JPH0193500A - Growth of fe-si-al alloy single crystal - Google Patents
Growth of fe-si-al alloy single crystalInfo
- Publication number
- JPH0193500A JPH0193500A JP24749087A JP24749087A JPH0193500A JP H0193500 A JPH0193500 A JP H0193500A JP 24749087 A JP24749087 A JP 24749087A JP 24749087 A JP24749087 A JP 24749087A JP H0193500 A JPH0193500 A JP H0193500A
- Authority
- JP
- Japan
- Prior art keywords
- rod
- single crystal
- alloy
- crucible
- heating means
- 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.)
- Pending
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 41
- 229910000838 Al alloy Inorganic materials 0.000 title description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 24
- 239000000956 alloy Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 20
- 229910002796 Si–Al Inorganic materials 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本発明は磁気ヘッド等の磁気製品に使用されるＦｅ−Ｓ
ｉ−Ａｌ系合金単結晶の育成法に関し、とくに大口径の
単結晶を形成するのに好適なＦｅ−Ｓｉ −Ａｉ系合金
単結晶の育成法に関する。[Detailed Description of the Invention] <Industrial Application Field> The present invention is directed to Fe-S used in magnetic products such as magnetic heads.
The present invention relates to a method for growing an i-Al alloy single crystal, and particularly to a method for growing a Fe-Si-Ai alloy single crystal suitable for forming a large-diameter single crystal.
〈従来の技術〉
第６図は従来の電子ビーム帯溶融法を用いたＦｅ −Ｓ
ｉ 、−Ａｌ系合金単結晶の育成法を示す図である。<Prior art> Figure 6 shows Fe-S using the conventional electron beam belt melting method.
FIG. 3 is a diagram showing a method for growing a single crystal of an -Al-based alloy.
Ｆｅ−Ｓｉ−Ａｎ系合金の多結晶からなる丸棒試料１を
下部チャック２及び上部チャック３に固定し、その丸棒
試料ｌに真空雰囲気で、フィラメント４、電源７を備え
た電子銃５から発生する電子ビームを照射して溶融帯１
ａを形成し、電子・銃５を駆動部６により下部から−Ｌ
部へ除々に移動することによりＦｅ−Ｓｉ−Ａｉ系合金
の単結晶をｒｆ成する。A round bar sample 1 made of polycrystalline Fe-Si-An alloy is fixed to a lower chuck 2 and an upper chuck 3, and an electron gun 5 equipped with a filament 4 and a power source 7 is attached to the round bar sample 1 in a vacuum atmosphere. Melt zone 1 is irradiated with the generated electron beam.
a, and the electron/gun 5 is driven from the bottom by the drive unit 6 to -L.
A single crystal of Fe-Si-Ai alloy is formed by RF.
又、他の従来例として一般にブリッジマン法と呼ばれる
ｆｆ成法がある。これはルツボに上記多結晶の大杯試料
を収納してルツボの外部に設けられた高周波加熱コイル
により、上記丸棒試料を溶融し、そのルツボあるいは高
周波加熱コイルを移動させ、溶融された試料を除々に冷
却し、その冷却部を単結晶にする育成法である。Further, as another conventional example, there is an ff formation method generally called the Bridgman method. This involves storing the large polycrystalline sample in a crucible, melting the round bar sample using a high-frequency heating coil installed outside the crucible, and then moving the crucible or high-frequency heating coil to heat the molten sample. This is a growth method in which the crystal is gradually cooled and the cooled portion is made into a single crystal.
〈発明が解決しようとする■１題点〉
しかしながら、上記電子ビーム帯溶融法によるＦｅ−５
ｉ−Ａｌ系合金単結晶の育成法では、丸棒試料の径が大
きくなると、溶融帯１ａが寸法的に大きくなり、このた
め溶融物が外へ流れ出してしまう等の問題点がある。<■1 problem to be solved by the invention> However, Fe-5 by the above electron beam belt melting method
In the method of growing an i-Al alloy single crystal, when the diameter of the round bar sample becomes large, the molten zone 1a becomes dimensionally large, which causes problems such as the melt flowing out.
又、ブリッジマン法によるＦｅ−Ｓｉ−Ａｎ系合金単結
晶の育成法では、多結晶の丸棒試料全体を溶融するので
重力及び蒸発による組成偏析が大きいという問題点があ
る。Furthermore, in the Bridgman method for growing Fe-Si-An alloy single crystals, the entire polycrystalline round rod sample is melted, so there is a problem in that compositional segregation due to gravity and evaporation is large.
そこで１本発明は、上記育成法における問題点を解決す
べく大口径のＦｅ−Ｓｉ−Ａｌｌ系合金単結晶の育成法
を目的としたものである。Therefore, one object of the present invention is to provide a method for growing a large-diameter Fe-Si-All alloy single crystal in order to solve the problems in the above-mentioned growth method.
く問題点を解決するための手段及び作用〉上記問題点を
解決するために本発明では、Ｆｅ、Ｓｉ、ＡｆＬの原料
を非酸化性の雰囲気中で加熱溶解してＦＦｅ−Ｓｉ−Ａ
系合金の多結晶棒を作製する工程と、該多結晶棒をルツ
ボ内に収納し、かつそれぞれを固定する工程と、加熱手
段で該ルツボを介して該多結晶棒の一部を溶解する工程
と、該加熱手段と該多結晶棒とを該多結晶棒の長手方向
に沿って相対的に除々に移動させてＦｅ−Ｓｉ−Ａ立県
合金の単結晶を成長させる工程とからなるＦｅ−Ｓｉ−
Ａｎ系合金単結晶の育成法である。Means and operation for solving the above problems> In order to solve the above problems, in the present invention, raw materials of Fe, Si, and AfL are heated and melted in a non-oxidizing atmosphere to form FFe-Si-A.
A step of producing a polycrystalline rod of a system alloy, a step of storing the polycrystalline rod in a crucible and fixing each, and a step of melting a part of the polycrystalline rod through the crucible using heating means. and a step of growing a single crystal of Fe-Si-A Riken alloy by gradually moving the heating means and the polycrystalline rod relative to each other along the longitudinal direction of the polycrystalline rod. Si-
This is a method for growing an An-based alloy single crystal.
Ｆｅ−Ｓｉ−Ａｌ系合金単結晶を上記育成法とすること
により、大口径の単結晶を育成する。A large-diameter single crystal is grown by using the above-mentioned growth method for a Fe-Si-Al alloy single crystal.
〈実施例〉
次に本発明になるＦｅ−Ｓｉ−Ａｌ系合金単結晶の育成
法の実施例について説明する。第１図は原料から（ｆ成
までのフローチャートである。このフローチャートに従
って本実施例を述べる。まず、高純度の原料例えば、Ｆ
ｅ９９．９８％、５ｉ９９．９９９％、Ａｌ９９．９９
９％の純度のＦｅ、Ｓｉ、Ａｌ原料を川、ｔｉする０次
に上記原料をＦｅ８３．５％、Ｓｉ９．５％、Ａｌ６．
０％の割合で秤２課して、これら秤量したＦｅ、Ｓｉ。<Example> Next, an example of the method for growing a Fe-Si-Al alloy single crystal according to the present invention will be described. FIG. 1 is a flowchart from the raw material to (f) formation. This example will be described according to this flowchart. First, a high-purity raw material, for example, F
e99.98%, 5i99.999%, Al99.99
Fe, Si, and Al raw materials with a purity of 9% are then mixed with Fe83.5%, Si9.5%, Al6.
Fe and Si were weighed using two scales at a ratio of 0%.
Ａｉ原料１を第２図に示す真空溶解鋳造装置のアルミナ
製ルツボ９に入れ、真空状態又は不活性ガス中の非酸化
性雰囲気で高周波コイル１ｏにより加熱溶解（溶湯１４
）する０次に、第２図の矢印４９口、への如くアルミナ
製ルツボ９内の溶湯１４を鉄製金型に鋳込んで多結晶の
丸棒試料１１を作成する０次に第３図の如く丸棒試料１
１をらせん状に形成された高周波加熱コイル２１内に貫
装され、下端の細径部を下部チャック１２で固定された
アルミナ製ルツボ２０内に収納し、その上端を上部チャ
ック１３で固定する。２２は高周波加熱コイル２１を上
下に移動する駆動部である。第４図、第５図は丸棒試料
１１を用いてＦｅ−３ｔ−Ａｎ系合金の単結晶を育成す
る様子を示す図である。第４図は単結晶の育成が開始さ
れる前の状態で、ルツボ２０の細径部内には予め種結晶
２３が納められ、駆動部２２により高周波加熱コイル２
１が種結晶の付近に位置している。この状態で高周波加
熱コイル２１に電流が流れ、丸棒試料ｌｌの下部が溶融
され、駆動部２２により高周波加熱コイル２１が図面上
方に除々に移動する。第５図は高周波加熱コイル２１が
移動した状態で、高周波加熱コイル２１によって加熱さ
れた部分（符号Ａ）が溶融状態になり、Ａ部より下の部
分は冷却されて、種結晶２３と同じ結晶方向の単結晶が
形成される。ここで、高周波加熱コイル２１の加熱によ
って生じる丸棒試料１１の溶融物はルツボ２０の存在に
より、外部に流れ出ないようになっており、又高周波加
熱コイル２１により多結晶の丸棒試料の一部のみを溶融
しているので重力及び革発による組成偏析を少なくして
いる。第５図の状態から駆動部２２により高周波加熱コ
イルが−Ｆ方に移動するにつれて溶融部Ａは下部より冷
却されて単結晶が形成される。そして高周波加熱コイル
２１がルツボ２０の上端付近にいたるまで駆動され、冷
却後ルツボ２０から単結晶化された丸棒試料を抜出し、
これによりＦｅ−Ｓｉ−Ａｎ系合金の単結晶ＹＴ成が終
了する。Ai raw material 1 is placed in an alumina crucible 9 of a vacuum melting and casting apparatus shown in FIG. 2, and heated and melted (molten metal 14
)Next, as indicated by arrow 49 in Fig. 2, the molten metal 14 in the alumina crucible 9 is cast into an iron mold to create a polycrystalline round rod sample 11.Next, as shown in Fig. 3 Gotoku round bar sample 1
1 is passed through a high-frequency heating coil 21 formed in a spiral shape, and the narrow diameter part at the lower end is housed in an alumina crucible 20 fixed with a lower chuck 12, and its upper end is fixed with an upper chuck 13. 22 is a drive unit that moves the high frequency heating coil 21 up and down. FIG. 4 and FIG. 5 are diagrams showing how a single crystal of Fe-3t-An alloy is grown using the round bar sample 11. FIG. 4 shows a state before single crystal growth is started, in which a seed crystal 23 is placed in the small diameter part of the crucible 20, and a high-frequency heating coil 2 is driven by the drive unit 22.
1 is located near the seed crystal. In this state, a current flows through the high-frequency heating coil 21, the lower part of the round bar sample 11 is melted, and the high-frequency heating coil 21 is gradually moved upward in the drawing by the drive section 22. FIG. 5 shows a state in which the high-frequency heating coil 21 has been moved, and the part (symbol A) heated by the high-frequency heating coil 21 is in a molten state, and the part below part A is cooled, and the same crystal as the seed crystal 23 is crystallized. oriented single crystals are formed. Here, the presence of the crucible 20 prevents the melt of the round bar sample 11 generated by the heating of the high frequency heating coil 21 from flowing out, and the high frequency heating coil 21 prevents a part of the polycrystalline round bar sample from flowing out. Since only the molten metal is melted, compositional segregation due to gravity and revolution is reduced. As the high-frequency heating coil is moved in the -F direction by the drive unit 22 from the state shown in FIG. 5, the melted zone A is cooled from the bottom and a single crystal is formed. Then, the high-frequency heating coil 21 is driven to near the upper end of the crucible 20, and after cooling, the single-crystalized round bar sample is extracted from the crucible 20.
This completes the single crystal YT formation of the Fe-Si-An alloy.
なお、上記説明中、高周波加熱コイル２１を移動させた
が、高周波加熱コイル２１を固定して丸棒試料１１及び
ルツボ２０を上、下部チャック１２．１３と共に移動さ
せてもよい。In the above description, the high-frequency heating coil 21 was moved, but the high-frequency heating coil 21 may be fixed and the round bar sample 11 and the crucible 20 moved together with the upper and lower chucks 12 and 13.
〈発明の効果〉
上述の如く、本発明になるＦｅ−Ｓｉ−Ａｌ系合金単結
晶の育成法は、Ｆｅ、Ｓｉ、Ａｌの原料を非酸化性の雰
囲気中で加熱溶解してＦｅ−Ｓｉ−Ａｌ系合金の多結晶
棒を作製する工程と、該多結晶棒をルツボ内に収納し、
かつそれぞれを固定する工程と、加熱手段で該ルツボを
介して該多結晶の一部を溶解する工程と、該加熱手段と
該多結晶棒とを該多結晶棒の長手方向に沿って相対的に
除々に移動させてＦｅ−Ｓｉ−Ａｎ系合金の単結晶を成
長させる工程とからなるため、単結晶育成時における溶
融物の流出を防止し得、大口径で組成偏析の少ない単結
晶を育成できる等の効果を有する。<Effects of the Invention> As described above, the method for growing the Fe-Si-Al alloy single crystal according to the present invention is to heat and melt raw materials of Fe, Si, and Al in a non-oxidizing atmosphere to produce Fe-Si- A step of producing a polycrystalline rod of an Al-based alloy, storing the polycrystalline rod in a crucible,
and a step of fixing each, a step of melting a part of the polycrystal through the crucible with heating means, and a step of moving the heating means and the polycrystalline rod relative to each other along the longitudinal direction of the polycrystalline rod. This process consists of the step of growing a single crystal of a Fe-Si-An alloy by gradually moving the metal to a single crystal, which prevents the melt from flowing out during single crystal growth, and grows a single crystal with a large diameter and less compositional segregation. It has the effect of being able to.
第１図〜第５図は本発明に係るＦｅ−Ｓｉ−Ａｌ系合金
の単結晶の育成法の実施例を示し、第１図は原料から育
成までのフロチャート、第２図は真空溶解鋳造装置の概
略図、第３図は単結晶育成装置の概略図、第４図は単結
晶育成開始前の状態を示す断面図、第５図は単結晶育成
時の状態を示す断面図、第６図は従来の単結晶装置の概
略図である。
１．１１・・・丸棒試料、２，１２・・・下部チャック
、３．１３・・・１一部チャック、 ２０・・・
ルツボ、２１・・・高周波加熱コイル、 ２２・・・
駆動部。
２３・・・種結晶、 Ａ・・・溶融部第１図
第２図
第３図 第６図
第４図
第５図Figures 1 to 5 show an example of the method for growing a single crystal of Fe-Si-Al alloy according to the present invention, with Figure 1 being a flowchart from raw materials to growth, and Figure 2 being vacuum melting and casting. 3 is a schematic diagram of the single crystal growth device, FIG. 4 is a sectional view showing the state before starting single crystal growth, FIG. 5 is a sectional view showing the state during single crystal growth, and FIG. 6 is a schematic diagram of the device. The figure is a schematic diagram of a conventional single crystal device. 1.11...Round bar sample, 2,12...Lower chuck, 3.13...1 part chuck, 20...
Crucible, 21...High frequency heating coil, 22...
Drive part. 23... Seed crystal, A... Melting part Figure 1 Figure 2 Figure 3 Figure 6 Figure 4 Figure 5
Claims (1)
解してＦｅ−Ｓｉ−Ａｌ系合金の多結晶棒を作製する工
程と、該多結晶棒をルツボ内に収納し、かつそれぞれを
固定する工程と、加熱手段で該ルツボを介して該多結晶
棒の一部を溶解する工程と、該加熱手段と該多結晶棒と
を該多結晶棒の長手方向に沿って相対的に除々に移動さ
せてＦｅ−Ｓｉ−Ａｌ系合金の単結晶を成長させる工程
とからなるＦｅ−Ｓｉ−Ａｌ系合金単結晶の育成法。A step of heating and melting raw materials of Fe, Si, and Al in a non-oxidizing atmosphere to produce a polycrystalline rod of Fe-Si-Al alloy, and storing the polycrystalline rod in a crucible and melting each of them. a step of fixing a part of the polycrystalline rod through the crucible using heating means; and a step of gradually separating the heating means and the polycrystalline rod from each other along the longitudinal direction of the polycrystalline rod. A method for growing a single crystal of an Fe-Si-Al alloy, comprising the step of growing a single crystal of an Fe-Si-Al alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24749087A JPH0193500A (en) | 1987-09-30 | 1987-09-30 | Growth of fe-si-al alloy single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24749087A JPH0193500A (en) | 1987-09-30 | 1987-09-30 | Growth of fe-si-al alloy single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0193500A true JPH0193500A (en) | 1989-04-12 |
Family
ID=17164242
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24749087A Pending JPH0193500A (en) | 1987-09-30 | 1987-09-30 | Growth of fe-si-al alloy single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0193500A (en) |
-
1987
- 1987-09-30 JP JP24749087A patent/JPH0193500A/en active Pending
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