[go: up one dir, main page]

JP2007084906A - Ag-based metal powder, Cu-based metal powder and method for producing the same - Google Patents

Ag-based metal powder, Cu-based metal powder and method for producing the same Download PDF

Info

Publication number
JP2007084906A
JP2007084906A JP2005278180A JP2005278180A JP2007084906A JP 2007084906 A JP2007084906 A JP 2007084906A JP 2005278180 A JP2005278180 A JP 2005278180A JP 2005278180 A JP2005278180 A JP 2005278180A JP 2007084906 A JP2007084906 A JP 2007084906A
Authority
JP
Japan
Prior art keywords
water
metal powder
diameter
jet
flow
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.)
Pending
Application number
JP2005278180A
Other languages
Japanese (ja)
Inventor
Shinri Kikukawa
真利 菊川
Kota Inaba
恒太 稲葉
Shinji Terai
臣治 寺居
Tadashi Koyama
忠司 小山
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.)
Fukuda Metal Foil and Powder Co Ltd
Original Assignee
Fukuda Metal Foil and Powder Co Ltd
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 Fukuda Metal Foil and Powder Co Ltd filed Critical Fukuda Metal Foil and Powder Co Ltd
Priority to JP2005278180A priority Critical patent/JP2007084906A/en
Publication of JP2007084906A publication Critical patent/JP2007084906A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

【課題】 小さな寸法変化率と良好な延性と低い凝集性とを有する金属粉末を提供する。
【解決手段】 水ジェットカーテンの噴射水流を噴射させる環状噴射スリット2を下向きに配置して中心軸に沿って溶融金属流を流下させる工程と、噴射水流が通過しない水ジェットカーテンの括れ状空洞7が形成されるように下降角度θと旋回角度ωとを有する向きへ水を噴射させる工程とを備えて一葉双曲面状水ジェットカーテンの噴射水流12を発生させて金属粉末を製造する水アトマイズ法を採用し、下降角度θを0〜30°、旋回角度ωを1〜20°とし、水の圧力を90〜150MPa及び水の流量を300〜800L/minとし、50%径が0.1〜5μm、球形度が0.6〜0.9、粒度幅指数が1以下、比酸素量が0.5〜7mg/m2、比水分量が1mg/m2以下である金属粉末を得る。
【選択図】 図1
PROBLEM TO BE SOLVED: To provide a metal powder having a small dimensional change rate, good ductility and low cohesiveness.
SOLUTION: An annular injection slit 2 for injecting an injection water flow of a water jet curtain is arranged downward to cause a molten metal flow to flow down along the central axis, and a constricted cavity 7 of the water jet curtain through which the injection water flow does not pass. Water atomizing method for producing metal powder by generating a jet water flow 12 of a single leaf hyperboloid water jet curtain with a step of jetting water in a direction having a descending angle θ and a turning angle ω The descent angle θ is 0-30 °, the turning angle ω is 1-20 °, the water pressure is 90-150 MPa, the water flow rate is 300-800 L / min, and the 50% diameter is 0.1-5 μm, sphericity of 0.6 to 0.9, particle size breadth index of 1 or less, the ratio of oxygen quantity 0.5~7mg / m 2, specific water content to obtain a metal powder is 1 mg / m 2 or less.
[Selection] Figure 1

Description

本発明は、回路設計用や電子材料用の導電ペースト、マイクロMIM、微細な形状を有する部品の造形用及びダイヤモンド工具用バインダー等に用いられるAg系(Ag又はAgベース合金)の金属粉末及びCu系(Cu又はCuベース合金)の金属粉末並びにその製造方法に関するものである。   The present invention relates to conductive paste for circuit design and electronic materials, micro MIM, Ag-based (Ag or Ag base alloy) metal powder and Cu used for forming fine parts and diamond tool binders. The present invention relates to a metal powder of a system (Cu or Cu base alloy) and a manufacturing method thereof.

周知の通り、Ag又はAgベース合金の金属粉末やCu又はCuベース合金の金属粉末は、充填性の高い5μm以下の微細球状粉末のものにおいて需要が増大しており、平均粒径が0.5〜5μm、真球度が0.7〜0.85、酸素量が500〜3000ppmである金属粉末が提案され(特許文献1)、微細な擬球形で粒度分布の幅が狭い金属粉末を効率よく製造する方法として、流下する溶融金属流に向けて1°≦ω≦20°の旋回角度ωおよび5°≦θ≦60°の下降角度θで溶融金属流を一葉双曲面状に取り囲むように連続的に放出させて一葉双曲面状括れ部の近傍の圧力を50〜750mmHgに減圧する金属粉末製造方法(特許文献2)が提案されている。   As is well known, the demand for Ag or Ag-based alloy metal powders or Cu or Cu-based alloy metal powders is increasing in the case of fine spherical powders of 5 μm or less with high filling properties, and the average particle size is 0.5 to 5 μm. A metal powder having a sphericity of 0.7 to 0.85 and an oxygen content of 500 to 3000 ppm has been proposed (Patent Document 1). As a method for efficiently producing a metal powder having a fine pseudospherical shape and a narrow particle size distribution, The molten metal flow is continuously discharged so as to surround the molten metal flow in a single-leaf hyperboloid with a swivel angle ω of 1 ° ≦ ω ≦ 20 ° and a descending angle θ of 5 ° ≦ θ ≦ 60 ° toward the molten metal flow. A metal powder manufacturing method (Patent Document 2) has been proposed in which the pressure in the vicinity of the hyperboloid constriction is reduced to 50 to 750 mmHg.

特開2005−8930号公報JP 2005-8930 A 国際公開WO00/38865号公報International Publication WO00 / 38865

しかし、近年、粒径が5μm以下でかつ小さい寸法変化率と良好な延性との焼結特性を両立させた金属粉末が必要とされているが、前記金属粉末では、粉末の50%径(メジアン径)が5μm以下になると非常に凝集しやすく、この凝集を抑制するにはさらなる製造費が嵩むという問題点があった。また、寸法変化率が小さいことと延性を有していることとは互いに相反する特性であるため、延びや曲げに対して軟らかく破壊しにくい延性を得られるように焼結すれば、おのずと寸法変化率が大きくなり、当該両特性を満足させる金属粉末を得ることは困難であった。   However, in recent years, a metal powder having a particle size of 5 μm or less and having both small dimensional change rate and good ductility sintering characteristics is required. However, in the metal powder, the 50% diameter (median of the powder) When the (diameter) is 5 μm or less, it is very easy to agglomerate, and there is a problem that the production cost increases to suppress this agglomeration. In addition, since the small dimensional change rate and having ductility are mutually contradictory characteristics, if sintered to obtain ductility that is soft against elongation and bending and that is difficult to break, the dimensional change will naturally occur. It was difficult to obtain a metal powder satisfying both of these characteristics.

また、前記特許文献1に開示されている金属粉末の真球度は平均粒径と比表面積とから計算されているが、比表面積は一般に金属粉末の平均粒径が小さくなればそれに従って大きくなるので、当該金属粉末の酸素量は粉末全体に対する含有量として捉えられており、比表面積が大きいほど酸素含有量は多くなるが、酸素量は個々の粉末によるものであるから、粉末全体に対する酸素量では、金属粉末の特性を正確には表現できないという問題点があった。   Further, the sphericity of the metal powder disclosed in Patent Document 1 is calculated from the average particle diameter and the specific surface area, but the specific surface area generally increases as the average particle diameter of the metal powder decreases. Therefore, the oxygen content of the metal powder is regarded as the content of the whole powder. The larger the specific surface area, the greater the oxygen content, but the oxygen content is due to individual powders. However, there is a problem that the characteristics of the metal powder cannot be expressed accurately.

そのため、前記従来の金属粉末を回路設計用や電子材料用の導電ペーストに使用した場合、焼結体の寸法変化及び寸法バラツキが大きくなり、延性が劣る等の問題が発生していた。また、導電ペースト用として回路基板にスクリーン印刷しこれを焼成した場合、接合している基板の歪みが大きくなって回路に亀裂が入る問題やセラミックス基板と接合している隙間が広がって気密性を保つことができないという問題や高周波導電率が低くなる等の問題が発生していた。また、マイクロMIMや造形用の粘土等に使用した場合、収縮により微細なコーナー亀裂が入る問題や延性が悪い等の不具合が発生していた。さらに、ダイヤモンド工具用に使用した場合においてもバインダー層の延性が低下する問題やダイヤモンド粒子と金属粉末の隙間が開きやすいことでダイヤモンド粒子が脱落しやすくなり最終的にダイヤモンド工具の寿命が短くなるという問題が発生していた。   For this reason, when the conventional metal powder is used as a conductive paste for circuit design or electronic material, there has been a problem that the dimensional change and dimensional variation of the sintered body increase and the ductility is inferior. In addition, when screen printing is performed on a circuit board for conductive paste, and this is fired, there is a problem that the distortion of the bonded substrate increases and the circuit cracks, and the gap bonded to the ceramic substrate widens to improve airtightness. Problems such as inability to maintain and low-frequency conductivity have occurred. In addition, when used for micro MIM, modeling clay, etc., there are problems such as a problem that fine corner cracks occur due to shrinkage and poor ductility. Furthermore, even when used for diamond tools, the problem is that the ductility of the binder layer decreases and the gap between the diamond particles and the metal powder tends to open, so that the diamond particles can easily fall off and ultimately the life of the diamond tool is shortened. There was a problem.

そこで、本発明者は、電子材料用のみならず微細な形状の部品の造形用やダイヤモンド工具用等の用途に需要が増大しつつある50%径が5μm以下の微粉金属粉末に対して、小さな寸法変化率と良好な延性、さらには低い凝集性を満足させる金属粉末を得ることを技術的課題として、その具現化をはかるべく研究・実験を重ねた。   Therefore, the present inventor has a small 50% diameter 5 μm or less fine metal powder whose demand is increasing not only for electronic materials but also for applications such as modeling of finely shaped parts and diamond tools. As a technical issue, we have researched and experimented to obtain a metal powder that satisfies the dimensional change rate, good ductility, and low cohesiveness.

先ず、5μm以下のAg及びCu金属粉末において球形に近い粉末が得られる条件を検討した。   First, conditions for obtaining a nearly spherical powder in Ag and Cu metal powders of 5 μm or less were examined.

前記5μm以下の球形に近い金属粉末は、水アトマイズ法における環状噴射スリットの縦断面側面図である図1、図1に図示する環状噴射スリットから噴射される一葉双曲面状水ジェットカーテンの下降角度θを説明する図2及び同じく旋回角度ωを説明する図3に図示すように、水ジェットカーテンの噴射水流1を噴射させる環状噴射スリット2を下向きに配置して当該環状噴射スリット2を面位置3とする内包面4中央を該内包面4に対して直角に上下方向へ走る中心軸5に沿って溶融金属流6を流下させる工程と、当該環状噴射スリット2に対して高圧水流を供給して前記噴射水流1が通過しない水ジェットカーテンの括れ状空洞7が形成されるように環状噴射スリット2の一部位8から前記中心軸5と平行に下ろした垂線9(内包面4に対して直角)に対する前記溶融金属流6への振れ角である下降角度θと前記一部位8から前記内包面4に投影された前記括れ状空洞7への接線10と前記一部位8から前記中心軸5を横切る環状噴射スリット2の径11とが成す角である旋回角度ωとを有する向きへ水を噴射させる工程とを備えて一葉双曲面状水ジェットカーテン12の噴射水流1を発生させて金属粉末を得る水アトマイズ法を採用して製造した。   The metal powder close to a sphere having a diameter of 5 μm or less is a vertical sectional side view of the annular injection slit in the water atomization method, and the descending angle of the single leaf hyperboloid water jet curtain ejected from the annular ejection slit shown in FIG. As shown in FIG. 2 for explaining θ and FIG. 3 for explaining the turning angle ω, an annular injection slit 2 for injecting the jet water flow 1 of the water jet curtain is arranged downward, and the annular injection slit 2 is positioned on the surface. 3, a step of flowing the molten metal flow 6 along the central axis 5 running in the vertical direction perpendicular to the inner surface 4 with respect to the center of the inner surface 4, and supplying a high-pressure water flow to the annular injection slit 2 Accordingly, a perpendicular line 9 (into the inner surface 4) is formed parallel to the central axis 5 from one portion 8 of the annular jet slit 2 so that a constricted cavity 7 of the water jet curtain through which the jet water flow 1 does not pass is formed. And a tangent line 10 to the constricted cavity 7 projected from the partial position 8 onto the inner envelope surface 4 and the center from the partial position 8 to the center. And a step of injecting water in a direction having a turning angle ω that is an angle formed by the diameter 11 of the annular injection slit 2 crossing the shaft 5 to generate an injection water flow 1 of the one-leaf hyperboloid water jet curtain 12. It was manufactured by employing a water atomization method to obtain metal powder.

前記水アトマイズ法におけるアトマイズ条件である噴射水流1の水の圧力及び流量、旋回角度ω、下降角度θについて検討した結果、表1のように旋回角度ωが0°では、球形度は0.6以下であるが、1°以上では球形度が0.6以上となっており、旋回角度ωと球形度とには関連性があることを確認した。   As a result of examining the water pressure and flow rate, the swirl angle ω, and the descending angle θ of the jet water stream 1 as atomizing conditions in the water atomizing method, as shown in Table 1, when the swirl angle ω is 0 °, the sphericity is 0.6 or less. However, the sphericity was 0.6 or more at 1 ° or more, and it was confirmed that the turning angle ω and the sphericity were related.

Figure 2007084906
Figure 2007084906

また、前記旋回角度ωが1〜20°、前記下降角度θが0〜30°、前記水の圧力が90〜150MPa、前記水の流量が300〜800L(リットル)/minの時に50%径が0.1〜5μmでかつ球形度が0.6〜0.9であるAg及びCu金属粉末を得られることを確認した(表3及び表4参照)。   Further, when the turning angle ω is 1 to 20 °, the descending angle θ is 0 to 30 °, the water pressure is 90 to 150 MPa, and the water flow rate is 300 to 800 L (liter) / min, the 50% diameter is It was confirmed that Ag and Cu metal powder having a sphericity of 0.1 to 5 μm and a sphericity of 0.6 to 0.9 can be obtained (see Tables 3 and 4).

次に、得られた金属粉末についてその粉末特性と焼結特性との関係について検討した。   Next, the relationship between the powder characteristics and the sintering characteristics of the obtained metal powder was examined.

金属粉末は50%径が小さいほど低温で焼結するため、各50%径の金属粉末について焼結温度を変えて実験を行った。Cu粉末は大気中では酸化が進行するので窒素中(N2)の焼結とし、Ag粉末は従来の焼結法にならって大気中(Air)の焼結とした。その結果、同程度の比表面積において、小さい寸法変化率で延性の良好な(曲げ角の大きな)粉末は寸法変化率が大きく延性が劣っている(曲げ角が小さい)粉末より酸素量や水分量がかなり少ないことを確認した(表3及び表4参照)。また、50%径が2μm以下になると急激に比表面積が大きくなって酸素量及び水分量とも急激に増加するので、特に微細な粉末は酸素量や水分量の数値のみで粉末を評価することは不適当であることを確認できた。そこで、単位表面積当りの酸素量と水分量とを得るために、酸素量と水分量とを粉末の比表面積で除したところ、粉末の焼結性が良好なものはその各数値が酸素量においては0.5〜7mg/m2(Ag粉末では0.5〜2mg/m2、Cu粉末では2〜7mg/m2)にあることを確認した(表3及び表4参照)。そこで、単位表面積当りの酸素量を比酸素量、単位表面積当りの水分量を比水分量として粉末特性を表現する値とした。 Since the metal powder sinters at a lower temperature as the 50% diameter is smaller, the experiment was carried out by changing the sintering temperature for each 50% diameter metal powder. Since Cu powder undergoes oxidation in the atmosphere, it was sintered in nitrogen (N 2 ), and Ag powder was sintered in air (Air) following the conventional sintering method. As a result, powders with a small dimensional change rate and good ductility (large bending angle) at the same specific surface area have a large dimensional change rate and poor ductility (small bending angle). Was confirmed to be considerably small (see Tables 3 and 4). In addition, when the 50% diameter is 2 μm or less, the specific surface area suddenly increases and both the amount of oxygen and the amount of water increase sharply. It was confirmed that it was inappropriate. Therefore, in order to obtain the amount of oxygen and the amount of moisture per unit surface area, the amount of oxygen and the amount of moisture were divided by the specific surface area of the powder. (in the Ag powder in 0.5~2mg / m 2, Cu powder 2~7mg / m 2) 0.5~7mg / m 2 was confirmed that in (see Table 3 and Table 4). Thus, the oxygen content per unit surface area is defined as the specific oxygen content, and the water content per unit surface area is defined as the specific water content to represent the powder characteristics.

前記比酸素量と前記水アトマイズ法における水の流量及び溶融金属の流量との関係について検討した。   The relationship between the specific oxygen amount, the flow rate of water and the flow rate of molten metal in the water atomization method was examined.

水の流量と溶湯の流量との比(水の流量/溶湯の流量)を水溶湯比として該水溶湯比と比酸素量との値によりアトマイズの能力を評価した。その結果、表2に示すように、Cuにおいては水溶湯比が小さい場合に明らかに酸素量が増加し、Agでは水溶湯比が小さいものにおいて比酸素量が少し高い傾向にあった。これにより、金属粉末の酸素量を上げないためには水溶湯比が40以上であることが好ましく、水溶湯比が小さくなると粉末の比酸素量が増加する傾向にあることを確認した。   The ratio of the flow rate of water to the flow rate of molten metal (flow rate of water / flow rate of molten metal) was used as the water solution ratio, and the ability of atomization was evaluated based on the value of the water solution ratio and the specific oxygen amount. As a result, as shown in Table 2, the amount of oxygen clearly increased in Cu when the ratio of the hot water was small, and the specific amount of oxygen tended to be slightly higher in Ag when the ratio of the hot water was small. Thereby, in order not to raise the oxygen content of the metal powder, the ratio of the water solution was preferably 40 or more, and it was confirmed that the specific oxygen content of the powder tends to increase as the water solution ratio decreases.

Figure 2007084906
Figure 2007084906

また、以上の検討結果から寸法変化率が小さく延性が大きい良好な焼結特性の金属粉末としては、0.1〜5μmの範囲であることが好ましいことを確認し、より低温で焼結できるためには0.1〜3μm、さらに好ましくは0.1〜1μmであり、さらなる低温でも焼結できるためには0.1〜0.5μmが好ましいことを確認し、50%径が5μmを超えると焼結温度が900℃以上と高くなり、また、0.1μm未満では粒子が非常に微細で比表面積が大きくなりすぎるので、常温域でも焼結が始まる可能性があり、凝集も発生しやすくなるため前記各用途には不向きであることを確認した(表3及び表4参照)。   In addition, from the above examination results, as a metal powder having good sintering characteristics with a small dimensional change rate and large ductility, it is confirmed that it is preferably in the range of 0.1 to 5 μm, and in order to be able to sinter at a lower temperature 0.1 to 3 μm, more preferably 0.1 to 1 μm. Confirm that 0.1 to 0.5 μm is preferable in order to be able to sinter at even lower temperatures. When the 50% diameter exceeds 5 μm, the sintering temperature is as high as 900 ° C. or higher. Also, if it is less than 0.1 μm, the particles are very fine and the specific surface area becomes too large, so there is a possibility that sintering may start even at room temperature, and aggregation is likely to occur, so it is not suitable for each application. Was confirmed (see Table 3 and Table 4).

また、金属粉末の形状は、実際の粉末と同等形状の球の比表面積と、粉末の実際の比表面積との比で表される球形度を採用して表した。粉末の径はレーザー回折散乱法を採用し、実際の比表面積の測定はBET法を採用して算出した。その結果、BET法では粉末粒子の表面の微細な凹凸による比表面積も測定してしまい、電子顕微鏡で観察して非常に球に近い粉末であったものでも球形度0.9を超える数値は実際には観察されないことを確認し、また、球形度0.6未満では形状が好ましくなく焼結後の収縮においても延性が得られないことを確認した。これにより、0.6〜0.9の範囲の球形度が良好であることを得た。   In addition, the shape of the metal powder is expressed by adopting a sphericity represented by a ratio between a specific surface area of a sphere having the same shape as that of the actual powder and an actual specific surface area of the powder. The diameter of the powder was calculated using the laser diffraction scattering method, and the actual specific surface area was calculated using the BET method. As a result, the BET method also measures the specific surface area due to fine irregularities on the surface of the powder particles, and even if the powder was very close to a sphere when observed with an electron microscope, the numerical value exceeding the sphericity of 0.9 is actually It was confirmed that it was not observed, and when the sphericity was less than 0.6, the shape was not preferable, and it was confirmed that ductility was not obtained even after shrinkage after sintering. Thereby, it was found that the sphericity in the range of 0.6 to 0.9 was good.

次に、集合体としての金属粉末の分布状態を数値で表現する方法について検討した。   Next, a method for numerically expressing the distribution state of the metal powder as an aggregate was examined.

金属粉末の粒度の幅に関しては幾何標準偏差が採用されているが、粉末の粒度分布が対数正規確率分布に従うとした場合に分布を近似直線の傾きで表現するため実状を表現しにくい面があった。実際の粉末は正規確率分布とならない場合が多い上に分布に偏りがある場合も多く、分布の裾の広がりにも微粉側と粗粉側で差が見られる場合が多々ある。そこで、粉末の粒度分布の広がりを直接表現するために、図4に示す横軸に粒度(μm)をとり縦軸に頻度(%)をとった粒度分布曲線に基づき、分布の両端に近い5%径と95%径を読み取り、分布の粒度目盛りに多く使われている対数での表記を参考に5%径と95%径との対数をとり、その差を求めることで粒度分布の広がりを表すことを試みたところ、5%径がAμm 、95%径がBμmである場合、log(B)−log(A)、即ち、log(B/A)により得られる数値(粒度幅指数)は、粉末の50%径によらず単純に粒度幅を表現でき、50%径が0.1μm〜5μmのいずれにあってもその幅を相対値によって表現できることを確認した。その結果、粒度分布の5%径と95%径間に存在する粉末粒度の幅、即ち、この間における粒度分布の広がりを相対的に表した粒度幅指数が1を超える場合は1以下の場合に比較してその焼結体の寸法変化も大きく、延性は低い傾向にあった。従って、寸法変化率を小さく延性を高くしようとすれば、1以下が好ましいことを確認した(表3及び表4参照)。   The geometric standard deviation is adopted for the particle size width of the metal powder, but when the particle size distribution of the powder follows a lognormal probability distribution, the distribution is expressed by the slope of the approximate straight line, so there are some aspects where it is difficult to express the actual state. It was. The actual powder often does not have a normal probability distribution, and there are many cases where the distribution is biased, and there is often a difference between the fine powder side and the coarse powder side in the spread of the distribution. Therefore, in order to directly express the spread of the particle size distribution of the powder, it is close to both ends of the distribution based on the particle size distribution curve shown in FIG. 4 with the particle size (μm) on the horizontal axis and the frequency (%) on the vertical axis. Read the% diameter and the 95% diameter, take the logarithm of the 5% diameter and the 95% diameter with reference to the logarithmic notation often used in the particle size scale of the distribution, and find the difference between them to widen the particle size distribution When trying to express, when the 5% diameter is Aμm and the 95% diameter is Bμm, the log (B) -log (A), that is, the numerical value (particle size index) obtained by log (B / A) is It was confirmed that the particle size width can be simply expressed regardless of the 50% diameter of the powder, and that the width can be expressed by a relative value regardless of the 50% diameter in any of 0.1 μm to 5 μm. As a result, the width of the powder particle size existing between the 5% diameter and the 95% diameter of the particle size distribution, that is, when the particle size width index relatively representing the spread of the particle size distribution in the meantime is greater than 1 is 1 or less In comparison, the dimensional change of the sintered body was large and the ductility tended to be low. Therefore, it was confirmed that 1 or less is preferable if the dimensional change rate is reduced and the ductility is increased (see Tables 3 and 4).

前記球形度と粒度幅指数との関係では、粒度幅指数が1以下で粒度幅が小さいものの方が球形度が高い傾向が見られ、50%径の測定が体積基準のため、同じ50%径であっても粒度幅が広いものは個数の少ない粗粉に対して数多くの微粉を含有していることになり、比表面積が増大する傾向があると考えられる。実際に粒度幅が小さいものにおいて球形度が高い傾向が観察された。   As for the relationship between the sphericity and the particle size width index, the smaller the particle size width index and the smaller the particle size width, the higher the sphericity tends to be seen. Even so, those having a wide particle size range contain a large number of fine powders relative to a small number of coarse powders, and it is considered that the specific surface area tends to increase. A tendency of high sphericity was observed in the actually small particle size range.

前記各研究・実験結果より、前記技術的課題は、次の通りの本発明によって解決できる。   From the results of the respective studies and experiments, the technical problem can be solved by the present invention as follows.

即ち、本発明に係るAg系金属粉末は、50%径が0.1〜5μm、球形度が0.6〜0.9、5%径と95%径間における粒度分布の広がり相対値を表す粒度幅指数が1以下、単位表面積当りの酸素量を表す比酸素量が0.5〜7mg/m2、単位表面積当りの水分量を表す比水分量が1mg/m2以下の金属粉末である。 That is, the Ag-based metal powder according to the present invention has a 50% diameter of 0.1 to 5 μm, a sphericity of 0.6 to 0.9, and a particle size width index representing a spread relative value of the particle size distribution between the 5% diameter and the 95% diameter is 1 or less. , the ratio of oxygen quantity representing the amount of oxygen per unit surface area of 0.5~7mg / m 2, the ratio amount of water which represents the water content per unit surface area of 1 mg / m 2 or less of the metal powder.

また、本発明に係るCu系金属粉末は、50%径が0.1〜5μm、球形度が0.6〜0.9、5%径と95%径間における粒度分布の広がり相対値を表す粒度幅指数が1以下、単位表面積当りの酸素量を表す比酸素量が0.5〜7mg/m2、単位表面積当りの水分量を表す比水分量が1mg/m2以下の金属粉末である。 Further, the Cu-based metal powder according to the present invention has a 50% diameter of 0.1 to 5 μm, a sphericity of 0.6 to 0.9, and a particle size width index representing a spread relative value of the particle size distribution between the 5% diameter and the 95% diameter is 1 or less. , the ratio of oxygen quantity representing the amount of oxygen per unit surface area of 0.5~7mg / m 2, the ratio amount of water which represents the water content per unit surface area of 1 mg / m 2 or less of the metal powder.

また、本発明に係るAg系金属粉末の製造方法は、水ジェットカーテンの噴射水流を噴射させる環状噴射スリットを下向きに配置して当該環状噴射スリットを面位置とする内包面中央を上下方向へ走る中心軸に沿って溶融金属流を流下させる工程と当該環状噴射スリットに対して高圧水流を供給して前記噴射水流が通過しない水ジェットカーテンの括れ状空洞が形成されるように環状噴射スリットの一部位から前記中心軸と平行に下ろした垂線に対する前記溶融金属流への振れ角である下降角度θと前記一部位から前記内包面に投影された前記括れ状空洞への接線と前記一部位から前記中心軸を横切る環状噴射スリットの径とが成す角である旋回角度ωとを有する向きへ水を噴射させる工程とを備えて一葉双曲面状水ジェットカーテンの噴射水流を発生させて金属粉末を製造する水アトマイズ法を採用し、前記下降角度θを0〜30°、前記旋回角度ωを1〜20°とし、水の圧力を90〜150MPa及び水の流量を300〜800L/minとして水を噴射させてAg系金属粉末を製造し、当該Ag系金属粉末を分級して50%径が0.1〜5μm、球形度が0.6〜0.9、5%径と95%径間における粒度分布の広がり相対値を表す粒度幅指数が1以下、単位表面積当りの酸素量を表す比酸素量が0.5〜7mg/m2、単位表面積当りの水分量を表す比水分量が1mg/m2以下である金属粉末を得るものである。 Further, in the method for producing an Ag-based metal powder according to the present invention, an annular injection slit for injecting an injection water flow of a water jet curtain is arranged downward and runs in the vertical direction at the center of the inner surface with the annular injection slit as a surface position. A step of causing the molten metal flow to flow down along the central axis and a high pressure water flow to the annular jet slit to form a constricted cavity of a water jet curtain through which the jet water flow does not pass. A descending angle θ, which is a swing angle of the molten metal flow with respect to a perpendicular line parallel to the central axis, and a tangent to the constricted cavity projected from the partial position onto the inner surface and the partial position Jetting water flow of a single leaf hyperboloid water jet curtain with a step of jetting water in a direction having a swivel angle ω, which is an angle formed by the diameter of the annular jet slit across the central axis Adopting a water atomization method for producing metal powder by generating, the descending angle θ is 0-30 °, the turning angle ω is 1-20 °, the water pressure is 90-150 MPa and the water flow rate is 300- Water is sprayed at 800 L / min to produce an Ag-based metal powder, and the Ag-based metal powder is classified to have a 50% diameter of 0.1 to 5 μm, a sphericity of 0.6 to 0.9, and between a 5% diameter and a 95% diameter. particle size range exponent representing the spread relative value of the particle size distribution is 1 or less, the ratio of oxygen quantity 0.5~7mg / m 2 representing the amount of oxygen per unit surface area, per unit surface area water content representing specific water content 1 mg / m 2 The following metal powder is obtained.

さらに、本発明に係るCu系金属粉末の製造方法は、水ジェットカーテンの噴射水流を噴射させる環状噴射スリットを下向きに配置して当該環状噴射スリットを面位置とする内包面中央を上下方向へ走る中心軸に沿って溶融金属流を流下させる工程と当該環状噴射スリットに対して高圧水流を供給して前記噴射水流が通過しない水ジェットカーテンの括れ状空洞が形成されるように環状噴射スリットの一部位から前記中心軸と平行に下ろした垂線に対する前記溶融金属流への振れ角である下降角度θと前記一部位から前記内包面に投影された前記括れ状空洞への接線と前記一部位から前記中心軸を横切る環状噴射スリットの径とが成す角である旋回角度ωとを有する向きへ水を噴射させる工程とを備えて一葉双曲面状水ジェットカーテンの噴射水流を発生させて金属粉末を製造する水アトマイズ法を採用し、前記下降角度θを0〜30°、前記旋回角度ωを1〜20°とし、水の圧力を90〜150MPa及び水の流量を300〜800L/minとして水を噴射させてCu系金属粉末を製造し、当該Cu系金属粉末を分級して50%径が0.1〜5μm、球形度が0.6〜0.9、5%径と95%径間における粒度分布の広がり相対値を表す粒度幅指数が1以下、単位表面積当りの酸素量を表す比酸素量が0.5〜7mg/m2、単位表面積当りの水分量を表す比水分量が1mg/m2以下である金属粉末を得るものである。 Furthermore, in the method for producing a Cu-based metal powder according to the present invention, an annular injection slit for injecting the water flow of the water jet curtain is disposed downward, and the center of the inner surface of the inner surface with the annular injection slit as a surface position runs in the vertical direction. A step of causing the molten metal flow to flow down along the central axis and a high pressure water flow to the annular jet slit to form a constricted cavity of a water jet curtain through which the jet water flow does not pass. A descending angle θ, which is a swing angle of the molten metal flow with respect to a perpendicular line parallel to the central axis, and a tangent to the constricted cavity projected from the partial position onto the inner surface and the partial position Spraying water in a one-leaf hyperboloid water jet curtain with a step of injecting water in a direction having a turning angle ω that is an angle formed by a diameter of an annular injection slit crossing the central axis Water atomization method is used to produce metal powder, the descending angle θ is 0-30 °, the turning angle ω is 1-20 °, the water pressure is 90-150 MPa, and the water flow rate is 300. Water is injected at a rate of ~ 800L / min to produce a Cu-based metal powder, and the Cu-based metal powder is classified to have a 50% diameter of 0.1 to 5μm, a sphericity of 0.6 to 0.9, and between a 5% diameter and 95% diameter The particle size distribution index representing the relative value of the spread of the particle size distribution is 1 or less, the specific oxygen amount representing the oxygen amount per unit surface area is 0.5 to 7 mg / m 2 , and the specific water amount representing the water amount per unit surface area is 1 mg / m The metal powder which is 2 or less is obtained.

本発明によれば、50%径が0.1〜5μm、球形度が0.6〜0.9、粒度幅指数が1以下、比酸素量が0.5〜7mg/m2及び比水分量が1mg/m2以下のAg系及びCu系金属粉末を提供できるので、従来の金属粉末より凝集性が低く、小さな寸法変化率を示し、90°曲げても破断しない優れた延性を持つ焼結体を得ることができる。 According to the present invention, the 50% size is 0.1 to 5 [mu] m, a sphericity of 0.6 to 0.9, particle size breadth index of 1 or less, the ratio of oxygen quantity 0.5~7mg / m 2 and the ratio water content 1 mg / m 2 or less of Ag And Cu-based metal powders can be provided, and a sintered body having lower ductility than conventional metal powders, a small dimensional change rate, and excellent ductility that does not break even when bent by 90 ° can be obtained.

以下、本発明の実施の形態を図1〜図4を参照して説明する。   Hereinafter, embodiments of the present invention will be described with reference to FIGS.

100は一葉双曲面状水ジェットカーテン12の噴射水流1を発生させてAg系又はCu系金属粉末を製造する水アトマイズ装置であり(図1参照)、1は水ジェットカーテンの噴射水流、2は噴出口を下向きに向けて配置した、噴射水流1を噴射させる環状噴射スリット、3は環状噴射スリット2の仮想上の面位置平面、4は円形環状噴射スリット2によって囲まれた面位置3の仮想上の円形内包面、5は内包面4中央を該内包面4に対して直角に上下方向へ走る仮想上の中心軸、6は中心軸5に沿って流下する溶融金属流、7は一葉双曲面状水ジェットカーテン12の噴射水流1が通過しない括れ状空洞、8は環状噴射スリット2の各一部位、9は一部位8から前記中心軸5と平行に下ろした仮想上の垂線(内包面4に対して直角)、10は一部位8から内包面4に投影された括れ状空洞7へ引いた仮想上の接線、11は一部位8から中心軸5を横切る環状噴射スリット2の仮想上の径である。そして、下降角度θは垂線9に対する溶融金属流6への振れ角、旋回角度ωは接線10と径11とが成す角である。   Reference numeral 100 is a water atomizing device for producing an Ag-based or Cu-based metal powder by generating a jet stream 1 of a single leaf hyperboloid water jet curtain 12 (see FIG. 1), 1 is a jet stream of the water jet curtain, An annular jet slit for jetting the jet water stream 1 with the jet port facing downward, 3 is a virtual plane position plane of the ring jet slit 2, and 4 is a virtual plane position 3 surrounded by the circular ring jet slit 2 The upper circular inner surface 5 is an imaginary central axis that runs vertically in the center of the inner surface 4 perpendicularly to the inner surface 4, 6 is a molten metal flow that flows down along the central axis 5, and 7 is a single-leaf biplane. A constricted cavity through which the jet stream 1 of the curved water jet curtain 12 does not pass, 8 is a part of each of the annular jet slits 2, and 9 is a hypothetical perpendicular (inclusive surface) drawn from the part 8 in parallel to the central axis 5. Right angle to 4), 10 is partly within 8 An imaginary tangent drawn to the constricted cavity 7 projected on the enveloping surface 4, 11 is an imaginary diameter of the annular injection slit 2 crossing the central axis 5 from the partial position 8. The descending angle θ is the swing angle of the molten metal flow 6 with respect to the perpendicular 9, and the turning angle ω is the angle formed by the tangent 10 and the diameter 11.

前記水アトマイズ装置100は、水ジェットカーテンの噴射水流1を噴射させる環状噴射スリット2を下向きに配置して当該環状噴射スリット2を面位置3とする内包面4中央を上下方向へ走る中心軸5に沿って溶融金属流6を流下させる工程と、当該環状噴射スリット2に対して高圧水流を供給して前記噴射水流1が通過しない水ジェットカーテンの括れ状空洞7が形成されるように前記下降角度θと前記旋回角度ωとを有する向きへ水を噴射させる工程とにより、一葉双曲面状水ジェットカーテン12の噴射水流1を発生させて前記金属粉末を製造している。   The water atomizing device 100 has an annular injection slit 2 for injecting the jet stream 1 of the water jet curtain arranged downward, and a central axis 5 that runs in the vertical direction at the center of the inner surface 4 with the annular injection slit 2 as the surface position 3. A step of causing the molten metal stream 6 to flow down along the line, and the lowering so as to form a constricted cavity 7 of the water jet curtain through which the high-pressure water stream is supplied to the annular jet slit 2 and the jet water stream 1 does not pass through. The metal powder is produced by generating the jet water flow 1 of the single leaf hyperboloid water jet curtain 12 by the step of jetting water in the direction having the angle θ and the turning angle ω.

前記水アトマイズ法を採用して前記下降角度θを0〜30°、前記旋回角度ωを1〜20°とし、水の圧力を90〜150MPa及び水の流量を300〜800L/minとして水を噴射させて金属粉末を製造し、当該金属粉末を分級して50%径が0.1〜5μm、球形度が0.6〜0.9、5%径と95%径間における粒度分布の広がり相対値を表す粒度幅指数が1以下、単位表面積当りの酸素量を表す比酸素量が0.5〜7mg/m2、単位表面積当りの水分量を表す比水分量が1mg/m2以下である金属粉末を得る。 Adopting the water atomization method, the downward angle θ is 0-30 °, the turning angle ω is 1-20 °, the water pressure is 90-150 MPa and the water flow rate is 300-800 L / min. To produce a metal powder, and classify the metal powder to give a 50% diameter of 0.1-5 μm, a sphericity of 0.6-0.9, and a particle size distribution index representing a relative value of the spread of the particle size distribution between the 5% diameter and the 95% diameter but 1 or less, 0.5~7mg / m 2 ratio of oxygen quantity representing the amount of oxygen per unit surface area, the specific amount of water which represents the water content per unit surface area to obtain a metal powder is 1 mg / m 2 or less.

前記水アトマイズ法によれば、吸引するガスとその後の高速水ジェットによって溶融金属流6を微細に粉砕することができ、一葉双曲面状水ジェットカーテン12によって粒子同士の衝突を大きく減少でき、これにより、得られる金属粉末の形状を球形に近いものにすることができ、微細化が可能になる。また、衝突を減少させながらも分裂した微細な溶融液滴を一葉双曲面で取り囲むように急速に冷却するので、内蔵する酸素量はもとより表面の酸素量も低く抑えることができ、合わせて比酸素量の低い粉末を得ることができる。   According to the water atomization method, the molten metal stream 6 can be finely pulverized by the gas to be sucked and the subsequent high-speed water jet, and the collision between the particles can be greatly reduced by the one-leaf hyperboloid water jet curtain 12. As a result, the shape of the obtained metal powder can be made nearly spherical, and miniaturization becomes possible. In addition, because it cools rapidly so as to surround the fine molten droplets that have been split while reducing collisions with a single leaf hyperboloid, the amount of oxygen contained in the surface as well as the amount of oxygen on the surface can be kept low. A low amount of powder can be obtained.

前記下降角度θは、垂線9が内包面4に対して直角に走っているので、0°以上であり、0°〜30°の範囲であれば良好にアトマイズできる。しかし、30°を超えればエゼクター効果が十分に発揮できず、吸引するガスの流量が不十分となり一次分裂が不十分で粉末は粗くなり、さらに、50%径が粗くなると共に、球形度が低下するので好ましくない。また、前記旋回角度ωは、1°以上で一葉双曲面状のジェットの特徴である衝突の減少が見られ、旋回角度ωを20°を超えて得ることは困難である。   Since the perpendicular line 9 runs perpendicular to the inner surface 4, the descending angle θ is not less than 0 ° and can be satisfactorily atomized within the range of 0 ° to 30 °. However, if the angle exceeds 30 °, the ejector effect cannot be fully exerted, the flow rate of the sucked gas is insufficient, the primary splitting is insufficient, the powder becomes coarse, and the 50% diameter becomes coarse and the sphericity decreases. This is not preferable. In addition, when the turning angle ω is 1 ° or more, a decrease in collision, which is a characteristic of a single leaf hyperboloid jet, is seen, and it is difficult to obtain the turning angle ω exceeding 20 °.

前記噴射水流1の水の圧力は、90MPa以上で微細な金属粉末の収率を高めることができ、150MPaを超える圧力ではエネルギー効率が低下してロスが大きくなるので、好ましくない。また、水の流量は、一葉双曲面状水ジェットカーテン12を発生させるには300L/min以上必要であり、多いほど好ましいが800L/minを超える流量では脱水処理、水の後処理、ポンプの容量等から無駄が多くなり、好ましくない。   The pressure of water in the jet water stream 1 is not preferable because the yield of fine metal powder can be increased at 90 MPa or more, and the energy efficiency is reduced and the loss is increased at a pressure exceeding 150 MPa. In addition, the flow rate of water needs to be 300 L / min or more to generate the single-leaf hyperboloid water jet curtain 12, and it is preferable that the flow rate exceeds 800 L / min. This is not preferable because of increased waste.

前記比酸素量は、0.5〜7mg/m2(Agベース合金を含むAg系金属粉末、Cuベース合金を含むCu系金属粉末)が良好であるが、Ag粉末の場合は0.5〜2mg/m2、酸化しやすいCu粉末の場合は2〜7mg/m2の範囲であることが好ましい。比酸素量が7mg/m2を超えれば、酸化膜の厚さの増加により、焼結性が低下し、延性が上昇せず、焼結体が脆く破損しやすくなるので、好ましくない。また、比酸素量が0.5mg/m2未満、あるいは、Cu粉末において比酸素量が2mg/m2未満では、樹脂と混練してペースト化して使用する場合にペースト中のC(カーボン)残留物を燃焼させて除去することができないので好ましくない。 The specific oxygen amount is 0.5 to 7 mg / m 2 (Ag-based metal powder including an Ag-based alloy, Cu-based metal powder including a Cu-based alloy), but 0.5 to 2 mg / m 2 in the case of Ag powder. In the case of Cu powder that easily oxidizes, it is preferably in the range of 2 to 7 mg / m 2 . If the specific oxygen amount exceeds 7 mg / m 2 , the increase in the thickness of the oxide film causes a decrease in the sinterability, the ductility does not increase, and the sintered body becomes brittle and easily broken. If the specific oxygen content is less than 0.5 mg / m 2 or the Cu powder has a specific oxygen content of less than 2 mg / m 2 , the C (carbon) residue in the paste is used when kneaded with resin and used as a paste. Is not preferable because it cannot be removed by burning.

前記比水分量は、1mg/m2を超えれば、異常な寸法変化や保管中の酸化・凝集を誘発するので好ましくない。 If the specific water content exceeds 1 mg / m 2 , abnormal dimensional changes and oxidation / aggregation during storage are not preferable.

なお、前記水アトマイズ装置100において、環状噴射スリット2の形状は円形の外、楕円形や三角形等の角形であってもよく、環状噴射スリット2が傾いて配置されている場合には、前記中心軸5が走る上下方向は内包面4に対して直角方向であるから、傾きを持った上下方向となり、溶融金属流6は中心軸5に沿って傾きを有して流下される。また、前記接線10は、内包面4に投影した空洞7が厚みを有している場合には空洞7の内円又は外円に対して引いた接線である。   In the water atomizing apparatus 100, the shape of the annular injection slit 2 may be a circular shape or a square shape such as an ellipse or a triangle. Since the vertical direction in which the shaft 5 runs is a direction perpendicular to the inner envelope surface 4, the vertical direction has an inclination, and the molten metal flow 6 flows down along the central axis 5 with an inclination. The tangent line 10 is a tangent line drawn with respect to the inner circle or outer circle of the cavity 7 when the cavity 7 projected onto the inner envelope surface 4 has a thickness.

実施例1〜10、比較例1〜8.   Examples 1-10, Comparative Examples 1-8.

図1〜図3に示す水アトマイズ法を採用して表3及び表4に示す条件にてCu金属粉末(実施例1〜5、比較例1〜4)とAg金属粉末(実施例6〜10、比較例5〜8)とを得た。   By adopting the water atomization method shown in FIGS. 1 to 3 under the conditions shown in Tables 3 and 4, Cu metal powder (Examples 1 to 5, Comparative Examples 1 to 4) and Ag metal powder (Examples 6 to 10) Comparative Examples 5 to 8) were obtained.

前記各金属粉末の5%径、50%径及び95%径は日機装株式会社製のマイクロトラックを使用してレーザー回折散乱法(体積%)を採用して測定した。また、比表面積はBET法による測定結果を採用した。球形度は50%径から計算できる真球の比表面積とBET法による比表面積との比により算出した。粒度幅指数はlog(95%径)−log(5%径)により算出した。例えば、実施例1では、粒度幅指数=log(0.78)−log(0.13)=−0.108−(−0.886)=0.778となり、粒度幅指数が小さいほど粒度の広がりが小さいこと、即ち、粒度幅が狭いことを示す。また、酸素量は高温でCと反応することで発生したCOガスの赤外線検出法に従って測定した。水分量はカールフィッシャー法により測定した数値によった。なお、分級は粉末毎に目標に応じた分級機で粉末毎に行った。   The 5% diameter, 50% diameter, and 95% diameter of each metal powder was measured using a laser diffraction scattering method (volume%) using a microtrack manufactured by Nikkiso Co., Ltd. The specific surface area was measured by the BET method. The sphericity was calculated from the ratio of the specific surface area of the true sphere that can be calculated from the 50% diameter to the specific surface area by the BET method. The particle size width index was calculated by log (95% diameter) -log (5% diameter). For example, in Example 1, the particle size width index = log (0.78) −log (0.13) = − 0.108 − (− 0.886) = 0.778, and the smaller the particle size width index, the smaller the particle size spread, that is, the particle size width Indicates narrow. The amount of oxygen was measured according to an infrared detection method for CO gas generated by reacting with C at high temperature. The moisture content was based on the value measured by the Karl Fischer method. In addition, classification was performed for each powder with a classifier corresponding to the target for each powder.

Figure 2007084906
Figure 2007084906

Figure 2007084906
Figure 2007084906

表中の粉末の凝集性において、「◎」は粒状の凝集がほとんどない状態、「○」は粒状の凝集は有るが均一に分散している状態、「△」は不規則な弱い凝集がある状態、「×」は不規則な強い凝集がある状態を示す。   In the agglomeration properties of the powders in the table, “◎” indicates a state in which there is almost no granular aggregation, “○” indicates a state in which granular aggregation is present but is uniformly dispersed, and “Δ” indicates irregular weak aggregation. The state, “x”, indicates a state where there is irregular strong aggregation.

寸法変化率と延性は各粉末を5MPaで厚さ約1.5×幅12×長さ30mmに成形し、表3及び表4に示す各温度、各雰囲気中で30分間焼結した後、折り曲げ試験を行った。焼結の前後での寸法変化を測定して寸法変化率を算出し、破断するまでの角度を測定して延性を判断した。表中、曲げ角90°は、90°でも破断しなかったことを表す。なお、粉末は微細なほど低い温度で焼結が進行するので、適正な焼結温度は各メジアン径で異なることから、メジアン径によって焼結温度を変更した。   The rate of dimensional change and ductility were determined by forming each powder at 5MPa in thickness of about 1.5x width 12x length 30mm, sintering for 30 minutes in each temperature and atmosphere shown in Table 3 and Table 4, and then performing a bending test. went. The dimensional change before and after sintering was measured to calculate the dimensional change rate, and the angle until fracture was measured to determine the ductility. In the table, a bending angle of 90 ° indicates that no fracture occurred even at 90 °. In addition, since sintering progresses at low temperature, so that powder is fine, since appropriate sintering temperature changes with each median diameter, sintering temperature was changed with the median diameter.

表3及び表4によれば、50%径が0.1〜5μm、球形度が0.6〜0.9、粒度幅指数が1以下、比酸素量が0.5〜7mg/m2及び比水分量が1mg/m2以下の金属粉末を焼結した場合に小さい寸法変化率と高い延性を兼ね備えた粉末が得られていた。 Table 3 and according to Table 4, the 50% size is 0.1 to 5 [mu] m, a sphericity of 0.6 to 0.9, particle size breadth index of 1 or less, the ratio of oxygen quantity 0.5~7mg / m 2 and the ratio water content 1 mg / m 2 When the following metal powder was sintered, a powder having both a small dimensional change rate and high ductility was obtained.

本発明によれば、小さな寸法変化率と良好な延性、さらには低い凝集性を満足させる金属粉末であるから、回路設計用や電子材料用の導電ペースト、マイクロMIMや造形用の粘土等、ダイヤモンド工具用バインダー等に利用できる。   According to the present invention, since it is a metal powder that satisfies a small dimensional change rate, good ductility, and low cohesiveness, conductive paste for circuit design and electronic materials, micro MIM, clay for modeling, diamond, etc. It can be used as a binder for tools.

従って、本発明の産業上利用性は非常に高いといえる。   Therefore, it can be said that the industrial applicability of the present invention is very high.

水アトマイズ法における環状噴射スリットの縦断面側面図である。It is a longitudinal cross-sectional side view of the cyclic | annular injection slit in a water atomization method. 図1に図示する環状噴射スリットから噴射される一葉双曲面状水ジェットカーテンの降下角度θを説明する図である。It is a figure explaining descent angle (theta) of the single leaf hyperboloid water jet curtain injected from the annular injection slit shown in FIG. 図1に図示する環状噴射スリットから噴射される一葉双曲面状水ジェットカーテンの旋回角度ωを説明する図である。It is a figure explaining the turning angle (omega) of the one leaf hyperboloid water jet curtain injected from the annular injection slit shown in FIG. 粒度分布曲線のグラフである。It is a graph of a particle size distribution curve.

符号の説明Explanation of symbols

1 噴射水流
2 環状噴射スリット
3 面位置
4 内包面
5 中心軸
6 溶融金属流
7 括れ状空洞
8 一部位
9 垂線
10 接線
11 径
12 一葉双曲面状水ジェットカーテン
100 水アトマイズ装置
θ 下降角度
ω 旋回角度
DESCRIPTION OF SYMBOLS 1 Jet water flow 2 Annular jet slit 3 Surface position 4 Inner surface 5 Center axis 6 Molten metal flow 7 Constricted cavity 8 One part 9 Perpendicular line 10 Tangent line 11 Diameter 12 Single-leaf hyperboloid water jet curtain 100 Water atomizing apparatus θ Descent angle ω Rotation angle

Claims (4)

50%径が0.1〜5μm、球形度が0.6〜0.9、5%径と95%径間における粒度分布の広がり相対値を表す粒度幅指数が1以下、単位表面積当りの酸素量を表す比酸素量が0.5〜7mg/m2、単位表面積当りの水分量を表す比水分量が1mg/m2以下であるAg系金属粉末。 50% diameter is 0.1-5μm, sphericity is 0.6-0.9, the spread of particle size distribution between 5% and 95% diameter is 1 or less, and the specific oxygen amount is the amount of oxygen per unit surface area. There 0.5~7mg / m 2, Ag-based metal powder ratio water quantity representing the amount of water per unit surface area of 1 mg / m 2 or less. 50%径が0.1〜5μm、球形度が0.6〜0.9、5%径と95%径間における粒度分布の広がり相対値を表す粒度幅指数が1以下、単位表面積当りの酸素量を表す比酸素量が0.5〜7mg/m2、単位表面積当りの水分量を表す比水分量が1mg/m2以下であるCu系金属粉末。 50% diameter is 0.1-5μm, sphericity is 0.6-0.9, the spread of particle size distribution between 5% and 95% diameter is 1 or less, and the specific oxygen amount is the amount of oxygen per unit surface area. There 0.5~7mg / m 2, Cu-based metal powder ratio water quantity representing the amount of water per unit surface area of 1 mg / m 2 or less. 水ジェットカーテンの噴射水流を噴射させる環状噴射スリットを下向きに配置して当該環状噴射スリットを面位置とする内包面中央を上下方向へ走る中心軸に沿って溶融金属流を流下させる工程と当該環状噴射スリットに対して高圧水流を供給して前記噴射水流が通過しない水ジェットカーテンの括れ状空洞が形成されるように環状噴射スリットの一部位から前記中心軸と平行に下ろした垂線に対する前記溶融金属流への振れ角である下降角度θと前記一部位から前記内包面に投影された前記括れ状空洞への接線と前記一部位から前記中心軸を横切る環状噴射スリットの径とが成す角である旋回角度ωとを有する向きへ水を噴射させる工程とを備えて一葉双曲面状水ジェットカーテンの噴射水流を発生させて金属粉末を製造する水アトマイズ法を採用し、前記下降角度θを0〜30°、前記旋回角度ωを1〜20°とし、水の圧力を90〜150MPa及び水の流量を300〜800L/minとして水を噴射させてAg系金属粉末を製造し、当該Ag系金属粉末を分級して50%径が0.1〜5μm、球形度が0.6〜0.9、5%径と95%径間における粒度分布の広がり相対値を表す粒度幅指数が1以下、単位表面積当りの酸素量を表す比酸素量が0.5〜7mg/m2、単位表面積当りの水分量を表す比水分量が1mg/m2以下である金属粉末を得ることを特徴とするAg系金属粉末の製造方法。 An annular injection slit for injecting the jet water flow of the water jet curtain is arranged downward and the molten metal flow is caused to flow down along the central axis that runs in the vertical direction on the center of the inner surface with the annular injection slit as the surface position. The molten metal with respect to a perpendicular drawn from one part of the annular jet slit in parallel with the central axis so as to form a constricted cavity of a water jet curtain that supplies a high-pressure water flow to the jet slit and does not allow the jet water flow to pass through The angle formed by the downward angle θ that is the deflection angle to the flow, the tangent to the constricted cavity projected from the partial position onto the inner envelope surface, and the diameter of the annular injection slit that crosses the central axis from the partial position A water atomization method for producing metal powder by generating a jet flow of a single leaf hyperboloid water jet curtain with a step of jetting water in a direction having a swivel angle ω The descent angle θ is 0 to 30 °, the turning angle ω is 1 to 20 °, the water pressure is 90 to 150 MPa, the water flow rate is 300 to 800 L / min, and water is injected to form an Ag system. Particle size index indicating the relative value of the distribution of the particle size distribution between the 5% and 95% diameters by producing the metal powder and classifying the Ag-based metal powder with a 50% diameter of 0.1 to 5 μm, a sphericity of 0.6 to 0.9, but less than 1, and characterized in that 0.5~7mg / m 2 ratio of oxygen quantity representing the amount of oxygen per unit surface area, the specific amount of water which represents the water content per unit surface area to obtain a metal powder is 1 mg / m 2 or less A method for producing an Ag-based metal powder. 水ジェットカーテンの噴射水流を噴射させる環状噴射スリットを下向きに配置して当該環状噴射スリットを面位置とする内包面中央を上下方向へ走る中心軸に沿って溶融金属流を流下させる工程と当該環状噴射スリットに対して高圧水流を供給して前記噴射水流が通過しない水ジェットカーテンの括れ状空洞が形成されるように環状噴射スリットの一部位から前記中心軸と平行に下ろした垂線に対する前記溶融金属流への振れ角である下降角度θと前記一部位から前記内包面に投影された前記括れ状空洞への接線と前記一部位から前記中心軸を横切る環状噴射スリットの径とが成す角である旋回角度ωとを有する向きへ水を噴射させる工程とを備えて一葉双曲面状水ジェットカーテンの噴射水流を発生させて金属粉末を製造する水アトマイズ法を採用し、前記下降角度θを0〜30°、前記旋回角度ωを1〜20°とし、水の圧力を90〜150MPa及び水の流量を300〜800L/minとして水を噴射させてCu系金属粉末を製造し、当該Cu系金属粉末を分級して50%径が0.1〜5μm、球形度が0.6〜0.9、5%径と95%径間における粒度分布の広がり相対値を表す粒度幅指数が1以下、単位表面積当りの酸素量を表す比酸素量が0.5〜7mg/m2、単位表面積当りの水分量を表す比水分量が1mg/m2以下である金属粉末を得ることを特徴とするCu系金属粉末の製造方法。
An annular injection slit for injecting the jet water flow of the water jet curtain is arranged downward and the molten metal flow is caused to flow down along the central axis that runs in the vertical direction on the center of the inner surface with the annular injection slit as the surface position. The molten metal with respect to a perpendicular drawn from one part of the annular jet slit in parallel with the central axis so as to form a constricted cavity of a water jet curtain that supplies a high-pressure water flow to the jet slit and does not allow the jet water flow to pass through The angle formed by the downward angle θ that is the deflection angle to the flow, the tangent to the constricted cavity projected from the partial position onto the inner envelope surface, and the diameter of the annular injection slit that crosses the central axis from the partial position A water atomization method for producing metal powder by generating a jet flow of a single leaf hyperboloid water jet curtain with a step of jetting water in a direction having a swivel angle ω The lowering angle θ is 0 to 30 °, the turning angle ω is 1 to 20 °, the water pressure is 90 to 150 MPa and the water flow rate is 300 to 800 L / min. A particle size index representing the relative value of the distribution of particle size distribution between a 5% diameter and a 95% diameter by producing a metal powder and classifying the Cu-based metal powder with a 50% diameter of 0.1-5 μm, a sphericity of 0.6-0.9, and a 5% diameter and a 95% diameter but less than 1, and characterized in that 0.5~7mg / m 2 ratio of oxygen quantity representing the amount of oxygen per unit surface area, the specific amount of water which represents the water content per unit surface area to obtain a metal powder is 1 mg / m 2 or less A method for producing Cu-based metal powder.
JP2005278180A 2005-09-26 2005-09-26 Ag-based metal powder, Cu-based metal powder and method for producing the same Pending JP2007084906A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2005278180A JP2007084906A (en) 2005-09-26 2005-09-26 Ag-based metal powder, Cu-based metal powder and method for producing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2005278180A JP2007084906A (en) 2005-09-26 2005-09-26 Ag-based metal powder, Cu-based metal powder and method for producing the same

Publications (1)

Publication Number Publication Date
JP2007084906A true JP2007084906A (en) 2007-04-05

Family

ID=37972183

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2005278180A Pending JP2007084906A (en) 2005-09-26 2005-09-26 Ag-based metal powder, Cu-based metal powder and method for producing the same

Country Status (1)

Country Link
JP (1) JP2007084906A (en)

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009167491A (en) * 2008-01-18 2009-07-30 Fukuda Metal Foil & Powder Co Ltd Metal powder excellent in sinterability, method for producing the same, and method for producing a sintered body using the metal powder
JP2009224201A (en) * 2008-03-17 2009-10-01 Kyoto Elex Kk Conductive paste for low-temperature baked multilayer board
CN103111625A (en) * 2013-03-19 2013-05-22 南京理工大学 Method of improving sphericity degree of metal powder prepared through water atomization
CN103128292A (en) * 2011-11-28 2013-06-05 重庆华浩冶炼有限公司 Copper bead catalyst and preparation method thereof
KR101600881B1 (en) * 2015-01-05 2016-03-09 공주대학교 산학협력단 Multi Cooling System for Producing Metal and Alloy Spherical Powders
JP2016084487A (en) * 2014-10-23 2016-05-19 Dowaエレクトロニクス株式会社 Metal powder and method for producing the same
KR20160084530A (en) * 2015-01-05 2016-07-14 공주대학교 산학협력단 Multi Cooling System for Producing Metal and Alloy Spherical Powders
JP2016216832A (en) * 2011-05-18 2016-12-22 戸田工業株式会社 Copper powder, copper paste, production method of conductive coating film, and conductive coating film
JP2016216824A (en) * 2015-05-18 2016-12-22 Dowaエレクトロニクス株式会社 Silver powder and method for producing the same
WO2017073057A1 (en) * 2015-10-30 2017-05-04 Dowaエレクトロニクス株式会社 Silver powder and method for producing same
JP2017082327A (en) * 2015-10-30 2017-05-18 Dowaエレクトロニクス株式会社 Silver powder and method for producing the same
WO2017115462A1 (en) * 2015-12-28 2017-07-06 Dowaエレクトロニクス株式会社 Silver alloy powder and method for producing same
JP2017119913A (en) * 2015-12-28 2017-07-06 Dowaエレクトロニクス株式会社 Silver alloy powder and method for producing the same
JPWO2016125355A1 (en) * 2015-02-06 2017-07-27 トクセン工業株式会社 Conductive fine particles
CN110614377A (en) * 2019-10-31 2019-12-27 江西铜业铜材有限公司 Production process for preparing copper powder by using SCR (Selective catalytic reduction) shaft furnace system
CN111014657A (en) * 2019-12-30 2020-04-17 吉林大学 FeCuNiSn alloy powder for diamond products and preparation method thereof
JPWO2019017467A1 (en) * 2017-07-21 2020-05-28 三井金属鉱業株式会社 Copper powder, method of manufacturing stereolithography product using the same, and stereolithography product of copper
CN112589109A (en) * 2020-11-27 2021-04-02 佛山市中研非晶科技股份有限公司 Gas atomization powder making method and gas atomization powder making system using same

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005008930A (en) * 2003-06-18 2005-01-13 Nippon Atomized Metal Powers Corp Metal powder, metal powder manufacturing apparatus and metal powder manufacturing method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005008930A (en) * 2003-06-18 2005-01-13 Nippon Atomized Metal Powers Corp Metal powder, metal powder manufacturing apparatus and metal powder manufacturing method

Cited By (31)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009167491A (en) * 2008-01-18 2009-07-30 Fukuda Metal Foil & Powder Co Ltd Metal powder excellent in sinterability, method for producing the same, and method for producing a sintered body using the metal powder
JP2009224201A (en) * 2008-03-17 2009-10-01 Kyoto Elex Kk Conductive paste for low-temperature baked multilayer board
JP2016216832A (en) * 2011-05-18 2016-12-22 戸田工業株式会社 Copper powder, copper paste, production method of conductive coating film, and conductive coating film
CN103128292A (en) * 2011-11-28 2013-06-05 重庆华浩冶炼有限公司 Copper bead catalyst and preparation method thereof
CN103111625A (en) * 2013-03-19 2013-05-22 南京理工大学 Method of improving sphericity degree of metal powder prepared through water atomization
JP2016084487A (en) * 2014-10-23 2016-05-19 Dowaエレクトロニクス株式会社 Metal powder and method for producing the same
KR101600881B1 (en) * 2015-01-05 2016-03-09 공주대학교 산학협력단 Multi Cooling System for Producing Metal and Alloy Spherical Powders
KR20160084530A (en) * 2015-01-05 2016-07-14 공주대학교 산학협력단 Multi Cooling System for Producing Metal and Alloy Spherical Powders
KR101667204B1 (en) * 2015-01-05 2016-10-19 공주대학교 산학협력단 Multi Cooling System for Producing Metal and Alloy Spherical Powders
JPWO2016125355A1 (en) * 2015-02-06 2017-07-27 トクセン工業株式会社 Conductive fine particles
JP2016216824A (en) * 2015-05-18 2016-12-22 Dowaエレクトロニクス株式会社 Silver powder and method for producing the same
JP7110421B2 (en) 2015-10-30 2022-08-01 Dowaエレクトロニクス株式会社 Silver powder and its manufacturing method
KR102446788B1 (en) 2015-10-30 2022-09-22 도와 일렉트로닉스 가부시키가이샤 Silver powder and its manufacturing method
JP2017082327A (en) * 2015-10-30 2017-05-18 Dowaエレクトロニクス株式会社 Silver powder and method for producing the same
KR20180075582A (en) * 2015-10-30 2018-07-04 도와 일렉트로닉스 가부시키가이샤 Silver powder and method for producing the same
US10828702B2 (en) 2015-10-30 2020-11-10 Dowa Electronics Materials Co., Ltd. Silver powder and method for producing same
US11407030B2 (en) 2015-10-30 2022-08-09 Dowa Electronics Materials Co., Ltd. Silver powder and method for producing same
WO2017073057A1 (en) * 2015-10-30 2017-05-04 Dowaエレクトロニクス株式会社 Silver powder and method for producing same
JP2021075799A (en) * 2015-10-30 2021-05-20 Dowaエレクトロニクス株式会社 Silver powder and method for producing the same
JP2017119913A (en) * 2015-12-28 2017-07-06 Dowaエレクトロニクス株式会社 Silver alloy powder and method for producing the same
WO2017115462A1 (en) * 2015-12-28 2017-07-06 Dowaエレクトロニクス株式会社 Silver alloy powder and method for producing same
JPWO2019017467A1 (en) * 2017-07-21 2020-05-28 三井金属鉱業株式会社 Copper powder, method of manufacturing stereolithography product using the same, and stereolithography product of copper
JP7143223B2 (en) 2017-07-21 2022-09-28 三井金属鉱業株式会社 Copper powder, method for manufacturing stereolithographic object using the same, and stereolithographic object using copper
JP2022172242A (en) * 2017-07-21 2022-11-15 三井金属鉱業株式会社 Copper powder, method for manufacturing stereolithographic object using the same, and stereolithographic object using copper
JP7377324B2 (en) 2017-07-21 2023-11-09 三井金属鉱業株式会社 Copper powder, method for manufacturing a stereolithographic object using the same, and stereolithographic object using copper
CN110614377A (en) * 2019-10-31 2019-12-27 江西铜业铜材有限公司 Production process for preparing copper powder by using SCR (Selective catalytic reduction) shaft furnace system
CN110614377B (en) * 2019-10-31 2022-06-10 江西铜业铜材有限公司 Production process for preparing copper powder by using SCR (Selective catalytic reduction) shaft furnace system
CN111014657B (en) * 2019-12-30 2021-08-27 吉林大学 FeCuNiSn alloy powder for diamond product and preparation method thereof
CN111014657A (en) * 2019-12-30 2020-04-17 吉林大学 FeCuNiSn alloy powder for diamond products and preparation method thereof
CN112589109B (en) * 2020-11-27 2022-03-25 佛山市中研非晶科技股份有限公司 Gas atomization powder making method and gas atomization powder making system using same
CN112589109A (en) * 2020-11-27 2021-04-02 佛山市中研非晶科技股份有限公司 Gas atomization powder making method and gas atomization powder making system using same

Similar Documents

Publication Publication Date Title
JP2007084906A (en) Ag-based metal powder, Cu-based metal powder and method for producing the same
US11840750B2 (en) Tungsten heavy metal alloy powders and methods of forming them
KR100545821B1 (en) Highly crystalline metal powder, manufacturing method thereof, ceramic paste containing the metal powder and ceramic laminated electronic component using conductor paste
JP7039126B2 (en) Copper powder and its manufacturing method
JP6817615B2 (en) Metal powder manufacturing method and metal powder manufacturing equipment
JP4264873B2 (en) Method for producing fine metal powder by gas atomization method
WO1999011407A1 (en) Method of producing metal powder by atomizing and apparatus therefor
Soong et al. Atomization of metal and alloy powders: Processes, parameters, and properties
JP4613362B2 (en) Metal powder for conductive paste and conductive paste
CN116475407A (en) Low melting point metal or alloy powder atomization production process
JP5181434B2 (en) Fine copper powder and method for producing the same
CN108473335A (en) Method for producing titanium oxide fine particles of no specific ratio
KR102294895B1 (en) Fine silver particle
KR102397204B1 (en) Copper powder and its manufacturing method
JP2005008930A (en) Metal powder, metal powder manufacturing apparatus and metal powder manufacturing method
Schade et al. Atomization
CN204818071U (en) Preparation metal spherical powder's for vibration material disk device
JP2002343135A (en) Copper powder for conductive paste, conductive paste, and method for producing copper powder for conductive paste
JP2009167491A (en) Metal powder excellent in sinterability, method for producing the same, and method for producing a sintered body using the metal powder
JP4425888B2 (en) Nano-spherical particles having a composite structure, powder, and manufacturing method thereof
JP4888769B2 (en) Copper powder and method for producing the same
JP4642487B2 (en) Thermal spray powder
JP2004169056A (en) Copper powder for conductive paste, conductive paste, and method for producing copper powder for conductive paste
JP6618749B2 (en) Thermal spray powder and method of forming thermal spray coating
JPWO2019124047A1 (en) Spherical Ti powder and its manufacturing method

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20080605

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20100427

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20100622

A02 Decision of refusal

Free format text: JAPANESE INTERMEDIATE CODE: A02

Effective date: 20110524