JPS6148566B2 - - Google Patents
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- Publication number
- JPS6148566B2 JPS6148566B2 JP5007580A JP5007580A JPS6148566B2 JP S6148566 B2 JPS6148566 B2 JP S6148566B2 JP 5007580 A JP5007580 A JP 5007580A JP 5007580 A JP5007580 A JP 5007580A JP S6148566 B2 JPS6148566 B2 JP S6148566B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- base
- base powder
- pressure
- alloy
- 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
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- 239000000843 powder Substances 0.000 claims description 170
- 238000005245 sintering Methods 0.000 claims description 38
- 238000002844 melting Methods 0.000 claims description 24
- 230000008018 melting Effects 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 22
- 229910000838 Al alloy Inorganic materials 0.000 claims description 21
- 230000005496 eutectics Effects 0.000 claims description 20
- 229910045601 alloy Inorganic materials 0.000 claims description 16
- 239000007791 liquid phase Substances 0.000 claims description 16
- 239000000956 alloy Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 5
- 150000002739 metals Chemical class 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 239000010949 copper Substances 0.000 description 15
- 239000011812 mixed powder Substances 0.000 description 14
- 238000003825 pressing Methods 0.000 description 14
- 229910018182 Al—Cu Inorganic materials 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 238000000465 moulding Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 229910000881 Cu alloy Inorganic materials 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000007423 decrease Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910018507 Al—Ni Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006023 eutectic alloy Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- -1 θ+L Alternatively Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Filtering Materials (AREA)
Description
本発明はAl若しくはAl合金の多孔質焼結体の
製造方法に係り、詳しくは、実質的にAlからな
るベース粉と、このベース粉の融点以下で、ベー
ス粉との間で共晶反応を生成して溶融し、共晶温
度がベース粉末以下である金属粉またはベース粉
末の融点以下で一部に液相に生成するAl合金粉
とを混合した混合粉を無加圧で所望形状に成型し
てから、焼結時に圧力をかけて焼結し、機械的強
度に優れる多孔質焼結体を製造する方法に係る。
従来から、多孔質焼結体、なかでも、銅焼結体
が液体等のフイルタとして用いられていたが、最
近は、無数の連通孔に着目し、吸音材としての用
途も開発されている。すなわち、多孔質焼結体で
は、隣接粉粒子の間に孔隙が形成され、この孔隙
が連続的に連なりかつ無限に屈曲しているため
に、そこに、音波が通過すると、エネルギーの大
部分を失なつて吸音される。また銅粉は高価であ
り、多孔質焼結体は非常に重くなるため、Al粉
やその合金粉から成る多孔質焼結体が望まれてい
るが、Al粉やその合金粉（以下、単にAl粉等と
いう。）から製造することはきわめてむづかしい
と云われている。この理由は、Al粉等の表面
は、Al2O3の難還元性の酸化皮膜でおおわれてい
るために、成型時に圧力を加えないと、焼結時
に、内部のAlや、Al合金が接触することなく、
焼結反応は進行しないからである。
この点からAl粉等であると、孔隙率35％以上
を有し、フイルタや吸音材等に好適な連通孔を具
える多孔質焼結体を製造することは困難である。
このため、本発明者等は孔隙率の大きいAl粉
等の多孔質焼結体製造法について研究し、先に、
Al粉等から成るベース粉に対して、そのベース
粉の融点より低い融点を有する低融点Al合金粉
を混合し、この混合粉を無加圧状態で成型し、そ
の成型体をそのまま低融点Al合金粉の融点以上
の温度で焼結し多孔質焼結体を製造する方法を提
案した。
この方法は成型時ならびに焼結時に圧力をかけ
ないため、孔隙率が30％以上保持でき、成型時に
Al粉等の酸化皮膜を機械的に破壊できなくとも
焼結時に局部的に破壊するとともに、低融点Al
合金からの液相によつて結合でき、孔隙率の高い
焼結体を製造するのには好適な方法である。
しかし、この方法では、酸化皮膜の破壊は焼結
時の昇温によつて表面の酸化皮膜と内部のAlと
で膨脹度合が相違することを利用して行なうので
あつて、破壊の程度が小さく、低融点のAl合金
粉の液相が作用するときに、この酸化皮膜が障害
になつて焼結性が向上せず大きな機械的強度が得
られない。
このところから、上記欠点を解決するものとし
て本発明は完成したのであつて、具体的には、本
発明は、Al粉等から成るベース粉に対し、焼結
時に適正範囲の圧力をかけると、クリープ現象に
よつてベース粉内部のAl基地が変形し、この変
形によつて表面の酸化皮膜が大きく破壊して焼結
性が向上することを利用して焼結する方法であ
る。
以下、本発明方法について詳しく説明する。
まず、ベース粉はAl粉等、つまり、実質的に
Alから成るAl粉末若しくはAlを含むAl合金粉末
の何れか一方または双方とする。このベース粉に
対して以下の粉末を混合する。
(1) ベース粉の融点以下で少なくとも一部に液相
が生成する組成のAl合金粉
(2) ベース粉中のAl基地との間で共晶反応を示
して溶融する際の共晶温度がベース粉の融点よ
り低い金属の粉末若しくはその金属を含む合金
粉末
すなわち、ベース粉に対し、(1)若しくは(2)粉末
または(1)ならびに(2)の粉末を混合する。この混合
において、添加粉末の組成や添加量はベース粉の
組成、配合量ならびに融点と関連して定められて
いる。例えば、ベース粉として実質的にAlから
成るAl粉末若しくはCuを含むAl−Cu合金粉末を
用いるときには、(1)の粉末としては、これらAl
粉末やAl−Cu粉末のベース粉融点以下において
一部に液相を生成する組成のAl合金粉末を添加
配合する。例えば、このAl合金粉末としてAl−
Cu合金粉末を配合するときには、第１図に示す
Al−Cu系状態図から定める。つまり、ベース粉
が実質的にAlから成るときには、その融点が660
℃であるから、660℃以下で部分的に液相が生成
するAl−Cu合金粉末を配合する。この合金粉末
を第１図から求めると、Cu約45％以上を含むAl
−Cu合金粉末であつても、例えば、70％Cu−30
％Al粉末の融点はベース粉融点より高いが、591
℃以上ではη１＋Ｌの如く、一部には液相Ｌが生
成し、626℃以上でもε２＋Ｌの如く、一部に液
相Ｌが安定して存在する。また、Cu45％以下を
含むAl−Cu合金粉末でも、548℃以上ではθ＋Ｌ
またはＫ＋Ｌの如く、一部に液相Ｌが生成する。
従つて、この組成のAl−Cu合金粉末を混合
し、例えば、660〜591℃または660〜548℃で焼結
すると、安定して部分的に液相が生成できる。な
お、Cu45％以下を含むAl−Cu合金の粉末を添加
するときには、この粉末はAlから成るベース粉
の融点より低いため、その混合率を調整し、孔隙
率を適正範囲に保つ必要がある。
また、(1)の粉末のかわりに、または(1)の粉末と
ともに(2)の粉末を添加するときには、ベース粉の
Al基地との間で共晶反応を考慮し、例えば、第
１表に示す共晶組成ならびに共晶温度との関連か
ら金属粉末や合金粉末の添加量を定めて添加す
る。このように(2)の粉末を添加すると、第１表か
ら明らかな通り、ベース粉が実質的にAlから成
るときは、その融点以下で各種の共晶合金が生成
し、この合金が焼結時に安定した液相として存在
する。
The present invention relates to a method for producing a porous sintered body of Al or Al alloy, and more specifically, a eutectic reaction is carried out between a base powder consisting essentially of Al and the base powder at a temperature below the melting point of the base powder. A mixed powder that is formed and melted and mixed with a metal powder whose eutectic temperature is below the base powder or an Al alloy powder that partially forms in a liquid phase below the melting point of the base powder is molded into the desired shape without pressure. The present invention relates to a method of manufacturing a porous sintered body having excellent mechanical strength by applying pressure during sintering. Traditionally, porous sintered bodies, especially copper sintered bodies, have been used as filters for liquids, etc., but recently, attention has been focused on the countless communicating pores, and their use as sound absorbing materials has also been developed. In other words, in a porous sintered body, pores are formed between adjacent powder particles, and since these pores are continuously connected and infinitely curved, when a sound wave passes through them, most of the energy is absorbed. The sound is lost and absorbed. In addition, copper powder is expensive and porous sintered bodies are very heavy, so porous sintered bodies made of Al powder or its alloy powder are desired. It is said to be extremely difficult to manufacture from Al powder, etc.). The reason for this is that the surface of Al powder, etc. is covered with a hard-to-reducible oxide film of Al 2 O 3 , so if pressure is not applied during molding, the internal Al and Al alloys will come into contact during sintering. without doing,
This is because the sintering reaction does not proceed. From this point of view, when using Al powder or the like, it is difficult to produce a porous sintered body having a porosity of 35% or more and having communicating pores suitable for filters, sound absorbing materials, and the like. For this reason, the present inventors researched methods for producing porous sintered bodies such as Al powder with high porosity, and first
A low melting point Al alloy powder having a melting point lower than that of the base powder is mixed with a base powder made of Al powder, etc., this mixed powder is molded without pressure, and the molded body is directly made of low melting point Al alloy powder. We proposed a method for manufacturing porous sintered bodies by sintering at temperatures above the melting point of alloy powder. Since this method does not apply pressure during molding and sintering, it is possible to maintain a porosity of 30% or more, and during molding.
Even if the oxide film of Al powder etc. cannot be destroyed mechanically, it can be locally destroyed during sintering, and the low melting point Al
This method is suitable for producing a sintered body with high porosity, which can be bonded by a liquid phase from the alloy. However, in this method, the oxide film is destroyed by taking advantage of the difference in the degree of expansion between the surface oxide film and the internal Al due to the temperature rise during sintering, and the degree of destruction is small. When the liquid phase of the low-melting-point Al alloy powder acts on the material, this oxide film becomes an obstacle, and the sinterability does not improve, making it impossible to obtain large mechanical strength. From this point, the present invention was completed to solve the above-mentioned drawbacks. Specifically, the present invention proposes that when a suitable range of pressure is applied to a base powder made of Al powder etc. during sintering, This sintering method takes advantage of the fact that the Al base inside the base powder is deformed due to the creep phenomenon, and this deformation greatly destroys the oxide film on the surface, improving sinterability. The method of the present invention will be explained in detail below. First, the base powder is Al powder, etc., that is, it is essentially
Either or both of Al powder consisting of Al and Al alloy powder containing Al. Mix the following powders with this base powder. (1) Al alloy powder with a composition that at least partially forms a liquid phase below the melting point of the base powder. (2) The eutectic temperature at which a eutectic reaction occurs with the Al base in the base powder and melts. A metal powder having a melting point lower than that of the base powder or an alloy powder containing the metal. That is, the base powder is mixed with the powders (1) or (2) or the powders (1) and (2). In this mixing, the composition and amount of the added powder are determined in relation to the composition, amount, and melting point of the base powder. For example, when using an Al powder consisting essentially of Al or an Al-Cu alloy powder containing Cu as the base powder, the powder (1) is
Al alloy powder having a composition that partially forms a liquid phase below the base melting point of the powder or Al-Cu powder is added and blended. For example, as this Al alloy powder, Al-
When blending Cu alloy powder, as shown in Figure 1.
Determined from the Al-Cu system phase diagram. In other words, when the base powder consists essentially of Al, its melting point is 660
Since the temperature is 660°C or lower, an Al-Cu alloy powder that partially forms a liquid phase is blended. When this alloy powder is determined from Figure 1, it is found that Al containing about 45% or more of Cu
-Cu alloy powder, for example, 70% Cu-30
The melting point of %Al powder is higher than the base powder melting point, but 591
At temperatures above 0.degree. C., a liquid phase L is generated in a portion, as shown in η 1 +L, and even at temperatures above 626° C., a liquid phase L is stably present in some portions, as shown in ε 2 +L. In addition, even for Al-Cu alloy powder containing 45% or less of Cu, θ+L
Alternatively, liquid phase L is partially generated, such as K+L. Therefore, when Al--Cu alloy powder having this composition is mixed and sintered at, for example, 660 to 591°C or 660 to 548°C, a liquid phase can be stably generated partially. Note that when adding Al-Cu alloy powder containing 45% or less of Cu, this powder has a melting point lower than the base powder made of Al, so it is necessary to adjust the mixing ratio and maintain the porosity within an appropriate range. Also, when adding powder (2) instead of powder (1) or together with powder (1), the base powder
Taking into account the eutectic reaction with the Al base, the amount of metal powder or alloy powder to be added is determined and added in relation to the eutectic composition and eutectic temperature shown in Table 1, for example. When powder (2) is added in this way, as is clear from Table 1, when the base powder consists essentially of Al, various eutectic alloys are formed below its melting point, and this alloy is sintered. Sometimes exists as a stable liquid phase.
【表】
次に、混合粉は圧力を加えることなく、所望の
形状に成型するが、焼結時には各ベース粉に対し
適正な圧力をかけて真空若しくは非酸化性雰囲気
中で焼結する。
この際の焼結温度はベース粉の融点より低い
が、(1)の粉末のみを添加したときは、そのAl合
金粉末の一部に液相が生成する温度以上であり、
(2)の粉末を添加したときには、ベース粉のAl基
地との間で共晶反応により溶融する温度、つま
り、共晶温度以上である。
また、焼結時の加圧力は、焼結温度でクリープ
現象によりベース粉が変形する程度であつて、加
圧力は本質的には焼結温度と関連して定められ
る。しかしながら、焼結温度の上限はベース粉の
融点であるから、工業的には600℃内外で焼結す
ることが多く、焼結温度600℃のベース粉の極限
強さが600ｇ/cm2〜70ｇ/cm2程度であるため、各ベ
ース粉末粒子に対して60ｇ/cm2以上の加圧力が加
えられる程度、なかでも、100〜1000Kg/cm2程度か
かるよう加圧する。
すなわち、Al若しくはその合金から成るベー
ス粉のクリープ現象におけるベース粉の極限強さ
と歪速度との関係を求めると、第２図に示す通り
であつて、第２図に示す如く、歪速度の上昇によ
つてベース粉の極限強さが上昇するのに反し、焼
結温度の上昇とともにベース粉の極限強さは低下
する。そこで、焼結時間を30分とし、焼結温度
600℃としたときは、ベース粉の極限強さは60〜
70ｇ/cm2程度であつて、これ以上の加圧力を加え
ると、ベース粉はクリープにより大巾に変形す
る。しかし、加圧力があまり大きいと、変形は大
きくなり焼結性は向上するが、孔隙率が低下し、
良好な吸音特性を示さない。このために、加圧力
の上限は1000ｇ/cm2程度が好ましい。
なお、上記の如く無加圧成型ならびに加圧焼結
を行なう場合、通常、混合粉と反応しない容器や
板、例えば、黒鉛容器、黒鉛板等を用いるのが好
ましい。すなわち、黒鉛容器の中に混合粉を散布
し、所要形状に成型し、焼結時には黒鉛容器中の
混合粉上に重りをおいて加圧する。このように成
型、焼結すると、各ベース粉上の酸化皮膜には無
数に近く割れ目が生じ、焼結が進行して、孔隙率
が高く、機械的強度に優れる多孔質焼結体が得ら
れる。
そこで、上記の如き本発明法の特徴を説明する
ために、更に詳しく焼結機構を説明すると、次の
通りである。
一般に、Al粉等のベース粉の表面は硬い酸化
皮膜におおわれているが、成型時に圧力を加えな
くとも、ベース粉の融点以下で(1)や(2)の粉末が部
分的に溶融し、この液相が、熱膨脹率の差によつ
て生成する酸化皮膜の亀裂から内部のAl基地が
露出したところに作用する。しかし、このように
熱膨脹率の差に起因する亀裂は小さく、焼結雰囲
気中に僅かでも酸素が存在すると、この酸素は破
壊部分に作用し、きわめて瞬間的に内部の露出部
分がただちに酸化されて、露出部分が封鎖され、
焼結の進行に支障が生じる。
これに対し、本発明方法においては、加圧状態
で焼結するために、ベース粉表面の酸化皮膜は従
来例の如く、静的な膨脹係数の差によつて亀裂を
発生させるほか、ベース粉内部のAl基地のクリ
ープ現象による伸びや変形によつて厚さ100〜500
Å程度の酸化皮膜は動的に破壊し、この動的破壊
によつて大きな亀裂を発生させて焼結性を大巾に
向上させる。
例えば、平均粒径175μ程度のベース粉１（実
質的にAlから成るもの）に、平均粒径74μ程度
の添加粉末２（ベース粉のAlと共晶組成で溶融
するもの、つまりNiから成る粉末）を混合す
る。混合物を無加圧で成型すると、第３図に示す
通り、ベース粉１の表面は酸化皮膜３におおわ
れ、この構造のベース粉１の間に小径の添加粉末
２が介在する。成型後、そのままの状態で焼結す
ると、酸化皮膜３は膨脹係数の差により破壊し、
この部分を通じて添加粉末２が作用してAl−Ni
の共晶組成で溶融するが、この破壊部分はきわめ
て小さい。これに対し、焼結時に加圧すると、第
４図に示す如く、ベース粉１の内部はクリープ現
象により変形し、この変形によつて酸化皮膜３が
動的に破壊するために、破壊部分がきわめて大き
くなり、添加粉末２の拡散が促進され、Al−Ni
の共晶反応により良好に焼結する。
なお、添加粉末として(2)の粉末を添加するとき
に、この粉末としては第１表に示す金属の粉末ま
たはこれら金属を含む合金の粉末を添加するが、
この中でCu粉末またはCu合金粉末を添加すると
きには、更に、Cr、Ti、Sb、Co、Se、Sn、Zn、
Mn等の成分を添加して耐食性の劣化を防止する
ことができる。
すなわち、ベース粉に対し２の粉末としてNi
粉とCu粉とを混合すると、焼結時に温度548℃で
CuとAlとが共晶反応を起して溶融し、その後、
温度640℃でNiとAlとが溶融してβ＋Ｌとα＋Ｌ
の共晶系から液相Ｌが発生する。この場合、Al
−Niの共晶組織は、ベース粉の結合部にのみと
どまるが、Al−Cuの共晶組織以上のCuはベース
粉のAl基地の粒界に沿つて入り、Cu若しくは金
属間化合物として析出し、結晶粒界に沿つて腐食
が進行し、耐食性が劣化する。しかし耐食性向上
成分としてCr、Ti、Sb、Co、Se、Sn、Zn若しく
はMnのうちの１種若しくは２種以上を添加する
と、ベース粉のAl基地の結晶粒界にこれら成分
が核になつて析出し、その表面にCuを吸収し、
これによつて結晶粒界に沿つて析出するCuは分
断されて腐食は進行しない。
また、焼結時に雰囲気を上記の如く真空若しく
は非酸化性に保持するのは、膨脹係数の差や、ク
リープ現象によつて発生する酸化皮膜の割れ目を
保持するためである。
また、焼結時にベース粉の各粉末粒子に対する
加圧力を60ｇ/cm2以上にするのは、30分間程度加
圧力をかけるときには、第２図に示す如く、600
℃で30分の歪速度では極限強さが60ｇ/cm2程度で
あつて、これ以下ではクリープ現象により変形が
生じないからである。
次に、実施例について説明する。
実施例 １
まず、平均粒度50メツシユの実質的にAlから
成るベース粉79wt％に対し、平均粒度200メツシ
ユのNi粉２重量部ならびに同粒度のCu粉1wt％を
混合した。この混合粉をセラミツク容器中に圧力
をかけることなく散布して充填し、容器に収容さ
れているままで板状体を成型した。
次に、この容器に入れたままで露点−40℃附近
に調整したH2ガス雰囲気中で30分間焼結した。
このときに容器の混合粉の上に重りをのせて、こ
の重りの重量を変化させて、ベース粉の各粒子当
りの加圧力が０〜７×10ｇ/cm2の如く変化させ、
加圧焼結後は、大気中で徐冷し、各焼結体につい
て、気孔率ならびに機械的性質（引張強度）を求
めたところ、第２表の通りであつた。[Table] Next, the mixed powder is molded into the desired shape without applying pressure, but during sintering, appropriate pressure is applied to each base powder and sintered in a vacuum or non-oxidizing atmosphere. The sintering temperature at this time is lower than the melting point of the base powder, but when only the powder (1) is added, it is above the temperature at which a liquid phase forms in a part of the Al alloy powder.
When the powder (2) is added, the temperature is higher than the temperature at which it melts due to a eutectic reaction with the Al base of the base powder, that is, the eutectic temperature. Further, the pressurizing force during sintering is such that the base powder is deformed due to the creep phenomenon at the sintering temperature, and the pressurizing force is essentially determined in relation to the sintering temperature. However, since the upper limit of the sintering temperature is the melting point of the base powder, industrially it is often sintered at around 600℃, and the ultimate strength of the base powder at a sintering temperature of 600℃ is 600g/cm 2 ~ 70g. /cm 2 , the pressure is applied to each base powder particle to the extent that a pressure of 60 g/cm 2 or more is applied, particularly about 100 to 1000 Kg/cm 2 . In other words, the relationship between the ultimate strength of the base powder and the strain rate in the creep phenomenon of base powder made of Al or its alloy is as shown in Figure 2. The ultimate strength of the base powder increases as the sintering temperature increases, whereas the ultimate strength of the base powder decreases as the sintering temperature increases. Therefore, the sintering time was set to 30 minutes, and the sintering temperature was
When the temperature is 600℃, the ultimate strength of the base powder is 60~
The pressure is approximately 70 g/cm 2 , and if a pressure greater than this is applied, the base powder will be significantly deformed due to creep. However, if the applied pressure is too large, the deformation will be large and the sinterability will improve, but the porosity will decrease.
Does not exhibit good sound absorption properties. For this reason, the upper limit of the pressing force is preferably about 1000 g/cm 2 . In addition, when performing pressureless molding and pressure sintering as described above, it is usually preferable to use a container or plate that does not react with the mixed powder, such as a graphite container or a graphite plate. That is, the mixed powder is spread in a graphite container, molded into a desired shape, and during sintering, a weight is placed on the mixed powder in the graphite container and pressurized. When molded and sintered in this way, nearly countless cracks occur in the oxide film on each base powder, and sintering progresses, resulting in a porous sintered body with high porosity and excellent mechanical strength. . Therefore, in order to explain the features of the method of the present invention as described above, the sintering mechanism will be explained in more detail as follows. Generally, the surface of base powder such as Al powder is covered with a hard oxide film, but powders (1) and (2) partially melt below the melting point of the base powder without applying pressure during molding. This liquid phase acts on the areas where the internal Al base is exposed through cracks in the oxide film that are generated due to the difference in coefficient of thermal expansion. However, the cracks caused by this difference in coefficient of thermal expansion are small, and if there is even a small amount of oxygen in the sintering atmosphere, this oxygen will act on the fractured part, and the exposed internal part will be immediately oxidized very instantaneously. , the exposed part is sealed off,
This will hinder the progress of sintering. In contrast, in the method of the present invention, since sintering is carried out under pressure, the oxide film on the surface of the base powder not only cracks due to the difference in static expansion coefficients, but also The thickness varies from 100 to 500 due to elongation and deformation due to the creep phenomenon of the internal Al base.
The oxide film having a thickness of approximately Å is dynamically destroyed, and this dynamic destruction generates large cracks and greatly improves sinterability. For example, base powder 1 (substantially made of Al) with an average particle size of about 175μ is added to additive powder 2 (made of Ni, which melts in a eutectic composition with Al in the base powder, with an average particle size of about 74μ). ) to mix. When the mixture is molded without pressure, the surface of the base powder 1 is covered with an oxide film 3 as shown in FIG. 3, and the small diameter additive powder 2 is interposed between the base powder 1 having this structure. If the oxide film 3 is sintered in that state after molding, it will be destroyed due to the difference in expansion coefficient.
Through this part, the additive powder 2 acts and the Al-Ni
It melts with a eutectic composition of , but the fractured portion is extremely small. On the other hand, when pressure is applied during sintering, the inside of the base powder 1 deforms due to the creep phenomenon as shown in FIG. 4, and this deformation dynamically destroys the oxide film 3, so that the destroyed part becomes extremely large, promoting the diffusion of additive powder 2, and Al-Ni
Good sintering due to eutectic reaction. When adding the powder (2) as the additive powder, the powder is a powder of the metals shown in Table 1 or a powder of an alloy containing these metals.
When adding Cu powder or Cu alloy powder, Cr, Ti, Sb, Co, Se, Sn, Zn,
Deterioration of corrosion resistance can be prevented by adding components such as Mn. In other words, Ni is added as the second powder to the base powder.
When powder and Cu powder are mixed, the temperature is 548℃ during sintering.
Cu and Al undergo a eutectic reaction and melt, and then
Ni and Al melt at a temperature of 640℃ to form β+L and α+L.
A liquid phase L is generated from the eutectic system. In this case, Al
-The eutectic structure of Ni remains only in the joints of the base powder, but the Cu, which is higher than the eutectic structure of Al-Cu, enters along the grain boundaries of the Al base of the base powder and precipitates as Cu or intermetallic compounds. , corrosion progresses along grain boundaries and corrosion resistance deteriorates. However, when one or more of Cr, Ti, Sb, Co, Se, Sn, Zn, or Mn is added as a corrosion resistance improving component, these components become nuclei at the grain boundaries of the Al base of the base powder. It precipitates and absorbs Cu on its surface,
As a result, the Cu precipitated along the grain boundaries is divided and corrosion does not progress. Furthermore, the reason why the atmosphere is maintained in a vacuum or non-oxidizing state as described above during sintering is to maintain cracks in the oxide film that occur due to differences in expansion coefficients and creep phenomena. In addition, the pressing force applied to each powder particle of the base powder during sintering must be 60 g/cm 2 or more when applying the pressing force for about 30 minutes, as shown in Figure 2.
This is because at a strain rate of 30 minutes at ℃, the ultimate strength is about 60 g/cm 2 , and below this, no deformation occurs due to the creep phenomenon. Next, examples will be described. Example 1 First, 2 parts by weight of Ni powder with an average particle size of 200 mesh and 1 wt% of Cu powder with the same particle size were mixed with 79 wt% of a base powder consisting essentially of Al with an average particle size of 50 mesh. This mixed powder was spread and filled into a ceramic container without applying pressure, and a plate-shaped body was molded while it was still housed in the container. Next, the material was sintered for 30 minutes in an H2 gas atmosphere whose dew point was adjusted to around -40° C. while it was kept in this container.
At this time, a weight is placed on top of the mixed powder in the container, and the weight of this weight is changed to change the pressing force per each particle of the base powder from 0 to 7 x 10 g/cm 2 ,
After pressure sintering, the sintered bodies were slowly cooled in the atmosphere, and the porosity and mechanical properties (tensile strength) of each sintered body were determined as shown in Table 2.
【表】【table】
【表】
第２表から、焼結時の加圧力が70ｇ/cm2では伸
びも十分にあり、引張強度が大きく、ベース粉の
クリープによる変形が観察できた。これに反し、
加圧力が60ｇ/cm2より低下すると、ほとんどクリ
ープによる変形がみられず、機械的性質は大巾に
低下し、加圧力０、２、５ｇ/cm2のときには引張
強度が大巾に低下していた。
また、加圧力を70ｇ/cm2から更に増加させたと
ころ、ある程度機械的性質が向上したが、1000
ｇ/cm2以上では通水性が低下し、連通孔が少な
く、孔隙率が30％以下の如く大巾に低下している
ことがわかつた。
実施例 ２
まず、平均粒度50メツシユの実質的にAlから
成べるベース粉87wt％対し、50％Cu−50％Al合
金粉（平均粒度200メツシユ）8wt％を配合する
と共に、Cr粉（平均粒度200メツシユ以下）1wt
％を配合し、これらを混合した。これら混合粉を
黒鉛容器中に散布充填し、板状のものとして形型
した。
次に、この容器の混合粉の上に重りをのせて、
この重りによつてベース粉の各粒子に対し、0.51
×103ｇ/cm2の加圧力をかけて、露点−40℃附近に
調整されたH2ガス雰囲気中で、温度645℃±３℃
×30分の条件で焼結した。
この多孔質焼結体の性質を験べたところ、孔隙
率は約38％であり、通水試験の結果良好であり、
引張強度は3.1Kg/mm2であり、きわめて良好であつ
た。
また、比較のために、上記の通りに配合した混
合粉を板状に成型したものを加圧せずにそのまま
焼結し、これを比較例１とした。
更に、実質的にAlから成るベース粉（平均粒
度50メツシユ）84wt％と50％Al−50％Cu合金粉
（平均粒度200メツシユ）12wt％とを混合し、こ
れを上記のところを同じ加圧力を加えて焼結し、
これを比較例２とした。この比較例２は本発明に
係るものであつて、比較例２は上記の本発明に係
るものと同等の通水性ならびに機械強度を示し
た。
次に、これら３種の多孔質焼結体について、
JIS Ｚ−2371に示される通り、5wt％の塩水を用
いて塩水噴霧試験を行ない、とくに、この試験に
おいて耐食、耐候性は各多孔質体の連通孔が粒界
腐食によつて簡単に割れてしまうまでの時間で比
較した。この結果、比較例２はCu粒界析出が連
続化することもあつて、20時間程度である。これ
に対し、比較例１は無加圧焼結のこともあつて
Cuの析出の程度が小さく、約120程度に高くなつ
ているが、上記の本発明に係るものは約150時間
以上向上した。
実施例 ３
実質的Al粉より成つて平均粒度80メツシユの
ベース粉91wt％に対して、60％Cu−40％Al合金
粉（平均粒度150メツシユ）7wt％ならびにNi粉
（平均粒度200メツシユ）5wt％を混合し、これら
の混合粉を黒鉛容器中に圧力をかけることなく散
布充填し、板状のものに成型した。この容器に散
布したままで、混合粉の上に重りをのせてベース
粉の各粉末粒子に60ｇ/cm2の加圧力がかかるよう
に加圧し、露点−45℃、温度645℃、30分の焼結
を行なつた。この多孔質焼結体は気孔率は42％で
あり、引張強度も1.5Kg/mm2であつた。[Table] From Table 2, when the pressing force during sintering was 70 g/cm 2 , there was sufficient elongation, high tensile strength, and deformation due to creep of the base powder was observed. On the contrary,
When the applied force is lower than 60 g/cm 2 , almost no deformation due to creep is observed, and the mechanical properties are drastically reduced, and when the applied force is 0, 2, and 5 g/cm 2 , the tensile strength is significantly reduced. was. In addition, when the pressing force was further increased from 70 g/cm 2 , the mechanical properties improved to some extent, but at 1000 g/cm 2
It was found that when it exceeds g/cm 2 , the water permeability decreases, the number of communicating pores decreases, and the porosity significantly decreases to 30% or less. Example 2 First, 87 wt% of a base powder consisting essentially of Al with an average particle size of 50 mesh is blended with 8 wt% of 50% Cu-50% Al alloy powder (average particle size of 200 mesh), and Cr powder (average Particle size 200 mesh or less) 1wt
% and mixed them. These mixed powders were scattered and filled into a graphite container and shaped into a plate. Next, place a weight on top of the mixed powder in this container,
This weight gives a weight of 0.51 to each particle of base flour.
A pressure of ×10 3 g/cm 2 was applied, and the temperature was 645°C ± 3°C in an H 2 gas atmosphere whose dew point was adjusted to around -40°C.
Sintering was performed under the conditions of ×30 minutes. When we tested the properties of this porous sintered body, the porosity was approximately 38%, and the results of the water flow test were good.
The tensile strength was 3.1Kg/mm 2 , which was extremely good. For comparison, a mixed powder blended as described above was molded into a plate shape and sintered as it was without applying pressure, and this was designated as Comparative Example 1. Furthermore, 84 wt% of base powder (average particle size: 50 mesh) consisting essentially of Al and 12 wt% of 50% Al-50% Cu alloy powder (average particle size: 200 mesh) were mixed, and this was applied under the same pressure as above. sintered by adding
This was designated as Comparative Example 2. Comparative Example 2 is according to the present invention, and exhibited water permeability and mechanical strength equivalent to those according to the present invention. Next, regarding these three types of porous sintered bodies,
As shown in JIS Z-2371, a salt spray test was conducted using 5wt% salt water. In particular, in this test, the corrosion resistance and weather resistance were determined because the communicating pores of each porous body were easily cracked due to intergranular corrosion. We compared the time it took to put them away. As a result, in Comparative Example 2, the time was about 20 hours, partly because Cu grain boundary precipitation was continuous. On the other hand, Comparative Example 1 also involved pressureless sintering.
Although the degree of Cu precipitation is small and is high at about 120 hours, the above-mentioned one according to the present invention improved by about 150 hours or more. Example 3 60% Cu-40% Al alloy powder (average particle size 150 mesh) 7wt% and Ni powder (average particle size 200 mesh) 5wt% to 91wt% base powder consisting essentially of Al powder with average particle size 80 mesh. %, and these mixed powders were scattered and filled into a graphite container without applying pressure, and molded into a plate. While the powder was being scattered in this container, a weight was placed on top of the mixed powder to apply pressure of 60 g/cm 2 to each powder particle of the base powder, and the mixture was heated at a dew point of -45°C and a temperature of 645°C for 30 minutes. Sintering was performed. This porous sintered body had a porosity of 42% and a tensile strength of 1.5 Kg/mm 2 .
第１図はAl−Cu系状態図、第２図はベース粉
に加圧力をかけたときのクリープ極限強さと歪速
度との関係を示すグラフ、第３図は実質的にAl
から成るベース粉とNi粉末とから成る混合粉を
無加圧で成型した成型体の構造を示す説明図、第
４図は第３図に示す成型体を加圧状態で焼結し、
クリープ現象により変形している状態を示す説明
図である。
符号１……ベース粉末、２……添加粉末、３…
…酸化皮膜。
Figure 1 is a phase diagram of the Al-Cu system, Figure 2 is a graph showing the relationship between the ultimate creep strength and strain rate when applying pressure to the base powder, and Figure 3 is a graph showing the relationship between the creep strength and the strain rate when applying pressure to the base powder.
An explanatory diagram showing the structure of a molded body formed by molding a mixed powder consisting of base powder consisting of base powder and Ni powder without pressure.
FIG. 3 is an explanatory diagram showing a state of deformation due to a creep phenomenon. Code 1...Base powder, 2...Additional powder, 3...
...Oxide film.
Claims (1)
Al合金粉末の何れか一方若しくは双方から成る
ベース粉に対し、このベース粉中のAl基地との
間で共晶反応を示して溶融する際の共晶温度が前
記ベース粉の融点より低い金属の粉末またはこれ
ら金属を含む合金の粉末のうちの１種若しくは２
種以上を混合してから、この混合物を無加圧状態
で所望形状に成型し、その後、真空若しくは非酸
化性雰囲気で、前記ベース粉末の各粉末粒子に対
して60ｇ/cm2以上の圧力がかかるよう加圧して焼
結することを特徴とするAl若しくはAl合金の多
孔質焼結体の製造方法。 ２ 実質的にAlからなるAl粉末またはAlを含む
Al合金粉末の何れか一方若しくは双方から成る
ベース粉に対し、このベース粉の融点以下の温度
で一部に液相を生成する組成のAl合金粉末のう
ちの１種若しくは２種以上を混合してから、無加
圧状態で所望形状に成型し、その後、真空若しく
は非酸化性雰囲気で、前記ベース粉末の各粉末粒
子に対して60ｇ/cm2以上の圧力がかかるよう加圧
して焼結することを特徴とするAl若しくはAl合
金の多孔質焼結体の製造方法。 ３ 実質的にAlからなるAl粉末またはAlを含む
Al合金粉末の何れか一方若しくは双方から成る
ベース粉に対し、このベース粉の融点以下の温度
で一部に液相を生成する組成のAl合金粉末と共
に、前記ベース粉中のAl基地との間で共晶反応
を示して溶融する際の共晶温度が前記ベース粉の
融点より低い金属の粉末またはこれら金属を含む
合金の粉末のうちの１種若しくは２種以上を混合
してから、この混合粉を無加圧状態で所望の形状
に成型し、その後、真空若しくは非酸化性雰囲気
で、前記ベース粉の各粉末粒子に対して60ｇ/cm2
以上の圧力がかかるよう加圧して焼結することを
特徴とするAl若しくはAl合金の多孔質焼結体の
製造方法。[Claims] 1 Al powder consisting essentially of Al or containing Al
A base powder consisting of either one or both of the Al alloy powders is used to produce a metal whose eutectic temperature is lower than the melting point of the base powder when it exhibits a eutectic reaction with the Al base in the base powder and melts. One or two of powders or powders of alloys containing these metals
After mixing the above seeds, this mixture is molded into a desired shape without pressure, and then a pressure of 60 g/cm 2 or more is applied to each powder particle of the base powder in a vacuum or non-oxidizing atmosphere. 1. A method for producing a porous sintered body of Al or Al alloy, which comprises performing sintering under such pressure. 2 Al powder consisting essentially of Al or containing Al
One or more Al alloy powders having a composition that partially forms a liquid phase at a temperature below the melting point of the base powder are mixed with a base powder consisting of one or both of the Al alloy powders. After that, it is molded into a desired shape without pressure, and then sintered by pressurizing each powder particle of the base powder to a pressure of 60 g/cm 2 or more in a vacuum or non-oxidizing atmosphere. A method for producing a porous sintered body of Al or Al alloy, characterized in that: 3 Al powder consisting essentially of Al or containing Al
A base powder consisting of one or both of Al alloy powders, together with an Al alloy powder having a composition that partially forms a liquid phase at a temperature below the melting point of the base powder, and an Al base powder in the base powder. After mixing one or more types of powders of metals or powders of alloys containing these metals, the eutectic temperature of which is lower than the melting point of the base powder when melting by a eutectic reaction, The powder is molded into the desired shape without pressure, and then in a vacuum or non-oxidizing atmosphere, 60 g/cm 2 is applied to each powder particle of the base powder.
1. A method for producing a porous sintered body of Al or an Al alloy, the method comprising sintering under pressure such that the above pressure is applied.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5007580A JPS56149363A (en) | 1980-04-15 | 1980-04-15 | Manufacture of porous sintered body such as aluminum |
| CA000374991A CA1176490A (en) | 1980-04-15 | 1981-04-08 | Method for the manufacture of a sintered porous body of aluminum or an aluminum-base alloy |
| AU69542/81A AU548796B2 (en) | 1980-04-15 | 1981-04-15 | Powder metallurgy shapes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5007580A JPS56149363A (en) | 1980-04-15 | 1980-04-15 | Manufacture of porous sintered body such as aluminum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS56149363A JPS56149363A (en) | 1981-11-19 |
| JPS6148566B2 true JPS6148566B2 (en) | 1986-10-24 |
Family
ID=12848880
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5007580A Granted JPS56149363A (en) | 1980-04-15 | 1980-04-15 | Manufacture of porous sintered body such as aluminum |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JPS56149363A (en) |
| AU (1) | AU548796B2 (en) |
| CA (1) | CA1176490A (en) |
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| RU2038217C1 (en) * | 1992-12-07 | 1995-06-27 | Лев Хатевич Певзнер | Laminated porous material |
| CA2190238A1 (en) * | 1996-07-15 | 1998-01-15 | Ryutaro Motoki | Sintered metal filters |
| JP5633658B2 (en) * | 2013-03-01 | 2014-12-03 | 三菱マテリアル株式会社 | Porous aluminum sintered body |
| JP6237500B2 (en) | 2014-07-02 | 2017-11-29 | 三菱マテリアル株式会社 | Porous aluminum heat exchange member |
| CN118321546B (en) * | 2024-06-13 | 2024-08-13 | 西安稀有金属材料研究院有限公司 | Low-cost preparation method of titanium-aluminum-based alloy and composite material thereof |
-
1980
- 1980-04-15 JP JP5007580A patent/JPS56149363A/en active Granted
-
1981
- 1981-04-08 CA CA000374991A patent/CA1176490A/en not_active Expired
- 1981-04-15 AU AU69542/81A patent/AU548796B2/en not_active Ceased
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010116679A1 (en) | 2009-03-30 | 2010-10-14 | 三菱マテリアル株式会社 | Process for producing porous sintered aluminum, and porous sintered aluminum |
| US9242297B2 (en) | 2009-03-30 | 2016-01-26 | Mitsubishi Materials Corporation | Process for producing porous sintered aluminum, and porous sintered aluminum |
| US9589732B2 (en) | 2009-03-30 | 2017-03-07 | Mitsubishi Materials Corporation | Process for producing porous sintered aluminum, and porous sintered aluminum |
| US9815116B2 (en) | 2009-03-30 | 2017-11-14 | Mitsubishi Materials Corporation | Process for producing porous sintered aluminum, and porous sintered aluminum |
| US8691328B2 (en) | 2009-06-04 | 2014-04-08 | Mitsubishi Materials Corporation | Process for production of aluminum complex comprising sintered porous aluminum body |
| CN106102966A (en) * | 2014-05-16 | 2016-11-09 | 三菱综合材料株式会社 | Porous aluminum sintered body and the manufacture method of porous aluminum sintered body |
| US10478895B2 (en) | 2014-05-16 | 2019-11-19 | Mitsubishi Materials Corporation | Porous aluminum sintered compact and method of producing porous aluminum sintered compact |
| US10981228B2 (en) | 2014-05-16 | 2021-04-20 | Mitsubishi Materials Corporation | Porous aluminum sintered compact and method of producing porous aluminum sintered compact |
| US10981230B2 (en) | 2014-05-30 | 2021-04-20 | Mitsubishi Materials Corporation | Porous aluminum complex and method of producing porous aluminum complex |
| CN107107196A (en) * | 2014-10-30 | 2017-08-29 | 三菱综合材料株式会社 | The manufacture method of porous aluminum sintered body and porous aluminum sintered body |
| US10543531B2 (en) | 2014-10-30 | 2020-01-28 | Mitsubishi Materials Corporation | Porous aluminum sintered material and method of producing porous aluminum sintered material |
Also Published As
| Publication number | Publication date |
|---|---|
| AU548796B2 (en) | 1986-01-02 |
| CA1176490A (en) | 1984-10-23 |
| JPS56149363A (en) | 1981-11-19 |
| AU6954281A (en) | 1981-10-22 |
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