JP3198281B2 - Coating material for cold crucible furnace and method for producing the same - Google Patents
Coating material for cold crucible furnace and method for producing the sameInfo
- Publication number
- JP3198281B2 JP3198281B2 JP16200692A JP16200692A JP3198281B2 JP 3198281 B2 JP3198281 B2 JP 3198281B2 JP 16200692 A JP16200692 A JP 16200692A JP 16200692 A JP16200692 A JP 16200692A JP 3198281 B2 JP3198281 B2 JP 3198281B2
- Authority
- JP
- Japan
- Prior art keywords
- zirconia
- cold crucible
- crucible furnace
- coating material
- yttria
- 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
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- Inorganic Compounds Of Heavy Metals (AREA)
- Crucibles And Fluidized-Bed Furnaces (AREA)
- Furnace Housings, Linings, Walls, And Ceilings (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、高融点材料を溶解する
際に、コールドクルーシブル（水冷銅るつぼ）炉を使用
する際の炉内壁に塗る塗型材及び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 coating material applied to an inner wall of a cold crucible (water-cooled copper crucible) furnace when a high melting point material is melted, and a method for producing the same.
【０００２】[0002]
【従来の技術】従来、チタン合金、ジルコニウム合金、
モリブデン合金等の高融点材料を溶解する際にるつぼと
してコールドクルーシブル炉を用い、高エネルギー熱源
を利用し、メルテイングストックを得ている。しかし、
この方法では、るつぼが水冷されているため、るつぼ壁
面での溶解ができないため、メルテイングストックが少
なくなるという問題が生じる。2. Description of the Related Art Conventionally, titanium alloys, zirconium alloys,
When melting a high melting point material such as a molybdenum alloy, a cold crucible furnace is used as a crucible, and a high energy heat source is used to obtain a melting stock. But,
In this method, since the crucible is water-cooled, it cannot be melted on the crucible wall surface, so that there is a problem that the melting stock is reduced.
【０００３】[0003]
【発明が解決しようとする課題】本発明は、前記したメ
ルテイングストックの減少を抑えるため、鋭意研究した
結果、コールドクルーシブル炉の壁面に塗布可能で、高
融点材料に対して化学的、熱的に安定な耐火材料となる
コールドクルーシブル炉用塗型材を見出した。即ち、本
発明は、コールドクルーシブル炉で高融点材料を溶解す
る際に、メルテイングストックを多くするコールドクル
ーシブル炉の壁面に塗布可能な塗型材の提供にある。SUMMARY OF THE INVENTION The present invention has been intensively studied in order to suppress the decrease in the melting stock described above. As a result, the present invention can be applied to the wall of a cold crucible furnace and is chemically and thermally applied to a high melting point material. We found a coating material for cold crucible furnaces which became a stable refractory material. That is, the present invention is to provide a coating material that can be applied to the wall of a cold crucible furnace that increases the melting stock when melting a high melting point material in the cold crucible furnace.
【０００４】[0004]
【課題を解決するための手段】即ち、本発明は、イット
リアとジルコニアを含み、イットリアとジルコニアの合
計量が３０〜９５重量％で、且つＹ2 Ｏ3 ／ＺｒＯ2 の
重量比が０．５〜４０であるｐＨ４〜１３のスラリーか
ら成ることを特徴とするコールドクルーシブル炉用塗型
材に関する。That SUMMARY OF THE INVENTION The present invention comprises a yttria and zirconia, the total amount of yttria and zirconia with 30 to 95 wt%, and Y 2 O 3 / ZrO 2 weight ratio of 0.5 The present invention relates to a coating material for a cold crucible furnace, which comprises a slurry having a pH of 4 to 13, which is 40.
【０００５】以下、本発明を更に詳細に説明する。本発
明のコールドクルーシブル炉用塗型材の製造方法は、ジ
ルコニアゾルにイットリア粉末、ジルコニア粉末を加
え、ｐＨ４〜１３のスラリーを得ることにより得られ
る。ジルコニアゾルへのイットリア粉末とジルコニア粉
末の添加量は、イットリアとジルコニアの合計量がスラ
リー中３０〜９５重量％で、且つＹ2 Ｏ3 ／ＺｒＯ2 の
重量比が０．５〜４０、好ましくは２０〜４０になるよ
うに加える。Hereinafter, the present invention will be described in more detail. The method for producing a coating material for a cold crucible furnace of the present invention is obtained by adding a yttria powder and a zirconia powder to a zirconia sol to obtain a slurry having a pH of 4 to 13. The addition amount of the yttria powder and the zirconia powder to the zirconia sol is such that the total amount of yttria and zirconia is 30 to 95% by weight in the slurry, and the weight ratio of Y 2 O 3 / ZrO 2 is 0.5 to 40, preferably Add to 20-40.
【０００６】スラリー中のイットリアとジルコニアの合
計量が３０重量％未満では塗型の膜が形成できず好まし
くない。９５重量％を越えると安定なスラリーとならな
い。Ｙ2 Ｏ3 ／ＺｒＯ2 の重量比が０．５未満では活性
金属の表面に対する汚染が起こり好ましくなく、重量比
が４０を越えると塗型の膜が形成できないので好ましく
ない。If the total amount of yttria and zirconia in the slurry is less than 30% by weight, a coating film cannot be formed, which is not preferable. If it exceeds 95% by weight, a stable slurry will not be obtained. When the weight ratio of Y 2 O 3 / ZrO 2 is less than 0.5, contamination of the surface of the active metal is not preferred, and when the weight ratio exceeds 40, a coating film cannot be formed, which is not preferred.
【０００７】このイットリアとジルコニアの混合の際
に、分散を十分にするために、ディスパー等で混合する
のが好ましい。更に、イットリア粉末及びジルコニア粉
末の分散を助け、塗布しやすくするため水、水溶性有機
溶剤、界面活性剤を加えても良い。水溶性有機溶媒とし
ては、ジメチルホルムアミド、ジメチルアセトアミド、
Ｎ−メチルピロリドン等の非プロトン性極性有機溶剤を
加えることが好ましい。また、メタノール、エタノー
ル、プロパノール等の水溶性アルコールを加えても良
い。水溶性有機溶媒の添加量は１〜１０重量％の範囲で
ある。At the time of mixing yttria and zirconia, it is preferable to mix them with a disper or the like in order to sufficiently disperse them. Further, water, a water-soluble organic solvent, and a surfactant may be added to assist in dispersing the yttria powder and the zirconia powder and to facilitate application. Examples of the water-soluble organic solvent include dimethylformamide, dimethylacetamide,
It is preferable to add an aprotic polar organic solvent such as N-methylpyrrolidone. Further, a water-soluble alcohol such as methanol, ethanol and propanol may be added. The amount of the water-soluble organic solvent added is in the range of 1 to 10% by weight.
【０００８】本発明で用いる、ジルコニアゾルは、例え
ば、特開昭５９- １０７９６９号公報に示された方法で
得られた。透過型電子顕微鏡法により測定した、粒子径
は２〜２００ｎｍで、かつ、ｐＨ２〜４、濃度１０〜３
０重量％の酸性ジルコニアゾル及びそのゾルを、特開平
２ -１６７８２６号公報に示された方法でアルカリ化
し、１０〜４０重量％に濃縮することで得る事ができ
る。ジルコニアゾル中のジルコニアの粒子径は２〜２０
０ｎｍの間で、より好ましくは２〜１００ｎｍである。
また、ジルコニアゾルのｐＨは４〜１３、好ましくは、
ｐＨ７〜１３、より好ましくはｐＨ７〜１０の間であ
る。The zirconia sol used in the present invention was obtained, for example, by the method disclosed in JP-A-59-107969. Particle size measured by transmission electron microscopy is 2 to 200 nm, pH 2 to 4, concentration 10 to 3
It can be obtained by alkalizing 0% by weight of acidic zirconia sol and its sol by the method disclosed in JP-A-2-167826, and concentrating to 10 to 40% by weight. The particle size of zirconia in the zirconia sol is 2 to 20
It is between 0 nm and more preferably between 2 and 100 nm.
Further, the pH of the zirconia sol is 4 to 13, preferably,
It is between pH 7 and 13, more preferably between pH 7 and 10.
【０００９】本発明に用いる、ジルコニア粉末は、粒子
径が０．０５μｍ〜１００μｍの間で、好ましくは、
０．１μｍ〜３０μｍの間であり、市販品として入手可
能である。The zirconia powder used in the present invention has a particle diameter of 0.05 μm to 100 μm, preferably
It is between 0.1 μm and 30 μm and is commercially available.
【００１０】イットリア粉末は、粒子径が０．１μｍ〜
１００μｍの間で、より好ましくは、０．１μｍ〜３０
μｍの間であり、市販品として入手可能可能である。本
発明に用いる、界面活性剤としては、カチオン系界面活
性剤、ノニオン系界面活性剤、アニオン系界面活性剤の
うちから選ばれる、一種または、一種以上の界面活性剤
を用いることができる。The yttria powder has a particle diameter of 0.1 μm or less.
100 μm, more preferably 0.1 μm to 30 μm
It is between μm and is commercially available. As the surfactant used in the present invention, one or more surfactants selected from a cationic surfactant, a nonionic surfactant, and an anionic surfactant can be used.
【００１１】上記の成分の濃度を調整して最適化を図
る。粘度の範囲はザーンカップＮｏ．５で、８秒から４
０秒の間が好ましい。The concentration of the above components is adjusted for optimization. The range of viscosity is Zahn Cup No. 5 from 8 seconds to 4
Preferably between 0 seconds.
【００１２】このようにして得た本発明のコールドクル
ーシブル炉用塗型材は、コールドクルーシブル炉用塗型
材をコールドクルーシブル炉の表面に塗布した後、乾燥
し、コールドクルーシブル炉の内壁に薄膜状のセラミッ
クス層を形成させるものである。[0012] The coating material for a cold crucible furnace of the present invention obtained as described above is obtained by applying the coating material for a cold crucible furnace to the surface of the cold crucible furnace, drying the coating material, and forming a thin ceramic on the inner wall of the cold crucible furnace. A layer is formed.
【００１３】本発明の塗型材を塗布することにより、コ
ールドクルーシブル炉への直接の熱の移動が阻止でき、
更に輻射熱による熱移動も抑えられるため、メルテイン
グストックの量を多くすることができ、また、内部塗型
材料による汚染も少なくできる。By applying the coating material of the present invention, direct heat transfer to the cold crucible furnace can be prevented,
Further, since heat transfer due to radiant heat is suppressed, the amount of the melting stock can be increased, and the contamination by the internal coating material can be reduced.
【００１４】以下実施例で本発明を更に詳細に説明す
る。Hereinafter, the present invention will be described in more detail with reference to Examples.
【実施例】実施例１ アルカリ性ジルコニアゾル（日産化学工業社製 ＮＺＳ
−３０ＢＥ ジルコニア濃度 ３０重量％、ｐＨ９．
４）１５ｇにイットリア粉末５０ｇ、ジルコニア粉末５
ｇ、ジメチルホルムアミド（ＤＭＦ）５ｇ、界面活性剤
（花王クエーカー社製 ＯＴＰ）０．１ｍｇ及び純水５
ｇを混合し、ｐＨ９のスラリーを得た。このスラリーの
組成はジルコニア１２．５重量％、イットリア６２．５
重量％、ＤＭＦ ６．２重量％、水１８．８％、界面活
性剤０．０００１２重量％であった。EXAMPLES Example 1 Alkaline zirconia sol (NZS manufactured by Nissan Chemical Industries, Ltd.)
-30BE Zirconia concentration 30% by weight, pH 9.
4) 50 g of yttria powder and 5 of zirconia powder in 15 g
g, dimethylformamide (DMF) 5 g, surfactant (OTP manufactured by Kao Quaker) 0.1 mg and pure water 5
g was mixed to obtain a slurry having a pH of 9. The composition of this slurry was 12.5% by weight of zirconia and 62.5% of yttria.
% By weight, 6.2% by weight of DMF, 18.8% of water, and 0.00012% by weight of surfactant.
【００１５】この得られたスラリーをコールドクルーシ
ブル炉内に塗布し、乾燥して、高融点材料であるＴｉＡ
ｌ合金（Ａｌ３４重量％ 大同特殊鋼社製 融点１５３
０℃）７０ｇを入れ、高周波コイル内に装着し、溶解し
た。コールドクルーシブル炉内で冷却後コールドクルー
シブル炉内のＴｉＡｌの付着高さを測定した。また、冷
却後のＴｉＡｌ合金中のジルコニア及びイットリアの濃
度を測定した。測定結果を表１に示す。尚、鋳物中のＺ
ｒとＹの含有量は波長分散型Ｘ線マイクロアナザー（Ｅ
ＰＭＡ−ＷＤＸ）を用いて測定した。The obtained slurry is applied in a cold crucible furnace and dried to obtain a high melting point material such as TiA.
1 alloy (Al 34% by weight, manufactured by Daido Steel Co., Ltd., melting point 153
(0 ° C.), 70 g was put in a high-frequency coil, and dissolved. After cooling in the cold crucible furnace, the adhesion height of TiAl in the cold crucible furnace was measured. In addition, the concentrations of zirconia and yttria in the TiAl alloy after cooling were measured. Table 1 shows the measurement results. In addition, Z in the casting
The content of r and Y is determined by the wavelength-dispersed X-ray microanalyzer (E
PMA-WDX).
【００１６】比較例１ 塗型材を用いてないコールドクルーシブル炉を用いて実
施例１と同じように、ＴｉＡｌ合金を溶解し、付着高さ
を測定した。結果を表１に示す。[0016] In the same manner as in Example 1 using a cold crucible furnace is not used Comparative Example 1 coating material to dissolve the TiAl alloy was measured adhesion height. Table 1 shows the results.
【００１７】[0017]
【表１】 [Table 1]
【００１８】[0018]
【発明の効果】表１に示したように、本発明の塗型をし
ても、高融点材料はあまり成分的に影響を受けないこと
がわかる。また、付着高さは、本発明の塗型を施すこと
により、著しく低下させることができる。これは、コー
ルドクルーシブル炉への瞬間的な熱移動を抑制できるこ
とを示すものであり、メルテイングストックの量を多く
できることを示しており、高効率の溶解ができ、工業上
有用な効果がもたらされる。As shown in Table 1, it can be seen that the high melting point material is not so affected by the components even when the mold of the present invention is applied. Also, the adhesion height can be significantly reduced by applying the coating of the present invention. This indicates that the instantaneous heat transfer to the cold crucible furnace can be suppressed, and that the amount of the melting stock can be increased. .
───────────────────────────────────────────────────── フロントページの続き (72)発明者 田中 弘明 東京都千代田区神田錦町３丁目７番地１ 日産化学工業株式会社内 審査官 長者 義久 (56)参考文献 特開 平５−322451（ＪＰ，Ａ) 特開 平５−133685（ＪＰ，Ａ) 特開 平３−134485（ＪＰ，Ａ) 特開 平４−362144（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) F27D 1/00,11/06 B22D 41/02 C01G 25/02 F27B 14/00 - 14/10 H05B 6/24 ──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Hiroaki Tanaka 3-7-1, Kandanishikicho, Chiyoda-ku, Tokyo Nissan Chemical Industry Co., Ltd. Examiner Chihisa Yoshihisa (56) References JP-A-5-322451 (JP, A JP-A-5-133685 (JP, A) JP-A-3-134485 (JP, A) JP-A-4-362144 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) F27D 1 / 00,11 / 06 B22D 41/02 C01G 25/02 F27B 14/00-14/10 H05B 6/24
Claims (2)
アとジルコニアの合計量が３０〜９５重量％で、且つＹ
2 Ｏ3 ／ＺｒＯ2 の重量比が０．５〜４０であるｐＨ４
〜１３のスラリーから成ることを特徴とするコールドク
ルーシブル炉用塗型材。1. The method according to claim 1, wherein the composition contains yttria and zirconia, the total amount of yttria and zirconia is 30 to 95% by weight, and Y
PH 4 where the weight ratio of 2 O 3 / ZrO 2 is 0.5 to 40
A coating material for a cold crucible furnace, comprising the slurry of any one of (1) to (13).
ニア粉末をイットリアとジルコニアの合計量が３０〜９
５重量％で、且つＹ2 Ｏ3 ／ＺｒＯ2 の重量比が０．５
〜４０になるように加え、ｐＨ４〜１３のスラリーを得
ることを特徴とする、コールドクルーシブル炉用塗型材
の製造方法。2. A zirconia sol containing yttria powder and zirconia powder in a total amount of 30 to 9 of yttria and zirconia.
5% by weight and the weight ratio of Y 2 O 3 / ZrO 2 is 0.5
A method for producing a mold material for a cold crucible furnace, characterized in that a slurry having a pH of 4 to 13 is obtained in addition to 40.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16200692A JP3198281B2 (en) | 1992-05-28 | 1992-05-28 | Coating material for cold crucible furnace and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16200692A JP3198281B2 (en) | 1992-05-28 | 1992-05-28 | Coating material for cold crucible furnace and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05322452A JPH05322452A (en) | 1993-12-07 |
| JP3198281B2 true JP3198281B2 (en) | 2001-08-13 |
Family
ID=15746256
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16200692A Expired - Lifetime JP3198281B2 (en) | 1992-05-28 | 1992-05-28 | Coating material for cold crucible furnace and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3198281B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4496623B2 (en) * | 2000-08-18 | 2010-07-07 | シンフォニアテクノロジー株式会社 | Induction heating melting furnace |
| JP5374063B2 (en) * | 2007-03-28 | 2013-12-25 | 三菱重工業株式会社 | Metal melting crucible and surface treatment method thereof |
| US8007712B2 (en) * | 2007-04-30 | 2011-08-30 | General Electric Company | Reinforced refractory crucibles for melting titanium alloys |
-
1992
- 1992-05-28 JP JP16200692A patent/JP3198281B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05322452A (en) | 1993-12-07 |
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