JPH0478698B2 - - Google Patents
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- Publication number
- JPH0478698B2 JPH0478698B2 JP61265611A JP26561186A JPH0478698B2 JP H0478698 B2 JPH0478698 B2 JP H0478698B2 JP 61265611 A JP61265611 A JP 61265611A JP 26561186 A JP26561186 A JP 26561186A JP H0478698 B2 JPH0478698 B2 JP H0478698B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- aluminum
- alloy
- degassing
- producing
- 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.)
- Expired - Lifetime
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Description
<産業上の利用分野>
本発明はアルミニウム(Al)系粉末よりAl系
粉末合金を得る方法に関する。
<従来の技術>
Al系粉末を含む粉末からAl合金いわゆる焼結
Al合金を製造する方法は古くから研究されてい
るが、Al粉末の表面は硬いアルミナ(酸化被覆)
で覆われているため、従来の如く、単に粉末を成
形した後融点以下の温度にて焼結する方法では十
分な強度が得られなかつた。
そこで、粉末を押出法にて固化する方法が考え
出されている。しかしながら、Al粉末の表面に
は、H2O,O2、N2等のガス(吸着ガス)が吸着
しており、押出し中の材料内において、又は固化
した後のAl合金を熱処理する段階において、又
はAl合金を高温下で使用する場合において、前
記吸着ガス特にH2OがH2Oガス又はH2ガス
(3H2O+2Al→Al2O3+3H2)として高温下で膨
張し、一般にブリスター(気泡)と呼ばれる材料
欠陥を生成させてしまう。
従つて、粉末を押出成形する場合には、H2O
の脱ガスが必要であり、従来は、真空中で加熱す
ることによりH2Oの脱ガスを行つていた。又、
加熱真空中でないと、十分なH2Oの脱ガスがで
きないと考えられていた(例えば、Advances in
Powder Technology P.194)。
加熱真空中で脱ガスを行う従来の脱ガス方法
は、成形した粉末又は粉末をそのままホツトプレ
スに入れ、高温真空下で脱ガス及び加圧成形し、
押出用ビレツトとするか、又は、缶の中に粉末成
形体又は粉末を直接投入し、缶を加熱し、真空引
きすることによつて脱ガスを行い、終了後真空封
入して押出用ビレツトとしていた。
<発明が解決しようとする問題点>
上記のようにして、押出用ビレツトなどのAl
系粉末合金を得る方法は、研究用としてはあまり
問題とはならないが、生産に際しては、プロセス
が複雑すぎる、経費がかかるなど製造上、経済上
の問題があつた。
本発明は以上のような従来の状況にかんがみて
なされたもので、ブリスターのないAl系粉末合
金を容易かつ経済的に得られるようにすることを
目的とする。
<問題点を解決するための手段及び作用>
上記目的を達成するための本発明の構成は、ア
ルミニウム系粉末を見掛け密度が真密度比で65〜
94%となるように成形し、当該粉末成形体を300
℃以上550℃以下の温度で大気中において加熱、
脱ガスを行い、塑性加工を施すことを特徴とす
る。
上記構成の各要件は以下のような考察から決定
される。
(1) 粉末成形体の密度
Al系粉末は吸着ガス特にH2Oを表面に吸着し
ている。このH2Oガスが十分粉末粒子から分離
されないと、固化後ブリスター等の材料欠陥が発
生する。
従つて、ブリスター等の材料欠陥の発生を防ぐ
ためにも粉末成形体の状態での脱ガスが必要で、
このためには、粉末成形体の見掛け密度が真密度
比で65%〜94%の範囲に調整されることが必要で
ある。密度が65%より低い場合には、粉末成形体
の強度が低く、持ち運び等の取扱い時に割れ等が
発生し、歩留りが悪く取扱いにくくなる。密度が
95%以上の場合には、粉末成形体中の空隙が外部
から閉鎖された状態となり、このまま押出時に加
熱を行うと、閉空間内のH2Oガスが膨張し、粉
末成形体を破壊する。このような閉空間が生ずる
限界が密度95%以上であり、従つて、粉末成形体
の密度は94%以下にする必要がある。
尚、より好ましくは、成形体割れや脱ガスの不
十分な状況が生じないように、70%〜90%の密度
とすることが望ましい。
(2) 粉末成形体の脱ガス条件
従来、粉末に吸着したガスの脱ガスは、熱力学
的な観点から、真空度と温度に平衡した平衡ガス
圧力を求める方法から脱ガスプロセスを予測する
のが一般的であつた(LEYBOLDHERAEUS
GMBH,Vacuum Degassing of Metal
Powders,by P.Flecher and R.Ruthardt参照)。
又、一般には、大気中では酸化が進行するた
め、大気中脱ガスは従来検討されたことがなかつ
た。
しかしながら、現実の脱ガスプロセスは、時
間の関係した速度論的な過程であり、しかも吸
着ガスのようには熱力学的に予測することのでき
ない水分を含んでおり、Al粉末は強固な酸化
被膜は還元することが困難である。しかしながら
実際に大気中加熱を行つて形成される酸化被膜の
増加はわずかである。
以上の点から大気中で脱水分(ガス)が可能で
あると考えられる。
各種粉末の温度T(K)において、脱ガスが十
分完了されたと考えられる1ppmの水蒸気量にな
るための平衡分圧(mbar)は、
P=2981√T3/exp(9562/T) (1)
で与えられる。
一方、大気中の飽和水蒸気圧は第1図に示す如
くなつている。すなわち、この図より、日本にお
いて最も高温多湿の梅雨時において、気温30℃で
相対湿度100%なら、飽和水蒸気圧は42mbarであ
り、この場合においても(1)式より408℃以上なら
粉末の水蒸気量を1ppm以下にできることがわか
る。又、冬期の温度5℃において、相対湿度が30
%なら大気中の水蒸気圧は約3mbarで、(1)式より
約320℃以上で加熱すれば粉末の水蒸気量を1ppm
以下とすることができることがわかる。
従つて、脱ガスの温度としては、300℃以上に
する必要がある。550℃以上において、粉末に吸
着している水分又は他のガスはほぼ完全に粉末粒
子から切り離されるためこれ以上にする必要はな
い。
(3) 加熱雰囲気
従来、Al粉末を大気中で加熱すると酸化被膜
が成長するため、大気中での加熱は不可と考えら
れていたが、実際に酸素量の測定をしてみると、
大気中加熱前のAl粉末の酸素量は0.15〜0.25wt%
程度であつたが、加熱後においても0.17〜0.25wt
%とほとんど変わらないことがわかつた。
従つて、大気中にて加熱脱ガスを行つても、何
ら酸化の影響は問題とはならない。しかし、大気
中には水蒸気が含まれているためH2O分圧がい
くらかあるが、N2やAr,He等の不活性ガス雰囲
気中にて脱ガスを行うと、この分圧が更に小さく
なり、より脱ガスが容易となる。
(4) 塑性加工法
粉末の塑性加工は粉末を密度100%の合金塊と
するための方法であり、一般的には押出が最も多
く用いられるが、鍛造や圧延などの採用も可能で
ある。
(5) 原料粉末
本発明で対象となるAl系粉末は、Al粉末を含
むすべての粉末、すなわち、Al粉末又はAl合金
粉末又はAl粉末とAl合金粉末との混合粉末又は
Al粉末もしくはAl合金粉末もしくはこれらの混
合粉末と他の金属粉末もしくは非金属粉末との混
合粉末である。
<実施例>
Al−20wt%Si−5wt%Fe−4wt%Cu−1wt%
MgのAl合金粉末(−100メツシユ)を約70%、
90%、96%の密度でそれぞれ成形し、できた粉末
成形体を300℃,400℃,500℃の各温度にて大気
中で7時間加熱した後、その温度にて押出比10:
1にて押出加工を行つた。
得られた押出材を500℃で加熱し、この時発生
するブリスターの有無を調査した。その結果を表
1に示す。
<Industrial Application Field> The present invention relates to a method for obtaining an Al-based powder alloy from aluminum (Al)-based powder. <Conventional technology> So-called sintering of Al alloy from powder containing Al-based powder
The method of producing Al alloys has been studied for a long time, but the surface of Al powder is hard alumina (oxidized coating).
Therefore, sufficient strength could not be obtained by the conventional method of simply molding the powder and then sintering it at a temperature below the melting point. Therefore, a method has been devised in which powder is solidified by extrusion. However, gases (adsorbed gases) such as H 2 O, O 2 and N 2 are adsorbed on the surface of Al powder, and gases such as H 2 O, O 2 and N 2 are adsorbed in the material during extrusion or during the heat treatment of the solidified Al alloy. or when Al alloy is used at high temperatures, the adsorbed gas, especially H 2 O, expands at high temperatures as H 2 O gas or H 2 gas (3H 2 O + 2Al→Al 2 O 3 + 3H 2 ), and generally forms blisters. This results in the generation of material defects called (bubbles). Therefore, when extruding powder, H 2 O
Conventionally, H 2 O was degassed by heating in a vacuum. or,
It was thought that sufficient H 2 O degassing could not be achieved without heating in a vacuum (for example, in Advances in
Powder Technology P.194). The conventional degassing method involves degassing in a heated vacuum. The molded powder or powder is put into a hot press as it is, and the powder is degassed and pressure-molded under a high-temperature vacuum.
Either make it into a billet for extrusion, or directly put the powder compact or powder into a can, heat the can, evacuate it to degas it, and then vacuum seal it after finishing to make it into a billet for extrusion. there was. <Problems to be solved by the invention> As described above, Al
The method of obtaining powder alloys does not pose much of a problem for research purposes, but when it comes to production, there are manufacturing and economic problems such as the process being too complicated and the cost being too high. The present invention was made in view of the above-mentioned conventional situation, and an object of the present invention is to make it possible to easily and economically obtain a blister-free Al-based powder alloy. <Means and effects for solving the problems> The structure of the present invention for achieving the above object is such that the aluminum powder has an apparent density of 65 to 65 as a true density ratio.
94%, and the powder compact is 300%
Heating in the atmosphere at a temperature of ℃ to 550℃,
It is characterized by degassing and plastic working. Each requirement of the above configuration is determined from the following considerations. (1) Density of powder compact Al-based powder adsorbs adsorbed gas, especially H 2 O, on its surface. If this H 2 O gas is not sufficiently separated from the powder particles, material defects such as blisters will occur after solidification. Therefore, in order to prevent material defects such as blisters, it is necessary to degas the powder compact.
For this purpose, it is necessary to adjust the apparent density of the powder compact to a true density ratio in the range of 65% to 94%. When the density is lower than 65%, the strength of the powder compact is low and cracks occur during handling such as transportation, resulting in poor yield and difficulty in handling. density is
In the case of 95% or more, the voids in the powder compact are closed from the outside, and if heating is continued during extrusion, the H 2 O gas in the closed space expands and destroys the powder compact. The limit at which such a closed space occurs is a density of 95% or more, so the density of the powder compact must be 94% or less. More preferably, the density is preferably 70% to 90% to prevent cracking of the molded product or insufficient degassing. (2) Degassing conditions for powder compacts Conventionally, degassing of gases adsorbed in powder has been done from a thermodynamic point of view by predicting the degassing process by finding the equilibrium gas pressure that is balanced with the degree of vacuum and temperature. was common (LEYBOLDHERAEUS
GMBH,Vacuum Degassing of Metal
Powders, by P. Flecher and R. Ruthardt). Furthermore, since oxidation generally progresses in the atmosphere, degassing in the atmosphere has not been considered in the past. However, the actual degassing process is a time-related kinetic process, and it also contains water, which cannot be predicted thermodynamically like adsorbed gas, and Al powder has a strong oxide film. is difficult to reduce. However, the increase in the oxide film formed by actually performing heating in the atmosphere is slight. From the above points, it is thought that dehydration (gas) is possible in the atmosphere. At the temperature T (K) of various powders, the equilibrium partial pressure (mbar) required to reach a water vapor content of 1 ppm, which is considered to be sufficient degassing, is P=2981√T 3 /exp(9562/T) (1 ) is given by On the other hand, the saturated water vapor pressure in the atmosphere is as shown in FIG. In other words, from this figure, during the rainy season, the hottest and humid season in Japan, if the temperature is 30°C and the relative humidity is 100%, the saturated water vapor pressure is 42 mbar.Even in this case, according to equation (1), if it is 408°C or higher, the water vapor in the powder is It can be seen that the amount can be reduced to 1 ppm or less. Also, at a temperature of 5℃ in winter, the relative humidity is 30℃.
%, the water vapor pressure in the atmosphere is about 3 mbar, and from equation (1), if heated above about 320°C, the amount of water vapor in the powder can be reduced to 1 ppm.
It can be seen that the following can be done. Therefore, the degassing temperature needs to be 300°C or higher. At temperatures above 550°C, moisture or other gases adsorbed on the powder are almost completely separated from the powder particles, so there is no need to increase the temperature above this temperature. (3) Heating atmosphere Conventionally, it was thought that heating Al powder in the atmosphere would cause an oxide film to grow, so heating in the atmosphere was not possible, but when we actually measured the amount of oxygen, we found that
The oxygen content of Al powder before heating in the atmosphere is 0.15-0.25wt%
Although it was only about 0.17~0.25wt after heating
It was found that there is almost no difference between % and Therefore, even if heating and degassing are performed in the atmosphere, the influence of oxidation will not be a problem. However, since the atmosphere contains water vapor, there is some partial pressure of H 2 O, but when degassing is performed in an atmosphere of inert gas such as N 2 , Ar, He, etc., this partial pressure becomes even smaller. This makes degassing easier. (4) Plastic processing method Powder plastic processing is a method for turning powder into an alloy lump with 100% density, and extrusion is generally used most often, but forging, rolling, etc. can also be used. (5) Raw material powder The Al-based powder targeted by the present invention includes all powders containing Al powder, that is, Al powder, Al alloy powder, mixed powder of Al powder and Al alloy powder, or
It is a mixed powder of Al powder, Al alloy powder, or a mixed powder of these and other metal powder or nonmetallic powder. <Example> Al-20wt%Si-5wt%Fe-4wt%Cu-1wt%
Approximately 70% Mg Al alloy powder (-100 mesh)
After molding at densities of 90% and 96%, the resulting powder compacts were heated in the air at temperatures of 300°C, 400°C, and 500°C for 7 hours, and then the extrusion ratio was 10:
Extrusion processing was performed in step 1. The obtained extruded material was heated at 500°C, and the presence or absence of blisters generated at this time was investigated. The results are shown in Table 1.
【表】
表1に示すように、真密度比が96%の場合は押
出前の加熱中に粉末成形体が割れることがあつ
た。
又、300℃加熱の場合にはどの密度のものも加
熱中に割れることはなかつたが、押出時又はその
後の短時間の500℃加熱によつてブリスターが発
生した。
しかし、400℃以上の加熱の場合には500℃,5
時間の加熱においてもブリスターは見られなかつ
た。
<発明の効果>
本発明に係るAl系粉末合金の製造方法によれ
ば、Al系粉末の脱ガスを大気圧で大気中又はN2,
Ar,He等の不活性ガス中において行うので、従
来の真空中での脱ガス処理等に比べて工程数が少
なく、設備も簡素であり、高能率で実施できるよ
うになる。
更に、このようにして得られるAl系粉末合金
は、従来方法で得られるものとほぼ同等の品質で
あり、空気中の加熱処理にもかかわらず酸化膜の
増大もなく、粉末Al合金の製造に極めて好適で
ある。[Table] As shown in Table 1, when the true density ratio was 96%, the powder compact sometimes cracked during heating before extrusion. Furthermore, when heated at 300°C, none of the densities cracked during heating, but blisters occurred during extrusion or after heating at 500°C for a short time. However, in the case of heating over 400℃, 500℃, 5
No blisters were observed even after heating for hours. <Effects of the Invention> According to the method for producing an Al-based powder alloy according to the present invention, the Al-based powder is degassed in the air at atmospheric pressure or in N 2 ,
Since it is carried out in an inert gas such as Ar or He, the number of steps is fewer than conventional degassing treatment in vacuum, etc., the equipment is simple, and it can be carried out with high efficiency. Furthermore, the Al-based powder alloy obtained in this way has almost the same quality as that obtained by conventional methods, and there is no increase in oxide film despite heat treatment in air, making it suitable for producing powdered Al alloy. Very suitable.
第1図は温度と大気中の飽和水蒸気圧との関係
を示すグラフである。
FIG. 1 is a graph showing the relationship between temperature and saturated water vapor pressure in the atmosphere.
Claims (1)
で65〜94%となるように成形し、当該粉末成形体
を300℃以上550℃以下の温度で大気中において加
熱、脱ガスを行い、塑性加工を施すことを特徴と
するアルミニウム系粉末合金の製造方法。 2 粉末成形体の見掛け密度が真密度比で70〜90
%である特許請求の範囲第1項に記載のアルミニ
ウム系粉末合金の製造方法。 3 脱ガス雰囲気ガスとしてN2ガス又はAr,He
等の不活性ガスを用いる特許請求の範囲第1項又
は第2項に記載のアルミニウム系粉末合金の製造
方法。 4 アルミニウム系粉末として、アルミニウム粉
末又はアルミニウム合金粉末又はアルミニウム粉
末とアルミニウム合金粉末との混合粉末又はアル
ミニウム粉末もしくはアルミニウム合金粉末もし
くはこれらの混合粉末と他の金属粉末もしくは非
金属粉末との混合粉末を用いる特許請求の範囲第
1項ないし第3項のいずれかに記載のアルミニウ
ム系粉末合金の製造方法。 5 塑性加工方法として、押出、鍛造、圧延を用
いる特許請求の範囲第1項ないし第4項のいずれ
かに記載のアルミニウム系粉末合金の製造方法。[Scope of Claims] 1. Shaped so that the apparent density of aluminum-based powder is 65 to 94% of the true density ratio, and the powder compact is heated in the air at a temperature of 300°C or higher and 550°C or lower to degas it. A method for producing an aluminum-based powder alloy, which comprises performing plastic working. 2 The apparent density of the powder compact is 70 to 90 in terms of true density ratio.
% of the aluminum-based powder alloy according to claim 1. 3 N2 gas or Ar, He as degassing atmosphere gas
A method for producing an aluminum-based powder alloy according to claim 1 or 2, using an inert gas such as 4 As the aluminum-based powder, use aluminum powder, aluminum alloy powder, mixed powder of aluminum powder and aluminum alloy powder, or mixed powder of aluminum powder or aluminum alloy powder, or mixed powder of these and other metal powder or non-metallic powder. A method for producing an aluminum-based powder alloy according to any one of claims 1 to 3. 5. The method for producing an aluminum-based powder alloy according to any one of claims 1 to 4, using extrusion, forging, and rolling as the plastic working method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26561186A JPS63121628A (en) | 1986-11-10 | 1986-11-10 | Manufacture of aluminum alloy powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26561186A JPS63121628A (en) | 1986-11-10 | 1986-11-10 | Manufacture of aluminum alloy powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63121628A JPS63121628A (en) | 1988-05-25 |
| JPH0478698B2 true JPH0478698B2 (en) | 1992-12-11 |
Family
ID=17419538
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26561186A Granted JPS63121628A (en) | 1986-11-10 | 1986-11-10 | Manufacture of aluminum alloy powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63121628A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2693181B2 (en) * | 1988-08-18 | 1997-12-24 | 昭和アルミニウム株式会社 | Aluminum brazing sheet |
| DE69225469T2 (en) * | 1991-11-22 | 1998-09-24 | Sumitomo Electric Industries | METHOD FOR DEGASSING AND FIXING ALUMINUM ALLOY POWDER |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5597447A (en) * | 1979-01-19 | 1980-07-24 | Sumitomo Electric Ind Ltd | Aluminum sintered alloy and production of the same |
| JPS5835562A (en) * | 1981-08-26 | 1983-03-02 | Fuji Xerox Co Ltd | Message information recording device |
| JPS6015687A (en) * | 1983-07-08 | 1985-01-26 | 日本電気株式会社 | Display |
| JPH0643628B2 (en) * | 1986-08-29 | 1994-06-08 | 三菱マテリアル株式会社 | Method for manufacturing aluminum alloy member |
-
1986
- 1986-11-10 JP JP26561186A patent/JPS63121628A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63121628A (en) | 1988-05-25 |
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