JP7451964B2 - Cu alloy plate and its manufacturing method - Google Patents
Cu alloy plate and its manufacturing method Download PDFInfo
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- JP7451964B2 JP7451964B2 JP2019214405A JP2019214405A JP7451964B2 JP 7451964 B2 JP7451964 B2 JP 7451964B2 JP 2019214405 A JP2019214405 A JP 2019214405A JP 2019214405 A JP2019214405 A JP 2019214405A JP 7451964 B2 JP7451964 B2 JP 7451964B2
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- 229910000881 Cu alloy Inorganic materials 0.000 title claims description 93
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 239000013078 crystal Substances 0.000 claims description 52
- 238000010438 heat treatment Methods 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 23
- 229910052802 copper Inorganic materials 0.000 claims description 15
- 239000012535 impurity Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 9
- 238000005266 casting Methods 0.000 claims description 6
- 230000007423 decrease Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 3
- 239000010949 copper Substances 0.000 description 42
- 239000000919 ceramic Substances 0.000 description 41
- 239000000758 substrate Substances 0.000 description 28
- 238000000034 method Methods 0.000 description 19
- 238000005219 brazing Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000002244 precipitate Substances 0.000 description 7
- 238000005097 cold rolling Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000005304 joining Methods 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005098 hot rolling Methods 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000011179 visual inspection Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
Description
本発明は、セラミック配線基板等の配線パターンに用いられるＣｕ合金板およびその製造方法に関するものである。 The present invention relates to a Cu alloy plate used for wiring patterns of ceramic wiring boards and the like, and a method for manufacturing the same.
パワーデバイスの半導体素子を実装する基板として、セラミック配線基板が広く用いられている。このセラミック配線基板は、セラミック基板と、セラミック基板上に設けられ、例えば、エッチングにより所定箇所が除去されて配線パターン（Ｃｕ配線）になるＣｕ板とを備えている。このＣｕ板としては、無酸素銅やタフピッチ銅等の純Ｃｕ板が用いられる他、Ｎｉ、Ｚｎ、ＺｒまたはＳｎの何れかを含むＣｕ合金板等が用いられている。 Ceramic wiring boards are widely used as substrates on which semiconductor elements of power devices are mounted. This ceramic wiring board includes a ceramic substrate and a Cu plate that is provided on the ceramic substrate and is formed into a wiring pattern (Cu wiring) by removing a predetermined portion by etching, for example. As this Cu plate, a pure Cu plate such as oxygen-free copper or tough pitch copper is used, as well as a Cu alloy plate containing any one of Ni, Zn, Zr, or Sn.
そして、セラミック基板とＣｕ板との接合方法は、例えば、Ｔｉなどの活性金属を含有したろう材を用いて接合する活性金属ろう付け法がある。また、別の接合方法として、ろう材を用いずにセラミック基板と表面を酸化させたＣｕ板とを接触配置して加熱して、界面に酸化Ｃｕからなる融液層を形成することで接合する直接接合法がある。
上記の各接合方法は、セラミック基板とＣｕ板とを、ろう材もしくは酸化Ｃｕを介して積層して積層体とし、この積層体を、加熱炉中で、例えば、５００℃以上１０５０℃以下の条件で加熱接合される（例えば、特許文献１）。
As a method for joining the ceramic substrate and the Cu plate, for example, there is an active metal brazing method in which the ceramic substrate and the Cu plate are joined using a brazing material containing an active metal such as Ti. Another bonding method is to bond a ceramic substrate and a Cu plate whose surface has been oxidized without using a brazing material by placing them in contact with each other and heating them to form a melt layer made of oxidized Cu at the interface. There is a direct bonding method.
In each of the above bonding methods, a ceramic substrate and a Cu plate are laminated via a brazing material or Cu oxide to form a laminate, and this laminate is heated in a heating furnace under conditions of, for example, 500°C or more and 1050°C or less. (for example, Patent Document 1).
このように、セラミック基板とＣｕ板の接合は、上述の加熱接合によって実施されるため、その処理中にＣｕ板の結晶粒が成長して粗大化するという現象が起こる場合がある。例えば、純Ｃｕ板の場合は、上述の加熱接合を経ると、配線パターンとなる圧延面の平均結晶粒径が粗大化し、目視で確認できるほどの大きさになる場合がある。
粗大化したＣｕの結晶粒は、配線パターンの外観検査等で結晶粒界を欠陥であると誤認される不具合が生じる。このため、セラミック配線基板に用いられるＣｕ板は、上述の加熱接合を受けた後でも結晶粒の粗大化を抑える必要がある。
As described above, since the ceramic substrate and the Cu plate are bonded by the above-described heating bonding, a phenomenon may occur in which the crystal grains of the Cu plate grow and become coarse during the process. For example, in the case of a pure Cu plate, after the above-described heat bonding, the average crystal grain size of the rolled surface that becomes the wiring pattern becomes coarse, and may become so large that it can be visually confirmed.
Coarse Cu crystal grains cause a problem in which grain boundaries are mistakenly recognized as defects during visual inspection of wiring patterns. For this reason, it is necessary for the Cu plate used in the ceramic wiring board to suppress coarsening of crystal grains even after being subjected to the above-described heat bonding.
本発明の目的は、セラミック基板との接合で実施される加熱接合を経ても、Ｃｕ板の圧延面における結晶粒の粗大化を抑制できる、セラミック配線基板等の配線パターンに好適な新規のＣｕ合金板およびその製造方法を提供することにある。 An object of the present invention is to provide a new Cu alloy suitable for wiring patterns of ceramic wiring boards, etc., which can suppress coarsening of crystal grains on the rolled surface of a Cu plate even after heat bonding is performed for joining with a ceramic substrate. An object of the present invention is to provide a board and a method for manufacturing the same.
上記の課題を解決するため、本発明は次のように構成される。
本発明のＣｕ合金板は、０．００３質量％以上０．０１０質量％未満のＺｒを含有し、残部がＣｕおよび不可避的不純物からなる組成を有し、導電率が９８％ＩＡＣＳ以上であり、９００℃で１時間加熱した後の圧延面における平均結晶粒径が５０μｍ以上３００μｍ以下である。
In order to solve the above problems, the present invention is configured as follows.
The Cu alloy plate of the present invention contains 0.003% by mass or more and less than 0.010% by mass of Zr, and has a composition with the balance consisting of Cu and inevitable impurities, and has an electrical conductivity of 98% IACS or more, The average crystal grain size on the rolled surface after heating at 900° C. for 1 hour is 50 μm or more and 300 μm or less.
また、本発明のＣｕ合金板は、０．００３質量％以上０．０１０質量％未満のＺｒと、０．０３質量％以上０．０８質量％以下のＡｇを含有し、残部がＣｕおよび不可避的不純物からなる組成を有し、導電率が９８％ＩＡＣＳ以上であり、９００℃で１時間加熱した後の圧延面における平均結晶粒径が５０μｍ以上３００μｍ以下である。 Further, the Cu alloy plate of the present invention contains 0.003% by mass or more and less than 0.010% by mass of Zr and 0.03% by mass or more and 0.08% by mass or less of Ag, with the balance being Cu and unavoidable It has a composition consisting of impurities, has an electrical conductivity of 98% IACS or more, and has an average crystal grain size on the rolled surface of 50 μm or more and 300 μm or less after heating at 900° C. for 1 hour.
本発明のＣｕ合金板は、０．００３質量％以上０．０１０質量％未満のＺｒを含有し、残部がＣｕおよび不可避的不純物からなるＣｕ合金を鋳造し、または、０．００３質量％以上０．０１０質量％未満のＺｒと、０．０３質量％以上０．０８質量％以下のＡｇを含有し、残部がＣｕおよび不可避的不純物からなるＣｕ合金を鋳造し、熱間圧延を行なった後、熱処理を挿んだ冷間圧延により、最終的な製品板厚の１．４倍以上２．０倍以下の板厚まで加工して得た素材を、７５０℃以上９５０℃未満で加熱した後、毎分５０℃以上の降温速度で３００℃以下まで冷却する熱処理を行ない、平均結晶粒径を５０μｍ以上３００μｍ以下にした後、前記素材を前記製品板厚まで圧延することで得ることができる。 The Cu alloy plate of the present invention is produced by casting a Cu alloy containing 0.003% by mass or more and less than 0.010% by mass of Zr, with the balance consisting of Cu and inevitable impurities, or by casting a Cu alloy containing 0.003% by mass or more and less than 0.010% by mass of Zr, or After casting and hot rolling a Cu alloy containing less than .010% by mass of Zr and 0.03% by mass or more and 0.08% by mass or less of Ag, with the balance consisting of Cu and unavoidable impurities, After heating the material obtained by processing it to a plate thickness of 1.4 times or more and 2.0 times or less than the final product plate thickness by cold rolling with heat treatment at a temperature of 750°C or more and less than 950°C, It can be obtained by performing heat treatment to cool down to 300°C or less at a temperature decreasing rate of 50°C or more per minute to make the average crystal grain size 50 μm or more and 300 μm or less, and then rolling the material to the product plate thickness.
本発明によれば、セラミック基板とＣｕ合金板との接合のための加熱接合を経ても、Ｃｕ合金板の圧延面における結晶粒が粗大化を抑制することができ、セラミック配線基板等の配線パターンの製造に有用な技術となる。 According to the present invention, coarsening of crystal grains on the rolled surface of the Cu alloy plate can be suppressed even after heat bonding for bonding the ceramic substrate and the Cu alloy plate, and wiring patterns of ceramic wiring boards, etc. This technology is useful for manufacturing.
本発明のＣｕ合金板は、０．００３質量％以上０．０１０質量％未満のＺｒを含有し、残部がＣｕおよび不可避的不純物からなる組成を有し、導電率が９８％ＩＡＣＳ以上であり、９００℃で１時間加熱した後の圧延面における平均結晶粒径が５０μｍ以上３００μｍ以下である。 The Cu alloy plate of the present invention contains 0.003% by mass or more and less than 0.010% by mass of Zr, and has a composition with the balance consisting of Cu and inevitable impurities, and has an electrical conductivity of 98% IACS or more, The average crystal grain size on the rolled surface after heating at 900° C. for 1 hour is 50 μm or more and 300 μm or less.
上述したように、セラミック配線基板の配線パターンを形成するＣｕ板として、従来から用いられている純Ｃｕ板は、セラミック基板との接合のための加熱接合を経ると、結晶粒が粗大化する場合がある。ここで、本発明で規定する９００℃で１時間加熱する条件は、セラミック基板とＣｕ合金板とを接合する際の加熱接合を想定した温度で、十分な時間加熱する条件として選択したものである。 As mentioned above, pure Cu plates conventionally used as Cu plates for forming the wiring patterns of ceramic wiring boards tend to have coarse grains when subjected to heat bonding for bonding with ceramic substrates. There is. Here, the condition of heating at 900° C. for 1 hour specified in the present invention is a temperature assuming heat bonding when bonding a ceramic substrate and a Cu alloy plate, and was selected as a condition of heating for a sufficient time. .
Ｃｕ合金板の圧延面における結晶粒が粗大化した場合は、結晶粒が目視で確認できるほどの大きさになり、Ｃｕ合金板の表面は結晶粒界が目立った外観を呈するようになる。このような状態のＣｕ合金板の表面について、外観検査を機械的な画像処理で実施した場合は、結晶粒界と疵との判別が難しくなり、結晶粒界をＣｕ合金板表面の疵と誤認することが数多く発生する。
本発明のＣｕ合金板は、９００℃で１時間加熱した後の圧延面における平均結晶粒径を３００μｍ以下にする。これにより、本発明のＣｕ合金板は、その圧延面の結晶粒が目視で確認することの困難な程に十分細かく、外観検査の画像処理において、結晶粒界と疵との判別が容易になる。また、上記と同様の理由から、本発明の実施形態にかかるＣｕ合金板は、９００℃で１時間加熱した後の圧延面における平均結晶粒径を２８０μｍ以下が好ましく、２６０μｍ以下がより好ましい。
When the crystal grains on the rolled surface of the Cu alloy plate become coarse, the crystal grains become so large that they can be visually confirmed, and the surface of the Cu alloy plate has an appearance in which grain boundaries are conspicuous. If the surface of a Cu alloy plate in such a state is visually inspected using mechanical image processing, it will be difficult to distinguish between grain boundaries and flaws, and grain boundaries may be mistaken for flaws on the surface of the Cu alloy plate. Many things happen.
The Cu alloy plate of the present invention has an average grain size of 300 μm or less on the rolled surface after being heated at 900° C. for 1 hour. As a result, in the Cu alloy plate of the present invention, the crystal grains on the rolled surface are sufficiently fine that they are difficult to visually confirm, and it becomes easy to distinguish between grain boundaries and flaws in image processing for appearance inspection. . Furthermore, for the same reason as above, the Cu alloy plate according to the embodiment of the present invention preferably has an average crystal grain size on the rolled surface after heating at 900° C. for 1 hour of 280 μm or less, more preferably 260 μm or less.
本発明のＣｕ合金板は、９００℃で１時間加熱した後の圧延面における平均結晶粒径を５０μｍ以上にすることで、過度な硬さの上昇が抑制され、Ｃｕ合金板の割れや欠けの誘発を抑制できる。
また、セラミック基板とＣｕ合金板では熱膨張率が異なるため、上述の加熱接合により接合されたセラミック基板とＣｕ合金板との接合体が冷却される際に、Ｃｕ合金板がセラミック基板よりもより大きく収縮しようとする。本発明のＣｕ合金板は、上述の平均結晶粒径を５０μｍ以上にすることで、加熱接合後の冷却における、セラミック基板とＣｕ合金板の収縮量の差を吸収させることができ、接合部の剥がれやセラミック基板の破損を抑制することができる。
By making the Cu alloy plate of the present invention have an average crystal grain size of 50 μm or more on the rolled surface after heating at 900°C for 1 hour, excessive increase in hardness is suppressed and cracks and chips of the Cu alloy plate are prevented. The trigger can be suppressed.
Furthermore, since the ceramic substrate and the Cu alloy plate have different coefficients of thermal expansion, when the joined body of the ceramic substrate and the Cu alloy plate bonded by the above-mentioned thermal bonding is cooled, the Cu alloy plate has a higher coefficient of thermal expansion than the ceramic substrate. Trying to shrink a lot. By making the average crystal grain size of the Cu alloy plate of the present invention 50 μm or more, it is possible to absorb the difference in the amount of shrinkage between the ceramic substrate and the Cu alloy plate during cooling after heat bonding, and the bonded portion Peeling and damage to the ceramic substrate can be suppressed.
また、セラミック配線基板は、パワーデバイス等に使用される場合において、搭載した半導体素子が通電によって発熱して温度上昇した際に、セラミック基板とＣｕ合金板との熱膨張差や、Ｃｕ合金板における結晶粒成長の助長化によって、接合部に剥がれようとする力が生じる場合がある。
これに対し、本発明のＣｕ合金板は、Ｃｕ合金板の９００℃で１時間加熱した後の圧延面における平均結晶粒径を５０μｍ以上にすることで、半導体素子の発熱によって生じる、セラミック基板とＣｕ合金板との熱膨張差を緩和できることに加え、Ｃｕ合金板における結晶粒成長の助長化を抑制できる。このため、本発明のＣｕ合金板は、セラミック基板との接合部の剥がれや、セラミック基板の破損を抑制できる。また、過度な硬さの上昇を抑え、Ｃｕ合金板を製造する際のハンドリング時に生じる割れや欠けを抑制する観点から、本発明の実施形態にかかるＣｕ合金板は、９００℃で１時間加熱した後の圧延面における平均結晶粒径を２００μｍ以上にすることが好ましく、２２０μｍ以上がより好ましい。
In addition, when ceramic wiring boards are used in power devices, etc., when the mounted semiconductor element generates heat due to electricity and its temperature rises, the difference in thermal expansion between the ceramic board and the Cu alloy plate, and the Encouraging crystal grain growth may generate a force that tends to cause the joint to peel.
On the other hand, the Cu alloy plate of the present invention has an average crystal grain size of 50 μm or more on the rolled surface after heating the Cu alloy plate at 900°C for 1 hour, so that the Cu alloy plate is free from ceramic substrates caused by heat generation of semiconductor elements. In addition to being able to alleviate the difference in thermal expansion with the Cu alloy plate, it is also possible to suppress the promotion of crystal grain growth in the Cu alloy plate. Therefore, the Cu alloy plate of the present invention can suppress peeling of the bonded portion with the ceramic substrate and damage to the ceramic substrate. In addition, from the viewpoint of suppressing an excessive increase in hardness and suppressing cracks and chips that occur during handling when manufacturing a Cu alloy plate, the Cu alloy plate according to the embodiment of the present invention was heated at 900 ° C. for 1 hour. The average grain size on the subsequent rolling surface is preferably 200 μm or more, more preferably 220 μm or more.
本発明のＣｕ合金板は、導電率が９８％ＩＡＣＳ以上である。セラミック配線基板の配線パターンに用いられるＣｕ板として、上述した純Ｃｕ板の導電率は、１００％ＩＡＣＳ前後であり、本発明のＣｕ合金板は、これに近似した優れた導電性を維持する。ここで、導電性の良否は、熱伝導性の良否と強い相関関係があるため、本発明のＣｕ合金板は、熱伝導性においても純Ｃｕ板と同等の優れた特性を維持するものである。
そして、パワーデバイスの実装基板として用いられるセラミック配線基板では、Ｃｕ配線に大きな電流が流れるため、上述した純Ｃｕ板に相当する優れた導電性や熱伝導性を具備する材料を、配線パターンの材料として用いることが求められる。このため、本発明のＣｕ合金板は、こうした要求に合ったものであるといえる。そして、本発明のＣｕ合金板は、導電率が９９％ＩＡＣＳ以上であることが好ましい。
The Cu alloy plate of the present invention has an electrical conductivity of 98% IACS or higher. The electrical conductivity of the pure Cu board mentioned above as a Cu board used in the wiring pattern of a ceramic wiring board is around 100% IACS, and the Cu alloy board of the present invention maintains excellent electrical conductivity close to this. Here, since the quality of electrical conductivity has a strong correlation with the quality of thermal conductivity, the Cu alloy plate of the present invention maintains excellent properties equivalent to pure Cu plates in terms of thermal conductivity. .
In the ceramic wiring board used as a mounting board for power devices, a large current flows through the Cu wiring, so a material with excellent electrical conductivity and thermal conductivity equivalent to the pure Cu board mentioned above is used as the material for the wiring pattern. It is required to be used as a Therefore, it can be said that the Cu alloy plate of the present invention meets these requirements. The Cu alloy plate of the present invention preferably has a conductivity of 99% IACS or higher.
本発明のＣｕ合金板は、０．００３質量％以上０．０１０質量％未満のＺｒを含有し、残部がＣｕおよび不可避的不純物からなる組成を有する。
Ｃｕ合金板中に含まれる微量成分の種類とその含有量は、Ｃｕ合金板の導電率や加熱接合した後の結晶粒径に大きく影響を及ぼす。一般に、微量成分の含有量が多くなるほど導電率は低下する一方、同時に、加熱接合において結晶粒が粗大化することを抑制する効果が得られる。
本発明のＣｕ合金板は、上記の特性を得るためにＺｒを採用する。そして、Ｃｕ合金板におけるＺｒの含有量は、０．００３質量％以上にすることで、９００℃で１時間加熱した後の平均結晶粒径を３００μｍ以下に抑えることができる。また、上記と同様の理由から、Ｚｒの含有量は、０．００５質量％以上にすることが好ましい。
一方、Ｃｕ合金板へのＺｒの含有量は、０．０１０質量％未満にすることで、９８％ＩＡＣＳ以上の導電率を安定して維持することができる。また、Ｃｕ合金板へのＺｒの含有量は、０．０１０質量％未満にすることで、過度な硬さの上昇が抑制され、Ｃｕ合金板の切断時のバリの発生を抑制できる上、割れや欠けの誘発を抑制できる。また、上記と同様の理由から、Ｚｒの含有量は、０．００９質量％以下にするこが好ましい。
The Cu alloy plate of the present invention has a composition containing 0.003% by mass or more and less than 0.010% by mass of Zr, with the balance consisting of Cu and inevitable impurities.
The type and content of trace components contained in the Cu alloy plate greatly affect the conductivity of the Cu alloy plate and the crystal grain size after heat bonding. Generally, as the content of trace components increases, the electrical conductivity decreases, while at the same time, the effect of suppressing coarsening of crystal grains during heat bonding can be obtained.
The Cu alloy plate of the present invention employs Zr in order to obtain the above characteristics. By setting the Zr content in the Cu alloy plate to 0.003% by mass or more, the average crystal grain size after heating at 900° C. for 1 hour can be suppressed to 300 μm or less. Further, for the same reason as above, the Zr content is preferably 0.005% by mass or more.
On the other hand, by setting the content of Zr in the Cu alloy plate to less than 0.010% by mass, conductivity of 98% IACS or higher can be stably maintained. In addition, by setting the Zr content in the Cu alloy plate to less than 0.010% by mass, it is possible to suppress an excessive increase in hardness, suppress the occurrence of burrs when cutting the Cu alloy plate, and prevent cracking. It can suppress the occurrence of cracking and chipping. Further, for the same reason as above, the Zr content is preferably 0.009% by mass or less.
また、本発明の実施形態にかかるＣｕ合金板は、上記のＺｒに加えて、０．０３質量％以上０．０８質量％以下のＡｇを含有し、残部がＣｕおよび不可避的不純物からなる組成を有する。
Ａｇは、Ｚｒよりも含有量に対する導電率の低下が少ない元素である。また、Ａｇは、高温加熱において結晶粒が粗大化することを抑制する効果も持つ。本発明の実施形態にかかるＣｕ合金板は、Ｚｒと共にＡｇを複合で含有させることにより、導電率のさらなる低下を抑制しつつ、結晶粒の粗大化を抑制する効果を高めることができる。
ここで、Ｃｕ合金板へのＡｇの含有量は、０．０３質量％以上にすることで、結晶粒の粗大化を抑制する効果を維持することができる。上記と同様の理由から、Ａｇの含有量は、０．０４質量％以上にすることが好ましい。
一方、Ｃｕ合金板へのＡｇの含有量は、０．０８質量％以下にすることで、導電率の低下を抑制できる。また、上記と同様の理由から、Ａｇの含有量は、０．０６質量％以下にすることが好ましい。
Further, the Cu alloy plate according to the embodiment of the present invention contains, in addition to the above-mentioned Zr, 0.03% by mass or more and 0.08% by mass or less of Ag, with the balance consisting of Cu and unavoidable impurities. have
Ag is an element whose conductivity decreases less with respect to its content than Zr. Furthermore, Ag also has the effect of suppressing coarsening of crystal grains during high-temperature heating. By containing Ag in combination with Zr, the Cu alloy plate according to the embodiment of the present invention can enhance the effect of suppressing coarsening of crystal grains while suppressing further reduction in electrical conductivity.
Here, by setting the content of Ag in the Cu alloy plate to 0.03% by mass or more, the effect of suppressing coarsening of crystal grains can be maintained. For the same reason as above, the content of Ag is preferably 0.04% by mass or more.
On the other hand, by setting the content of Ag in the Cu alloy plate to 0.08% by mass or less, the decrease in electrical conductivity can be suppressed. Further, for the same reason as above, the content of Ag is preferably 0.06% by mass or less.
次に、本発明のＣｕ合金板の製造方法について説明する。
本発明のＣｕ合金板は、上述した添加元素の含有量を調整し、０．００３質量％以上０．０１０質量％未満のＺｒを含有し、残部がＣｕおよび不可避的不純物からなるＣｕ合金を鋳造し、これに熱間圧延を行なった後、熱処理を挿んだ冷間圧延を行ない、目的の製品板厚まで加工することにより得る。ここで、本発明の意図する特性を安定して得るためには、先ず、熱間圧延を行なった後、熱処理を挿んだ冷間圧延により、最終的な製品板厚の１．４倍以上２．０倍以下の板厚まで加工して素材を得る。そして、この素材を７５０℃以上９５０℃未満に加熱してから、毎分５０℃以上の降温速度で３００℃以下まで冷却する熱処理を行ない、圧延面における平均結晶粒径を５０μｍ以上３００μｍ以下に調整する。そして、この素材を製品板厚まで冷間圧延することで、本発明のＣｕ合金板を得ることができる。
Next, a method for manufacturing a Cu alloy plate according to the present invention will be explained.
The Cu alloy plate of the present invention is produced by adjusting the content of the above-mentioned additive elements and casting a Cu alloy containing 0.003% by mass or more and less than 0.010% by mass of Zr, with the remainder consisting of Cu and unavoidable impurities. This is then hot rolled, followed by cold rolling with heat treatment, and processed to the desired product plate thickness. Here, in order to stably obtain the characteristics intended by the present invention, first hot rolling is performed, followed by cold rolling with heat treatment, which is at least 1.4 times the final product board thickness. The material is obtained by processing the plate to a thickness that is 2.0 times or less. Then, this material is heated to 750°C or more and less than 950°C, and then heat treated to cool down to 300°C or less at a cooling rate of 50°C or more per minute, and the average grain size on the rolled surface is adjusted to 50 μm or more and 300 μm or less. do. Then, the Cu alloy plate of the present invention can be obtained by cold rolling this material to the product thickness.
本発明のＣｕ合金板の製造方法において、熱処理を行なう素材の板厚を、製品板厚の１．４倍以上２．０倍以下にするのは、熱処理後の冷間圧延において、Ｃｕ合金板に蓄積される歪みの量を適正な範囲にするためである。
ここで、結晶粒の粗大化に影響する因子の一つとして、Ｃｕ合金板の内部に蓄積された歪みがあり、この歪みの蓄積量が多くなると、結晶粒が粗大化しやすくなる。一方、歪みの蓄積量が少なくなると、Ｃｕ合金板は軟らかくなるため、切断時にバリを発生させたり、ハンドリング時に変形を誘発させたりする等、製造する際の取り扱いが難しくなる。
In the method for manufacturing a Cu alloy plate of the present invention, the thickness of the material to be heat treated is set to 1.4 times or more and 2.0 times or less than the product plate thickness, because the Cu alloy plate is cold rolled after heat treatment. This is to keep the amount of distortion accumulated in the image within an appropriate range.
Here, one of the factors that influences the coarsening of crystal grains is the strain accumulated inside the Cu alloy plate, and as the amount of accumulated strain increases, the crystal grains tend to coarsen. On the other hand, when the amount of accumulated strain decreases, the Cu alloy plate becomes softer, which makes handling during manufacturing difficult, such as generating burrs during cutting and inducing deformation during handling.
本発明の製造方法において、熱処理を行なう素材の板厚は、得ようとする製品板厚の２．０倍以下にすることで、冷間圧延でＣｕ合金板に蓄積される歪みの量を抑制でき、得られるＣｕ合金板を加熱接合した際にも結晶粒の粗大化を抑制できる。
また、本発明の製造方法において、熱処理を行なう素材の板厚は、得ようとする製品板厚の１．４倍以上にすることで、Ｃｕ合金板に蓄積される歪みの量を適性化でき、Ｃｕ合金板の硬さを適正に維持でき、切断時のバリの発生を抑制できる上、ハンドリング時の変形を抑制できる等、製造する際の取り扱いが容易になる。
In the manufacturing method of the present invention, the thickness of the material to be heat treated is 2.0 times or less than the desired product thickness, thereby suppressing the amount of distortion accumulated in the Cu alloy plate during cold rolling. Therefore, coarsening of crystal grains can be suppressed even when the resulting Cu alloy plates are heat-bonded.
In addition, in the manufacturing method of the present invention, by making the thickness of the material to be heat-treated at least 1.4 times the thickness of the product to be obtained, the amount of distortion accumulated in the Cu alloy plate can be optimized. The hardness of the Cu alloy plate can be maintained appropriately, the generation of burrs can be suppressed during cutting, and deformation during handling can be suppressed, making it easier to handle during manufacturing.
本発明の製造方法では、素材に施す熱処理を、７５０℃以上９５０℃未満の条件で行なう。熱処理の加熱温度は、７５０℃以上にすることで、その目的である加工中の歪みの開放を促進することができ、続く冷間圧延で疵が発生することを抑制できる他、加熱接合時の結晶粒粗大化を抑制できる。
一方、熱処理の加熱温度は、９５０℃未満にすることで、Ｚｒの析出物を微細にすることができ、加熱接合時の結晶粒粗大化を抑制できることに加え、導電率の低下を抑えることもできる。
In the manufacturing method of the present invention, the heat treatment applied to the material is performed at a temperature of 750°C or higher and lower than 950°C. By setting the heating temperature for heat treatment to 750°C or higher, it is possible to promote the release of strain during processing, which is the purpose of heat treatment, to suppress the occurrence of flaws in the subsequent cold rolling, and to prevent defects during heat bonding. Coarsening of crystal grains can be suppressed.
On the other hand, by setting the heating temperature for heat treatment to less than 950°C, it is possible to make the Zr precipitates finer, suppress grain coarsening during heat bonding, and also suppress a decrease in electrical conductivity. can.
Ｃｕ合金板中のＺｒは、Ｃｕに固溶した状態、もしくはＺｒ単体や化合物として析出した状態で存在する。ここで、析出した状態で存在するＺｒは、微細な析出物として存在する場合には加熱接合での結晶粒粗大化を抑える効果に寄与する一方、粗大に成長した析出物として存在する場合には結晶粒粗大化を抑える効果に寄与することは困難となる。
本発明の主旨である、加熱接合後の結晶粒粗大化を抑制する効果を安定して得るためには、Ｚｒの析出物を大きく成長させないことが重要である。ここで、Ｃｕ中のＺｒは、４００℃以上６００℃以下の範囲で加熱保持されると析出し、析出物の成長が進む。このため、本発明の製造方法において、４００℃以上６００℃以下の温度領域で加熱される時間をなるべく短くすることが重要である。
したがって、本発明の製造方法において、素材に施す熱処理は、毎分５０℃以上の降温速度で３００℃以下まで冷却する。これにより、本発明の製造方法は、得られるＣｕ合金板のＺｒの析出物の成長を抑制でき、加熱接合後の結晶粒粗大化を抑制できる。
Zr in the Cu alloy plate exists in a state in which it is dissolved in Cu, or in a state in which it is precipitated as Zr alone or as a compound. Here, when Zr exists in a precipitated state, it contributes to the effect of suppressing crystal grain coarsening during heat bonding when it exists as fine precipitates, but when it exists as coarsely grown precipitates, it contributes to the effect of suppressing grain coarsening. It becomes difficult to contribute to the effect of suppressing crystal grain coarsening.
In order to stably obtain the effect of suppressing grain coarsening after heat bonding, which is the gist of the present invention, it is important that Zr precipitates do not grow large. Here, Zr in Cu precipitates when heated and maintained in a range of 400° C. or more and 600° C. or less, and the growth of the precipitates progresses. Therefore, in the manufacturing method of the present invention, it is important to shorten the heating time in the temperature range of 400° C. or higher and 600° C. or lower as much as possible.
Therefore, in the manufacturing method of the present invention, the heat treatment performed on the material is performed by cooling the material to 300° C. or less at a temperature decreasing rate of 50° C. or more per minute. Thereby, the manufacturing method of the present invention can suppress the growth of Zr precipitates in the obtained Cu alloy plate, and can suppress coarsening of crystal grains after heat bonding.
本発明のＣｕ合金板は、セラミック配線基板の配線パターンとなる部材として好適である。セラミック配線基板は、Ｃｕ板またはＣｕ合金板と、セラミック基板とが接合されている。ここで、セラミック基板としては、例えば、アルミナ（Ａｌ２Ｏ３）や窒化アルミニウム（ＡｌＮ）等で構成されるセラミック焼結体が用いられる。
本発明のＣｕ合金板は、セラミック基板との間に、接合層を介して接合される。そして、その接合層は、直接接合法または活性金属ろう付け法等によって形成できる。
The Cu alloy plate of the present invention is suitable as a member serving as a wiring pattern of a ceramic wiring board. A ceramic wiring board includes a Cu plate or a Cu alloy plate and a ceramic substrate bonded together. Here, as the ceramic substrate, for example, a ceramic sintered body made of alumina (Al 2 O 3 ), aluminum nitride (AlN), or the like is used.
The Cu alloy plate of the present invention is bonded to a ceramic substrate via a bonding layer. The bonding layer can be formed by a direct bonding method, an active metal brazing method, or the like.
直接接合法は、接合面を酸化させたＣｕ合金板と、セラミック基板を積層して所定の条件（例えば、５００℃以上１１００℃以下の温度で１分加熱）で加熱して、接合界面に酸化Ｃｕからなる融液層を形成した後に冷却することで接合する方法である。そして、本発明のＣｕ合金板に、この直接接合法を適用すると、Ｃｕ合金板とセラミック基板の間に形成される接合層は、酸化Ｃｕ合金となる。
また、活性金属ろう付け法は、Ｃｕ板とセラミック基板をＴｉなどの活性金属を含むろう材を挿んで積層し、所定の条件（例えば８００℃以上１０００℃以下の温度で５分加熱など）で加熱して、ろう材を溶融した後に冷却することで接合する方法である。そして、本発明のＣｕ合金板に、この活性金属ろう付け法を適用すると、Ｃｕ合金板とセラミック基板の間に形成される接合層は、ろう材層となる。
In the direct bonding method, a Cu alloy plate with an oxidized bonding surface and a ceramic substrate are laminated and heated under predetermined conditions (for example, heating at a temperature of 500°C to 1100°C for 1 minute) to oxidize the bonding interface. This is a method of joining by forming a melt layer made of Cu and then cooling it. When this direct bonding method is applied to the Cu alloy plate of the present invention, the bonding layer formed between the Cu alloy plate and the ceramic substrate becomes an oxidized Cu alloy.
In addition, in the active metal brazing method, a Cu plate and a ceramic substrate are laminated with a brazing material containing an active metal such as Ti inserted, and then heated under predetermined conditions (for example, heated for 5 minutes at a temperature of 800°C or more and 1000°C or less). This is a method of joining by heating to melt the brazing filler metal and then cooling it. When this active metal brazing method is applied to the Cu alloy plate of the present invention, the bonding layer formed between the Cu alloy plate and the ceramic substrate becomes a brazing material layer.
無酸素銅を母材にして、表１に示すＺｒ、Ａｇを添加し、高周波溶解炉を用いて窒素雰囲気下で溶製し、厚さ２５ｍｍ、幅３０ｍｍ、長さ１５０ｍｍのインゴットを得た。
このインゴットを加熱して、厚さ５ｍｍまで熱間圧延した後、冷間圧延によって厚さ０．５ｍｍまで加工して、Ｃｕ合金素材を得た。各Ｃｕ合金素材に対して、表１に示す条件で加熱した後、各降温速度で３００℃以下まで冷却する熱処理を行なった。
熱処理後の各Ｃｕ合金素材の結晶組織を観察し、熱処理後の圧延面における平均結晶粒径を測定した。
Using oxygen-free copper as a base material, Zr and Ag shown in Table 1 were added and melted in a nitrogen atmosphere using a high frequency melting furnace to obtain an ingot with a thickness of 25 mm, width of 30 mm, and length of 150 mm.
This ingot was heated and hot rolled to a thickness of 5 mm, and then cold rolled to a thickness of 0.5 mm to obtain a Cu alloy material. Each Cu alloy material was heated under the conditions shown in Table 1, and then subjected to heat treatment in which it was cooled to 300° C. or lower at each cooling rate.
The crystal structure of each Cu alloy material after heat treatment was observed, and the average crystal grain size on the rolled surface after heat treatment was measured.
平均結晶粒径の測定は、ＪＩＳ－Ｈ０５０１「伸銅品結晶粒度試験方法」に規定された切断法によって実施した。具体的には、被測定試料の圧延面を研磨後にエッチングして結晶組織を鮮明化し、その結晶組織を金属顕微鏡で２５倍に拡大して撮影した。そして、その結晶組織の写像（写真）上において、その写像（写真）の中心を通り互いが直交するように、その写像（写真）の水平方向（圧延方向）および上下方向（圧延幅方向）に直線を引いた。次いで、水平方向の直線の写像（写真）内の線分の長さＬ１と、上下方向の直線の写像（写真）内の線分の長さＬ２を求め、線分の全長Ｌ（Ｌ１＋Ｌ２）を算定した。また、長さＬ１の線分が通過する結晶粒の個数Ｐ１および長さＬ２の線分が通過する結晶粒の個数Ｐ２を求め、結晶粒の総数Ｐ（Ｐ１＋Ｐ２）を算定した。そして、結晶粒１個あたりの切断長さ、つまり、全長Ｌ／総数Ｐの値を求め、その値を平均結晶粒径とした。 The average crystal grain size was measured by the cutting method specified in JIS-H0501 "Crystal grain size testing method for rolled copper products". Specifically, the rolled surface of the sample to be measured was polished and then etched to clarify the crystal structure, and the crystal structure was photographed using a metallurgical microscope at a magnification of 25 times. Then, on the map (photograph) of the crystal structure, the horizontal direction (rolling direction) and the vertical direction (rolling width direction) of the map (photo) are aligned so that they pass through the center of the map (photo) and are orthogonal to each other. I drew a straight line. Next, find the length L1 of the line segment in the horizontal straight line mapping (photo) and the length L2 of the line segment in the vertical straight line mapping (photo), and calculate the total length L (L1 + L2) of the line segment. Calculated. In addition, the number P1 of crystal grains through which a line segment of length L1 passes and the number P2 of crystal grains through which a line segment of length L2 passes were determined, and the total number of crystal grains P(P1+P2) was calculated. Then, the cutting length per crystal grain, that is, the value of total length L/total number P was determined, and this value was taken as the average grain size.
そして、上記で得た各Ｃｕ合金素材について、表１の板厚比欄に示した熱処理前板厚／製品板厚の値に合わせて冷間圧延をして、本発明例となる試料Ｎｏ．１～Ｎｏ．１０、従来例となる試料Ｎｏ．１１、および比較例となる試料Ｎｏ．１２～Ｎｏ．２４のＣｕ合金板を得た。 Then, each of the Cu alloy materials obtained above was cold rolled according to the value of thickness before heat treatment/product thickness shown in the sheet thickness ratio column of Table 1, and sample No. 1, which is an example of the present invention, was obtained. 1~No. 10. Sample No. 1, which is a conventional example. 11, and sample No. 11, which is a comparative example. 12~No. No. 24 Cu alloy plates were obtained.
各Ｃｕ合金板の導電率を測定した。また、各Ｃｕ合金板を９００℃で１時間加熱し、圧延面の結晶組織を観察し、平均結晶粒径を測定した。その結果を表１に示す。
従来例となる試料Ｎｏ．１１の純ＣｕからなるＣｕ板は、９００℃で１時間加熱後の平均結晶径が７００μｍを超える程度まで大きく成長していた。
比較例となる試料Ｎｏ．１２、Ｎｏ．１３、Ｎｏ．１５、Ｎｏ．２２～Ｎｏ．２４は、いずれも、導電率が９６％ＩＡＣＳ以下であった。また、比較例となる試料Ｎｏ．１４、Ｎｏ．１６～Ｎｏ．２４は、いずれも、９００℃で１時間加熱後の平均結晶粒径が３００μｍを超えていた。
The electrical conductivity of each Cu alloy plate was measured. In addition, each Cu alloy plate was heated at 900° C. for 1 hour, the crystal structure of the rolled surface was observed, and the average crystal grain size was measured. The results are shown in Table 1.
Sample No., which is a conventional example. The Cu plate made of pure Cu of No. 11 had grown so large that the average crystal diameter after heating at 900° C. for 1 hour exceeded 700 μm.
Sample No., which is a comparative example. 12, No. 13, No. 15, No. 22~No. No. 24 had a conductivity of 96% IACS or less. In addition, sample No. 1, which serves as a comparative example. 14, No. 16~No. No. 24 had an average crystal grain size of more than 300 μm after heating at 900° C. for 1 hour.
これに対して、本発明例となるＣｕ合金板は、セラミック基板とＣｕ合金板とを接合する際の熱処理を想定した９００℃で１時間の加熱接合を経ても、平均結晶粒径が３００μｍ以下であった。このため、本発明のＣｕ合金板は、圧延面の結晶粒の粗大化が抑えられ、外観検査の画像処理において、結晶粒界が欠陥であると誤認される不具合が抑制できる。
また、本発明のＣｕ合金板は、従来の純Ｃｕ板に相当する優れた導電性を維持できることも確認できた。
On the other hand, the Cu alloy plate according to the present invention has an average crystal grain size of 300 μm or less even after being heated at 900°C for 1 hour, which is assumed to be a heat treatment when bonding a ceramic substrate and a Cu alloy plate. Met. Therefore, in the Cu alloy plate of the present invention, coarsening of the crystal grains on the rolled surface is suppressed, and in image processing for visual inspection, it is possible to suppress the problem of grain boundaries being mistakenly recognized as defects.
It was also confirmed that the Cu alloy plate of the present invention can maintain excellent electrical conductivity equivalent to that of a conventional pure Cu plate.
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