【０００１】[0001]
【産業上の利用分野】この発明は、刃物、あるいは、ギ
ア、シャフトなどの耐磨耗性を必要とする部品に適用出
来る合金系焼結体の製法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an alloy-based sintered body which can be applied to blades, gears, shafts and other parts requiring wear resistance.
【０００２】[0002]
【従来の技術】従来、このような用途には、セラミック
材料あるいは合金材料が用いられていた。 セラミック材料の使用 原料用セラミック粉末と有機バインダーとを混合し、射
出成形あるいは直圧成形により所定の形状に成形し、熱
処理でバインダーを飛ばした後、焼結させたセラミック
焼結品がある。このようにして製造された焼結品は、硬
度がＨｖ＝２０００以上と硬いが、靱性がないため、欠
けたり、割れたりし易いという欠点があった。2. Description of the Related Art Conventionally, ceramic materials or alloy materials have been used for such applications. Use of Ceramic Material There is a ceramic sintered product obtained by mixing raw material ceramic powder and an organic binder, molding the mixture into a predetermined shape by injection molding or direct pressure molding, removing the binder by heat treatment, and then sintering. The sintered product manufactured in this manner has a hardness as high as Hv = 2000 or more, but has a defect that it is easily chipped or cracked because it has no toughness.
【０００３】 合金材料を使用する場合、一方、超硬
材料として賞用される金属材料は、靱性は優れている反
面、表面硬度（Ｈｖ＝１１００程度）がセラミック焼結
品の表面硬度（Ｈｖ＝２０００以上）と比べ相当に低
く、耐磨耗性が十分とは言い難い。そこで、金属の表面
に耐磨耗性を有する皮膜を形成し複合化によって、耐磨
耗性を向上させる試みもなされている。具体的に言う
と、例えばスパッタ法やＣＶＤ法などの方法で、金属表
面にＴｉＮやＺｒＮ等の膜を形成するのである。この場
合、金属の表面に形成された皮膜と金属の間には、異質
材料を複合化した場合に固有的に形成される境界面が存
在するために相互の密着強度が小さいという問題や、皮
膜の厚みを十分に厚くすることが現実的に難しく膜厚に
制限が加わるため十分な耐磨耗性を確保することができ
ないという問題がある。In the case of using an alloy material, on the other hand, a metal material that is awarded as a super hard material has excellent toughness, but has a surface hardness (Hv = 1100) of that of a ceramic sintered product. It is considerably lower than that of 2000 or more), and it cannot be said that the abrasion resistance is sufficient. Therefore, attempts have been made to improve wear resistance by forming a film having wear resistance on the surface of metal to form a composite film. Specifically, a film of TiN, ZrN or the like is formed on the metal surface by a method such as a sputtering method or a CVD method. In this case, between the film formed on the surface of the metal and the metal, there is a boundary surface that is uniquely formed when a heterogeneous material is compounded, so that the mutual adhesion strength is small, It is practically difficult to make the thickness sufficiently thick and the thickness is limited, so that there is a problem that sufficient abrasion resistance cannot be secured.
【０００４】[0004]
【発明が解決しようとする課題】この発明は、上記の事
情に鑑み、表面硬度が大きく、耐磨耗性に優れ、しか
も、欠けや割れが生じ難い合金系焼結体を得ることがで
きるとともに量産化適性を有する方法を提供することを
課題とする。In view of the above circumstances, the present invention makes it possible to obtain an alloy-based sintered body having a large surface hardness, excellent wear resistance, and less likely to be chipped or cracked. It is an object to provide a method having suitability for mass production.
【０００５】[0005]
【課題を解決するための手段】前記課題を解決するた
め、この発明の合金系焼結体の製法では、Ａｌを含むフ
ェライト合金粉末を所定の形状に成型した成形体を非酸
化性雰囲気中で焼結し、酸化性ガス雰囲気中で熱処理す
ることにより表面にアルミナ成分を析出させるようにす
る。In order to solve the above-mentioned problems, in the method for producing an alloy-based sintered body of the present invention, a molded body obtained by molding a ferrite alloy powder containing Al into a predetermined shape is placed in a non-oxidizing atmosphere. The alumina component is deposited on the surface by sintering and heat treatment in an oxidizing gas atmosphere.
【０００６】非酸化性雰囲気としては、請求項２の如き
不活性ガス雰囲気、あるいは、請求項３の如き還元性ガ
ス雰囲気、さらには、請求項４の如き真空雰囲気が挙げ
られる。非酸化性雰囲気での焼結の際の熱処理温度は、
請求項４のように、１３００〜１４００℃の温度範囲が
好ましい。勿論、焼結の際の熱処理温度は、この範囲に
限らないが、１３００〜１４００℃の温度範囲を外れる
と適用できる成形圧力範囲が狭くなったりする等の制限
を受ける不都合がある。Examples of the non-oxidizing atmosphere include an inert gas atmosphere as defined in claim 2, a reducing gas atmosphere as defined in claim 3, and a vacuum atmosphere as defined in claim 4. The temperature of heat treatment during sintering in a non-oxidizing atmosphere is
As in claim 4, a temperature range of 1300 to 1400 ° C is preferable. Of course, the heat treatment temperature at the time of sintering is not limited to this range, but if it deviates from the temperature range of 1300 to 1400 ° C., there is a disadvantage that the applicable molding pressure range is narrowed.
【０００７】Ａｌを含むフェライト合金としては、Ｆｅ
−Ｃｒ−Ａｌ系合金やＦｅ−Ｃｒ−Ｎｉ−Ａｌ系合金等
がある。これらの合金の母材の硬度は、その合金を構成
する金属元素の種類や含有量の多少によりＨｖ＝２００
以下であったり、Ｈｖ＝３００以上であったり、その値
は異なる。Ｆｅ−Ｃｒ−Ａｌ系合金は概して靱性を満た
しても、硬度がＨｖ＝２００以下であるので、硬度が要
求される用途（例えば、ギアやシャフトの如き機構部
品）には適していない。As a ferrite alloy containing Al, Fe
There are -Cr-Al-based alloys, Fe-Cr-Ni-Al-based alloys, and the like. The hardness of the base material of these alloys is Hv = 200 depending on the kind and content of the metal elements constituting the alloy.
It is less than or equal to or more than Hv = 300, and its value is different. Even if the Fe-Cr-Al-based alloy generally satisfies the toughness, the hardness is Hv = 200 or less, and therefore it is not suitable for applications requiring hardness (for example, mechanical parts such as gears and shafts).
【０００８】したがって、用途に応じてＡｌを含むフェ
ライト合金の種類は選択される。Ｈｖ＝３００以上の硬
度が要求される用途にはＦｅ−Ｃｒ−Ｎｉ−Ａｌ系合金
が適し、特に、その組成がＣｒ：２０〜３５重量％：Ｎ
ｉ：２〜２５重量％、Ａｌ：２〜８重量％、Ｔｉ：０．
５重量％以下、Ｚｒ、Ｙ、Ｈｆ、Ｃｅ、Ｌａ、Ｎｄおよ
びＧｄのうちのいずれか１種又は２種以上：０．０５〜
１．０重量％、Ｆｅ：残部からなるＦｅ−Ｃｒ−Ｎｉ−
Ａｌ系フェライト合金が最適である。刃物、あるいは、
ギア、シャフトなどの耐磨耗性を必要とする機械部品用
として適した焼結品が得やすい。もちろん、この発明の
Ａｌを含むフェライト合金は、このＦｅ−Ｃｒ−Ｎｉ−
Ａｌ系フェライト合金に限定されるものではない。Therefore, the type of the ferrite alloy containing Al is selected according to the application. The Fe-Cr-Ni-Al alloy is suitable for applications requiring a hardness of Hv = 300 or more, and in particular, its composition is Cr: 20 to 35% by weight: N.
i: 2 to 25% by weight, Al: 2 to 8% by weight, Ti: 0.
5% by weight or less, any one or more of Zr, Y, Hf, Ce, La, Nd and Gd: 0.05 to
1.0% by weight, Fe: Fe-Cr-Ni- with the balance
Al-based ferrite alloy is most suitable. Cutlery, or
It is easy to obtain a sintered product suitable for mechanical parts such as gears and shafts that require abrasion resistance. As a matter of course, the ferrite alloy containing Al of the present invention is the Fe--Cr--Ni--
It is not limited to the Al-based ferrite alloy.
【０００９】以下、この発明を、より具体的に説明す
る。まず、例えば、Ｃｒ：２０〜３５重量％：Ｎｉ：２
〜２５重量％、Ａｌ：２〜８重量％、Ｔｉ：０．５重量
％以下、Ｚｒ、Ｙ、Ｈｆ、Ｃｅ、Ｌａ、ＮｄおよびＧｄ
のうちのいずれか１種又は２種以上：０．０５〜１．０
重量％、残部が実質的にＦｅという配合割合で全成分を
溶解し、例えば、アトマイズ法により微粉化したり、機
械的粉砕法で合金を微粉化したりすることで、Ａｌを含
むフェライト合金粉末を得る。The present invention will be described in more detail below. First, for example, Cr: 20 to 35% by weight: Ni: 2
-25 wt%, Al: 2-8 wt%, Ti: 0.5 wt% or less, Zr, Y, Hf, Ce, La, Nd and Gd.
Any one or two or more of the above: 0.05 to 1.0
A ferrite alloy powder containing Al is obtained by dissolving all components in a blending ratio of wt% and the balance being substantially Fe, for example, by atomizing by an atomizing method or atomizing an alloy by a mechanical grinding method. ..
【００１０】このようにして得たＡｌを含むフェライト
合金粉末を有機のバインダーと混合し、射出成形あるい
は直圧成形などの方法で金型によって所定形状に成型
（賦形）して成形体とする。この成形体は用途に応じた
製品、部品の形状に賦形された物であり、次工程で研削
の如き加工が施されるインゴットの如き母材とは異なる
ものである。有機のバインダーの一例を示しておくと、
ポリビニルアルコール（ＰＶＡ）、エチレングリコール
等の有機化合物が挙げられる。The ferrite alloy powder containing Al thus obtained is mixed with an organic binder and molded (shaped) into a predetermined shape by a mold by a method such as injection molding or direct pressure molding to obtain a molded body. .. This molded product is a product or product shaped according to the purpose of use, and is different from a base material such as an ingot which is subjected to processing such as grinding in the next step. To give an example of an organic binder,
Organic compounds such as polyvinyl alcohol (PVA) and ethylene glycol may be mentioned.
【００１１】成型時の圧力は、この発明の場合、４００
ＭＰａ程度の低い圧力の適用もあり、通常、４００〜１
０００ＭＰａ程度、あるいは、４５０〜６００ＭＰａ程
度の範囲から選ばれる。ただ、成型時の圧力が４００Ｍ
Ｐａ未満だと寸法精度等が出難い等の傾向がみられる。
つぎに、この成形体を、非酸化性雰囲気において熱処理
することにより焼結させる。熱処理は、１２５０〜１４
００℃（好ましくは１３００〜１４００℃）で行う。こ
の熱処理温度範囲であれば、液相を生じることなく十分
な硬度（Ｈｖ＝３００程度）や抗張力１００ｋｇ／ｍｍ
以上とすることができ、機構部品としても十分な強度の
母材たりえるものが得られる。The pressure during molding is 400 in the case of the present invention.
There is also the application of a low pressure of about MPa, usually 400 to 1
It is selected from the range of about 000 MPa or about 450 to 600 MPa. However, the molding pressure is 400M
If it is less than Pa, it tends to be difficult to obtain dimensional accuracy.
Next, this compact is sintered by heat treatment in a non-oxidizing atmosphere. Heat treatment is 1250-14
It is carried out at 00 ° C (preferably 1300 to 1400 ° C). Within this heat treatment temperature range, sufficient hardness (Hv = about 300) and tensile strength of 100 kg / mm without forming a liquid phase
The above can be obtained, and a base material having sufficient strength can be obtained as a mechanical part.
【００１２】非酸化性雰囲気で熱処理を行う理由は、酸
化が生じると焼結が進まず合金としての靱性を確保する
ことができないからである。不活性ガス雰囲気の場合、
例えば、アルゴン、ヘリウムなどの不活性ガスが用いら
れる。還元性ガス雰囲気の場合、例えば、水素ガスなど
が用いられる。このようにして得られた焼結体は、母材
がセラミックとは異なり、フェライト合金粉末の焼結体
であるから、アルミナ析出前では、割れや欠けを生ずる
ことなく、研削、研磨などの機械加工あるいは放電加工
が容易に出来るという利点がある。したがって、要すれ
ばアルミナ析出前に機械加工や放電加工を施すことがで
きる。The reason why the heat treatment is performed in a non-oxidizing atmosphere is that if oxidation occurs, the sintering does not proceed and the toughness as an alloy cannot be secured. In the case of an inert gas atmosphere,
For example, an inert gas such as argon or helium is used. In the case of a reducing gas atmosphere, for example, hydrogen gas is used. Since the base material of the sintered body thus obtained is a sintered body of ferrite alloy powder, which is different from ceramics, it does not cause cracks or chips before precipitation of alumina, and is used for mechanical processing such as grinding and polishing. There is an advantage that machining or electric discharge machining can be easily performed. Therefore, if necessary, machining or electric discharge machining can be performed before alumina precipitation.
【００１３】従来のセラミック材料の場合、焼結に伴う
２０％前後の収縮のため、寸法精度が出難くいのである
が、加工は困難であるため、後加工で寸法精度を上げる
ことが難しい。超硬材料の場合も、切削、研削などの後
加工が容易ではなく、やはり寸法精度が出難い。いずれ
の場合も、精度を要求されるところに用いるには適して
いないのである。In the case of the conventional ceramic material, it is difficult to obtain the dimensional accuracy due to the shrinkage of about 20% due to the sintering, but it is difficult to process it, and it is difficult to improve the dimensional accuracy in the post-processing. Even in the case of super hard materials, post-processing such as cutting and grinding is not easy, and dimensional accuracy is difficult to obtain. In either case, it is not suitable for use where precision is required.
【００１４】しかし、この発明の場合、上のように、ア
ルミナ析出前では、割れや欠けを生ずることなく、研
削、研磨などの機械加工あるいは放電加工で寸法精度を
上げることができる。そのため、この発明は、寸法精度
を要求されるところにも十分に適用できる。次に、この
焼結体を、例えば、大気又は酸素ガス等の酸化性ガス雰
囲気中において、例えば、１０００℃を超す温度で熱処
理を行い、表面にアルミナ（酸化アルミニウム）成分を
析出させる。この熱処理で、例えば、アルミナを主成分
とする表面層（アルミナ皮膜）付のＦｅ−Ｃｒ−Ｎｉ−
Ａｌ合金系焼結品が出来上がる。However, in the case of the present invention, as described above, the dimensional accuracy can be improved by machining such as grinding and polishing or electric discharge machining without causing cracks or chips before the precipitation of alumina. Therefore, the present invention can be sufficiently applied to a place where dimensional accuracy is required. Next, this sintered body is heat-treated at a temperature higher than 1000 ° C., for example, in the atmosphere or an oxidizing gas atmosphere such as oxygen gas to deposit an alumina (aluminum oxide) component on the surface. By this heat treatment, for example, Fe-Cr-Ni- with a surface layer (alumina film) containing alumina as a main component is attached.
Al alloy type sintered product is completed.
【００１５】ここで、焼結体を構成する合金の表面に析
出される成分をアルミナに限定するのは、酸化性ガス雰
囲気中で熱処理すると、容易にＡｌ元素が酸化され硬度
の高いアルミナからなるセラミックを生成することがで
きるからである。このようにして得られた合金系焼結体
は、アルミナを主成分とする表面層を有するため表面硬
度は大きくなり、かつ焼結体の内部を充たす母材が合金
であるため靱性に優れる。その上、金属表面にスパッタ
法やＣＶＤ法などによりセラミックの皮膜を形成した場
合には、皮膜と金属の母材とに境界面が形成されるので
皮膜と母材との密着強度が小さく、更に皮膜層の膜厚が
制限されるため充分な耐磨耗性が得られないのに対し、
この発明によるアルミナを主成分とする表面層は母材中
にアルミナの根が張っているため母材との密着強度が大
きく、しかも、この表面層の厚さは１０〜５０μｍに高
めることも出来る。さらには、成型、焼結の工程により
目的とする形状に賦形し、効率の悪い切削などの加工を
要さずに製造することが可能であり、この場合には、工
業的生産に要求される経済性、大量生産効果も顕著であ
ると言える。つまり、量産適性があるのである。Here, the reason why the component deposited on the surface of the alloy forming the sintered body is limited to alumina is that the aluminum element is easily oxidized when heat-treated in an oxidizing gas atmosphere and is made of alumina having high hardness. This is because ceramic can be produced. The alloy-based sintered body thus obtained has a large surface hardness because it has a surface layer containing alumina as a main component, and is excellent in toughness because the base material that fills the inside of the sintered body is an alloy. In addition, when a ceramic coating is formed on the metal surface by a sputtering method or a CVD method, since a boundary surface is formed between the coating and the metal base material, the adhesion strength between the coating and the base material is small. In contrast to the fact that sufficient abrasion resistance cannot be obtained because the film thickness of the coating layer is limited,
The surface layer containing alumina as a main component according to the present invention has high adhesion strength to the base material because the root of the alumina is stretched in the base material, and the thickness of the surface layer can be increased to 10 to 50 μm. .. Furthermore, it is possible to shape it into the desired shape through the steps of molding and sintering, and to manufacture it without the need for machining such as inefficient cutting. In this case, it is required for industrial production. It can be said that the economy and the effect of mass production are remarkable. In other words, it is suitable for mass production.
【００１６】この発明の方法が適用できる物品として
は、以下のようなものが挙げられる。 〔家庭用に使われる刃物〕電気カミソリの刃、バリカン
（特に小石などの噛み込みの可能性のあるペット用バリ
カンや庭園用の庭木バリカン）の刃、草刈機や料理用ミ
キサー、カッターなどの刃、小刀、ハサミ、日曜大工用
ノコギリ刃など。Articles to which the method of the present invention can be applied include the following. [Cutters used for home] Blades of electric razors, hair clippers (especially pet hair clippers and garden tree hair clippers that can bite small stones, etc.), blades of mowers, cooking mixers, cutters, etc. , Knives, scissors, saw blade for DIY carpenters, etc.
【００１７】〔業務用に使われる刃物〕各種帯ノコ刃、
回転刃、バイト、ダイスなどの工具類、混練機のスクリ
ューなど。 〔耐磨耗性部品〕電動ドリルの刃、ドリルチャック部
品、ギア、回転軸、軸受けなど。[Blade used for business] Various band saw blades,
Tools such as rotary blades, cutting tools and dies, screws for kneading machines, etc. [Abrasion resistant parts] Electric drill blades, drill chuck parts, gears, rotary shafts, bearings, etc.
【００１８】[0018]
【作用】この発明の製法で得られた合金系焼結体におい
ては、表面層を形成するアルミナ成分が内部を充たす合
金の中に根を張って形成されるため表面層と合金との密
着力を大きくする作用をし、表面にアルミナが析出する
ことは表面硬度を高くする作用をし、また焼結体の内部
を充たす合金は焼結体の靱性を高くする作用をする。In the alloy-based sintered body obtained by the manufacturing method of the present invention, the alumina component forming the surface layer is formed by rooting in the alloy filling the interior, so that the adhesion between the surface layer and the alloy is high. And the precipitation of alumina on the surface has the effect of increasing the surface hardness, and the alloy filling the interior of the sintered body has the effect of increasing the toughness of the sintered body.
【００１９】そして、目的とする形状に成型、焼結工程
によることは、工業的生産に要求される経済性、大量生
産性を向上させるため、量産適性が出てくる。また、焼
結後であってアルミナ析出前の合金焼結体には、欠けや
割れなどを生じずに所定形状に正確に見合うように加工
が施せるため、寸法精度の向上を図ることができるた
め、精度を要求される場合にも適用可能である。[0019] Further, the step of molding and sintering into a desired shape improves the economical efficiency and the mass productivity required for industrial production, and therefore suitability for mass production comes out. Further, since the alloy sintered body after sintering but before alumina precipitation can be processed so as to accurately match a predetermined shape without causing chips or cracks, it is possible to improve dimensional accuracy. It is also applicable when accuracy is required.
【００２０】[0020]
【実施例】以下、この発明の実施例を説明する。この発
明は、下記の実施例に限らない。 −実施例１− Ｃｒ：２４重量％、Ｎｉ：４重量％、Ａｌ：３．５重量
％、Ｚｒ：０．０５重量％、残部：Ｆｅの組成の合金を
高周波溶解炉で溶解した。出来たインゴットを１〜２ｍ
ｍの厚みに圧延し、得られた板を２〜３ｍｍ角のチップ
状に切断した後、粉砕し５０メッシュ以下のフェライト
合金粉末にした。Embodiments of the present invention will be described below. The present invention is not limited to the following embodiments. -Example 1-Cr: 24% by weight, Ni: 4% by weight, Al: 3.5% by weight, Zr: 0.05% by weight, and the balance: Fe were alloyed in a high frequency melting furnace. 1 to 2 m of the finished ingot
After rolling to a thickness of m, the obtained plate was cut into chips of 2 to 3 mm square, and then pulverized to obtain a ferrite alloy powder of 50 mesh or less.
【００２１】この粉末にバインダーとしてＰＶＡを混合
しスラリー状にした後、周りに突条を平行に並べたギア
を成型するキャビティにこれを充填し直圧成型で焼結前
のギアを成型した。成形体であるこの生のギアをアルゴ
ンガス雰囲気中で１２５０℃、５時間の焼結をし、焼結
体を得た。次に大気中で１１５０℃、１０時間の加熱を
して、表面にアルミナを析出させた結果、表面が灰色を
した目的物であるギアを得た。PVA was mixed with this powder as a binder to form a slurry, which was then filled in a cavity for molding a gear around which ridges are arranged in parallel, and the gear before sintering was molded by direct pressure molding. This raw gear, which is a compact, was sintered in an argon gas atmosphere at 1250 ° C. for 5 hours to obtain a sintered compact. Next, heating was performed at 1150 ° C. for 10 hours in the atmosphere to deposit alumina on the surface, and as a result, a target gear having a gray surface was obtained.
【００２２】表１に、このアルミナを析出させた焼結体
の表面硬度および内部の合金の硬度（母材硬度として示
す）並びに表面のアルミナ成分の含有率を示す。なお、
電子顕微鏡で表面層の断面を観察したところ、アルミナ
は表面から内部に進行するにしたがって針条の突起が内
部の合金に突き刺さったような状態であることを確認し
た。Table 1 shows the surface hardness of the alumina-precipitated sintered body, the hardness of the internal alloy (shown as the base metal hardness), and the content of the alumina component on the surface. In addition,
When the cross section of the surface layer was observed with an electron microscope, it was confirmed that the alumina had a state in which the protrusions of the needle streak penetrated the alloy inside as it progressed inward from the surface.
【００２３】−実施例２− Ｃｒ：３０重量％、Ｎｉ：２１重量％、Ａｌ：６重量
％、Ｔｉ：０．５重量％、Ｚｒ：０．２重量％、残部：
Ｆｅの組成の合金を高周波溶解炉で溶解し、出来たイン
ゴットをアトマイズ法によりフェライト合金粉末にした
後、実施例１と同じ方法で成型、焼結、熱処理を行っ
た。-Example 2-Cr: 30% by weight, Ni: 21% by weight, Al: 6% by weight, Ti: 0.5% by weight, Zr: 0.2% by weight, balance:
An alloy having a composition of Fe was melted in a high-frequency melting furnace, the resulting ingot was made into a ferrite alloy powder by an atomizing method, and then molding, sintering and heat treatment were performed in the same manner as in Example 1.
【００２４】表１に得られた焼結体の表面硬度および合
金の硬度（母材硬度として示す）並びに表面のアルミナ
成分の含有率を示す。なお、電子顕微鏡で表面層の断面
を観察したところ、アルミナは表面から内部に進行する
にしたがって針状の突起が内部の合金に突き刺さったよ
うな状態であることを確認した。 −実施例３− Ｃｒ：２６重量％、Ｎｉ：２１重量％、Ａｌ：６．５重
量％、Ｚｒ：０．２重量％、残部：Ｆｅの組成の合金を
高周波溶解炉で溶解し、出来たインゴットをアトマイズ
法によりフェライト合金粉末にした後、実施例１と同じ
方法で焼結前のギアを成型した。成形体であるこの生の
ギアを水素ガス雰囲気中で１３５０℃、５時間の焼結を
し、焼結体を得た。次に大気中で１１５０℃、１０時間
の加熱をして、表面にアルミナを析出させた結果、表面
が灰色をした目的物であるギアを得た。Table 1 shows the surface hardness of the obtained sintered body, the hardness of the alloy (shown as the base metal hardness), and the content of the alumina component on the surface. When the cross section of the surface layer was observed with an electron microscope, it was confirmed that the needle-like protrusions penetrated the alloy inside as the alumina progressed inward from the surface. -Example 3-Cr: 26% by weight, Ni: 21% by weight, Al: 6.5% by weight, Zr: 0.2% by weight, balance: Fe was prepared by melting in an induction melting furnace. After the ingot was made into a ferrite alloy powder by an atomizing method, a gear before sintering was molded by the same method as in Example 1. The green gear, which is a compact, was sintered in a hydrogen gas atmosphere at 1350 ° C. for 5 hours to obtain a sintered compact. Next, heating was performed at 1150 ° C. for 10 hours in the atmosphere to deposit alumina on the surface, and as a result, a target gear having a gray surface was obtained.
【００２５】表１に、このアルミナを析出させた焼結体
の表面硬度および内部の合金の硬度（母材硬度として示
す）並びに表面のアルミナ成分の含有率を示す。なお、
電子顕微鏡で表面層の断面を観察したところ、アルミナ
は表面から内部に進行するにしたがって針条の突起が内
部の合金に突き刺さったような状態であることを確認し
た。Table 1 shows the surface hardness of the alumina-precipitated sintered body, the hardness of the internal alloy (shown as the base metal hardness), and the content of the alumina component on the surface. In addition,
When the cross section of the surface layer was observed with an electron microscope, it was confirmed that the alumina had a state in which the protrusions of the needle streak penetrated the alloy inside as it progressed inward from the surface.
【００２６】−参考例１、２− 超硬金属材料であるＳＫＨ５とセラミック材料であるア
ルミナについての硬度（この場合は表面硬度と母材硬度
は等しい）を表１にそれぞれ参考例１、２として併記す
る。Reference Examples 1 and 2 The hardness (in this case, the surface hardness and the base material hardness) of SKH5, which is a superhard metal material, and alumina, which is a ceramic material, are shown in Table 1 as Reference Examples 1 and 2, respectively. Write together.
【００２７】[0027]
【表１】[Table 1]
【００２８】−実施例４− Ｃｒ：３２重量％、Ｎｉ：２１重量％、Ａｌ：６．５重
量％、Ｚｒ：０．８重量％、残部：Ｆｅという割合で溶
解し、アトマイズ法により微粉化しＦｅ−Ｃｒ−Ｎｉ−
Ａｌ系フェライト合金粉末を得た。このようにして得た
合金粉末とバインダー用のＰＶＡとを混ぜ合わせ、４５
０ＭＰａの圧力で成型した。ついで、成形体を真空中に
おいて、１３５０℃、３時間の熱処理をすることにより
焼結させた後、研削加工し所定の形状に正確に合わせ
た。次に、大気中において、１１５０℃、２０時間の熱
処理および１２５０℃、３０分の熱処理を施しアルミナ
皮膜の形成を行い、空冷してＦｅ−Ｃｒ−Ｎｉ−Ａｌ系
焼結品（合金系焼結体）を得た。-Example 4-Cr: 32% by weight, Ni: 21% by weight, Al: 6.5% by weight, Zr: 0.8% by weight, the balance: Fe, dissolved in the following proportions and atomized by atomization. Fe-Cr-Ni-
An Al-based ferrite alloy powder was obtained. The alloy powder thus obtained and PVA for the binder are mixed, and 45
It was molded at a pressure of 0 MPa. Then, the molded body was sintered by being heat-treated at 1350 ° C. for 3 hours in a vacuum, and then ground and precisely adjusted to a predetermined shape. Next, in an atmosphere, heat treatment is performed at 1150 ° C. for 20 hours and heat treatment at 1250 ° C. for 30 minutes to form an alumina film, which is air-cooled and then Fe—Cr—Ni—Al-based sintered product (alloy-based sintering Got the body).
【００２９】−実施例５− 成形圧力が６００ＭＰａである他は、実施例４と同様に
して、Ｆｅ−Ｃｒ−Ｎｉ−Ａｌ系焼結品を得た。 −実施例６− Ｃｒ：２４重量％、Ｎｉ：４重量％、Ａｌ：３．５重量
％、Ｚｒ：０．０５重量％、残部が実質的にＦｅという
割合で高周波溶解炉で溶解するようにして、合金インゴ
ットを得た。このインゴットを１〜２ｍｍの厚みまで圧
延し、この板を２〜３ｍｍ角のチップ状に細断した後、
機械的に粉砕し、５０メッシュ以下のＦｅ−Ｃｒ−Ｎｉ
−Ａｌ系フェライト合金粉末を得た。Example 5-A Fe-Cr-Ni-Al-based sintered product was obtained in the same manner as in Example 4 except that the molding pressure was 600 MPa. -Example 6-Cr: 24% by weight, Ni: 4% by weight, Al: 3.5% by weight, Zr: 0.05% by weight, the balance being substantially Fe so that the components are melted in a high frequency melting furnace. As a result, an alloy ingot was obtained. After rolling this ingot to a thickness of 1 to 2 mm and cutting this plate into chips of 2 to 3 mm square,
Mechanically crushed and Fe-Cr-Ni with 50 mesh or less
-Al type ferrite alloy powder was obtained.
【００３０】このようにして得た合金粉末とバインダー
用のＰＶＡとを混ぜ合わせ、１０００ＭＰａの範囲の適
当な圧力で成形した。ついで、成形体をアルゴンガス雰
囲気において、１３００℃、５時間の熱処理をすること
により焼結させた後、研削加工し所定の形状に正確に合
わせた。次に、大気中において、１１５０℃、２０時間
の熱処理および１２５０℃、３０分の熱処理を施しアル
ミナ皮膜の形成を行い、空冷してＦｅ−Ｃｒ−Ｎｉ−Ａ
ｌ系焼結品を得た。The alloy powder thus obtained and PVA for a binder were mixed and molded at an appropriate pressure in the range of 1000 MPa. Then, the molded body was heat-treated at 1300 ° C. for 5 hours in an argon gas atmosphere to sinter it, followed by grinding to accurately match it with a predetermined shape. Next, in the atmosphere, heat treatment at 1150 ° C. for 20 hours and heat treatment at 1250 ° C. for 30 minutes are performed to form an alumina film, which is air-cooled and then Fe—Cr—Ni—A.
An l-based sintered product was obtained.
【００３１】−実施例７− Ｃｒ：３５重量％、Ｎｉ：２１重量％、Ａｌ：７重量
％、Ｚｒ：０．４重量％、残部が実質的にＦｅという割
合で高周波溶解炉で溶解し、アトマイズ法により微粉化
しＦｅ−Ｃｒ−Ｎｉ−Ａｌ系フェライト合金粉末を得
た。このようにして得た合金粉末とバインダー用のＰＶ
Ａとを混ぜ合わせ、７００ＭＰａの範囲の適当な圧力で
成形した。ついで、成形体を真空中において、１３５０
℃、４時間の熱処理をすることにより焼結させた後、研
削加工し所定の形状に合わせた。次に、大気中におい
て、１１５０℃、２０時間の熱処理および１２５０℃、
３０分の熱処理を施しアルミナ皮膜の形成を行い、空冷
してＦｅ−Ｃｒ−Ｎｉ−Ａｌ系焼結品を得た。Example 7-Cr: 35% by weight, Ni: 21% by weight, Al: 7% by weight, Zr: 0.4% by weight, the balance being substantially Fe, dissolved in a high frequency melting furnace, Fe-Cr-Ni-Al ferrite alloy powder was obtained by atomizing by atomization method. Alloy powder thus obtained and PV for binder
A was mixed and molded at an appropriate pressure in the range of 700 MPa. Then, the formed body is vacuumed at 1350.
After heat treatment at 4 ° C. for 4 hours to sinter, it was ground and adjusted to a predetermined shape. Next, in the atmosphere, heat treatment at 1150 ° C. for 20 hours and 1250 ° C.
A heat treatment was applied for 30 minutes to form an alumina film, which was air-cooled to obtain a Fe-Cr-Ni-Al-based sintered product.
【００３２】−実施例８− 成形圧力が９００ＭＰａであり、焼結のための熱処理温
度が１３００℃である他は、実施例７と同様にして、Ｆ
ｅ−Ｃｒ−Ｎｉ−Ａｌ系焼結品を得た。 −実施例９− 実施例４で使用した合金粉末を分級し、３０μｍ以下と
した合金粉末と、約１０重量％のパラフィンワックス、
ステアリン酸を主成分としたバインダーとを混練し、１
５０℃で所定の形状に射出成形した。得られた成形体
を、真空中、４００℃で５０時間保持して脱脂した。脱
脂した成形体を、真空中、１３５０℃に３時間保持して
焼結させた後、炉中に酸素ガスを送給て、１２５０℃で
３０分保持して、表面にアルミナ皮膜を析出させ、Ｆｅ
−Ｃｒ−Ｎｉ−Ａｌ系焼結品を得た。Example 8 F was prepared in the same manner as in Example 7 except that the molding pressure was 900 MPa and the heat treatment temperature for sintering was 1300 ° C.
An e-Cr-Ni-Al-based sintered product was obtained. -Example 9-The alloy powder used in Example 4 was classified to 30 μm or less, and about 10% by weight of paraffin wax,
Knead with a binder containing stearic acid as the main component, and
It was injection-molded into a predetermined shape at 50 ° C. The obtained molded body was held in vacuum at 400 ° C. for 50 hours to be degreased. The degreased molded body is held in vacuum at 1350 ° C. for 3 hours to be sintered, then oxygen gas is fed into the furnace and held at 1250 ° C. for 30 minutes to deposit an alumina film on the surface, Fe
A -Cr-Ni-Al-based sintered product was obtained.
【００３３】−実施例１０− 実施例９と同様にして得た射出成形体を、アルゴンガス
雰囲気中、５００℃で５０時間保持して脱脂した。脱脂
した成形体を、アルゴンガス雰囲気中、１３５０℃に３
時間保持して焼結させた後、炉内ガスを酸素ガスに置換
し、１２５０℃で３０分保持して、表面にアルミナ皮膜
を析出させ、Ｆｅ−Ｃｒ−Ｎｉ−Ａｌ系焼結品を得た。Example 10 An injection-molded article obtained in the same manner as in Example 9 was degreased by holding it at 500 ° C. for 50 hours in an argon gas atmosphere. The degreased molded body was heated to 1350 ° C. in an argon gas atmosphere for 3 hours.
After holding for a time to sinter, the gas in the furnace was replaced with oxygen gas, and the furnace was held at 1250 ° C. for 30 minutes to deposit an alumina film on the surface to obtain a Fe—Cr—Ni—Al-based sintered product. It was
【００３４】−実施例１１− 実施例７で使用した合金粉末を分級し、３０μｍ以下と
した合金粉末を用いた他は、実施例９と同様にして、Ｆ
ｅ−Ｃｒ−Ｎｉ−Ａｌ系焼結品を得た。実施例４〜１１
の焼結品のアルミナ皮膜状態、母材硬度および寸法精度
を調べた。調べた結果を、表２に示す。表２において、
寸法精度のデータ欄の○は５％未満の寸法誤差に収まっ
ていることを示す。-Example 11-F was prepared in the same manner as in Example 9 except that the alloy powder used in Example 7 was classified and the alloy powder having a particle size of 30 μm or less was used.
An e-Cr-Ni-Al-based sintered product was obtained. Examples 4-11
The state of the alumina coating, the hardness of the base metal and the dimensional accuracy of the sintered product were examined. The results of the examination are shown in Table 2. In Table 2,
A circle in the dimensional accuracy data column indicates that the error is within 5%.
【００３５】[0035]
【表２】[Table 2]
【００３６】表２の結果から、実施例４〜１１の焼結品
は、寸法精度がよくて表面硬度が大きく、丈夫であるこ
とがよく分かる。なお、図１は実施例４のアルミナ皮膜
付Ｆｅ−Ｃｒ−Ｎｉ−Ａｌ系焼結品の表面付近の金属組
織をあらわす光学顕微鏡写真（倍率７００倍）である。
図１の写真では、略下半を占める黒の斑点のある白地部
分が母材であり、その上方の黒地の層がアルミナ皮膜で
あり、さらにその上方の黒地層は保護Ｎｉ膜である。図
２は実施例４のアルミナ皮膜付Ｆｅ−Ｃｒ−Ｎｉ−Ａｌ
系焼結品の内部の金属組織をあらわす光学顕微鏡写真
（倍率７００倍）である。図３は、実施例４の焼結品の
表面付近の金属組織の大略を模式的にあらわしたもので
ある。そして、図１、２の母材部分では、図２にみるよ
うに、黒色部は空洞、灰色部はＮｉＡｌ相、白色部はフ
ェライト相である。また、図３は、母材３の表面にアル
ミナ皮膜２が形成され、アルミナ皮膜２の上には保護Ｎ
ｉ膜３のある構成を図示するものである。From the results shown in Table 2, it is clearly understood that the sintered products of Examples 4 to 11 have good dimensional accuracy, large surface hardness and are durable. Note that FIG. 1 is an optical microscope photograph (magnification 700 times) showing a metal structure near the surface of the alumina-coated Fe—Cr—Ni—Al-based sintered product of Example 4.
In the photograph of FIG. 1, a white background portion having black spots occupying substantially the lower half is a base material, a black background layer above the base material is an alumina film, and a black background layer above the black background layer is a protective Ni film. FIG. 2 shows the Fe-Cr-Ni-Al with alumina coating of Example 4.
It is an optical microscope photograph (magnification 700 times) showing the metallographic structure inside the system sintered product. FIG. 3 schematically shows the metal structure of the vicinity of the surface of the sintered product of Example 4. As shown in FIG. 2, in the base material portions of FIGS. 1 and 2, the black portion is a cavity, the gray portion is a NiAl phase, and the white portion is a ferrite phase. Further, in FIG. 3, the alumina film 2 is formed on the surface of the base material 3, and the protective film N is formed on the alumina film 2.
1 illustrates a configuration with an i-film 3.
【００３７】また、実施例４において、焼結のための処
理温度を１２００℃とした場合は、母材硬度が十分なも
のになり難い傾向がみられた。そして、実施例６におい
て、成形圧力を３５０ＭＰａとした他は全く同様にして
Ｆｅ−Ｃｒ−Ｎｉ−Ａｌ系焼結品を得たが、寸法精度
（誤差が５％を越える）、母材硬度およびアルミナ皮膜
状態は、いずれも実施例６よりもかなり劣る傾向がみら
れた。Further, in Example 4, when the processing temperature for sintering was 1200 ° C., there was a tendency that the base material hardness was difficult to be sufficient. Then, in Example 6, an Fe-Cr-Ni-Al-based sintered product was obtained in exactly the same manner except that the molding pressure was set to 350 MPa, but the dimensional accuracy (the error exceeds 5%), the base metal hardness and the The alumina coating state tended to be considerably inferior to that of Example 6.
【００３８】[0038]
【発明の効果】以上に述べたように、この発明は、表面
の硬度が高く、かつ欠けや割れが生じにくい耐磨耗性に
優れる有用な合金系焼結体を得ることができ、しかも、
量産適性があるため、非常に有用である。また、請求項
６に示す組成のＡｌを含むフェライト合金粉末を用いた
場合は、機構部品などのように表面硬度と母材硬度が共
に必要な用途に適する合金系焼結体が確実に得られると
いう利点がある。As described above, according to the present invention, it is possible to obtain a useful alloy-based sintered body having a high surface hardness and excellent abrasion resistance in which chipping and cracking are unlikely to occur, and
It is very useful because it is suitable for mass production. Further, when the ferrite alloy powder containing Al having the composition described in claim 6 is used, an alloy-based sintered body suitable for an application in which both surface hardness and base material hardness are required, such as mechanical parts, can be reliably obtained. There is an advantage that.
【図１】実施例４の焼結品の表面付近の金属組織をあら
わす光学顕微鏡写真（倍率７００倍）である。FIG. 1 is an optical micrograph (magnification: 700 times) showing a metal structure near the surface of a sintered product of Example 4.
【図２】実施例４の焼結品の内部の金属組織をあらわす
光学顕微鏡写真（倍率７００倍）である。FIG. 2 is an optical micrograph (magnification: 700 times) showing the metallographic structure inside the sintered product of Example 4.
【図３】実施例４の焼結品の表面付近の金属組織の概略
をあらわす説明図である。FIG. 3 is an explanatory diagram showing an outline of a metal structure near the surface of the sintered product of Example 4.
１ 保護Ｎｉ膜 ２ アルミナ皮膜 ３ 母材 1 Protective Ni film 2 Alumina film 3 Base material
───────────────────────────────────────────────────── フロントページの続き (72)発明者 児島 肇 大阪府門真市大字門真1048番地松下電工株 式会社内 (72)発明者 棚橋 正雄 大阪府門真市大字門真1048番地松下電工株 式会社内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hajime Kojima 1048, Kadoma, Kadoma City, Osaka Prefecture Matsushita Electric Works Co., Ltd. (72) Masao Tanahashi, 1048, Kadoma, Kadoma City, Osaka Matsushita Electric Works Co., Ltd.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3176221AJP2806511B2 (en) | 1990-07-31 | 1991-06-19 | Manufacturing method of sintered alloy |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20357890 | 1990-07-31 | ||
| JP2-414305 | 1990-12-25 | ||
| JP2-203578 | 1990-12-25 | ||
| JP41430590 | 1990-12-25 | ||
| JP3176221AJP2806511B2 (en) | 1990-07-31 | 1991-06-19 | Manufacturing method of sintered alloy |
| Publication Number | Publication Date |
|---|---|
| JPH055106Atrue JPH055106A (en) | 1993-01-14 |
| JP2806511B2 JP2806511B2 (en) | 1998-09-30 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3176221AExpired - Fee RelatedJP2806511B2 (en) | 1990-07-31 | 1991-06-19 | Manufacturing method of sintered alloy |
| Country | Link |
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| JP (1) | JP2806511B2 (en) |
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