JPH01283324A - Production of grain-oriented electrical steel sheet having high magnetic flux density - Google Patents
Production of grain-oriented electrical steel sheet having high magnetic flux densityInfo
- Publication number
- JPH01283324A JPH01283324A JP63112551A JP11255188A JPH01283324A JP H01283324 A JPH01283324 A JP H01283324A JP 63112551 A JP63112551 A JP 63112551A JP 11255188 A JP11255188 A JP 11255188A JP H01283324 A JPH01283324 A JP H01283324A
- Authority
- JP
- Japan
- Prior art keywords
- annealing
- steel sheet
- cold rolling
- magnetic flux
- steel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 230000004907 flux Effects 0.000 title claims abstract description 40
- 229910001224 Grain-oriented electrical steel Inorganic materials 0.000 title claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 27
- 238000000137 annealing Methods 0.000 claims abstract description 71
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 47
- 239000010959 steel Substances 0.000 claims abstract description 47
- 238000005097 cold rolling Methods 0.000 claims abstract description 33
- 238000001953 recrystallisation Methods 0.000 claims abstract description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 238000005261 decarburization Methods 0.000 claims abstract description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 238000005121 nitriding Methods 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012298 atmosphere Substances 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 13
- 229910000976 Electrical steel Inorganic materials 0.000 claims abstract description 11
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 8
- 238000000746 purification Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 34
- 230000008569 process Effects 0.000 claims description 25
- 229910052748 manganese Inorganic materials 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 abstract description 21
- 238000005098 hot rolling Methods 0.000 abstract description 14
- 229910052796 boron Inorganic materials 0.000 abstract description 11
- 229910052710 silicon Inorganic materials 0.000 abstract description 8
- 239000003795 chemical substances by application Substances 0.000 abstract 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 33
- 239000000047 product Substances 0.000 description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 239000002244 precipitate Substances 0.000 description 18
- 239000007789 gas Substances 0.000 description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 11
- 239000003112 inhibitor Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 9
- 239000006104 solid solution Substances 0.000 description 9
- 238000009776 industrial production Methods 0.000 description 7
- 230000009467 reduction Effects 0.000 description 7
- 229910000616 Ferromanganese Inorganic materials 0.000 description 6
- -1 ferromanganese nitride Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 229910052787 antimony Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000008439 repair process Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052839 forsterite Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic 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
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000000576 supplementary effect Effects 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002747 voluntary effect Effects 0.000 description 1
Landscapes
- Manufacturing Of Steel Electrode Plates (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、電気機器の鐵芯として用いられる一方向性電
磁鋼板の製造に際し、基本的冶金現象として利用される
二次再結晶の発現に対して有効な析出物（一般にインヒ
ビターと呼ばれている）として新規な成分組成とそれを
前提とするプロセスに関する。[Detailed Description of the Invention] [Field of Industrial Application] The present invention is directed to the development of secondary recrystallization, which is used as a basic metallurgical phenomenon in the production of unidirectional electrical steel sheets used as iron cores of electrical equipment. The present invention relates to a new component composition as an effective precipitate (generally called an inhibitor) and a process based on it.
一方向性電磁鋼板は、鋼板面が（１１０１面で圧延方向
に＜００１＞軸を有する所謂ゴス方位（ミラー指数で（
１１０） ＜００１＞方位と表す）を持つ結晶粒から構
成されており、軟磁性材料として変圧器および電機用の
鐵芯に使用される。The unidirectional electrical steel sheet has a so-called Goss orientation (Miller index: (
110) It is composed of crystal grains with <001> orientation), and is used as a soft magnetic material in transformers and iron cores for electrical equipment.
この鋼板は、磁気特性として磁化特性と鐵損特性が良好
でなければならない。This steel plate must have good magnetic properties such as magnetization properties and iron loss properties.
磁化特性の良否は、かけられた一定の磁場の下で鐵芯内
に誘起される磁束密度で決まり、磁束密度が高い製品（
一方向性電磁銅板）を用いると鐵芯を小型化できる。The quality of magnetization characteristics is determined by the magnetic flux density induced within the iron core under a constant applied magnetic field, and products with high magnetic flux density (
By using a unidirectional electromagnetic copper plate (unidirectional electromagnetic copper plate), the iron core can be made smaller.
磁束密度が高い鋼板は、結晶粒の方位を（１１０１＜０
０１＞に高度に揃えることによって得られる。Steel sheets with high magnetic flux density have crystal grain orientations (1101<0
01>.
鐵損は、鐵芯に所定の交流磁場を与えたときに熱エネル
ギとして消費される電力損失であり、その良否に対して
、磁束密度、板厚、鋼中の不純物量、比抵抗、結晶粒度
等が影響する。Iron loss is the power loss consumed as thermal energy when a predetermined alternating magnetic field is applied to the iron core. etc. are affected.
磁束密度が高い銅ｊ板は、電気機器の識芯を小さくでき
るととも乙こ識損も低くなるから望ましく、当該分野で
はできる限り磁束密度の高い製品を低コスＩ・で製造す
る方法の開発が課題となっている。Copper J-boards with high magnetic flux density are desirable because they can reduce the center of gravity of electrical equipment and also reduce the loss of power, and in this field, development of methods to manufacture products with as high a magnetic flux density as possible at a low cost is required. has become an issue.
処で、一方向性電磁鋼板は、スラブを熱間圧延して得ら
れる熱延機を適切な冷間圧延と焼鈍との組合せにより最
終板厚とした鋼板を仕上焼鈍することにより、（１１０
１＜００１＞方位を有する一次再結晶粒を選択成畏させ
る所謂二次再結晶によって得られる。The unidirectional electrical steel sheet is produced by finishing annealing the steel sheet to a final thickness by a combination of appropriate cold rolling and annealing using a hot rolling mill obtained by hot rolling a slab.
It is obtained by so-called secondary recrystallization in which primary recrystallized grains having a 1<001> orientation are selectively formed.
二次再結晶は、二次再結晶前の鋼板中に微細な析出物、
たとえばＭｎＳ 、 八ｎＮ 、ＭｎＳｅ、 （
ＡＡ 。Secondary recrystallization is caused by the formation of fine precipitates in the steel sheet before secondary recrystallization.
For example, MnS, 8nN, MnSe, (
A.A.
５ｉ）Ｎ、 ＣｕｚＳ等が存在すること或はＳｎ、Ｓｂ
等の粒界存在型の元素が存在するごとによって達成され
る。ごれら析出物、粒界存在型の元素は、Ｊ。5i) The presence of N, CuzS, etc. or Sn, Sb
This is achieved by the presence of grain boundary-existing elements such as. Elements existing in grain boundaries and precipitates are J.
Ｅ、 Ｍａｙ ａｎｄ Ｄ、Ｔｕｒｎｂｕｌｌ （Ｔｒ
ａｎｓ、Ｍｅｔ、Ｓｏｃ、ＡＩＭＥ２１２（１９５８）
ｐ７６９／７８１）によって説明されているように、
仕上焼鈍工程で（１１０） ＜００１＞方位以外の一次
再結晶粒の成長を抑え、ｆｌｌｏｌ ＜００１＞方位粒
を選択的に成長させる機能を持つ。E, May and D, Turnbull (Tr
ans, Met, Soc, AIME212 (1958)
p769/781),
In the final annealing step, it has the function of suppressing the growth of primary recrystallized grains other than the (110) <001> orientation and selectively growing flol <001> oriented grains.
このような、粒成長の抑制効果は、一般にインヒビター
効果と呼ばれている。Such a grain growth suppressing effect is generally called an inhibitor effect.
従って、当該分野における研究開発の重点課題は、如何
なる種類の析出物或は粒界存在型の元素を用いて二次再
結晶を安定させるか、そして正確な（１１０） ＜００
１＞方位粒の存在割合を高めるために、それらの適切な
存在状態を如何に達成するかにある。Therefore, the key issue for research and development in this field is what kind of precipitates or grain boundary-existing elements should be used to stabilize secondary recrystallization, and how to achieve accurate (110) <00
In order to increase the proportion of 1> oriented grains, the problem lies in how to achieve an appropriate state of their existence.
特に、最近では、一種類の析出物による（１１０）＜０
０１＞方位の高度な制御に限界がある処から、種々の析
出物について短所、長所を深く解明することにより幾つ
かの析出物を有機的に組合せて、より磁束密度の高い製
品を安定してかつ低コストで製造し得る技術の開発が進
められている。In particular, recently, (110)<0 due to one type of precipitate
01> Since there is a limit to advanced control of orientation, by deeply understanding the disadvantages and advantages of various precipitates, it is possible to organically combine several precipitates to stably produce products with higher magnetic flux density. Further, the development of technology that can be manufactured at low cost is progressing.
析出物の種類として、Ｎ、Ｆ、Ｌｉｔｔｍａｎｎは、特
公昭３０−３６５１号公報にまた、Ｊ、Ｅ、Ｍａｙおよ
びり、Ｔｕｒｎｂｕｌｌは、ＴｒａｎｓｏＭｅｔ、Ｓｏ
ｃ、八ＩＭＥ ２１２（１９５８） ｐ７６９／７８１
にＭｎＳを、日日および叛意は、特公昭３３−４７１０
号公報にＡｊｌ！ＮとＭｎＳを、Ｆ ｉｅｄ ｌｅｒは
、Ｔｒａｎｓ、Ｍｅｔ、Ｓｏｃ。Regarding the types of precipitates, N, F, Littmann, J, E, May, Turnbull, TransoMe, So
c, 8 IME 212 (1958) p769/781
The MnS, Japan, and rebellion were published in the Special Publication No. 33-4710.
Ajl in the issue! N and MnS, Fiedler is Trans, Met, Soc.
ＡＩＭＥ ２１２（１９６１） ｐ、１２０１〜１２０
５にＶＮを、今生らは、特公昭５１−１３４６９号公報
にＭｎＳｅ、Ｓｂを、Ｊ、Ａ。AIME 212 (1961) p, 1201-120
5, and Imao et al. published MnSe, Sb in Japanese Patent Publication No. 51-13469, J, A.
Ｓａｌｓｇｉｖｅｒらは特公昭５７−４５８１８号公報
にＡｆｆｉＮと硫化銅を小松らは、特公昭６２−４５２
８５号公報に（ＡＡ、５ｉ）Ｎを提示している。その他
に、ＴｉＳ 。Salsgiver et al. reported AffiN and copper sulfide in Japanese Patent Publication No. 57-45818, and Komatsu et al.
(AA, 5i)N is presented in Publication No. 85. In addition, TiS.
ＣｒＳ 、ＣｒＣ、ＮｂＣ，５ｉＯｚ等も知られてい
る。CrS, CrC, NbC, 5iOz, etc. are also known.
一方、粒界存在型の元素として、日本金属学会誌２７（
１９６３） ｐ、１８６に、斉藤達雄がＡｓ、Ｓｎ、Ｓ
ｂ等を提示しているが、工業生産においては、これら元
素が単独で使用される例は無く、何れも析出物と共存さ
せてその補助的効果を狙って使用される。On the other hand, as a grain boundary existing element, the Journal of the Japan Institute of Metals 27 (
1963) p. 186, Tatsuo Saito describes As, Sn, S
b, etc., but in industrial production, there are no examples of these elements being used alone, and they are all used together with the precipitate to achieve a supplementary effect.
さらに、特徴のあるインヒビターとして、Ｉｔ、Ｇｒｅ
ｎｏｂｌｅにより合衆国特許第３．９０５．８４２号（
１９７５）に提示されているもの、Ｈ，Ｆｉｅｄｌｅｒ
により合衆国特許第３，９０５，８４３号（１９７５）
に提示されているものがある。即ち、固溶のＳ、Ｂ、Ｎ
を適当量だけ存在させることによって、磁束密度の高い
一方向性電磁鋼板の製造を可能にしている。Furthermore, as characteristic inhibitors, It, Gre
U.S. Patent No. 3.905.842 by Noble (
1975), H. Fiedler
No. 3,905,843 (1975)
There are some that are presented. That is, S, B, N in solid solution
By having an appropriate amount of , it is possible to manufacture unidirectional electrical steel sheets with high magnetic flux density.
二次再結晶に効果のある析出物の選択基準は、必ずしも
明らかにされていないが、その代表他見解か、検問によ
り［鐵と鋼Ｊ ５３（１９６７） ｐ、１００７〜１０
７３に述べられている。要約すると、（１）大きさは、
０，１μＩｎ程度
（２）必要容積は、０．１ｖｏ１．％以上（３）二次再
結晶温度域で完全に）容けてしまっても、全く溶けなく
ても不可であり、適当な程度固溶すること
である。The selection criteria for precipitates that are effective in secondary recrystallization are not necessarily clear, but representative opinions or other opinions or inquiries have shown that [Tetsu-to-Hagane J 53 (1967) p. 1007-10]
73. To summarize, (1) the size is
Approximately 0.1 μIn (2) The required volume is 0.1 vol. % or more (3) Even if it is completely dissolved in the secondary recrystallization temperature range, it is impossible even if it does not melt at all, and it is necessary to form a solid solution to an appropriate degree.
上に述べた種々の析出物は、これらの条件Ｇ°こ当ては
まる部分もあるが、全ての現象かこの条件に当てはまる
わけではない。本発明の冷間圧延以降に鋼板を窒化する
プロセスにおいては、−に記（１）は重要な意味を持た
ない。Although some of the various precipitates described above meet these conditions G°, this does not apply to all phenomena. In the process of nitriding a steel sheet after cold rolling according to the present invention, (1) in - does not have any important meaning.
このように、現状では、析出物の選択をする際の指導原
理は確立しておらず、試行錯誤の繰返しで新しいインヒ
ビター制御技術が探索されている。Thus, at present, no guiding principles have been established for selecting precipitates, and new inhibitor control techniques are being searched for through repeated trial and error.
何れにしても、高い磁束密度（＋１１（１１＜００１．
＞方位の高い集積度）を得るためには、析出物を微細で
均一かつ多量に、仕上焼鈍前の鋼板中に存在させること
が必要であり、析出物の制御と併せその析出物の特性に
合致する圧延、熱処理の適切な組合せにより、二次再結
晶前の性状を調整することが重要である。In any case, the high magnetic flux density (+11 (11<001.
> In order to obtain a high degree of accumulation in orientation, it is necessary to have fine, uniform, and large amounts of precipitates in the steel sheet before final annealing. It is important to adjust the properties before secondary recrystallization by appropriate combinations of rolling and heat treatment.
現在、］二業生産されている代表的な一方向性電磁釦、
Ｉ板の製造方法として３種類あり、それぞれ長所および
短所をもっでいる。Currently, a typical unidirectional electromagnetic button that is produced in two industries,
There are three methods for manufacturing I-plates, each with its own advantages and disadvantages.
第１の製造方法は、Ｍ、Ｆ、ｌｉｔｔｍａｎｎにより特
公昭３０ ３６５１号公幸旧こ提示された、ＭｎＳをイ
ンヒビターとして用いる２凹冷延プロセスである。−次
再結晶粒は安定して発達するけれども、高い磁束密度か
得られない。The first manufacturing method is a two-concave cold rolling process using MnS as an inhibitor, which was proposed by M. F. Littmann in Japanese Patent Publication No. 3651/1983. Although -order recrystallized grains develop stably, high magnetic flux density cannot be obtained.
第２の製造方法は、田［」、板金らにより特公昭４０４
５６４４号公報乙こ提示された、ＡｐＮ＋ＭｎＳをイン
ヒビターとして用い、最終冷延を８０％を超える強圧下
とする１凹冷延プロセスであり、極めて高い磁束密度か
得られるけれども、工業生産に際して製造条件の適正範
囲が狭く、高い磁性の製品の安定した生産か困難である
。The second manufacturing method was developed by Takashi, Shekin et al.
The one-concave cold rolling process proposed in Publication No. 5644 uses ApN+MnS as an inhibitor and subjects the final cold rolling to a strong reduction of over 80%.Although extremely high magnetic flux density can be obtained, it is difficult to meet the manufacturing conditions during industrial production. The suitable range is narrow and it is difficult to stably produce highly magnetic products.
第３の製造方法は、今生らにより特公昭５１−１３４６
１号公報に提示された、Ｍｎ５（および／またはＭｎ５
ｅ）＋ｓｂをインヒビターとして用いる２凹冷延プロセ
スであって、比較的高い磁束密度が得られるけれども、
Ｓｂ 、Ｓｅといった有害かつ高価な元素を使用し、し
かも２回冷延法である処から製造コストが高い。The third manufacturing method was developed by Imao et al.
Mn5 (and/or Mn5
e) a two-concave cold rolling process using +sb as an inhibitor, although a relatively high magnetic flux density is obtained;
The manufacturing cost is high because harmful and expensive elements such as Sb and Se are used, and the process requires a double cold rolling process.
上記３種類の製造方法には、共通ずる次の問題がある。The above three types of manufacturing methods have a number of common problems.
即ち、これら製造方法においては、何れも析出物を微細
かつ均一に析出させるために、析出物を一旦固溶させる
。そのために、スラブ加熱温度が必然的に高くなる。That is, in all of these manufacturing methods, the precipitates are once dissolved in solid solution in order to finely and uniformly precipitate the precipitates. Therefore, the slab heating temperature inevitably becomes high.
因みに、第１の製造方法においては、スラブ加熱温度は
１２６０℃以−トであり、第２の製造方法においては、
特開昭４８−５１８５２号公報に開示されているように
、素材のＳｉ含有量によるか、Ｓｉ：３％の場合で１３
５０℃である。第３の製造方法においても、特開昭５１
−２０７１６号公報に開示されているように、スラブ加
熱温度は１２３０℃以上てあり、高い磁束密度か得られ
た実施例によれば１３２０℃といった極めて高い／精度
である。Incidentally, in the first manufacturing method, the slab heating temperature is 1260°C or higher, and in the second manufacturing method,
As disclosed in Japanese Unexamined Patent Publication No. 48-51852, 13
The temperature is 50°C. Also in the third manufacturing method, JP-A-51
As disclosed in Japanese Patent No. 20716, the slab heating temperature is 1230° C. or higher, and in an example where a high magnetic flux density is obtained, it is 1320° C., which is extremely high/accurate.
このように、スラブを高温に加熱して析出物を固溶さ・
已、その後の熱間圧延中或ば熱処理中に析出させる。In this way, the slab is heated to a high temperature to dissolve the precipitates into solid solution.
Then, it precipitates during subsequent hot rolling or heat treatment.
スラブ加熱温度が高くなると、加熱のためのエネルギ消
費か多くなるとともに、ノロの発生による歩留りの低下
といった問題がある他加熱炉の補修コス）・の増大、設
備稼働率の低下といった問題を惹起する。さらに、特公
昭５７−４１５２６号公報に開示されているように、ス
ラブの加熱温度が高いごとに起因して線状の二次再結晶
不良部が発生するため、連続鋳造スラブを使用できない
という問題がある。As the slab heating temperature increases, energy consumption for heating increases, and this also causes problems such as a decrease in yield due to the generation of slag, an increase in heating furnace repair costs, and a decrease in equipment operating rate. . Furthermore, as disclosed in Japanese Patent Publication No. 57-41526, continuous casting slabs cannot be used because linear secondary recrystallization defects occur each time the slab is heated to a high temperature. There is.
ＪＪｉｌえて、１−゛記コスト面の問題以−ヒに重要な
問題は、鐵）員を低下せしめるべくｓｉ含有量を多く、
製品板厚を）Ｎくするといった１１段を採ると、前記綿
状の二次再結晶不良部か多発し、高温スラブ加熱法を前
提とするプロセスでは、将来の鐵損特性１ｉ＋ＩＩＪこ
希望か持てないことである。In addition, the more important problem than the cost problem described in 1-2 is to increase the Si content in order to reduce the
If 11 steps are adopted, such as reducing the product board thickness by N, the aforementioned flocculent secondary recrystallization defects will occur frequently, and in a process based on high-temperature slab heating, future iron loss characteristics of 1i + IIJ will be difficult to achieve. There is no such thing.
かかる問題を解決すべく、特公昭６１−６０８９６号公
報に、鋼中のＳ含有量を少なくすることによって、二次
再結晶を極めて安定させ、高Ｓｉ化、薄手化を可能なら
しめるプロセスが提案された。しかしながら、このプロ
セスにも工業生産において、磁束密度を高い水準で安定
させることが困難であるという問題がある。In order to solve this problem, Japanese Patent Publication No. 61-60896 proposes a process that makes secondary recrystallization extremely stable by reducing the S content in the steel, making it possible to increase the Si content and make the steel thinner. It was done. However, this process also has the problem that it is difficult to stabilize the magnetic flux density at a high level in industrial production.
一方、）１．Ｇｒｅｎｏｂｌｅにより合衆国特許第３，
９０５，８４２号に提示された方法或はＨ，Ｆｉｅｄｌ
ｅｒにより合衆国特許第３ 、９０５ 、８４３号に提
示された方法があるが、これらの技術には本質的な矛盾
があり、工業生産されていない。即ち、この技術ではイ
ンヒビターとして固溶Ｓを主体としているから、固溶Ｓ
を確保するためにＭｎ含有量を低くし、ＭｎＳを形成さ
せないことが必須の要件である。具体的には、Ｍｎ／Ｓ
≦２．１が必須の要件となる。処で、広べ知られている
ように、固溶Ｓは材料の靭性に極めて悪影響を持つ。従
って、Ｓｉ含有量が多く、割れ易い一方向性電磁鋼板に
あっては、このような固溶Ｓのある状態で材料を冷間圧
延することは、工業生産では極めて困難である。On the other hand, )1. U.S. Patent No. 3 by Grenoble,
905,842 or H. Fiedl.
er in US Pat. No. 3,905,843, but these techniques have inherent inconsistencies and have not been commercially produced. In other words, since this technology mainly uses solid solution S as an inhibitor, solid solution S
In order to ensure this, it is essential to reduce the Mn content and prevent the formation of MnS. Specifically, Mn/S
≦2.1 is an essential requirement. As is widely known, solid solution S has a very negative effect on the toughness of materials. Therefore, in the case of unidirectional electrical steel sheets that have a high Si content and are easily cracked, it is extremely difficult in industrial production to cold-roll the material in a state where such solid solution S is present.
前述のように、低コストで、高い磁束密度を有し、将来
、低鐵損の可能性の高い高Ｓｉ、薄手製品の製造を可能
ならしめるためには、インヒビター設計を再構築する必
要がある。さらに、安定して磁束密度の高い製品を得る
ためには、製造条件による不安定性を除く必要がある。As mentioned above, the inhibitor design needs to be restructured in order to make it possible to manufacture high-Si, thin products with low cost, high magnetic flux density, and a high possibility of low iron loss in the future. . Furthermore, in order to obtain a product with a stable high magnetic flux density, it is necessary to eliminate instability caused by manufacturing conditions.
即ち、１つの製造条件、たとえば冷延圧下率を指定した
とき、高いＧｔｉ束密度を有する製品を得るための他の
条件、たとえば熱延板焼鈍における冷却条件、脱炭焼鈍
温度等の条件の許容範囲が狭くなることは、電磁鋼板の
製造上不利でありまた、歩留りの低下にも結び付く。こ
れらの条件の許容範囲を広くするＣとが、安定した工業
生産のためには重要である。That is, when one manufacturing condition, for example, the cold rolling reduction ratio, is specified, other conditions, such as cooling conditions in hot-rolled plate annealing, decarburization annealing temperature, etc., are allowed in order to obtain a product with a high Gti bundle density. A narrow range is disadvantageous in manufacturing electrical steel sheets and also leads to a decrease in yield. C, which widens the allowable range of these conditions, is important for stable industrial production.
本発明は、これらの問題を解決することを、発明におけ
る技術的課題としている。The technical objective of the present invention is to solve these problems.
本発明の特徴とする処は、重量で、Ｓｉ ：１．５〜
４．８％、酸可溶性Ａβ： ０．０１２〜０．０５０％
、５またはＳｅの１種又は２種を合計量で０．０１２％
以下、Ｎ ： ０．００１０〜０．０１２０％、Ｍｎ
／ （Ｓ ＋ Ｓｅ）≧４．０、Ｂ ： ０．０００５
〜０．００８０％、残部二Ｆｅおよび不可避的不純物か
らなるスラブを、熱間圧延し、１回または、中間焼鈍を
挟む２回以上の冷間圧延工程によって最終板厚とし、次
いで、湿水素雰囲気中で脱炭焼鈍し、焼鈍分離剤を塗布
した後二次再結晶と鋼の純化を目的とする仕上焼鈍を行
い、さらに、最終冷延後から仕上焼鈍における二次再結
晶開始までの間に鋼板の窒化処理を行うことを特徴とす
る磁束密度の高い一方向性電磁鋼板の製造方法にあり、
更に、前記スラブを熱間圧延前に１２００℃未満の温度
に加熱すること、及び最終板厚を０．１０〜０．２３＋
＋ｎに特定するところに特徴を有する。The feature of the present invention is that Si: 1.5 to 1.5 by weight.
4.8%, acid soluble Aβ: 0.012-0.050%
, 5 or one or two of Se in a total amount of 0.012%
Hereinafter, N: 0.0010 to 0.0120%, Mn
/ (S + Se)≧4.0, B: 0.0005
A slab consisting of ~0.0080%, balance di-Fe and unavoidable impurities is hot rolled, subjected to one or two or more cold rolling steps with intermediate annealing to achieve the final thickness, and then rolled in a wet hydrogen atmosphere. The steel is decarburized and annealed in the steel, after which an annealing separator is applied, followed by secondary recrystallization and finish annealing for the purpose of purifying the steel. A method for manufacturing a unidirectional electrical steel sheet with high magnetic flux density, characterized by performing nitriding treatment on the steel sheet,
Further, heating the slab to a temperature below 1200°C before hot rolling, and a final thickness of 0.10 to 0.23+
+n.
以下に、本発明の詳細な説明する。The present invention will be explained in detail below.
本発明者等は、溶鋼中のＳを一定量以下に少なくしかつ
、固溶Ｓを少なくする条件下で、適当量のＡ７！とＮお
よびＢを含有せしめた素材を、熱間圧延して熱延板とし
た後、１回または２回の冷間圧延工程で最終板厚とする
プロセスとするとともに、最終冷延から仕上焼鈍におけ
る二次再結晶開始までの間に鋼板の窒化処理を行うよう
にすることにより、広い冷延圧下率範囲に互り安定して
磁束密度の高い電磁鋼板を製造することに成功した。The present inventors have determined that an appropriate amount of A7! under the conditions of reducing S in molten steel to below a certain amount and reducing solid solution S! After hot-rolling a material containing N and B to form a hot-rolled plate, the final thickness is obtained through one or two cold rolling steps, and the process includes final cold rolling and final annealing. By performing the nitriding treatment on the steel sheet before the start of secondary recrystallization, we succeeded in producing an electrical steel sheet with stable high magnetic flux density over a wide range of cold rolling reductions.
次に、本発明を特徴づける構成要件について説明する。Next, the constituent elements characterizing the present invention will be explained.
Ｓｉ含有量が過度に多くなると、製品（ストリップ）の
長さ方向に線状の二次再結晶不良が多発し、安定した生
産を不可能にする。この傾向は、特にＳｉ含有量が３．
２％を超える高Ｓｉ範囲でまた、最終板厚が０．２３＋
＋ｍ （９ｍ１ｄ）以下の薄手製品において顕著となる
。このような問題をよりよく解決するための要件の１つ
としてＳ＋Ｓｅの含有量を規定しなければならない。If the Si content is excessively high, linear secondary recrystallization defects occur frequently in the length direction of the product (strip), making stable production impossible. This tendency is particularly observed when the Si content is 3.
In the high Si range above 2%, the final plate thickness is 0.23+
This is noticeable in thin products of +m (9m1d) or less. In order to better solve such problems, the content of S+Se must be defined as one of the requirements.
即ち、線状の二次再結晶不良部が全く発生しないように
するためには、Ｓ＋Ｓｅ量上限値上限値０１２％としな
ければならない。この限定範囲内にあっても、可及的に
低Ｓ＋Ｓｅとする方がよい。本発明のプロセスにおいて
は、従来、有効であるとされていたＳまたはＳｅ含有量
ではむしろ磁束密度は劣化し、ＳまたはＳｅ含有量が少
ないものほど良好な磁束密度を有する製品を得ることが
できる。That is, in order to prevent the occurrence of linear secondary recrystallization defects at all, the upper limit value of the amount of S+Se must be set to 012%. Even within this limited range, it is better to keep S+Se as low as possible. In the process of the present invention, the magnetic flux density deteriorates with the S or Se content, which was conventionally considered to be effective, and it is possible to obtain a product with a better magnetic flux density as the S or Se content is lower. .
しかしながら、現在の工業的な電磁鋼溶製技術でコスト
を過度に高くすることなく低くし得るＳ含有量は、重量
で、０．０００５％か一般的である。However, the S content, which can be reduced without excessively increasing the cost using current industrial electromagnetic steel melting technology, is generally 0.0005% by weight.
一方、本発明においては、製造コストを低くずべく、熱
間圧延および冷間圧延過程で材料の割れを皆無にするこ
とを狙っており、固溶Ｓによる材料の靭性劣化に起因す
る材料の割れを防くために、Ｍｎ ／ （Ｓ ＋ Ｓｅ
）≧４として鋼中に存在する微量のＳ 、Ｓｅを可及的
にＭｎＳ 、ＭｎＳｅとして固着するようにしている
。On the other hand, the present invention aims to completely eliminate material cracking during hot rolling and cold rolling processes in order to reduce manufacturing costs. In order to prevent
)≧4, so that trace amounts of S and Se present in the steel are fixed as MnS and MnSe as much as possible.
第１図に、Ｃ： ０．０５３％、Ｓｉ：３．３５％、Ｐ
；０．０３０％、Ａｌ：ｏ、０３０％、Ｎ ： ０．０
０７５％、Ｂ；０．００３９％、を含有し、さらに、Ｍ
ｎ：０．４％および０．１２％を含む溶鋼にＳ含有量を
変化させた５０ｋｇインゴットを１３６０℃および１１
５０’Ｃに加熱し、熱間圧延して得られた熱延板端部の
割れの状況を示す。Ｍｎ／Ｓ≧４で急激に割れが減少し
、特にＭｎＳを固溶させない１１５０℃の低い加熱温度
とじた材料は、殆ど割れか発生していない。In Figure 1, C: 0.053%, Si: 3.35%, P
;0.030%, Al: o, 030%, N: 0.0
075%, B; 0.0039%, and further contains M
50 kg ingots with varying S contents were heated to 1360°C and 11% to molten steel containing n: 0.4% and 0.12%.
The state of cracking at the end of a hot rolled sheet obtained by heating to 50'C and hot rolling is shown. When Mn/S≧4, the number of cracks decreases rapidly, and in particular, the material heated at a low heating temperature of 1150° C., which does not dissolve MnS, has almost no cracks.
また、Ｍｎの含有量は、Ｓ含有量との関係において、上
述の如く、Ｍｎ ／ （Ｓ ＋ Ｓｅ）≧４．０で、熱
延板の耳割れを防止するという観点からは十分であるが
、Ｍｎ含有量の上限は、０．４５％が好ましい。０．４
５％を超えると、製品にフォルステライト皮膜欠陥か出
る。Furthermore, in relation to the S content, the Mn content is Mn/(S + Se)≧4.0, which is sufficient from the viewpoint of preventing edge cracking in the hot rolled sheet, as described above. , the upper limit of the Mn content is preferably 0.45%. 0.4
If it exceeds 5%, forsterite film defects will appear in the product.
次に、Ｂの添加効果について説明する。Next, the effect of adding B will be explained.
Ｃ： ０．０５３％、Ｓｉ ： ３．２７％、Ｍ ｎ
： ０．１５％、Ｓ ： ０．００７％、Ｐ ： ０．
０２５％、Ａｉ ： ０．０２７％、Ｎ ： ０．００
８０％、Ｂ ： ０．０００２％および０．００９５％
、残部二Ｆｅおよび不可避的不純物からなる５０ｋｇイ
ンゴットを、１１５０℃に加熱した後熱間圧延して２．
０鶴の熱延板とした。次いで、１１２０°ｃｘ３分間の
熱延板焼鈍を施した後０．２ ｍｍの最終板厚に冷間圧
延し、８１０℃８８３０’Ｃ１８５０℃１８７０℃１８
９０℃８９１０℃の各温度で脱炭焼鈍を施した後、窒化
フェロマンガンを含有し向０を主成分とする焼鈍分離剤
を塗布した後仕上焼鈍を施した。その結果を、第２図に
示す。C: 0.053%, Si: 3.27%, Mn
: 0.15%, S: 0.007%, P: 0.
025%, Ai: 0.027%, N: 0.00
80%, B: 0.0002% and 0.0095%
, a 50 kg ingot consisting of the remainder Fe and unavoidable impurities was heated to 1150° C. and then hot rolled.
It was made into a hot rolled sheet of 0 Tsuru. Next, the hot-rolled plate was annealed at 1120°C for 3 minutes, and then cold-rolled to a final thickness of 0.2 mm.
After performing decarburization annealing at various temperatures of 90° C. and 8910° C., a post-finish annealing was performed by applying an annealing separator containing ferromanganese nitride and having orientation 0 as a main component. The results are shown in FIG.
第２図から明らかな如く、脱炭焼鈍温度を高くすると製
品の磁束密度は高くなるけれども、Ｓ含有量の少ないも
のは、細粒が発生し易くかつＢｅの最高値が低い。As is clear from FIG. 2, when the decarburization annealing temperature is increased, the magnetic flux density of the product increases, but products with a low S content tend to generate fine grains and have a low maximum Be value.
一方、Ｓ含有量が多過ぎると、脱炭焼鈍温度によっては
高いＢＢ値の製品が得られない。Ｓ含有量の適正な範囲
は、０．０００５〜０．００８０％である。On the other hand, if the S content is too high, a product with a high BB value cannot be obtained depending on the decarburization annealing temperature. The appropriate range of S content is 0.0005 to 0.0080%.
このＢの効果は、Ｎが適当量台まれる場合に意味がある
。恐らく、ＢＮとして効果を持つと考えられる。Ｎ ＜
０．００１％では効果がなく、Ｎ ＞Ｏ，Ｏ］、２０
％ではブリスターと呼ばれる鋼板の脹れが発生ずる。This effect of B becomes meaningful when N is reduced by an appropriate amount. It is thought that it is probably effective as a BN. N<
There is no effect at 0.001%, N > O, O], 20
%, swelling of the steel plate called blister occurs.
次に、八〇はＮと結合して八ＥＮとなるが、本発明にお
いては、後工程即ち最終冷間圧延以降の工程で鋼を窒化
することによりＡｆｆを含む化合物を形成せしめること
を必須としているから、フリーのＡＰが一定量以上必要
である。そのためには、０．０１２〜０．０５０％必要
である。Next, 80 is combined with N to become 8EN, but in the present invention, it is essential to form a compound containing Aff by nitriding the steel in a subsequent process, that is, a process after final cold rolling. Therefore, a certain amount or more of free AP is required. For that purpose, 0.012 to 0.050% is required.
スラブ加熱温度については、従来技術におけるように、
インヒビターを固溶させる高温スラブ加熱でもまた、従
来、無理であると考えられていた普通銅皿の低温スラブ
加熱でも二次再結晶は生しる。しかしながら、第１図に
示すように、熱延板の側縁部の割れを少なくできること
、スラブ加熱のためのエネルギ消費量を少なくするごと
ができること、ノロ（鋼滓）の発生がなく炉の補修の頻
度、程度を著しく軽減できること等の理由から、１２０
０℃以下の低温スラブ加熱が好ましい。Regarding the slab heating temperature, as in the prior art,
Secondary recrystallization occurs both in high-temperature slab heating to dissolve the inhibitor, and in low-temperature slab heating in an ordinary copper pan, which was previously thought to be impossible. However, as shown in Figure 1, it is possible to reduce cracks on the side edges of hot-rolled sheets, reduce energy consumption for slab heating, and repair furnaces without generating slag (steel slag). 120 because it can significantly reduce the frequency and severity of
Low-temperature slab heating of 0° C. or lower is preferred.
冷間圧延に際しては、最も高い磁束密度を有する製品を
得るために、短時間の熱延板焼鈍を材料に施す。磁気特
性が若干劣ることを我慢するならば、コストを低下せし
めるべく、熱延板焼鈍を省略することもできる。During cold rolling, the material is subjected to a short hot-roll annealing to obtain a product with the highest magnetic flux density. If a slight deterioration in magnetic properties is tolerated, hot-rolled sheet annealing can be omitted in order to reduce costs.
また、最終製品の結晶粒を小さくするために、中間焼鈍
を挟む２回以上の冷間圧延工程を採ることもできる。Further, in order to reduce the crystal grain size of the final product, two or more cold rolling steps with intermediate annealing may be performed.
また、第３の発明において最終板厚を０．１０〜０．２
３１１としたのは、次の理由による。たとえば、特開昭
５７−４１３２６号公報に開示されているように、板厚
を減少させると、渦流損か減少するけれども、ヒステリ
シス損は増大し、両者の妥協点として鉄損の低い特定板
厚範囲が存在する。０．１０〜０．２３ｍｍの範囲であ
る。Further, in the third invention, the final plate thickness is 0.10 to 0.2
The reason for choosing 311 is as follows. For example, as disclosed in Japanese Patent Application Laid-Open No. 57-41326, when the plate thickness is reduced, the eddy current loss decreases, but the hysteresis loss increases. A range exists. It is in the range of 0.10 to 0.23 mm.
本発明では、二次再結晶が安定し高い磁束密度を有する
製品が得られる冷間圧延圧下率範囲が、高い圧下率側ま
で許容できるから、このような薄手の製品を製造するに
際し、極めて有利である。In the present invention, the cold rolling reduction range in which products with stable secondary recrystallization and high magnetic flux density can be obtained can be tolerated up to the high reduction ratio side, so it is extremely advantageous when manufacturing such thin products. It is.
例えば、板厚０．１５ｍｍの薄手高磁束密度の製品を低
コストの一回冷延で得るためには、Ｂ無添加材でハ板厚
１．５ｍｍの熱延板が必要となる。しがし、工業生産規
模で１．５鶴厚までの熱延を行なうことは、生産性の低
下、制御の困難さから極めて不利である。For example, in order to obtain a thin product with a thickness of 0.15 mm and a high magnetic flux density by a single low-cost cold rolling process, a hot-rolled sheet with a thickness of 1.5 mm made of B-free material is required. However, hot rolling to a thickness of up to 1.5 mm on an industrial production scale is extremely disadvantageous due to decreased productivity and difficulty in control.
実施例３から明らかなようにＢ添加材では最終冷延率９
３％の製品まで、高い磁束密度が得られるから、板厚２
．０＋ｎの熱延板からでも高磁束密度が一回冷延で得ら
れ安定した工業生産を行なう上で有利である。As is clear from Example 3, the final cold rolling rate of the B additive material was 9.
High magnetic flux density can be obtained for products with a thickness of up to 3%.
．． Even from a 0+n hot-rolled sheet, a high magnetic flux density can be obtained in one cold rolling process, which is advantageous for stable industrial production.
最終冷延後の材料は、湿水素或は湿水素、窒素混合雰囲
気ガス中で脱炭焼鈍される。The material after the final cold rolling is decarburized and annealed in wet hydrogen or a mixed atmosphere of wet hydrogen and nitrogen.
このときの温度は、特に拘らないが、８００〜９００℃
の範囲内が好ましい。また、そのときの雰囲気の露点は
、水素、窒素の混合比によるが、＋３０℃以上とするこ
とが望ましい。The temperature at this time is not particularly limited, but is 800 to 900°C.
It is preferably within the range of . Further, the dew point of the atmosphere at that time depends on the mixture ratio of hydrogen and nitrogen, but is preferably +30° C. or higher.
次いで、焼鈍分離剤を塗布し、高温（通常１１００〜１
２００℃）長時間の仕上焼鈍を行う。本発明においては
、最終冷間圧延以降仕上焼鈍での二次再結晶発現前まで
の過程で鋼を窒化することにより二次再結晶に必要なイ
ンヒビターを作り込む点に特徴がある。その際、最も好
ましい実施態様は、仕上焼鈍の昇温過程で鋼を窒化する
方法である。これを達成するために、焼鈍分離剤中に窒
化能のある化合物、たとえば、ＭｎＮ 、 ＣｒＮ等を
適当量添加するか或ばＮ１１３等窒化能のある気体を雰
囲気ガス中に添加する必要がある。Next, an annealing separator is applied and heated to a high temperature (usually 1100 to 1
(200°C) long-term final annealing. The present invention is characterized in that an inhibitor necessary for secondary recrystallization is created by nitriding the steel during the process after the final cold rolling until the onset of secondary recrystallization in final annealing. In this case, the most preferred embodiment is a method in which the steel is nitrided during the temperature raising process of final annealing. In order to achieve this, it is necessary to add an appropriate amount of a compound capable of nitriding, such as MnN, CrN, etc., to the annealing separator, or to add a gas capable of nitriding, such as N113, to the atmospheric gas.
その他の実施態様として、脱炭焼鈍工程の均熱過程以降
において、ＮＨ３等窒化能のあるガスを含有するガスを
雰囲気として鋼板（ストリップ）を処理するか或は脱炭
焼鈍後、Ｎト１３等窒化能のあるガスを含有するガスを
雰囲気とする熱処理炉で鋼板を窒化する方法がある。As another embodiment, after the soaking process of the decarburization annealing process, the steel plate (strip) is treated in an atmosphere containing a gas with nitriding ability such as NH3, or after decarburization annealing, the steel plate (strip) is treated with a gas containing a gas with nitriding ability such as NH3, or after decarburization annealing, There is a method of nitriding a steel plate in a heat treatment furnace in which the atmosphere is a gas containing a gas capable of nitriding.
また、上に述べた方法を組合せて実施してもよい。Moreover, the methods described above may be combined and implemented.
二次再結晶を完了した鋼板は、水素雰囲気中で純化焼鈍
される。The steel plate that has undergone secondary recrystallization is subjected to purification annealing in a hydrogen atmosphere.
実施例１
重量％で、Ｃ： ０．０５５％、Ｓｉ ：３．５０％
、Ｐ：０．０３１％、Ａｆｉ ：０．０２６％、Ｎ ：
０．００７７％、Ｂ：（ａ）０．０００３％、（ｂ）
０．００１５％、（ｃ）０．００６０％、および、（ｄ
）０．０１００％を含有した溶鋼を鋳造したスラブを１
１９５℃に加熱後、熱延し、２．３ｍｍの熱延板を得た
。次いで１１５０℃×１分間の熱延板焼鈍を施した後０
．２３１１の板厚に冷延し、８３０℃で２分間、湿水素
窒素混合気中で脱炭焼鈍をした。この時の雰囲気露点は
５５℃であった。更に、窒化フェロマンガンを重量で４
％添加した触０からなる焼鈍分離剤を塗布し、１０℃／
ｈｒの昇温速度で１２００℃に加熱し、２０時間保持す
る仕上焼鈍を施した。Example 1 In weight%, C: 0.055%, Si: 3.50%
, P: 0.031%, Afi: 0.026%, N:
0.0077%, B: (a) 0.0003%, (b)
0.0015%, (c) 0.0060%, and (d
) A slab made of molten steel containing 0.0100%
After heating to 195° C., hot rolling was performed to obtain a 2.3 mm hot rolled sheet. Then, after hot-rolled plate annealing at 1150°C for 1 minute,
．． It was cold rolled to a thickness of 2311 mm and decarburized annealed at 830° C. for 2 minutes in a wet hydrogen/nitrogen mixture. The atmospheric dew point at this time was 55°C. Furthermore, 4 ferromanganese nitride by weight
Apply an annealing separator consisting of 0% additive and heat at 10℃/
Finish annealing was performed by heating to 1200° C. at a heating rate of hr and holding it for 20 hours.
この時の雰囲気は、１２００℃までの昇温過程ではＮ２
ニア５％、Ｎ２：２５％１２００℃の保定中は、Ｎ２：
１００％とした。The atmosphere at this time was N2 during the heating process up to 1200℃.
Near 5%, N2: 25% During retention at 1200℃, N2:
It was set as 100%.
得られた製品の磁束密度は次の通りであった。The magnetic flux density of the obtained product was as follows.
この結果から明らかに、適正なりの成分範囲が存在する
。From this result, it is clear that there is an appropriate range of ingredients.
実施例２
重量で、Ｃ： ０．０５０％、Ｓ ｉ ： ３．３０
％、Ｍｎ：０．１５０％、Ｐ：０．０２５％、Ｓ：０．
００６％、Ａβ−０，０２８％、Ｎ ： ０．００７５
％、Ｃｒ ：０．１２０％、残部：Ｆｅおよび不可避
的不純物からなる電磁鋼スラブ（Ａ）と、前記成分系に
Ｂを０．００３０％添力ｕした電磁鋼スラブｌ）を、１
１５０℃に加熱した後、熱間圧延してそれぞれ板厚１．
６．２．０．２．５．２．８ 。Example 2 By weight, C: 0.050%, Si: 3.30
%, Mn: 0.150%, P: 0.025%, S: 0.
006%, Aβ-0,028%, N: 0.0075
%, Cr: 0.120%, balance: Fe and unavoidable impurities (A), and an electromagnetic steel slab l) with 0.0030% B added to the above component system, 1
After heating to 150°C, hot rolling was performed to give each plate a thickness of 1.
6.2.0.2.5.2.8.
３．５＋＋ｍの熱延板を得た。A hot rolled sheet of 3.5++ m was obtained.
これらに、１１２０°ｃｘ２分間の焼鈍を施し、１回の
冷間圧延で板厚０．２９ｍｍの最終板厚とした。次いで
、８５０℃Ｘ１５０秒間の脱炭焼鈍を、露点＋６０℃の
湿水素窒素混合ガス中で施した後、）ＩｇＯ中にＴｌＯ
２：３重量％とフェロ窒化マンガン：５重量％を添加し
た焼鈍分離剤を塗布した。These were annealed at 1120°c for 2 minutes and cold rolled once to give a final plate thickness of 0.29 mm. Next, decarburization annealing was performed at 850°C for 150 seconds in a wet hydrogen-nitrogen mixed gas with a dew point of +60°C.
An annealing separator containing 2:3% by weight and ferromanganese nitride: 5% by weight was applied.
この材料に、１０℃／ｈｒの昇温速度で１２００℃に加
熱し、２０時間保持する仕上焼鈍を施した。このときの
雰囲気は、昇温中はＮｚ：２５％、Ｎ２・ニア５％の混
合ガス、１２００℃に保定中はＮ２ ：１００％のガス
であった。This material was subjected to final annealing by heating to 1200° C. at a heating rate of 10° C./hr and holding it for 20 hours. The atmosphere at this time was a mixed gas of 25% Nz and 5% N2.Nia during the temperature rise, and a 100% N2 gas while the temperature was maintained at 1200°C.
このときの結果を、第３図に示す。The results at this time are shown in FIG.
第３図から明らかな如く、材料（Ａ）では、熱延板の厚
さ２．５．２．８ｍｍのもののみが高磁束密度を示した
のに対し、材料ＣＢ）では、熱延板の厚さ２．０ 、２
．５ 、２．８ 、３．５顛のもので高磁束密度を示し
、冷延時の圧下率を変動させても製品の磁気特性が高い
水準で安定している。As is clear from Fig. 3, in material (A), only the hot-rolled sheets with a thickness of 2.5 and 2.8 mm showed high magnetic flux density, whereas in material CB), the hot-rolled sheets with a thickness of 2.5 and 2.8 mm showed high magnetic flux density. Thickness 2.0, 2
．． 5, 2.8, and 3.5 sizes exhibit high magnetic flux densities, and the magnetic properties of the products remain stable at a high level even when the rolling reduction during cold rolling is varied.
実施例３
実施例２におけると同一の成分系および厚さの熱延板を
得、これらに１１２０’ｃ ｘ ２分間の焼鈍を施した
後、１回の冷間圧延で０．２（ｂｍ厚さの最終板厚とし
た。Example 3 Hot-rolled sheets with the same composition and thickness as those in Example 2 were obtained, and after annealing them at 1120'c x 2 minutes, the thickness was reduced to 0.2 (bm) by one cold rolling. The final plate thickness was taken as the final thickness.
この材料に、８５０ ’ＣＸ９０秒間の脱炭焼鈍を、湿
水素、窒素雰囲気中で施し、次いで焼鈍分離剤を塗布し
た後、実施例２におけると同一の条件で仕上焼鈍を施し
た。This material was subjected to decarburization annealing at 850'CX for 90 seconds in a wet hydrogen and nitrogen atmosphere, and then, after applying an annealing separator, final annealing was performed under the same conditions as in Example 2.
その結果を、第４図に示す。The results are shown in FIG.
第４図から明らかな如く、材料（Ａ）では、熱延板の厚
さが１．６．２．Ｏｕ＋のちののみが高い磁束密度を示
したのに対し、材料ＣＢ）では、熱延板の厚さ１．６
、２．０ 、２．５ 、２．８鶴のものについて高い磁
束密度を示した。As is clear from FIG. 4, for material (A), the thickness of the hot rolled sheet is 1.6.2. Only Ou+ later showed a high magnetic flux density, whereas material CB) had a hot-rolled plate thickness of 1.6
, 2.0, 2.5, and 2.8 Tsuru showed high magnetic flux density.
実施例４
Ｃ： ０．０５５％、Ｓ ｉ ： ３．２８％、Ｍｎ
：０．１５％、Ｓ ： ｏ、ｏｏ６％、Ｐ ： ０
．０２５％、Ａβ： ０．０２７％、Ｎ ： ０．００
７７％に、Ｂ ： ０．０００３％と０．００２０％、
を添力１１したスラブを１１５０℃に加熱後、熱間圧延
し、２、６＋ｕの熱延板を得た。スケールを落した後、
１、８ ＊＊まで冷間圧延し、次いで１１００“ＣＸ２
分間の焼鈍を施した。この後酸洗し、０．１５＋＋ｍ厚
に冷延し、８４０℃×７０秒の脱炭焼鈍を行なった。こ
の鋼板に、ＭｇＯ中に、重量で３％のフェロ窒化マンガ
ンを添加した焼鈍分離剤を塗布して、１２００℃まで８
℃／ｈの昇温速度で加熱後２０時間の焼鈍を施した。Example 4 C: 0.055%, Si: 3.28%, Mn
: 0.15%, S: o, oo6%, P: 0
．． 025%, Aβ: 0.027%, N: 0.00
77%, B: 0.0003% and 0.0020%,
After heating the slab with a loading force of 11 to 1150°C, it was hot rolled to obtain a 2,6+u hot rolled plate. After dropping the scale,
Cold rolled to 1,8**, then 1100"CX2
Annealing was performed for 1 minute. Thereafter, it was pickled, cold rolled to a thickness of 0.15++m, and decarburized annealed at 840°C for 70 seconds. This steel plate was coated with an annealing separator containing 3% by weight of ferromanganese nitride in MgO, and then heated to 1200°C.
After heating at a temperature increase rate of °C/h, annealing was performed for 20 hours.
この昇温過程の雰囲気はＮ２５０％とＮ２５０％の混合
カスを使用し、１２００′Ｃの均熱時は１１゜１００％
とした。The atmosphere for this heating process is a mixture of N250% and N250%, and when soaking at 1200'C, the temperature is 11°100%.
And so.
得られた、成品の磁気特性、及び結晶粒径は、以下のと
おりである。The magnetic properties and crystal grain size of the obtained product are as follows.
実施例５
重量％で、Ｃ： ０．０５２％、Ｓ ｉ ： ３．３
０％、Ｍｎ；０．１４％、Ｐ ： ０．０３３％、／Ｍ
！ ：０．０２７％、Ｎ：０．００７５％、Ｂ ： ０
．００２０％残部Ｆｅおよび不可避的不純物からなる溶
鋼にＳを（ａ） ０．００４％、（ｂ）０．０１０％、
（ｃ） ０．０１８％添加して得たスラブを１１９５
℃に加熱後、熱延し２． Ｏ＊＊厚さの熱延板を得た。Example 5 In weight %, C: 0.052%, S i : 3.3
0%, Mn: 0.14%, P: 0.033%, /M
! : 0.027%, N: 0.0075%, B: 0
．． (a) 0.004%, (b) 0.010%,
(c) 1195 slab obtained by adding 0.018%
After heating to ℃, hot rolling 2. A hot rolled sheet having a thickness of O** was obtained.
これに１１２０℃Ｘ２分間＋９００℃Ｘ１分間の熱延板
焼鈍を施し酸洗した後、０．２０ｍ１の板厚まで冷間圧
延した。次いで８５０℃Ｘ１００秒間の脱炭焼鈍を湿水
素中で施し、ｈｇｏに？ＩｎＮを重量％て３％添加した
焼鈍分離剤を塗布した後、１２００℃×２０時間の仕上
焼鈍を施した。この仕上焼鈍の雰囲気ガスは昇温過程で
はＮ２：２５％、Ｈ□ ニア５％の混合ガスであり、１
２００℃の均熱時はＮ２：１００％であった。磁束密度
は下表の通りであった。This was subjected to hot-rolled plate annealing at 1120°C for 2 minutes + 900°C for 1 minute, pickled, and then cold rolled to a plate thickness of 0.20 m1. Next, decarburization annealing was performed at 850°C for 100 seconds in wet hydrogen to give hgo? After applying an annealing separator containing 3% by weight of InN, final annealing was performed at 1200° C. for 20 hours. The atmosphere gas for this final annealing is a mixed gas of 25% N2 and 5% H□ in the temperature rising process.
When soaking at 200°C, N2:100%. The magnetic flux density was as shown in the table below.
実施例６
重量で、Ｃ： ０．０４５％、Ｓ ｉ ： ３．５０
％、Ｍｎ：０．１６％、Ｐ ： ０．０３５％１，１１
：０．０２８％、Ｎ：０．００８０９１０． Ｂ ：
０．００２５％、残部Ｆｅおよび不可避的不純物からな
る溶鋼に、Ｓｅを（ａ） ０．００５０％。Example 6 By weight, C: 0.045%, Si: 3.50
%, Mn: 0.16%, P: 0.035%1,11
:0.028%, N:0.0080910. B:
(a) 0.0050% Se to molten steel consisting of 0.0025%, the balance Fe and unavoidable impurities.
（ｂ） ０．０１００％、 （ｃ） ０．０２００％添
加して得られた鋼スラブをｌｌ５０゛ｃに加熱した後、
熱間圧延し２．０Ｈｊ〃さの熱延板を得た。これに、１
１５０℃×２分間＋９００“ＣＸ２分間の熱延板焼鈍を
施した後急冷し、次いで酸洗した後、０．２０ｍｍの最
終板厚まで冷間圧延した。After heating the steel slab obtained by adding (b) 0.0100% and (c) 0.0200% to 1150゛c,
A hot rolled sheet having a thickness of 2.0 Hj was obtained by hot rolling. To this, 1
The hot rolled sheet was annealed at 150°C for 2 minutes + 900"CX for 2 minutes, then rapidly cooled, then pickled, and then cold rolled to a final thickness of 0.20 mm.
引き続き、８３０℃×９０秒間の脱炭焼鈍を鋼板に施し
、ＭｇＯに、重量で５％のフェロ窒化マンガンを添加し
た焼鈍分離剤を塗布した。Subsequently, the steel plate was subjected to decarburization annealing at 830° C. for 90 seconds, and an annealing separator containing 5% by weight of ferromanganese nitride added to MgO was applied.
次いで、鋼板に、１０℃／ｈｒの昇温速度で１２００℃
に加熱し、２０時間保持する仕」二焼鈍を施した。Next, the steel plate was heated to 1200°C at a heating rate of 10°C/hr.
The material was then annealed by heating it to a temperature and holding it for 20 hours.
このときの雰囲気は、１２００℃までの昇温過程ではＮ
２：２５％、Ｈｚニア５％の混合ガス、１２００’Ｃの
均熱時はＮ２ ：１００％のガスであった。The atmosphere at this time was N during the heating process up to 1200°C.
The mixed gas was 25% N2 and 5% near Hz, and the gas was 100% N2 during soaking at 1200'C.
得られた製品の磁気特性は、次の如くであった。The magnetic properties of the obtained product were as follows.
この結果から明らかな如く、Ｓｅ含有量が多過ぎると、
高磁束密度の製品が得られない。As is clear from this result, if the Se content is too high,
Products with high magnetic flux density cannot be obtained.
実施例７
重量で、Ｃ： ０．０４８％、Ｓ ｉ ： ３．３０
％、Ｍｎ；０．１４５％、Ｓ ： ０．００８％、７Ｂ
：０．０３０％、Ｎ；０、００７５％、Ｂ ： ０．
００２４％、残部Ｆｅおよび不可避的不純物からなるス
ラブを１１００℃で加熱後熱延し、２．３１１厚の熱延
板を得た。Example 7 By weight, C: 0.048%, Si: 3.30
%, Mn; 0.145%, S: 0.008%, 7B
: 0.030%, N: 0,0075%, B: 0.
A slab consisting of 0.024% Fe and unavoidable impurities was heated at 1100° C. and then hot rolled to obtain a hot rolled sheet with a thickness of 2.311 mm.
この熱延板に（１）熱延板焼鈍なし、（２）９００°ｃ
ｘ６分の熱延板焼鈍、（３）１１３０°ｃｘ２分＋９０
０℃×１分の熱延板焼鈍後急冷却を、それぞれ施した。This hot-rolled sheet has (1) no hot-rolled sheet annealing, (2) 900°C
Hot rolled sheet annealing for x6 minutes, (3) 1130°c x 2 minutes +90
The hot rolled sheets were annealed at 0° C. for 1 minute and then rapidly cooled.
これを０．３０ｍｍ厚まで１回で冷延し、８４０℃×１
８０秒の脱炭焼鈍を湿水素、窒素混合気中で行ない、Ｍ
ｇＯに重量で５％のフェロ窒化マンガンを添加した。焼
鈍分離剤を塗布した後、１２００℃×２０時間の仕上焼
鈍を施した。この昇温過程の昇温速度は１５℃／ｈｒで
あり、雰囲気ガスは窒素：２５％、水素；７５％の混合
ガスを用いた。また、１２００℃の均熱時の雰囲気ガス
は水素１００％であった。This was cold-rolled in one step to a thickness of 0.30 mm, and 840℃ x 1
Decarburization annealing was performed for 80 seconds in a wet hydrogen and nitrogen mixture, and M
5% by weight of ferromanganese nitride was added to gO. After applying the annealing separator, final annealing was performed at 1200° C. for 20 hours. The temperature increase rate in this temperature increase process was 15° C./hr, and the atmospheric gas used was a mixed gas of 25% nitrogen and 75% hydrogen. Further, the atmospheric gas during soaking at 1200° C. was 100% hydrogen.
磁気特性は以下のとおりであった。The magnetic properties were as follows.
本発明は、以上述べたように構成しかつ、作用せしめる
ようにしたから、磁気特性の極めて優れた一方向性電磁
鋼板を−採り得る冷延圧下率範囲等、製造条件の自由度
を大きくし得るから安定した生産を可能にする格別の効
果を奏する。Since the present invention is constructed and operated as described above, the degree of freedom in manufacturing conditions such as the range of cold rolling reduction in which grain-oriented electrical steel sheets with extremely excellent magnetic properties can be obtained is increased. It has an exceptional effect in making stable production possible.
第１図は、Ｍｎ／Ｓと熱延板端部割れ深さの関係を示す
図、
第２図は、Ｂ添加量と脱炭焼鈍温度の関係が、製品の磁
束密度（ＢＩｌ）に及ぼす影響を示す図、第３図は、Ｂ
を添加しない方向性電磁鋼素材（Ａ）と、Ｂを０．００
３０％添加した方向性型１鋼素材（Ｂ）について、熱延
板と板厚と製品の磁束密度（Ｂｌｌ（Ｔ））の関係を示
す図、
第４図は、Ｂを添加しない方向性電磁鋼素材・（Ａ）と
、Ｂを０．００３０％添加した方向性電磁鋼素材（Ｂ）
について、最終板厚を０．２（ｂｍとしたときの、熱延
板の厚さ（ゲージ）と製品の磁束密度（Ｂｅ（Ｔ））の
関係を示す図である。
手続補正書（自発）
昭和６３年７り／７日Figure 1 shows the relationship between Mn/S and the depth of cracking at the end of a hot rolled sheet. Figure 2 shows the effect of the relationship between B addition amount and decarburization annealing temperature on the magnetic flux density (BIl) of the product. Figure 3 shows B
Grain-oriented electrical steel material (A) with no added B and 0.00 B
Figure 4 shows the relationship between the magnetic flux density (Bll(T)) of the hot-rolled plate, plate thickness, and product for the grain-oriented type 1 steel material (B) with 30% additive. Steel material (A) and grain-oriented electrical steel material (B) with 0.0030% B added
This is a diagram showing the relationship between the thickness (gauge) of the hot-rolled sheet and the magnetic flux density (Be(T)) of the product, when the final sheet thickness is 0.2 (bm). Procedural amendment (voluntary) July 7th, 1985
Claims (1)
０．０１２〜０．０５０％、ＳまたはＳｅの１種又は２
種を合計量で０．０１２％以下、Ｎ：０．００１０〜０
．０１２０％、Ｍｎ／（Ｓ＋Ｓｅ）≧４．０、Ｂ：０．
０００５〜０．００８０％、残部：Ｆｅおよび不可避的
不純物からなるスラブを、熱間圧延し、１回または、中
間焼鈍を挟む２回以上の冷間圧延工程によって最終板厚
とし、次いで、湿水素雰囲気中で脱炭焼鈍し、焼鈍分離
剤を塗布した後二次再結晶と鋼の純化を目的とする仕上
焼鈍を行い、さらに、最終冷延後から仕上焼鈍における
二次再結晶開始までの間に鋼板の窒化処理を行うことを
特徴とする磁束密度の高い一方向性電磁鋼板の製造方法
。 ２）重量で、Ｓｉ：１．５〜４．８％、酸可溶性Ａｌ：
０．０１２〜０．０５０％、ＳまたはＳｅの１種又は２
種を合計量で０．０１２％以下、Ｎ：０．００１０〜０
．０１２０％、Ｍｎ／（Ｓ＋Ｓｅ）≧４．０、Ｂ：０．
０００５〜０．００８０％、残部：Ｆｅおよび不可避的
不純物からなるスラブを、１２００℃未満の温度に加熱
した後熱間圧延し、１回または、中間焼鈍を挟む２回以
上の冷間圧延工程によって最終板厚とし、次いで、湿水
素雰囲気中で脱炭焼鈍し、焼鈍分離剤を塗布した後二次
再結晶と鋼の純化を目的とする仕上焼鈍を行い、さらに
、最終冷延後から仕上焼鈍における二次再結晶開始まで
の間に鋼板の窒化処理を行うことを特徴とする磁束密度
の高い一方向性電磁鋼板の製造方法。 ３）最終板厚が０．１０〜０．２３ｍｍである、請求項
１又は２記載の方法。[Claims] 1) By weight, Si: 1.5 to 4.8%, acid-soluble Al:
0.012-0.050%, one or two of S or Se
Total amount of seeds is 0.012% or less, N: 0.0010-0
．． 0120%, Mn/(S+Se)≧4.0, B:0.
A slab consisting of 0.0005% to 0.0080%, balance: Fe and unavoidable impurities is hot rolled, subjected to one cold rolling process or two or more cold rolling steps with intermediate annealing in between, to obtain a final thickness, and then subjected to wet hydrogen treatment. After decarburization annealing in an atmosphere and applying an annealing separator, secondary recrystallization and finish annealing are performed for the purpose of purifying the steel, and then from the final cold rolling to the start of secondary recrystallization in finish annealing. A method for producing a unidirectional electrical steel sheet with high magnetic flux density, characterized by subjecting the steel sheet to nitriding treatment. 2) By weight, Si: 1.5-4.8%, acid-soluble Al:
0.012-0.050%, one or two of S or Se
Total amount of seeds is 0.012% or less, N: 0.0010-0
．． 0120%, Mn/(S+Se)≧4.0, B:0.
A slab consisting of 0005 to 0.0080%, balance: Fe and unavoidable impurities is heated to a temperature of less than 1200°C, then hot rolled, and then subjected to one cold rolling process or two or more cold rolling steps with intermediate annealing in between. After obtaining the final thickness, decarburization annealing is performed in a wet hydrogen atmosphere, and after applying an annealing separator, final annealing is performed for the purpose of secondary recrystallization and purification of the steel.Further, final annealing is performed after the final cold rolling. A method for producing a grain-oriented electrical steel sheet with high magnetic flux density, characterized in that the steel sheet is subjected to nitriding treatment before the start of secondary recrystallization. 3) The method according to claim 1 or 2, wherein the final plate thickness is 0.10 to 0.23 mm.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63112551A JPH0686631B2 (en) | 1988-05-11 | 1988-05-11 | Method for manufacturing unidirectional electrical steel sheet with high magnetic flux density |
| EP88118993A EP0321695B1 (en) | 1987-11-20 | 1988-11-14 | Process for production of grain oriented electrical steel sheet having high flux density |
| DE88118993T DE3882502T2 (en) | 1987-11-20 | 1988-11-14 | Process for the production of grain-oriented electrical steel sheets with high flux density. |
| US07/274,432 US4994120A (en) | 1987-11-20 | 1988-11-18 | Process for production of grain oriented electrical steel sheet having high flux density |
| KR1019880015250A KR930001330B1 (en) | 1987-11-20 | 1988-11-19 | Process for production of grain oriented electrical steel sheet having high flux density |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63112551A JPH0686631B2 (en) | 1988-05-11 | 1988-05-11 | Method for manufacturing unidirectional electrical steel sheet with high magnetic flux density |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01283324A true JPH01283324A (en) | 1989-11-14 |
| JPH0686631B2 JPH0686631B2 (en) | 1994-11-02 |
Family
ID=14589493
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63112551A Expired - Lifetime JPH0686631B2 (en) | 1987-11-20 | 1988-05-11 | Method for manufacturing unidirectional electrical steel sheet with high magnetic flux density |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0686631B2 (en) |
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| US5653821A (en) * | 1993-11-09 | 1997-08-05 | Pohang Iron & Steel Co., Ltd. | Method for manufacturing oriented electrical steel sheet by heating slab at low temperature |
| US6451128B1 (en) | 1997-06-27 | 2002-09-17 | Pohang Iron & Steel Co., Ltd. | Method for manufacturing high magnetic flux denshy grain oriented electrical steel sheet based on low temperature slab heating method |
| KR100345696B1 (en) * | 1997-08-04 | 2002-09-18 | 주식회사 포스코 | A method for manufacturing grain oriented electrical steel sheets by heating its slab at low tempreatures |
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|---|---|
| JPH0686631B2 (en) | 1994-11-02 |
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