JP2009068086A - Electrically conductive composite powder and method for producing the same - Google Patents
Electrically conductive composite powder and method for producing the same Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 87
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 129
- 239000000956 alloy Substances 0.000 claims abstract description 129
- 239000012071 phase Substances 0.000 claims abstract description 56
- 239000007791 liquid phase Substances 0.000 claims abstract description 38
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 229910052709 silver Inorganic materials 0.000 claims abstract description 19
- 229910052802 copper Inorganic materials 0.000 claims abstract description 13
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 12
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims abstract description 7
- 229910002482 Cu–Ni Inorganic materials 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 25
- 229910017827 Cu—Fe Inorganic materials 0.000 claims description 12
- 229910017816 Cu—Co Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 11
- 239000011231 conductive filler Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 8
- 239000004332 silver Substances 0.000 abstract description 7
- 239000010949 copper Substances 0.000 description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 24
- 239000002245 particle Substances 0.000 description 19
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 6
- 239000006104 solid solution Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000005191 phase separation Methods 0.000 description 5
- 238000009689 gas atomisation Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 229910002701 Ag-Co Inorganic materials 0.000 description 1
- 229910017937 Ag-Ni Inorganic materials 0.000 description 1
- 229910017984 Ag—Ni Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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Abstract
Description
本発明は、導電性複合粉末およびその製造方法に関し、特に、導電性ペーストに使用する導電性複合粉末およびその製造方法に関する。 The present invention relates to a conductive composite powder and a method for producing the same, and particularly relates to a conductive composite powder used for a conductive paste and a method for producing the same.
従来、積層コンデンサの内部電極、回路基板の導体パターン、太陽電池やフラットパネルディスプレイ（ＦＰＤ）用基板の電極や回路などの電子部品に使用する導電性ペーストとして、銀粉をガラスフリットとともに有機ビヒクル中に加えて混練することによって製造される導電性ペーストが使用されている。 Conventionally, silver powder is put together with glass frit in an organic vehicle as a conductive paste used for internal electrodes of multilayer capacitors, conductor patterns of circuit boards, electrodes of solar cells and flat panel display (FPD) boards, and circuits. In addition, a conductive paste produced by kneading is used.
近年、ＦＰＤの生産量の著しい増大に伴い、その電極材料などに使用される導電性ペーストの使用量も著しく増大し、その導電性フィラー材料として使用される銀粉の使用量も著しく増大している。そのため、銀の価格が高騰したり、資源の枯渇が懸念されており、銀粉に代わる新しい導電性フィラー材料を開発することが望まれている。 In recent years, with a significant increase in the production amount of FPD, the amount of conductive paste used for the electrode material and the like has also increased significantly, and the amount of silver powder used as the conductive filler material has also increased significantly. . For this reason, there is a concern that the price of silver will rise or that resources will be depleted, and it is desired to develop a new conductive filler material that can replace silver powder.
このような新しい導電性フィラー材料の一つとして、銅やニッケルなどの微粉末の表面に銀をコートした銀コート導電性粉末が提案されている（例えば、特許文献１参照）。 As one of such new conductive filler materials, a silver-coated conductive powder in which silver is coated on the surface of a fine powder such as copper or nickel has been proposed (for example, see Patent Document 1).
しかし、特許文献１の方法では、母体となる金属粉末を作製した後に、その金属粉末の表面に無電解めっきによって銀をコートする複数の工程が必要になるため、製造プロセスが煩雑であり、コストも高くなるという問題がある。そのため、銀粉と比べて大幅な省資源化を図ることができるだけでなく、製造プロセスの大幅な簡略化によるコストダウンも図ることができる導電性フィラー材料を開発することが望まれている。 However, in the method of Patent Document 1, since a plurality of steps of coating the surface of the metal powder by electroless plating is necessary after the metal powder as the base is manufactured, the manufacturing process is complicated and costly There is a problem that it becomes higher. Therefore, it is desired to develop a conductive filler material that not only can save resources significantly compared to silver powder, but also can reduce costs by greatly simplifying the manufacturing process.
したがって、本発明は、このような従来の問題点に鑑み、導電性ペースト用の導電性フィラー材料として使用することができるとともに、銀の使用量を削減して安価且つ容易に製造することができる、導電性複合粉末およびその製造方法を提供することを目的とする。 Therefore, the present invention can be used as a conductive filler material for a conductive paste in view of such conventional problems, and can be manufactured inexpensively and easily by reducing the amount of silver used. An object of the present invention is to provide a conductive composite powder and a method for producing the same.
本発明者らは、上記課題を解決するために鋭意研究した結果、ＡｇとＣｕとＸ（ＸはＮｉ、ＦｅまたはＣｏ）とからなり、三元系において液相の二相領域内の組成を有するＡｇ−Ｃｕ−Ｘ合金の溶湯を噴霧して急冷して、Ａｇマトリックス中にＣｕ−Ｘ基合金の微細な分散相が分散した組織およびＣｕ−Ｘリッチ相からなるコア部がＡｇリッチ相によって取り囲まれた組織の少なくとも一方の組織を有する導電性複合粉末を製造することにより、導電性ペースト用の導電性フィラー材料として使用することができるとともに、銀の使用量を削減して安価且つ容易に製造することができる、導電性複合粉末およびその製造方法を提供することができることを見出し、本発明を完成するに至った。 As a result of diligent research to solve the above problems, the inventors of the present invention are composed of Ag, Cu, and X (X is Ni, Fe, or Co), and the composition in the two-phase region of the liquid phase in the ternary system. The molten Ag-Cu-X alloy is sprayed and rapidly cooled, and the Ag-rich phase has a structure in which the fine dispersed phase of the Cu-X-based alloy is dispersed in the Ag matrix and the core portion made of the Cu-X-rich phase. By producing a conductive composite powder having at least one of the surrounded structures, it can be used as a conductive filler material for conductive paste, and the amount of silver used can be reduced and cheaply and easily. It has been found that a conductive composite powder and a method for producing the same can be provided, and the present invention has been completed.
すなわち、本発明による導電性複合粉末の製造方法は、ＡｇとＣｕとＸ（ＸはＮｉ、ＦｅまたはＣｏ）とからなり、三元系において液相の二相領域内の組成を有するＡｇ−Ｃｕ−Ｘ合金の溶湯を噴霧して急冷して、Ａｇマトリックス中にＣｕ−Ｘ基合金の微細な分散相が分散した組織およびＣｕ−Ｘリッチ相からなるコア部がＡｇリッチ相によって取り囲まれた組織の少なくとも一方の組織を有する導電性複合粉末を製造することを特徴とする。 That is, the method for producing a conductive composite powder according to the present invention comprises Ag, Cu, and X (X is Ni, Fe, or Co), and has a composition in a liquid phase two-phase region in a ternary system. A structure in which a fine dispersed phase of a Cu-X based alloy is dispersed in an Ag matrix and a core part composed of a Cu-X rich phase surrounded by the Ag rich phase by spraying a molten metal of -X alloy A conductive composite powder having at least one of the following structures is produced.
この導電性複合粉末の製造方法において、Ａｇ−Ｃｕ−Ｘ合金が、３．６〜９６．８質量％のＡｇと０．１〜４０．０質量％のＣｕと０．１〜９６．２質量％のＮｉとからなるＡｇ−Ｃｕ−Ｎｉ合金、２０．０質量％を超え且つ９６．８質量％以下のＡｇと０．１〜４０．０質量％のＣｕと１．０〜９６．０質量％のＦｅとからなるＡｇ−Ｃｕ−Ｆｅ合金、あるいは、２０．０質量％を超え且つ９６．８質量％以下のＡｇと０．１〜４０．０質量％のＣｕと１．１〜９６．２質量％のＣｏとからなるＡｇ−Ｃｕ−Ｃｏ合金であるのが好ましい。 In this method for producing a conductive composite powder, the Ag—Cu—X alloy contains 3.6 to 96.8% by mass of Ag, 0.1 to 40.0% by mass of Cu, and 0.1 to 96.2% by mass. Ag-Cu-Ni alloy composed of 2% Ni, more than 20.0% by mass and up to 96.8% by mass Ag, 0.1-40.0% by mass Cu and 1.0-96.0% by mass % Ag-Cu-Fe alloy, or more than 20.0 mass% and not more than 96.8 mass% Ag, 0.1-40.0 mass% Cu, and 1.1-96. An Ag—Cu—Co alloy composed of 2 mass% Co is preferable.
また、本発明による導電性複合粉末は、ＡｇとＣｕとＸ（ＸはＮｉ、ＦｅまたはＣｏ）とからなるＡｇ−Ｃｕ−Ｘ合金粉末であり、三元系において液相の二相領域内の組成を有し、Ａｇマトリックス中にＣｕ−Ｘ基合金の微細な分散相が分散した組織およびＣｕ−Ｘリッチ相からなるコア部がＡｇリッチ相によって取り囲まれた組織の少なくとも一方の組織を有することを特徴とする。 The conductive composite powder according to the present invention is an Ag-Cu-X alloy powder composed of Ag, Cu, and X (X is Ni, Fe, or Co), and is in a two-phase region of a liquid phase in a ternary system. The composition has a structure in which a fine dispersed phase of a Cu-X-based alloy is dispersed in an Ag matrix and a core portion composed of a Cu-X rich phase is surrounded by an Ag rich phase. It is characterized by.
この導電性複合粉末において、Ａｇ−Ｃｕ−Ｘ合金粉末が、３．６〜９６．８質量％のＡｇと０．１〜４０．０質量％のＣｕと０．１〜９６．２質量％のＮｉとからなるＡｇ−Ｃｕ−Ｎｉ合金、２０．０質量％を超え且つ９６．８質量％以下のＡｇと０．１〜４０．０質量％のＣｕと１．０〜９６．０質量％のＦｅとからなるＡｇ−Ｃｕ−Ｆｅ合金、あるいは、２０．０質量％を超え且つ９６．８質量％以下のＡｇと０．１〜４０．０質量％のＣｕと１．１〜９６．２質量％のＣｏとからなるＡｇ−Ｃｕ−Ｃｏ合金であるのが好ましい。 In this conductive composite powder, the Ag—Cu—X alloy powder comprises 3.6 to 96.8% by mass of Ag, 0.1 to 40.0% by mass of Cu, and 0.1 to 96.2% by mass. Ag—Cu—Ni alloy composed of Ni, more than 20.0% by mass and up to 96.8% by mass of Ag, 0.1 to 40.0% by mass of Cu, and 1.0 to 96.0% by mass of Ni Ag—Cu—Fe alloy composed of Fe, or more than 20.0 mass% and not more than 96.8 mass% of Ag, 0.1 to 40.0 mass% of Cu, and 1.1 to 96.2 mass An Ag—Cu—Co alloy composed of% Co is preferable.
本発明によれば、導電性ペースト用の導電性フィラー材料として使用することができるとともに、銀の使用量を削減して安価且つ容易に製造することができる、導電性複合粉末およびその製造方法を提供することができる。 According to the present invention, there is provided a conductive composite powder that can be used as a conductive filler material for a conductive paste, and can be manufactured inexpensively and easily by reducing the amount of silver used, and a method for manufacturing the same. Can be provided.
本発明による導電性複合粉末の製造方法の実施の形態では、ＡｇとＣｕとＸ（ＸはＮｉ、ＦｅまたはＣｏ）とからなり、三元系において液相の二相領域内の組成を有するＡｇ−Ｃｕ−Ｘ合金の溶湯を、ガスアトマイズ法により急冷微粉化することによって、Ａｇマトリックス中にＣｕ−Ｘ基合金の微細な分散相が分散した組織（以下「分散型組織」という）およびＣｕ−Ｘリッチ相からなるコア部が（耐酸化性に富み且つ高導電率を有する）Ａｇリッチ相によって取り囲まれた組織（粒径数１０μｍのＣｕ−Ｘ合金微粒子の表面が厚さ数μｍのＡｇで覆われた二重構造の組織（以下「卵型分離組織」という））の少なくとも一方の組織を有する導電性複合粉末を製造する。なお、ガスアトマイズ法による急冷では、例えば、通常のアトマイズ装置における冷却速度にすればよい。 In the embodiment of the method for producing a conductive composite powder according to the present invention, Ag is composed of Ag, Cu and X (X is Ni, Fe or Co), and has a composition in a liquid phase two-phase region in a ternary system. A structure in which a fine dispersed phase of a Cu—X based alloy is dispersed in an Ag matrix (hereinafter referred to as “dispersed structure”) and Cu—X by rapidly cooling and pulverizing the molten Cu—X alloy by a gas atomization method. The structure (the surface of the Cu-X alloy fine particles having a particle diameter of several tens of μm is covered with Ag having a thickness of several μm, and the core portion made of the rich phase is surrounded by the Ag rich phase (which has high oxidation resistance and high conductivity). A conductive composite powder having at least one tissue of a broken double structure (hereinafter referred to as “egg-type separated tissue”) is produced. In the rapid cooling by the gas atomizing method, for example, the cooling rate in a normal atomizing apparatus may be used.
この導電性複合粉末の製造方法において、Ａｇ−Ｃｕ−Ｘ合金が、３．６〜９６．８質量％のＡｇと０．１〜４０．０質量％のＣｕと０．１〜９６．２質量％のＮｉとからなるＡｇ−Ｃｕ−Ｎｉ合金、２０．０質量％を超え且つ９６．８質量％以下のＡｇと０．１〜４０．０質量％のＣｕと１．０〜９６．０質量％のＦｅとからなるＡｇ−Ｃｕ−Ｆｅ合金、あるいは、２０．０質量％を超え且つ９６．８質量％以下のＡｇと０．１〜４０．０質量％のＣｕと１．１〜９６．２質量％のＣｏとからなるＡｇ−Ｃｕ−Ｃｏ合金であるのが好ましい。 In this method for producing a conductive composite powder, the Ag—Cu—X alloy contains 3.6 to 96.8% by mass of Ag, 0.1 to 40.0% by mass of Cu, and 0.1 to 96.2% by mass. Ag-Cu-Ni alloy composed of 2% Ni, more than 20.0% by mass and up to 96.8% by mass Ag, 0.1-40.0% by mass Cu and 1.0-96.0% by mass % Ag-Cu-Fe alloy, or more than 20.0 mass% and not more than 96.8 mass% Ag, 0.1-40.0 mass% Cu, and 1.1-96. An Ag—Cu—Co alloy composed of 2 mass% Co is preferable.
Ａｇ−Ｃｕ−Ｎｉ合金の場合には、Ａｇ含有量が３．６質量％未満であると、Ａｇ量が少な過ぎてＡｇが分散できなくなり、９６．８質量％を越えると、Ａｇ量が多過ぎてＡｇの固溶体になってしまう。また、Ｃｕ含有量が１．０質量％未満であると、Ａｇ−Ｎｉの液相の二相分離領域になって導電性が低下し、４０．０質量％を越えると、Ａｇ−Ｃｕ−Ｎｉの三元系における液相の二相分離領域から外れてしまう。また、Ｎｉ含有量が０．１質量％未満であると、Ｎｉ量が少な過ぎてＡｇの固溶体になり、９６．２質量％を超えると、Ｎｉ量が多過ぎてＡｇが分散できなくなってしまう。 In the case of an Ag—Cu—Ni alloy, if the Ag content is less than 3.6% by mass, the Ag content is too small to disperse Ag, and if it exceeds 96.8% by mass, the Ag content is large. After that, it becomes a solid solution of Ag. Further, if the Cu content is less than 1.0% by mass, it becomes a two-phase separation region of the liquid phase of Ag—Ni, and the conductivity is lowered. If it exceeds 40.0% by mass, the Ag—Cu—Ni Of the liquid phase in the ternary system. Further, when the Ni content is less than 0.1% by mass, the Ni content is too small to form a solid solution of Ag. When the Ni content exceeds 96.2% by mass, the Ni content is excessive and Ag cannot be dispersed. .
Ａｇ−Ｃｕ−Ｆｅ合金の場合には、Ａｇ含有量が２０．０質量未満であると、Ａｇ量が少な過ぎてＡｇが分散できなくなり、９６．８質量％を超えると、Ａｇ量が多過ぎてＡｇの固溶体になってしまう。また、Ｃｕ含有量が１．０質量％未満であると、Ａｇ−Ｆｅの液相の二相分離領域になって導電性が低下し、４０．０質量％を超えると、Ａｇ−Ｃｕ−Ｆｅの三元系における液相の二相分離領域から外れてしまう。また、Ｆｅ含有量が１．０質量％未満であると、Ｆｅ量が少な過ぎてＡｇの固溶体になり、９６．０質量％を超えると、Ｆｅ量が多過ぎてＡｇが分散できなくなってしまう。 In the case of an Ag—Cu—Fe alloy, if the Ag content is less than 20.0 mass, the Ag content is too small to disperse Ag, and if it exceeds 96.8 mass%, the Ag content is too large. It becomes a solid solution of Ag. Moreover, when Cu content is less than 1.0 mass%, it will become a two-phase separation area | region of the liquid phase of Ag-Fe, and electroconductivity will fall, and when it exceeds 40.0 mass%, it will be Ag-Cu-Fe. Of the liquid phase in the ternary system. Further, when the Fe content is less than 1.0% by mass, the Fe content is too small to be a solid solution of Ag, and when it exceeds 96.0% by mass, the Fe content is too large to disperse Ag. .
Ａｇ−Ｃｕ−Ｃｏ合金の場合には、Ａｇ含有量が２０％質量未満であると、Ａｇ量が少な過ぎてＡｇが分散できなくなり、９６．８質量％を超えると、Ａｇ量が多過ぎてＡｇの固溶体になってしまう。また、Ｃｕ含有量が０．１％未満であると、Ａｇ−Ｃｏの液相の二相分離領域となって導電性が低下し、４０．０質量％を超えると、Ａｇ−Ｃｕ−Ｃｏの三元系における液相の二相分離領域から外れてしまう。また、Ｃｏ含有量が１．１質量％未満であると、Ｃｏ量が少な過ぎてＡｇの固溶体になり、９６．２質量％を超えると、Ｃｏ量が多過ぎてＡｇが分散できなくなってしまう。 In the case of an Ag-Cu-Co alloy, if the Ag content is less than 20% by mass, the Ag content is too small to disperse Ag, and if it exceeds 96.8% by mass, the Ag content is too large. It becomes a solid solution of Ag. Further, when the Cu content is less than 0.1%, it becomes a two-phase separation region of the liquid phase of Ag—Co, and the conductivity is reduced. When the Cu content exceeds 40.0% by mass, the Ag—Cu—Co The liquid phase in the ternary system deviates from the two-phase separation region. Further, if the Co content is less than 1.1% by mass, the Co content is too small to form a solid solution of Ag, and if it exceeds 96.2% by mass, the Co content is too large to disperse Ag. .
本発明による導電性複合粉末の製造方法の実施の形態によって製造される導電性複合粉末は、ＡｇとＣｕとＸ（ＸはＮｉ、ＦｅまたはＣｏ）の液相の二相分離を示す合金組成から得られる導電性複合粉末である。 The conductive composite powder manufactured by the embodiment of the method for manufacturing the conductive composite powder according to the present invention is obtained from an alloy composition showing two-phase separation of liquid phases of Ag, Cu and X (X is Ni, Fe or Co). The resulting conductive composite powder.
例えば、Ａｇ−Ｃｕ−Ｎｉ合金の場合、上述した組成のＡｇ−Ｃｕ−Ｎｉ合金の溶湯は、１５００〜２３００℃程度の高温で保持されると、Ａｇの液相とＣｕ−Ｎｉの液相に分離した状態になり、高周波で攪拌するとドレッシングを振ったような状態になる。この状態で急冷して凝固させると、マランゴニ効果を示しながら凝固するため、組成や冷却条件によって分散型組織や卵型分離組織の形態になる。得られた導電性複合粉末の表面は、大部分がＡｇ相を有する形態になる。一方、Ａｇ−Ｃｕ−Ｎｉ合金の溶湯の組成が、高温で保持されたときに単一液相になる組成である場合には、組織の形成過程が異なる。すなわち、単一液相（Ａｇ＋Ｃｕ＋Ｎｉ）になる組成のＡｇ−Ｃｕ−Ｎｉ合金の溶湯を冷却して凝固させると、Ａｇ液相中にＣｕ−Ｎｉの固相が初晶として析出凝固し、その冷却凝固中にＡｇ液相も凝固するため、初晶＋ラメラーの複合凝固組織（以下「凝固組織」という）になる。 For example, in the case of an Ag—Cu—Ni alloy, if the molten Ag—Cu—Ni alloy having the above-described composition is held at a high temperature of about 1500 to 2300 ° C., the liquid phase of Ag and the liquid phase of Cu—Ni It becomes a separated state, and when it is stirred at a high frequency, it becomes a state where the dressing is shaken. When solidified by rapid cooling in this state, it solidifies while exhibiting the Marangoni effect, so that it becomes a dispersed tissue or egg-shaped separated tissue depending on the composition and cooling conditions. Most of the surface of the obtained conductive composite powder is in a form having an Ag phase. On the other hand, when the composition of the molten Ag-Cu-Ni alloy is a composition that becomes a single liquid phase when held at a high temperature, the formation process of the structure is different. That is, when a molten Ag—Cu—Ni alloy having a composition that becomes a single liquid phase (Ag + Cu + Ni) is cooled and solidified, a solid phase of Cu—Ni is precipitated and solidified as an initial crystal in the Ag liquid phase. Since the Ag liquid phase also solidifies during solidification, it becomes a primary solid + lamellar composite solidified structure (hereinafter referred to as “solidified structure”).
以下、本発明による導電性複合粉末およびその製造方法の実施例について詳細に説明する。 Hereinafter, the Example of the electroconductive composite powder by this invention and its manufacturing method is described in detail.
［実施例１］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、７６．３質量％のＡｇと１７．３質量％のＣｕと６．４質量％のＮｉからなるＡｇ−Ｃｕ−Ｎｉ合金を用意し、高周波誘導溶解して融液温度１６００℃の溶融物（混合溶湯）とした。
[Example 1]
As an Ag-Cu-X base alloy, it has a composition in a two-phase region of a liquid phase in a ternary system, and consists of 76.3% by mass of Ag, 17.3% by mass of Cu and 6.4% by mass of Ni. An Ag—Cu—Ni alloy was prepared and melted at high frequency to obtain a melt (mixed molten metal) having a melt temperature of 1600 ° C.
次に、この溶融物をＡｒガスによる高圧ガスアトマイズ法によってガス圧５ＭＰａで噴霧急冷（凝固）して、平均粒径１５０μｍ以下の合金粉末を得た。 Next, this melt was spray-quenched (solidified) at a gas pressure of 5 MPa by a high-pressure gas atomization method using Ar gas to obtain an alloy powder having an average particle size of 150 μm or less.
得られた合金粉末の粒子断面組織を図１の金属顕微鏡写真に示す。図１に示すように、合金粉末の組織は、Ａｇマトリックス中にＣｕ−Ｎｉ基合金の多数の微細な分散相が分散した組織（分散型組織）であることがわかった。 The metal cross-sectional structure of the obtained alloy powder is shown in the metal micrograph of FIG. As shown in FIG. 1, the structure of the alloy powder was found to be a structure (dispersed structure) in which many fine dispersed phases of the Cu—Ni-based alloy were dispersed in an Ag matrix.
また、得られた合金粉末を４５ＭＰａで直径１５ｍｍの円盤状に圧縮成型し、真空雰囲気中において９００℃で１分間熱処理した後、氷水中に焼入れして、得られた焼結合金の電気抵抗を四端子法により室温で測定したところ、比抵抗は２．４０μΩ・ｃｍであった。 Further, the obtained alloy powder is compression-molded into a disk shape having a diameter of 15 mm at 45 MPa, heat-treated at 900 ° C. for 1 minute in a vacuum atmosphere, and then quenched in ice water. When measured at room temperature by the four probe method, the specific resistance was 2.40 μΩ · cm.
［実施例２］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、２４．１質量％のＡｇと１９．０質量％のＣｕと５６．９質量％のＮｉからなるＡｇ−Ｃｕ−Ｎｉ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例１と同様の分散型組織を有し、実施例１と同様の方法により測定した比抵抗は１１．５μΩ・ｃｍであった。
[Example 2]
As an Ag-Cu-X-based alloy, it is composed of 24.1% by mass of Ag, 19.0% by mass of Cu and 56.9% by mass of Ni having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Ni alloy was used. The obtained alloy powder had the same dispersive structure as in Example 1, and the specific resistance measured by the same method as in Example 1 was 11.5 μΩ · cm.
［実施例３］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、１６．６質量％のＡｇと２４．５質量％のＣｕと５８．９質量％のＮｉからなるＡｇ−Ｃｕ−Ｎｉ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例１と同様の分散型組織を有し、実施例１と同様の方法により測定した比抵抗は１２．３μΩ・ｃｍであった。
[Example 3]
As an Ag-Cu-X-based alloy, it is composed of 16.6% by mass of Ag, 24.5% by mass of Cu and 58.9% by mass of Ni having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Ni alloy was used. The obtained alloy powder had the same dispersive structure as in Example 1, and the specific resistance measured by the same method as in Example 1 was 12.3 μΩ · cm.
［実施例４］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、３７．４質量％のＡｇと２２．０質量％のＣｕと４０．６質量％のＮｉからなるＡｇ−Ｃｕ−Ｎｉ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。
[Example 4]
As an Ag-Cu-X base alloy, it is composed of 37.4% by mass of Ag, 22.0% by mass of Cu and 40.6% by mass of Ni having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Ni alloy was used.
得られた合金粉末の粒子断面組織を図２の金属顕微鏡写真に示す。図２に示すように、合金粉末の組織は、コア部（中心部）がＣｕ−Ｎｉリッチ相によって形成され、コア部を取り囲む外周部がＡｇリッチ相によって形成されて、二相に明確に分離された組織（卵型分離組織）と、実施例１と同様の分散型組織であることがわかった。なお、卵型分離組織と分散型組織の割合は９０％：１０％であった。また、実施例１と同様の方法により測定した比抵抗は５．２８μΩ・ｃｍであった。 The metal cross-sectional structure of the obtained alloy powder is shown in the metal micrograph of FIG. As shown in FIG. 2, the structure of the alloy powder is clearly separated into two phases in which the core portion (center portion) is formed by the Cu—Ni rich phase and the outer peripheral portion surrounding the core portion is formed by the Ag rich phase. It was found that the obtained tissue (egg-shaped separated tissue) and the same dispersed type tissue as in Example 1 were obtained. The ratio between the egg-shaped separated tissue and the dispersed tissue was 90%: 10%. The specific resistance measured by the same method as in Example 1 was 5.28 μΩ · cm.
［実施例５］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、５９．１質量％のＡｇと１９．４質量％のＣｕと２１．５質量％のＮｉからなるＡｇ−Ｃｕ−Ｎｉ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例４と同様の卵型分離組織と実施例１と同様の分散型組織（卵型分離組織と分散型組織の割合は５０％：５０％）を有し、実施例１と同様の方法により測定した比抵抗は４．２７μΩ・ｃｍであった。
[Example 5]
As an Ag-Cu-X-based alloy, it is composed of 59.1% by mass of Ag, 19.4% by mass of Cu and 21.5% by mass of Ni having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Ni alloy was used. The obtained alloy powder had an egg-shaped separated structure similar to that in Example 4 and a dispersed structure similar to that in Example 1 (the ratio between the egg-shaped separated structure and the dispersed structure was 50%: 50%). The specific resistance measured by the same method as in Example 1 was 4.27 μΩ · cm.
［比較例１］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域外の組成を有する、１６．３質量％のＡｇと４８．１質量％のＣｕと３５．６質量％のＮｉからなるＡｇ−Ｃｕ−Ｎｉ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。
[Comparative Example 1]
As an Ag-Cu-X-based alloy, it is composed of 16.3% by mass of Ag, 48.1% by mass of Cu, and 35.6% by mass of Ni having a composition outside the two-phase region of the liquid phase in the ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Ni alloy was used.
得られた合金粉末の粒子断面組織を図３の金属顕微鏡写真に示す。図３に示すように、合金粉末の組織は、Ｃｕ−Ｎｉ初晶とＡｇ相とＣｕ−Ｎｉ相が層状に折り重なるように形成される凝固組織になることがわかった。また、実施例１と同様の方法により測定した比抵抗は２２．３μΩ・ｃｍであった。 The metal cross-sectional structure of the obtained alloy powder is shown in the metal micrograph of FIG. As shown in FIG. 3, it was found that the structure of the alloy powder was a solidified structure formed so that the Cu—Ni primary crystal, the Ag phase, and the Cu—Ni phase were folded in layers. The specific resistance measured by the same method as in Example 1 was 22.3 μΩ · cm.
なお、このような凝固組織の合金粉末の表面には、Ｃｕ−Ｎｉ相またはＡｇ相が形成され、このような合金粉末を導電性ペースト用の導電性粉末として使用すると、Ａｇのコネクト部が制限されて、良好な特性を得ることができない。また、この合金粉末の表面も凝固組織であり、酸化し易い。一方、実施例１〜５のように、三元系において液相の二相領域内の組成の合金粉末では、表面がＡｇリッチ相になり、圧紛成型し易い。 A Cu-Ni phase or an Ag phase is formed on the surface of the alloy powder having such a solidified structure. When such an alloy powder is used as a conductive powder for a conductive paste, the Ag connecting portion is limited. Therefore, good characteristics cannot be obtained. Further, the surface of the alloy powder is also a solidified structure and is easily oxidized. On the other hand, as in Examples 1 to 5, the alloy powder having a composition in the two-phase region of the liquid phase in the ternary system has an Ag rich phase on the surface and is easy to be compacted.
［比較例２］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域外の組成を有する、４２．６質量％のＡｇと４１．９質量％のＣｕと１５．５質量％のＮｉからなるＡｇ−Ｃｕ−Ｎｉ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、比較例１と同様の凝固組織を有し、実施例１と同様の方法により測定した比抵抗は５．５６μΩ・ｃｍであった。
[Comparative Example 2]
As an Ag-Cu-X base alloy, it is composed of 42.6% by mass of Ag, 41.9% by mass of Cu and 15.5% by mass of Ni having a composition outside the two-phase region of the liquid phase in the ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Ni alloy was used. The obtained alloy powder had the same solidified structure as in Comparative Example 1, and the specific resistance measured by the same method as in Example 1 was 5.56 μΩ · cm.
［比較例３］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域外の組成を有する、１６．０質量％のＡｇと７０．９質量％のＣｕと１３．１質量％のＮｉからなるＡｇ−Ｃｕ−Ｎｉ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、比較例１と同様の凝固組織を有し、実施例１と同様の方法により測定した比抵抗は１１．１μΩ・ｃｍであった。
[Comparative Example 3]
As an Ag-Cu-X base alloy, it is composed of 16.0% by mass of Ag, 70.9% by mass of Cu and 13.1% by mass of Ni having a composition outside the two-phase region of the liquid phase in the ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Ni alloy was used. The obtained alloy powder had the same solidified structure as in Comparative Example 1, and the specific resistance measured by the same method as in Example 1 was 11.1 μΩ · cm.
これらの実施例１〜５および比較例１〜３の合金の組成および分析結果を表１に示す。 Table 1 shows the compositions and analysis results of the alloys of Examples 1 to 5 and Comparative Examples 1 to 3.
［実施例６］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、２０．１質量％のＡｇと２５．５質量％のＣｕと５４．４質量％のＣｏからなるＡｇ−Ｃｕ−Ｃｏ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例４と同様の卵型分離組織を有し、実施例１と同様の方法により測定した比抵抗は５．８０μΩ・ｃｍであった。
[Example 6]
As an Ag-Cu-X-based alloy, it is composed of 20.1% by mass of Ag, 25.5% by mass of Cu and 54.4% by mass of Co having a composition in a two-phase region of a liquid phase in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Co alloy was used. The obtained alloy powder had the same egg-shaped separated structure as in Example 4, and the specific resistance measured by the same method as in Example 1 was 5.80 μΩ · cm.
［実施例７］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、３７．３質量％のＡｇと２２．０質量％のＣｕと４０．７質量％のＣｏからなるＡｇ−Ｃｕ−Ｃｏ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例４と同様の卵型分離組織と実施例１と同様の分散型組織（卵型分離組織と分散型組織の割合は９０％：１０％）を有し、実施例１と同様の方法により測定した比抵抗は５．２８μΩ・ｃｍであった。
[Example 7]
As an Ag-Cu-X-based alloy, it is composed of 37.3 mass% Ag, 22.0 mass% Cu, and 40.7 mass% Co having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Co alloy was used. The obtained alloy powder had an egg-shaped separated structure similar to that in Example 4 and a dispersed structure similar to that in Example 1 (the ratio between the egg-shaped separated structure and the dispersed structure was 90%: 10%). The specific resistance measured by the same method as in Example 1 was 5.28 μΩ · cm.
［実施例８］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、５９．２質量％のＡｇと１９．３質量％のＣｕと２１．５質量％のＣｏからなるＡｇ−Ｃｕ−Ｃｏ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例４と同様の卵型分離組織と実施例１と同様の分散型組織（卵型分離組織と分散型組織の割合は４０％：６０％）を有し、実施例１と同様の方法により測定した比抵抗は３．３３μΩ・ｃｍであった。
[Example 8]
As an Ag-Cu-X-based alloy, it is composed of 59.2% by mass of Ag, 19.3% by mass of Cu and 21.5% by mass of Co having a composition in the two-phase region of the liquid phase in the ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Co alloy was used. The obtained alloy powder had an egg-shaped separated structure similar to that in Example 4 and a dispersed structure similar to that in Example 1 (the ratio between the egg-shaped separated structure and the dispersed structure was 40%: 60%). The specific resistance measured by the same method as in Example 1 was 3.33 μΩ · cm.
［実施例９］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、７６．３質量％のＡｇと１７．３質量％のＣｕと６．４質量％のＣｏからなるＡｇ−Ｃｕ−Ｃｏ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例１と同様の分散型組織（を有し、実施例１と同様の方法により測定した比抵抗は２．６６μΩ・ｃｍであった。
[Example 9]
As an Ag-Cu-X-based alloy, it is composed of 76.3% by mass of Ag, 17.3% by mass of Cu and 6.4% by mass of Co having a composition in a two-phase region of a liquid phase in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Co alloy was used. The obtained alloy powder had the same dispersion type structure as in Example 1 and the specific resistance measured by the same method as in Example 1 was 2.66 μΩ · cm.
［実施例１０］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、７６．６質量％のＡｇと１７．３質量％のＣｕと６．１質量％のＦｅからなるＡｇ−Ｃｕ−Ｆｅ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例１と同様の分散型組織を有し、実施例１と同様の方法により測定した比抵抗は３．０８Ω・ｃｍであった。
[Example 10]
As an Ag-Cu-X-based alloy, it is composed of 76.6% by mass of Ag, 17.3% by mass of Cu and 6.1% by mass of Fe having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Fe alloy was used. The obtained alloy powder had the same dispersed structure as in Example 1, and the specific resistance measured by the same method as in Example 1 was 3.08 Ω · cm.
［実施例１１］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、２０．１質量％のＡｇと２７．４質量％のＣｕと５２．５質量％のＦｅからなるＡｇ−Ｃｕ−Ｆｅ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例４と同様の卵型分離組織と実施例１と同様の分散型組織（卵型分離組織と分散型組織の割合は４０％：６０％）を有し、実施例１と同様の方法により測定した比抵抗は１１．０μΩ・ｃｍであった。
[Example 11]
As an Ag-Cu-X base alloy, it is composed of 20.1% by mass of Ag, 27.4% by mass of Cu and 52.5% by mass of Fe having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Fe alloy was used. The obtained alloy powder had an egg-shaped separated structure similar to that in Example 4 and a dispersed structure similar to that in Example 1 (the ratio between the egg-shaped separated structure and the dispersed structure was 40%: 60%). The specific resistance measured by the same method as in Example 1 was 11.0 μΩ · cm.
［実施例１２］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、５９．８質量％のＡｇと１９．６質量％のＣｕと２０．６質量％のＦｅからなるＡｇ−Ｃｕ−Ｆｅ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例４と同様の卵型分離組織と実施例１と同様の分散型組織（卵型分離組織と分散型組織の割合は５０％：５０％）を有し、実施例１と同様の方法により測定した比抵抗は３．９７μΩ・ｃｍであった。
[Example 12]
As an Ag-Cu-X-based alloy, it is composed of 59.8% by mass of Ag, 19.6% by mass of Cu and 20.6% by mass of Fe having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Fe alloy was used. The obtained alloy powder had an egg-shaped separated structure similar to that in Example 4 and a dispersed structure similar to that in Example 1 (the ratio between the egg-shaped separated structure and the dispersed structure was 50%: 50%). The specific resistance measured by the same method as in Example 1 was 3.97 μΩ · cm.
［実施例１３］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、４８．９質量％のＡｇと３２．９質量％のＣｕと１８．２質量％のＦｅからなるＡｇ−Ｃｕ−Ｆｅ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例４と同様の卵型分離組織と実施例１と同様の分散型組織（卵型分離組織と分散型組織の割合は５０％：５０％）を有し、実施例１と同様の方法により測定した比抵抗は２．４５μΩ・ｃｍであった。
[Example 13]
As an Ag-Cu-X-based alloy, it is composed of 48.9% by mass of Ag, 32.9% by mass of Cu and 18.2% by mass of Fe having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Fe alloy was used. The obtained alloy powder had an egg-shaped separated structure similar to that in Example 4 and a dispersed structure similar to that in Example 1 (the ratio between the egg-shaped separated structure and the dispersed structure was 50%: 50%). The specific resistance measured by the same method as in Example 1 was 2.45 μΩ · cm.
［実施例１４］
Ａｇ−Ｃｕ−Ｘ基合金として、三元系において液相の二相領域内の組成を有する、３８．１質量％のＡｇと２２．４質量％のＣｕと３９．５質量％のＦｅからなるＡｇ−Ｃｕ−Ｆｅ合金を使用した以外は、実施例１と同様の方法によって、平均粒径１５０μｍ以下の合金粉末を得た。得られた合金粉末は、実施例４と同様の卵型分離組織を有し、実施例１と同様の方法により測定した比抵抗は３．４７μΩ・ｃｍであった。
[Example 14]
As an Ag-Cu-X-based alloy, it is composed of 38.1% by mass of Ag, 22.4% by mass of Cu and 39.5% by mass of Fe having a composition in a liquid phase two-phase region in a ternary system. An alloy powder having an average particle size of 150 μm or less was obtained in the same manner as in Example 1 except that an Ag—Cu—Fe alloy was used. The obtained alloy powder had the same egg-shaped separated structure as in Example 4, and the specific resistance measured by the same method as in Example 1 was 3.47 μΩ · cm.
これらの実施例６〜１４の合金の組成および分析結果を表２に示す。
Claims (8)
The Ag-Cu-X alloy powder is more than 20.0% by mass and 96.8% by mass or less of Ag, 0.1 to 40.0% by mass of Cu, and 1.1 to 96.2% by mass. The conductive composite powder according to claim 5, which is an Ag—Cu—Co alloy composed of Co.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102873324A (en) * | 2012-10-17 | 2013-01-16 | 厦门大学 | Covering-type copper-nickel-silver composite powder and preparation method thereof |
| CN105598467A (en) * | 2016-01-20 | 2016-05-25 | 哈尔滨工业大学深圳研究生院 | High-temperature-resistant silver-coated and nickel-coated copper conductive powder of core-shell structure and preparation method thereof |
| WO2020105688A1 (en) * | 2018-11-22 | 2020-05-28 | 株式会社カネカ | Multicomponent metal compound |
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| JPH03245404A (en) * | 1990-02-23 | 1991-11-01 | Asahi Chem Ind Co Ltd | Silver alloy conductive paste and conductor using same paste |
| JPH1192805A (en) * | 1997-09-17 | 1999-04-06 | Sumitomo Metal Mining Co Ltd | Copper alloy powder and its production |
| JP2003197032A (en) * | 2001-12-25 | 2003-07-11 | Teikoku Tsushin Kogyo Co Ltd | Conductive paste |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03245404A (en) * | 1990-02-23 | 1991-11-01 | Asahi Chem Ind Co Ltd | Silver alloy conductive paste and conductor using same paste |
| JPH1192805A (en) * | 1997-09-17 | 1999-04-06 | Sumitomo Metal Mining Co Ltd | Copper alloy powder and its production |
| JP2003197032A (en) * | 2001-12-25 | 2003-07-11 | Teikoku Tsushin Kogyo Co Ltd | Conductive paste |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102873324A (en) * | 2012-10-17 | 2013-01-16 | 厦门大学 | Covering-type copper-nickel-silver composite powder and preparation method thereof |
| CN105598467A (en) * | 2016-01-20 | 2016-05-25 | 哈尔滨工业大学深圳研究生院 | High-temperature-resistant silver-coated and nickel-coated copper conductive powder of core-shell structure and preparation method thereof |
| WO2020105688A1 (en) * | 2018-11-22 | 2020-05-28 | 株式会社カネカ | Multicomponent metal compound |
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