JP5247293B2 - Brazing and joining structure of steel and aluminum material and brazing method - Google Patents
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- 239000000463 material Substances 0.000 title claims description 146
- 238000005219 brazing Methods 0.000 title claims description 96
- 229910000831 Steel Inorganic materials 0.000 title claims description 84
- 239000010959 steel Substances 0.000 title claims description 84
- 229910052782 aluminium Inorganic materials 0.000 title claims description 48
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims description 46
- 238000000034 method Methods 0.000 title claims description 28
- 229910045601 alloy Inorganic materials 0.000 claims description 67
- 239000000956 alloy Substances 0.000 claims description 67
- 229910018191 Al—Fe—Si Inorganic materials 0.000 claims description 48
- 239000000758 substrate Substances 0.000 claims description 25
- 229910001220 stainless steel Inorganic materials 0.000 claims description 23
- 239000010935 stainless steel Substances 0.000 claims description 20
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 19
- 239000004065 semiconductor Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 229910017758 Cu-Si Inorganic materials 0.000 claims description 9
- 229910017931 Cu—Si Inorganic materials 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 7
- 229910017767 Cu—Al Inorganic materials 0.000 claims description 5
- 239000000945 filler Substances 0.000 claims description 4
- 239000011159 matrix material Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
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- 239000011247 coating layer Substances 0.000 claims 1
- 239000012071 phase Substances 0.000 description 67
- 238000007747 plating Methods 0.000 description 27
- 239000010949 copper Substances 0.000 description 15
- 229910052710 silicon Inorganic materials 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000004020 conductor Substances 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000002436 steel type Substances 0.000 description 7
- 238000005336 cracking Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
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- 229910052761 rare earth metal Inorganic materials 0.000 description 4
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- 229910018125 Al-Si Inorganic materials 0.000 description 3
- 229910018520 Al—Si Inorganic materials 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
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- 229910018084 Al-Fe Inorganic materials 0.000 description 2
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- 229910017082 Fe-Si Inorganic materials 0.000 description 2
- 229910017133 Fe—Si Inorganic materials 0.000 description 2
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 2
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- 229910052804 chromium Inorganic materials 0.000 description 2
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- 230000000644 propagated effect Effects 0.000 description 2
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- 229910052727 yttrium Inorganic materials 0.000 description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
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Description
本発明は、鋼材とアルミニウム材料とをろう付けすることによって得られるろう付け接合構造、およびそのろう付け方法に関する。 The present invention relates to a brazed joint structure obtained by brazing a steel material and an aluminum material, and a brazing method thereof.
鋼材とアルミニウム材料を接合する方法としては、ボルト/ナットやかしめなどにより機械的に締結する方法、接着剤による方法、ろう付けによる方法がある。このうち、ろう付けによる接合方法は、例えば自動車のラジエーター部材など、鋼材とアルミニウム材料との間の熱伝導を重視する用途において特に有効である。鋼材とアルミニウム材料のろう付けは、従来、主としてAl−Si系合金のろう材(例えばAl:88原子%、Si:12原子%)を用いて行われている。 As a method of joining a steel material and an aluminum material, there are a method of mechanically fastening with a bolt / nut or caulking, a method using an adhesive, and a method using brazing. Among these, the joining method by brazing is particularly effective in applications that place importance on heat conduction between a steel material and an aluminum material, such as a radiator member of an automobile. Conventionally, brazing of a steel material and an aluminum material is performed mainly using a brazing material of an Al—Si alloy (for example, Al: 88 atomic%, Si: 12 atomic%).
しかし、従来のろう付けでは、鋼材と、ろう材の溶融凝固層との界面に脆いAl−Fe系合金層(反応層)が成長しやすく、必ずしも十分な接合強度が得られないという問題があった。特許文献1には、より融点の低いAl−Si−高Zn系のろう材を用いてろう付け温度を低くすることにより、脆い反応層の成長を抑制する手法が記載されている。 However, the conventional brazing has a problem that a brittle Al—Fe alloy layer (reaction layer) is likely to grow at the interface between the steel material and the molten and solidified layer of the brazing material, and sufficient bonding strength cannot always be obtained. It was. Patent Document 1 describes a technique of suppressing the growth of a fragile reaction layer by lowering the brazing temperature using an Al—Si—high Zn brazing material having a lower melting point.
一方、一般的な鋼材はアルミニウム材料に比べ耐食性に劣ることなどから、鋼材としてAlめっき鋼板を使用し、これをアルミニウム材料とろう付けする手法が試みられてきた。特許文献2には、溶融Alめっき鋼板とアルミニウム合金とをろう付けする際に、Alめっき鋼板の原板としてNを添加した鋼を使用することが開示されている。鋼中のNは鋼素地とAlめっき層との間にN濃化層を形成し、これがバリアーとなって、ろう付け時に鋼中のFeがろう材側に拡散するのを阻害し、その結果、脆いAl−Fe系合金層(反応層)の成長が抑制される。 On the other hand, since general steel materials are inferior in corrosion resistance as compared with aluminum materials, Al-plated steel plates are used as steel materials, and a method of brazing them with aluminum materials has been attempted. Patent Document 2 discloses that, when brazing a hot-dip Al-plated steel plate and an aluminum alloy, steel added with N is used as an original plate of the Al-plated steel plate. N in steel forms an N-enriched layer between the steel substrate and the Al plating layer, which acts as a barrier and inhibits diffusion of Fe in the steel to the brazing material side during brazing, and as a result Growth of a brittle Al—Fe alloy layer (reaction layer) is suppressed.
鋼材とアルミニウム材料のろう付け接合は、アルミニウム材料の高い熱伝導性を利用して鋼材側を冷却する目的で利用されることが多い。アルミニウム材料は鋼材に比べ熱膨張率が大きいことから、両者間のろう付け接合部には、部材として使用されるときの昇温・降温によって、熱膨張率の差に起因した応力が付与される。鋼材とアルミニウム材料のろう付け接合部には前述のように脆い合金層が形成され、ろう付け接合界面での耐久性が問題となることがある。このような合金層の問題は特許文献1、2の技術によりある程度改善することができる。 Brazing joining of a steel material and an aluminum material is often used for the purpose of cooling the steel material side by utilizing the high thermal conductivity of the aluminum material. Since aluminum material has a higher coefficient of thermal expansion than steel, stress due to the difference in coefficient of thermal expansion is applied to the brazed joint between the two due to temperature rise and fall when used as a member. . As described above, a brittle alloy layer is formed at a brazed joint between a steel material and an aluminum material, and durability at the brazed joint interface may be a problem. The problem of such an alloy layer can be improved to some extent by the techniques of Patent Documents 1 and 2.
しかしながら、用途によっては耐食性の観点から鋼材としてステンレス鋼を使用することが想定される。ステンレス鋼の場合は特にろう付け温度が約580℃を超えると脆いAl−Fe−Si系合金層が発達しやすい。このため例えば、従来一般的なAl−Si系のろう材を用いて、従来と同様に高温でのろう付けを行った場合、脆いAl−Fe−Si系合金層の厚さが増大し、高い接合強度を安定して得ることが難しい。 However, depending on the application, it is assumed that stainless steel is used as a steel material from the viewpoint of corrosion resistance. In the case of stainless steel, particularly when the brazing temperature exceeds about 580 ° C., a brittle Al—Fe—Si based alloy layer tends to develop. For this reason, for example, when brazing at a high temperature as in the prior art using a conventional Al-Si brazing material, the thickness of the brittle Al-Fe-Si alloy layer increases and is high. It is difficult to obtain a stable joint strength.
また、ステンレス鋼の場合には特許文献1に開示されるような低融点のろう材を用いて、低温でのろう付けを試みても、接合自体が不可能であるという問題がある。これは、ステンレス鋼に特有の不動態皮膜が何らかの影響を及ぼしているものと考えられる。さらに、特許文献2に示されるようなN添加の手法はステンレス鋼に対して有効でないことがわかった。すなわち、N含有量の高いステンレス鋼にAlめっきを施す手法を採用しても、脆い合金層の成長を抑制することは困難である。これは、ステンレス鋼にはNとの親和力の大きいCrが多量に含有されているので、溶融Alめっき層の下にバリアーとなるN濃化層を形成することが困難となるからではないかと推察される。
したがって、鋼材としてステンレス鋼を使用した場合でも、鋼材とアルミニウム材料の間のろう付け接合界面における耐久性を十分に確保できるろう付け技術の確立が強く求められている。
Further, in the case of stainless steel, there is a problem that even if brazing at a low temperature is attempted using a low melting point brazing material as disclosed in Patent Document 1, joining itself is impossible. This is considered that the passive film peculiar to stainless steel has some influence. Furthermore, it was found that the N-added technique as shown in Patent Document 2 is not effective for stainless steel. That is, even if a technique of applying Al plating to stainless steel having a high N content is employed, it is difficult to suppress the growth of a brittle alloy layer. This is probably because stainless steel contains a large amount of Cr having a high affinity with N, so that it is difficult to form an N-enriched layer serving as a barrier under the molten Al plating layer. Is done.
Therefore, even when stainless steel is used as the steel material, establishment of a brazing technique that can sufficiently ensure the durability at the brazed joint interface between the steel material and the aluminum material is strongly demanded.
一方、最近ではパワーモジュールなどの半導体基板の放熱板として、安価かつ薄肉の鋼板素材を適用しようという試みがなされている。
図1に一般的なパワーモジュールの構成例を模式的に示す。半導体素子1を搭載する半導体基板2は、アルミナや窒化アルミニウム等のセラミックスからなる絶縁基板4の表面に銅またはアルミニウムの導体層3が接合されており、その上に半導体素子1が取り付けられる。絶縁基板4の裏面(半導体素子1と反対側の面)には熱伝導性の良好な銅またはアルミニウムからなる裏面導体層5が接合されている。半導体基板2の裏面導体層5は、ろう付けにより放熱板6と接合される。放熱板6は例えばヒートシンク7に取り付けられる。
On the other hand, recently, an attempt has been made to apply an inexpensive and thin steel plate material as a heat sink for a semiconductor substrate such as a power module.
FIG. 1 schematically shows a configuration example of a general power module. A semiconductor substrate 2 on which a semiconductor element 1 is mounted has a copper or aluminum conductor layer 3 bonded to the surface of an insulating substrate 4 made of ceramics such as alumina or aluminum nitride, and the semiconductor element 1 is mounted thereon. A back conductor layer 5 made of copper or aluminum having good thermal conductivity is bonded to the back surface of the insulating substrate 4 (the surface opposite to the semiconductor element 1). The back conductor layer 5 of the semiconductor substrate 2 is joined to the heat sink 6 by brazing. The heat sink 6 is attached to the heat sink 7, for example.
絶縁基板4のセラミックスは放熱板6の金属材料に比べ熱膨張率が小さいため、絶縁基板4に拘束されている裏面導体層5の見かけの熱膨張率は放熱板6よりも小さい状態となっている。したがって、電子部品として使用されるときの繰り返しの昇温・降温によって接合界面10には双方の熱膨張率の差に起因した応力が繰り返し付与され、接合界面10での耐久性が問題となることがある。接合界面10に生じるこのような応力を緩和するためには、放熱板6をできるだけ熱膨張率の小さい金属材料で構成することが有利となる。このため、例えば熱膨張率が小さく熱伝導性も比較的良好なCu−Mo合金板を2枚の銅板の間に挟んだ構造の放熱板材料が採用されることもある。しかし、この種の放熱板材料は非常に高価であるという欠点がある。 Since the ceramic of the insulating substrate 4 has a smaller coefficient of thermal expansion than the metal material of the heat sink 6, the apparent thermal expansion coefficient of the back conductor layer 5 constrained by the insulating substrate 4 is smaller than that of the heat sink 6. Yes. Therefore, the stress at the joint interface 10 is repeatedly applied to the joint interface 10 due to repeated temperature rise and fall when used as an electronic component, and durability at the joint interface 10 becomes a problem. There is. In order to relieve such stress generated at the joint interface 10, it is advantageous to configure the heat sink 6 with a metal material having a thermal expansion coefficient as small as possible. For this reason, for example, a heat sink material having a structure in which a Cu—Mo alloy plate having a small thermal expansion coefficient and relatively good thermal conductivity is sandwiched between two copper plates may be employed. However, this type of heat sink material has the disadvantage of being very expensive.
安価で、かつ熱膨張率の小さい金属材料として、マトリクスがフェライト相である鋼材を挙げることができる。鋼材は銅やアルミニウムと比べ熱伝導性には劣るが、発明者らの検討によれば板厚を薄くすることで放熱板に要求される熱伝導特性を満たすことが可能であると考えられる。しかしながら、例えば裏面導体層5がアルミニウム材料である場合、放熱板6に鋼材を用いると、接合界面10に生じる脆い合金層によって接合界面10での耐久性が不十分となることが懸念される。放熱板用途に鋼材を適用する場合、耐食性の良好なステンレス鋼を採用することが想定される。ステンレス鋼を用いるとアルミニウム材料とのろう付け接合界面における耐久性を改善することが一層難しくなることは前述の通りである。 As an inexpensive metal material having a low coefficient of thermal expansion, a steel material whose matrix is a ferrite phase can be given. Steel materials are inferior in thermal conductivity compared to copper and aluminum, but according to the study by the inventors, it is considered that thermal conductivity characteristics required for a heat sink can be satisfied by reducing the plate thickness. However, for example, when the back conductor layer 5 is made of an aluminum material, there is a concern that if a steel material is used for the heat radiating plate 6, durability at the joint interface 10 becomes insufficient due to a brittle alloy layer generated at the joint interface 10. When applying a steel material to a heat sink application, it is assumed that stainless steel having good corrosion resistance is adopted. As described above, it is more difficult to improve the durability at the brazed joint interface with the aluminum material when stainless steel is used.
本発明はこのような現状に鑑み、鋼材とアルミニウム材料とのろう付けにおいて、たとえ鋼材がステンレス鋼であっても、昇温・降温を繰り返した場合の接合界面での耐久性を安定して顕著に向上させることができる手法を提供しようというものである。 In view of such a current situation, the present invention provides a stable and durable durability at the joint interface when the temperature rise and fall are repeated even when the steel material is stainless steel in the brazing of the steel material and the aluminum material. This is to provide a technique that can be improved.
上記目的は、Alめっき鋼材とアルミニウム材料を、Mg含有量が0.3〜4質量%であり融点が550℃未満であるAl−Cu−Si系合金組成のろう材を用いてろう付けした接合構造であって、鋼材側から順に、鋼素地、Al−Fe−Si系合金層、Al素地により構成され、前記Al素地中にはCu−Al合金の晶出相またはそれに由来するCu濃化相、Si濃化相、およびMg濃化相が存在し、前記Al−Fe−Si系合金層は下記(1)および(2)の条件を満たすものである鋼材とアルミニウム材料のろう付け接合構造によって達成される。
(1)Al−Fe−Si系合金層の平均厚さが15μm以下であること
(2)Al−Fe−Si系合金層は、Cu濃度が異なる2種類のAl−Fe−Si系合金の相が混在した構成を有するものであること
The purpose is to join Al-plated steel material and aluminum material by brazing using a brazing material having an Al-Cu-Si alloy composition with an Mg content of 0.3 to 4% by mass and a melting point of less than 550 ° C. a structure, in order from the steel material side, the steel basis material, Al-Fe-Si alloy layer, the more configured Al-containing fabric, Cu concentrated from crystallized Desho or that of Cu-Al alloy in the Al matrix reduction phase, Si concentrated phase, and there is Mg concentrated phase, brazing conditions are met der Ru steel and aluminum material of the Al-Fe-Si-based alloy layer (1) and (2) below Achieved by the joint structure.
(1) The average thickness of the Al—Fe—Si alloy layer is 15 μm or less. (2) The Al—Fe—Si alloy layer is a phase of two types of Al—Fe—Si alloys having different Cu concentrations. Have a mixed configuration
上記のろう付け接合構造は、例えば半導体基板と放熱板との接合に適用できる。すなわち本発明では、前記アルミニウム材料が半導体基板の素子搭載面と反対側の面を構成する部材であり、前記鋼材が半導体基板と接合される放熱板である前記のろう付け接合構造が提供される。 The brazed joint structure described above can be applied, for example, to joining a semiconductor substrate and a heat sink. That is, in the present invention, the brazing joint structure is provided in which the aluminum material is a member constituting the surface opposite to the element mounting surface of the semiconductor substrate, and the steel material is a heat radiating plate joined to the semiconductor substrate. .
このようなろう付け接合構造を構築するために手法として、本発明では、Si:5〜13質量%を含有する溶融Alめっき層を表面に有する鋼材と、アルミニウム材料を、それら双方の材料間にMgを0.3〜4質量%の範囲で含有する融点550℃未満のAl−Cu−Si系ろう材が介在する状態で、530℃以上かつろう材の融点以上、580℃以下の温度の炉中に装入してろう材を溶融させ、ろう付け接合部の鋼素地表面に成長するAl−Fe−Si系合金層の平均厚さが15μm以下となるように上記温度範囲における保持を終了し冷却過程に移行させる、鋼材とアルミニウム材料の真空ろう付け方法が提供される。ここでいう「真空ろう付け」は上記保持温度における雰囲気の圧力を1×10-2Pa以下として行うろう付けである。「Al−Fe−Si系合金層の平均厚さ」は、ろう付け熱処理終了後(上記保持温度から常温まで冷却された時点)におけるAl−Fe−Si系合金層の平均厚さ、すなわち、ろう付け後の材料で観察されるAl−Fe−Si系合金層の平均厚さである。 As a method for constructing such a brazed joint structure, in the present invention, a steel material having a molten Al plating layer containing Si: 5 to 13% by mass on the surface and an aluminum material are interposed between the two materials. A furnace having a temperature not lower than 530 ° C. and not lower than the melting point of the brazing material and not higher than 580 ° C. with an Al—Cu—Si brazing material containing Mg in the range of 0.3 to 4% by mass and having a melting point of less than 550 ° C. The brazing material was melted by inserting into the brazing material, and the holding in the above temperature range was terminated so that the average thickness of the Al—Fe—Si based alloy layer growing on the steel base surface of the brazed joint became 15 μm or less. A method of vacuum brazing of steel and aluminum material is provided that transitions to a cooling process . Referred to here "vacuum brazing" is brazed to perform the pressure of the atmosphere in the holding temperature of less 1 × 10 -2 Pa. “The average thickness of the Al—Fe—Si based alloy layer” is the average thickness of the Al—Fe—Si based alloy layer after the brazing heat treatment is completed (when the temperature is cooled from the holding temperature to room temperature), that is, the brazing It is the average thickness of the Al—Fe—Si based alloy layer observed in the material after being attached.
前記の鋼材としてはステンレス鋼を採用することができる。 Stainless steel can be adopted as the steel material.
本発明によれば、鋼材とアルミニウム材料のろう付けにおいて、その接合界面に両材料の熱膨張率の相違に起因した応力が繰り返し付与された場合でも高い耐久性を示す接合構造が安定して得られるようになった。鋼材としてはステンレス鋼を使用することもでき、また真空ろう付けにも対応可能である。したがって本発明は、鋼材とアルミニウム材料との間で熱伝達を行う各種部材に広く適用できるものである。 According to the present invention, in the brazing of a steel material and an aluminum material, even when stress due to the difference in thermal expansion coefficient between the two materials is repeatedly applied to the joint interface, a joint structure having high durability can be stably obtained. It came to be able to. As the steel material, stainless steel can be used, and vacuum brazing can be supported. Therefore, the present invention can be widely applied to various members that transfer heat between a steel material and an aluminum material.
〔鋼材〕
本発明では鋼材としては「Alめっき鋼材」を使用する。鋼材の表面にAlめっき層が存在することにより、ろう材との反応性が向上し、ろう付け温度の低減が可能となる。
Alめっき層は、Siを5〜13質量%含有するAl−Si合金浴に鋼材を浸漬することによって得られる溶融Alめっき層とすることが好ましい。
[Steel]
In the present invention, “Al plated steel” is used as the steel. The presence of the Al plating layer on the surface of the steel material improves the reactivity with the brazing material and makes it possible to reduce the brazing temperature.
The Al plating layer is preferably a molten Al plating layer obtained by immersing a steel material in an Al—Si alloy bath containing 5 to 13 mass% of Si.
図2に、溶融Alめっき鋼材のめっき層を含む断面のSEM写真を例示する。この例は母材として板厚0.8mmのSUH409を用いたものである。めっき浴組成はAl−9質量%Siであり、Siの残部はAlと不可避的不純物である。めっき層の鋼素地近傍には反応層が形成されている。この反応層はめっき浴のAlおよびSiと母材のFeが反応して形成されたものであり、母材がステンレス鋼の場合はこの反応層が成長しやすい傾向にある。ただし、めっき層の組成は浴組成とほぼ同じになることが確認されている。ろう付けを行うと、Alめっき層および反応層は溶融したろう材と反応し、鋼素地近傍には新たな反応層(後述のAl−Fe−Si系合金層)が形成されることになる。 In FIG. 2, the SEM photograph of the cross section containing the plating layer of hot-dip Al plating steel materials is illustrated. In this example, SUH409 having a thickness of 0.8 mm is used as a base material. The plating bath composition is Al-9 mass% Si, and the balance of Si is Al and inevitable impurities. A reaction layer is formed in the vicinity of the steel substrate of the plating layer. This reaction layer is formed by the reaction of Al and Si of the plating bath with Fe of the base material. When the base material is stainless steel, this reaction layer tends to grow easily. However, it has been confirmed that the composition of the plating layer is almost the same as the bath composition. When brazing is performed, the Al plating layer and the reaction layer react with the molten brazing material, and a new reaction layer (an Al—Fe—Si alloy layer described later) is formed in the vicinity of the steel base.
溶融Alめっき浴中にSiを含有させることにより融点が低下し、めっき浴温を下げることができる。また形成されるAlめっき層の融点も低下することから、ろう付け時にろう材との反応性も良好となる。このような効果を十分に得るためにはAlめっき層中のSi含有量を5〜13質量%とすることが好ましく、7〜11質量%の範囲に管理しても構わない。母材として「鋼板」を使用する場合、一般的な連続溶融めっきラインを用いて製造される溶融Alめっき鋼板が好適な対象となる。Alめっき付着量は鋼板片面あたり例えば15〜150g/m2とすれば良く、30〜100g/m2とすることがより好ましい。 By containing Si in the molten Al plating bath, the melting point is lowered, and the plating bath temperature can be lowered. In addition, since the melting point of the formed Al plating layer is also lowered, the reactivity with the brazing material is improved during brazing. In order to sufficiently obtain such an effect, the Si content in the Al plating layer is preferably 5 to 13% by mass, and may be managed in the range of 7 to 11% by mass. When using a “steel plate” as a base material, a hot-dip Al-plated steel plate manufactured using a general continuous hot-dip plating line is a suitable target. The Al plating adhesion amount may be, for example, 15 to 150 g / m 2 per one surface of the steel sheet, and more preferably 30 to 100 g / m 2 .
母材の鋼は、溶融Alめっきを施すことが可能な種々の鋼種を適用することができ、用途に応じて選択すればよい。耐食性が要求される用途に対してはステンレス鋼を採用することが望ましい。「ステンレス鋼」はJIS G0203:2000の番号4201に示されるようにCr含有量10.5質量%以上の鋼であるが、製造性やコストを考慮するとCr含有量は32質量%以下の範囲とすることが望ましい。フェライト系鋼種はオーステナイト系鋼種よりも熱膨張率が小さいことから、例えば半導体基板を接合する放熱板の用途ではフェライト系ステンレス鋼を適用することが望ましい。アルミニウム材料自体の熱膨張率にできるだけ近い鋼材を適用したい場合はオーステナイト系ステンレス鋼が有利となる。 As the base steel, various steel types that can be subjected to hot-dip Al plating can be applied, and may be selected according to the intended use. For applications where corrosion resistance is required, it is desirable to use stainless steel. “Stainless steel” is a steel having a Cr content of 10.5% by mass or more as shown in the number 4201 of JIS G0203: 2000, but considering the manufacturability and cost, the Cr content is in the range of 32% by mass or less. It is desirable to do. Since the ferritic steel type has a smaller coefficient of thermal expansion than the austenitic steel type, it is desirable to use ferritic stainless steel, for example, in the application of a heat sink for joining semiconductor substrates. When it is desired to apply a steel material that is as close as possible to the thermal expansion coefficient of the aluminum material itself, austenitic stainless steel is advantageous.
フェライト系ステンレス鋼の成分組成を例示すると、C:0.12%以下、Si:1%以下、Mn:1%以下、P:0.04%以下、S:0.03%以下、Cr:10.5〜32%とくに11〜20%であり、必要に応じてMo:3%以下、Cu:1%以下、Ti+Nb+Zrの合計:0.8%以下、Ni:0.6%以下、B:0.1%以下、V:1%以下、Ca:0.1%以下、Mg:0.1%以下、Y:0.1%以下、REM(希土類元素):0.1%以下の1種以上を含有し、残部Feおよび不可避的不純物からなる組成を挙げることができる。既存の規格鋼種としては、例えばJIS 4305:2005の表4や、JIS G4312−1991の表3に記載されるフェライト系鋼種を採用することができる。 Examples of the composition of ferritic stainless steel include C: 0.12% or less, Si: 1% or less, Mn: 1% or less, P: 0.04% or less, S: 0.03% or less, Cr: 10 0.5 to 32%, particularly 11 to 20%, and Mo: 3% or less, Cu: 1% or less, Ti + Nb + Zr total: 0.8% or less, Ni: 0.6% or less, B: 0 as necessary 1% or less, V: 1% or less, Ca: 0.1% or less, Mg: 0.1% or less, Y: 0.1% or less, REM (rare earth element): 0.1% or less And a composition comprising the balance Fe and inevitable impurities. As existing standard steel types, for example, ferritic steel types described in Table 4 of JIS 4305: 2005 and Table 3 of JIS G4312-1991 can be adopted.
オーステナイト系ステンレス鋼の成分組成を例示すると、質量%で、C:0.12%以下、Si:4%以下とくに1%以下、Mn:5%以下とくに2%以下、P:0.045%以下、S:0.03%以下、Ni:6〜28%とくに8〜14%、Cr:15〜32%とくに16〜26%、N:0.3%以下であり、必要に応じてMo:7%以下とくに3%以下、Cu:4%以下とくに2%以下、Ti+Nb+Zrの合計:0.8%以下、B:0.1%以下、V:1%以下、Ca:0.1%以下、Mg:0.1%以下、Y:0.1%以下、REM(希土類元素):0.1%以下の1種以上を含有し、残部Feおよび不可避的不純物からなる組成を挙げることができる。既存の規格鋼種としては、例えばJIS 4305:2005の表2や、JIS G4312−1991の表2に記載されるオーステナイト系鋼種を採用することができる。 The component composition of austenitic stainless steel is exemplified by mass%, C: 0.12% or less, Si: 4% or less, particularly 1% or less, Mn: 5% or less, particularly 2% or less, P: 0.045% or less. , S: 0.03% or less, Ni: 6-28%, especially 8-14%, Cr: 15-32%, especially 16-26%, N: 0.3% or less, and Mo: 7 if necessary % Or less, particularly 3% or less, Cu: 4% or less, particularly 2% or less, Ti + Nb + Zr: 0.8% or less, B: 0.1% or less, V: 1% or less, Ca: 0.1% or less, Mg A composition comprising one or more of: 0.1% or less, Y: 0.1% or less, REM (rare earth element): 0.1% or less, the balance being Fe and inevitable impurities can be given. As existing standard steel types, for example, austenitic steel types described in Table 2 of JIS 4305: 2005 and Table 2 of JIS G4312-1991 can be adopted.
〔アルミニウム材料〕
アルミニウム材料は、純Alや、マトリクスがAl相である種々のAl合金(Al含有量80質量%以上、好ましくは85質量%以上)が適用対象となる。既存の規格材料としては、JIS H4000に規定される種々のもの(1000系〜8000系)が採用できる。
[Aluminum material]
As the aluminum material, pure Al and various Al alloys whose matrix is an Al phase (Al content of 80 mass% or more, preferably 85 mass% or more) are applicable. As existing standard materials, various materials (1000 series to 8000 series) defined in JIS H4000 can be adopted.
〔ろう材〕
ろう材は、融点が550℃未満のものを使用する。540℃未満のものがより好ましい。アルミニウム合金用の従来一般的なろう材としてはAl−Si系のものが知られており、例えばSi:約12原子%を含む組成のものが主流である。しかし、Al−Si系は融点が570℃を超えて高く、Al−Fe−Si系合金層の厚さをできるだけ薄くすることが重要となる本発明では使用できない。
[Brazing material]
A brazing material having a melting point of less than 550 ° C. is used. The thing below 540 degreeC is more preferable. Conventionally known brazing materials for aluminum alloys are Al-Si based materials, for example, Si: a composition containing about 12 atomic% is the mainstream. However, the Al—Si system has a high melting point exceeding 570 ° C. and cannot be used in the present invention where it is important to make the thickness of the Al—Fe—Si alloy layer as thin as possible.
種々検討の結果、本発明ではCuを含有するAl−Cu−Si系合金で、融点が550℃未満となる組成のろう材を使用する。具体的にはAl−Cu−Si三元共晶点のAl−26.7質量%Cu−5.3質量%Si組成(共晶点温度;約524℃)またはこれに近い組成であって融点が550℃未満好ましくは540℃未満となる範囲の組成を採用する。ただし、フラックスを使用しない真空ろう付けに供する場合は、上記のAl−Cu−Si系合金にMgを4質量%以下の範囲で添加した組成のものを適用することが好ましい。被接合材であるAlめっき鋼材およびアルミニウム材料の表面は安定なAl酸化物に覆われている。ろう材中に配合されるMgはろう材が溶融したときにAl酸化物の還元剤として働き、フラックスを使用しなくてもAlめっき鋼材およびアルミニウム材料との反応性を確保することができる。このような作用を十分に引き出すためにはろう材中のMg含有量を0.3質量%以上とすることが望ましく、0.5質量%以上とすることがより好ましい。ただし、Mgをあまり多量に含有させる必要はなく、4質量%以下の範囲で調整すればよい。例えば2.5質量%以下の範囲に管理しても構わない。Mgを含有させることにより、ろう材の融点は若干変動することがあるが、Al、Cu、Siの配合比が前記の共晶組成またはそれに近い組成であれば融点が550℃未満好ましくは540℃未満となるMg含有Al−Cu−Si系ろう材を得ることが十分可能である。 As a result of various studies, in the present invention, an Al—Cu—Si based alloy containing Cu and a brazing material having a melting point of less than 550 ° C. is used. Specifically, Al-26.7 mass% Cu-5.3 mass% Si composition (eutectic point temperature; about 524 ° C.) of Al—Cu—Si ternary eutectic point or a composition close to this melting point Is employed in a range of less than 550 ° C., preferably less than 540 ° C. However, in the case of subjecting to vacuum brazing without using a flux, it is preferable to apply a composition in which Mg is added to the Al—Cu—Si based alloy in a range of 4 mass% or less. The surfaces of the Al-plated steel material and the aluminum material that are the materials to be joined are covered with stable Al oxide. Mg mixed in the brazing material acts as a reducing agent for the Al oxide when the brazing material is melted, and can ensure the reactivity with the Al-plated steel material and the aluminum material without using a flux. In order to sufficiently bring out such an action, the Mg content in the brazing material is desirably 0.3% by mass or more, and more preferably 0.5% by mass or more. However, it is not necessary to contain Mg in a large amount, and it may be adjusted within a range of 4% by mass or less. For example, you may manage in the range of 2.5 mass% or less. By containing Mg, the melting point of the brazing material may vary slightly, but if the blending ratio of Al, Cu, Si is the above eutectic composition or a composition close thereto, the melting point is less than 550 ° C., preferably 540 ° C. It is sufficiently possible to obtain an Mg-containing Al—Cu—Si brazing material that is less than the above.
〔ろう付け接合構造〕
Alめっき鋼材とアルミニウム材料を上記Al−Cu−Si系ろう材を用いてろう付け接合すると、ろう付け部の構造は、鋼材側から順に、「鋼素地」、「Al−Fe−Si系合金層」、「Al素地」となる。Al素地は、アルミニウム材料が元から存在していた領域と、鋼材のAlめっき層、ろう材およびアルミニウム材料が反応して形成された領域からなるが、それら双方の領域の境界は必ずしも明瞭ではない。本発明のろう付け接合構造においては多くの場合、Al−Fe−Si系合金層に近い部分には通常、Cu−Al合金の晶出相またはそれに由来するCu濃化相が残存している。また、Si濃化相やMg濃化相も存在する。本明細書では、このような「Al相ではなくAl−Fe−Si系合金の相でもない相」を「異相」と呼んでいる。ろう付け接合部において異相が存在する領域、すなわち、ろう付け時に溶融凝固した部分であることが明らかである領域についても、素地はAl相であり、このAl相はアルミニウム材料が元から存在していた部分のAl相と明瞭な境界を有しないことから、本明細書ではこれら異相が存在する領域も「Al素地」に含めている(後述図4〜図6のSEM像参照)。特に、ろう材の使用量が比較的少ない場合やろう付け時間が比較的長い場合には、凝固組織に由来する異相の大部分が拡散により消失しており、溶融凝固した部分を把握することが一層困難となる。なお、Al相に固溶されるろう材由来のCuの濃度は、Al−Fe−Si系合金層から遠ざかるにしたがって徐々に減少する傾向にある。
[Brazed joint structure]
When the Al-plated steel material and the aluminum material are brazed and joined using the Al-Cu-Si-based brazing material, the structure of the brazed portion is, in order from the steel material side, "steel base", "Al-Fe-Si-based alloy layer "," Al substrate ". The Al substrate consists of a region where the aluminum material originally existed and a region formed by the reaction of the Al plating layer of the steel material, the brazing material and the aluminum material, but the boundary between these two regions is not always clear. . In many cases, in the brazed joint structure of the present invention, a crystallized phase of a Cu-Al alloy or a Cu-concentrated phase derived from it usually remains in a portion close to the Al-Fe-Si-based alloy layer. In addition, there are Si concentrated phase and Mg concentrated phase. In the present specification, such a “phase that is not an Al phase and not an Al—Fe—Si alloy phase” is referred to as a “different phase”. Even in a region where a heterogeneous phase exists in the brazed joint, that is, a region that is clearly melted and solidified during brazing, the substrate is the Al phase, and the Al phase originally contains the aluminum material. In this specification, the region where these different phases exist is also included in the “Al substrate” (see SEM images in FIGS. 4 to 6 described later). In particular, when the amount of brazing material used is relatively small or when the brazing time is relatively long, most of the heterogeneous phase originating from the solidified structure has disappeared due to diffusion, and it is possible to grasp the melted and solidified part. It becomes even more difficult. Note that the concentration of Cu derived from the brazing filler metal dissolved in the Al phase tends to gradually decrease as the distance from the Al—Fe—Si alloy layer increases.
発明者らの検討によれば、上記のような「鋼素地」、「Al−Fe−Si系合金層」、「Al素地」により構成される鋼材とアルミニウム材料のろう付け接合部において、Al−Fe−Si系合金層は他の部分と比較して脆く、ろう付け接合部での破断はAl−Fe−Si系合金層の内部に生じるクラックによって引き起こされることがわかった。発明者らはさらに詳細な検討の結果、このAl−Fe−Si系合金層の平均厚さを15μm以下とすることによって昇温・降温を繰り返したときのろう付け接合部における耐久性が顕著に改善されることを見出した。Al−Fe−Si系合金層の平均厚さを10μm以下とすることがより効果的である。 According to the study by the inventors, in the brazed joint between the steel material and the aluminum material constituted by the “steel base”, “Al—Fe—Si alloy layer”, and “Al base” as described above, Al— It has been found that the Fe—Si based alloy layer is brittle compared to other portions, and the breakage at the brazed joint is caused by a crack generated in the Al—Fe—Si based alloy layer. As a result of further detailed study, the inventors have made the average thickness of the Al—Fe—Si alloy layer 15 μm or less, and the durability at the brazed joint when the temperature rise / fall is repeated is remarkable. I found it to be improved. It is more effective to set the average thickness of the Al—Fe—Si based alloy layer to 10 μm or less.
図3に、本発明のろう付け接合構造における断面のSEM写真を例示する。これは後述実施例における試験No.6の例である。鋼素地表面に(A)と表示したA相と(B)と表示したB相(Aよりも黒っぽく見える相)が混在する層が形成されている。分析の結果、A相、B相ともAl−Fe−Si系合金層であるが、A相中にはB相中よりもCuが多く存在する。また、鋼材がステンレス鋼である場合には、A相中にはB相中よりもCrが多く存在する。これらの相の近傍には白っぽく見える相が観察されるが、これはCu−Al合金の晶出相またはそれに由来するCu濃化相である。Al−Fe−Si系合金層の平均厚さは、図3のような断面の組織観察を行い、鋼素地表面に沿う方向(図3の写真では横方向)の一定距離Lの観察領域に観測されるA相とB相の合計面積を算出し、これを距離Lで除することにより求めることができる。この場合、A相またはB相に接しているCu−Al合金の晶出相またはそれに由来するCu濃化相や、その他の異相は、Al−Fe−Si系合金層の構成要素ではないので、Al−Fe−Si系合金層の平均厚さの測定においては無視する。観察される相がA相であるか、B相であるか、あるいはその他の相であるかは、EDX等を用いた微視的分析などによって特定することができる。A相、B相それぞれの面積は画像処理によって定めることが可能である。 FIG. 3 illustrates an SEM photograph of a cross section in the brazed joint structure of the present invention. This is an example of Test No. 6 in Examples described later. A layer in which the A phase indicated as (A) and the B phase indicated as (B) (a phase that looks darker than A) is formed on the surface of the steel substrate. As a result of the analysis, both the A phase and the B phase are Al—Fe—Si based alloy layers, but more Cu exists in the A phase than in the B phase. Further, when the steel material is stainless steel, there is more Cr in the A phase than in the B phase. A whitish phase is observed in the vicinity of these phases, which is a crystallized phase of Cu-Al alloy or a Cu concentrated phase derived therefrom. The average thickness of the Al—Fe—Si alloy layer is observed in the observation region of a certain distance L in the direction along the steel substrate surface (lateral direction in the photograph of FIG. 3) by observing the structure of the cross section as shown in FIG. The total area of the A phase and the B phase to be calculated can be calculated and divided by the distance L. In this case, the crystallization phase of the Cu-Al alloy in contact with the A phase or the B phase, or the Cu concentrated phase derived therefrom, and other different phases are not constituent elements of the Al-Fe-Si alloy layer. Ignored in measuring the average thickness of the Al-Fe-Si alloy layer. Whether the observed phase is the A phase, the B phase, or another phase can be specified by microscopic analysis using EDX or the like. The areas of the A phase and the B phase can be determined by image processing.
Al−Fe−Si系合金層の平均厚さが15μm以下と薄い場合には、通常多くの場合、A相とB相が混在する組織状態となる。そして、Al−Fe−Si系合金層とAl素地中のAl相の界面は、主としてB相の晶出形態を反映した凹凸形態を呈している。Al−Fe−Si系合金層の平均厚さが15μm以下好ましくは10μm以下と薄いことだけでも、Al−Fe−Si系合金層中での割れの発生および伝播は大幅に軽減されると考えられる。それに加え、Al−Fe−Si系合金層が種類の異なるA相とB相の複相構造を有し、しかもAl相との界面が凹凸形態を呈することによって、Al−Fe−Si系合金層がさらに強化され、昇温・降温の繰り返しに対する耐久性がより向上するものと考えられる。 When the average thickness of the Al—Fe—Si-based alloy layer is as thin as 15 μm or less, in many cases, a structural state in which the A phase and the B phase are mixed is obtained. The interface between the Al-Fe-Si-based alloy layer and the Al phase in the Al substrate exhibits a concavo-convex form mainly reflecting the crystallization form of the B phase. It is considered that the occurrence and propagation of cracks in the Al—Fe—Si based alloy layer is greatly reduced only by the fact that the average thickness of the Al—Fe—Si based alloy layer is as thin as 15 μm or less, preferably 10 μm or less. . In addition, the Al—Fe—Si based alloy layer has a multiphase structure of different types of A phase and B phase, and the interface with the Al phase exhibits an uneven shape, whereby the Al—Fe—Si based alloy layer Is further strengthened, and it is considered that durability against repeated heating and cooling is further improved.
ろう付け温度での保持中には、溶融したろう材が周囲の固相と反応するので、液相の組成は三元共晶組成からずれて融点が上昇し、ろう付け温度での保持時間がある程度長い場合には、その保持時間中に液相が消失するものと考えられる。そして、保持時間が長いほど原子の拡散が進行し、凝固組織は形を失っていく。発明者らの検討によれば、この原子の拡散に伴ってAl−Fe−Si系合金層の厚さが増大し、Cu濃度が相対的に高いA相がB相を吸収して、やがてAl−Fe−Si系合金層はほとんどA相のみで構成されるようになる。このような状態になると、Al−Fe−Si系合金層の内部で粗大な割れが生じやすい。詳細な検討の結果、Al−Fe−Si系合金層の平均厚さが15μmを超えるようになる前にろう付け温度での保持を終了し、冷却過程に移行することによって、粗大な割れが生じやすいAl−Fe−Si系合金層の形成が回避される。Al−Fe−Si系合金層の平均厚さが10μmを超えるようになる前に冷却過程に移行することがより好ましい。Al−Fe−Si系合金層に占めるB相の割合は3〜70体積%程度であることが好ましい。なお、液相が消失するまでの時間は、保持温度およびろう材の使用量(生成する液相の量)に依存すると考えられるが、予備実験によりろう付け条件に応じたデータを収集しておくことによって、Al−Fe−Si系合金層の平均厚さを15μm以下好ましくは10μm以下にコントロールすることができる。 During the holding at the brazing temperature, the molten brazing material reacts with the surrounding solid phase, so that the composition of the liquid phase deviates from the ternary eutectic composition and the melting point increases, and the holding time at the brazing temperature is increased. When it is long to some extent, it is considered that the liquid phase disappears during the holding time. The longer the holding time, the more the atom diffuses and the solidified structure loses its shape. According to the study by the inventors, the thickness of the Al—Fe—Si alloy layer increases with the diffusion of the atoms, the A phase having a relatively high Cu concentration absorbs the B phase, and eventually Al. The -Fe-Si alloy layer is almost composed of only the A phase. In such a state, coarse cracks are likely to occur inside the Al—Fe—Si based alloy layer. As a result of detailed investigation, coarse cracking occurs when the holding at the brazing temperature is terminated before the average thickness of the Al—Fe—Si alloy layer exceeds 15 μm and the process proceeds to the cooling process. Easy formation of an Al-Fe-Si alloy layer is avoided. It is more preferable to shift to the cooling process before the average thickness of the Al—Fe—Si based alloy layer exceeds 10 μm. The proportion of the B phase in the Al—Fe—Si based alloy layer is preferably about 3 to 70% by volume. The time until the liquid phase disappears is considered to depend on the holding temperature and the amount of brazing material used (the amount of the liquid phase to be generated), but data corresponding to the brazing conditions is collected by preliminary experiments. Thus, the average thickness of the Al—Fe—Si based alloy layer can be controlled to 15 μm or less, preferably 10 μm or less.
〔ろう付け方法〕
ろう付けの方法は、
(i)ろう付け温度を530℃以上かつろう材の融点以上、580℃以下の温度範囲とすること、
(ii)前記のAl−Fe−Si系合金層の平均厚さが15μm以下好ましくは10μm以下となるように短時間でろう付け温度での保持を終了し、冷却過程に移行させること、
を除き、従来一般的な方法に従えばよい。ろう付け温度は570℃以下あるいは570℃未満に管理することが一層好ましい。真空ろう付けの場合は、Mgを含有する前記ろう材を適用し、上記(i)(ii)の条件を採用した上で、従来公知の真空ろう付け技術を利用すればよい。
[Brazing method]
The method of brazing is
(I) the brazing temperature is 530 ° C. or higher and the melting point of the brazing material is 580 ° C. or lower;
(Ii) ending the holding at the brazing temperature in a short time so that the average thickness of the Al—Fe—Si based alloy layer is 15 μm or less, preferably 10 μm or less, and shifting to the cooling process;
Except for the above, conventional general methods may be followed. It is more preferable to control the brazing temperature to 570 ° C. or lower or lower than 570 ° C. In the case of vacuum brazing, a conventionally known vacuum brazing technique may be used after applying the brazing material containing Mg and adopting the above conditions (i) and (ii).
鋼材として、フェライト系ステンレス鋼SUH409をめっき原板とする溶融Alめっき鋼板を用意した。板厚は0.8mm、片面あたりのめっき付着量は120g/m2、めっき層組成はAl−9質量%Siである。
アルミニウム材料として、JIS H4000、合金番号1050に相当するAl:99.5質量%以上のアルミニウム合金板材を用意した。板厚は5mmである。
ろう材として、Al−27質量%Cu−4.5質量%Si−2質量%Mg組成の合金シートを用意した。シート厚さは0.1mm、融点は約535℃である。
As a steel material, a hot-dip Al-plated steel plate using ferritic stainless steel SUH409 as a plating base plate was prepared. The plate thickness is 0.8 mm, the plating adhesion amount per side is 120 g / m 2 , and the plating layer composition is Al-9 mass% Si.
As an aluminum material, an aluminum alloy plate material of Al: 99.5 mass% or more corresponding to JIS H4000 and alloy number 1050 was prepared. The plate thickness is 5 mm.
As a brazing material, an alloy sheet having an Al-27 mass% Cu-4.5 mass% Si-2 mass% Mg composition was prepared. The sheet thickness is 0.1 mm and the melting point is about 535 ° C.
鋼材、アルミニウム材料、ろう材からそれぞれ25mm×25mm寸法の試料を切り出し、ステンレス鋼製の水平なトレイ上に、鋼材(0.8mm厚)、ろう材(0.1mm厚)、アルミニウム材料(5mm厚)の順で積み重ねて積層体とした。この積層体を水平に保った状態でトレイごと550℃の炉中に装入し、雰囲気圧力1×10-3Paで真空ろう付けに供した。積層体表面に取り付けた熱電対により材料温度をモニターし、材料温度が530℃に到達した時点からの在炉時間を「ろう付け保持時間」とした。ろう付け保持時間を2〜20分の種々の段階に設定し、所定のろう付け保持時間が経過した時点で積層体を炉外に出して冷却過程に移行させた。このようにして、ろう付け保持時間の異なる種々の「ろう付け接合体」を得た。 Samples of 25 mm × 25 mm are cut out from the steel, aluminum material and brazing material, and the steel material (0.8 mm thickness), brazing material (0.1 mm thickness), aluminum material (5 mm thickness) are placed on a horizontal tray made of stainless steel. ) To obtain a laminate. The laminated body was placed in a horizontal state with the tray placed in a furnace at 550 ° C. and subjected to vacuum brazing at an atmospheric pressure of 1 × 10 −3 Pa. The material temperature was monitored by a thermocouple attached to the surface of the laminate, and the in-furnace time from when the material temperature reached 530 ° C. was defined as “brazing holding time”. The brazing holding time was set at various stages of 2 to 20 minutes, and when the predetermined brazing holding time had elapsed, the laminate was taken out of the furnace and shifted to the cooling process. In this way, various “brazed joints” having different brazing holding times were obtained.
各保持時間のろう付け接合体について、ろう付け接合部の断面組織を観察し、鋼素地表面に沿う方向の一定距離Lの観察領域に観測される前述のA相とB相の合計面積を算出し、これを距離Lで除することにより、Al−Fe−Si系合金層の平均厚さを求めた。また、Al−Fe−Si系合金層(A相とB相の合計面積)に占めるB相の割合を算出し、B相の割合が3〜70体積%であるものを○、3体積%未満のものを×と評価した。○評価のものは、A相+B相の複相構造によるAl−Fe−Si系合金層の耐久性向上に効果的であると考えられる。 For the brazed joint of each holding time, observe the cross-sectional structure of the brazed joint, and calculate the total area of the A phase and B phase observed in the observation region of a certain distance L in the direction along the steel substrate surface. Then, by dividing this by the distance L, the average thickness of the Al—Fe—Si based alloy layer was determined. Further, the proportion of the B phase in the Al—Fe—Si based alloy layer (the total area of the A phase and the B phase) is calculated, and the proportion of the B phase is 3 to 70% by volume is less than 3% by volume. Was rated as x. O The thing of evaluation is thought to be effective for the durability improvement of the Al-Fe-Si type alloy layer by the double phase structure of A phase + B phase.
また、各保持時間のろう付け接合体について、「−40℃の気相中で30分保持 → 130℃の気相中で30分保持」を1サイクルとする冷熱衝撃試験を100サイクル実施し、試験後のろう付け接合部の断面組織を観察した。Al−Fe−Si系合金層に生じた割れの程度により、以下の基準で冷熱衝撃特性を評価した。
◎:割れが認められない
○:割れが認められるが、局部的な微小な割れであり、上記冷熱サイクルでの伝播性はほとんどないと考えられる
△:発生した微小割れが伝播して繋がったと考えられる割れが部分的に認められるが、上記冷熱サイクルで連続的な割れに進展する可能性はほとんどないと考えられる
×:発生した割れが伝播して繋がったと考えられる連続的な割れが認められ、この割れは材料破断を招く恐れがある
上記において、△評価以上であれば、昇温・降温の繰り返しを伴う多くの伝熱用途において使用可能であると判断されることから、△評価以上を合格と判定した。○評価以上であれば、昇温・降温の繰り返しを伴う多くの伝熱用途において高い信頼性が得られる。
In addition, with respect to the brazed joint of each holding time, 100 cycles of a thermal shock test in which “holding in a gas phase of −40 ° C. for 30 minutes → holding in a gas phase of 130 ° C. for 30 minutes” is 1 cycle, The cross-sectional structure of the brazed joint after the test was observed. The thermal shock characteristics were evaluated according to the following criteria depending on the degree of cracking generated in the Al—Fe—Si based alloy layer.
◎: No cracking is observed ○: Cracking is recognized, but it is a local minute crack, and it is considered that there is almost no propagation property in the above-mentioned cooling cycle △: The generated microcrack is considered to have propagated and connected It is considered that there is almost no possibility of progressing to continuous cracking in the above-described cooling cycle. ×: The continuous cracking that the generated crack is considered to have propagated and connected is recognized, This crack may lead to material breakage. In the above, if it is more than △ evaluation, it is judged that it can be used in many heat transfer applications with repeated heating and cooling, so it passes △ evaluation or more. It was determined. ○ If it is above evaluation, high reliability can be obtained in many heat transfer applications involving repeated heating and cooling.
これらの結果を表1に示す。また参考のため、図4、図5および図6に、それぞれ試験No.6、No.5およびNo.2について、冷熱衝撃試験前のろう付け接合部断面のSEM像およびEPMAによる元素検出結果を示す。 These results are shown in Table 1. For reference, FIGS. 4, 5 and 6 show the SEM image of the brazed joint cross section before the thermal shock test and the element detection results by EPMA for Test No. 6, No. 5 and No. 2, respectively. Show.
表1からわかるように、Al−Fe−Si系合金層の平均厚さが15μm以下となるようにろう付け保持を終了し冷却過程に移行したものは、昇温・降温の繰り返しによる冷熱衝撃特性が良好である。 As can be seen from Table 1, the thermal shock characteristics due to repeated temperature increase and decrease are those in which the brazing and holding are finished so that the average thickness of the Al—Fe—Si based alloy layer is 15 μm or less. Is good.
1 半導体素子
2 半導体基板
3 導体層
4 絶縁基板
5 裏面導体層
6 放熱板
7 ヒートシンク
10 接合界面
DESCRIPTION OF SYMBOLS 1 Semiconductor element 2 Semiconductor substrate 3 Conductor layer 4 Insulating substrate 5 Back surface conductor layer 6 Heat sink 7 Heat sink 10 Bonding interface
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