JPH0625855A - Crucible and its production - Google Patents
Crucible and its productionInfo
- Publication number
- JPH0625855A JPH0625855A JP18514292A JP18514292A JPH0625855A JP H0625855 A JPH0625855 A JP H0625855A JP 18514292 A JP18514292 A JP 18514292A JP 18514292 A JP18514292 A JP 18514292A JP H0625855 A JPH0625855 A JP H0625855A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- molybdenum
- peripheral surface
- tungsten
- tungsten film
- 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.)
- Granted
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は，金属モリブデンを含む
金属材料から形成されたルツボ（以下，モリブデンルツ
ボと呼ぶ）とその製造方法に関し，詳しくは，１８００
℃以上の超高温での使用に適した高温強度の優れたモリ
ブデンルツボとその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a crucible made of a metallic material containing metallic molybdenum (hereinafter referred to as molybdenum crucible) and a manufacturing method thereof.
TECHNICAL FIELD The present invention relates to a molybdenum crucible having excellent high-temperature strength suitable for use at an ultrahigh temperature of ℃ or more and a method for producing the same.
【０００２】[0002]
【従来の技術】一般に金属又は金属酸化物等の高融点材
料は，ルツボ中で，不活性ガス或いは真空の雰囲気中で
溶解される。高融点金属溶解用のルツボとしては，金属
モリブデン又はモリブデン合金のように，金属モリブデ
ンを含むルツボ（以下，全てこの種のルツボをモリブデ
ンルツボと呼ぶ）が使用されている。2. Description of the Related Art Generally, a high melting point material such as a metal or a metal oxide is melted in a crucible, an inert gas atmosphere or a vacuum atmosphere. As a crucible for melting a high melting point metal, a crucible containing molybdenum metal such as molybdenum metal or molybdenum alloy (hereinafter, this type of crucible is referred to as a molybdenum crucible) is used.
【０００３】しかし，モリブデンルツボとして，純モリ
ブデン製のルツボを使用した場合，モリブデンの再結晶
温度が約１０００℃であるため，使用温度が高くなるほ
ど，また，高温での使用時間が長くなるほど，ルツボを
構成するモリブデン結晶粒の粗大化が起こる。そのた
め，純モリブデン製のルツボは，結晶粒界の脆弱化によ
る粒界に割れ，又はひびが生じ，この部分からルツボ中
の被溶解物が漏れ出して使用不能となるという欠点を有
している。この欠点を解消するために，例えば，特願昭
６２−１５４２号（以下，参考文献１と呼ぶ）に示され
た改良されたルツボが提案されている。この改良された
ルツボは，モリブデンにランタン又はランタン酸化物を
０．０１〜１ｗｔ％を含有させた材料によって形成され
ており，鍛造における加工率を余り高くしないで加工す
ることで，加工が容易で，強度が高く優れているという
利点を有する。However, when a molybdenum crucible made of pure molybdenum is used as the molybdenum crucible, the recrystallization temperature of molybdenum is about 1000 ° C. Therefore, the higher the operating temperature and the longer the operating time at a high temperature, the crucible. The coarsening of the molybdenum crystal grains that constitute Therefore, the crucible made of pure molybdenum has a drawback that the grain boundary is cracked or cracked due to the weakening of the crystal grain boundary, and the melted substance in the crucible leaks out from this portion to make it unusable. . In order to solve this drawback, for example, an improved crucible disclosed in Japanese Patent Application No. 62-1542 (hereinafter referred to as Reference Document 1) has been proposed. This improved crucible is made of molybdenum containing 0.01 to 1 wt% of lanthanum or lanthanum oxide, and can be easily processed by processing without increasing the processing rate in forging. ， It has the advantage of high strength and excellent.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら，このモ
リブデンルツボは，外部から加熱するように使用される
ので，ルツボ外壁の熱による亀裂等の損傷に対しては十
分とはいえなかった。このため，被溶解物の粒界への溶
入を避けることができなかった。そこで，モリブデンル
ツボに代えて更に高温強度の優れたルツボ材料として，
注目されるのが，純金属タングステン又はタングステン
合金等の金属タングステンを含む材料（以下，単にタン
グステンと呼ぶ）である。However, since this molybdenum crucible is used so as to be heated from the outside, it cannot be said that the molybdenum crucible is sufficiently protected against damage such as cracks due to heat on the outer wall of the crucible. For this reason, it was impossible to avoid infiltration of the material to be melted into the grain boundaries. Therefore, instead of the molybdenum crucible, as a crucible material with superior high temperature strength,
Attention is focused on a material containing metallic tungsten such as pure metallic tungsten or a tungsten alloy (hereinafter, simply referred to as tungsten).
【０００５】しかし，現実に必要とされるルツボは，直
径で６０〜２２０ｍｍ程度，高さが３０〜１００ｍｍ程
度とかなり大型のものであり，現在のタングステン加工
技術では，このような大型のタングステンルツボを加工
することは実際上困難である。However, the crucible actually required is quite large with a diameter of about 60 to 220 mm and a height of about 30 to 100 mm, and in the present tungsten processing technology, such a large size crucible is used. Is difficult to process in practice.
【０００６】そこで，本発明の技術的課題は，タングス
テンの高温強度を備えたモリブデンルツボとその製造方
法を提供することにある。Therefore, a technical object of the present invention is to provide a molybdenum crucible having high-temperature strength of tungsten and a method for manufacturing the same.
【０００７】[0007]
【課題を解決するための手段】本発明では，ＣＶＤ法又
は溶射法によって，微細で且つ緻密なタングステン材料
からなる膜を作製することによって，上記課題を解決し
たものである。The present invention has solved the above-mentioned problems by forming a film made of a fine and dense tungsten material by a CVD method or a thermal spraying method.
【０００８】本発明によれば，高融点金属又は高融点金
属酸化物の溶解に用いるモリブデンからなるルツボであ
って，少なくとも外周面にタングステン膜を有すること
を特徴とするモリブデンルツボが得られる。According to the present invention, there is provided a molybdenum crucible which is used for melting a refractory metal or a refractory metal oxide and has a tungsten film on at least the outer peripheral surface.
【０００９】ここで，本発明において，タングステンと
は，少なくとも金属タングステンを含む金属材料を呼
び，純金属タングステン，タングステン合金等を含む。Here, in the present invention, the term "tungsten" refers to a metallic material containing at least metallic tungsten, and includes pure metallic tungsten, a tungsten alloy and the like.
【００１０】本発明者の実験によれば，タングステン膜
でモリブデンルツボを被覆することによって，実質的に
タングステンの特性を具備したルツボが得られることが
判明した。According to the experiments conducted by the present inventor, it was found that by coating a molybdenum crucible with a tungsten film, a crucible having substantially the characteristics of tungsten can be obtained.
【００１１】ここで，本発明において，タングステン膜
は，熱又は機械的衝撃に対する剥離強度を考慮して，５
０〜１００μｍより大とすることが好ましい。また，前
記ＣＶＤ法の代わりに，低廉で，使用温度の著しく高く
ないものは，溶射法によって被覆しても，ＣＶＤ法によ
るタングステン膜と同等の特性が得られることがわかっ
た。In the present invention, the tungsten film has a peel strength of 5 in consideration of the peel strength against heat or mechanical impact.
It is preferable that it is larger than 0 to 100 μm. Further, it has been found that, instead of the CVD method, a material which is inexpensive and whose usage temperature is not extremely high can obtain the same characteristics as the tungsten film formed by the CVD method, even if the coating is performed by the thermal spraying method.
【００１２】[0012]
【作用】本発明においては，モリブデンルツボ本体の少
なくとも外周面に，タングステン膜を設けることで，タ
ングステンの高温強度を備えたルツボが得られる。In the present invention, by providing the tungsten film on at least the outer peripheral surface of the molybdenum crucible body, the crucible having the high temperature strength of tungsten can be obtained.
【００１３】[0013]
【実施例】以下に，本発明の実施例について，図面を参
照して説明する。Embodiments of the present invention will be described below with reference to the drawings.
【００１４】図１は，本発明のルツボの一例を示す図で
ある。図１において，ルツボ１０は，モリブデンルツボ
本体１と，タングステン膜を備えている。FIG. 1 is a diagram showing an example of the crucible of the present invention. In FIG. 1, a crucible 10 includes a molybdenum crucible body 1 and a tungsten film.
【００１５】モリブデンルツボ本体１は，モリブデン材
料から切削加工されており，内周面１２，外周面１４，
縁面１６，内底面１７及び外底面１８とによって，構成
されている。The molybdenum crucible body 1 is machined from a molybdenum material, and has an inner peripheral surface 12, an outer peripheral surface 14,
It is constituted by the edge surface 16, the inner bottom surface 17 and the outer bottom surface 18.
【００１６】内周面１２と内底面１７及び外周面１４と
外底面１８との境界部は，曲率を持つように形成されて
いる。タングステン膜２は，縁面１６の略中央部から外
周面１４及び凹部に渡って施されている。The boundary between the inner peripheral surface 12 and the inner bottom surface 17 and the outer peripheral surface 14 and the outer bottom surface 18 is formed to have a curvature. The tungsten film 2 is applied from the substantially central portion of the edge surface 16 to the outer peripheral surface 14 and the recess.
【００１７】図２は，本発明のルツボの他の例を示す図
である。図１のルツボ１０との相違点は，図２で示すル
ツボ２０は，タングステン膜２´が，モリブデンルツボ
本体１の縁面１６全体を覆い，更に内底面１７及び内周
面１２にも施されている点である。このように外周面１
４だけでなく，内底面１７及び内周面１２をもタングス
テン膜２´によって，覆うことによって，溶解した液に
よる粒界への侵入を防止するに適し，図１のルツボ１０
よりも高温強度が高いルツボを得ることができる。FIG. 2 is a diagram showing another example of the crucible of the present invention. The difference from the crucible 10 in FIG. 1 is that the crucible 20 shown in FIG. That is the point. Thus, the outer peripheral surface 1
4, not only the inner bottom surface 17 and the inner peripheral surface 12 are covered with the tungsten film 2 ′, which is suitable for preventing the melted liquid from entering the grain boundaries.
It is possible to obtain a crucible having a higher high temperature strength than that.
【００１８】図３は，本発明のルツボの更に他の例を示
す図である。図２のルツボ２０との相違点は，図３のル
ツボ３０は，タングステン膜２''が外底面１８にも施さ
れている点である。このルツボ３０は，２３００〜２４
００℃の超高温で使用した場合においても，モリブデン
ルツボ粒界に発生する外壁の亀裂は見られなかった。FIG. 3 is a diagram showing still another example of the crucible of the present invention. The difference from the crucible 20 of FIG. 2 is that the crucible 30 of FIG. 3 has the tungsten film 2 ″ also applied to the outer bottom surface 18. This crucible 30 is 2300-24
Even when used at an ultrahigh temperature of 00 ° C., no cracks on the outer wall occurred at the molybdenum crucible grain boundaries.
【００１９】また，外底面１８に施すことで，更に高温
強度を高め，寿命を長くすることができる。Further, by applying to the outer bottom surface 18, the high temperature strength can be further enhanced and the life can be extended.
【００２０】以下，上記したルツボの具体的方法を実施
例として説明する。A specific method of the above crucible will be described below as an embodiment.
【００２１】（実施例１）純モリブデン材と，この純モ
リブデン材に結晶粒界の脆弱防止に添加されたランタン
を含む化合物とを含むモリブデン材を最終的に切削加工
することによって，ルツボ形状に加工し，モリブデンル
ツボ本体１を得た。充分にＡｒ置換して，その後，減圧
された反応槽に，Ｈ2 を５００ｃｃ／ｍｉｎ，ＷＦ6 を
５０ｃｃ／ｍｉｎを夫々導入した。モリブデンルツボ本
体１を高周波電源等によって，４００℃に加熱し，水素
還元ＣＶＤ法によって，このモリブデンルツボ本体１表
面に，純タングステン膜２を被覆した。被覆後，約４０
分経過後，ルツボを取り出したところ，図１で示すよう
に外周面に８５μｍの厚さのタングステン膜２を有する
ルツボ１０が得られた。Example 1 A molybdenum material containing a pure molybdenum material and a compound containing lanthanum added to the pure molybdenum material to prevent brittleness of grain boundaries is finally cut into a crucible shape. By processing, a molybdenum crucible body 1 was obtained. After sufficiently replacing with Ar, 500 cc / min of H 2 and 50 cc / min of WF 6 were introduced into the depressurized reaction tank. The molybdenum crucible body 1 was heated to 400 ° C. by a high frequency power source or the like, and the surface of the molybdenum crucible body 1 was coated with a pure tungsten film 2 by a hydrogen reduction CVD method. About 40 after coating
After a lapse of minutes, the crucible was taken out to obtain a crucible 10 having a tungsten film 2 having a thickness of 85 μm on the outer peripheral surface as shown in FIG.
【００２２】（実施例２）実施例１と同様に切削加工を
施したモリブデンルツボ本体１を，アルミナ粒にてブラ
スト処理した。市販の溶射用造粒Ｗ粉（メテコ社製，N
o.61 ）を６５Ｖ，５００Ａのパワー，Ａｒ流速７ｋｇ
／ｃｍ2 ，Ｈ2 流速３．５ｋｇ／ｃｍ2 で噴霧速度１２
７ｂｓ／Ｈ（ポンド／時間）で，溶射を行った。この溶
射に用いたガンは，４０ｍ／ｍｉｎ送りで，加工物であ
るモリブデンルツボ本体１との距離を１００ｍｍとして
溶射を行った。数回溶射し，約３００μｍの純タングス
テン層を形成し，図１で示すようなルツボ１０が得られ
た。(Example 2) The molybdenum crucible body 1 that was cut in the same manner as in Example 1 was blasted with alumina grains. Commercially available thermal spray granulation W powder (Metco, N
o.61) 65V, 500A power, Ar flow rate 7kg
/ Cm 2 , H 2 flow rate 3.5 kg / cm 2 and spray rate 12
Thermal spraying was performed at 7 bs / H (pounds / hour). The gun used for this thermal spraying was carried out at a feed rate of 40 m / min, with the distance from the molybdenum crucible body 1 being the workpiece being 100 mm. Thermal spraying was performed several times to form a pure tungsten layer of about 300 μm, and the crucible 10 as shown in FIG. 1 was obtained.
【００２３】実施例２に係るＷ粉の溶射による被覆方法
は，使用状態において過酷さを求められないルツボに
は，適用することができる。この方法は，実施例１で示
したＣＶＤ法よりも操作，取扱いが容易であるととも
に，上記実施例１で示したようなＷＦ6 等の有害ガスを
使用しないで済むという利点も兼ね備えている。The coating method by thermal spraying of W powder according to the second embodiment can be applied to a crucible which is not required to be harsh in use. This method is easier to operate and handle than the CVD method shown in the first embodiment, and also has the advantage that no harmful gas such as WF 6 is used as shown in the first embodiment.
【００２４】しかし，実施例２で説明した溶射法では，
何回か繰り返し溶射しないと，１回当り２〜３％の空孔
が残るので，この空孔を塞ぐには，減圧溶射を繰り返す
ことが好ましい。However, in the thermal spraying method described in the second embodiment,
If the thermal spraying is not repeated several times, 2-3% of the pores remain, so it is preferable to repeat the reduced pressure spraying to close the pores.
【００２５】以上の実施例１，２においては，図１で示
すように，外周面のみにタングステン膜２を施したが，
施行する配置を考えると，図２で示すようなルツボ２０
も形成することができる。また，実施例１及び２で述べ
た方法を，複数回行うと，図３で示すルツボ３０を得る
ことができる。図２又は図３で示すルツボ２０，３０
は，ルツボ本体１の内壁部１２に至るタングステン膜２
´，２''を施すと，中味の溶融物のモリブデンルツボの
粒界への侵入も抑制できる。In Examples 1 and 2 described above, the tungsten film 2 was applied only to the outer peripheral surface as shown in FIG.
Considering the arrangement to be applied, the crucible 20 as shown in FIG.
Can also be formed. Further, the crucible 30 shown in FIG. 3 can be obtained by performing the method described in the first and second embodiments a plurality of times. Crucible 20, 30 shown in FIG. 2 or FIG.
Is the tungsten film 2 reaching the inner wall 12 of the crucible body 1.
By applying ′, 2 ″, it is also possible to suppress the intrusion of the molten material into the grain boundary of the molybdenum crucible.
【００２６】ただし，ルツボ３０の場合，実施例２で示
すノズルの施工においては２度に分けて行う必要があ
り，１８００℃以上の高温とはいえ，寿命と経費とのバ
ランスを考慮しながら適用することが必要とされる。However, in the case of the crucible 30, it is necessary to perform the nozzle construction shown in Example 2 in two steps. Even though the temperature is higher than 1800 ° C., the crucible 30 is applied while considering the balance between life and cost. Required to do.
【００２７】[0027]
【発明の効果】以上，説明したように，本発明によれ
ば，タングステンの高温強度を備えたモリブデンルツボ
とその製造方法を提供することができる。As described above, according to the present invention, it is possible to provide a molybdenum crucible having high-temperature strength of tungsten and a method for manufacturing the same.
【図１】本発明のルツボの一例を示す図である。FIG. 1 is a diagram showing an example of a crucible of the present invention.
【図２】本発明のルツボの他の例を示す図である。FIG. 2 is a diagram showing another example of the crucible of the present invention.
【図３】本発明のルツボの更に他の例を示す図である。FIG. 3 is a view showing still another example of the crucible of the present invention.
１ モリブデンルツボ本体 ２，２´，２''タングステン膜 １０ モリブデンルツボ １１ 内周面 １４ 外周面 １６ 縁面 １７ 内底面 １８ 外底面 1 molybdenum crucible main body 2, 2 ', 2' 'tungsten film 10 molybdenum crucible 11 inner peripheral surface 14 outer peripheral surface 16 edge surface 17 inner bottom surface 18 outer bottom surface
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【手続補正書】[Procedure amendment]
【提出日】平成４年７月２７日[Submission date] July 27, 1992
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００２２[Name of item to be corrected] 0022
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００２２】（実施例２）実施例１と同様に切削加工を
施したモリブデンルツボ本体１を，アルミナ粒にてブラ
スト処理した。市販の溶射用造粒Ｗ粉（メテコ社製，Ｎ
ｏ．６１）を６５Ｖ，５００Ａのパワー，Ａｒ流速７ｋ
ｇ／ｃｍ２，Ｈ２流速３．５ｋｇ／ｃｍ２で噴霧速度１
２ｌ（エル）ｂｓ／Ｈ（ポンド／時間）で，溶射を行っ
た。この溶射に用いたガンは，４０ｍ／ｍｉｎ送りで，
加工物であるモリブデンルツボ本体１との距離を１００
ｍｍとして溶射を行った。数回溶射し，約３００μｍの
純タングステン層を形成し，図１で示すようなルツボ１
０が得られた。(Example 2) The molybdenum crucible body 1 that was cut in the same manner as in Example 1 was blasted with alumina grains. Commercially available granulation W powder for thermal spray (Metco, N
o. 61) 65V, 500A power, Ar flow rate 7k
g / cm 2 , H 2 flow rate 3.5 kg / cm 2 , spray rate 1
In 2 l (el) bs / H (lbs / hr), was sprayed. The gun used for this spraying is 40 m / min feed,
The distance from the molybdenum crucible body 1, which is a workpiece, is 100
Thermal spraying was performed in mm. It is sprayed several times to form a pure tungsten layer of about 300 μm, and the crucible 1 as shown in FIG.
0 was obtained.
【手続補正２】[Procedure Amendment 2]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】図面の簡単な説明[Name of item to be corrected] Brief description of the drawing
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【図面の簡単な説明】[Brief description of drawings]
【図１】本発明のルツボの一例を示す図である。FIG. 1 is a diagram showing an example of a crucible of the present invention.
【図２】本発明のルツボの他の例を示す図である。FIG. 2 is a diagram showing another example of the crucible of the present invention.
【図３】本発明のルツボの更に他の例を示す図である。FIG. 3 is a view showing still another example of the crucible of the present invention.
【符号の説明】 １ モリブデンルツボ本体 ２，２′，２’’タングステン膜 １０ モリブデンルツボ １２ 内周面 １４ 外周面 １６ 縁面 １７ 内底面 １８ 外底面 ─────────────────────────────────────────────────────
[Explanation of reference symbols] 1 molybdenum crucible body 2, 2 ', 2''tungsten film 10 molybdenum crucible 1 2 inner peripheral surface 14 outer peripheral surface 16 edge surface 17 inner bottom surface 18 outer bottom surface ─────────── ───────────────────────────────────────────
【手続補正書】[Procedure amendment]
【提出日】平成４年７月３１日[Submission date] July 31, 1992
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】特許請求の範囲[Name of item to be amended] Claims
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【特許請求の範囲】[Claims]
【手続補正２】[Procedure Amendment 2]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１１[Correction target item name] 0011
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００１１】ここで，本発明において，タングステン膜
は，熱又は機械的衝撃に対する剥離強度を考慮して，５
０〜１００μｍより大とすることが好ましい。また，タ
ングステン膜を形成する方法としては，ＣＶＤ法及び溶
射法のいずれかまたは両方を併用してもよいが，低廉で
使用温度の著しく高くないものについては，溶射法のみ
によって被覆しても，ＣＶＤ法によるタングステン膜と
同等の特性が得られる。 In the present invention, the tungsten film has a peel strength of 5 in consideration of the peel strength against heat or mechanical impact.
It is preferable that it is larger than 0 to 100 μm. In addition, data
As a method for forming a tungsten film, a CVD method and a melting method are used.
Either or both of archery may be used together, but for those not significantly higher use temperatures inexpensive, be coated only by the spraying method, Ru obtained tungsten film characteristics equivalent by CVD.
Claims (3)
体と，少なくとも外周面に形成されたタングステン膜と
を有することを特徴とするルツボ。1. A crucible having a molybdenum body having an inner peripheral surface and an outer peripheral surface, and a tungsten film formed on at least the outer peripheral surface.
ツボ本体を製作した後，前記モリブデンルツボ本体の少
なくとも外周面に，ＣＶＤ法によって，タングステン膜
を形成することを特徴とするルツボの製造方法。2. A method of manufacturing a crucible, which comprises forming a molybdenum crucible body having an inner peripheral surface and an outer peripheral surface, and then forming a tungsten film on at least the outer peripheral surface of the molybdenum crucible main body by a CVD method.
ツボ本体を製作した後，前記モリブデンルツボ本体の少
なくとも外周面に，ＣＶＤ法によって，タングステン膜
を形成することを特徴とするモリブデンルツボの製造方
法。3. A method for manufacturing a molybdenum crucible, which comprises forming a molybdenum crucible body having an inner peripheral surface and an outer peripheral surface, and then forming a tungsten film on at least the outer peripheral surface of the molybdenum crucible main body by a CVD method. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18514292A JPH0811824B2 (en) | 1992-07-13 | 1992-07-13 | Crucible and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18514292A JPH0811824B2 (en) | 1992-07-13 | 1992-07-13 | Crucible and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0625855A true JPH0625855A (en) | 1994-02-01 |
| JPH0811824B2 JPH0811824B2 (en) | 1996-02-07 |
Family
ID=16165613
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18514292A Expired - Lifetime JPH0811824B2 (en) | 1992-07-13 | 1992-07-13 | Crucible and manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0811824B2 (en) |
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|---|---|
| JPH0811824B2 (en) | 1996-02-07 |
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