JPH07179901A - Production of raw powder for dispersed oxide-reinforced cr-base sintered alloy - Google Patents
Production of raw powder for dispersed oxide-reinforced cr-base sintered alloyInfo
- Publication number
- JPH07179901A JPH07179901A JP5324217A JP32421793A JPH07179901A JP H07179901 A JPH07179901 A JP H07179901A JP 5324217 A JP5324217 A JP 5324217A JP 32421793 A JP32421793 A JP 32421793A JP H07179901 A JPH07179901 A JP H07179901A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- oxide
- finely dispersed
- mechanical alloying
- sintered alloy
- 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.)
- Withdrawn
Links
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、アトライタ装置を用い
て、酸化物分散強化型Ｃｒ基耐熱合金の焼結用原料粉末
を製造する方法の改良に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an improvement in a method for producing a raw material powder for sintering an oxide dispersion strengthened Cr-base heat resistant alloy using an attritor device.
【０００２】[0002]
【従来技術及び問題点】出願人は、以前に、高温におけ
る強度及び耐酸化性にすぐれた酸化物分散強化耐熱焼結
合金を提案した(特開平４−３２５６５１)。2. Description of the Related Art The applicant has previously proposed an oxide dispersion strengthened heat resistant sintered alloy having excellent strength and oxidation resistance at high temperatures (Japanese Patent Laid-Open No. 4-325651).
【０００３】この耐熱焼結合金の焼結用原料粉末は、Ｃ
ｒ基金属(実質的にＣｒからなる金属又はＣｒを主体と
する金属)粉末及びＹ2Ｏ3の如き酸化物粉末を、アトラ
イタ装置(高エネルギー攪拌ボールミル)の中で攪拌して
メカニカルアロイング処理を施し、金属マトリックス中
に、平均粒径約0.1μm以下の酸化物0.2〜2.0％を微細分
散させた粒子である。The raw material powder for sintering of this heat-resistant sintered alloy is C
Mechanical alloying treatment by stirring an r-based metal (metal substantially consisting of Cr or a metal mainly composed of Cr) powder and an oxide powder such as Y 2 O 3 in an attritor device (high energy stirring ball mill). And 0.2 to 2.0% of oxides having an average particle size of about 0.1 μm or less are finely dispersed in a metal matrix.
【０００４】メカニカルアロイング処理は、従来、図１
に示す如きアトライタ装置を用いて行なわれている。鋼
球(2)を一杯入れたタンク(4)の中に、Ｃｒ基合金粉末と
酸化物粉末を装入し、攪拌棒(6)を高速回転させて粉末
と鋼球を激しく衝突させることにより機械的合金化(メ
カニカルアロイング)が達成される。なお、アトライタ
装置の運転中、粉末は鋼球からの衝撃を受けて、圧縮、
粉砕、凝着が繰り返される。これらの粉末は、粉砕され
ると新たな表面が露出するが、新しい表面は活性である
ため、大気雰囲気中では、酸化、窒化を招来する不都合
がある。このため、通常、Ａｒガス雰囲気中で行なわれ
る。つまり、粉末をタンク(4)に投入後、施蓋密閉し、
弁(12)(14)を開いて入口導管(8)からＡｒガスを導入し
て、所定時間、出口導管(10)から排出し、タンク(4)内
の空気をＡｒガスと完全に置換してから、弁(12)(14)を
閉じることによりタンク内はＡｒガス雰囲気となる。The mechanical alloying process is conventionally performed as shown in FIG.
It is performed using an attritor device as shown in FIG. By loading Cr-based alloy powder and oxide powder into a tank (4) filled with steel balls (2) and rotating the stirring rod (6) at high speed to violently collide the powder with the steel balls. Mechanical alloying is achieved. During operation of the attritor device, the powder was compressed by the impact of the steel balls.
Crushing and adhesion are repeated. When these powders are crushed, a new surface is exposed, but since the new surface is active, there is a disadvantage that it causes oxidation and nitriding in the air atmosphere. Therefore, it is usually performed in an Ar gas atmosphere. That is, after pouring the powder into the tank (4), sealing the lid,
Open the valves (12) and (14) to introduce Ar gas from the inlet conduit (8) and discharge it from the outlet conduit (10) for a predetermined time to completely replace the air in the tank (4) with Ar gas. Then, by closing the valves (12) and (14), the inside of the tank becomes an Ar gas atmosphere.
【０００５】しかし、このように細心の注意を払ってメ
カニカルアロイング処理を施しても、金属粉末の材料ロ
ットによっては、金属マトリックス中に微細酸化物が均
一に分散した組織を得られないことがあった。そこで、
処理時間を長くすると、どの材料ロットの金属粉末を使
用しても、所望通りの酸化物微細分散組織を得られるこ
とが判った。このような現象は、金属粉末中に含まれる
不純物等が機械的合金化(メカニカルアロイング)に微妙
な影響を及ぼしているものと推測されるが、はっきりと
した原因は不明である。However, even with such a careful mechanical alloying treatment, it is not possible to obtain a structure in which fine oxides are uniformly dispersed in the metal matrix depending on the material lot of the metal powder. there were. Therefore,
It has been found that when the treatment time is extended, the desired oxide fine dispersion structure can be obtained regardless of the material powder of any material lot. It is presumed that such a phenomenon has a delicate influence on the mechanical alloying (mechanical alloying) by impurities contained in the metal powder, but the definite cause is unknown.
【０００６】もし、金属マトリックス中への酸化物の微
細分散状態が不十分な粉末を原料に用いて焼結を行なう
と、焼結品は所定の高温圧縮強度を具備することができ
ない。従って、どの材料ロットの金属粉末に対しても、
酸化物の微細分散状態を良好にするためには、メカニカ
ルアロイングの処理時間は十分な余裕(例えば、通常の
処理時間約48時間に対して、72時間の処理)をみて実施
せねばならず、生産効率が悪かった。また、メカニカル
アロイング処理に付す前に、金属粉末の検査を行ない、
その検査結果に応じて粉末に最適な処理時間を設定する
ことも可能であるが、検査に膨大な手間がかかるため、
実用的ではない。[0006] If sintering is performed by using as a raw material a powder in which the fine dispersion state of the oxide in the metal matrix is insufficient, the sintered product cannot have a predetermined high temperature compressive strength. Therefore, for any material lot of metal powder,
In order to improve the finely dispersed state of the oxide, the mechanical alloying treatment time must be performed with a sufficient margin (for example, the treatment time of 72 hours against the usual treatment time of 48 hours). , Production efficiency was poor. In addition, before subjecting to mechanical alloying treatment, inspection of metal powder is performed,
Although it is possible to set the optimum processing time for powders according to the inspection results, it takes a lot of time and labor for inspection, so
Not practical.
【０００７】[0007]
【発明が解決しようとする課題】本発明は、メカニカル
アロイング処理によって得られた焼結用原料粉末につい
て、金属マトリックスへの酸化物の分散状態が仮に不十
分であっても、その後の焼結によって、所定の高温圧縮
強度を備えた焼結品を形成できる方法を提供することを
目的とする。DISCLOSURE OF THE INVENTION The present invention relates to a sintering raw material powder obtained by a mechanical alloying treatment, even if the dispersion state of the oxide in the metal matrix is insufficient, the subsequent sintering is performed. It is an object of the present invention to provide a method capable of forming a sintered product having a predetermined high temperature compressive strength.
【０００８】[0008]
【課題を解決するための手段】アトライタ装置には、Ｃ
ｒ基金属粉末と酸化物粉末と共に、既にＣｒ金属マトリ
ックス中に酸化物が微細分散した粉末を同時に投入して
メカニカルアロイング処理を行なうようにしたものであ
る。投入する酸化物微細分散金属粉末は、メカニカルア
ロイングの通常の処理時間よりも十分余裕をみて実施し
たものを使用する。酸化物微細分散金属粉末の投入量
は、Ｃｒ基金属粉末100重量部に対して、約10〜50重量
部が望ましい。[Means for Solving the Problems] The attritor device includes a C
The mechanical alloying treatment is carried out by simultaneously charging the powder containing finely dispersed oxide in the Cr metal matrix together with the r-based metal powder and the oxide powder. As the oxide finely dispersed metal powder to be charged, one which is used with a sufficient margin compared to the usual processing time of mechanical alloying is used. The amount of the oxide finely dispersed metal powder added is preferably about 10 to 50 parts by weight with respect to 100 parts by weight of the Cr-based metal powder.
【０００９】[0009]
【作用】使用したＣｒ基金属粉末が機械的合金化しにく
い材料ロットのものであって、通常の処理時間内に金属
マトリックス中に酸化物が十分に微細分散しなかった場
合でも、既に金属マトリックス中に酸化物が微細分散し
ている粉末が含まれている。これらの粉末を原料に用い
て焼結を行なうと、その酸化物微細分散粉末が種となっ
て焼結され、全ての粒子が金属マトリックス中に酸化物
が微細分散された粉末を原料に用いた場合と同じ様な要
領にて焼結される。[Function] Even when the Cr-based metal powder used is a material lot that is difficult to mechanically alloy and the oxide is not sufficiently finely dispersed in the metal matrix within the normal processing time, it is already in the metal matrix. Contains powder in which oxides are finely dispersed. When these powders were used as raw materials for sintering, the oxide finely dispersed powders were used as seeds for sintering, and all the particles were finely dispersed oxides in the metal matrix. It is sintered in the same way as the case.
【００１０】[0010]
【発明の効果】メカニカルアロイング処理後における酸
化物の微細分散状態の如何に拘わらず、得られた焼結品
は所定の高温圧縮強度を具備することができるから、従
来のように、メカニカルアロイングの処理時間を必要以
上に長くしなくてもよい。結果的に処理時間を短縮する
ことができ、生産性を高めることができる。EFFECTS OF THE INVENTION The sintered product obtained can have a predetermined high-temperature compressive strength regardless of the finely dispersed state of the oxide after the mechanical alloying treatment. The processing time of the ing does not have to be made longer than necessary. As a result, the processing time can be shortened and the productivity can be improved.
【００１１】[0011]
【実施例】Ｆｅ15％、残部実質的にＣｒからなり、平均
粒度約100μmのＦｅ−Ｃｒ合金粉末2kgと、平均粒度約1
μmのＹ2Ｏ3粉末20gをアトライタ装置に投入し、48時
間、メカニカルアロイング処理を行なった。使用したア
トライタ装置は三井化工機製のＭＡ−１Ｄであり、タン
ク内には3/8インチのSUJ-2鋼球を17.5kg充填し、装置の
運転中は雰囲気ガスとしてＡｒガスを導入した。[Example] 2 kg of Fe-Cr alloy powder having an average particle size of about 100 μm, consisting of 15% Fe and the balance substantially Cr, and an average particle size of about 1
20 g of the Y 2 O 3 powder of μm was put into the attritor device, and mechanical alloying treatment was performed for 48 hours. The attritor device used was MA-1D manufactured by Mitsui Kakoki, 17.5 kg of 3/8 inch SUJ-2 steel balls was filled in the tank, and Ar gas was introduced as an atmospheric gas during the operation of the device.
【００１２】このときに得られた粉末を原料に用いて、
1250℃、1200kgf/cm2の条件でＨＩＰ(熱間静水圧加圧)
処理に付し、直径50mm、長さ70mmの焼結品を作った。Using the powder obtained at this time as a raw material,
HIP (hot isostatic pressurization) under the conditions of 1250 ° C and 1200 kgf / cm 2.
After processing, a sintered product with a diameter of 50 mm and a length of 70 mm was made.
【００１３】得られた焼結品について高温圧縮試験を行
なったところ、変形量は10％もあった。このときの原料
粉末は酸化物の微細分散状態が不十分であったと思われ
る。When a high-temperature compression test was conducted on the obtained sintered product, the amount of deformation was 10%. At this time, it is considered that the raw material powder had an insufficient oxide finely dispersed state.
【００１４】そこで、同じ材料ロットの合金粉末を用い
て、72時間、同じ要領にてメカニカルアロイング処理を
行ない、得られた粉末を同じようにＨＩＰ処理して高温
圧縮試験を行なったところ、変形量は0.5％と小さく良
好であった。このときの原料粉末は酸化物が十分均一に
微細分散されている状態にあると思われる。Therefore, the alloy powder of the same material lot was subjected to mechanical alloying treatment for 72 hours in the same manner, and the obtained powder was subjected to HIP treatment in the same manner and subjected to a high temperature compression test. The amount was as small as 0.5% and was good. It is considered that the raw material powder at this time is in a state where the oxide is finely and uniformly dispersed.
【００１５】更に、同じ材料ロットの合金粉末の10％
を、前記の72時間の処理により得られた粉末と置き換え
てメカニカルアロイング処理を行ない、得られた粉末を
ＨＩＰ処理して高温圧縮試験を行なったところ、変形量
は０.５％と小さく良好であった。Furthermore, 10% of alloy powder of the same material lot
Was replaced with the powder obtained by the treatment for 72 hours, and mechanical alloying treatment was performed. The obtained powder was HIP-treated and subjected to a high temperature compression test. The deformation amount was as small as 0.5% and was good. Met.
【００１６】上記の結果から、メカニカルアロイング処
理での酸化物の分散状態が不十分であっても、酸化物が
十分に微細分散されている良質な粉末が若干量含まれて
さえいれば、その良質粉末が焼結時に種となって所定品
質の焼結品を形成できることがわかる。From the above results, even if the dispersion state of the oxide in the mechanical alloying treatment is insufficient, as long as a small amount of good quality powder in which the oxide is sufficiently finely dispersed is contained, It can be seen that the high-quality powder becomes a seed during sintering and can form a sintered product of a predetermined quality.
【００１７】なお、高温圧縮試験は、1350℃の電気炉の
中で、ラムの昇降により、圧縮荷重0.5kgf/mm2を反復負
荷して行なった。荷重反復パターンは、圧縮荷重0.5kgf
/mm2の負荷を5秒間、無負荷5秒間(負荷状態から無負荷
状態への移行1秒、無負荷状態3秒、無負荷状態から負荷
状態への移行1秒)の10秒サイクルにて、焼結品に104回
圧縮荷重を作用させて変形量(単位：％)を調べた。な
お、変形量は、試験前の長さをＬ1、試験後の長さをＬ2
としたとき、次式により求めた。 圧縮変形量(％) ＝ (Ｌ1−Ｌ2)／Ｌ1 × 100The high temperature compression test was carried out by repeatedly raising and lowering a compression load of 0.5 kgf / mm 2 in an electric furnace at 1350 ° C. by raising and lowering the ram. Repeated load pattern is 0.5kgf compression load
/ mm 2 load for 5 seconds, no load for 5 seconds (1 second from load state to no load state, 3 seconds from no load state, 1 second from no load state to load state) in 10 second cycle The amount of deformation (unit:%) was examined by applying a compressive load 10 4 times to the sintered product. The amount of deformation is L1 before the test and L2 after the test.
Was calculated by the following formula. Compressive deformation amount (%) = (L1-L2) / L1 x 100
【図１】アトライタ装置の概要図である。FIG. 1 is a schematic diagram of an attritor device.
(2) 鋼球 (4) タンク (6) 攪拌棒 (2) Steel ball (4) Tank (6) Stir bar
Claims (1)
タ装置の中でメカニカルアロイング処理を施し、Ｃｒ基
金属のマトリックス中に酸化物が微細分散した組織を有
する焼結合金用原料粉末を製造する方法において、メカ
ニカルアロイング処理は、既にＣｒ金属マトリックス中
に酸化物が微細分散した粉末を、Ｃｒ基金属粉末と酸化
物粉末と共にアトライタ装置に投入して行なうことを特
徴とする、酸化物分散強化型Ｃｒ基焼結合金用原料粉末
の製法。1. A Cr-based metal powder and an oxide powder are mechanically alloyed in an attritor to produce a raw material powder for a sintered alloy having a structure in which an oxide is finely dispersed in a Cr-based metal matrix. In the method described above, the mechanical alloying treatment is carried out by introducing a powder in which an oxide is finely dispersed in a Cr metal matrix into an attritor device together with a Cr-based metal powder and an oxide powder. A method for producing a raw material powder for a reinforced Cr-based sintered alloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5324217A JPH07179901A (en) | 1993-12-22 | 1993-12-22 | Production of raw powder for dispersed oxide-reinforced cr-base sintered alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5324217A JPH07179901A (en) | 1993-12-22 | 1993-12-22 | Production of raw powder for dispersed oxide-reinforced cr-base sintered alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH07179901A true JPH07179901A (en) | 1995-07-18 |
Family
ID=18163356
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5324217A Withdrawn JPH07179901A (en) | 1993-12-22 | 1993-12-22 | Production of raw powder for dispersed oxide-reinforced cr-base sintered alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07179901A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016534228A (en) * | 2013-09-02 | 2016-11-04 | プランゼー エスエー | Powder or powder granule containing chromium |
-
1993
- 1993-12-22 JP JP5324217A patent/JPH07179901A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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|---|---|---|---|
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