JPS62202033A - Method and apparatus for zone refining - Google Patents
Method and apparatus for zone refiningInfo
- Publication number
- JPS62202033A JPS62202033A JP61042993A JP4299386A JPS62202033A JP S62202033 A JPS62202033 A JP S62202033A JP 61042993 A JP61042993 A JP 61042993A JP 4299386 A JP4299386 A JP 4299386A JP S62202033 A JPS62202033 A JP S62202033A
- Authority
- JP
- Japan
- Prior art keywords
- zone
- purified
- impurities
- refining
- boat
- 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
- 238000007670 refining Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims description 17
- 239000012535 impurity Substances 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 230000006698 induction Effects 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000002826 coolant Substances 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 239000012264 purified product Substances 0.000 claims 1
- 238000002844 melting Methods 0.000 abstract description 11
- 230000008018 melting Effects 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 10
- 239000010453 quartz Substances 0.000 abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- 229910002804 graphite Inorganic materials 0.000 abstract description 6
- 239000010439 graphite Substances 0.000 abstract description 6
- 239000000498 cooling water Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 239000010949 copper Substances 0.000 abstract description 2
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000000746 purification Methods 0.000 description 13
- 229910052782 aluminium Inorganic materials 0.000 description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 11
- 230000000694 effects Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910052776 Thorium Inorganic materials 0.000 description 3
- 229910052770 Uranium Inorganic materials 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、偏析を利用して。種々の金属および半導体
、あるいはその他無機材料並びに宵機材料の精製Ｃ二個
用されるゾーン精製方法および装置に関し、特に、加熱
手段として高周波誘導加熱な利用するゾーンｎ製方法お
よび装置において１歩留りよく、シかも迅速にこれらの
材料を精製できるよう（二改良されたゾーンｎ製方法お
よび装置（：関するものである。[Detailed Description of the Invention] [Industrial Application Field] This invention utilizes segregation. Regarding the zone refining method and apparatus used for the purification of various metals and semiconductors, or other inorganic materials and organic materials, in particular, the zone refining method and apparatus using high frequency induction heating as the heating means has a high yield. The present invention relates to an improved Zone N manufacturing method and apparatus (2), which allows for the rapid purification of these materials.
一般に溶融状態にろる物質を徐々に凝固させると、偏析
によって、不純物は後で凝固し九部分に集まり、先に凝
固した部分の不純物製電は低下するので、その不純物が
集中した部分を切取って除去すれば、不純物良質の低下
した部分、すなわち精製された部分を得ることができる
ので、その精製効率を高めるｔめ１例えば金属や半導体
な棒状体（−成形し、それを長手方向に移動させながら
帯状の加熱帯域に通すことによって、その棒状体におい
て幅の狭い溶融帯（ゾーン）を数回繰返して通過させ、
その中の不純物を一端に効率よく掃き寄せて、これらの
材料を精製するゾーン・メルティング、すなわちゾーン
ｎ製法が近年盛んに利用されるようになつ九。In general, when a substance that melts into a molten state is gradually solidified, the impurities solidify later due to segregation and collect in 9 parts, and the impurity production in the part that solidifies first decreases, so the part where the impurities are concentrated is cut. By removing the impurities, you can obtain a refined part, which is a refined part.The purpose of this is to increase the purification efficiency. By passing through a belt-shaped heating zone while moving, the rod-shaped body is repeatedly passed through a narrow melting zone (zone) several times,
In recent years, zone melting, or the zone n manufacturing method, which purifies these materials by efficiently sweeping away impurities in them, has come into widespread use9.
このゾーン精製法によると、金属や半導体中に混在する
極〈微量の不純物も除去されて、非常に線間の高い製品
が得られるので、ゾーン精整法は。According to this zone refining method, extremely small amounts of impurities mixed in metals and semiconductors are removed, and products with extremely high line density can be obtained, so the zone refining method is
極めて高い特品紳闇が要求されるとともに、精製工程中
にこうむる汚染を極端に嫌う隠子材料の精製または映造
において今日広く採用されており。It is widely used today in the refining or imaging of secret materials, which require extremely high standards of confidentiality and are extremely sensitive to contamination during the refining process.
例えば半導体デバイス内の配線および成極材料として供
給される高純電アルミニウム中の極〈機敏のウランおよ
びトリウムを除去するのに好都合に利用されている。For example, it is advantageously used to remove extremely sensitive uranium and thorium from high-purity electrolytic aluminum, which is supplied as wiring and polarization material in semiconductor devices.
前記ゾーン精製法は種々の方法で遂行されるが。The zone purification process can be accomplished in a variety of ways.
それは１例えば、棒状体に成形した被精製物を。For example, the product to be purified is shaped into a rod.
そのまま、６るいは大気中のほこりによって製品が汚染
されるのを防ぐために、真空中または不活性ガス雰囲気
中において、高周波誘導加熱によって帯状の局部的な加
熱が引起される加熱帯域に通過させて、その被精製物に
おいて先端から末端へ次第に移動する溶融帯な形成させ
、それＣ二よって被精製物中に含まれる不純物を順次溶
融帯の中へ寄せ集めて、その不純物が集積された最終凝
固部を被精製物の末端部分に形成させ、ついで、その末
端部分を取除いて、それ以外の部分、すなわち精をされ
た部分？得るという方法によって遂行される。In order to prevent the product from being contaminated by dirt or dust in the atmosphere, it is passed through a heating zone in which localized band-like heating is induced by high-frequency induction heating in a vacuum or in an inert gas atmosphere. , a molten zone is formed in the object to be purified that gradually moves from the tip to the end, and thereby impurities contained in the object to be purified are successively gathered into the molten zone, resulting in final solidification where the impurities are accumulated. A part is formed on the end part of the object to be purified, and then the end part is removed and the other part, that is, the purified part? It is accomplished by the method of obtaining.
このようにゾーン精整法は、ある幅の溶融帯を被精製物
中（二逼過させて、その中の不純物を被精製物の一端に
掃き寄せるものでるるから、その幅が広いほど、その不
純物が掃き寄せられて切取られる最終凝固部の幅も広く
なって、１Ｍ品の歩留り。In this way, the zone refining method involves passing a molten zone of a certain width through the object to be purified, and sweeping the impurities therein to one end of the object. The width of the final solidified part where the impurities are swept away and cut is also wider, resulting in a 1M product yield.
すなわち精製効率（精製部の長さ／全長）が低下すると
いう性格を有し、そして加熱手段として上述のような高
周波誘導加熱を使用するゾーンＮ１１！法においては、
その高周波出力を増大させると溶融帯の幅が広くなって
製品の精製効率が悪くなるところから、従来その出力を
低く１例えば上述のアルミニウムのｎ９Ｊの場合、ｓｘ
ｗａ下のように低くしていたが、出力を低下させると溶
融帯中の攪拌が不十分で、精＠凝固部と溶融帯との境界
付近において不純物が濃縮されや丁＜、シたがって積装
後に不純物濃邸の高い領域が精製部の方に広がるため、
切取るべき部分が拡大してｆｆｔ製効率が悪くなるとい
う問題がめり、しかも出力が低いと上述のように溶融帯
における攪拌が十分でないために精製効果（不純物分離
効果）が小さく、シたがって溶融帯の移動速ずを速くす
ることができないので、従来のゾーン精整法は生産性が
低いという問題！１あった。In other words, zone N11 has the characteristic that the refining efficiency (length of the refining section/total length) decreases, and uses the above-mentioned high-frequency induction heating as the heating means! In law,
If the high frequency output is increased, the width of the molten zone becomes wider and the refining efficiency of the product becomes worse.
However, when the power is lowered, stirring in the melting zone is insufficient, and impurities are concentrated near the boundary between the coagulation zone and the melting zone. After refining, the area with high concentration of impurities spreads toward the refining section.
The problem arises that the part to be cut expands and fft production efficiency deteriorates, and if the output is low, the purification effect (impurity separation effect) is small due to insufficient stirring in the melting zone as described above, and therefore The problem with conventional zone refining methods is that productivity is low because the moving speed of the molten zone cannot be increased! There was 1.
〔研究に基づく５見事項〕
そこで本発明者等は、上述のような従来ゾーン精整法の
問題を解決すべく種々研究した結果。[Five observations based on research] The inventors of the present invention have conducted various studies to solve the problems of the conventional zone adjustment method as described above.
高周波誘導コイルによって供給される磁力の大きさの分
布は、そのコイルから最も近い場所を頂点として左右に
裾を伸ばした山形ななすので、その供給電力を増大させ
ると、その山の裾野は広がって、溶融帯の幅も広がるが
、力■熱帯域から出た被ｎ＠物の精製部を冷却媒体によ
って強制冷却すると、溶融帯が狭くなるとともに、狭い
幅の中（＝高出力が集中して溶融帯における攪拌作用が
高まることによって、溶融帯と精＠！凝固部との境界付
近に不純物が集中しなくなって、最後に除去丁べき不純
物濃邸の高い部分の幅も狭くなり、また溶融帯の移動迷
電を高めても精製部の線間が低下することがなく、さら
にこの冷却媒体による急冷によって焼入効果も得られる
こと。The distribution of the magnitude of the magnetic force supplied by a high-frequency induction coil is shaped like a mountain with the peak located at the point closest to the coil and the skirts extending from side to side.As the supplied power increases, the base of the mountain widens. , the width of the molten zone also widens, but if the purified part of the material coming out of the tropical zone is forcibly cooled with a cooling medium, the molten zone becomes narrower and the width of the molten zone (= high power is concentrated). By increasing the stirring action in the molten zone, impurities no longer concentrate near the boundary between the molten zone and the solidified zone, and the width of the high part of the impurity concentration that should be removed at the end becomes narrower. Even if the moving stray electricity is increased, the line spacing of the refining section will not decrease, and furthermore, the quenching effect can be obtained by rapid cooling with this cooling medium.
を見出した。I found out.
〔問題点を解決するための手段］
この発明は、上記知見に基づいて発明されたもので、ゾ
ーン＃製方法および装置において精製効率と精製速すを
向上させ、さらに焼入効果も付加的に得ることを目的と
し。[Means for Solving the Problems] This invention was invented based on the above knowledge, and improves the refining efficiency and refining speed in the zone # manufacturing method and apparatus, and additionally improves the quenching effect. with the aim of obtaining.
（１）真空中または不活性ガス雰囲気中において。(1) In a vacuum or in an inert gas atmosphere.
長手方向に沿って移動する棒状の襟ｎ製物を、高周波誘
導加熱Ｃ二よって帯状の局部的な加熱が引起されるカロ
熱帯域に適過させて、その被精製物において先端から末
端へ次第に移動する浴融帯を形成させ、それによって、
前記被精製物中（：含まれる不純物を順次溶融帯の中へ
寄せ集めて、＠記被精侍物において、その不純物が集積
された最終凝固部？前記被精製物の末端部分（−形成さ
せるとともに、前記不純物が除かれた精製部をその末端
部分以外の部分に形成させ、・ついで、不純物が集積し
た前記末端部分な取除くこと（二よって前記被精特物？
精製するゾーン精製方法において、前記加熱帯域から出
た被精製物を冷却媒体によって冷却することを特徴とす
る。前記ゾーン精製方法、および
（２）ト・内部が真空または不活性ガス雰囲気に保持さ
れた耐熱性へウジング、牽引装置と連結してそのハウジ
ング内に入れられた被精製物収納用のボート状容器、お
よび前記ハウジングの外側を所定の幅で囲む高周波誘導
加熱コイルが備えられたゾーン精製装置１Ｃ：おいて、
前記高周波誘導加熱コイルで囲まれ丸帯状の空間を境と
して部分される前記ハウジング中の空間領域のうち、前
記被精製物が前記帯状空間を出て牽引されていく側に、
＠記ボート状容器と接触する冷却板？設けたことを特徴
とする。＠記ゾーン′！ｆ４製装置。A rod-shaped product moving along the longitudinal direction is applied to the Calorie zone where localized band-like heating is caused by high-frequency induction heating, and the product is gradually heated from the tip to the end of the product to be purified. forming a moving bath melt zone, thereby
The impurities contained in the object to be purified are successively collected into the molten zone, and the final solidified part where the impurities are accumulated in the object to be purified is formed. At the same time, a purified part from which the impurities are removed is formed in a part other than the end part, and then the end part where the impurities have accumulated is removed (2) the purified part?
The zone refining method is characterized in that the product to be purified exiting the heating zone is cooled by a cooling medium. the zone purification method; and (2) a heat-resistant housing whose interior is maintained in a vacuum or an inert gas atmosphere; a boat-shaped container for storing the object to be purified, which is connected to a traction device and placed in the housing; , and a zone purifier 1C equipped with a high-frequency induction heating coil surrounding the outside of the housing with a predetermined width:
Of the space area in the housing that is surrounded by the high-frequency induction heating coil and divided by a round band-shaped space as a boundary, on the side where the object to be purified leaves the band-shaped space and is pulled,
＠Cooling plate in contact with the boat-shaped container? It is characterized by having been established. @Ki zone'! F4 device.
を提供するものである。It provides:
この発明においては、精製工程中（二製品が汚染される
のな防ぐためＣ：５ Ｘ １０−６Ｔｏｒｒ ｐ下のよ
うな真空開を有する真空中まｔはアルゴンのような不活
性ガス中において遂行され、このような雰囲気を保つた
めには１例えば０石英管のような耐熱性のハウジングが
使用される。In this invention, during the purification process (to prevent contamination of the two products, the process is carried out in a vacuum such as under a vacuum of 5 x 10-6 Torr or in an inert gas such as argon). In order to maintain such an atmosphere, a heat-resistant housing such as a quartz tube is used.
被精製物は一般Ｃ：ボート状の容器に入れられるが、必
ずしも容器に入れることなく、別の手段で被精製物を保
持してもよい。The product to be purified is placed in a general C: boat-shaped container, but the product to be purified may be held by another means without necessarily being placed in a container.
ｗｔｆｆ特物収納用のボート状容器を使用する場合その
材料としては、映品を汚染するおそれがなくて耐熱性を
具えたもの、ＩＩＡえば黒鉛または石英が使用され、黒
鉛ボートの場合はそれ自体誘導加熱によって加熱できる
ので、その熱で被精特物？間接的に９口熱することもで
き、ボート状容器は１例えば、モータ及び減速機を介し
た牽引機構に牽引棒を組み込み、＠記ハウジングと牽引
棒とをＯリングシールしｔような牽引装置道によって牽
引される。When using a boat-shaped container for storing wtff special items, the material should be one that does not pose a risk of contaminating the film and is heat resistant, such as graphite or quartz. Since it can be heated by induction heating, the special object can be heated using that heat. It is also possible to heat the boat-shaped container indirectly.For example, a tow rod is incorporated into a tow mechanism via a motor and a speed reducer, and the housing and the tow rod are sealed with an O-ring. Towed by the road.
この発明のゾーン精喪装噴の運転条件は被精製物の種類
や寸法、あるいは除去すべき不純物の種類並びに目的と
する純Ｉ復等によって様々に変（ヒするので一層に言う
ことはできないが、前述の高純間アルミニウムからＵお
よびＴｈを除去する場合を例にとると、一般に１５〜２
５ＫＷの高周波出力においで１．５〜３．０ ｍ ／
ｍｉｎの移動迷電を使用して幅３０〜４０ｍの溶融帯を
形成し、その溶融帯をアルミニウム中に通常２〜３回繰
返して通過させる。The operating conditions of the zone seimiso jet of this invention vary depending on the type and size of the object to be purified, the type of impurities to be removed, the intended purity recovery, etc., so it is difficult to say more. , taking as an example the case of removing U and Th from the aforementioned high-purity aluminum, generally 15 to 2
1.5-3.0 m/at 5KW high frequency output
A moving stray current of min is used to form a 30-40 m wide molten zone, which is passed through the aluminum typically 2-3 times.
加熱帯域から出た被精製物を冷却媒体によって冷却する
Ｃ二は１例えば、前記ボート状容器の底と接する位置に
＠製冷却板を設けて、その中で冷却水を循環するのが好
都合である。For example, it is convenient to provide a cooling plate made of @ at a position in contact with the bottom of the boat-shaped container and circulate the cooling water within it. be.
ついで、半導体デバイス内の配線および成極材料として
使用される高純間アルミニウムからウランおよびトリウ
ムを除去する場合？例に挙げて。What about removing uranium and thorium from high-purity aluminum used as wiring and polarization material in semiconductor devices? Take an example.
この発明の実施例を説明する。Examples of this invention will be described.
実施例 １
第１図はこの発明（二よるゾーン精裂装ｑの一例をしめ
す縦断・側面図であって１図示のように、内部が真空排
気系に連絡して昼間のＸ空に保たれた外径８３鰭の石英
管１の中に、黒鉛ボート２が牽引棒３によって＠後へ移
動可能（＝ボート保持具４の上に装置されている。Embodiment 1 Figure 1 is a longitudinal cross-sectional view and a side view showing an example of this invention (two-way zone serif equipment q). In a quartz tube 1 with an outer diameter of 83 fins, a graphite boat 2 is mounted on a boat holder 4, which can be moved backwards by means of a tow rod 3.
石英管１のほぼ中央部には、それを囲む高周波誘導コイ
ル５が配置され、その誘導コイル５によって囲まれた帯
域、すなわち加熱帯域Ｈ中に、前記ボート２に納められ
たアルミニウム棒状体Ａを徐々に通過させると、その先
端から徐々に後方へ移動する溶融帯Ａ１が形成され、棒
状体Ａの天端には、この溶融帯Ａ１によって順次寄せ集
められた不純物が集積する最終凝固部Ａ２が形成される
。A high-frequency induction coil 5 surrounding the quartz tube 1 is placed approximately in the center of the quartz tube 1, and the aluminum rod-shaped body A housed in the boat 2 is placed in a zone surrounded by the induction coil 5, that is, a heating zone H. When the rod-shaped body A is gradually passed through, a molten zone A1 is formed that gradually moves backward from the tip, and at the top end of the rod-shaped body A, there is a final solidified zone A2 where impurities successively gathered by this molten zone A1 accumulate. It is formed.
１前記加熱帯域Ｈから出た棒状体Ａの精製部Ａ、側には
銅製の水冷板６が前記黒鉛ボート２の底と接する位置に
設けられ、その水冷板６の中には冷却水を循環する九め
の一組の導管７が挿入されている。1. A copper water-cooling plate 6 is provided on the side of the refining section A of the rod-shaped body A coming out of the heating zone H at a position in contact with the bottom of the graphite boat 2, and cooling water is circulated in the water-cooling plate 6. A ninth set of conduits 7 are inserted.
このようなゾーン精ａ装置により、３５１角で２Ｋｆの
大きさを耳し、かつ不純物としてＵｌｏｏｐｐｂ 、
Ｔｈ １４０ｐｐｂを含む線間ファイブナイン（９９，
９９９％）の電解アルミニウムを１発振周波数：２０（
’１ＫＨｚ、高周波出カニ２０ＫＷ、溶融帯の幅： ３
５ ｗｍ 、 ｍ融帯移動速ＩＩＩ’ ： １．５ ｗ
／ ｍ１ｒｌ ＊ Ｘ−？２藺： ３．５ Ｘ １０
−’Ｔｏｒｒおよびゾーン通過回数＝３の条件下で処理
した。得られた製品の不純物濃ｉＷはＵ ： ６ ｐｐ
ｂ以下、Ｔｈ：３ｐｐｂ以下で精製効率は８２％であっ
た。With such a zone precision a device, a magnitude of 2 Kf at 351 squares can be detected, and Ulooppb, Ulooppb, and other impurities can be detected.
Line-to-line five nines (99,
999%) electrolytic aluminum at 1 oscillation frequency: 20(
'1KHz, high frequency output 20KW, width of melting zone: 3
5 wm, m-fusion zone moving speed III': 1.5 w
/ m1rl *X-? 2: 3.5 x 10
-'Torr and the number of times of passing through the zone=3. The impurity concentration iW of the obtained product is U: 6 pp.
The purification efficiency was 82% with Th: 3 ppb or less.
ま九、比較のため、上記の水冷板が備えられていない点
だけが上記装置と異なる従来装置によって、上記と同じ
電解アルミニウムを発振周波数＝２００ＫＨｚ、高周波
出カニ７ＫＷ、溶融帯移動速＃ ： １．５ ｍ ／
ｍｉｎ ＋真空曜： ３．５ Ｘ １０−’Ｔｏｒｒ
。For comparison, the same electrolytic aluminum as above was oscillated at 200 KHz, high frequency output 7 KW, and molten zone moving speed #: 1 using a conventional device that differs from the above device only in that it does not include the water cooling plate. .5 m/
min + vacuum: 3.5 x 10-'Torr
.
ゾーン通過回数：３の条件下で処理し九ところ。Number of zone passes: 9 times processed under 3 conditions.
製品中の不純物製電はＵ ： ８ ｐｐｂ 、 Ｔｈニ
ア ｐｐｂで。The impurities in the product are U: 8 ppb, Th near ppb.
必要な線質（＝達せず、精製効率は６５％であった。The required radiation quality (= not achieved, purification efficiency was 65%).
実施例 ２
実施例１で述べたのと同じ本発明装置および従来装置を
使用し、絹製速邸（溶融帯移動速１）？０．４１−とじ
九以外は実施例１と同じ操作条件下で上記と同じ電解ア
ルミニウムを処理したところ。Example 2 Using the same apparatus of the present invention and the conventional apparatus as described in Example 1, silk production was carried out (melting zone movement speed 1). 0.41 - The same electrolytic aluminum as above was treated under the same operating conditions as in Example 1, except for the number of steps.
本発明装置および従来装置（二よって得られた製品の不
純物製電は、とも＋：Ｕ ： ６ ｐｐｂ以下、Ｔｈ：
３ｐｐｂ Ｉｄ下となって、いずれも必要な線間を得る
ことができたけれども、上記の原料（被Ｍ製物）となっ
たば解アルミニウムの全長１０００ｍに対する精製効率
は、従来装置によると６７％であう念のに対し１本発明
装置では８４％に達した。The impurity content of the products obtained by the device of the present invention and the conventional device (2) is +: U: 6 ppb or less, Th:
Although we were able to obtain the necessary line spacing under 3 ppb Id, the refining efficiency for the total length of 1000 m of precipitated aluminum, which was the raw material (product to be manufactured), was 67% using the conventional equipment. In contrast, the device of the present invention achieved a rate of 84%.
実ｉ例 ３
この発明のように高周波誘導加熱を利用するゾーン精製
方法および装置において上記のような冷却板を使用する
場合には、同−電源（−よって運転される各ゾーン精製
装置を並列に配置し、その各ゾーン精製装置にそれぞれ
冷却板を配して溶融帯の幅および温叶が均一になるよう
に調節することができるから、簡単な操作によって生Ｎ
量を増やすことができる。ここでは実権例１で述べた本
発明ｆ２置５基を並列に並べ、これら装置の丁べてに共
通する同一の加熱［源を使用して、各装置ごとに冷却板
を働らかせた本発明方法と、？＠却板を全く働らかせな
かった比軸方法（−よって、上記と同じ電解アルミニウ
ムを発振高周波：２００ＫＨｚ、扁周波出カニ１００Ｋ
Ｗ、ｆ５融帯移動速＃：１．５ｍ／醜、真空Ｉｖ： ３
．５ Ｘ １ （’）−’Ｔｏｒｒ 、ゾーン通過回数
：３の条件下で精映し友。 その結果得られた。Practical Example 3 When using a cooling plate as described above in a zone purification method and apparatus using high-frequency induction heating as in the present invention, each zone purification apparatus operated by the same power source (-) may be connected in parallel. It is possible to adjust the width and temperature of the melting zone to be uniform by placing a cooling plate in each zone of the purification device.
You can increase the amount. Here, five units of the present invention f2 described in Practical Example 1 are arranged in parallel, and the same heating source common to all of these units is used, and a cooling plate is operated for each unit. The invention method and? @ Ratio method in which the cooling plate does not work at all (- Therefore, the same electrolytic aluminum as above is oscillated at high frequency: 200 KHz, flat frequency output crab is 100 K)
W, f5 fusion zone movement speed #: 1.5m/ugly, vacuum Iv: 3
．． 5 X 1 (')-'Torr, number of zone passages: 3. The result was obtained.
各′ｎｎ張装置との製品の下純物濃明とＭ特効率を第１
表に示し九。The lower purity concentration and M characteristic efficiency of the product with each 'nn stretching device are determined first.
9 shown in the table.
実権例１の結果から１本発明は従来技術と比べて、ｎ製
速ぜを増大できることがわかり、また実施例２の結果か
ら１本発明は従来技術よりも精製効率に丁ぐれ、ま九実
施例３の結果から、本発明は多数の装置を平行（二並べ
て同時ｆ：操作しても。From the results of Practical Example 1, it was found that the present invention can increase the production speed compared to the conventional technology, and from the results of Example 2, it can be seen that the present invention has better purification efficiency than the conventional technology, From the results of Example 3, it can be seen that the present invention allows multiple devices to be operated in parallel (even if two devices are operated simultaneously).
すぐれた精璧速嘲と精仰効率を達成できることがわかる
。It can be seen that excellent speed and efficiency can be achieved.
以上述べた説明から明らかなように、この発明によると
、精仰効率が向上するとともに、ｒＩ製速Ｖも増大し、
しかも多数のゾーン積装装置を平行させて同時に操作で
きるので、線間のすぐれた整品を高い生産速度で製造す
ることができ、さらに冷却媒体による急冷によって、被
精特物において溶入効果を得ることもできる。As is clear from the above explanation, according to the present invention, not only the precision efficiency is improved, but also the rI manufacturing speed V is increased.
Moreover, since multiple zone loading devices can be operated in parallel and at the same time, products with excellent line spacing can be manufactured at a high production rate.Furthermore, rapid cooling with a cooling medium can improve the welding effect in the special material. You can also get it.
第１図は、この発明の装置の一例を概略的に示す縦断側
面図でるる。 図面において。
１・・・石英管、 ２・・・黒鉛ボート。
３・・・牽引棒、 ４・・・黒鉛ボート支持具。
５・・・訪辱コイル、 ６・・・水冷板、 ７・・・導
管。
Ａ・・・アルミニウム棒状体、 Ｈ・・・加熱帯域。FIG. 1 is a longitudinal side view schematically showing an example of the apparatus of the present invention. In the drawing. 1...Quartz tube, 2...Graphite boat. 3... Towing rod, 4... Graphite boat support. 5... Visiting coil, 6... Water cooling plate, 7... Conduit. A... Aluminum rod, H... Heating zone.
Claims (2)
方向に沿つて移動する棒状の被精製物を、高周波誘導加
熱によつて帯状の局部的な加熱が引起される加熱帯域に
通過させて、その被精製物において先端から末端へ次第
に移動する溶融帯を形成させ、それによつて、前記被精
製物中に含まれる不純物を順次溶融帯の中へ寄せ集めて
、前記被精製物において、その不純物が集積された最終
凝固部を前記被精製物の末端部分に形成させるとともに
、前記不純物が除かれた精製部をその末端部分以外の部
分に形成させ、ついで、不純物が集積した前記末端部分
を取除くことによつて前記被精製物を精製するゾーン精
製方法において、前記加熱帯域から出た被精製物を冷却
媒体によつて冷却することを特徴とする、前記ゾーン精
製方法。(1) In a vacuum or in an inert gas atmosphere, a rod-shaped object to be purified that moves along the longitudinal direction is passed through a heating zone where local heating in a band-like manner is caused by high-frequency induction heating, A molten zone is formed in the object to be purified that gradually moves from the tip to the end, and thereby impurities contained in the object to be purified are successively gathered into the molten zone, and the impurities are removed from the object in the object to be purified. A final solidified part in which impurities are accumulated is formed at the end of the object to be purified, a purified part from which the impurities are removed is formed in a part other than the end, and then the end part in which impurities are accumulated is removed. The zone refining method for refining the object to be purified by removing the object, characterized in that the object to be purified exiting the heating zone is cooled by a cooling medium.
耐熱性ハウジング、牽引装置と連結してそのハウジング
内に入れられた被精製物収納用のボート状容器、および
前記ハウジングの外側を所定の幅で囲む高周波誘導加熱
コイルが備えられたゾーン精製装置において、前記高周
波誘導加熱コイルで囲まれた帯状の空間を境として二分
される前記ハウジング中の空間領域のうち、前記被精製
物が前記帯状空間を出て牽引されていく側に、前記ボー
ト状容器と接触する冷却板を設けたことを特徴とする、
前記ゾーン精製装置。(2) A heat-resistant housing whose inside is maintained in a vacuum or an inert gas atmosphere, a boat-shaped container for storing the purified product that is connected to a traction device and placed inside the housing, and the outside of the housing is arranged in a predetermined manner. In a zone refining device equipped with a high-frequency induction heating coil surrounded by a width, the object to be purified is divided into two by a band-shaped space surrounded by the high-frequency induction heating coil. A cooling plate that comes into contact with the boat-shaped container is provided on the side where the container is being towed after exiting the space.
The zone purifier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61042993A JPS62202033A (en) | 1986-02-28 | 1986-02-28 | Method and apparatus for zone refining |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61042993A JPS62202033A (en) | 1986-02-28 | 1986-02-28 | Method and apparatus for zone refining |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62202033A true JPS62202033A (en) | 1987-09-05 |
Family
ID=12651549
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61042993A Pending JPS62202033A (en) | 1986-02-28 | 1986-02-28 | Method and apparatus for zone refining |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62202033A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100326591B1 (en) * | 1999-12-02 | 2002-03-12 | 김현진 | A contact bar for refining metal and method for preparation thereof |
| CN102002606A (en) * | 2010-12-14 | 2011-04-06 | 株洲钻石切削刀具股份有限公司 | Graphite boat and graphite boat group for hard alloy sintering technology |
| KR20170022306A (en) * | 2015-08-20 | 2017-03-02 | 한국기초과학지원연구원 | Apparatus for increasing the purity of the low melting metal |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS564515A (en) * | 1979-06-15 | 1981-01-17 | Nippon Electric Co | Automatic sorting*packing apparatus for paper leaf |
-
1986
- 1986-02-28 JP JP61042993A patent/JPS62202033A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS564515A (en) * | 1979-06-15 | 1981-01-17 | Nippon Electric Co | Automatic sorting*packing apparatus for paper leaf |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100326591B1 (en) * | 1999-12-02 | 2002-03-12 | 김현진 | A contact bar for refining metal and method for preparation thereof |
| CN102002606A (en) * | 2010-12-14 | 2011-04-06 | 株洲钻石切削刀具股份有限公司 | Graphite boat and graphite boat group for hard alloy sintering technology |
| KR20170022306A (en) * | 2015-08-20 | 2017-03-02 | 한국기초과학지원연구원 | Apparatus for increasing the purity of the low melting metal |
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