JP7294336B2 - Fe-Ni alloy sheet - Google Patents
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- 229910001030 Iron–nickel alloy Inorganic materials 0.000 title claims description 31
- 229910045601 alloy Inorganic materials 0.000 title claims description 31
- 239000000956 alloy Substances 0.000 title claims description 31
- 239000012535 impurity Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 description 31
- 238000005096 rolling process Methods 0.000 description 28
- 238000005097 cold rolling Methods 0.000 description 27
- 238000000137 annealing Methods 0.000 description 26
- 230000009467 reduction Effects 0.000 description 26
- 238000001953 recrystallisation Methods 0.000 description 12
- 230000017525 heat dissipation Effects 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 229910000990 Ni alloy Inorganic materials 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 229910000734 martensite Inorganic materials 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000006872 improvement Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000002648 laminated material Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Heat Treatment Of Sheet Steel (AREA)
- Conductive Materials (AREA)
Description
本発明は、Ｆｅ－Ｎｉ系合金薄板に関するものである。 The present invention relates to Fe--Ni alloy sheets.
リードフレームやメタルマスク等に使用されるＦｅ－Ｎｉ系合金薄板は、性能向上のために従来より様々な検討がなされている。例えば特許文献１には、エッチング精度を向上させるために、熱延板に冷間圧延および焼鈍をそれぞれ１回以上行い、最終再結晶焼鈍の前の冷間圧延の冷圧率を９０％以上、最終再結晶焼鈍の焼鈍温度を８５０℃以上、最終冷圧率を３０％以下として製造することを特徴とする、Ｎｉを３０～３４％含有するＦｅ－Ｎｉ系薄板の製造方法が開示されている。また特許文献２には、良好なエッチング性と高い強度を得るために、８５％以上の冷間圧延率と７００℃以上の焼鈍を少なくとも一回行い、その後前記冷間圧延率を超えない圧延率の冷間圧延と８５０℃を超えない温度の焼鈍をこの順に行うことを特徴とする、Ｎｉを３０～４０％含有するシャドウマスク材料の製造方法が開示されている。 2. Description of the Related Art Various studies have been made to improve the performance of Fe--Ni alloy sheets used for lead frames, metal masks, and the like. For example, in Patent Document 1, in order to improve the etching accuracy, the hot rolled sheet is cold rolled and annealed once or more, and the cold rolling rate before the final recrystallization annealing is 90% or more. Disclosed is a method for producing an Fe—Ni-based thin sheet containing 30 to 34% Ni, characterized in that the final recrystallization annealing is performed at an annealing temperature of 850° C. or higher and a final cold reduction rate of 30% or lower. . Further, in Patent Document 2, in order to obtain good etchability and high strength, a cold rolling reduction of 85% or more and annealing at 700 ° C. or more are performed at least once, and then a rolling reduction that does not exceed the cold rolling reduction. and annealing at a temperature not exceeding 850° C. in this order.
上記のようなＮｉを３０～４０％含有するＦｅ－Ｎｉ系合金薄板は、その優れた低熱膨張特性から、電子部品を搭載する基板に組み込まれる場合がある。しかし近年の電子部品の点数増加や低背化、小型化に伴い、Ｆｅ－Ｎｉ系合金薄板にもさらなる薄型化、高強度化、放熱特性の向上が要求されている。一般的に板厚は薄くなればなるほど、断面積が減ることにより、熱放出効率が低下して放熱性は悪くなる傾向にある。その為放熱性を向上させる技術として、熱伝導性が良好な材料とＦｅ－Ｎｉ系合金薄板とを接合した積層材も考えられるが、接合工程を含むため生産性やコストの点で好ましくない。特許文献１や特許文献２には、上述したような放熱特性の向上については記載されておらず、検討の余地が残されている。
そこで本発明の目的は、厚さが０．５ｍｍ以下の薄いＦｅ－Ｎｉ系合金薄板において、従来のものと比較して高強度で放熱性が良好なＦｅ－Ｎｉ系合金薄板を提供することである。The Fe—Ni alloy thin plate containing 30 to 40% of Ni as described above is sometimes incorporated into a substrate on which electronic parts are mounted because of its excellent low thermal expansion characteristics. However, with the recent increase in the number of electronic parts and the reduction in height and size of the electronic parts, further reduction in thickness, increase in strength, and improvement in heat dissipation properties are required for Fe--Ni alloy thin plates. In general, the thinner the plate, the less the cross-sectional area, and the lower the heat dissipation efficiency, and the worse the heat dissipation tends to be. Therefore, as a technique for improving heat dissipation, a laminated material in which a material with good thermal conductivity is joined to an Fe—Ni alloy thin plate can be considered. Patent Document 1 and Patent Document 2 do not describe the above-described improvement in heat dissipation characteristics, and there is room for further study.
Accordingly, an object of the present invention is to provide a thin Fe—Ni alloy sheet having a thickness of 0.5 mm or less, which has higher strength and better heat dissipation than conventional ones. be.
本発明の一態様は、質量％で、Ｎｉ＋Ｃｏ：１．０％以上３０．０％未満（但し、Ｃｏは０～６．０％）、Ｓｉ：０．５％以下、Ｍｎ：１．０％以下、残部はＦｅ及び不純物からなり、厚さが０．５ｍｍ以下のＦｅ－Ｎｉ系合金薄板であって、前記Ｆｅ－Ｎｉ系合金薄板の組織は、α相が１０％以上であるα相とγ相との複相組織またはα単相組織を有しており、前記Ｆｅ－Ｎｉ系合金薄板の電気抵抗率が６５×１０－８Ω・ｍ以下である、Ｆｅ－Ｎｉ系合金薄板である。
好ましくは、上記の組織が、α単相組織である。また、好ましくは、上記の薄板の０．２％耐力が７５０ＭＰａ以上、かつヤング率が１４５ＧＰａ以上である。One aspect of the present invention is, in mass %, Ni + Co: 1.0% or more and less than 30.0% (where Co is 0 to 6.0%), Si: 0.5% or less, Mn: 1.0% Hereinafter, an Fe—Ni alloy sheet having a thickness of 0.5 mm or less, the balance being composed of Fe and impurities, the structure of the Fe—Ni alloy sheet having an α phase content of 10% or more. An Fe—Ni alloy sheet having a dual phase structure with a γ phase or an α single phase structure, and having an electrical resistivity of 65×10 −8 Ω·m or less. .
Preferably, the above structure is an α-single-phase structure. Further, preferably, the thin plate has a 0.2% proof stress of 750 MPa or more and a Young's modulus of 145 GPa or more.
本発明によれば、厚さが０．５ｍｍ以下の薄いＦｅ－Ｎｉ系合金薄板において、従来のものと比較して高強度で放熱性が良好なＦｅ－Ｎｉ系合金薄板を提供することができる。 According to the present invention, it is possible to provide a thin Fe—Ni alloy sheet having a thickness of 0.5 mm or less, which has higher strength and better heat dissipation than conventional ones. .
以下に本発明の実施形態について説明する。なお、本明細書中において、「～」を用いて表される数値範囲は、「～」の前後に記載される数値を下限値及び上限値として含む範囲を意味する。また、本明細書において、「工程」との語は、独立した工程だけでなく、他の工程と明確に区別できない場合であっても工程の所期の目的が達成されれば、本用語に含まれる。
まず、本発明のＦｅ－Ｎｉ系合金薄板に関する実施形態について説明する。Embodiments of the present invention are described below. In this specification, a numerical range represented by "-" means a range including the numerical values before and after "-" as lower and upper limits. In addition, in this specification, the term "step" refers not only to an independent step, but also to the term if the intended purpose of the step is achieved even if it cannot be clearly distinguished from other steps. included.
First, an embodiment of the Fe—Ni alloy thin plate of the present invention will be described.
本発明では、質量％で、Ｎｉ＋Ｃｏ：１．０％以上３０．０％未満（但し、Ｃｏは０～６．０％）、Ｓｉ：０．５％以下、Ｍｎ：１．０％以下、残部はＦｅ及び不純物からなる組成を有する。本発明で規定する組成を有するＦｅ－Ｎｉ系合金は、所望の放熱性を発揮するために必要な組成を有するものである。
[Ｎｉ＋Ｃｏ：１．０％以上３０．０％未満（但し、Ｃｏは０～６．０％）]
本実施形態におけるＮｉ含有量は１．０％以上３０．０％未満とする。Ｎｉを上記の範囲に設定することで、本実施形態の薄板は後述するα相とγ相との複合組織を有することができ、γ相単相の薄板よりも高強度にすることが可能である。さらには電気抵抗が下がる事から、放熱性の向上も期待できる。Ｎｉ含有量が１．０％未満では純鉄に近い組成になるため錆が発生し易くなり、靭性も低下する傾向にあるため、好ましくない。好ましいＮｉの下限は３．０％であり、より好ましいＮｉの下限は５．０％、さらに好ましいＮｉの下限は７．０％であり、よりさらに好ましいＮｉの下限は８．０％であり、特に好ましいＮｉの下限は８．５％であり、最も好ましいＮｉの下限は９．０％である。上記のＮｉ含有量の下限において、本実施形態のＦｅ－Ｎｉ系合金薄板の組織は、通常、α単相組織である。そして、このＮｉ含有量の下限からＮｉ含有量を増やしていって、Ｎｉ含有量が２０％に達した辺りで、Ｆｅ－Ｎｉ系合金薄板の組織はα単相組織からα相とγ相との複相組織へと移行する。
そして、更にＮｉ含有量を増やしていくと、Ｎｉ含有量が３０．０％の辺りに達したときに、上記のα相とγ相との複相組織は、一転してγ相単相に移行する。薄板の組織がγ相単相であると、強度や放熱性の低下を招く傾向にある。よって、Ｎｉ含有量は３０．０％未満とする。好ましいＮｉの上限は、２７．０％である。０．２％耐力とヤング率をより高い水準で得るためには、Ｎｉ量を２５％以下に調整することがさらに好ましい。また本実施形態では、熱膨張特性の調整や高強度を持たせるために、Ｎｉの一部をＣｏで置換することができる。上述した効果を材料に付与させやすくするために、Ｃｏの上限は６．０％に設定することが好ましい。そして、Ｃｏの上限は６．０％に設定して、かつＮｉ量より低い含有量に設定することがより好ましい。In the present invention, in mass%, Ni + Co: 1.0% or more and less than 30.0% (where Co is 0 to 6.0%), Si: 0.5% or less, Mn: 1.0% or less, the balance has a composition consisting of Fe and impurities. The Fe--Ni alloy having the composition specified in the present invention has the composition necessary for exhibiting the desired heat dissipation properties.
[Ni + Co: 1.0% or more and less than 30.0% (however, Co is 0 to 6.0%)]
The Ni content in this embodiment is 1.0% or more and less than 30.0%. By setting Ni in the above range, the thin plate of the present embodiment can have a composite structure of the α phase and the γ phase, which will be described later, and can have a higher strength than a single γ phase thin plate. be. Furthermore, since the electrical resistance is lowered, an improvement in heat dissipation can be expected. If the Ni content is less than 1.0%, the composition will be close to that of pure iron, so rusting is likely to occur and the toughness tends to decrease, which is not preferable. A preferable lower limit of Ni is 3.0%, a more preferable lower limit of Ni is 5.0%, a further preferable lower limit of Ni is 7.0%, and a still more preferable lower limit of Ni is 8.0%, A particularly preferred lower limit of Ni is 8.5%, and the most preferred lower limit of Ni is 9.0%. At the lower limit of the Ni content described above, the structure of the Fe—Ni alloy sheet of the present embodiment is usually an α single-phase structure. Then, the Ni content is increased from the lower limit of the Ni content, and when the Ni content reaches 20%, the structure of the Fe—Ni alloy sheet changes from an α single phase structure to α phase and γ phase. transition to a dual-phase structure.
As the Ni content is further increased, when the Ni content reaches around 30.0%, the multi-phase structure of the α phase and the γ phase turns into a single γ phase. Transition. If the structure of the thin plate is a γ-phase single phase, it tends to cause a decrease in strength and heat dissipation. Therefore, the Ni content should be less than 30.0%. A preferable upper limit of Ni is 27.0%. In order to obtain a higher level of 0.2% yield strength and Young's modulus, it is more preferable to adjust the Ni content to 25% or less. In addition, in this embodiment, Ni can be partially replaced with Co in order to adjust the thermal expansion characteristics and provide high strength. It is preferable to set the upper limit of Co to 6.0% in order to easily impart the above effects to the material. Further, it is more preferable to set the upper limit of Co to 6.0% and to set the content lower than the Ni content.
[Ｓｉ：０．５％以下、Ｍｎ：１．０％以下]
Ｓｉ、Ｍｎは通常Ｆｅ－Ｎｉ系合金では、脱酸を目的に微量含有されているが、過剰に含有すれば偏析を起こし易くなるため、Ｓｉは０．５％以下とし、Ｍｎは１．０％以下とする。なお、ＳｉとＭｎの下限は特に限定しないが、例えばＳｉは０．０５％、Ｍｎは０．０５％と設定することができる。
[残部はＦｅ及び不可避的不純物]
上記の元素以外は実質的にＦｅおよび不可避的不純物とすることができるが、本発明の効果を阻害しない範囲で本明細書にて説明した元素以外の元素が含まれていてもよい。例えば不純物として含有される元素であって、特に制限の必要な元素としてＣがあり、例えば、エッチングを行う用途に使用する場合は、エッチング性の阻害を抑制しないようにＣの上限を０．０５％と制限すると良い。また、Ｓを０．０２０％以下、Ｂを０．００５０％以下含有させても良い。ＳとＢはいずれか一方でも良いし、両方を含有させても良い。Ｓは快削性元素として、プレス打抜き性を向上させる効果を備え、Ｂは熱間加工性を向上させる効果を備える。[Si: 0.5% or less, Mn: 1.0% or less]
Si and Mn are usually contained in small amounts in Fe—Ni alloys for the purpose of deoxidation, but if they are contained excessively, segregation is likely to occur. % or less. Although the lower limits of Si and Mn are not particularly limited, for example, Si can be set to 0.05% and Mn to 0.05%.
[Remainder is Fe and unavoidable impurities]
Elements other than the above elements can be substantially Fe and unavoidable impurities, but elements other than the elements described in this specification may be contained within a range that does not impair the effects of the present invention. For example, C is an element that is contained as an impurity and particularly needs to be restricted. For example, when used for etching, the upper limit of C is set to 0.05 so as not to suppress etching inhibition. It is better to limit it to %. Also, S may be contained in an amount of 0.020% or less and B may be contained in an amount of 0.0050% or less. Either one of S and B may be contained, or both may be contained. As a free-cutting element, S has the effect of improving press punchability, and B has the effect of improving hot workability.
本実施形態のＦｅ－Ｎｉ系合金薄板は、α相とγ相との複合組織またはα相単相組織を有し、体積率でα相が１０％以上形成されている。これにより、γ相単相のものと比較してより高強度な薄板とすることができる。α相の上限は、特に限定せず、用途に合わせて適宜α相の量を調整することができる。またこのα相は、マルテンサイト単相組織、フェライト単相組織、フェライト‐マルテンサイト複相組織も含まれる。マルテンサイト単相組織の場合は、加工性が良好な立方晶マルテンサイト相が含まれていることが好ましい。そして、Ｆｅ－Ｎｉ系合金薄板の組織がα相単相組織であることがより好ましい。なお本実施形態におけるα相の体積率は、例えばＸ線回折を用いて、α相とγ相との強度分布を求め、それぞれのピーク強度面積から求める事が可能である。 The Fe—Ni alloy sheet of this embodiment has a composite structure of α phase and γ phase or a single α phase structure, and the α phase is formed at a volume ratio of 10% or more. As a result, it is possible to obtain a thin plate having a higher strength than that of a γ-phase single-phase plate. The upper limit of the α phase is not particularly limited, and the amount of the α phase can be appropriately adjusted according to the application. The α-phase also includes a martensite single-phase structure, a ferrite single-phase structure, and a ferrite-martensite dual-phase structure. In the case of a martensite single-phase structure, it is preferable that a cubic martensite phase with good workability is included. Further, it is more preferable that the structure of the Fe—Ni alloy sheet is an α-phase single-phase structure. The volume fraction of the α-phase in the present embodiment can be determined from the peak intensity areas of the respective peak intensity distributions of the α-phase and the γ-phase, for example, using X-ray diffraction.
本実施形態のＦｅ－Ｎｉ系合金薄板は、電気抵抗率が６５×１０－８Ω・ｍ以下である。これにより、リードフレームや電子部品の基板に適用しても、熱が発生し難く、優れた放熱性を発揮することができる。好ましい電気抵抗率は６０×１０－８Ω・ｍ以下、より好ましい電気抵抗率は５５×１０－８Ω・ｍ以下、さらに好ましい電気抵抗率は５０×１０－８Ω・ｍ以下、特に好ましい電気抵抗率は４５×１０－８Ω・ｍ以下である。この本実施形態の電気抵抗率は、組成の調整と後述するような製造方法を適用することで、調整することができる。また本実施形態のＦｅ－Ｎｉ系合金薄板は、硬さが２５０ＨＶ以上であることが好ましい。より好ましくは２７０ＨＶ以上、さらに好ましくは３００ＨＶ以上である。上限は特に限定しないが、あまり硬すぎると製造が困難であるため、例えば６００ＨＶと設定することができる。The Fe—Ni alloy thin plate of this embodiment has an electric resistivity of 65×10 −8 Ω·m or less. As a result, even when applied to a lead frame or a substrate of an electronic component, heat is less likely to be generated, and excellent heat dissipation can be exhibited. Preferable electrical resistivity is 60×10 −8 Ω·m or less, more preferably 55×10 −8 Ω·m or less, still more preferably 50×10 −8 Ω·m or less, particularly preferably electrical resistivity The resistivity is 45×10 −8 Ω·m or less. The electrical resistivity of this embodiment can be adjusted by adjusting the composition and applying a manufacturing method as described later. Further, the Fe—Ni alloy thin plate of the present embodiment preferably has a hardness of 250 HV or more. It is more preferably 270 HV or higher, still more preferably 300 HV or higher. The upper limit is not particularly limited, but if it is too hard, it is difficult to manufacture, so it can be set to 600 HV, for example.
本実施形態のＦｅ－Ｎｉ系合金薄板は、０．２％耐力が７５０ＭＰａ以上であることが好ましい。この特性を有することにより、薄板の曲げ伸ばし時に折れ曲がりが発生しにくく、高強度なＦｅ－Ｎｉ系合金薄板を得ることができる。より好ましくは７６０ＭＰａ以上、さらに好ましくは７８０ＭＰａ以上である。また上記の０．２％耐力を達成するために、引張強度７８０ＭＰａ以上であることが好ましい。より好ましくは８００ＭＰａ以上である。
また本実施形態のＦｅ－Ｎｉ系合金薄板は、ヤング率が１４５ＧＰａ以上であることが好ましい。これにより曲がりにくく高剛性な薄板を得ることが可能であり、例えば電子回路の基板に使用した場合、基板上の回路が変形しにくいといった優れた効果を発揮することがが可能である。より好ましいヤング率は１５０ＧＰａ以上であり、さらに好ましいヤング率は１６０ＧＰａ以上であり、特に好ましくは１７０ＧＰａ以上である。The Fe—Ni alloy sheet of the present embodiment preferably has a 0.2% yield strength of 750 MPa or more. Owing to this characteristic, the thin sheet is less likely to bend during bending and stretching, and a high-strength Fe—Ni alloy thin sheet can be obtained. It is more preferably 760 MPa or higher, and still more preferably 780 MPa or higher. In order to achieve the above 0.2% yield strength, the tensile strength is preferably 780 MPa or more. More preferably, it is 800 MPa or more.
Further, the Fe—Ni alloy thin plate of the present embodiment preferably has a Young's modulus of 145 GPa or more. This makes it possible to obtain a thin plate that is hard to bend and has high rigidity. For example, when it is used as a substrate for an electronic circuit, it is possible to exhibit an excellent effect that the circuit on the substrate is difficult to deform. Young's modulus is more preferably 150 GPa or more, more preferably 160 GPa or more, and particularly preferably 170 GPa or more.
本実施形態の薄板の厚さは、様々な用途に対応するために０．５ｍｍ以下とする。これにより、本実施形態のＦｅ－Ｎｉ系合金薄板は、例えば、リードフレームに用いた場合では多ピン化に対応しやすく、例えばメタルマスクに用いた場合は、エッチング加工による高精細化に対応が可能である。また電子部品の基板に適用すれば小型化・低背化要求にも対応できるなど、多様な要求に応える事が可能である。好ましい厚さの上限は０．２ｍｍである。より好ましい上限は０．１５ｍｍ、さらに好ましい上限は０．１ｍｍ、特に好ましい上限は０．０８ｍｍである。なお下限は特に限定しないが、材料が薄すぎると形状変化が生じやすくなる傾向にあるため、０．０２ｍｍと設定することができる。本発明のＦｅ－Ｎｉ系合金薄板は、広幅（例えば、板幅が５００～１２００ｍｍ）であることが特に好ましい。なお本実施形態での薄板とは、コイル状に巻き回されている鋼帯や、その鋼帯を切断して作製された矩形状の薄板も含む。矩形状薄板の場合、「板幅」とは短辺のことを示す。 The thickness of the thin plate of this embodiment is set to 0.5 mm or less in order to accommodate various uses. As a result, the Fe—Ni alloy thin plate of the present embodiment can be easily adapted to a multi-pin configuration when used for lead frames, for example, and can be adapted to high definition by etching when used for metal masks, for example. It is possible. In addition, it is possible to respond to a variety of demands, such as the need for miniaturization and low profile when applied to substrates for electronic components. A preferred upper thickness limit is 0.2 mm. A more preferable upper limit is 0.15 mm, a still more preferable upper limit is 0.1 mm, and a particularly preferable upper limit is 0.08 mm. Although the lower limit is not particularly limited, it can be set to 0.02 mm, because if the material is too thin, the shape tends to change easily. It is particularly preferable that the Fe—Ni alloy sheet of the present invention has a wide width (for example, a width of 500 to 1200 mm). Note that the thin plate in this embodiment includes a steel strip wound in a coil shape and a rectangular thin plate produced by cutting the steel strip. In the case of a rectangular thin plate, the "plate width" indicates the short side.
続いて、本実施形態のＦｅ－Ｎｉ系合金薄板を得ることができる製造方法の一例について説明する。
＜熱間圧延材の厚さ：２ｍｍ以上＞
本実施形態で用いる熱間圧延材は、その厚さを２ｍｍ以上とする。熱間圧延材の厚さが２ｍｍ未満となると、本実施形態で規定する圧下率５０％以上の冷間圧延が行えないおそれがある。また、熱間圧延材の厚さを２ｍｍ未満にしようとすると、特殊な圧延設備が必要になる場合がある。そのため、本実施形態では熱間圧延材の厚さを２ｍｍ以上とする。
なお、熱間圧延材の厚さを厚くすると圧下率を高くすることが可能であるが、一方で、冷間圧延工程中のパス回数が増えたり、圧延中のＦｅ－Ｎｉ系合金の形状の調整が困難になる場合があるため、厚さの上限を５ｍｍとするのが現実的である。
この熱間圧延材は、表面に酸化層が形成されており、熱間圧延材の厚さとは、その酸化層を含めた厚さである。Next, an example of a manufacturing method for obtaining the Fe—Ni alloy thin plate of the present embodiment will be described.
<Thickness of hot-rolled material: 2 mm or more>
The hot-rolled material used in this embodiment has a thickness of 2 mm or more. If the thickness of the hot-rolled material is less than 2 mm, it may not be possible to perform cold-rolling with a rolling reduction of 50% or more specified in this embodiment. Moreover, when trying to reduce the thickness of the hot-rolled material to less than 2 mm, special rolling equipment may be required. Therefore, in this embodiment, the thickness of the hot-rolled material is set to 2 mm or more.
It is possible to increase the reduction rate by increasing the thickness of the hot-rolled material. Since adjustment may become difficult, it is realistic to set the upper limit of the thickness to 5 mm.
This hot-rolled material has an oxide layer formed on its surface, and the thickness of the hot-rolled material is the thickness including the oxide layer.
＜冷間圧延用素材＞
本実施形態では、前述の熱間圧延材を用いて冷間圧延用素材とする。熱間圧延材には酸化層が形成されていることから、その酸化層を、例えば、機械的、或いは化学的に除去することが好ましい。また、冷間圧延中の冷間圧延材のエッジから割れ等の不良が発生しないように、エッジをスリッターを用いて裁断してもよい。このような加工を行って冷間圧延用素材とすることができる。<Material for cold rolling>
In this embodiment, the above-described hot rolled material is used as a material for cold rolling. Since an oxide layer is formed in the hot-rolled material, it is preferable to remove the oxide layer, for example, mechanically or chemically. Also, the edges of the cold-rolled material may be cut using a slitter so that defects such as cracks do not occur from the edges of the cold-rolled material being cold-rolled. A material for cold rolling can be obtained by performing such processing.
次に、冷間圧延工程について、詳しく説明する。
＜冷間圧延工程＞
本実施形態では、冷間圧延用素材に対し、圧下率５０％以上の冷間圧延を行う。この冷間圧延は、複数パスの圧延工程としても良く、その場合の圧下率は、トータルの圧下率である。この冷間圧延は、再結晶焼鈍工程の前に行われる。このように再結晶焼鈍前の圧下率を高くすることにより、電気抵抗率をより低く調整することができる傾向にある。また、冷間圧延や焼鈍工程の回数を減らすことができるため、より低コストでの製造も可能となる。圧下率が５０％未満であると、機械特性が劣化する。また圧下率が低すぎると、所望の板厚に調整するまでの冷間圧延や焼鈍工程の回数が増え、コストが増大する。好ましい圧下率は６０％以上である。より好ましい圧下率は７０％以上であり、さらに好ましい圧下率は８０％以上であり、特に好ましい圧下率は８５％以上である。なお、圧下率の上限は特に定めないが、圧下率が９９％を超えると、過大な圧延時間によるコストの増大を招く可能性があるため、上限は９９％とするのが現実的である。Next, the cold rolling process will be described in detail.
<Cold rolling process>
In this embodiment, the cold rolling material is cold rolled at a rolling reduction of 50% or more. This cold rolling may be a multiple-pass rolling process, and the rolling reduction in that case is the total rolling reduction. This cold rolling is performed before the recrystallization annealing step. By increasing the rolling reduction before recrystallization annealing in this way, there is a tendency that the electrical resistivity can be adjusted to be lower. In addition, since the number of cold rolling and annealing steps can be reduced, it is possible to manufacture at a lower cost. If the rolling reduction is less than 50%, the mechanical properties deteriorate. On the other hand, if the rolling reduction is too low, the number of cold rolling and annealing processes required to adjust the sheet thickness to the desired thickness will increase, resulting in an increase in cost. A preferable rolling reduction is 60% or more. A more preferred rolling reduction is 70% or more, a further preferred rolling reduction is 80% or more, and a particularly preferred rolling reduction is 85% or more. Although the upper limit of the rolling reduction is not particularly defined, if the rolling reduction exceeds 99%, the cost may increase due to excessive rolling time, so it is realistic to set the upper limit to 99%.
＜再結晶焼鈍工程＞
本実施形態では前述した冷間圧延された圧延材に対し、８００℃以上の温度で再結晶焼鈍を行う。この工程により、強圧下により加工硬化した圧延材（薄板）の歪みを除去し軟化させ、後の最終冷間圧延により所望の板厚と特性を付与させることができる。焼鈍温度が８００℃未満であると材料が十分に軟化しないおそれがある。また焼鈍温度の上限は特に限定しないが、高すぎると所望の特性が得られない可能性があるため、１１００℃と設定することができる。
また本実施形態の再結晶焼鈍で使用する焼鈍炉は、設定温度が一定である均熱帯と、均熱帯の後に形成され、均熱帯の設定温度よりも低い温度に設定される冷却帯を有する。この冷却帯を設けることで、加工性が良好なα相をより容易に形成させることが可能である。この冷却帯は、焼鈍炉全長の１０％程度形成されていればよい。好ましくは２０％程度形成されていることが良く、より好ましくは３０％程度、さらに好ましくは４０％程度形成されていることが良い。この冷却帯の設定温度は、均熱帯の設定温度Ｔ（℃）に対して０．０５Ｔ（℃）以上０．９Ｔ（℃）未満であることが好ましく、要求特性に合わせて、上記温度範囲内で連続的または段階的に温度を下げることができる。<Recrystallization annealing process>
In this embodiment, the cold-rolled material described above is subjected to recrystallization annealing at a temperature of 800° C. or higher. This step removes the distortion of the rolled material (thin plate) that has been work-hardened under high pressure, softens it, and allows the desired plate thickness and properties to be imparted by subsequent final cold rolling. If the annealing temperature is less than 800°C, the material may not soften sufficiently. The upper limit of the annealing temperature is not particularly limited, but if it is too high, the desired properties may not be obtained, so it can be set at 1100°C.
The annealing furnace used in the recrystallization annealing of the present embodiment has a soaking zone with a constant set temperature and a cooling zone formed after the soaking zone and set at a temperature lower than the set temperature of the soaking zone. By providing this cooling zone, it is possible to more easily form the α phase with good workability. This cooling zone should be formed in about 10% of the total length of the annealing furnace. It is preferably formed about 20%, more preferably about 30%, still more preferably about 40%. The set temperature of this cooling zone is preferably 0.05 T (° C.) or more and less than 0.9 T (° C.) with respect to the set temperature T (° C.) of the soaking zone. , the temperature can be lowered continuously or in steps.
さらに本実施形態は、薄板が焼鈍炉に入っている時間（保持時間）を０．１分以上に調整する。好ましくは、焼鈍炉内での保持時間を比較的短時間にすることで、生産効率を落とさず、α相主体の組織に調整するために、保持時間を０．１～３．０分に調整する。保持時間が０．１分未満だと歪みが十分除去されない場合がある。３．０分を超えると、合金薄板の特性の変動や、焼鈍時間の増大によりコストが増大する可能性がある。保持時間の下限は０．２分であることがより好ましい。また保持時間の上限は、さらなる低コスト化を狙って、２．０分であることがより好ましく、１．５分であることがさらに好ましく、１．０分であることが特に好ましく、０．６分であることが最も好ましい。尚、この再結晶焼鈍は、所望の温度に設定された焼鈍炉に冷間圧延された圧延材（薄板）を連続的に通して行うことができる。例えば、冷間圧延された圧延材がロール状に巻かれた状態から引き出し、焼鈍炉を通り、ロール状に巻き取る方法で行うことができる。また、この再結晶焼鈍工程は少なくとも一回行えばよく、複数回行っても良い。 Furthermore, in this embodiment, the time (holding time) during which the thin plate is in the annealing furnace is adjusted to 0.1 minute or longer. Preferably, the holding time in the annealing furnace is set to a relatively short time to adjust the holding time to 0.1 to 3.0 minutes in order to adjust the structure to the α-phase-based structure without reducing the production efficiency. do. If the holding time is less than 0.1 minute, the distortion may not be sufficiently removed. If it exceeds 3.0 minutes, there is a possibility that the cost will increase due to variations in the properties of the alloy sheet and an increase in the annealing time. More preferably, the lower limit of the retention time is 0.2 minutes. Further, the upper limit of the holding time is more preferably 2.0 minutes, still more preferably 1.5 minutes, particularly preferably 1.0 minutes, and 0.5 minutes for further cost reduction. Most preferably 6 minutes. The recrystallization annealing can be performed by continuously passing the cold-rolled material (thin sheet) through an annealing furnace set at a desired temperature. For example, it can be carried out by a method in which a cold-rolled material is pulled out from a rolled state, passed through an annealing furnace, and wound into a roll. Moreover, this recrystallization annealing step may be performed at least once, and may be performed multiple times.
本実施形態の製造方法では、前述した再結晶焼鈍された焼鈍材に、要求特性に合わせて圧下率を調整した最終冷間圧延を施すことができる。例えば、良好な生産性を確保する場合は、圧下率を５０％未満（好ましくは４５％以下、より好ましくは４０％以下）に調整することができる。また、より硬質な薄板としたい場合は、圧下率を５０％以上（好ましくは６０％以上、より好ましくは７０％以上）とすることができる。また、最終冷間圧延での圧延前方張力を２００～５００ＭＰａ、圧延後方張力を１００～２００ＭＰａ、圧延速度を２５０ｍ／分以下とすることが好ましい。より好ましい圧延前方張力の下限は２５０ＭＰａであり、より好ましい圧延前方張力の上限は４００ＭＰａである。またより好ましい圧延後方張力の下限は１２０ＭＰａであり、より好ましい圧延後方張力の上限は１８０ＭＰａである。なお圧延速度の下限については特に限定しないが、作業性を考慮すると１００ｍ／分程度とすることが好ましい。また本実施形態の製造方法において、最終冷間圧延は、薄板表面の疵を抑制しつつ所望の特性を得るために、１パスで圧延することが好ましい。 In the production method of the present embodiment, the annealed material that has been recrystallized and annealed as described above can be subjected to final cold rolling in which the rolling reduction is adjusted according to the required properties. For example, when ensuring good productivity, the rolling reduction can be adjusted to less than 50% (preferably 45% or less, more preferably 40% or less). Further, when a harder thin plate is desired, the rolling reduction can be 50% or more (preferably 60% or more, more preferably 70% or more). In the final cold rolling, the pre-rolling tension is preferably 200 to 500 MPa, the post-rolling tension is preferably 100 to 200 MPa, and the rolling speed is preferably 250 m/min or less. A more preferable lower limit of the forward rolling tension is 250 MPa, and a more preferable upper limit of the forward rolling tension is 400 MPa. A more preferable lower limit of the post-rolling tension is 120 MPa, and a more preferable upper limit of the post-rolling tension is 180 MPa. Although the lower limit of the rolling speed is not particularly limited, it is preferably about 100 m/min in consideration of workability. In the manufacturing method of the present embodiment, the final cold rolling is preferably performed in one pass in order to obtain desired properties while suppressing defects on the surface of the thin plate.
本実施形態では、上述した最終冷間圧延後には、熱処理を行わないことが好ましい。この熱処理とは、例えば、再結晶温度以下で行う歪取り焼鈍である。熱処理を省略することによって、残留歪みの開放による薄板形状の変化や機械特性の変動を抑制することができる。本実施形態では上述した製法により歪みを除去しなくても機械特性では異方性のない製品となる為、省略可能である。なお、熱処理の省略は、省エネ効果を高め、経済的である。 In this embodiment, heat treatment is preferably not performed after the final cold rolling described above. This heat treatment is, for example, strain relief annealing performed at a recrystallization temperature or lower. By omitting the heat treatment, it is possible to suppress changes in the shape of the thin plate and fluctuations in the mechanical properties due to the release of the residual strain. In the present embodiment, even if the strain is not removed by the manufacturing method described above, the product can be obtained without anisotropy in terms of mechanical properties, so it can be omitted. Omitting the heat treatment is economical because it enhances the energy-saving effect.
真空溶解、均熱化熱処理、熱間加工を行って熱間圧延材（厚さ約３．０ｍｍ）を準備した。準備した本発明例と比較例との熱間圧延材の化学組成を表１に示す。
前述の熱間圧延材に化学研磨、機械研磨を行い熱間圧延材表面の酸化層を除去して冷間圧延用素材を準備した。前述の冷間圧延用素材に、中間冷間圧延、再結晶焼鈍、最終冷間圧延を施し、本発明例と比較例のＦｅ－Ｎｉ系薄板を作成した。中間冷間圧延は圧下率９０％で行い、再結晶焼鈍は温度９００℃、圧下率３５％の条件で最終冷間圧延を１パスで行い、厚さ０．２ｍｍとした。また、最終冷間圧延後は熱処理を行っていない。Vacuum melting, soaking heat treatment, and hot working were performed to prepare a hot-rolled material (about 3.0 mm thick). Table 1 shows the chemical compositions of the prepared hot-rolled materials of the present invention example and the comparative example.
The above hot rolled material was subjected to chemical polishing and mechanical polishing to remove the oxide layer on the surface of the hot rolled material to prepare a material for cold rolling. The cold rolling materials described above were subjected to intermediate cold rolling, recrystallization annealing, and final cold rolling to prepare Fe—Ni sheets of the present invention and comparative examples. Intermediate cold rolling was performed at a reduction rate of 90%, and recrystallization annealing was performed at a temperature of 900°C and a reduction rate of 35%, and final cold rolling was performed in one pass to obtain a thickness of 0.2 mm. No heat treatment was performed after the final cold rolling.
前述の最終冷間圧延を終えたＦｅ－Ｎｉ系合金薄板から、各種試験片を採取し、引張強度、０．２％耐力、ヤング率、電気抵抗率を測定した。試験の結果を表２に纏めて示す。引張強度、０．２％耐力及びヤング率は、ＪＩＳ－Ｚ２２４１に規定された方法に従って求めた。電気抵抗率は４端子抵抗測定が可能な抵抗測定器にて、測定電極間の距離を５０ｍｍに設定して測定を行った。その結果、試料Ｎｏ．１～４の本発明例では、引張強度、０．２％耐力、ヤング率、電気抵抗率ともに良好な値であることが確認できた。特にＮｉ量が１０．０％の場合はヤング率が最高値を示し、Ｎｉ量が２４．８％の場合には０．２％耐力が最高値を示した。これはＮｉ量を調整したことによりα相主体の組織に制御できたためと考えられる。反面、比較例である試料Ｎｏ．１１～１３は、引張強度、０．２％耐力、ヤング率共に本発明例に比べ低い値となることを確認した。また、本発明例（試料Ｎｏ．１～４）のα相の体積率は１０％以上であり、試料Ｎｏ．１、２、３の組織は、実質、α相単相であった。そして、試料Ｎｏ．１～４の電気抵抗率が６５×１０－８Ω・ｍ以下であった。一方、比較例（Ｎｏ．１１～１３）は、電気抵抗率が６５×１０－８Ω・ｍを越えていた。そして、γ相が主体となっており、実質、γ相単相であったことを確認した。例として、試料Ｎｏ．１のＸＲＤ測定結果を図１に、試料Ｎｏ．１３のＸＲＤ測定結果を図２に示す。装置は（株）リガク製ＲＩＮＴ２５００ＰＣを用い、Ｃｏ－Ｋα線を入射して得られたピークを測定した。図１および図２より、試料Ｎｏ．１は回折角度２θ＝約７７°、約１００°に明瞭なピークが確認できた。これはα‐Ｆｅ（２００）、（２１１）に一致するピークである。その他にγ‐Ｆｅの明瞭なピークが確認されないことから、試料Ｎｏ．１がα単相組織であることが確認できた。一方で試料Ｎｏ．１３は、回折角度２θ＝が約６０°、約９０°、約１１１°に明瞭なピークが確認できた。これはγ‐Ｆｅ（２００）、（２２０）、（３１１）に一致するピークである。その他にα‐Ｆｅの明瞭なピークが確認されないことから、試料Ｎｏ．１３がγ単相組織であることが確認できた。Various test pieces were taken from the Fe—Ni alloy sheets after the final cold rolling, and the tensile strength, 0.2% yield strength, Young's modulus, and electrical resistivity were measured. Table 2 summarizes the test results. Tensile strength, 0.2% yield strength and Young's modulus were determined according to the method specified in JIS-Z2241. The electrical resistivity was measured by using a resistance measuring instrument capable of four-terminal resistance measurement, setting the distance between measurement electrodes to 50 mm. As a result, sample no. In Examples 1 to 4 of the present invention, it was confirmed that the tensile strength, 0.2% yield strength, Young's modulus and electrical resistivity were all good values. In particular, when the Ni content was 10.0%, Young's modulus showed the highest value, and when the Ni content was 24.8%, the 0.2% yield strength showed the highest value. It is considered that this is because the adjustment of the Ni content enabled the structure to be mainly composed of the α phase. On the other hand, sample No. 1, which is a comparative example, It was confirmed that the tensile strength, 0.2% proof stress and Young's modulus of Nos. 11 to 13 were all lower than those of the invention examples. In addition, the volume fraction of the α phase of the examples of the present invention (Sample Nos. 1 to 4) was 10% or more. The structures of 1, 2, and 3 were substantially α-phase single phase. And sample no. The electrical resistivity of 1 to 4 was 65×10 −8 Ω·m or less. On the other hand, the comparative examples (Nos. 11 to 13) had electrical resistivities exceeding 65×10 −8 Ω·m. Then, it was confirmed that the γ phase was the main component, and that it was substantially a γ phase single phase. As an example, sample no. The XRD measurement result of sample No. 1 is shown in FIG. The XRD measurement results of 13 are shown in FIG. RINT2500PC manufactured by Rigaku Co., Ltd. was used as an apparatus, and the peak obtained by injecting Co-Kα rays was measured. 1 and 2, sample no. In No. 1, clear peaks were confirmed at diffraction angles 2θ of about 77° and about 100°. This is a peak consistent with α-Fe (200), (211). Since no other clear peaks of γ-Fe were confirmed, sample No. 1 was confirmed to be an α single-phase structure. On the other hand, sample no. In No. 13, clear peaks were confirmed at diffraction angles 2θ= of about 60°, about 90°, and about 111°. This is the peak corresponding to γ-Fe (200), (220), (311). Since no other clear α-Fe peak was observed, sample No. It was confirmed that No. 13 had a γ single-phase structure.
Claims (3)
前記Ｆｅ－Ｎｉ系合金薄板の組織は、α相が１０％以上であるα相とγ相との複相組織
、またはα単相組織を有しており、
前記Ｆｅ－Ｎｉ系合金薄板の電気抵抗率が６５×１０－８Ω・ｍ以下である、Ｆｅ－Ｎ
ｉ系合金薄板。 % by mass, Ni: 9.0% or more and 25.0% or less, Si: 0.5% or less, Mn: 1.0% or less, the balance being Fe and impurities, and having a thickness of 0.5 mm or less An Fe—Ni alloy sheet,
The structure of the Fe—Ni alloy sheet has a multi-phase structure of an α phase and a γ phase in which the α phase is 10% or more, or an α single phase structure,
Fe—N, wherein the Fe—Ni alloy thin plate has an electrical resistivity of 65×10 −8 Ω·m or less
i-based alloy sheet.
系合金薄板。 The Fe—Ni according to claim 1, wherein the structure of the Fe—Ni alloy sheet is an α single phase structure.
based alloy sheet.
または２に記載のＦｅ－Ｎｉ系合金薄板。
Claim 1, wherein the 0.2% yield strength is 750 MPa or more and the Young's modulus is 145 GPa or more.
2. The Fe—Ni alloy sheet according to 2 above.
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| JP2002004007A (en) | 2000-04-21 | 2002-01-09 | Nippon Yakin Kogyo Co Ltd | Fe-Ni ALLOY COLD ROLLED SHEET AND METHOD FOR REFINING Fe-Ni ALLOY |
| JP2003073779A (en) | 2001-08-27 | 2003-03-12 | Nippon Yakin Kogyo Co Ltd | Fe-Ni ALLOY SHEET FOR HIGH CLEANLINESS SHADOW MASK AND MANUFACTURING METHOD THEREFOR |
| JP2010214447A (en) | 2009-03-18 | 2010-09-30 | Hitachi Metals Ltd | Method for manufacturing material for etching, and material for etching |
| JP2017064763A (en) | 2015-09-30 | 2017-04-06 | 日立金属株式会社 | PRODUCTION METHOD OF Fe-Ni-BASED ALLOY THIN SHEET |
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| JP2002004007A (en) | 2000-04-21 | 2002-01-09 | Nippon Yakin Kogyo Co Ltd | Fe-Ni ALLOY COLD ROLLED SHEET AND METHOD FOR REFINING Fe-Ni ALLOY |
| JP2003073779A (en) | 2001-08-27 | 2003-03-12 | Nippon Yakin Kogyo Co Ltd | Fe-Ni ALLOY SHEET FOR HIGH CLEANLINESS SHADOW MASK AND MANUFACTURING METHOD THEREFOR |
| JP2010214447A (en) | 2009-03-18 | 2010-09-30 | Hitachi Metals Ltd | Method for manufacturing material for etching, and material for etching |
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