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JP6852965B2 - Electrical steel sheet and its manufacturing method - Google Patents
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JP6852965B2 - Electrical steel sheet and its manufacturing method - Google Patents

Electrical steel sheet and its manufacturing method Download PDF

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JP6852965B2
JP6852965B2 JP2015182866A JP2015182866A JP6852965B2 JP 6852965 B2 JP6852965 B2 JP 6852965B2 JP 2015182866 A JP2015182866 A JP 2015182866A JP 2015182866 A JP2015182866 A JP 2015182866A JP 6852965 B2 JP6852965 B2 JP 6852965B2
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脇坂 岳顕
岳顕 脇坂
俊介 谷口
俊介 谷口
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Description

本発明は、強度を向上させた電磁鋼板とその製造方法に関し、特に高強度の無方向性電磁鋼板とその製造方法に関する。 The present invention relates to an electromagnetic steel sheet having improved strength and a method for producing the same, and particularly to a high-strength non-oriented electrical steel sheet and a method for producing the same.

近年、ハイブリッド電気自動車(HEV)や電気自動車(EV)に使用される駆動モータの高速回転化が著しく、それらの駆動モータの鉄心などに用いられる無方向性電磁鋼板については、低鉄損などの電磁特性に加えて、高強度化の要求が高くなっている。鋼板の高強度化には、固溶強化、析出強化、結晶粒微細化強化、転位強化、変態強化等が適用されるが、固溶強化以外は磁気特性を劣化させるため、電磁鋼板には好ましくない。また、固溶強化は磁気特性劣化を回避した高強度化には大きな効果があるが、同時に圧延荷重増大や脆性破断の課題もあり、生産性の観点から添加量に上限がある。 In recent years, drive motors used in hybrid electric vehicles (HEVs) and electric vehicles (EVs) have been remarkably rotated at high speeds, and non-oriented electrical steel sheets used for the iron cores of these drive motors have low iron loss. In addition to electromagnetic characteristics, there is an increasing demand for higher strength. Solid solution strengthening, precipitation strengthening, grain refinement strengthening, dislocation strengthening, transformation strengthening, etc. are applied to increase the strength of the steel sheet, but other than solid solution strengthening, the magnetic properties deteriorate, so it is preferable for electromagnetic steel sheets. Absent. In addition, solid solution strengthening has a great effect on increasing strength while avoiding deterioration of magnetic properties, but at the same time, there are problems of increasing rolling load and brittle fracture, and there is an upper limit to the amount of addition from the viewpoint of productivity.

従来、このような無方向性電磁鋼板の高強度化に関し、特許文献1に示すように、質量%で、C:0.0400%以下、Si:0.2〜4.0%、Mn:0.05〜5.0%、P:0.30%以下、S:0.020%以下、Al:8.0%以下、N:0.0400%以下を含有し、残部Feおよび不可避的不純物からなり、組織が体積率でフェライト相:50%以上、マルテンサイト相:50%以下を満足する範囲で主としてフェライト相からなる電磁鋼板について、鋼材内部に直径0.050μm以下の金属間化合物を20個/μm3以上の密度で含有させることで強度を向上させる技術を開示している。 Conventionally, regarding the increase in strength of such non-oriented electrical steel sheets, as shown in Patent Document 1, in mass%, C: 0.0400% or less, Si: 0.2 to 4.0%, Mn: 0.05 to 5.0%, P: It contains 0.30% or less, S: 0.020% or less, Al: 8.0% or less, N: 0.0400% or less, and consists of the balance Fe and unavoidable impurities. Disclosure of technology for improving the strength of electrical steel sheets mainly composed of ferrite phase within the range satisfying 50% or less by containing 20 intermetallic compounds with a diameter of 0.050 μm or less at a density of 20 pieces / μm 3 or more inside the steel material. ing.

特開2005−264315号公報Japanese Unexamined Patent Publication No. 2005-264315

しかしながら、金属間化合物を鋼材内部に析出させて高強度化をはかった電磁鋼板は熱伝導性が劣化しやすいという課題があった。上述のように近年の高速回転化に伴い発熱も大きくなるため、モータコアには優れた熱伝導性が求められており、駆動モータを高速回転化させるためには、熱伝導性を劣化させずに高強度化をはかった電磁鋼板の出現が望まれる。 However, there is a problem that the thermal conductivity of an electromagnetic steel sheet in which an intermetallic compound is precipitated inside a steel material to increase its strength tends to deteriorate. As described above, heat generation increases with the recent increase in high-speed rotation, so that the motor core is required to have excellent thermal conductivity. In order to rotate the drive motor at high speed, the thermal conductivity is not deteriorated. It is hoped that electromagnetic steel sheets with higher strength will appear.

本発明は電磁特性と熱伝導性を劣化させずに強度を向上させた電磁鋼板とその製造方法を提供することを目的とする。 An object of the present invention is to provide an electromagnetic steel sheet having improved strength without deteriorating electromagnetic characteristics and thermal conductivity, and a method for manufacturing the same.

本発明者らは、電磁特性と熱伝導性を劣化させずに強度を向上させた電磁鋼板を得るために種々実験し検討を重ねてきた。本発明者らは上記課題を解決するために主としてAl、Niからなる微細な金属間化合物を鋼中に析出させ、その円相当径の平均値と標準偏差、および、析出密度を適正に制御することで、電磁特性と熱伝導性を劣化させずに強度を向上できることを知見した。本発明の技術の要点は、焼鈍後において鋼板中に転位を生じさせ、その転位を析出サイトとして、鋼板中に大きさがなるべく均一なAl−Niの金属間化合物を分散させて析出させることで、電磁鋼板の電磁特性と熱伝導性を劣化させずに強度を向上させることにある。本発明によれば以下の電磁鋼板とその製造方法が提供される。 The present inventors have conducted various experiments and studies in order to obtain an electromagnetic steel sheet having improved strength without deteriorating electromagnetic properties and thermal conductivity. In order to solve the above problems, the present inventors deposit fine intermetallic compounds mainly composed of Al and Ni in steel, and appropriately control the average value and standard deviation of the equivalent circle diameter and the precipitation density. As a result, it was found that the strength can be improved without deteriorating the electromagnetic characteristics and thermal conductivity. The main point of the technique of the present invention is to generate dislocations in a steel sheet after annealing, and to use the dislocations as precipitation sites to disperse and precipitate Al—Ni intermetallic compounds having a size as uniform as possible in the steel sheet. The purpose is to improve the strength of the electromagnetic steel sheet without deteriorating the electromagnetic characteristics and thermal conductivity. According to the present invention, the following electromagnetic steel sheets and a method for producing the same are provided.

(1)
質量%で、Si:2〜4%、Al:1〜3%、Ni:1.5〜4%を含有し、さらに、Cr:0.01〜4%、Cu:0.01〜4%、Sn:0.01〜0.2%の1または2以上を含有し、残部Feおよび不可避的不純物からなり、
面積基準で求められる円相当径の平均値が1〜10nmで、標準偏差が1以下であるAl−Niの金属間化合物が、30000個/μm以上析出している、電磁鋼板。
(2)
(1)に記載の電磁鋼板を製造する方法であって、質量%で、Si:2〜4%、Al:1〜3%、Ni:1.5〜4%を含有し、さらに、Cr:0.01〜4%、Cu:0.01〜4%、Sn:0.01〜0.2%の1または2以上を含有し、残部Feおよび不可避的不純物からなる鋼スラブを、熱間圧延、冷間圧延および焼鈍をした後、転位密度を1×1014/m以上とする塑性変形を加え、さらに400〜600℃で時効処理を行う、電磁鋼板の製造方法
(1)
By mass%, Si: 2-4%, Al: 1-3%, Ni : 1.5-4%, Cr: 0.01-4%, Cu: 0.01-4%, Sn: Containing 1 or 2 or more of 0.01 to 0.2%, consisting of the balance Fe and unavoidable impurities.
An electromagnetic steel plate in which 30,000 pieces / μm 3 or more of Al—Ni intermetallic compounds having an average value of the equivalent circle diameter determined on an area basis of 1 to 10 nm and a standard deviation of 1 or less are precipitated.
(2)
The method for producing an electromagnetic steel sheet according to (1), which contains Si: 2 to 4%, Al: 1 to 3%, Ni: 1.5 to 4% in mass%, and further comprises Cr: Hot-rolled steel slab containing 1 or 2 or more of 0.01 to 4%, Cu: 0.01 to 4%, Sn: 0.01 to 0.2%, and consisting of the balance Fe and unavoidable impurities. after cold rolling and annealing, plastic deformation to 1 × 10 14 / m 2 or more dislocation density was added, further performing aging treatment at 400 to 600 ° C., the manufacturing method of the electromagnetic steel sheets.

本発明によれば、磁気特性と熱伝導性に優れ、強度や疲労強度、耐磨耗性が向上した無方向性電磁鋼板を得ることができる。これにより、近年のハイブリッド電気自動車(HEV)や電気自動車(EV)などで求められている特性を満足する高速回転モータやロータに磁石を組み込んだモータが得られる。また、本発明によれば、モータ以外についても、例えば電磁開閉器用材料の高効率化、小型化、長寿命化などが達成される。 According to the present invention, a non-oriented electrical steel sheet having excellent magnetic properties and thermal conductivity and improved strength, fatigue strength, and abrasion resistance can be obtained. As a result, a high-speed rotary motor or a motor in which a magnet is incorporated in a rotor that satisfies the characteristics required for a hybrid electric vehicle (HEV) or an electric vehicle (EV) in recent years can be obtained. Further, according to the present invention, for example, high efficiency, miniaturization, and long life of materials for electromagnetic switch can be achieved for other than motors.

実施例の粒内析出物TEM観察写真である。It is a TEM observation photograph of an intragranular precipitate of an example.

以下、本発明の実施の形態について説明する。 Hereinafter, embodiments of the present invention will be described.

先ず、本発明の電磁鋼板における成分組成について説明する。本発明の電磁鋼板は、質量%で、Si:2〜4%、Al:1〜3%以下、Ni:1.5〜4%を含有し、残部Feおよび不可避的不純物からなることを基本とする。 First, the component composition of the electromagnetic steel sheet of the present invention will be described. The electromagnetic steel sheet of the present invention basically contains Si: 2 to 4%, Al: 1 to 3% or less, Ni: 1.5 to 4% in mass%, and is composed of the balance Fe and unavoidable impurities. To do.

Si:2〜4%
Siは鋼の固有抵抗を高めて渦電流を減らし、鉄損を低下せしめるとともに、抗張力を高めるが、添加量が2.0%未満ではその効果が小さい。また、添加により加工硬化能が高まるため、時効熱処理前に実施する加工による転位密度を効果的に増加させる効果もある。一方、Siが4%を超えると鋼を脆化させ、さらに製品の磁束密度を低下させるため4%以下とする。
Si: 2-4%
Si increases the intrinsic resistance of steel, reduces eddy currents, reduces iron loss, and increases tensile strength, but the effect is small when the amount added is less than 2.0%. Further, since the work hardening ability is enhanced by the addition, there is also an effect of effectively increasing the dislocation density by the processing performed before the aging heat treatment. On the other hand, if Si exceeds 4%, the steel is embrittled and the magnetic flux density of the product is further reduced, so the content is set to 4% or less.

Al:1〜3%
本発明ではAlは金属間化合物の構成元素として積極的に添加される重要な元素であるが、3%を超えると脆化が問題になるため、上限を3%とする。Alは通常、脱酸剤として添加されるが、Alの添加を抑えSiにより脱酸を図ることも可能である。一方、金属間化合物の析出強化の効果を得るためには少なくとも1%は含有する。また、固溶Alは電気抵抗を高め鉄損を改善する効果が知られており、この目的でAl−Ni析出物を形成する以上のAlを含有させることは有効である。
Al: 1-3%
In the present invention, Al is an important element positively added as a constituent element of an intermetallic compound, but if it exceeds 3%, embrittlement becomes a problem, so the upper limit is set to 3%. Al is usually added as a deoxidizing agent, but it is also possible to suppress the addition of Al and deoxidize with Si. On the other hand, in order to obtain the effect of strengthening the precipitation of the intermetallic compound, it is contained at least 1%. Further, the solid solution Al is known to have the effect of increasing the electric resistance and improving the iron loss, and for this purpose, it is effective to contain more Al than the Al—Ni precipitate is formed.

Ni:1.5〜4%
従来一般的には、Niは主として固溶体強化元素または炭化物、窒化物等による析出強化元素として利用されていた。本発明では、NiはAlとの金属間化合物を形成し、Al−Niの金属間化合物による析出強化を発現させるために含有させられる。Al−Niの金属間化合物による析出強化を発現させるためには、1.5%以上のNiが必要である。一方、過剰な添加は鋼板の延性を劣化させ通板性が低下する他、磁束密度を低下させるとともに製造工程での金属間化合物の好ましい形成抑制が困難となる場合がある。添加コストも考え上限を4%とする。
Ni: 1.5-4%
Conventionally, in general, Ni has been mainly used as a solid solution strengthening element or a precipitation strengthening element due to carbides, nitrides and the like. In the present invention, Ni is contained to form an intermetallic compound with Al and to develop precipitation strengthening by the intermetallic compound of Al—Ni. In order to develop precipitation strengthening due to the intermetallic compound of Al—Ni, 1.5% or more of Ni is required. On the other hand, excessive addition may deteriorate the ductility of the steel sheet and reduce the passability, reduce the magnetic flux density, and make it difficult to suppress the preferable formation of the intermetallic compound in the manufacturing process. Considering the addition cost, the upper limit is set to 4%.

また、本発明の電磁鋼板は、任意含有成分として、さらに質量%で、Cr:0.01〜4%、Cu:0.01〜4%、Sn:0.01〜0.2%の1または2以上を含有しても良い。これらの元素は、本発明が対象とする電磁鋼板において金属間化合物を形成する元素として知られており、必要に応じて1または2以上を含有することができる。しかし、過剰な含有は鋼板の延性を劣化させ通板性が低下する他、製造工程での金属間化合物の好ましい形成抑制が困難になる場合がある。また、添加コストを考え、Crについては0.01〜4%、Cuについては0.01〜4%、Snについては0.01〜0.2%とする。 Further, the electromagnetic steel sheet of the present invention is 1 or 1 of Cr: 0.01 to 4%, Cu: 0.01 to 4%, Sn: 0.01 to 0.2% in mass% as an optional content component. It may contain 2 or more. These elements are known as elements that form an intermetallic compound in the electromagnetic steel sheet targeted by the present invention, and can contain 1 or 2 or more as required. However, if it is excessively contained, the ductility of the steel sheet is deteriorated and the sheet-passability is lowered, and it may be difficult to suppress the preferable formation of the intermetallic compound in the manufacturing process. Further, considering the addition cost, Cr is 0.01 to 4%, Cu is 0.01 to 4%, and Sn is 0.01 to 0.2%.

本発明の電磁鋼板は以上の成分組成を基本とし、残部Feおよび不可避的不純物からなる。 The electromagnetic steel sheet of the present invention is based on the above component composition, and is composed of the balance Fe and unavoidable impurities.

Cは磁気特性を劣化させる場合があるので0.0400%以下とすることが好ましい。一方、加工硬化能を高め、時効熱処理前に実施する加工による転位密度を効果的に増加させる効果もある。製造コストの観点からは溶鋼段階で脱ガス設備によりC量を低減しておくことが有利で、0.0030%以下とすれば磁気時効抑制の効果が著しく、高強度化の主たる手段として炭化物等の非金属析出物を用いない本発明鋼においては0.0020%以下とすることがさらに好ましく、0.0015%以下がさらに好ましい。0%であっても構わない。 Since C may deteriorate the magnetic characteristics, it is preferably 0.0400% or less. On the other hand, it also has the effect of increasing the work hardening ability and effectively increasing the dislocation density due to the processing performed before the aging heat treatment. From the viewpoint of manufacturing cost, it is advantageous to reduce the amount of C by degassing equipment at the molten steel stage. If it is 0.0030% or less, the effect of suppressing magnetic aging is remarkable, and carbides, etc. are the main means of increasing the strength. In the steel of the present invention which does not use the non-metal precipitate of the above, it is more preferably 0.0020% or less, further preferably 0.0015% or less. It may be 0%.

Mnは、固溶による高強度化や電気抵抗を高め鉄損を改善する元素としても有効であり、本発明鋼でも公知技術に準じた使用が可能である。また、加工硬化能を高め、時効熱処理前に実施する加工による転位密度を効果的に増加させる効果もある。高強度化の観点では、微細金属間化合物を活用する本発明では特に必要としない。0%でも構わないが、鉄鉱石を原料とする工業的製法では、0.01%程度は不可避的に含有される。 Mn is also effective as an element for increasing strength by solid solution, increasing electrical resistance, and improving iron loss, and the steel of the present invention can also be used according to a known technique. It also has the effect of increasing the work hardening ability and effectively increasing the dislocation density due to the processing performed before the aging heat treatment. From the viewpoint of increasing the strength, it is not particularly required in the present invention utilizing the fine intermetallic compound. 0% may be used, but in an industrial manufacturing method using iron ore as a raw material, about 0.01% is inevitably contained.

NはCと同様に磁気特性を劣化させるので0.0400%以下とすることが好ましい。含有により加工硬化能を高め、時効熱処理前に実施する加工による転位密度を効果的に増加させる効果もある。特に本発明ではAlとの強い窒化物の生成を避けるためNは低い方が好ましく、0.0027%以下とすれば磁気時効や微細な窒化物形成による特性劣化の抑制効果は顕著で、さらに好ましくは0.0022%、さらに好ましくは0.0015%以下、0%であっても構わない。 Since N deteriorates the magnetic characteristics like C, it is preferably 0.0400% or less. The content also has the effect of increasing the work hardening ability and effectively increasing the dislocation density due to the processing performed before the aging heat treatment. In particular, in the present invention, it is preferable that N is low in order to avoid the formation of a strong nitride with Al, and if it is 0.0027% or less, the effect of suppressing the deterioration of characteristics due to magnetic aging and the formation of fine nitrides is remarkable, which is more preferable. May be 0.0022%, more preferably 0.0015% or less, or 0%.

Cuは鉄の飽和磁束密度Bsを大幅に低下させ、B50(磁化力が5000[A/m]における磁束密度[T])も大幅に低下させる。BsやB50の低下はモータトルクの低下につながるため、本発明ではCuの含有を必須とすることなく、BsやB50の低下を伴わずに、高強度かつ低鉄損な無方向性電磁鋼板及びその製造方法を実現できる。一方でCu析出による高強度化なども知られており、本発明鋼でも公知技術に準じた使用が可能である。 Cu significantly lowers the saturation magnetic flux density Bs of iron, and also significantly lowers B50 (magnetic flux density [T] when the magnetization force is 5000 [A / m]). Since a decrease in Bs and B50 leads to a decrease in motor torque, in the present invention, the inclusion of Cu is not essential, and the non-oriented electrical steel sheet having high strength and low iron loss is not accompanied by a decrease in Bs and B50. The manufacturing method can be realized. On the other hand, it is also known that the strength is increased by Cu precipitation, and the steel of the present invention can be used according to the known technique.

Nbは、NbCなどの析出物は高強度化には有効であるが、これら析出物が磁壁移動を阻害し、鉄損を大幅に劣化させるため、この目的であえて添加する必要はない。一方で、固溶Nbは固溶強化のみならず結晶粒微細化による高強度化や高周波特性改善にも有効であり、本発明鋼でも公知技術に準じた使用が可能である。 Nb is not necessary to be added for this purpose because precipitates such as NbC are effective for increasing the strength, but these precipitates hinder the movement of the domain wall and significantly deteriorate the iron loss. On the other hand, the solid solution Nb is effective not only for solid solution strengthening but also for increasing the strength and improving the high frequency characteristics by refining the crystal grains, and the steel of the present invention can also be used according to the known technique.

Pは固溶体強化により抗張力を高める効果の著しい元素であるが、この目的ではあえて添加する必要はない。0%であっても構わない。一方、添加により加工硬化能を高め、時効熱処理前に実施する加工による転位密度を効果的に増加させる効果もある。0.3%を超えると脆化が激しく、工業的規模での熱延、冷延等の処理が困難になるため、上限を0.30%とすることが好ましく、さらに好ましくは0.10%以下である。 P is an element having a remarkable effect of increasing the tensile strength by strengthening the solid solution, but it is not necessary to add it for this purpose. It may be 0%. On the other hand, the addition also has the effect of increasing the work hardening ability and effectively increasing the dislocation density due to the processing performed before the aging heat treatment. If it exceeds 0.3%, embrittlement becomes severe and processing such as hot spreading and cold spreading on an industrial scale becomes difficult. Therefore, the upper limit is preferably 0.30%, more preferably 0.10%. It is as follows.

Sは硫化物を形成し磁気特性、特に鉄損を劣化させる場合があるので、Sの含有量はできるだけ低いことが好ましく0%であっても構わない。本発明では0.020%以下が好ましく、さらに好ましくは0.0040%以下、さらに好ましくは0.0020%以下、さらに好ましくは0.0010%以下である。 Since S may form sulfides and deteriorate magnetic properties, particularly iron loss, the content of S is preferably as low as possible and may be 0%. In the present invention, it is preferably 0.020% or less, more preferably 0.0040% or less, still more preferably 0.0020% or less, still more preferably 0.0010% or less.

次に、本発明の電磁鋼板の製造方法について説明する。先ず、前記成分を含む鋼を、通常の電磁鋼板と同様に転炉で溶製し、連続鋳造で鋼スラブとし、ついで熱間圧延、冷間圧延および焼鈍をした後、転位密度を1×1014/m以上とする塑性変形を加え、さらに400〜600℃で時効処理を行う。これらの工程に加え絶縁皮膜の形成や脱炭工程などを経ることも本発明の効果を何ら損なうものではない。 Next, the method for manufacturing the electromagnetic steel sheet of the present invention will be described. First, the steel containing the above components is melted in a converter in the same manner as an ordinary electromagnetic steel plate, continuously cast into steel slabs, and then hot-rolled, cold-rolled and annealed, and then the dislocation density is 1 × 10. Plastic deformation to 14 / m 2 or more is added, and further aging treatment is performed at 400 to 600 ° C. In addition to these steps, the process of forming an insulating film, decarburizing, etc. does not impair the effect of the present invention.

焼鈍後の鋼板を転位密度1×1014/m以上とする塑性変形は、例えばスキンパス圧延、レベラー矯正によって行うことができる。また、モータコア形状に打抜く際の加工により、転位密度1×1014/m以上とすることもできる。そして、これらスキンパス圧延、レベラー矯正、打抜き加工などによって鋼板を転位密度1×1014/m以上とした後、さらに400〜600℃で時効処理を行う。このような塑性変形と時効処理を行うことにより、面積基準で求められる円相当径の平均値が1〜10nmで、標準偏差が1以下であるAl−Niの金属間化合物が、30000個/μm以上析出した、低鉄損、高磁束密度といった優れた電磁特性と高強度を兼ね備え、熱伝導性も劣化していない無方向性電磁鋼板を得ることができる。 The plastic deformation of the annealed steel sheet so that the dislocation density is 1 × 10 14 / m 2 or more can be performed by, for example, skin pass rolling or leveler straightening. Further, the dislocation density can be set to 1 × 10 14 / m 2 or more by processing when punching into the shape of the motor core. Then, the steel sheet is subjected to a dislocation density of 1 × 10 14 / m 2 or more by skin pass rolling, leveler straightening, punching, etc., and then further subjected to aging treatment at 400 to 600 ° C. By performing such plastic deformation and aging treatment, the average value of the equivalent circle diameter determined on an area basis is 1 to 10 nm, and the standard deviation is 1 or less. The number of Al—Ni intermetallic compounds is 30,000 / μm. It is possible to obtain a non-oriented electrical steel sheet having three or more precipitates, excellent electromagnetic characteristics such as low iron loss and high magnetic flux density, and high strength, and the thermal conductivity is not deteriorated.

従来、電磁鋼板で高強度化のために利用されている殆どの元素は添加コストが問題視されるだけではなく磁気特性に少なからず悪影響を及ぼす割に、高強度化効果が小さくコストパフォーマンスに問題があった。本発明でも高強度化の目的のためにSi、Al、Niを含有するが、その技術的効果および技術的目的は従来とは全く異なる。つまり、従来の添加元素は主として固溶体強化元素または炭化物、窒化物等による析出強化元素として利用されていたのに対し、本発明ではAl−Niの金属間化合物を形成し、それによる析出強化効果を発現させるために含有するのである。 Most of the elements conventionally used for high strength in electrical steel sheets not only have a problem of addition cost, but also have a considerable adverse effect on magnetic characteristics, but the high strength effect is small and cost performance is a problem. was there. The present invention also contains Si, Al, and Ni for the purpose of increasing the strength, but its technical effect and technical purpose are completely different from the conventional ones. That is, while the conventional additive element is mainly used as a solid solution strengthening element or a precipitation strengthening element due to carbides, nitrides, etc., in the present invention, an intermetallic compound of Al—Ni is formed, and the precipitation strengthening effect due to the formation is formed. It is contained for expression.

なお、Niによる固溶強化や結晶粒の微細化では、鉄損が少なからず劣化する。また、結晶粒を微細化させずに、固溶強化のみで顧客の満足する強度を確保するためには、Si、Al、Niの含有量を増加しなければならず、合金コストが上昇し、さらに圧延荷重の増加、脆化に伴う生産性低下等の課題がある。 It should be noted that the iron loss is not a little deteriorated by the solid solution strengthening by Ni and the miniaturization of the crystal grains. Further, in order to secure the strength satisfying the customer only by solid solution strengthening without making the crystal grains finer, the contents of Si, Al and Ni must be increased, and the alloy cost increases. Further, there are problems such as an increase in rolling load and a decrease in productivity due to embrittlement.

塑性加工後の鋼板の転位密度を1×1014/m以上とするのは、塑性加工によって鋼板中に転位を十分に生じさせ、その転位を析出サイトとして、鋼板中に大きさがなるべく均一なAl−Niの金属間化合物を分散させて析出させるためである。転位密度が1×1014/m未満では、金属間化合物の析出サイトが不十分であり、時効後において個数密度が30000個/μm以上のAl−Niの金属間化合物が得られなくなってしまう。また、Al−Niの金属間化合物の個数密度が少ないと、金属間化合物の円相当径の平均値が10nmよりも大きくなり、さらに個々の金属間化合物の大きさのばらつきも大きくなり、標準偏差が1を超えてしまう。なお、焼鈍後の鋼板の転位密度が3×1016/mを超えてしまうと却って電磁特性が劣化し、さらに時効後においてAl−Niの金属間化合物の大きさや標準偏差、個数密度が本発明の範囲内から外れる恐れがある。そのため、焼鈍後の鋼板の転位密度は3×1016/m以下であることが望ましい。 The reason why the dislocation density of the steel plate after plastic working is set to 1 × 10 14 / m 2 or more is that the dislocations are sufficiently generated in the steel plate by the plastic working, and the dislocations are used as precipitation sites to make the size as uniform as possible in the steel plate. This is because the intermetallic compound of Al—Ni is dispersed and precipitated. If the dislocation density is less than 1 × 10 14 / m 2 , the precipitation sites of the intermetallic compounds are insufficient, and after aging, an intermetallic compound of Al—Ni having a number density of 30,000 / μm 3 or more cannot be obtained. It ends up. Further, when the number density of the intermetallic compounds of Al-Ni is small, the average value of the equivalent circle diameters of the intermetallic compounds becomes larger than 10 nm, and the size variation of each intermetallic compound becomes large, and the standard deviation becomes large. Exceeds 1. If the dislocation density of the steel sheet after annealing exceeds 3 × 10 16 / m 2 , the electromagnetic characteristics will deteriorate, and after aging, the size, standard deviation, and number density of the Al—Ni intermetallic compound will be reduced. It may be out of the scope of the invention. Therefore, it is desirable that the dislocation density of the steel sheet after annealing is 3 × 10 16 / m 2 or less.

また時効処理は、400〜600℃で行う。400℃未満では、十分な金属間化合物が得られず、一方、600℃を超えると形成される金属間化合物が粗大となってしまう。この際の保持時間は1〜120分とすることが好ましい。短過ぎると十分な金属間化合物が得られず、一方、長過ぎると形成される金属間化合物が粗大となってしまう。この他、加熱速度や冷却速度なども、本発明の特徴である析出物の状態に影響を及ぼす可能性がある。これらの熱処理条件は目的とする特性に応じて成分や生産性なども考慮して決定される。当業者であれば、本発明の技術思想に従い、数度の試行により適切な条件を決定することは容易である。 The aging treatment is performed at 400 to 600 ° C. If the temperature is lower than 400 ° C, a sufficient intermetallic compound cannot be obtained, while if the temperature exceeds 600 ° C, the formed intermetallic compound becomes coarse. The holding time at this time is preferably 1 to 120 minutes. If it is too short, a sufficient intermetallic compound cannot be obtained, while if it is too long, the formed intermetallic compound becomes coarse. In addition, the heating rate, cooling rate, and the like may also affect the state of the precipitate, which is a feature of the present invention. These heat treatment conditions are determined in consideration of components, productivity, etc. according to the desired characteristics. It is easy for a person skilled in the art to determine appropriate conditions by several trials according to the technical idea of the present invention.

以上のような製造工程を経ることで、面積基準で求められる円相当径の平均値が1〜10nmで、標準偏差が1以下であるAl−Niの金属間化合物が、30000個/μm以上析出し、磁気特性と熱伝導性を殆ど損なわず高強度の電磁鋼板を得ることができる。本発明の電磁鋼板は硬質化のための時効熱処理により引張強度が100MPa以上上昇し、または硬度が1.1倍以上増加する。また、時効処理後の最終的な強度は600MPa以上となるものを本発明の対象とする。 Through the above manufacturing process, the number of Al—Ni intermetallic compounds having an average circle-equivalent diameter of 1 to 10 nm and a standard deviation of 1 or less, which is obtained on an area basis, is 30,000 / μm 3 or more. High-strength electrical steel sheets can be obtained by precipitating and hardly impairing magnetic properties and thermal conductivity. The magnetic steel sheet of the present invention has a tensile strength increased by 100 MPa or more or a hardness increased by 1.1 times or more by aging heat treatment for hardening. Further, the object of the present invention is one having a final strength of 600 MPa or more after the aging treatment.

金属間化合物の円相当径の平均値が10nmを超える粗大な化合物が多量に生成すると高強度化の効率が低下し、磁気特性も劣化させる恐れがある。本発明ではサイズの細かい金属間化合物を高密度に生成させることで、優れた磁気特性と熱伝導性を維持しつつ、電磁鋼板の強度を向上させる。一方、金属間化合物の円相当径の平均値が1nm未満と微細では強化能が小さくなる。さらに高強度化を確実に達成するためには、円相当径の標準偏差が1以下となるように個々の金属間化合物の大きさが揃っていることが必要である。この標準偏差が1を超えると、金属間化合物の大きさが不均一となり、磁気特性と熱伝導性を維持しつつ、電磁鋼板の強度を向上させることが困難となる。なお、鉄鋼材料中に形成するAl−Niの金属間化合物としては、NiAl、NiAlなどが通常知られている。また、これらの化合物の元素比は相当に変動することは知られており、また何らかの不純物元素を含んだものも本発明に相当する。 If a large amount of coarse compounds having an average value of the equivalent circle diameter of the intermetallic compound exceeding 10 nm are produced, the efficiency of increasing the strength may decrease and the magnetic characteristics may also deteriorate. In the present invention, by producing a fine-sized intermetallic compound at a high density, the strength of the electrical steel sheet is improved while maintaining excellent magnetic properties and thermal conductivity. On the other hand, if the average value of the equivalent circle diameters of the intermetallic compounds is less than 1 nm, the reinforcing ability becomes small. In order to further increase the strength reliably, it is necessary that the sizes of the individual intermetallic compounds are uniform so that the standard deviation of the equivalent circle diameter is 1 or less. If this standard deviation exceeds 1, the size of the intermetallic compound becomes non-uniform, and it becomes difficult to improve the strength of the electrical steel sheet while maintaining the magnetic properties and thermal conductivity. As the intermetallic compounds of Al-Ni to form in the steel material, NiAl, such as Ni 3 Al is commonly known. Further, it is known that the elemental ratios of these compounds fluctuate considerably, and those containing some impurity elements also correspond to the present invention.

高強度化の観点から、金属間化合物の数密度は30000個/μm以上の析出が必要である。金属間化合物サイズと数密度の制御は、優れた高強度化と磁気特性を両立し、熱伝導性の劣化を防ぐ観点から非常に重要である。その理由は、これらが強度および磁気特性と熱伝導性にそれぞれ影響するのみならず、これらを変化させたときの強度、磁気特性および熱伝導性が変化する挙動がそれぞれ異なるためである。すなわち、強度上昇効果が高く、磁気特性劣化と熱伝導性の劣化が少ない領域に制御する必要がある。このためには前述のように成分および熱処理条件、さらには時効処理前の転位密度を適切に制御し、金属間化合物のサイズと数密度を所望の範囲とすることが有効である。 From the viewpoint of increasing the strength, the number density of the intermetallic compound needs to be precipitated at 30,000 / μm 3 or more. Controlling the intermetallic compound size and number density is extremely important from the viewpoint of achieving both excellent strength and magnetic properties and preventing deterioration of thermal conductivity. The reason is that not only do they affect the strength, magnetic properties and thermal conductivity, respectively, but the behavior of changing the strength, magnetic properties and thermal conductivity when they are changed is different. That is, it is necessary to control the region where the strength increasing effect is high and the deterioration of magnetic characteristics and the deterioration of thermal conductivity are small. For this purpose, it is effective to appropriately control the components and heat treatment conditions, as well as the dislocation density before the aging treatment, and to set the size and number density of the intermetallic compound within a desired range as described above.

本発明では高強度化の主要な手段として結晶組織の微細化を利用しないため、結晶粒径は磁気特性の観点から最適な範囲に調整が可能である。高強度化に寄与する金属間化合物のサイズや密度は成分のみならず、最終的な熱処理により制御が可能であるため結晶粒径はこの熱処理以前の、例えば再結晶焼鈍の最高到達温度およびその温度域での保持時間等により金属間化合物の制御とは独立に制御が可能となる。結晶粒径は通常は300μm以下であり、好ましくは30〜250μmに制御される。さらに好ましくは60〜200μmである。一般的には鋼板を使用する際の励磁電流の周波数が高い場合には結晶粒は微細にしておくことが好ましい。また、方向性電磁鋼板のように二次再結晶等を利用して数cmにまで結晶粒径を粗大化させても本発明の効果は何ら損なわれるものではない。 Since the present invention does not utilize the miniaturization of the crystal structure as the main means for increasing the strength, the crystal grain size can be adjusted to the optimum range from the viewpoint of magnetic properties. Since the size and density of the intermetallic compound that contributes to high strength can be controlled not only by the components but also by the final heat treatment, the crystal grain size is the maximum reached temperature of recrystallization annealing and its temperature before this heat treatment, for example. It is possible to control the intermetallic compound independently of the control of the intermetallic compound depending on the retention time in the region and the like. The crystal grain size is usually 300 μm or less, and is preferably controlled to 30 to 250 μm. More preferably, it is 60 to 200 μm. Generally, when the frequency of the exciting current when using the steel sheet is high, it is preferable to keep the crystal grains fine. Further, even if the grain size is coarsened to several cm by using secondary recrystallization or the like as in the grain-oriented electrical steel sheet, the effect of the present invention is not impaired at all.

なお、本発明の効果は通常電磁鋼板の表面に形成されている表面皮膜の有無および種類によらず、さらに製造工程にはよらないため無方向性または方向性の電磁鋼板に適用できる。また、用途も特に限定されるものではなく、家電または自動車等で用いられるモータのロータ用途の他、強度と磁気特性が求められる全ての用途に適用される。 It should be noted that the effect of the present invention can be applied to non-oriented or directional electromagnetic steel sheets because it does not depend on the presence and type of the surface film normally formed on the surface of the electrical steel sheet and further does not depend on the manufacturing process. The application is not particularly limited, and is applied to all applications requiring strength and magnetic characteristics, in addition to motor rotor applications used in home appliances or automobiles.

表1に示す真空溶解した熱延鋼板を、酸洗後、0.20mm厚に冷延し、焼鈍した。その後、転位密度を表1に示す条件とする塑性変形を加え、350〜750℃×2時間の時効処理を行い、磁気特性、機械特性を評価した。その結果を表1に示す。なお、表1において、本発明の範囲外の数値には下線を付した。 The vacuum-melted hot-rolled steel sheet shown in Table 1 was pickled, cold-rolled to a thickness of 0.20 mm, and annealed. Then, plastic deformation with the dislocation density as the condition shown in Table 1 was added, and aging treatment was performed at 350 to 750 ° C. for 2 hours to evaluate the magnetic properties and mechanical properties. The results are shown in Table 1. In Table 1, the numerical values outside the scope of the present invention are underlined.

成分が本発明範囲の材料は、通常の仕上焼鈍後に550℃×2時間の時効処理を行うことで、YP:140〜160MPa、TS:160〜180MPaの上昇を、鉄損劣化なしに得た(到達YP:570〜910MPa、TS:710〜1130MPa)。図1に示すように、高分解能TEMを用いて、α−Feとβ’−NiAlの結晶構造の違いを考慮した暗視野TEM観察を行うことで、結晶粒内に5nm程度の微細析出物が3,000個/μmの密度で大量に観察され、これが強度上昇の原因である事が分かった。図1中、白く見える析出物は直径約5nmのAl−Ni金属間化合物であり、個数密度は約3,000個/μmであった。これは、本観察技術を用いることで初めて判明した強度上昇のメカニズムである。なお、暗視野TEM観察の観察部位の厚さは約0.1μmであり、3,000個/μmは30,000個/μmに相当する。 Materials whose components are in the range of the present invention were subjected to aging treatment at 550 ° C. for 2 hours after normal finish annealing to obtain an increase in YP: 140 to 160 MPa and TS: 160 to 180 MPa without iron loss deterioration ( Reach YP: 570 to 910 MPa, TS: 710 to 1130 MPa). As shown in FIG. 1, by performing dark-field TEM observation considering the difference in crystal structure between α-Fe and β'-NiAl using a high-resolution TEM, fine precipitates of about 5 nm are formed in the crystal grains. It was observed in large quantities at a density of 3,000 grains / μm 2 , and it was found that this was the cause of the increase in strength. In FIG. 1, the white-looking precipitate was an Al—Ni intermetallic compound having a diameter of about 5 nm, and the number density was about 3,000 / μm 2 . This is the mechanism of strength increase that was first discovered by using this observation technique. The thickness of the observation site for dark-field TEM observation is about 0.1 μm, and 3,000 / μm 2 corresponds to 30,000 / μm 3.

塑性変形後の転位密度が約5×1013/mの場合には、析出物の円相当平均径は約3nmと小さかったが標準偏差が1よりも大きく、個数密度は約5000個/μmと非常に少なくなった。この場合、時効処理後の強度上昇は得られず、YP=480MPaであった。塑性変形後の転位密度が約1×1014/mの場合でも、時効処理温度が350℃の場合には、Al−Ni析出物はほとんど観察されず、時効処理後の強度上昇が得られなかった。一方で、塑性変形後の転位密度が約1×1014/mで、時効処理温度が750℃の場合、円相当平均径10nm以上の析出物が増加し、個数密度は約20000個/μmと少なかった。この場合、時効処理後の強度上昇が得られなかっただけではなく、鉄損W10/800も32.0W/kgと大きく劣化した。 When the dislocation density after plastic deformation was about 5 × 10 13 / m 2 , the average circle-equivalent diameter of the precipitate was as small as about 3 nm, but the standard deviation was larger than 1, and the number density was about 5000 / μm. It became very small with 3. In this case, no increase in strength was obtained after the aging treatment, and YP = 480 MPa. Even when the dislocation density after plastic deformation is about 1 × 10 14 / m 2 , when the aging treatment temperature is 350 ° C., almost no Al—Ni precipitates are observed, and the strength after aging treatment is increased. There wasn't. On the other hand, when the dislocation density after plastic deformation is about 1 × 10 14 / m 2 and the aging treatment temperature is 750 ° C., precipitates with an average circle diameter of 10 nm or more increase, and the number density is about 20000 pieces / μm. It was as small as 3. In this case, not only was the strength not increased after the aging treatment, but the iron loss W10 / 800 was also significantly deteriorated to 32.0 W / kg.

各材料から直径10mmの円板試料をそれぞれ10枚切り出し、レーザフラッシュ法にて熱伝導率を測定したところ、本発明の材料に比べて、比較例では熱伝導率測定値のばらつきが大きくなった。これは析出物のサイズ分布が大きいためと推定され、特に標準偏差が1を超えるものは、熱伝導率測定値のばらつきが平均値±10%程度と大きくなった。 When 10 disc samples having a diameter of 10 mm were cut out from each material and the thermal conductivity was measured by the laser flash method, the variation in the measured thermal conductivity was larger in the comparative example than in the material of the present invention. .. It is presumed that this is because the size distribution of the precipitates is large, and especially when the standard deviation exceeds 1, the variation of the measured thermal conductivity values becomes large as an average value of about ± 10%.

さらに、Cuを質量%で0.01%以上添加することでYPが向上し、本発明例では1%または2%の添加でYP830MPa以上が得られた。Cr添加は鉄損W10/800低減に効果があり、Sn添加は磁束密度B50が向上した。それぞれ質量%で0.01%以上添加することで効果が得られた。 Further, YP was improved by adding 0.01% or more of Cu in mass%, and in the example of the present invention, YP of 830 MPa or more was obtained by adding 1% or 2%. The addition of Cr was effective in reducing the iron loss W10 / 800, and the addition of Sn improved the magnetic flux density B50. The effect was obtained by adding 0.01% or more in mass% of each.

Figure 0006852965
Figure 0006852965

Claims (2)

質量%で、Si:2〜4%、Al:1〜3%、Ni:1.5〜4%を含有し、さらに、Cr:0.01〜4%、Cu:0.01〜4%、Sn:0.01〜0.2%の1または2以上を含有し、残部Feおよび不可避的不純物からなり、
面積基準で求められる円相当径の平均値が1〜10nmで、標準偏差が1以下であるAl−Niの金属間化合物が、30000個/μm以上析出している、電磁鋼板。
By mass%, Si: 2-4%, Al: 1-3%, Ni : 1.5-4%, Cr: 0.01-4%, Cu: 0.01-4%, Sn: Containing 1 or 2 or more of 0.01 to 0.2%, consisting of the balance Fe and unavoidable impurities.
An electromagnetic steel plate in which 30,000 pieces / μm 3 or more of Al—Ni intermetallic compounds having an average value of the equivalent circle diameter determined on an area basis of 1 to 10 nm and a standard deviation of 1 or less are precipitated.
請求項1に記載の電磁鋼板を製造する方法であって、The method for manufacturing an electromagnetic steel sheet according to claim 1.
質量%で、Si:2〜4%、Al:1〜3%、Ni:1.5〜4%を含有し、さらに、Cr:0.01〜4%、Cu:0.01〜4%、Sn:0.01〜0.2%の1または2以上を含有し、残部Feおよび不可避的不純物からなる鋼スラブを、熱間圧延、冷間圧延および焼鈍をした後、転位密度を1×10 By mass%, Si: 2-4%, Al: 1-3%, Ni: 1.5-4%, Cr: 0.01-4%, Cu: 0.01-4%, A steel slab containing 1 or 2 or more of Sn: 0.01 to 0.2% and composed of the balance Fe and unavoidable impurities is hot-rolled, cold-rolled and annealed, and then the dislocation density is 1 × 10. 1414 /m/ M 2 以上とする塑性変形を加え、さらに400〜600℃で時効処理を行う、電磁鋼板の製造方法。A method for manufacturing an electromagnetic steel sheet, which is subjected to the above plastic deformation and further subjected to an aging treatment at 400 to 600 ° C.
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