JP3121901B2 - Manufacturing method of alloy powder - Google Patents
Manufacturing method of alloy powderInfo
- Publication number
- JP3121901B2 JP3121901B2 JP04034079A JP3407992A JP3121901B2 JP 3121901 B2 JP3121901 B2 JP 3121901B2 JP 04034079 A JP04034079 A JP 04034079A JP 3407992 A JP3407992 A JP 3407992A JP 3121901 B2 JP3121901 B2 JP 3121901B2
- Authority
- JP
- Japan
- Prior art keywords
- molten metal
- nozzle
- alloy powder
- alloy
- crystallized
- 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
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
【0001】[0001]
【産業上の利用分野】本発明は、アトマイズ法による合
金粉末の製造方法に関し、特に溶湯ノズルの壁面に晶出
した晶出物により該ノズルが閉塞するのを防止できるよ
うにした方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an alloy powder by an atomizing method, and more particularly to a method for preventing a nozzle of a molten metal from being clogged by a crystallized substance crystallized on a wall surface of the nozzle.
【0002】[0002]
【従来の技術】近年、Yを含むFe基の耐熱合金(Fe
−20〜25%Cr−5〜7%Al−0.005 〜1.00%Y合
金)は耐熱性, 耐酸化性に優れており、溶射用,PTA
(肉盛り溶接)用,自動車の排気ガス浄化用触媒の担体
用材料として広く利用されている。これは合金粉末の原
料が、材料送給性,組織制御,薄板化の面で特性向上に
寄与しているからである。このFe−Cr−Al−Y合
金粉末を工業的規模で製造する場合、従来、製造コスト
の点から大気溶解又は真空溶解と、水又はガス噴射との
組み合わせによるアトマイズ法が採用されている。な
お、上記真空溶解は高純度粉末の製造のみに限定されて
いる。このようなアトマイズ法では、ノズル径2〜10mm
φの溶湯ノズルから溶融金属を細く流下させ、これに高
圧ガス又は高圧水を噴射することにより合金粉末を製造
する。この場合、上記溶湯ノズル部分の温度が低下する
と溶融金属が凝固してノズルを閉塞する場合があること
から、上記溶融金属の温度、タンディッシュ,及び溶湯
ノズルの予熱温度を制御してノズルの閉塞を防止するの
が一般的である。2. Description of the Related Art In recent years, Fe-based heat-resistant alloys containing Y (Fe
-20 to 25% Cr-5 to 7% Al-0.005 to 1.00% Y alloy) has excellent heat resistance and oxidation resistance, and is used for thermal spraying and PTA.
It is widely used as a carrier material for catalysts for exhaust gas purification of automobiles (overlay welding). This is because the raw material of the alloy powder contributes to the improvement of characteristics in terms of material feedability, structure control, and thinning. In the case of producing this Fe-Cr-Al-Y alloy powder on an industrial scale, an atomizing method based on a combination of atmospheric melting or vacuum melting and water or gas injection has conventionally been adopted from the viewpoint of production cost. In addition, the above-mentioned vacuum melting is limited to only the production of high-purity powder. In such an atomizing method, the nozzle diameter is 2 to 10 mm
An alloy powder is produced by causing a molten metal to flow down finely from a melt nozzle of φ and injecting a high-pressure gas or high-pressure water into the molten metal. In this case, if the temperature of the molten metal nozzle portion decreases, the molten metal may solidify and block the nozzle. Therefore, the temperature of the molten metal, the tundish, and the preheating temperature of the molten metal nozzle are controlled to close the nozzle. Is generally prevented.
【0003】また、例えばYやAlのような活性金属元
素を含む合金の場合、溶融金属成分,大気,耐火物等が
酸素,窒素の供給源となって酸化物,窒化物が生成し易
く、これらが上記溶湯ノズルの内壁に生成,成長し、ア
トマイズの途中で溶融金属が流下しなくなり、その結果
ノズルを閉塞する場合がある。これは、溶湯ノズル内壁
の温度が溶融金属の温度より低下することにより、過飽
和状態になった溶融金属中の酸素,窒素が酸化物,窒化
物となるためであり、これらの酸化物等は熱力学的によ
り安定したものとなる。これらの酸化物,窒化物は、温
度が低くなった溶湯ノズルの内壁から溶融金属中に生
成,成長する。この晶出物の融点が溶融金属の温度より
高い場合、あるいは晶出物がクラスター状に成長した場
合、溶融金属流の流動によって流下し難くなり、この結
果ノズルの閉塞に至ることとなる。ちなみに、上記晶出
物の融点は、Y2 O3 で2500℃, Al2 O3 で2050℃,
AlNで2230℃であり、上記溶融金属の温度、例えば17
00℃より高くなっている。また、上記Fe−Cr−Al
−Y合金で生成する晶出物は、Yが例えば50ppm 以下の
少量の場合Al2 O3 又はAlNを主成分とし、Yが多
い場合Y2 O3 を主成分としている。In the case of an alloy containing an active metal element such as Y or Al, for example, a molten metal component, the atmosphere, a refractory or the like serves as a supply source of oxygen and nitrogen to easily form oxides and nitrides. These are formed and grown on the inner wall of the molten metal nozzle, and the molten metal does not flow down during the atomization, and as a result, the nozzle may be blocked. This is because oxygen and nitrogen in the supersaturated molten metal become oxides and nitrides when the temperature of the inner wall of the molten metal nozzle becomes lower than the temperature of the molten metal. It becomes more stable mechanically. These oxides and nitrides are generated and grown in the molten metal from the inner wall of the molten metal nozzle at a lowered temperature. If the melting point of the crystallized material is higher than the temperature of the molten metal, or if the crystallized material grows in a cluster, it becomes difficult to flow down due to the flow of the molten metal flow, and as a result, the nozzle is clogged. Incidentally, the crystallizate of melting point, 2500 ° C. in Y 2 O 3, 2050 ℃ in Al 2 O 3,
2230 ° C. for AlN and the temperature of the molten metal, for example, 17
It is higher than 00 ° C. In addition, the above Fe-Cr-Al
The crystallized substance generated from the -Y alloy has Al 2 O 3 or AlN as a main component when Y is a small amount of, for example, 50 ppm or less, and Y 2 O 3 as a main component when Y is large.
【0004】このような晶出物の生成による溶湯ノズル
の閉塞を防止する方法として、従来、溶湯ノズルの径を
大きくしたり,溶融金属の温度を晶出物の融点より高く
したりする方法がある。また、溶湯ノズルの壁面からガ
ス等をバブリングさせて晶出物の生成を防止したり,溶
湯ノズルを加熱したりする方法が試みられている。さら
に、O,Nの低い原料を採用したり,真空溶解法により
溶融金属中のO,Nを低減する方法もある。Conventionally, as a method of preventing the blockage of the molten metal nozzle due to the generation of the crystallized material, a method of increasing the diameter of the molten metal nozzle or increasing the temperature of the molten metal above the melting point of the crystallized material has been known. is there. Further, a method of bubbling a gas or the like from the wall surface of the molten metal nozzle to prevent generation of crystallized substances or heating the molten metal nozzle has been attempted. Further, there is a method of using a raw material having a low O and N, and a method of reducing the amount of O and N in the molten metal by a vacuum melting method.
【0005】[0005]
【発明が解決しようとする課題】しかしながら上記従来
の方法では、ノズル径を大きくしたり,溶湯温度を高く
する方法は、合金粉末の粒度分布が大きくなり、溶融金
属中の酸素が増大することから限界がある。また、溶湯
ノズルにガス等をバブリングさせるには、その構造が複
雑となり、またO,Nの低減方法では、製造コストがア
ップするという問題がある。However, in the above-mentioned conventional methods, the method of increasing the nozzle diameter or the temperature of the molten metal increases the particle size distribution of the alloy powder and increases the oxygen in the molten metal. There is a limit. In addition, bubbling gas or the like to the molten metal nozzle requires a complicated structure, and the method of reducing O and N has a problem that the manufacturing cost is increased.
【0006】本発明は上記従来の状況に鑑みてなされた
もので、合金粉末のばらつきや溶融金属中の酸素増大を
生じさせることなく、かつコストを上昇させることなく
溶湯ノズルの閉塞を防止できる合金粉末の製造方法を提
供することを目的としている。SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned conventional circumstances, and it is an alloy capable of preventing clogging of a molten metal nozzle without causing variation in alloy powder or increase in oxygen in a molten metal and without increasing cost. It is intended to provide a method for producing a powder.
【0007】[0007]
【課題を解決するための手段】そこで本発明は、Yを含
むFe系溶融金属を溶湯ノズルから流出させ、該溶融金
属に高圧ガス又は高圧水を吹きつけて合金粉末を製造す
る方法において、上記溶融金属にLaを、晶出物の融点
が溶湯温度より低くなる量だけ添加したことを特徴とし
ている。SUMMARY OF THE INVENTION Accordingly, the present invention provides a method for producing an alloy powder by causing a Fe-based molten metal containing Y to flow out of a molten metal nozzle and blowing a high-pressure gas or high-pressure water onto the molten metal. It is characterized in that La is added to the molten metal in such an amount that the melting point of the crystallized product becomes lower than the temperature of the molten metal.
【0008】ここで、上記Laの添加量は、上記溶融金
属中のYが全てY2 O3 となり、La2 O3 −20mol %
Y2 O3 に相当するLa量の0.5 〜5倍とするのが望ま
しい。例えば、100ppmYの場合、Laの添加量は312 〜
3125ppm となる。Here, the amount of La added is such that Y in the molten metal becomes Y 2 O 3 , and La 2 O 3 -20 mol%
It is desirable to set the amount of La corresponding to Y 2 O 3 to 0.5 to 5 times. For example, in the case of 100 ppmY, the amount of La added is 312 to
It becomes 3125ppm.
【0009】また、本発明方法においては、上記溶湯ノ
ズルに、溶融金属流によるエロージョンで消失する傾向
にある材料を用いるのが望ましい。このような材料で溶
湯ノズルを構成した場合は、該溶湯ノズル内壁に晶出し
た晶出物をこの壁面とともに消失させる効能があり、こ
れにより晶出物の成長の抑制効果をさらに向上できるか
らである。上記材料としては、100 %カーボン, ジルコ
ニア-30 %カーボン,ジルコニア-10 %カルシア-30 %
カーボン等が採用でき、製品粉末のカーボン汚染を考慮
して適宜選択する。In the method of the present invention, it is desirable to use, for the molten metal nozzle, a material which tends to disappear by erosion due to a molten metal flow. When the molten metal nozzle is formed of such a material, there is an effect of eliminating the crystallized material crystallized on the inner wall of the molten metal nozzle together with the wall surface, whereby the effect of suppressing the growth of the crystallized material can be further improved. is there. The above materials include 100% carbon, zirconia-30% carbon, zirconia-10% calcia-30%
Carbon or the like can be used, and is appropriately selected in consideration of carbon contamination of the product powder.
【0010】[0010]
【作用】本発明の製造方法では、Yを含むFe系溶融金
属を溶湯ノズルから流出させ、該溶融金属に高圧ガス又
は高圧水を吹きつけて合金粉末を製造する際に、上記溶
融金属にLaを所定量添加したので、これにより晶出物
の形態が変化して該晶出物の融点が溶融金属の温度より
低くなることから、晶出物は溶融金属中で液体となって
溶融流に容易に流されることとなる。その結果、溶湯ノ
ズル内壁に結晶となって析出した晶出物は、溶融流によ
り溶融金属内部への生成,成長を抑制されることとな
り、溶湯ノズルの閉塞を防止できる。ちなみに、Laの
添加により、例えばY2 O3 はY2 O3 −La2 O3 に
変化してこれの融点は約1550℃となることから、上記F
e系溶融金属の1700℃より低くなる。このように本発明
の製造方法によれば、Yを含むFe系溶融金属にLaを
添加するだけで溶湯ノズルの閉塞を確実に防止でき、上
述した従来の合金粉末の粒度分布のばらつきや溶融金属
中の酸素増大を防止できるとともに、製造コストの上昇
を抑制できる。According to the production method of the present invention, when an Fe-based molten metal containing Y is caused to flow out of a molten metal nozzle and high-pressure gas or high-pressure water is sprayed on the molten metal to produce an alloy powder, La is added to the molten metal. Is added in a predetermined amount, whereby the morphology of the crystallized material changes and the melting point of the crystallized material becomes lower than the temperature of the molten metal. It will be easily washed away. As a result, the crystallized substance precipitated as crystals on the inner wall of the molten metal nozzle is prevented from being generated and grown inside the molten metal by the molten flow, so that the molten metal nozzle can be prevented from being clogged. Incidentally, by the addition of La, for example, Y 2 O 3 changes to Y 2 O 3 -La 2 O 3 and its melting point becomes about 1550 ° C.
It is lower than 1700 ° C of e-type molten metal. As described above, according to the production method of the present invention, clogging of the molten metal nozzle can be reliably prevented only by adding La to the Fe-based molten metal containing Y, and the above-described variation in the particle size distribution of the conventional alloy powder and the molten metal It is possible to prevent an increase in oxygen inside, and to suppress an increase in manufacturing cost.
【0011】[0011]
【実施例】以下、本発明の実施例を説明する。本実施例
では、本発明の製造方法の効果を確認するために行った
実験結果について説明する。Embodiments of the present invention will be described below. Example 1 In this example, results of an experiment performed to confirm the effects of the manufacturing method of the present invention will be described.
【0012】[0012]
【表1】 [Table 1]
【0013】この実験は、表1に示すように、Fe−25
%Cr−6%Al−0.01%Y合金に、Laをそれぞれ0.
3 %,0.15 %,0.07 %添加して500Kg の本発明試料を作
成した(第1欄〜第3欄参照)。次に、この各本発明試
料を大気溶解により1700℃に溶融し、これをジルコニア
+30%カーボンからなる溶湯ノズルから流出させるとと
もに、該溶湯ノズルに高圧窒素を噴射して合金粉末を製
造した。そして、この合金粉末の回収量を調べた。ま
た、比較するために、上記合金のみの比較試料(第4欄
参照)、上記合金にLaを0.01%添加した比較試料( 第
5欄参照) 、及び上記合金をジルコニアだけからなる溶
湯ノズルから流出させた従来試料( 第6欄参照) を作成
し、同様に回収量を調べた。In this experiment, as shown in Table 1, Fe-25
% Cr-6% Al-0.01% Y alloy with La
500 kg of the sample of the present invention was prepared by adding 3%, 0.15% and 0.07% (see columns 1 to 3). Next, each of the samples of the present invention was melted at 1700 ° C. by melting in the air, and was discharged from a melt nozzle composed of zirconia + 30% carbon, and high-pressure nitrogen was injected into the melt nozzle to produce an alloy powder. Then, the recovered amount of the alloy powder was examined. Further, for comparison, a comparative sample containing only the above alloy (see column 4), a comparative sample obtained by adding 0.01% of La to the above alloy (see column 5), and a melt nozzle made of only zirconia containing the above alloy flowed out. A conventional sample (see column 6) was prepared and the amount of recovery was examined in the same manner.
【0014】表1からも明らかなように、ジルコニアか
らなる溶湯ノズルを使用した従来試料(第6欄)の場
合、合金粉末は投入量500Kg に対して50Kgしか回収でき
ておらず、溶湯ノズルの閉塞が著しい。また、溶湯ノズ
ルにジルコニア+カーボンを使用した比較試料(第4
欄)の場合は、回収量が400Kg と従来試料に比べて向上
している。これは、上記カーボンにより晶出物が溶湯ノ
ズルの壁面とともに消失したからである。さらに、La
を0.01%添加した比較試料(第5欄)の場合は、回収量
が410Kg と若干向上しているものの、該La量が少ない
ことから不充分な結果となっている。これに対して、本
発明試料(第1〜第3欄)の場合は、いずれも回収量が
455 〜475Kg と90%以上の回収率が得られている。この
ように、Laを所定量添加することによって、晶出物Y
2 O3 はY2 O3 −La2 O3 に変化して約1550℃の融
点となることから上記溶融金属の1700℃より低くなる。
この結果、上記晶出物は溶融金属中で容易に溶けること
から、溶湯ノズルの閉塞を防止できる。ここで、Laの
添加により得られた製品粉末は、耐熱性の点においても
向上することが確認できた。As is clear from Table 1, in the case of the conventional sample (column 6) using a molten metal nozzle made of zirconia, only 50 kg of the alloy powder could be recovered with respect to 500 kg of the charged amount. Obstruction is significant. In addition, a comparative sample using zirconia + carbon for the melt nozzle (No. 4)
Column), the recovered amount is 400 kg, which is higher than that of the conventional sample. This is because the crystallization disappeared together with the wall surface of the molten metal nozzle due to the carbon. Furthermore, La
In the case of the comparative sample (column 5) to which 0.01% was added, although the recovered amount was slightly improved to 410 kg, the result was insufficient because the La amount was small. On the other hand, in the case of the sample of the present invention (columns 1 to 3), the recovered amount was
A recovery rate of 455 to 475 kg and over 90% has been obtained. As described above, by adding a predetermined amount of La, the crystallized substance Y
Since 2 O 3 changes to Y 2 O 3 -La 2 O 3 and has a melting point of about 1550 ° C., it is lower than 1700 ° C. of the molten metal.
As a result, the crystallized substance is easily melted in the molten metal, so that it is possible to prevent the molten metal nozzle from being blocked. Here, it was confirmed that the product powder obtained by adding La also improved in heat resistance.
【0015】[0015]
【発明の効果】以上のように本発明に係る合金粉末の製
造方法によれば、Yを含むFe系溶融金属を溶湯ノズル
から流出させ、該溶融金属に高圧ガス又は高圧水を吹き
つけて合金粉末を製造する際に上記溶融金属にLaを添
加して晶出物の融点を溶融金属より低くしたので、それ
だけ晶出物の生成,成長を抑制でき、溶湯ノズルの閉塞
を防止できる効果がある。As described above, according to the method for producing an alloy powder according to the present invention, an Fe-based molten metal containing Y is caused to flow out of a molten metal nozzle, and a high-pressure gas or high-pressure water is blown onto the molten metal to form an alloy. Since La is added to the molten metal during the production of the powder to lower the melting point of the crystallized material compared to the molten metal, the generation and growth of the crystallized material can be suppressed accordingly, and the clogging of the molten metal nozzle can be prevented. .
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7,DB名) B22F 9/08 ──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. 7 , DB name) B22F 9/08
Claims (1)
ら流出させ、該溶融金属に高圧ガス又は高圧水を吹きつ
けて合金粉末を製造する方法において、上記溶融金属に
Laを、晶出物の融点が溶融金属の温度より低くなる量
だけ添加したことを特徴とする合金粉末の製造方法。1. A method for producing an alloy powder by causing a Fe-based molten metal containing Y to flow out of a molten metal nozzle and blowing a high-pressure gas or high-pressure water on the molten metal, wherein La is added to the molten metal, A method for producing an alloy powder, wherein the melting point of the alloy is lower than the temperature of the molten metal.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP04034079A JP3121901B2 (en) | 1992-01-24 | 1992-01-24 | Manufacturing method of alloy powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP04034079A JP3121901B2 (en) | 1992-01-24 | 1992-01-24 | Manufacturing method of alloy powder |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH05202403A JPH05202403A (en) | 1993-08-10 |
JP3121901B2 true JP3121901B2 (en) | 2001-01-09 |
Family
ID=12404260
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP04034079A Expired - Lifetime JP3121901B2 (en) | 1992-01-24 | 1992-01-24 | Manufacturing method of alloy powder |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP3121901B2 (en) |
-
1992
- 1992-01-24 JP JP04034079A patent/JP3121901B2/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
JPH05202403A (en) | 1993-08-10 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
KR20140027335A (en) | Low cost processing to produce spherical titanium and titanium alloy powder | |
JPH068170B2 (en) | Method for producing high-purity magnesium oxide fine powder | |
JP3121901B2 (en) | Manufacturing method of alloy powder | |
JPH06179930A (en) | Graphite-made crucible or mold | |
JPH09256122A (en) | Ferrous amorphous alloy | |
JP2749267B2 (en) | Method for producing Fe-Cr-Al-REM alloy powder | |
JPH09202611A (en) | Removal of boron from metallic silicon | |
JPH06279811A (en) | Production of fe-cr-al alloy powder | |
JPH09248665A (en) | Manufacture of al base alloy ingot containing high melting point metal by spray forming method | |
EP0645466B1 (en) | Catalyst material, based on a titanium-copper alloy and process for producing the same | |
JP2002030374A (en) | Hydrogen storage alloy and its production method | |
JP2867888B2 (en) | Method of preventing immersion nozzle clogging during continuous casting of Ti-containing Cr steel | |
JP3151677B2 (en) | Nozzle and melting crucible for Ti-Ni alloy | |
JPH10130011A (en) | Removing method of boron from metal silicon | |
JP2745372B2 (en) | Method for producing deformed ultrafine particles and aggregates thereof | |
SU1639893A1 (en) | Method of producing iron powder | |
JPS6013967B2 (en) | Ferroboron manufacturing method | |
JPH0273905A (en) | Production of alloy powder for rare earth element-fe-b permanent magnet | |
JPH02197507A (en) | Production of alloy powder | |
JPH0441063A (en) | Spray forming method | |
JP3089381B2 (en) | Continuous casting method of Ti-containing steel | |
JPS59220299A (en) | Production of tape-like titanium alloy for brazing | |
JPH0429726B2 (en) | ||
JP3892569B2 (en) | Method for cleaning molten steel | |
JPH02175854A (en) | Formation of porous thermally sprayed coating film |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20001010 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20081020 Year of fee payment: 8 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20081020 Year of fee payment: 8 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091020 Year of fee payment: 9 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20091020 Year of fee payment: 9 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20101020 Year of fee payment: 10 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20111020 Year of fee payment: 11 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20111020 Year of fee payment: 11 |
|
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121020 Year of fee payment: 12 |
|
EXPY | Cancellation because of completion of term | ||
FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20121020 Year of fee payment: 12 |