JPH08188844A - Oxide dispersion reinforced type heat resistant alloy - Google Patents
Oxide dispersion reinforced type heat resistant alloyInfo
- Publication number
- JPH08188844A JPH08188844A JP7016371A JP1637195A JPH08188844A JP H08188844 A JPH08188844 A JP H08188844A JP 7016371 A JP7016371 A JP 7016371A JP 1637195 A JP1637195 A JP 1637195A JP H08188844 A JPH08188844 A JP H08188844A
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- Japan
- Prior art keywords
- resistant alloy
- oxide dispersion
- less
- heat resistant
- refractory metal
- 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.)
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、耐酸化性及び高温強度
に優れたＣｒを主成分とする酸化物分散強化型耐熱合
金、特にＺｒなどを含有させて耐窒化性を向上させたＣ
ｒを主成分とする酸化物分散強化型耐熱合金に関する。BACKGROUND OF THE INVENTION The present invention relates to an oxide dispersion strengthened heat-resistant alloy containing Cr as a main component, which is excellent in oxidation resistance and high-temperature strength, and in particular, C containing Ni and the like to improve nitriding resistance.
The present invention relates to an oxide dispersion strengthened heat resistant alloy containing r as a main component.
【０００２】[0002]
【従来の技術】従来、１４５０℃以上の高温でしかも大
気中において、長時間繰返し荷重を受けるような用途に
使用できる金属材料はなかった。そこで、高温で加熱鋼
材の繰返し荷重を受ける加熱炉のスキッドレール及びス
キッドボタンには、セラミックス焼結材、耐熱合金とセ
ラミックスとの複合材料、特開平２─３８５１６号公報
に記載されている酸化物分散強化型耐熱合金（１８〜４
０％のＣｒ、５％以下のＦｅ、５％以下のＡｌ、５％以
下のＴｉ、微細な高融点金属酸化物：０．１〜２％、残
部が実質的にＮｉ）などが使用されていた。2. Description of the Related Art Heretofore, there has been no metal material which can be used for applications where it is subjected to repeated load for a long time at a high temperature of 1450 ° C. or higher and in the atmosphere. Therefore, in the skid rail and skid button of the heating furnace which receives the repeated load of the heated steel material at high temperature, a ceramic sintered material, a composite material of a heat-resistant alloy and ceramics, and an oxide described in JP-A-2-38516. Dispersion strengthened heat resistant alloy (18-4
0% Cr, 5% or less Fe, 5% or less Al, 5% or less Ti, fine refractory metal oxide: 0.1 to 2%, the balance being substantially Ni), etc. are used. It was
【０００３】[0003]
【発明が解決しようとする課題】しかし、セラミックス
焼結材は高温強度が高いが、構造材料としては使用する
ことができない。また耐熱合金は衝撃に強いが、１３０
０℃以上の高温では強度、耐酸性に乏しい。また耐熱合
金とセラミックスとの複合材料は、高温強度はある程度
改善されているが、１３００℃以上の高温では強度、耐
酸性がまだ十分でなかった。また、上記酸化物分散強化
型耐熱合金は、１４００℃まで加熱する炉には有効であ
るが、それ以上の温度に加熱される炉には使用できなか
った。さらに、従来のＣｒを主成分とした酸化物分散強
化型耐熱合金は、高温で加熱をされるような条件で使用
すると、Ｃｒ2 Ｎが析出して脆化するので、１４５０℃
以上の温度で長時間使用することができなかった。本発
明は、１４５０℃以上の高温での繰返し荷重及び繰返し
加熱をされても窒化により脆化がないＣｒを主成分とし
た酸化物分散強化型耐熱合金を提供することを目的とす
る。However, although the ceramic sintered material has high high temperature strength, it cannot be used as a structural material. Also, heat-resistant alloys are strong against impact, but 130
At high temperatures above 0 ° C, it lacks strength and acid resistance. The high temperature strength of the composite material of heat resistant alloy and ceramics has been improved to some extent, but the strength and acid resistance were still insufficient at high temperatures of 1300 ° C. or higher. Further, the above oxide dispersion strengthened heat-resistant alloy is effective in a furnace heated to 1400 ° C., but could not be used in a furnace heated to a temperature higher than that. Further, the conventional oxide dispersion strengthened heat-resistant alloy containing Cr as the main component, when used under the condition of being heated at high temperature, causes Cr 2 N to precipitate and becomes brittle.
It could not be used for a long time at the above temperature. An object of the present invention is to provide an oxide dispersion strengthened heat-resistant alloy containing Cr as a main component, which does not become brittle due to nitriding even when subjected to repeated load and repeated heating at a high temperature of 1450 ° C. or higher.
【０００４】[0004]
【課題を解決するための手段】上記目的を達成するため
に、本発明の酸化物分散強化型耐熱合金においては、重
量％で、Ｆｅ：２０％以下、高融点金属酸化物：０．２
〜２．０％含有し、残部が実質的にＣｒである酸化物分
散強化型耐熱合金にＺｒ、Ｌａ、Ｃｅ、Ｎｄ及びＹの１
種又は２種以上を合計量で０．５〜５％含有させたこと
である。また、重量％で、Ｆｅ：２０％以下、Ｍｏ及び
Ｗの１種または２種を合計量で０．５〜１０％、高融点
金属酸化物を０．２〜２．０％含有し、残部実質的にＣ
ｒである酸化物分散強化型耐熱合金にＺｒ、Ｌａ、Ｃ
ｅ、Ｎｄ及びＹの１種又は２種以上を合計量で０．５〜
５％含有させたことである。さらに、不純物としてＳ
ｉ：３％以下及びＭｎ：３％以下を含有している上記各
酸化物分散強化型耐熱合金にＺｒ、Ｌａ、Ｃｅ、Ｎｄ及
びＹの１種又は２種以上を合計量で０．５〜５％含有さ
せたことである。In order to achieve the above object, in the oxide dispersion strengthened heat-resistant alloy of the present invention, Fe: 20% or less by weight%, refractory metal oxide: 0.2
˜2.0% and the balance is substantially Cr, and the oxide dispersion strengthened heat-resistant alloy contains 1 of Zr, La, Ce, Nd and Y.
That is, 0.5 to 5% in total is contained. Further, in weight%, Fe: 20% or less, 0.5 to 10% in total of one or two kinds of Mo and W, and 0.2 to 2.0% of refractory metal oxide, and the balance. Substantially C
Zr, La, C in the oxide dispersion strengthened heat resistant alloy which is r
One or two or more of e, Nd, and Y in a total amount of 0.5 to
That is, 5% was included. Furthermore, S as an impurity
i: 3% or less and Mn: 3% or less, each of the above oxide dispersion strengthened heat-resistant alloys contains one or more of Zr, La, Ce, Nd, and Y in a total amount of 0.5 to That is, 5% was included.
【０００５】上記発明をさらに説明すると、高融点金属
酸化物はＹ2 Ｏ3 、ＺｒＯ2 、Ａｌ2 Ｏ3 、Ｇｄ2 Ｏ3
などであり、その大きさは０．１μ以下が好ましい。ま
た本発明の合金の用途は、上記加熱炉のスキッドレール
及びスキッドボタン、極超音速航空機材料などである。
そして、本発明の酸化物分散強化型耐熱合金は、Ｆｅ−
Ｃｒの合金粉末、若しくはＦｅ、Ｃｒ単体金属粉末、Ｚ
ｒ、Ｌａ、Ｃｅ、Ｎｄ及びＹの金属粉末及び高融点金属
酸化物粉末、又はこれらの粉末にＭｏ及びＷ粉末を加え
た粉末をメカニカル・アロイング法により各成分が微細
粉末の緊密かつ均一な混合物粉末をつくり、この混合物
を熱間押出又は熱間静水圧プレスにより圧粉成形及び焼
結して製造することができる。To further explain the above invention, refractory metal oxides include Y 2 O 3 , ZrO 2 , Al 2 O 3 and Gd 2 O 3.
Etc., and the size is preferably 0.1 μm or less. Applications of the alloy of the present invention include skid rails and skid buttons of the above heating furnace, and hypersonic aircraft materials.
The oxide dispersion strengthened heat resistant alloy of the present invention is Fe-
Alloy powder of Cr, or Fe, Cr simple metal powder, Z
A close and uniform mixture of fine powders of each component by mechanical alloying of r, La, Ce, Nd and Y metal powders and refractory metal oxide powders or powders obtained by adding Mo and W powders to these powders. It can be produced by making a powder, pressing and sintering the mixture by hot extrusion or hot isostatic pressing.
【０００６】[0006]
【作用】本発明は、重量％で、Ｆｅ：２０％以下、高融
点金属酸化物：０．２〜２．０％含有し、残部実質的に
Ｃｒである酸化物分散強化型耐熱合金、又はこの合金に
Ｍｏ及びＷの１種または２種を合計量で０．５〜１０％
含有する酸化物分散強化型耐熱合金にＺｒ、Ｌａ、Ｃ
ｅ、Ｎｄ及びＹの１種又は２種以上を合計量で０．５〜
５％含有させたことにより、高温においてＺｒ、Ｌａ、
Ｃｅ、Ｎｄ又はＹが先に窒化され、Ｃｒが窒化されるこ
とがないので、その結果Ｃｒ2 Ｎが析出することによる
脆化を防ぐことができる。According to the present invention, an oxide dispersion strengthened heat resistant alloy containing, by weight, Fe: 20% or less, refractory metal oxide: 0.2 to 2.0%, and the balance being substantially Cr, or This alloy contains one or two of Mo and W in a total amount of 0.5 to 10%.
Zr, La, C in the oxide dispersion strengthened heat resistant alloy contained
One or two or more of e, Nd, and Y in a total amount of 0.5 to
By containing 5%, Zr, La,
Since Ce, Nd, or Y is nitrided first and Cr is not nitrided, as a result, embrittlement due to precipitation of Cr 2 N can be prevented.
【０００７】次に、各成分を限定した理由を説明する。 Ｆｅ：２０％以下 Ｆｅは、合金の微細な空隙を少なくし、強度及び靱性を
高くするために有効な元素であるが、２０％を超えて含
有させると融点を下げ、耐酸化性を劣化するので、その
含有量を２０％以下とした。 Ｍｏ及びＷの１種又は２種：０．５〜１０％ Ｍｏ及びＷは、マトリックスを固溶強化する元素である
が、０．５％より少なくないとその効果が殆どなく、ま
た多くなると耐酸化性を劣化するので、その含有量を
０．５〜１０％とした。 高融点金属酸化物：０．２〜２．０％ 高融点金属酸化物は、マトリックスに分散してその高温
強度を高くする成分である。この効果は０．２％以上で
得られ、２．０％で飽和するので、その含有量を０．２
〜２．０％にした。Next, the reason for limiting each component will be described. Fe: 20% or less Fe is an element effective for reducing fine voids in the alloy and increasing strength and toughness, but if it exceeds 20%, the melting point is lowered and the oxidation resistance is deteriorated. Therefore, the content is set to 20% or less. One or two kinds of Mo and W: 0.5 to 10% Mo and W are elements that solid-solution strengthen the matrix. Therefore, its content is set to 0.5 to 10% because it deteriorates the chemical conversion property. High-melting point metal oxide: 0.2 to 2.0% The high-melting point metal oxide is a component dispersed in a matrix to increase its high temperature strength. This effect is obtained at 0.2% or more and saturated at 2.0%, so the content is 0.2%.
~ 2.0%.
【０００８】Ｚｒ、Ｌａ、Ｃｅ、Ｎｄ及びＹの１種又は
２種以上：０．５〜５％ Ｚｒ、Ｌａ、Ｃｅ、Ｎｄ及びＹは、上記の如くＣｒが窒
素と結合してＣｒ2 Ｎを析出して脆化するのを防ぐため
であるが、その含有量が０．５％より少ないと添加効果
が僅かであり、また５％を超えると、Ｃｒのもつ優れた
耐酸化性が損なわれるので、その含有量を０．５〜５％
とした。 Ｓｉ：３％以下、Ｍｎ：３％以下 Ｓｉ及びＭｎは不純物で、少ないほうが好ましいが、３
％以下であれば、高温強度及び耐酸化性を低下すること
が少ないので、その含有量を３％以下とした。One or more of Zr, La, Ce, Nd and Y: 0.5 to 5% Zr, La, Ce, Nd and Y are Cr 2 N in which Cr is bonded to nitrogen as described above. This is to prevent the precipitation and embrittlement of Cr, but if the content is less than 0.5%, the effect of addition is slight, and if it exceeds 5%, the excellent oxidation resistance of Cr is impaired. Therefore, its content is 0.5-5%
And Si: 3% or less, Mn: 3% or less Si and Mn are impurities, and the smaller the amount, the better.
%, The high temperature strength and the oxidation resistance are less likely to decrease, so the content is set to 3% or less.
【０００９】[0009]
【実施例】以下、本発明の実施例について説明する。Ｆ
ｅ、Ｃｒ、Ｗ、Ｍｏ、Ｚｒ、Ｌａ、Ｃｅ、Ｎｄ及びＹの
平均粒径約１００μの粉末及び高融点金属酸化物の約１
μの粉末を表１及び表２に示した割合になるようにボー
ルミルに入れ、メカニカル・アロイング処理を行い、出
来た粉末を金属カプセルに充填し、脱気した後密封し
た。これをこれを１２５０℃で熱間押出しにより成形
し、更に１５５０℃で２時間加熱して二次再結晶により
結晶粒を５００μｍ以上に調整して各種供試材を作っ
た。これらの供試材から試験片を切り出し、各種の試験
をした。Embodiments of the present invention will be described below. F
e, Cr, W, Mo, Zr, La, Ce, Nd and Y powders having an average particle size of about 100 μ and about 1% of a refractory metal oxide.
The powder of μ was put in a ball mill so that the ratio was as shown in Table 1 and Table 2, mechanical alloying treatment was performed, and the resulting powder was filled in a metal capsule, deaerated, and sealed. This was molded by hot extrusion at 1250 ° C., and further heated at 1550 ° C. for 2 hours to adjust the crystal grain to 500 μm or more by secondary recrystallization to make various test materials. Test pieces were cut out from these test materials and subjected to various tests.
【００１０】（１）クリープ破断試験 供試材から直径６ｍｍの試験片を切り出し、１４００
℃、３ｋｇｆ／ｍｍ2 の条件でクリープ破断試験を行っ
た。その結果を表１及び表２のクリープ破断時間の欄に
記載した。 （２）繰り返し酸化試験 供試材から直径１０ｍｍ、長さ５０ｍｍの円柱状試験片
を切り出し、図１に示した加熱と冷却を大気中で３回行
い、試験片に残ったスケールをアルカリ溶液及び酸溶液
で除去し、その前後の試験片重量の変化から、重量の変
化を求めた。その結果を表１の重量減量欄に記載した。(1) Creep rupture test A test piece with a diameter of 6 mm was cut out from the test material, and 1400
A creep rupture test was performed under the conditions of 3 ° C. and 3 kgf / mm 2 . The results are shown in the creep rupture time column of Tables 1 and 2. (2) Repeated Oxidation Test A cylindrical test piece having a diameter of 10 mm and a length of 50 mm was cut out from the test material and heated and cooled as shown in FIG. 1 three times in the atmosphere, and the scale remaining on the test piece was treated with an alkaline solution and The acid solution was removed, and the change in weight was determined from the change in the weight of the test piece before and after the removal. The results are shown in the weight loss column of Table 1.
【００１１】[0011]
【表１】 [Table 1]
【００１２】[0012]
【表２】 [Table 2]
【００１３】表１及び表２より明らかなように、Ｚｒ、
Ｌａ、Ｃｅ、Ｎｄ及びＹを添加した酸化物分散強化型耐
熱合金は、これらを添加していない比較例の合金と比較
すると、クリープ破断時間が大幅に改善され、また酸化
による重量減量もかなり改善されていることが分かる。
また、繰り返し酸化試験をした試験片を切断し、断面を
ＥＰＭＡによる測定をしたところ、Ｚｒ、Ｌａ、Ｃｅ、
Ｎｄ及びＹを添加しなかった比較例の酸化物分散強化型
耐熱合金は、粒界にＣｒ2 Ｎが析出していたのに対し
て、Ｚｒ、Ｌａ、Ｃｅ、Ｎｄ及びＹを添加した本発明の
実施例のものは、ＺｒＮなどの窒化物が結晶粒全体に均
一に分散していることが確認された。As is clear from Tables 1 and 2, Zr,
The oxide dispersion strengthened heat-resistant alloy with La, Ce, Nd and Y added has significantly improved creep rupture time and significantly reduced weight loss due to oxidation, as compared with the alloys of Comparative Examples in which these are not added. You can see that it is done.
In addition, when a test piece subjected to repeated oxidation test was cut and the cross section was measured by EPMA, Zr, La, Ce,
In the oxide dispersion strengthened heat-resistant alloy of the comparative example in which Nd and Y were not added, Cr 2 N was precipitated at the grain boundaries, whereas the present invention in which Zr, La, Ce, Nd and Y were added was used. It was confirmed that in the example, the nitride such as ZrN was uniformly dispersed throughout the crystal grains.
【００１４】本発明は、上記以外の点においても実施例
に限定されることなく、要旨を変更しない範囲において
種々の変更をすることが出来ることはもちろんである。The present invention is not limited to the embodiments in points other than the above, and it is needless to say that various modifications can be made without departing from the scope of the invention.
【００１５】[0015]
【本発明の効果】本発明は、上記成分組成にしたことに
より、１４５０℃以上の高温における耐酸化性、耐窒化
性及び高温強度が改善するという優れた効果を奏する。
また、この結果１４５０℃以上の高温で使用するスラ
ブ、ビレットなどの鋼材加熱用ウォーキングビームコン
ベアー式加熱炉のスキッドレール、スキッドボタンなど
の各種部材、極超音速航空機材料などに使用することが
できるようになった。EFFECTS OF THE INVENTION The present invention has the excellent effects of improving the oxidation resistance, nitriding resistance and high temperature strength at a high temperature of 1450 ° C. or higher by virtue of the above composition.
Further, as a result, it can be used for slabs used at high temperatures of 1450 ° C. or higher, skid rails of walking beam conveyor type heating furnaces for heating steel materials such as billets, various members such as skid buttons, and hypersonic aircraft materials. Became.
【図１】 本発明及び比較例の酸化物分散強化型耐熱合
金の耐酸化性を試験するための繰り返し酸化試験におけ
る加熱及び冷却条件を説明するための説明図である。FIG. 1 is an explanatory diagram for explaining heating and cooling conditions in a repeated oxidation test for testing the oxidation resistance of oxide dispersion strengthened heat resistant alloys of the present invention and a comparative example.
Claims (4)
属酸化物：０．２〜２．０％、Ｚｒ、Ｌａ、Ｃｅ、Ｎｄ
及びＹの１種又は２種以上を合計量で０．５〜５％含有
し、残部が実質的にＣｒであることを特徴とする酸化物
分散強化型耐熱合金。1. By weight%, Fe: 20% or less, refractory metal oxide: 0.2 to 2.0%, Zr, La, Ce, Nd.
And 1 or 2 or more of Y in a total amount of 0.5 to 5%, and the balance being substantially Cr.
属酸化物：０．２〜２．０％、Ｍｏ及びＷの１種または
２種を合計量で０．５〜１０％、Ｚｒ、Ｌａ、Ｃｅ、Ｎ
ｄ及びＹの１種又は２種以上を合計量で０．５〜５％含
有し、残部実質的にＣｒであることを特徴とする酸化物
分散強化型耐熱合金。2. By weight%, Fe: 20% or less, refractory metal oxide: 0.2 to 2.0%, one or two of Mo and W in a total amount of 0.5 to 10%, Zr, La, Ce, N
An oxide dispersion-strengthened heat-resistant alloy, containing one or more of d and Y in a total amount of 0.5 to 5%, and the balance being substantially Cr.
属酸化物：０．２〜２．０％、Ｓｉ：３％以下、Ｍｎ：
３％以下、Ｚｒ、Ｌａ、Ｃｅ、Ｎｄ及びＹの１種又は２
種以上を合計量で０．５〜５％含有し、残部が実質的に
Ｃｒであることを特徴とする酸化物分散強化型耐熱合
金。3. By weight%, Fe: 20% or less, refractory metal oxide: 0.2 to 2.0%, Si: 3% or less, Mn:
3% or less, one or two of Zr, La, Ce, Nd and Y
An oxide dispersion-strengthened heat-resistant alloy, characterized in that it contains 0.5 to 5% in total of at least one species, and the balance is substantially Cr.
属酸化物：０．２〜２．０％、Ｍｏ及びＷの１種または
２種を合計量で０．５〜１０％、Ｓｉ：３％以下、Ｍ
ｎ：３％以下、Ｚｒ、Ｌａ、Ｃｅ、Ｎｄ及びＹの１種又
は２種以上を合計量で０．５〜５％を含有し、残部実質
的にＣｒであることを特徴とする酸化物分散強化型耐熱
合金。4. By weight%, Fe: 20% or less, refractory metal oxide: 0.2 to 2.0%, one or two kinds of Mo and W in a total amount of 0.5 to 10%, Si: 3% or less, M
n: 3% or less, one or two or more of Zr, La, Ce, Nd and Y in a total amount of 0.5 to 5%, and the balance being substantially Cr. Dispersion strengthened heat resistant alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7016371A JPH08188844A (en) | 1995-01-09 | 1995-01-09 | Oxide dispersion reinforced type heat resistant alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7016371A JPH08188844A (en) | 1995-01-09 | 1995-01-09 | Oxide dispersion reinforced type heat resistant alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08188844A true JPH08188844A (en) | 1996-07-23 |
Family
ID=11914450
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7016371A Pending JPH08188844A (en) | 1995-01-09 | 1995-01-09 | Oxide dispersion reinforced type heat resistant alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08188844A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010219045A (en) * | 2009-03-12 | 2010-09-30 | Plansee Se | Inter-connector for high-temperature solid electrolyte fuel cell |
| JP2016534228A (en) * | 2013-09-02 | 2016-11-04 | プランゼー エスエー | Powder or powder granule containing chromium |
-
1995
- 1995-01-09 JP JP7016371A patent/JPH08188844A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010219045A (en) * | 2009-03-12 | 2010-09-30 | Plansee Se | Inter-connector for high-temperature solid electrolyte fuel cell |
| US9029044B2 (en) | 2009-03-12 | 2015-05-12 | Plansee Se | Interconnector for a high-temperature solid electrolyte fuel cell, method of producing a fuel cell, and high-temperature solid electrolyte fuel cell |
| JP2016534228A (en) * | 2013-09-02 | 2016-11-04 | プランゼー エスエー | Powder or powder granule containing chromium |
| US10464130B2 (en) | 2013-09-02 | 2019-11-05 | Plansee Se | Chromium-containing powder or granulated powder |
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