JPH06116607A - Production of sealed fe base sintered alloy parts excellent in airtightness - Google Patents

Production of sealed fe base sintered alloy parts excellent in airtightness

Info

Publication number
JPH06116607A
JPH06116607A JP29203992A JP29203992A JPH06116607A JP H06116607 A JPH06116607 A JP H06116607A JP 29203992 A JP29203992 A JP 29203992A JP 29203992 A JP29203992 A JP 29203992A JP H06116607 A JPH06116607 A JP H06116607A
Authority
JP
Japan
Prior art keywords
sintered alloy
sealed
alloy
atmosphere
airtightness
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
JP29203992A
Other languages
Japanese (ja)
Other versions
JP2946972B2 (en
Inventor
Sekihin You
楊  積彬
Masakazu Watarai
正和 渡会
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.)
Mitsubishi Materials Corp
Original Assignee
Mitsubishi Materials 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 Mitsubishi Materials Corp filed Critical Mitsubishi Materials Corp
Priority to JP29203992A priority Critical patent/JP2946972B2/en
Publication of JPH06116607A publication Critical patent/JPH06116607A/en
Application granted granted Critical
Publication of JP2946972B2 publication Critical patent/JP2946972B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Abstract

PURPOSE:To produce the sealed Fe base sintered alloy parts excellent in airtightness by modifying an Fe base sintered alloy having a specified porosity at a specified temp. in a hydrogen-contg. atmosphere and then sealing the alloy with steam. CONSTITUTION:An Fe base alloy powder of specified composition is press- formed, and the formed body is sintered in a nitrogen-contg. atmosphere to obtain the Fe base sintered alloy having 10-30% porosity. The alloy is heated at 400-600 deg.C in a hydrogen-contg. atmosphere and modified, hence the nitrogen absorbed on the alloy surface and intered solid solution and inhibiting the progress of the oxidation reaction when the alloy is sealed reacts with hydrogen and is removed. Consequently, the oxidation reaction with steam is promoted in the succeeding sealing stage, a dense oxide film is formed, and the sealed Fe base sintered alloy parts having about >=20kg/cm<2> withstanding pressure and excellent in airtightness are obtained.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】この発明は、気密性のすぐれた封
孔Fe基焼結合金部品を製造する方法に関するものであ
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a sealed Fe-based sintered alloy part having excellent airtightness.

【0002】[0002]

【従来の技術】従来、一般に耐圧性が要求される油圧ポ
ンプやエアコン、さらにコンプレッサなどの構造部材と
して封孔Fe基焼結合金部品が用いられている。この封
孔Fe基焼結合金部品は、通常所定の配合組成を有する
混合粉末からプレス成形された圧粉体を、還元性雰囲気
中、1100〜1200℃の温度で焼結し、この結果得
られた気孔率:10〜30%を有するFe基焼結合金基
体に、連続炉またはバッチ炉を用い、温度:500〜6
50℃、圧力:5〜40mmAq、保持時間:1〜5時間
の条件で、過熱水蒸気を作用させて緻密なFe3 4
酸化皮膜を生成させることからなる水蒸気による封孔処
理を施して、20kg/cm2以上の耐圧力を具備せしめる
ことにより製造されるものである。
2. Description of the Related Art Conventionally, sealed Fe-based sintered alloy parts have been used as structural members such as hydraulic pumps, air conditioners, and compressors, which generally require pressure resistance. This sealed Fe-based sintered alloy part is obtained by sintering a green compact press-molded from a mixed powder having a predetermined compounding composition at a temperature of 1100 to 1200 ° C. in a reducing atmosphere. For the Fe-based sintered alloy substrate having a porosity of 10 to 30%, a continuous furnace or a batch furnace is used, and the temperature is 500 to 6
Under conditions of 50 ° C., pressure: 5 to 40 mmAq, and holding time: 1 to 5 hours, a superheated steam is allowed to act to form a dense oxide film of Fe 3 O 4 , and a sealing treatment with steam is performed, It is manufactured by providing a withstand pressure of 20 kg / cm 2 or more.

【0003】[0003]

【発明が解決しようとする課題】一方、近年、化石資源
の有限性、Fe基焼結合金基体の炭素濃度の制御、およ
び焼結炉設備の寿命などの点から、焼結雰囲気を、還元
性雰囲気(例えば変成ガス)にかえて窒素含有雰囲気と
する傾向にある。しかし、窒素含有雰囲気で焼結された
Fe基焼結合金に、上記水蒸気による封孔処理を施した
場合、十分な気密性が得られず、約5kg/cm2 以下程度
の耐圧力しか得られないのが現状である。
On the other hand, in recent years, from the viewpoints of finite fossil resource, control of carbon concentration of Fe-based sintered alloy substrate, life of sintering furnace equipment, etc. A nitrogen-containing atmosphere tends to be used instead of the atmosphere (for example, the metamorphic gas). However, when the Fe-based sintered alloy sintered in a nitrogen-containing atmosphere is subjected to the pore-sealing treatment with the above steam, sufficient airtightness cannot be obtained, and only a withstand pressure of about 5 kg / cm 2 or less is obtained. The current situation is that there are none.

【0004】[0004]

【課題を解決するための手段】そこで、本発明者等は、
上述のような観点から、窒素含有雰囲気で焼結したFe
基焼結合金基体の水蒸気による封孔処理に着目し研究を
行なった結果、水蒸気による封孔処理に先だって、焼結
雰囲気を窒素含有雰囲気としたFe基焼結合金基体に、
水素含有雰囲気、望ましくはH2 :10容量%以上を含
有する雰囲気中、400〜600℃の温度に加熱保持の
条件で改質処理を施すと、焼結時に合金表面部に吸着固
溶して、封孔処理の際の酸化反応の進行を阻害していた
窒素が前記改質処理の雰囲気中の水素との反応で除去さ
れ、この結果水蒸気による酸化反応の進行が著しく早め
られ、緻密な酸化皮膜が形成されることから、耐圧力で
20kg/cm2 以上の気密性のすぐれた封孔Fe基焼結合
金部品が得られるようになるという研究結果を得たので
ある。
Therefore, the present inventors have
From the above viewpoint, Fe sintered in a nitrogen-containing atmosphere
As a result of conducting a study focusing on the sealing treatment of the base sintered alloy substrate with steam, the Fe-based sintered alloy substrate whose sintering atmosphere was a nitrogen-containing atmosphere prior to the sealing treatment with steam was
When a hydrogen-containing atmosphere, preferably an atmosphere containing H 2 : 10 vol% or more, is subjected to a modification treatment under the condition of heating and holding at a temperature of 400 to 600 ° C., it is adsorbed and solid-solved on the alloy surface portion during sintering. Nitrogen, which hindered the progress of the oxidation reaction during the sealing treatment, was removed by the reaction with hydrogen in the atmosphere of the reforming treatment, and as a result, the progress of the oxidation reaction by steam was significantly accelerated, resulting in a dense oxidation. Since the film is formed, a research result was obtained that a sealed Fe-based sintered alloy part having a pressure resistance of 20 kg / cm 2 or more and excellent airtightness can be obtained.

【0005】この発明は、上記の研究結果にもとづいて
なされたものであって、窒素含有雰囲気中で焼結された
気孔率:10〜30%を有するFe基焼結合金基体に、
水素含有雰囲気中、400〜600℃の温度に加熱保持
の条件で改質処理を施した後、水蒸気による封孔処理を
施すことにより気密性のすぐれた封孔Fe基焼結合金部
品を製造する方法に特徴を有するものである。
The present invention has been made on the basis of the above-mentioned research results, and is based on an Fe-based sintered alloy substrate having a porosity of 10 to 30% sintered in a nitrogen-containing atmosphere.
In a hydrogen-containing atmosphere, a reforming treatment is performed at a temperature of 400 to 600 ° C. under a condition of heating and holding, and then a sealing treatment with steam is performed to manufacture a sealed Fe-based sintered alloy part having excellent airtightness. It is characterized by the method.

【0006】なお、この発明の方法において、Fe基焼
結合金基体の気孔率を10〜30%としたのは、その気
孔率を10%未満に緻密化するには、圧粉体成形時に大
型のプレス成形装置を必要とし、実用的でなく、一方そ
の気孔率が30%を越えると強度が急激に低下するよう
になるという理由にもとづくものである。
In the method of the present invention, the porosity of the Fe-based sintered alloy substrate is set to 10 to 30%, because the porosity of the Fe-based sintered alloy substrate is to be densified to less than 10%. It is not practical and requires a press-molding device (1), and on the other hand, when the porosity exceeds 30%, the strength rapidly decreases.

【0007】また、この発明の方法において、改質処理
温度を400〜600℃と定めたのは、その温度が40
0℃未満では、基体中の吸着固溶窒素と雰囲気中の水素
との結合反応が遅く、したがって脱窒素反応に長時間を
要するようになり、一方その温度が600℃を越えて
も、前記の脱窒素反応の進行が抑制されるようになると
いう理由によるものである。
In the method of the present invention, the temperature of the reforming treatment is set to 400 to 600 ° C.
When the temperature is lower than 0 ° C, the binding reaction between the adsorbed solid solution nitrogen in the substrate and hydrogen in the atmosphere is slow, and therefore the denitrification reaction takes a long time, while even if the temperature exceeds 600 ° C, the above-mentioned This is because the progress of the denitrification reaction is suppressed.

【0008】[0008]

【実施例】つぎに、この発明の方法を実施例により具体
的に説明する。原料粉末として、いずれも20〜200
μmの範囲内の所定の平均粒径を有する、Cu粉末、お
よび黒鉛粉末、さらに表1に示される成分組成をもった
Fe基合金粉末を用意し、これら原料粉末を表1に示さ
れる配合組成に配合し、混合した後、6〜7ton /cm2
の範囲内の圧力でプレス成形して圧粉体A〜Iを形成
し、これらの圧粉体A〜Iに、それぞれ、容量%で、
(a) N2 :42.2%,H2 :33.4%,CO:
24.0%,CH4 :0.4%、(b) N2 :25.
0%,H2 :75.0%、(c) N2 :98.0%,
2 :2.0%、以上(a)〜(c)のいずれかの窒素
含有焼結雰囲気中、表2,3に示される温度に20分間
保持の条件で焼結して、同じく表2,3に示される気孔
率を有し、かついずれも直径:50mmφ×厚さ:5mmの
寸法をもったFe基焼結合金基体を形成し、引続いて焼
結後の冷却過程(この場合を連続処理という)または一
旦室温に冷却後(この場合を断続処理という)、(i)
2 +H2 混合ガス(H2 :10容量%含有)、(i
i) アンモニア分解ガス+N2 ガス(H2 :30容量
%含有)、(iii) H2 ガス、以上(i)〜(ii
i)のいずれかの水素含有雰囲気中、表2,3に示され
る条件で前記Fe基焼結合金基体に改質処理を施し、つ
いで、連続炉を用い、温度:560℃、圧力:20mmA
q、保持時間:1.5時間の条件で水蒸気による封孔処
理を施すことからなる本発明方法1〜9を実施し、封孔
Fe基焼結合金部品をそれぞれ製造した。また、比較の
目的で、表2,3に示される通り、上記改質処理を行な
わない以外は同一の条件で比較方法1〜9を行ない、封
孔Fe基焼結合金部品を製造した。
EXAMPLES Next, the method of the present invention will be specifically described by way of examples. 20-200 as raw material powder
A Cu powder, a graphite powder, and an Fe-based alloy powder having the component composition shown in Table 1 having a predetermined average particle diameter within the range of μm were prepared, and these raw material powders were mixed with the composition shown in Table 1. 6 ton / cm 2 after mixing and mixing
By press molding at a pressure within the range to form green compacts A to I.
(A) N 2 : 42.2%, H 2 : 33.4%, CO:
24.0%, CH 4: 0.4% , (b) N 2: 25.
0%, H 2 : 75.0%, (c) N 2 : 98.0%,
H 2 : 2.0%, sintered in a nitrogen-containing sintering atmosphere of any of the above (a) to (c) at the temperature shown in Tables 2 and 3 for 20 minutes, and then the same as Table 2 , 3 and having a porosity of 50 mmφ × thickness: 5 mm, each of which was formed into a Fe-based sintered alloy substrate, followed by a cooling process after sintering (in this case, (Continuous processing) or once cooled to room temperature (this case is called intermittent processing), (i)
N 2 + H 2 mixed gas (H 2 : containing 10% by volume), (i
i) Ammonia decomposition gas + N 2 gas (H 2 content: 30% by volume), (iii) H 2 gas, above (i) to (ii)
In any of the hydrogen-containing atmospheres of i), the Fe-based sintered alloy substrate is subjected to a modification treatment under the conditions shown in Tables 2 and 3, and then a continuous furnace is used to temperature: 560 ° C., pressure: 20 mmA.
q, holding time: the methods 1 to 9 of the present invention, which consist of performing a sealing treatment with steam under the conditions of 1.5 hours, were carried out to produce sealed Fe-based sintered alloy parts. For the purpose of comparison, as shown in Tables 2 and 3, Comparative Methods 1 to 9 were carried out under the same conditions except that the above-mentioned modification treatment was not carried out to manufacture a sealed Fe-based sintered alloy part.

【0009】[0009]

【表1】 [Table 1]

【0010】[0010]

【表2】 [Table 2]

【0011】[0011]

【表3】 [Table 3]

【0012】つぎに、この結果得られた各種の封孔Fe
基焼結合金部品(以下、単に部品という)について、図
1に概略縦断面図で示される通り、孔あき基板1の上
に、前記孔を中心にして上下面にOリングパッキングを
有する下部リング2を載置し、この下部リング2の上に
上記部品3を重ね、その上に下面に同じくOリングパッ
キングを有し、かつ側面に貫通孔4を有する蓋付上部リ
ング5を載置し、さらに前記部品3の外周側面を覆うよ
うにカバーリング6を嵌着して、これを前記下部および
上部リング2,5にボルト(図示せず)で取付け、前記
貫通孔4には他方端を流量計7に取付けたパイプ8の一
方端を取付け、上記上部リング5に押えバンチ9で50
kg/cm2 の圧力を付加した状態で、基板1の孔から上記
部品3の下面に加圧窒素ガスを導入し、上記部品3の上
面からリークした窒素ガスの流量が前記流量計7で検知
して、3cc/min.となった時点の前記加圧窒素ガスの圧
力を測定し、耐圧力とした。この結果を表2,3に示し
た。
Next, various kinds of sealing Fe obtained as a result are obtained.
Regarding a base sintered alloy component (hereinafter, simply referred to as a component), as shown in a schematic longitudinal sectional view in FIG. 1, a lower ring having O-ring packings on the upper and lower surfaces centering on the hole on a perforated substrate 1. 2 is placed on the lower ring 2, and the component 3 is placed on the lower ring 2, and the upper ring 5 with a lid having the O-ring packing on the lower surface and the through hole 4 on the side surface is placed thereon. Further, a cover ring 6 is fitted so as to cover the outer peripheral side surface of the component 3, and is attached to the lower and upper rings 2 and 5 with bolts (not shown). Attach one end of the pipe 8 attached to the total 7, and press it against the upper ring 5 with the bunch 9
With the pressure of kg / cm 2 applied, pressurized nitrogen gas was introduced from the hole of the substrate 1 to the lower surface of the component 3, and the flow rate of the nitrogen gas leaked from the upper surface of the component 3 was detected by the flow meter 7. Then, the pressure of the pressurized nitrogen gas at the time of reaching 3 cc / min. The results are shown in Tables 2 and 3.

【0013】表2,3に示される通り、本発明方法1〜
9によって製造された封孔Fe基焼結合金部品は、いず
れも改質処理を行なわない比較方法1〜9で製造された
封孔Fe基焼結合金部品に比して、一段と高い耐圧力を
示すことが明らかである。上述のように、この発明の方
法によれば窒素含有雰囲気を適用して焼結されたFe基
焼結合金であっても、水蒸気による封孔処理前に、これ
に改質処理を施すことにより気密性のすぐれた封孔Fe
基焼結合金部品を製造することができるのである。
As shown in Tables 2 and 3, the method 1 of the present invention
The sealed Fe-based sintered alloy parts manufactured according to No. 9 have much higher pressure resistance than the sealed Fe-based sintered alloy parts manufactured according to Comparative Methods 1 to 9 in which no modification treatment is performed. It is clear to show. As described above, according to the method of the present invention, even if the Fe-based sintered alloy is sintered by applying the nitrogen-containing atmosphere, by subjecting it to the modification treatment before the sealing treatment with the steam, Sealing Fe with excellent airtightness
It is possible to manufacture a base sintered alloy part.

【図面の簡単な説明】[Brief description of drawings]

【図1】封孔Fe基焼結合金部品の耐圧力の測定態様を
示す概略縦断面図である。
FIG. 1 is a schematic vertical sectional view showing a measurement mode of pressure resistance of a sealed Fe-based sintered alloy part.

【符号の説明】[Explanation of symbols]

1 基板 2 下部リング 3 封孔Fe基焼結合金部品 4 貫通孔 5 上部リング 6 カバーリング 7 流量計 8 パイプ 9 押えパンチ 1 substrate 2 lower ring 3 sealing Fe-based sintered alloy component 4 through hole 5 upper ring 6 cover ring 7 flow meter 8 pipe 9 presser punch

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 窒素含有雰囲気中で焼結された気孔率:
10〜30%を有するFe基焼結合金基体に、水蒸気に
よる封孔処理を施すに先だって、 水素含有雰囲気中、400〜600℃の温度に加熱保持
の条件で改質処理を施すことを特徴とする気密性のすぐ
れた封孔Fe基焼結合金部品の製造方法。
1. Porosity sintered in a nitrogen-containing atmosphere:
The Fe-based sintered alloy substrate having 10 to 30% is characterized by being subjected to a modification treatment under a condition of heating and holding at a temperature of 400 to 600 ° C. in a hydrogen-containing atmosphere before the sealing treatment with steam. A method for producing a sealed Fe-based sintered alloy component having excellent airtightness.
JP29203992A 1992-10-06 1992-10-06 Method for producing sealed Fe-based sintered alloy part with excellent airtightness Expired - Fee Related JP2946972B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP29203992A JP2946972B2 (en) 1992-10-06 1992-10-06 Method for producing sealed Fe-based sintered alloy part with excellent airtightness

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP29203992A JP2946972B2 (en) 1992-10-06 1992-10-06 Method for producing sealed Fe-based sintered alloy part with excellent airtightness

Publications (2)

Publication Number Publication Date
JPH06116607A true JPH06116607A (en) 1994-04-26
JP2946972B2 JP2946972B2 (en) 1999-09-13

Family

ID=17776745

Family Applications (1)

Application Number Title Priority Date Filing Date
JP29203992A Expired - Fee Related JP2946972B2 (en) 1992-10-06 1992-10-06 Method for producing sealed Fe-based sintered alloy part with excellent airtightness

Country Status (1)

Country Link
JP (1) JP2946972B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005256062A (en) * 2004-03-10 2005-09-22 Sumitomo Denko Shoketsu Gokin Kk Bearing for compressor
JP2006299324A (en) * 2005-04-19 2006-11-02 Mazda Motor Corp Method for surface-treating steel member, steel member and toothed gear

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005256062A (en) * 2004-03-10 2005-09-22 Sumitomo Denko Shoketsu Gokin Kk Bearing for compressor
JP4528542B2 (en) * 2004-03-10 2010-08-18 住友電工焼結合金株式会社 Compressor bearing
JP2006299324A (en) * 2005-04-19 2006-11-02 Mazda Motor Corp Method for surface-treating steel member, steel member and toothed gear

Also Published As

Publication number Publication date
JP2946972B2 (en) 1999-09-13

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