JPH04272102A - Vessel for heat treating iron powder - Google Patents

Vessel for heat treating iron powder

Info

Publication number
JPH04272102A
JPH04272102A JP3034602A JP3460291A JPH04272102A JP H04272102 A JPH04272102 A JP H04272102A JP 3034602 A JP3034602 A JP 3034602A JP 3460291 A JP3460291 A JP 3460291A JP H04272102 A JPH04272102 A JP H04272102A
Authority
JP
Japan
Prior art keywords
iron powder
container
vessel
heat treatment
powder
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.)
Granted
Application number
JP3034602A
Other languages
Japanese (ja)
Other versions
JPH07116484B2 (en
Inventor
Hiroshi Yano
浩史 矢埜
Osamu Furukimi
修 古君
Shigeaki Takagi
高城 重彰
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.)
JFE Steel Corp
Original Assignee
Kawasaki Steel Corp
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 Kawasaki Steel Corp filed Critical Kawasaki Steel Corp
Priority to JP3034602A priority Critical patent/JPH07116484B2/en
Publication of JPH04272102A publication Critical patent/JPH04272102A/en
Publication of JPH07116484B2 publication Critical patent/JPH07116484B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Abstract

PURPOSE:To prevent the easy sticking of heat treated powder by using stainless steel in which an oxidized film is formed on the surface as a vessel for heat treating iron powder and concentrating elements such as Si within a specified thickness from the surface of the oxidized film. CONSTITUTION:A vessel 1 having a partition wall 2 for heat treating iron powder or alloy steel powder 3 is constituted by stainless steel in which an oxidized film 5 is formed on the surface and one or >= two kinds of elements of Si, Al Ti, Mn and Cr are concentrated within 10Angstrom from the surface of the oxidized film on the inside of the vessel. This vessel 1 is filled with iron powder or allay steel powder 3, is charged to the inside of a heat treating furnace and is subjected to heat treatment. In this way, the sticking of the heat treated powder to the vessel 1 can be prevented, its discharge from the vessel 1 is facilitated and the service life of the vessel can be increased.

Description

【発明の詳細な説明】[Detailed description of the invention]

【0001】0001

【産業上の利用分野】本発明は、容器内に鉄粉又は合金
粉を入れ、主に減圧炉を使って、還元、焼鈍などの熱処
理を施し、高品質な鉄粉などを製造する分野で用いる鉄
粉熱処理用容器に関するものである。
[Industrial Application Field] The present invention is applied to the field of manufacturing high-quality iron powder by placing iron powder or alloy powder in a container and subjecting it to heat treatment such as reduction and annealing, mainly using a reduced pressure furnace. This invention relates to a container for iron powder heat treatment.

【0002】0002

【従来の技術】粉末冶金用の鉄粉は品質向上のため、ア
トマイズ鉄粉などを還元、焼鈍(熱処理)して製造する
。従来の鉄粉の熱処理方法は図2(a)、(b)に示す
ごとく金属製の熱処理容器1に鉄粉3を充填し、図3に
示すごとく棚状に組み立てたグラファイト製トレイ4に
鉄粉3を充填した熱処理容器1を積載し、熱処理炉に装
入する。鉄粉3は熱処理炉において高温で熱処理され、
熱処理が終了すると鉄粉3は熱処理容器1から排出され
、粉砕−分級−梱包−出荷する工程を通って製品となる
BACKGROUND OF THE INVENTION Iron powder for powder metallurgy is manufactured by reducing and annealing (heat treating) atomized iron powder to improve its quality. In the conventional heat treatment method for iron powder, a metal heat treatment container 1 is filled with iron powder 3 as shown in FIGS. The heat treatment container 1 filled with powder 3 is loaded and charged into the heat treatment furnace. The iron powder 3 is heat treated at high temperature in a heat treatment furnace,
When the heat treatment is completed, the iron powder 3 is discharged from the heat treatment container 1 and becomes a product through the steps of pulverization, classification, packaging, and shipping.

【0003】ところで、このような従来の鉄粉を皿形熱
処理容器にいれて還元、焼鈍するという工程には、次の
ような問題点があった。 (1)熱処理時、容器そのものと鉄粉が反応焼結してし
まい、鉄粉を排出する工程で容器から容易に排出できな
い。 (2)均一加熱及び粉砕性を確保する目的で一般に実開
昭61−137629号公報にみられるように容器内に
人工仕切壁を設けてあるが、これが排出を一層困難にす
る。
However, the conventional process of placing iron powder in a dish-shaped heat treatment container and reducing and annealing it has the following problems. (1) During heat treatment, the container itself and the iron powder react and sinter, making it impossible to easily discharge the iron powder from the container during the process of discharging the iron powder. (2) For the purpose of ensuring uniform heating and crushability, an artificial partition wall is generally provided inside the container as seen in Japanese Utility Model Application No. 61-137629, but this makes discharging even more difficult.

【0004】このように鉄粉が容器へしばしば付着する
ため、現在は容器にハンマー等で衝撃を与えて排出を行
っている。このために容器の変形、損傷が甚だしくなる
。また、完全には容器に付着した鉄粉を除去することが
できず、一部が残留することになり、この残留した付着
鉄粉が容器を次回使用したときに、付着の起点となり、
一層付着が激しくなる。他に、成分組成の異なる鉄粉を
同じ容器を使って熱処理しようとする場合に望ましくな
い成分が混入する恐れも生じる。
[0004] Since iron powder often adheres to the container in this way, it is currently discharged by applying an impact to the container with a hammer or the like. This causes severe deformation and damage to the container. In addition, it is not possible to completely remove the iron powder adhering to the container, and some of it remains, and this remaining adhering iron powder becomes the starting point of adhesion when the container is used next time.
The adhesion becomes even more intense. In addition, when iron powders having different compositions are heat-treated in the same container, there is a risk that undesirable components may be mixed in.

【0005】そこで、このような熱処理粉の容器付着を
防止するために、水溶性の黒鉛を塗布する手段が、特公
昭55−30044号公報に開示されている。しかしな
がら、容器には一般に安価な鉄製容器(ステンレス製)
が用いられており、高温熱処理に繰り返し使用している
うちに、塗布された黒鉛が浸炭し、容器が劣化し、容器
自体の寿命が著しく低下する問題があった。
[0005] Therefore, in order to prevent such heat-treated powder from adhering to the container, Japanese Patent Publication No. 55-30044 discloses a means of coating water-soluble graphite. However, containers are generally made of inexpensive iron containers (stainless steel).
However, when used repeatedly for high-temperature heat treatment, the coated graphite carburizes, causing the container to deteriorate, resulting in a significant shortening of the lifespan of the container itself.

【0006】更に、これを改良するために前記黒鉛塗布
層の下に高融点酸化物の塗布層を設けたものが特開平2
−200701号公報に提案されているが施工が煩雑で
あるという問題がある。
[0006] Furthermore, in order to improve this, a coating layer of a high melting point oxide is provided under the graphite coating layer, as disclosed in Japanese Patent Application Laid-Open No.
Although it has been proposed in Japanese Patent No. 200701, there is a problem that the construction is complicated.

【0007】[0007]

【発明が解決しようとする課題】本発明の目的は、鉄粉
を容器中に充填し、還元焼鈍などの熱処理を施した際に
、容器と鉄粉の焼結(付着)を防止し、鉄粉の排出を容
易ならしめる鉄粉熱処理用容器を提案することである。 また、鉄粉の高温熱処理に繰り返し使用することに関し
ても、その劣化が小さく、従って高寿命の鉄粉熱処理用
容器を提案するものである。
[Problems to be Solved by the Invention] An object of the present invention is to prevent sintering (adhesion) between the container and iron powder when iron powder is filled into a container and subjected to heat treatment such as reduction annealing, It is an object of the present invention to propose a container for heat treatment of iron powder that makes it easy to discharge the powder. In addition, the present invention proposes a container for heat treatment of iron powder that exhibits little deterioration when repeatedly used for high-temperature heat treatment of iron powder, and therefore has a long life.

【0008】[0008]

【課題を解決するための手段】本発明は、鉄粉又は合金
鋼粉用熱処理容器であって、表面に酸化皮膜を形成した
ステンレス鋼で構成され、かつ該酸化皮膜表面から10
Å以内にSi、Al、Ti、Mn及びCrの1種又は2
種以上の元素が濃化していることを特徴とする鉄粉熱処
理用容器である。
[Means for Solving the Problems] The present invention is a heat treatment container for iron powder or alloy steel powder, which is made of stainless steel with an oxide film formed on the surface, and which is made of stainless steel with an oxide film formed on the surface.
One or two of Si, Al, Ti, Mn and Cr within Å
This is a container for heat treatment of iron powder, characterized by the fact that more than one element is concentrated.

【0009】[0009]

【作  用】本発明者らは、鉄粉と熱処理容器との焼結
による付着を防止するために種々検討した結果、容器表
面に形成された酸化皮膜表面から10Å以内にSi、A
l、Ti、Mn及びCrの1種又は2種以上の元素が濃
化したステンレス鋼製の容器を用いることが付着防止に
効果があることを発見した。
[Function] As a result of various studies to prevent adhesion of iron powder and heat treatment container due to sintering, the present inventors found that Si, A
It has been discovered that using a stainless steel container enriched with one or more of the following elements: L, Ti, Mn, and Cr is effective in preventing adhesion.

【0010】次に本発明者らが容器への鉄粉の付着性を
容器の組成及び表面状態を変化させて検討した結果を詳
細に説明する。鉄粉と容器の付着は、鉄粉を還元する雰
囲気中で容器表面の酸化物も還元され、容器の地金が表
れた時点で鉄粉と焼結する現象であることが明らかにな
った。また、表面から10Å以内にSi、Al、Ti、
Mn、Crのうち1種又は2種以上の元素が濃化した酸
化皮膜を形成したステンレス鋼製の容器においては、鉄
粉が付着しないことを見出した。
[0010] Next, the results of studies conducted by the present inventors on the adhesion of iron powder to containers by varying the composition and surface condition of the containers will be explained in detail. It has become clear that the adhesion of iron powder to the container is a phenomenon in which oxides on the surface of the container are also reduced in an atmosphere that reduces iron powder, and when the bare metal of the container is exposed, it sinters with the iron powder. In addition, within 10 Å from the surface, Si, Al, Ti,
It has been found that iron powder does not adhere to stainless steel containers in which an oxide film containing one or more of Mn and Cr is concentrated.

【0011】容器内側の表面にSi、Al、Ti、Mn
、Crのうち1種または2種以上の元素が濃化している
ということは、Si、Al、Ti、Mn、Crなどが酸
化していることを意味している。すなわちこの濃化層厚
が容器の表面からの酸素元素の拡散(いわゆる酸化層厚
)の程度を示しており、これがステンレス鋼表面の酸化
皮膜の欠陥の程度に非常に影響を受けると考えられる。 濃化層厚が表面から10Å以内の場合、付着が起きない
のは容器表面の酸化皮膜の欠陥が少なく、酸化皮膜が容
器の使用される雰囲気中では還元され難くなり、還元時
間に長時間を要するようになるためである。
[0011] Si, Al, Ti, Mn on the inner surface of the container.
The concentration of one or more elements among , Cr means that Si, Al, Ti, Mn, Cr, etc. are oxidized. In other words, this concentrated layer thickness indicates the degree of diffusion of oxygen elements from the surface of the container (so-called oxide layer thickness), and it is thought that this is greatly influenced by the degree of defects in the oxide film on the stainless steel surface. When the thickness of the concentrated layer is within 10 Å from the surface, adhesion does not occur because there are few defects in the oxide film on the container surface, and the oxide film is difficult to reduce in the atmosphere in which the container is used, and the reduction time takes a long time. This is because it becomes necessary.

【0012】また、この酸化皮膜の濃化元素をSi、A
l、Ti、Mn、Crのうち1種または2種以上の元素
としたのは、難還元性元素であるSi、Al、Ti、M
n、Crのうち1種または2種以上の元素を含むことに
より、酸化皮膜が容器の使用される雰囲気中で容易に還
元されないためである。この表面から10Å以内にSi
、Al、Ti、Mn、Crのうち1種または2種以上の
元素が濃化し、表面に酸化皮膜を形成したステンレス鋼
製の容器において、鉄粉の付着は抑えることができた。
[0012] Also, the concentration elements of this oxide film are Si, A
One or more elements among L, Ti, Mn, and Cr are difficult to reduce elements such as Si, Al, Ti, and Mn.
This is because the oxide film is not easily reduced in the atmosphere in which the container is used by containing one or more elements among n and Cr. Si within 10 Å from this surface
, Al, Ti, Mn, and Cr, the adhesion of iron powder could be suppressed in stainless steel containers in which one or more elements among Cr, Al, Ti, Mn, and Cr were concentrated and an oxide film was formed on the surface.

【0013】なお、濃化とは念のため付言すれば、これ
らの元素の濃度が酸化膜中の平均濃度より高いことを言
い、グロー放電分光分析により容易に測定できる。繰り
返し使用の面においても表面から10Å以内にSi、A
l、Ti、Mn、Crのうち1種または2種以上の元素
が濃化し、表面の欠陥が少ないということは、容器が使
用される雰囲気中で容器成分中に含まれる難還元性元素
の雰囲気中への飛散(蒸発)が少なくなる。この難還元
性元素の飛散が少ないと、一度還元されて薄くなった酸
化皮膜も炉の冷却中に再酸化し、厚い難還元性元素を含
む酸化膜が再生するので容器寿命も伸びる。
It should be noted that enrichment means that the concentration of these elements is higher than the average concentration in the oxide film, and can be easily measured by glow discharge spectrometry. Even in the aspect of repeated use, Si, A
The fact that one or more elements among L, Ti, Mn, and Cr are concentrated and there are few defects on the surface means that the atmosphere in which the container is used contains the refractory elements contained in the container components. Less scattering (evaporation) inside. If the scattering of these refractory elements is small, the oxide film that has been reduced and becomes thinner will be re-oxidized during cooling of the furnace, and the thick oxide film containing the refractory element will be regenerated, extending the life of the container.

【0014】容器材質にステンレス鋼を用いたのは、高
温特性に優れ、安価であるためである。以上のように、
このような容器に鉄粉を充填して、熱処理しても、容器
を反転させることにより、容易に鉄粉を排出できるよう
になった。また、容器より鉄粉を完全に排出できるため
、付着の起点となる残留鉄粉がなくなり、繰り返し使用
の面でも有効である。
Stainless steel is used as the container material because it has excellent high temperature properties and is inexpensive. As mentioned above,
Even if such a container is filled with iron powder and subjected to heat treatment, the iron powder can now be easily discharged by inverting the container. In addition, since the iron powder can be completely discharged from the container, there is no residual iron powder that can become a starting point for adhesion, making it effective for repeated use.

【0015】[0015]

【実施例】実施例1 図1は本発明に係る容器の断面図を示す。本発明の容器
1Aは、従来のステンレス製容器1の内面に9Åの厚さ
のSi濃化層を、比較例では20ÅのSi濃化層を持ち
、表面に酸化膜を形成している。このステンレス製容器
1の内面にSi濃化層を持ち表面に酸化膜を形成するた
めの方法は、この場合SUS 304を用い露点を制御
した雰囲気中で焼鈍酸化させて所望のSi濃化層を形成
させた。このステンレス製容器に鉄粉3を充填し、グラ
ファイト製トレイ4に積載し、熱処理炉に装入し、真空
中1150℃の高温にて3時間熱処理を行った。熱処理
後、鉄粉3を排出するため容器2を反転したところ、表
面に9Åの厚さのSi濃化層を持ったステンレス鋼を用
いた容器2は鉄粉が付着せず、鉄粉3は容易に完全に排
出することができた。 もちろん、容器2をハンマーにて衝撃を加える必要がな
いので、容器2の変形、損傷はなかった。これに対して
、表面に20Åの厚さのSi濃化層を持ったステンレス
鋼を用いた容器では鉄粉3が容易に排出できず、ハンマ
ーにて衝撃を加えて排出したため容器2が変形、損傷し
てしまった。
EXAMPLES Example 1 FIG. 1 shows a sectional view of a container according to the present invention. The container 1A of the present invention has a Si enriched layer with a thickness of 9 Å on the inner surface of the conventional stainless steel container 1, and the comparative example has a Si enriched layer with a thickness of 20 Å, and an oxide film is formed on the surface. The method for forming a Si-concentrated layer on the inner surface of the stainless steel container 1 and an oxide film on the surface is to form a desired Si-concentrated layer by annealing and oxidizing SUS 304 in an atmosphere with a controlled dew point. formed. This stainless steel container was filled with iron powder 3, loaded onto a graphite tray 4, placed in a heat treatment furnace, and heat treated in vacuum at a high temperature of 1150° C. for 3 hours. After the heat treatment, when the container 2 was turned over to discharge the iron powder 3, the iron powder did not adhere to the container 2, which was made of stainless steel with a 9 Å thick Si enriched layer on the surface, and the iron powder 3 It could be easily and completely drained. Of course, since there was no need to apply an impact to the container 2 with a hammer, there was no deformation or damage to the container 2. On the other hand, in a container made of stainless steel with a 20 Å thick Si-enriched layer on its surface, the iron powder 3 could not be easily discharged, and the container 2 was deformed because it was discharged by applying impact with a hammer. It was damaged.

【0016】実施例2 表面に8Åおよび12ÅのSiとAlの濃化層を持ち、
表面に酸化皮膜を形成したステンレス鋼を用いて容器を
作製し、実施例1と同様の実験を行った。8Åの場合鉄
粉3は容器2より容易に排出することができたのに対し
、12Åの場合には付着がみられた。
Example 2 Having Si and Al concentrated layers of 8 Å and 12 Å on the surface,
A container was prepared using stainless steel with an oxide film formed on its surface, and an experiment similar to that in Example 1 was conducted. In the case of 8 Å, the iron powder 3 could be easily discharged from the container 2, whereas in the case of 12 Å, adhesion was observed.

【0017】実施例3 表面に9Åの厚さのSi濃化層を持ち、表面に酸化皮膜
を形成したステンレス鋼を用いて図1の熱処理容器2を
作製し、それぞれの熱処理容器の上に鉄粉3を充填し、
グラファイト製トレイ4に積載し、熱処理炉に装入した
。 熱処理条件は、真空中1150℃の高温にて4時間と8
時間で行った。(通常、鉄粉の熱処理は4時間以内で行
う。)熱処理後、鉄粉3を排出するため容器2を反転し
たところ、表面に4時間および8時間熱処理を行った容
器2は両方とも鉄粉が付着せず、鉄粉3は容易に完全に
排出することができた。もちろん、容器2をハンマーに
て衝撃を加える必要がないので、容器2の変形、損傷は
なかった。
Example 3 The heat treatment containers 2 shown in FIG. 1 were fabricated using stainless steel with a 9 Å thick Si-enriched layer and an oxide film formed on the surface, and iron was placed on top of each heat treatment container. Fill with powder 3,
It was loaded onto a graphite tray 4 and charged into a heat treatment furnace. The heat treatment conditions were 4 hours and 8 hours at a high temperature of 1150°C in vacuum.
I went in time. (Usually, iron powder is heat-treated within 4 hours.) After the heat treatment, when the container 2 was turned over to discharge the iron powder 3, it was found that both the containers 2 whose surfaces had been heat-treated for 4 hours and 8 hours had iron powder. The iron powder 3 could be easily and completely discharged without any adhesion. Of course, since there was no need to apply an impact to the container 2 with a hammer, there was no deformation or damage to the container 2.

【0018】[0018]

【発明の効果】以上、説明したように、本発明の容器を
用いることによって鉄粉の排出が容易となり、従来の人
手による排出作業が不用になった。また、残留した付着
鉄粉がなくなったため、容器の劣化が防止され容器の寿
命も大幅に向上させることができた。回収歩留りが向上
するほか、残留付着鉄粉の影響を受けないので高純度の
品質のものが得られる。
[Effects of the Invention] As explained above, by using the container of the present invention, iron powder can be easily discharged, and the conventional manual discharge operation is no longer necessary. Additionally, since the remaining adhering iron powder was eliminated, deterioration of the container was prevented and the life of the container was significantly extended. In addition to improving the recovery yield, high-purity products can be obtained because they are not affected by residual adhering iron powder.

【図面の簡単な説明】[Brief explanation of the drawing]

【図1】本発明の鉄粉熱処理用容器の断面図である。FIG. 1 is a sectional view of a container for iron powder heat treatment of the present invention.

【図2】(A)は従来の鉄粉熱処理容器の平面図、(B
)はその断面図である。
[Figure 2] (A) is a plan view of a conventional iron powder heat treatment container, (B)
) is its cross-sectional view.

【図3】グラファイト製トレイに収容した鉄粉熱処理容
器の側面図である。
FIG. 3 is a side view of an iron powder heat treatment container housed in a graphite tray.

【符号の説明】[Explanation of symbols]

1  容器本体 2  仕切壁 3  鉄粉 4  トレイ 5  酸化膜 1 Container body 2 Partition wall 3 Iron powder 4 Tray 5 Oxide film

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】  鉄粉又は合金鋼粉用熱処理容器であっ
て、表面に酸化皮膜を形成したステンレス鋼で構成され
、かつ該酸化皮膜表面から10Å以内にSi、Al、T
i、Mn及びCrの1種又は2種以上の元素が濃化して
いることを特徴とする鉄粉熱処理用容器。
1. A heat treatment container for iron powder or alloy steel powder, which is made of stainless steel with an oxide film formed on the surface, and contains Si, Al, T, etc. within 10 Å from the surface of the oxide film.
A container for heat treatment of iron powder, characterized in that one or more of the following elements: i, Mn, and Cr are concentrated.
JP3034602A 1991-02-28 1991-02-28 Iron powder heat treatment container Expired - Lifetime JPH07116484B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3034602A JPH07116484B2 (en) 1991-02-28 1991-02-28 Iron powder heat treatment container

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3034602A JPH07116484B2 (en) 1991-02-28 1991-02-28 Iron powder heat treatment container

Publications (2)

Publication Number Publication Date
JPH04272102A true JPH04272102A (en) 1992-09-28
JPH07116484B2 JPH07116484B2 (en) 1995-12-13

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
JP3034602A Expired - Lifetime JPH07116484B2 (en) 1991-02-28 1991-02-28 Iron powder heat treatment container

Country Status (1)

Country Link
JP (1) JPH07116484B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08152279A (en) * 1994-11-30 1996-06-11 Matsushita Electric Ind Co Ltd Box for calcining ceramic powder
JP2014005160A (en) * 2012-06-21 2014-01-16 Ibiden Co Ltd Base body used for sintering graphite material, sintering container and sintering method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08152279A (en) * 1994-11-30 1996-06-11 Matsushita Electric Ind Co Ltd Box for calcining ceramic powder
JP2014005160A (en) * 2012-06-21 2014-01-16 Ibiden Co Ltd Base body used for sintering graphite material, sintering container and sintering method

Also Published As

Publication number Publication date
JPH07116484B2 (en) 1995-12-13

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