JPH1017958A - Production of oxide dispersion strengthened type chromium base alloy - Google Patents

Production of oxide dispersion strengthened type chromium base alloy

Info

Publication number
JPH1017958A
JPH1017958A JP8176297A JP17629796A JPH1017958A JP H1017958 A JPH1017958 A JP H1017958A JP 8176297 A JP8176297 A JP 8176297A JP 17629796 A JP17629796 A JP 17629796A JP H1017958 A JPH1017958 A JP H1017958A
Authority
JP
Japan
Prior art keywords
alloy
oxide dispersion
sintered
powder
inert gas
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
Application number
JP8176297A
Other languages
Japanese (ja)
Inventor
Michio Okabe
道生 岡部
Tomoki Yamamoto
知己 山本
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Daido Steel Co Ltd
Original Assignee
Daido Steel Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Daido Steel Co Ltd filed Critical Daido Steel Co Ltd
Priority to JP8176297A priority Critical patent/JPH1017958A/en
Publication of JPH1017958A publication Critical patent/JPH1017958A/en
Pending legal-status Critical Current

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  • Powder Metallurgy (AREA)

Abstract

PROBLEM TO BE SOLVED: To improve the toughness of an alloy material and to enable machining thereto by heating a sintered allay material at a prescribed temp. in an inert gas. SOLUTION: This alloy is produced from powder contg. at least, by mass, high m.p. metallic oxide and >=57% Cr and produced by a mechanical allaying method. As the above high m.p. metallix oxide, Y2 O3 or the like can be adopted. Furthermore, the above powder may contain a small amt. of Zr, La or the like as well as <=20% Fe. Then, it is subjected to hot hydrostatic pressing and is subjected to compacting and sintering to obtain a sintered alloy having high density. Next, this material is heated at >=1400 deg.C in an inert gas. In this way, the strains stored at the inside of the sintered alloy material are released to improve its toughness, and, in the subsequent machining such as cutting, the generation of defects such as cracking, chipping or the like can be prevented.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、酸化物分散強化型
クロム基合金の製造性の改善に関する。
The present invention relates to an improvement in the productivity of an oxide dispersion strengthened chromium-based alloy.

【0002】[0002]

【従来の技術】出願人らは、特願平7−16371号に
おいて高温における耐酸化性および強度に優れる酸化物
分散強化型合金を提案した。この合金は、Cr基金属粉
末と、高融点金属酸化物粉末と、Zr、La、Ce、N
d、Yなどの金属粉末とを、メカニカルアロイング法に
よって処理することにより、各成分の緊密かつ均一な混
合物粉末に加工し、該混合物粉末を熱間押出し加工また
は熱間静水圧加圧(HIP)処理により圧粉成形すると
共に焼結する。
2. Description of the Related Art The applicants have proposed an oxide dispersion strengthened alloy having excellent oxidation resistance and strength at high temperatures in Japanese Patent Application No. 7-16371. This alloy comprises a Cr-based metal powder, a high melting point metal oxide powder, Zr, La, Ce, N
By processing a metal powder such as d and Y by a mechanical alloying method, it is processed into a tight and uniform mixture powder of each component, and the mixture powder is subjected to hot extrusion or hot isostatic pressing (HIP). ) The powder is compacted and sintered by the treatment.

【0003】次いで、前記焼結合金材を熱間押出し加工
することによって該合金材に組織異方性と内部歪とを付
与し、さらに高温加熱することによって結晶粒を粗大化
する。この状態において、合金は高い高温強度を有する
とともに、常温で適度な靭性を有するので、機械加工等
の成形加工によって所要の形状に加工して使用する。と
ころで前記混合物粉末を圧粉成形、焼結するための熱間
押出し加工またはHIP処理を行うに際しては、混合物
粉末を金属製のカプセルまたはシースに封入して行う必
要がある。また、処理後には前記カプセルまたはシース
を切削加工によって除去して焼結合金材の表面状態を整
備する必要がある。
Then, the sintered alloy material is subjected to hot extrusion to impart structural anisotropy and internal strain to the alloy material, and further heated to a high temperature to coarsen crystal grains. In this state, the alloy has high high-temperature strength and appropriate toughness at room temperature, and is used after being processed into a required shape by molding such as machining. Meanwhile, when performing the hot extrusion or the HIP treatment for compacting and sintering the mixture powder, it is necessary to encapsulate the mixture powder in a metal capsule or sheath. After the treatment, it is necessary to remove the capsule or sheath by cutting to maintain the surface condition of the sintered alloy material.

【0004】しかし、本酸化物分散強化型合金は、圧粉
成形、焼結状態では極めて脆いため、切削、研削等の機
械加工により材料に割れ、欠け等を生じという問題があ
った。表面状態が悪いと、次の工程である方向性と内部
歪とを付与するための熱間押出し加工の際に割れを生
じ、著しく歩留りを低減する。
However, the oxide dispersion-strengthened alloy of the present invention is extremely brittle in the state of compacting and sintering, and thus has a problem that the material is cracked or chipped by machining such as cutting and grinding. If the surface condition is poor, cracks occur during the next step of hot extrusion for imparting directionality and internal strain, which significantly reduces the yield.

【0005】[0005]

【発明が解決しようとする課題】本発明の目的は、酸化
物分散強化型クロム基合金の圧粉成形、焼結状態におけ
る靭性を改善することによって機械加工を可能とし、健
全で歩留の高い合金の製造方法を提供することにある。
SUMMARY OF THE INVENTION An object of the present invention is to improve the toughness of a dispersion-strengthened chromium-based alloy by compacting and sintering, thereby enabling machining, and providing a sound and high yield. An object of the present invention is to provide a method for manufacturing an alloy.

【0006】[0006]

【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クロム基合金の製造方法
は、少なくともクロム:57質量%以上と高融点金属酸
化物:0.2〜2.0質量%とを含み、メカニカルアロ
イング法により製造した粉末を、熱間静水圧加圧処理し
た後、不活性気体中において1400℃以上の温度で加
熱する工程を含むことを特徴とする。
In order to achieve the above-mentioned object, a method for producing an oxide dispersion-strengthened chromium-based alloy according to the present invention comprises the following steps: And a step of heating the powder produced by the mechanical alloying method at a temperature of 1400 ° C. or more in an inert gas after hot isostatic pressing. I do.

【0007】[0007]

【発明の実施の形態】本発明に係る酸化物分散強化型ク
ロム基合金は、少なくとも0.2〜2.0質量%の高融
点金属酸化物と57質量%以上のクロムとを含み、メカ
ニカルアロイング法によって製造した粉末から製造され
る。前記高融点金属酸化物としてはY 2 3 、Zr
2 、Al2 3 、Gd2 3 などが挙げられる。また
前記粉末には、20%以下のFeのほか、少量のZr、
La、Ce、Nd、Y、Mo、W、Si、Mn等を含ん
でいてもよい。
BEST MODE FOR CARRYING OUT THE INVENTION
ROM-based alloys have a high melting point of at least 0.2-2.0% by mass.
It contains point metal oxide and 57% by mass or more of chromium.
Manufactured from powders manufactured by the nickel alloying method
You. The refractory metal oxide is Y TwoOThree, Zr
OTwo, AlTwoOThree, GdTwoOThreeAnd the like. Also
The powder contains 20% or less of Fe, a small amount of Zr,
Including La, Ce, Nd, Y, Mo, W, Si, Mn, etc.
You may go out.

【0008】HIP処理は、通常、粉末を処理する方法
によってHIP装置を用いて行う。これによって、粉末
は、圧粉成形されるとともに焼結し、高密度の焼結合金
材となる。次いで、前記焼結合金材を不活性気体中にお
いて1400℃以上の温度で加熱する。1400℃以上
の温度で加熱することによって、焼結合金材の内部に蓄
えられた歪が開放されて靭性が改善され、その後の切削
加工等の加工によって割れや欠け等の欠陥を生じること
がなくなる。加熱温度が1400℃未満ではその効果が
十分ではないので、加熱温度は1400℃以上とする必
要がある。
[0008] The HIP process is usually performed using a HIP apparatus by a method of processing powder. As a result, the powder is compacted and sintered, and becomes a high-density sintered alloy material. Next, the sintered alloy material is heated at a temperature of 1400 ° C. or more in an inert gas. By heating at a temperature of 1400 ° C. or more, the strain stored inside the sintered alloy material is released, and the toughness is improved, and defects such as cracks and chips are not generated by subsequent processing such as cutting. . If the heating temperature is lower than 1400 ° C., the effect is not sufficient, so the heating temperature needs to be 1400 ° C. or higher.

【0009】上記の加熱を大気中等の酸素を含む雰囲気
中で行うと、前記焼結合金材の生地であるCrは、14
00℃以上の高温では、緻密で安定なCr2 3 ではな
く、蒸気圧の高いCrO3 を形成し、昇華する。これに
よって、合金内にはカーケンダールボイドが形成され、
合金が脆化する。また、窒素含有雰囲気中で加熱すると
きは、表面に硬脆なCrNが形成され、合金の加工性を
害する。それゆえ、前記加熱は不活性気体中で行う必要
がある。不活性気体としてはVIIIb 属希有ガスが挙げら
れるが、性能およびコストの面からアルゴンが好適であ
る。
When the above-mentioned heating is performed in an atmosphere containing oxygen, such as the air, Cr, which is a material of the sintered alloy material, becomes 14%.
At a high temperature of 00 ° C. or more, instead of dense and stable Cr 2 O 3 , CrO 3 having a high vapor pressure is formed and sublimates. As a result, Kirkendall voids are formed in the alloy,
The alloy becomes brittle. Further, when heating in a nitrogen-containing atmosphere, hard and brittle CrN is formed on the surface, which impairs the workability of the alloy. Therefore, the heating needs to be performed in an inert gas. As the inert gas, a rare gas belonging to Group VIIIb can be mentioned, but argon is preferred in terms of performance and cost.

【0010】以上の処理により合金の靭性が改善される
ので、HIP処理時に用いた金属カプセルの切削、研削
による除去、次工程の熱間押出し加工のための切削成形
などの機械加工が可能となる。
[0010] Since the toughness of the alloy is improved by the above treatment, machining such as cutting and grinding of the metal capsule used in the HIP treatment, and cutting and forming for hot extrusion in the next step can be performed. .

【0011】[0011]

【実施例】メカニカルアロイングによって、表1に示す
各化学組成を有する微細粉末の緊密かつ均一な混合物粉
末を作り、それぞれ軟鋼製のカプセルに充填し、脱気し
た後密封した。これを1300℃、1200kgf/c
2 の条件でHIP処理し、φ40×100mmの焼結
体を得た。
EXAMPLES Tight and uniform mixture powders of fine powders having the respective chemical compositions shown in Table 1 were prepared by mechanical alloying, filled into mild steel capsules, degassed, and sealed. This is 1300 ° C, 1200kgf / c
HIP treatment was performed under the conditions of m 2 to obtain a sintered body of φ40 × 100 mm.

【0012】[0012]

【表1】 [Table 1]

【0013】該焼結体をアルゴン雰囲気中において表2
に示す温度で3時間加熱し供試材とした。各供試材から
旋削によって平行部直径6mmのJIS14A号引張試
験片を削り出し、浸透探傷法を用いて各試験片について
割れの有無を調べた。試験は各3本の試験片について行
った。割れが発見された試験片の数を表2に示す。
The sintered body was placed in an argon atmosphere as shown in Table 2.
Was heated for 3 hours at the temperature shown in Table 1 to obtain a test material. A JIS No. 14A tensile test piece having a parallel portion diameter of 6 mm was cut out from each test material by turning, and the presence or absence of cracks was examined for each test piece using a penetrant inspection method. The test was performed on each of three test pieces. Table 2 shows the number of test pieces where cracks were found.

【0014】[0014]

【表2】 [Table 2]

【0015】表2から明らかなように、本発明の実施例
においては機械加工時の割れ感受性が改善されているこ
とが判る。
As is clear from Table 2, it can be seen that in the embodiment of the present invention, the crack sensitivity during machining is improved.

【0016】[0016]

【発明の効果】以上のように、本発明によれば、酸化物
分散強化型クロム基合金の圧粉成形、焼結状態における
靭性が改善され、機械加工が可能となる。これによって
健全で歩留の高い酸化物分散強化型クロム基合金の経済
的な製造方法を提供することができる。
As described above, according to the present invention, the toughness of the oxide dispersion strengthened chromium-based alloy in the state of compacting and sintering is improved, and machining becomes possible. Thus, a sound and economical method for producing an oxide dispersion strengthened chromium-based alloy having a high yield can be provided.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 少なくともクロム:57質量%以上と高
融点金属酸化物:0.2〜2.0質量%とを含み、メカ
ニカルアロイング法により製造した粉末を、熱間静水圧
加圧処理した後、不活性気体中において1400℃以上
の温度で加熱する工程を含むことを特徴とする酸化物分
散強化型クロム基合金の製造方法。
1. A powder containing at least 57% by mass of chromium and at least 0.2 to 2.0% by mass of a high-melting metal oxide and produced by a mechanical alloying method is subjected to hot isostatic pressing. A method of manufacturing an oxide dispersion strengthened chromium-based alloy, comprising a step of heating at a temperature of 1400 ° C. or higher in an inert gas.
JP8176297A 1996-07-05 1996-07-05 Production of oxide dispersion strengthened type chromium base alloy Pending JPH1017958A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP8176297A JPH1017958A (en) 1996-07-05 1996-07-05 Production of oxide dispersion strengthened type chromium base alloy

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP8176297A JPH1017958A (en) 1996-07-05 1996-07-05 Production of oxide dispersion strengthened type chromium base alloy

Publications (1)

Publication Number Publication Date
JPH1017958A true JPH1017958A (en) 1998-01-20

Family

ID=16011127

Family Applications (1)

Application Number Title Priority Date Filing Date
JP8176297A Pending JPH1017958A (en) 1996-07-05 1996-07-05 Production of oxide dispersion strengthened type chromium base alloy

Country Status (1)

Country Link
JP (1) JPH1017958A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
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

Cited By (2)

* Cited by examiner, † Cited by third party
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

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