals. Furthermore, as mentioned above, the pressure applied in this bonding process makes the compound layer on the bonding surface almost uniformly thin, but this thin compound layer is formed by salting out the ferrite component during heating during the subsequent solid phase reaction. is decomposed to form a thin oxide layer, and this thin oxide layer has the effect of promoting the desired solid phase reaction. (Example) Examples of the present invention will be described in detail below. Although the method for producing a single crystal of the present invention can be applied to polycrystals of any composition, the following compositions are actually preferred. Ferrite MnO 20-40 mol% ZnO 5-3 mol% Fe 2 O 3 remainder (preferably 48-60 mol%) Ferrite NiO 15-40 mol% ZnO 15-40 mol% Fe 2 O 3 remainder (preferably 45-60 mol%) 55 mol%) Garnet: Garnet contains 3Y 2 O 3 .
There are 5Fe 2 O 3 and 3Y 2 O 3 .5Al 2 O 3 , both of which can be produced by the method of the present invention. The mixing ratio is
Y 2 O 3 :Fe 2 O 3 =3:5 or Y 2 O 3 :Al 2 O 3 =
The ratio is 3:5. Spinel: Spinel has a composition of MgO.Al 2 O 3 and the blending ratio is MgO:Al 2 O 3 =1:1. A polycrystalline block having such a composition is prepared. This block is approximately 6 times larger in bonding area and approximately 10 times larger in volume than the conventional block. Next, the joint surfaces of this polycrystalline block are mirror polished with diamond abrasive grains. On the other hand, a single crystal having the same composition and having the same surface area as the bonding surface of the polycrystalline body is prepared as a seed single crystal, and the bonding surface is mirror-polished in the same manner. Thereafter, a strong acid such as hydrochloric acid or nitric acid was dropped onto the bonding surfaces of the seed single crystal and the polycrystalline block, and the seed single crystal was rubbed against the polycrystal using tweezers to bond the single crystal and the polycrystal. At this time, a dummy material is attached to the surface of the polycrystalline body opposite to the surface to be joined to the single crystalline body. This attachment is also carried out by mirror polishing both the joint surfaces of the polycrystalline body and the dummy material, and then using strong acid. After that, the pasted dummy material is rubbed against the polycrystalline body and bonded. Next, the bonded body obtained as described above is subjected to a pressure of 0.1 kg/cm 2 to 250 using a pressing jig according to the present invention.
While applying pressure at Kg/cm 2 , the joint is held in an atmosphere at a temperature of 100°C to 300°C for 0.1 hour or more to firmly bond the joint surfaces. Thereafter, by a conventional solid phase reaction method, this joined body is heated at a temperature lower than the temperature at which discontinuous crystal grain growth of the polycrystalline body occurs, thereby converting the entire polycrystalline body into a single crystal. The above is an outline of the method of the present invention. Next, the case where the pressure, time and temperature for joining the seed single crystal to the polycrystal, which are requirements of the method of the present invention, are changed will be considered. The polycrystal used for this has a purity of 99.9
The raw materials are manganese oxide obtained by roasting % manganese carbonate, zinc oxide and ferric oxide with a purity of 99.9%, and the composition is MnO = 32 mol%, ZnO
= 16 mol% and Fe 2 O 3 = 52 mol% is molded and fired at 1320° C. for 4 hours under oxygen partial pressure to prepare a manganese zinc ferrite polycrystal. As the single crystal, a ferrite single crystal manufactured by the high-pressure Bridgeman method and having almost the same composition as the ferrite polycrystal is prepared. A 27 x 32 x 13 mm block and a 27 x 32 x 0.5 mm plate were cut out from this ferrite polycrystal and ferrite single crystal, respectively.
Each joint surface was polished using diamond abrasive grains. Thereafter, 6N hydrochloric acid was applied to the joint surfaces, and the polycrystalline ferrite block and single-crystal ferrite plate were stacked and rubbed together. A seed single crystal was fixed to the polycrystalline body of this ferrite bonded body under the conditions shown in Table 1 on the next page. After fixation, at 1350°C, which is a temperature below 1360°C where discontinuous grain growth of ferrite polycrystals occurs.
The mixture was held for 15 hours to cause a solid phase reaction to obtain a single crystal. The results are shown in Table 1 in terms of yield (%).
【表】
第１表から明らかなように、加圧圧力0.1〜250
Kg／cm2、加圧温度100℃〜300℃の範囲で歩留70％
以上となり、種貼付不十分等に起因する多結晶フ
エライトの異常成長が少なく良好な結果が得られ
ている。
このように加圧時の温度および加圧時間につい
ては、或る一定値以上を選定すればよいが、加圧
圧力については、種単結晶と多結晶体との接合面
積に応じて、特定の圧力を有することが分る。そ
のため、加熱・加圧中に多結晶フエライトおよび
種単結晶が熱膨張しても、加圧圧力が変化しない
ような加圧治具を必要とする。この加圧治具は、
一例をあげれば、第１図Ａ，Ｂに示すものがあ
る。第１図Ａに示す加圧治具は、弾性的に押圧し
得るクリツプ１０の間に、圧力を均等に加えるた
めの押え板１１と種単結晶への傷つきを防止する
ためのテフロン１２を介して種単結晶１、多結晶
体２およびバツクダミー３を配置して加圧するも
のである。また、第２図Ｂに示す加圧治具は、ば
ねクランプ２０によりテフロン１２を介して同様
に加圧するものである。
（発明の効果）
本発明は製造法では、種単結晶が多結晶体に緊
密に固着されるため、単結晶成長すべき多結晶体
ブロツクを、従来に比べて大きくすることがで
き、しかも歩留も良好にすることができる。[Table] As is clear from Table 1, pressurization pressure 0.1 to 250
Kg/cm 2 , yield 70% at pressurizing temperature range of 100℃ to 300℃
As described above, good results were obtained with less abnormal growth of polycrystalline ferrite due to insufficient seed attachment. In this way, the temperature and pressurizing time during pressurization may be selected to be above a certain value, but the pressurizing pressure may be set at a specific value depending on the bonding area between the seed single crystal and the polycrystalline body. It can be seen that there is pressure. Therefore, a pressurizing jig is required that does not change the pressurizing pressure even if the polycrystalline ferrite and the seed single crystal expand thermally during heating and pressurizing. This pressure jig is
An example is shown in FIGS. 1A and 1B. The pressing jig shown in FIG. 1A has a holding plate 11 for applying pressure evenly and a Teflon 12 for preventing damage to the seed single crystal between clips 10 that can be pressed elastically. A seed single crystal 1, a polycrystalline body 2, and a back dummy 3 are arranged and pressurized. Further, the pressurizing jig shown in FIG. 2B similarly applies pressure via the Teflon 12 using a spring clamp 20. (Effects of the Invention) In the production method of the present invention, since the seed single crystal is tightly fixed to the polycrystal, the polycrystalline block to be grown as a single crystal can be made larger compared to the conventional method, and at a faster speed. The retention can also be improved.
第１図Ａ，Ｂはそれぞれ本発明の方法に使用さ
れる加圧治具の一例を示す説明図、第２図ａ，ｂ
はそれぞれ典型的な不良例を示す斜視図である。
１……種単結晶、２……多結晶体、３……バツ
クダミー、４……異常結晶成長部。
Figures 1A and B are explanatory diagrams showing an example of a pressurizing jig used in the method of the present invention, and Figures 2a and b are respectively
are perspective views showing typical defective examples. 1... Seed single crystal, 2... Polycrystalline body, 3... Back dummy, 4... Abnormal crystal growth part.
Claims (1)
面を鏡面研磨し、その鏡面間に酸を介在させて接
合し、多結晶フエライトの不連続粒成長温度未満
の温度で加熱して、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
を得る単結晶フエライトの製造法において、前記
結晶成長のための加熱を行う前に、前記多結晶フ
エライトと単結晶フエライトとの接合体を、加熱
温度：100〜300℃、加圧圧力：0.1〜250Kg／cm2の
条件で接合熱処理をすることを特徴とする単結晶
フエライトの製造法。1. The joint surfaces of polycrystalline ferrite and single-crystal ferrite are polished to a mirror surface, and the joint is bonded with acid interposed between the mirror surfaces. The single-crystal ferrite is heated at a temperature lower than the discontinuous grain growth temperature of polycrystalline ferrite. In a method for producing single crystal ferrite in which single crystal ferrite is obtained by growing crystals in the crystal ferrite direction, before heating for crystal growth, the joined body of the polycrystal ferrite and single crystal ferrite is heated at a heating temperature: A method for producing single-crystal ferrite, characterized by carrying out bonding heat treatment under conditions of 100 to 300°C and pressure: 0.1 to 250 Kg/ cm2 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4045887A JPS63210091A (en) | 1987-02-25 | 1987-02-25 | Production of single crystal ferrite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4045887A JPS63210091A (en) | 1987-02-25 | 1987-02-25 | Production of single crystal ferrite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63210091A JPS63210091A (en) | 1988-08-31 |
| JPH0561238B2 true JPH0561238B2 (en) | 1993-09-03 |
Family
ID=12581201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4045887A Granted JPS63210091A (en) | 1987-02-25 | 1987-02-25 | Production of single crystal ferrite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63210091A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0624899A (en) * | 1992-03-31 | 1994-02-01 | Ngk Insulators Ltd | Production of composite-type ferrite |
-
1987
- 1987-02-25 JP JP4045887A patent/JPS63210091A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63210091A (en) | 1988-08-31 |
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