JPH0633166A - Manufacture of oxide dispersion-strengthened heat resistant alloy sintered compact - Google Patents
Manufacture of oxide dispersion-strengthened heat resistant alloy sintered compactInfo
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- JPH0633166A JPH0633166A JP4193551A JP19355192A JPH0633166A JP H0633166 A JPH0633166 A JP H0633166A JP 4193551 A JP4193551 A JP 4193551A JP 19355192 A JP19355192 A JP 19355192A JP H0633166 A JPH0633166 A JP H0633166A
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- powder
- sintered
- metal
- weight
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、酸化物分散耐熱合金粒
子からなる粉末の焼結に関し、特に複雑形状焼結体の製
造に好適な粉末焼結方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to the sintering of powder made of oxide-dispersed heat-resistant alloy particles, and more particularly to a powder sintering method suitable for producing a complex-shaped sintered body.
【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(特願平３−９７０００)。BACKGROUND OF THE INVENTION The applicant has previously proposed an oxide dispersion strengthened heat-resistant sintered alloy having excellent strength and oxidation resistance at high temperatures (Japanese Patent Application No. 3-97000).
【０００３】この焼結合金は、実質的にＣｒからなる金
属又はＣｒを主体とする金属のマトリックス中に、平均
粒径0.1μm以下のＹ2Ｏ3を0.2〜2.0重量％微細分散させ
た原料粉末をメカニカルアロイング法によって調製し、
該原料粉末を適当な金属カプセルに充填した後、脱気密
封し、約1000〜1300℃の温度にて、約1000〜2000kgf/cm
2の圧力下で熱間静水圧処理(ＨＩＰ)される。これは、
いわゆるカプセルＨＩＰ焼結法といわれるもので、この
カプセルＨＩＰ焼結によって、略完全に緻密な焼結品を
製造することができる。This sintered alloy is a raw material prepared by finely dispersing 0.2 to 2.0% by weight of Y 2 O 3 having an average particle size of 0.1 μm or less in a matrix of a metal consisting essentially of Cr or a metal mainly composed of Cr. The powder is prepared by the mechanical alloying method,
After filling the raw material powder in a suitable metal capsule, it is degassed and hermetically sealed, and at a temperature of about 1000 to 1300 ° C., about 1000 to 2000 kgf / cm 2.
Hot isostatic pressing (HIP) is performed under a pressure of 2 . this is,
This is called a so-called capsule HIP sintering method, and a substantially completely dense sintered product can be manufactured by this capsule HIP sintering.
【０００４】ウォーキングビーム式加熱炉用スキッドボ
タンの如きブロック形状の焼結品は、一般に、このカプ
セルＨＩＰ焼結によって製造されている。A block-shaped sintered product such as a skid button for a walking beam heating furnace is generally manufactured by this capsule HIP sintering.
【０００５】しかし、例えばタービンブレードの如く、
複雑形状の製品を作る場合も、一旦ＨＩＰによって緻密
な焼結体ブロックを作製した後、機械加工によって所望
形状に切り出していた。このため、複雑形状の焼結品
は、材料歩留りが非常に悪く、製品コストが高くなる問
題があった。However, for example, as in a turbine blade,
Also in the case of producing a product having a complicated shape, a dense sintered body block is once produced by HIP and then cut into a desired shape by machining. Therefore, the sintered product having a complicated shape has a problem that the material yield is very low and the product cost is high.
【０００６】複雑形状の焼結品も、このように焼結体ブ
ロックを形成してから切削等の機械加工を行なうのは、
カプセルＨＩＰ焼結の場合、複雑形状のカプセルを製作
することが非常に困難だからである。また、多大の工数
をかけて複雑形状のカプセルを製作しても、カプセル内
の全ての場所で均一密度になるように原料粉末を充填す
ることはできない。特にカプセルの隅部は、充填密度が
小さくなるため、ＨＩＰ後の収縮量も多くなる。このた
め、カプセルの隅部については、その後の機械加工のた
めの加工しろを十分に考慮してカプセル設計せねばなら
ず、焼結体ブロックから切り出すのと実質的に変わらな
くなってしまう。For a sintered product having a complicated shape, it is necessary to perform machining such as cutting after forming the sintered body block in this way.
This is because in the case of capsule HIP sintering, it is very difficult to manufacture a capsule having a complicated shape. Further, even if a capsule having a complicated shape is manufactured by taking a great number of man-hours, it is not possible to fill the raw material powder so as to have a uniform density at every place in the capsule. In particular, in the corners of the capsules, the packing density is small, so the amount of shrinkage after HIP is also large. Therefore, the corners of the capsule must be designed with sufficient consideration of the machining allowance for the subsequent machining, which is substantially the same as cutting out from the sintered block.
【０００７】一方、この酸化物分散強化耐熱合金粒子か
らなる粉末の焼結をカプセルを使用せずに、プレス、鋳
込み、射出成形、冷間静水圧加圧(ＣＩＰ)等によって所
望形状のグリーンコンパクトに形成した後、該コンパク
トを高温で焼結すると次のような問題があった。On the other hand, sintering of the powder consisting of the oxide dispersion strengthened heat-resistant alloy particles is carried out by pressing, casting, injection molding, cold isostatic pressing (CIP), etc., without using a capsule, to obtain a green compact of a desired shape. When the compact was sintered at a high temperature after being formed into the above, there were the following problems.
【０００８】上記焼結合金はＣｒを約70％以上含んでい
るから、融点は約1700℃以上もの高温になる。また、そ
の融点はＣｒの含有量が多くなるほど高くなる。緻密な
焼結体を得るには、原則として原料成分の融点近傍の温
度で焼結せねばならないが、このような高温で焼結する
と、金属マトリックス中に微細分散していた酸化物が金
属結晶の粒界に凝集し、強度が著しく低下する不都合が
あった。これでは、酸化物を均一に微細分散させて高温
圧縮強度を向上させる意味がない。Since the above-mentioned sintered alloy contains about 70% or more of Cr, the melting point becomes as high as about 1700 ° C. or more. Further, the melting point increases as the Cr content increases. In principle, in order to obtain a dense sintered body, it is necessary to sinter at a temperature near the melting point of the raw material components, but when sintered at such a high temperature, the oxide finely dispersed in the metal matrix becomes a metal crystal. However, there is a problem in that the particles are aggregated at the grain boundaries and the strength is significantly reduced. In this case, there is no point in improving the high temperature compressive strength by uniformly finely dispersing the oxide.
【０００９】一方、Ｃｒを約70％以上含むグリーンコン
パクトを、酸化物の凝集を起こさない温度条件(約1500
℃以下)で焼結すると、焼結品の密度は完全緻密体の約7
5％程度にまでしか達しないため、所望の高温強度が得
られず、実用に供することはできない。焼結品の気孔を
消失させて、より緻密な構造とするためには、更に熱間
静水圧加圧(ＨＩＰ)を行なえばよいが、ＨＩＰ前の焼結
品の密度が完全緻密体の約94％以上なければ、ＨＩＰを
行なっても圧力がかからず、ＨＩＰによる密度向上効果
は殆んど期待できない。On the other hand, the green compact containing about 70% or more of Cr is subjected to a temperature condition (about 1500
When sintered at a temperature below ℃), the density of the sintered product is about 7
Since it reaches only about 5%, the desired high temperature strength cannot be obtained and it cannot be put to practical use. In order to eliminate the pores of the sintered product and make it a more dense structure, hot isostatic pressing (HIP) may be performed, but the density of the sintered product before HIP is about the same as that of a completely dense body. If it is not more than 94%, no pressure is applied even if HIP is carried out, and the density improving effect by HIP can hardly be expected.
【００１０】[0010]
【発明が解決しようとする課題】本発明は、酸化物分散
耐熱合金粒子からなる粉末の焼結において、金属カプセ
ルを使用せず、かつ約1500℃よりも高温に加熱せずに緻
密な焼結品が得られる焼結法を提供することを目的とす
る。DISCLOSURE OF THE INVENTION The present invention is directed to the sintering of powder consisting of oxide-dispersed heat-resistant alloy particles, without using a metal capsule and without performing heating to a temperature higher than about 1500 ° C. The object is to provide a sintering method by which a product can be obtained.
【００１１】[0011]
【課題を解決するための手段】本発明は、実質的にＣｒ
からなる金属又はＣｒを主体とする金属のマトリックス
中に、平均粒径0.1μm以下のＹ2Ｏ3を0.2〜2.0重量％微
細分散させた原料粉末の焼結において、グリーンコンパ
クトを約1500℃以下の温度で焼結することによって、完
全緻密体の約94％以上の密度を有する焼結体を形成でき
るようにしたもので、この焼結体をさらにＨＩＰするこ
とによって非常に緻密な焼結品が得られるようにしたも
のである。The present invention substantially comprises Cr.
In the sintering of the raw material powder in which 0.2 to 2.0% by weight of Y 2 O 3 having an average particle diameter of 0.1 μm is finely dispersed in the matrix of the metal consisting of It is possible to form a sintered body having a density of about 94% or more of a completely dense body by sintering at the temperature of, and a very dense sintered product by further HIPing this sintered body. Is obtained.
【００１２】本発明の焼結法は、実質的にＣｒからなる
金属又はＣｒを主体とする金属のマトリックス中に、平
均粒径0.1μm以下のＹ2Ｏ3を0.2〜2.0重量％微細分散さ
せた原料粉末100重量部に対して、Ｆｅ粉末、Ｎｉ粉末
及びＣｏ粉末からなる群から選択された少なくとも１種
以上の粉末１〜５重量部(合計量)を混合する工程、得ら
れた混合物を所定形状のグリーンコンパクトに形成する
工程、該コンパクトを焼結する工程、及び、得られた焼
結体を熱間静水圧加圧する工程を有している。According to the sintering method of the present invention, 0.2 to 2.0% by weight of Y 2 O 3 having an average particle diameter of 0.1 μm or less is finely dispersed in a matrix of a metal substantially consisting of Cr or a metal mainly composed of Cr. A step of mixing 1 to 5 parts by weight (total amount) of at least one powder selected from the group consisting of Fe powder, Ni powder and Co powder with 100 parts by weight of the raw material powder, The method includes a step of forming a green compact having a predetermined shape, a step of sintering the compact, and a step of hot isostatic pressing of the obtained sintered body.
【００１３】なお、前記混合工程では、実質的にＣｒか
らなる金属又はＣｒを主体とする金属の粉末と0.2〜2.0
重量％のＹ2Ｏ3を混合した原料粉末100重量部に対し
て、Ｆｅ粉末、Ｎｉ粉末及びＣｏ粉末からなる群から選
択された少なくとも１種以上の粉末１〜５重量部(合計
量)をメカニカルアロイング処理することにより、金属
のマトリックス中に平均粒径0.1μm以下のＹ2Ｏ3を微細
分散させた酸化物分散強化合金粉末の調製と、前記１種
以上の粉末との混合を同時に行なうこともできる。In the mixing step, a metal powder consisting essentially of Cr or a metal powder mainly composed of Cr and 0.2 to 2.0 are mixed.
1 to 5 parts by weight (total amount) of at least one kind of powder selected from the group consisting of Fe powder, Ni powder and Co powder is added to 100 parts by weight of the raw material powder mixed with wt% Y 2 O 3. Preparation of oxide-dispersion-strengthening alloy powder in which Y 2 O 3 having an average particle size of 0.1 μm or less is finely dispersed in a metal matrix by mechanical alloying treatment and mixing with the one or more powders at the same time are performed. You can also do it.
【００１４】なお、グリーンコンパクトの焼結体は、完
全緻密体の約94％以上の密度を具備できるようにする。
その後のＨＩＰによって、ほぼ完全に緻密な焼結体が得
られるようにするためである。The green compact sintered body can have a density of about 94% or more of that of a completely compact body.
This is because it is possible to obtain an almost completely dense sintered body by the subsequent HIP.
【００１５】金属は、実質的にＣｒからなる金属、又は
Ｆｅ20％以下を含み、残部実質的にＣｒからなる金属、
又はＡｌ、Ｍｏ、Ｗ、Ｎｂ、Ｔａ、Ｈｆ及びＡｌ−Ｔｉ
から構成される群の中から選択される少なくとも一種を
合計量で10％以下含み、残部実質的にＣｒからなる金
属、又はＡｌ、Ｍｏ、Ｗ、Ｎｂ、Ｔａ、Ｈｆ及びＡｌ−
Ｔｉから構成される群の中から選択される少なくとも一
種を合計量で10％以下並びにＦｅ20％以下を含み、残部
実質的にＣｒからなる金属である。なお、Ａｌ−Ｔｉは
金属間化合物である。これら金属のマトリックスに、平
均粒径0.1μm以下のＹ2Ｏ3を0.2〜2.0重量％微細分散さ
せることにより、焼結製品として、1300℃を超える温度
域で使用した場合、高い圧縮変形抵抗性を有し、また酸
化性雰囲気において安定した酸化抵抗性を確保できる。The metal is a metal consisting essentially of Cr, or a metal containing 20% or less of Fe and the balance consisting essentially of Cr,
Or Al, Mo, W, Nb, Ta, Hf and Al-Ti
A metal containing 10% or less in total of at least one selected from the group consisting of, and the balance consisting essentially of Cr, or Al, Mo, W, Nb, Ta, Hf and Al-
It is a metal that contains at least one selected from the group consisting of Ti in a total amount of 10% or less and Fe of 20% or less, and the balance substantially consists of Cr. Al-Ti is an intermetallic compound. By finely dispersing 0.2 to 2.0% by weight of Y 2 O 3 having an average particle size of 0.1 μm or less in the matrix of these metals, when used as a sintered product in a temperature range exceeding 1300 ° C., high compression deformation resistance is obtained. In addition, stable oxidation resistance can be ensured in an oxidizing atmosphere.
【００１６】酸化物分散強化耐熱合金粒子からなる原料
粉末と、Ｆｅ、Ｎｉ、Ｃｏ粉末の少なくとも１種とを略
均一に混合する。原料粉末の粒子間にＦｅ等の微細粒子
を介在させることにより、これら微細粒子が焼結の橋渡
し的役割を発揮し、原料粉末の焼結性を向上させること
ができる。Ｆｅ、Ｎｉ、Ｃｏ粉末の添加量が、原料粉末
100重量部に対して１重量部に満たないと、原料粉末の
焼結性向上効果は期待できない。一方、添加量が５重量
部を超えると、焼結時に添加粉末粒子が母合金に十分固
溶されずに粒子界面に残存し、酸化物分散強化耐熱合金
粒子が本来的に備える特性が損なわれ、高温における強
度が低下する。かかる理由から、添加混合するＦｅ、Ｎ
ｉ、Ｃｏの粉末は、酸化物分散強化耐熱合金100重量部
に対して１〜５重量部とする。A raw material powder composed of oxide dispersion strengthened heat resistant alloy particles and at least one of Fe, Ni and Co powders are mixed substantially uniformly. By interposing fine particles such as Fe between the particles of the raw material powder, these fine particles play a bridging role in sintering, and the sinterability of the raw material powder can be improved. The addition amount of Fe, Ni, and Co powder is the raw material powder
If the amount is less than 1 part by weight with respect to 100 parts by weight, the effect of improving the sinterability of the raw material powder cannot be expected. On the other hand, if the amount added exceeds 5 parts by weight, the additive powder particles do not form a solid solution in the mother alloy during sintering and remain at the particle interface, impairing the inherent properties of the oxide dispersion strengthened heat resistant alloy particles. , The strength at high temperature decreases. For this reason, Fe and N to be added and mixed
The powder of i and Co is 1 to 5 parts by weight with respect to 100 parts by weight of the oxide dispersion strengthened heat resistant alloy.
【００１７】添加するＦｅ、Ｎｉ、Ｃｏ粉末の粒径は微
細であることが望ましく、少なくとも原料粉末よりも粒
径を小さくする必要がある。望ましい粒径サイズは、約
10μm以下である。The Fe, Ni and Co powders to be added preferably have a fine particle size, and it is necessary to make the particle size at least smaller than that of the raw material powder. The desired particle size is about
It is 10 μm or less.
【００１８】[0018]
【作用】原料粉末の合金粒子間に、Ｆｅ、Ｎｉ、Ｃｏの
１種又は２種以上の微細粒子が介在するから、原料粉末
の粒子界面で拡散が起こり易くなり、融点よりも低温で
相互拡散が起こり、焼結緻密化するものと考えられる。
従って、Ｃｒを70％以上含有し、融点が約1700℃を超え
る原料粉末であっても、約1500℃以下の温度での焼結に
よって、完全緻密体の約94％以上の密度を備えた焼結体
を得ることができる。[Function] Since one or more fine particles of Fe, Ni, and Co are present between the alloy particles of the raw material powder, diffusion easily occurs at the particle interface of the raw material powder, and mutual diffusion occurs at a temperature lower than the melting point. Is considered to occur, resulting in sintering and densification.
Therefore, even if the raw material powder contains 70% or more of Cr and has a melting point of more than about 1700 ° C., it can be sintered at a temperature of about 1500 ° C. or less and burned with a density of about 94% or more of a completely dense body. You can get a unity.
【００１９】この焼結体をＨＩＰすることによって、気
孔は取り除かれ、ほぼ完全に緻密な構造に生成される。By subjecting this sintered body to HIP, the pores are removed and an almost completely dense structure is produced.
【００２０】[0020]
【実施例】Ｆｅ14％、Ｃｒ85％及びＹ2Ｏ3１％の合金粒
子からなる供試原料粉末Ａと、Ｆｅ４％、Ｃｒ95％及び
Ｙ2Ｏ3１％の合金粒子からなる供試原料粉末Ｂについ
て、Ｆｅ、Ｃｏ、Ｎｉ粉末の添加による焼結性向上効果
を調べた。EXAMPLES FE14%, and subjected trial original material powder A consisting of Cr85% and Y 2 O 3 1% of the alloy particles, Fe4%, consisting of Cr95% and Y 2 O 3 1% of the alloy particles subjected trial original material powder B The effect of improving the sinterability by adding Fe, Co, and Ni powders was investigated.
【００２１】原料粉末は、金属粉末とＹ2Ｏ3粉末をアト
ライター等の高エネルギーボールミルを用いることによ
り、十分にメカニカルアロイング処理を施したもので、
平均粒径10μm以下の酸化物分散強化合金粒子を得た。The raw material powder is a metal powder and a Y 2 O 3 powder which are sufficiently mechanically alloyed by using a high energy ball mill such as an attritor.
Oxide dispersion strengthened alloy particles having an average particle size of 10 μm or less were obtained.
【００２２】原料粉末に、Ｆｅ、Ｎｉ、Ｃｏの粉末少な
くとも１種を加えて略均一に混合する。添加粉末は、粒
子径サイズ約２μm以下の純Ｆｅ、純Ｎｉ、純Ｃｏ粉末
を用いた。At least one of Fe, Ni, and Co powders is added to the raw material powder and mixed substantially uniformly. As the additive powder, pure Fe, pure Ni, and pure Co powders having a particle diameter size of about 2 μm or less were used.
【００２３】混合の一例として、ポリプロピレン製広口
瓶に、酸化物分散強化耐熱合金粉末(例えば、500g)、及
びＦｅ、Ｎｉ、Ｃｏの粉末少なくとも１種を入れ、更に
大小２種類のＷＣボール(例えば、直径19.2mm、6.8mm)
を入れて密封した後、ボールミル(例えば、24時間)を行
なうことができる。As an example of mixing, an oxide dispersion strengthened heat-resistant alloy powder (for example, 500 g) and at least one of Fe, Ni, and Co powders are put into a polypropylene wide-mouthed bottle, and two kinds of WC balls (for example, large and small) (for example, , Diameter 19.2mm, 6.8mm)
After putting and sealing, a ball mill (for example, 24 hours) can be performed.
【００２４】或はまた、酸化物分散強化耐熱合金粉末
(例えば、1800g)と、Ｆｅ、Ｎｉ、Ｃｏの粉末少なくと
も１種とを、アトライター等の高エネルギーボールミル
によって混練(例えば、5時間)してもよい。なお、Ｃｒ
合金粉末(例えば、1800g)とＹ2Ｏ3(例えば、9g)の混合
粉末を、アトライター等の高エネルギーボールミルによ
って十分な時間(例えば65時間以上)混練してメカニカル
アロイング効果を得た後、同じボールミルの中にＦｅ、
Ｎｉ、Ｃｏの粉末少なくとも１種を投入して混練を行な
ってもよい。Alternatively, oxide dispersion strengthened heat resistant alloy powder
(For example, 1800 g) and at least one powder of Fe, Ni, and Co may be kneaded (for example, 5 hours) by a high energy ball mill such as an attritor. In addition, Cr
After a mixed powder of alloy powder (eg, 1800 g) and Y 2 O 3 (eg, 9 g) is kneaded with a high energy ball mill such as an attritor for a sufficient time (eg, 65 hours or more) to obtain a mechanical alloying effect. , Fe in the same ball mill,
Kneading may be performed by adding at least one of Ni and Co powders.
【００２５】供試原料粉末Ａ又はＢと、Ｆｅ、Ｎｉ、Ｃ
ｏの粉末少なくとも１種添加して混合した種々の実施例
を表１に示す。供試No.１〜No.５は供試原料粉末Ａと混
合したもので、供試No.６〜No.８は供試原料粉末Ｂと混
合したものである。なお、表１において、添加粉末の量
は、供試原料粉末を100重量部としたときの重量部を示
している。Raw material powder A or B and Fe, Ni, C
Table 1 shows various examples in which at least one powder of o was added and mixed. Sample Nos. 1 to 5 are mixed with the sample raw material powder A, and sample Nos. 6 to 8 are mixed with the sample raw material powder B. In addition, in Table 1, the amount of the added powder is parts by weight when the test raw material powder is 100 parts by weight.
【００２６】供試材No.１〜No.８を、夫々、ゴム筒に充
填し、冷間静水圧加圧(ＣＩＰ)に付し、加圧力1500kgf/
cm2、加圧時間１分の条件で成形し、グリーンコンパク
ト(直径30mm×長さ30mm)を作製した。Each of the test materials No. 1 to No. 8 was filled in a rubber cylinder and subjected to cold isostatic pressing (CIP) to apply a pressing force of 1500 kgf /
It was molded under the conditions of cm 2 and a pressing time of 1 minute to produce a green compact (diameter 30 mm × length 30 mm).
【００２７】次に、これらのグリーンコンパクトを、電
気炉のＡｒとＨ2の雰囲気ガス中にて、温度1500℃、加
熱時間４時間の条件で焼結した。焼結体の表面に付着し
た酸化被膜を除去した後、アルキメデス法に基づいて密
度測定を行なった。なお、供試原料粉末Ａ、Ｂとも、完
全緻密体の密度を7.2g/cm3とみなして、相対焼結密度を
算出した。算出結果は、表１中、「ＨＩＰ前」の欄に示
す。Next, these green compacts were sintered in an atmosphere gas of Ar and H 2 in an electric furnace under the conditions of a temperature of 1500 ° C. and a heating time of 4 hours. After removing the oxide film attached to the surface of the sintered body, the density was measured based on the Archimedes method. The relative sintered densities of both the sample raw material powders A and B were calculated assuming that the density of the completely dense body was 7.2 g / cm 3 . The calculation results are shown in the column "Before HIP" in Table 1.
【００２８】得られた各焼結体は、温度1250℃、加圧力
1200kgf/cm2、ＨＩＰ時間２時間の条件にてＨＩＰを行
なった。ＨＩＰ後、前記と同じ要領にて密度測定を行な
った。ＨＩＰ後の相対焼結密度の算出結果を表１に示
す。Each of the obtained sintered bodies had a temperature of 1250 ° C. and a pressing force.
HIP was performed under the conditions of 1200 kgf / cm 2 and HIP time of 2 hours. After HIP, the density was measured in the same manner as described above. Table 1 shows the calculation results of the relative sintered density after HIP.
【００２９】比較例として、供試材No.11〜No.15を作製
した。供試材No.11とNo.15は、Ｆｅ、Ｎｉ、Ｃｏ粉末の
いずれも含まない比較例、供試材No.12〜No.14は、Ｆ
ｅ、Ｎｉ、Ｃｏ粉末の添加量が本発明の規定量に達して
いない比較例である。これら比較例について、前記と同
じ要領にて、グリーンコンパクトを形成し、その後、焼
結及びＨＩＰを行ない、相対焼結密度を調べた。その結
果を表１に示す。As comparative examples, test materials No. 11 to No. 15 were produced. Specimens Nos. 11 and 15 are comparative examples containing no Fe, Ni, Co powders, and specimens Nos. 12 to 14 are F.
This is a comparative example in which the amounts of e, Ni, and Co powders added have not reached the prescribed amounts of the present invention. For these comparative examples, green compacts were formed in the same manner as described above, and thereafter, sintering and HIP were performed to examine the relative sintering density. The results are shown in Table 1.
【００３０】[0030]
【表１】 [Table 1]
【００３１】表１の結果から明らかなように、供試原料
粉末100重量部に対して、Ｆｅ、Ｎｉ、Ｃｏ粉末の少な
くとも１種を１〜５重量部添加混合した供試材(No.１〜
No.８)は、ＨＩＰ前の段階で、既に完全緻密体の93.8〜
95.5％の緻密焼結体が得られており、更にＨＩＰするこ
とによってほぼ完全に緻密な焼結品を得られることがわ
かる。As is clear from the results shown in Table 1, the test material (No. 1) was prepared by adding 1 to 5 parts by weight of at least one of Fe, Ni and Co powders to 100 parts by weight of the raw material powder to be tested. ~
No. 8) is a fully dense body of 93.8-
A dense sintered body of 95.5% was obtained, and it can be seen that a HIP is performed to obtain a sintered product that is almost completely dense.
【００３２】これに対し、供試材No.11及びNo.15は、Ｆ
ｅ、Ｎｉ、Ｃｏ粉末を添加していないため、ＨＩＰ前の
段階では、相対密度が約75％程度の焼結体しか得られて
いない。この供試材は更にＨＩＰを行なっても、密度向
上効果は殆んど認められない。また、供試材No.12〜No.
14は、Ｆｅ、Ｎｉ、Ｃｏ粉末の添加量が少ないため、約
80％程度の焼結体しか得られない。これらの焼結体に更
にＨＩＰを行なっても、密度向上効果は不十分である。On the other hand, the test materials No. 11 and No. 15 are F
Since e, Ni, and Co powders were not added, only a sintered body having a relative density of about 75% was obtained before the HIP. Even if HIP is further performed on this test material, the density improving effect is hardly recognized. In addition, the test materials No. 12 to No.
No. 14 has a small addition amount of Fe, Ni and Co powders,
Only 80% sintered body can be obtained. Even if HIP is performed on these sintered bodies, the effect of improving the density is insufficient.
【００３３】以上の結果から、酸化物分散強化耐熱合金
の原料粉末に、所定量のＦｅ、Ｎｉ、Ｃｏ粉末を少なく
とも１種混合することによって、焼結性が向上し、融点
よりもかなり低い温度で焼結を行なっても、少なくとも
約94％の相対密度を有する焼結体を得られることがわか
る。From the above results, it is possible to improve the sinterability by mixing at least one kind of Fe, Ni, and Co powders in a predetermined amount with the raw material powder of the oxide dispersion strengthened heat-resistant alloy, and to raise the temperature considerably below the melting point. It can be seen that a sintered body having a relative density of at least about 94% can be obtained even if the sintering is performed at.
【００３４】[0034]
【発明の効果】酸化物分散強化耐熱合金粉末のＨＩＰ焼
結を、カプセルを使用せずに行なうことができるから、
焼結すべき製品形状の自由度は大きい。従って、原料粉
末からほぼ任意形状の製品を成形してグリーンコンパク
トを作り、これを通常の焼結及びＨＩＰを行なうだけ
で、非常に緻密な焼結品を得ることができる。高融点の
酸化物分散強化耐熱合金粉末から複雑形状の焼結品を作
る場合でも、カプセルの製作、緻密な焼結体ブロック形
成後の機械加工等は不要となるから、その経済的効果は
極めて大きい。The HIP sintering of the oxide dispersion strengthened heat resistant alloy powder can be carried out without using a capsule.
There is a high degree of freedom in the shape of the product to be sintered. Therefore, a very compact sintered product can be obtained only by forming a green compact from a raw material powder into a green compact, and subjecting this to normal sintering and HIP. Even when making a complex shaped sintered product from a high melting point oxide-dispersion-strengthening heat-resistant alloy powder, the production of capsules and machining after forming a dense sintered body block are unnecessary, so the economic effect is extremely high. large.
フロントページの続き (72)発明者 北川 貴宏 兵庫県尼崎市浜１丁目１番１号 株式会社 クボタ技術開発研究所内 (72)発明者 西 隆 兵庫県尼崎市西向島町64番地 株式会社ク ボタ尼崎工場内Front page continuation (72) Inventor Takahiro Kitagawa 1-1-1 Hama, Amagasaki City, Hyogo Prefecture Kubota R & D Co., Ltd.
Claims (1)
以下のＹ2Ｏ3を0.2〜2.0重量％微細分散させた粒子から
なる原料粉末100重量部に対して、Ｆｅ粉末、Ｎｉ粉末
及びＣｏ粉末からなる群から選択された少なくとも１種
以上の粉末１〜５重量部(合計量)を混合する工程、得ら
れた混合物を所定形状のグリーンコンパクトに形成する
工程、該コンパクトを焼結する工程、及び、得られた焼
結体を熱間静水圧加圧する工程を有しており、前記金属
は、実質的にＣｒからなる金属、又はＦｅ20％以下を含
み、残部実質的にＣｒからなる金属、又はＡｌ、Ｍｏ、
Ｗ、Ｎｂ、Ｔａ、Ｈｆ及びＡｌ−Ｔｉから構成される群
の中から選択される少なくとも一種を合計量で10％以下
含み、残部実質的にＣｒからなる金属、又はＡｌ、Ｍ
ｏ、Ｗ、Ｎｂ、Ｔａ、Ｈｆ及びＡｌ−Ｔｉから構成され
る群の中から選択される少なくとも一種を合計量で10％
以下並びにＦｅ20％以下を含み、残部実質的にＣｒから
なる金属である、酸化物分散強化耐熱合金焼結体の製
法。1. An average particle size of 0.1 μm in a metal matrix.
At least one or more powders 1 selected from the group consisting of Fe powder, Ni powder and Co powder with respect to 100 parts by weight of raw material powder composed of particles in which 0.2 to 2.0% by weight of Y 2 O 3 is finely dispersed below 1 ~ 5 parts by weight (total amount), a step of forming the obtained mixture into a green compact having a predetermined shape, a step of sintering the compact, and hot isostatic pressing of the obtained sintered body. And a metal comprising substantially Cr, or a metal containing 20% or less of Fe, and a balance comprising substantially Cr, or Al, Mo,
W, Nb, Ta, Hf, and Al-Ti containing at least one selected from the group consisting of Al-Ti in a total amount of 10% or less, and the balance being substantially Cr.
10% in total of at least one selected from the group consisting of o, W, Nb, Ta, Hf and Al-Ti.
A method for producing an oxide dispersion strengthened heat-resistant alloy sintered body, which is a metal containing the following and Fe 20% or less and the balance being substantially Cr.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4193551A JP2898475B2 (en) | 1992-07-21 | 1992-07-21 | Manufacturing method of oxide dispersion strengthened heat-resistant alloy sintered body |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4193551A JP2898475B2 (en) | 1992-07-21 | 1992-07-21 | Manufacturing method of oxide dispersion strengthened heat-resistant alloy sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0633166A true JPH0633166A (en) | 1994-02-08 |
| JP2898475B2 JP2898475B2 (en) | 1999-06-02 |
Family
ID=16309938
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4193551A Expired - Lifetime JP2898475B2 (en) | 1992-07-21 | 1992-07-21 | Manufacturing method of oxide dispersion strengthened heat-resistant alloy sintered body |
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| Country | Link |
|---|---|
| JP (1) | JP2898475B2 (en) |
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1992
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103422001A (en) * | 2012-05-14 | 2013-12-04 | 东睦新材料集团股份有限公司 | Chromium-based alloy material and production method thereof |
| CN103422000A (en) * | 2012-05-14 | 2013-12-04 | 东睦新材料集团股份有限公司 | Chromium-based alloy material and production method thereof |
| CN103422002A (en) * | 2012-05-14 | 2013-12-04 | 东睦新材料集团股份有限公司 | Chromium-based alloy material and manufacturing method thereof |
| CN104419856A (en) * | 2013-08-20 | 2015-03-18 | 东睦新材料集团股份有限公司 | Chromium-based alloy and manufacturing method thereof |
| CN104419855A (en) * | 2013-08-20 | 2015-03-18 | 东睦新材料集团股份有限公司 | Chromium-based alloy and manufacturing method thereof |
| CN104419857A (en) * | 2013-08-20 | 2015-03-18 | 东睦新材料集团股份有限公司 | Chromium-based alloy and preparation method thereof |
| CN104419858A (en) * | 2013-08-20 | 2015-03-18 | 东睦新材料集团股份有限公司 | Chromium-based alloy and preparation method thereof |
| JP2016532783A (en) * | 2013-09-02 | 2016-10-20 | プランゼー エスエー | Powder metallurgy parts |
| US10211465B2 (en) | 2013-09-02 | 2019-02-19 | Plansee Se | Powdered metal component |
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| Publication number | Publication date |
|---|---|
| JP2898475B2 (en) | 1999-06-02 |
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