JP2001026822A - Silicon steel sheet and its manufacture - Google Patents
Silicon steel sheet and its manufactureInfo
- Publication number
- JP2001026822A JP2001026822A JP11372351A JP37235199A JP2001026822A JP 2001026822 A JP2001026822 A JP 2001026822A JP 11372351 A JP11372351 A JP 11372351A JP 37235199 A JP37235199 A JP 37235199A JP 2001026822 A JP2001026822 A JP 2001026822A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- rolling
- sheet
- silicon steel
- thickness
- 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.)
- Pending
Links
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 60
- 238000000137 annealing Methods 0.000 claims abstract description 46
- 238000005096 rolling process Methods 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 39
- 238000005245 sintering Methods 0.000 claims abstract description 34
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 33
- 239000000956 alloy Substances 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 29
- 238000005097 cold rolling Methods 0.000 claims abstract description 28
- 238000009703 powder rolling Methods 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000009792 diffusion process Methods 0.000 claims description 38
- 229910000676 Si alloy Inorganic materials 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 229910017082 Fe-Si Inorganic materials 0.000 abstract description 12
- 229910017133 Fe—Si Inorganic materials 0.000 abstract description 12
- 229910052710 silicon Inorganic materials 0.000 abstract description 7
- 238000004663 powder metallurgy Methods 0.000 abstract description 3
- 239000011369 resultant mixture Substances 0.000 abstract 2
- 238000007493 shaping process Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 21
- 230000008569 process Effects 0.000 description 16
- 239000000463 material Substances 0.000 description 9
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 229910018619 Si-Fe Inorganic materials 0.000 description 3
- 229910008289 Si—Fe Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000000573 anti-seizure effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 150000001728 carbonyl compounds Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229940087654 iron carbonyl Drugs 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005475 siliconizing Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
- Soft Magnetic Materials (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、珪素鋼板の製造方
法に関する。本発明により、従来技術では製造が困難と
されていた、Ｓｉ含有量５．０％以上の高い珪素含有量
をもつ珪素鋼板が容易に提供できる。[0001] The present invention relates to a method for manufacturing a silicon steel sheet. According to the present invention, it is possible to easily provide a silicon steel sheet having a high silicon content of 5.0% or more, which has been difficult to manufacture in the related art.
【０００２】[0002]
【従来の技術】変圧器の鉄心のような電磁気材料として
の珪素鋼板にとって好適な組成としては、よく知られて
いるように、６．５％Ｓｉ−Ｆｅ（磁歪がゼロ）があ
る。一方で、最近の電子・電気機器の小型化・高効率化
および高周波化の傾向から、高磁束密度で高周波特性の
すぐれた電磁材料が要求されるようになってきた。その
ような要求を満たし得る特性をもつ材料として、Ｓｉ：
１１．５％を含有量の上限とする珪素鋼板がある。とこ
ろが、Ｆｅ−Ｓｉ系においては、Ｓｉ含有量が高くなる
につれて合金の加工性が悪くなり、４．５％を超えると
冷間圧延が不可能になる。2. Description of the Related Art As a well-known composition, 6.5% Si--Fe (zero magnetostriction) is a well-known composition for a silicon steel sheet as an electromagnetic material such as an iron core of a transformer. On the other hand, with the recent trend of miniaturization, high efficiency, and high frequency of electronic and electric devices, an electromagnetic material having high magnetic flux density and excellent high frequency characteristics has been required. As a material having characteristics capable of satisfying such requirements, Si:
There is a silicon steel sheet in which the upper limit of the content is 11.5%. However, in the Fe-Si system, as the Si content increases, the workability of the alloy deteriorates, and when it exceeds 4.5%, cold rolling becomes impossible.
【０００３】そこで、在来の溶製−圧延法によるとき
は、圧延可能な範囲の合金組成を選択するが、どうして
もこの限界を超えようとする努力の現われとして、いわ
ゆる浸珪法が提案された。これは、加工性のよい合金、
たとえばＦｅ−３％Ｓｉ合金を圧延して薄板をつくり、
ＳｉＣｌ4を使用したＣＶＤ法により表面のＳｉ量を高
め、続く加熱によってＳｉを拡散させ、全体のＳｉ量を
６．５％近辺にする方法である。この技術は、有毒なガ
スを使用するため、設備上ガス漏洩対策が必要であり、
十分な事故対策を前提とするには、設備・操業の両面に
おいて、コスト高を免れない。[0003] Therefore, when the conventional smelting-rolling method is used, an alloy composition within a range that can be rolled is selected, but as a manifestation of efforts to exceed this limit, the so-called siliconizing method has been proposed. . This is an alloy with good workability,
For example, rolling a Fe-3% Si alloy to make a thin plate,
In this method, the amount of Si on the surface is increased by a CVD method using SiCl 4, and Si is diffused by subsequent heating to make the total amount of Si approximately 6.5%. Since this technology uses toxic gas, it is necessary to take measures against gas leakage on the equipment,
Assuming sufficient accident countermeasures, high costs are inevitable in both facilities and operations.
【０００４】別の方法として、粉末冶金法による高いＳ
ｉ量の実現が試みられている。しかし、この方法によっ
ても、得られた板材が高珪素含有量のため加工性が低
く、冷間圧延が困難であって任意の厚さの薄板を得るこ
とができない点で、やはり限界がある。[0004] Alternatively, high S by powder metallurgy is used.
Attempts have been made to realize the i quantity. However, even with this method, there is still a limitation in that the obtained sheet material has low workability due to a high silicon content, and is difficult to be cold-rolled to obtain a thin sheet having an arbitrary thickness.
【０００５】これ以外の競合プロセスとしては、まず、
Ｆｅ−Ｓｉ合金の微粉末を適宜のバインダーと混練し、
混練物をドクターブレードで一定の厚さにしたものを圧
延する技術がある。このプロセスは、とくに微細な粉末
を必要とすることと、バインダーを用いることとから、
コストがかかる。バインダーは工程の途中で除去しなけ
ればならず、除去には長時間を要する。その上、焼結を
高温度で行なわなければならないなどの制約があり、薄
板の量産には不向きなプロセスである。[0005] Other competing processes include:
Knead the fine powder of the Fe-Si alloy with an appropriate binder,
There is a technique of rolling a kneaded product having a certain thickness with a doctor blade. This process requires a particularly fine powder and the use of a binder,
costly. The binder must be removed during the process, and it takes a long time to remove the binder. In addition, there is a restriction that sintering must be performed at a high temperature, and this process is not suitable for mass production of thin plates.
【０００６】粉末圧延を容易にする目的で、加工性のよ
い材料たとえば軟鋼の缶に粉末を入れ、密封して熱間で
加工するという方策もある。加工後に脱キャンする必要
があり、これがコスト高の要因になる。また、熱間加工
後の冷間圧延ができず、そのため、厚さ０．５mm以下の
薄板を製造することはできない。[0006] For the purpose of facilitating powder rolling, there is a method in which powder is put into a material having good workability, for example, a mild steel can, sealed, and hot-worked. It is necessary to decant after the processing, which causes a high cost. In addition, cold rolling after hot working cannot be performed, so that a thin plate having a thickness of 0.5 mm or less cannot be manufactured.
【０００７】[0007]
【発明が解決しようとする課題】本発明の目的は、粉末
冶金法の改良により、高いＳｉ含有量をもった珪素鋼板
を容易に製造する方法を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a method for easily producing a silicon steel sheet having a high Si content by improving a powder metallurgy method.
【０００８】[0008]
【課題を解決するための手段】本発明の珪素鋼板の製造
方法には、基本的な態様とそれを簡略化した態様とがあ
り、基本的な態様は、図１にそのフローチャートを示す
ように、下記の諸工程からなる： Ａ）Ｆｅの粉末と、８〜６５重量％のＳｉを含有するＦ
ｅ−Ｓｉ合金の粉末とを、混合物中のＳｉが５〜１２重
量％を占める割合で混合する粉末混合工程、 Ｂ）この混合物を粉末圧延法により厚さ０．０５〜０．
５mmの薄板に成形する粉末圧延工程、 Ｃ）粉末圧延によって得た薄板を、９５０℃以上１４０
０℃未満の温度で焼結する焼結工程、 Ｄ）焼結した薄板を冷間圧延して、板厚を所定の厚さに
するとともにカサ密度を９８％以上に高める冷間圧延工
程、 Ｅ）冷間圧延後の薄板を１１５０〜１４００℃未満の温
度で、非酸化性雰囲気下に加熱して合金組成を均一化す
る拡散焼鈍工程、および Ｆ）拡散焼鈍をへて合金組成が均一化された薄板に、圧
下率０．５〜５％のスキンパス圧延を行って板厚を所定
の厚さにする仕上圧延工程。The method for manufacturing a silicon steel sheet according to the present invention has a basic mode and a simplified mode. The basic mode is as shown in the flowchart of FIG. A) Fe powder and F containing 8 to 65% by weight of Si
a powder mixing step of mixing the powder of the e-Si alloy with Si in the mixture at a ratio of 5 to 12% by weight, and B) a thickness of 0.05 to 0.
A powder rolling step of forming into a 5 mm thin plate; C) a thin plate obtained by powder rolling
A sintering step of sintering at a temperature lower than 0 ° C., D) a cold rolling step of cold rolling the sintered thin plate to a predetermined thickness and a bulk density of 98% or more; D) a diffusion annealing step of heating the cold-rolled sheet at a temperature of 1150 to less than 1400 ° C. in a non-oxidizing atmosphere to make the alloy composition uniform; and F) Diffusion annealing to make the alloy composition uniform. A finish rolling step of subjecting the thin sheet to skin pass rolling at a rolling reduction of 0.5 to 5% to reduce the sheet thickness to a predetermined thickness.
【０００９】本発明に従う珪素鋼板の製造方法の、簡略
化した態様は、図２にそのフローチャートを示すよう
に、下記の諸工程からなる： Ａ）Ｆｅの粉末と、８〜６５重量％のＳｉを含有するＦ
ｅ−Ｓｉ合金の粉末とを、混合物中のＳｉが５〜１２重
量％を占める割合で混合する粉末混合工程、 Ｂ）この混合物を粉末圧延法により厚さ０．０５〜０．
５mmの薄板に成形する粉末圧延工程、 Ｅ’）粉末圧延によって得た薄板を、１１５０〜１４０
０℃未満の温度で、非酸化性雰囲気下に加熱して、密度
を高めるとともに合金組成を均一化する拡散焼鈍工程、
および Ｆ）拡散焼鈍をへて合金組成が均一化された薄板に、圧
下率０．５〜５％のスキンパス圧延を行なって板厚を所
定の厚さにする仕上圧延工程。A simplified embodiment of the method for manufacturing a silicon steel sheet according to the invention comprises, as shown in the flow chart in FIG. 2, the following steps: A) Fe powder and 8 to 65% by weight of Si. F containing
a powder mixing step of mixing the powder of the e-Si alloy with Si in the mixture at a ratio of 5 to 12% by weight, and B) a thickness of 0.05 to 0.
A powder rolling step of forming into a 5 mm thin plate; E ′) a thin plate obtained by powder rolling is processed into 1150 to 140
A diffusion annealing step of heating at a temperature lower than 0 ° C. in a non-oxidizing atmosphere to increase the density and homogenize the alloy composition;
And F) a finish rolling step of subjecting the thin plate having a uniform alloy composition by diffusion annealing to skin pass rolling at a rolling reduction of 0.5 to 5% to a predetermined thickness.
【００１０】[0010]
【発明の実施の形態】上記の基本的な態様および簡略化
された態様のどちらにも、さまざまな変更態様が可能で
ある。DETAILED DESCRIPTION Various modifications of both the basic and simplified aspects described above are possible.
【００１１】そのひとつの例は、仕上圧延工程（Ｆ）に
続いて、下記の工程を行なうことである： Ｇ）薄板に対しその長手方向に張力を加えつつ焼鈍、い
わゆる「テンションアニ−リング」を行なう平坦化処
理。基本的な態様に対してこの平坦化処理の工程を付加
した場合のフローチャートは、図３にみるとおりであ
り、簡略化された態様に平坦化処理の工程を付加した場
合のフローチャートは、図４にみるとおりである。One example is to carry out the following steps following the finishing rolling step (F): G) Annealing while applying tension in the longitudinal direction to the thin plate, so-called "tension annealing". Flattening process. FIG. 3 is a flowchart showing a case where the flattening process is added to the basic mode, and FIG. 4 is a flowchart showing a case where the flattening process is added to the simplified mode. It is as seen in.
【００１２】もうひとつの例は、とくに薄い板を高い板
厚精度で得ようとする場合、拡散焼鈍工程（Ｅまたは
Ｅ’）に先立って、下記の工程のいずれかを、少なくと
も１回行なうことである： Ｈ）冷間圧延と、それに後続する６００℃以上９５０℃
未満の温度に加熱する中間焼鈍の組み合わせ、または Ｉ）６００℃以上９００℃以下の温度における温間圧
延。Another example is that, in the case where a particularly thin plate is to be obtained with high plate thickness accuracy, one of the following steps is performed at least once before the diffusion annealing step (E or E ′). H) cold rolling followed by 600 ° C. or more and 950 ° C.
A combination of intermediate annealing to a temperature of less than or less, or I) warm rolling at a temperature of 600 ° C or more and 900 ° C or less.
【００１３】図１に示した基本的な態様に、上記の平坦
化処理（Ｇ）に加えて冷間圧延−焼鈍（Ｈ）を行う変更
態様のフローチャートは、図５に示すようになる。FIG. 5 is a flowchart showing a modification of the basic mode shown in FIG. 1 in which cold rolling and annealing (H) are performed in addition to the flattening process (G).
【００１４】簡略化した態様の変更態様としては、拡散
焼鈍工程（Ｅ’）に先立って、下記の工程を１回行なう
ことが推奨される： Ｉ）６００℃以上９５０℃未満の温度に加熱する焼鈍
と、それに後続する冷間圧延の組み合わせ。図２に示し
た簡略化された態様に、上記の焼鈍−冷間圧延（Ｉ）を
付加して行なう変更態様のフローチャートは、図６に示
すようになる。As a modification of the simplified embodiment, it is recommended to perform the following step once prior to the diffusion annealing step (E ′): I) Heat to a temperature of 600 ° C. or more and less than 950 ° C. Combination of annealing followed by cold rolling. FIG. 6 is a flowchart of a modified embodiment in which the above-described annealing-cold rolling (I) is added to the simplified embodiment shown in FIG.
【００１５】原料とするＦｅの粉末は、いわゆる還元鉄
粉およびアトマイズ鉄粉が好適である。鉄カルボニル化
合物から製造した鉄粉があるが、高価である上に、粒度
が微細に過ぎることと、形状が球に近く圧粉成形性がよ
くないことから、適切とはいえない。Ｓｉ−Ｆｅ合金粉
末は、合金溶湯の水噴霧により製造したものが適当であ
る。Ｆｅ粉末もＳｉ−Ｆｅ合金粉末も、粒度が１００メ
ッシュ通過程度の微細かつ不規則形状のものが好適であ
る。２種の原料粉末の平均粒度および粒度分布は、なる
べく近似していることが好ましい。大きく異なると、混
合粉末の取り扱い中に、二種類が分離するおそれがあ
る。As the Fe powder as a raw material, so-called reduced iron powder and atomized iron powder are preferable. Although there is an iron powder produced from an iron carbonyl compound, it is not suitable because it is expensive, has too fine a particle size, and has a shape close to a sphere and has poor compactability. As the Si-Fe alloy powder, one produced by spraying molten alloy with water is suitable. It is preferable that both the Fe powder and the Si—Fe alloy powder have a fine and irregular shape having a particle size of about 100 mesh. It is preferable that the average particle size and the particle size distribution of the two raw material powders are as close as possible. If they are significantly different, the two types may be separated during handling of the mixed powder.
【００１６】非酸化性の雰囲気は、アルゴン、窒素、水
素などのガスの雰囲気、または真空を使用すればよい。The non-oxidizing atmosphere may be an atmosphere of a gas such as argon, nitrogen or hydrogen, or a vacuum.
【００１７】前記した基本的な製造方法の各工程は、つ
ぎに説明するような意義を有する。すなわち、粉末の混
合は、Ｓｉ含有量が高いＳｉ−Ｆｅ合金粉末の成形性の
低さを、それと混合するＦｅ粉末の成形性の高さで緩和
し、混合物全体として高い成形性を有する状態で粉末圧
延を行なうことにある。粉末圧延によって成形した板の
焼結は、混合物としての加工性は維持したままで、続く
冷間圧延の結果得られる製品が強度を発現することを可
能にする。冷間圧延は、所定の板厚を実現するととも
に、焼結体内部の空孔をつぶしてカサ密度を高め、内部
歪みエネルギーを与えることにより、次工程の拡散焼鈍
の条件を軽減することができる。ここでいう「冷間圧
延」とは、再結晶が起らない温度域での圧延を指す。こ
のようにして密度を高めた冷間圧延材は、拡散焼鈍によ
って組成が均一化されるとともに緻密化が促進され、意
図した電磁的な特性を示すに至るから、これを仕上圧延
によって、所定の板厚にする。仕上のためのスキンパス
圧延は、得られる珪素鋼板の板厚精度を向上させるだけ
でなく、製品の可撓性を高めるという利点もある。可撓
性の改善は予期していなかった利益であって、加工性の
向上が打ちぬき性を高め、複雑な形状の、または細い部
分をもつ製品の製造を可能にする。Each step of the above-mentioned basic manufacturing method has the following significance. That is, the mixing of the powder reduces the low formability of the Si-Fe alloy powder having a high Si content by the high formability of the Fe powder mixed therewith, and the mixture as a whole has high formability. To perform powder rolling. The sintering of the plate formed by powder rolling allows the product obtained as a result of the subsequent cold rolling to develop strength, while maintaining the workability as a mixture. Cold rolling achieves a predetermined plate thickness, increases the bulk density by crushing the pores inside the sintered body, and imparts internal strain energy, thereby reducing the conditions of diffusion annealing in the next step. . The term “cold rolling” as used herein refers to rolling in a temperature range where recrystallization does not occur. The cold-rolled material whose density has been increased in this way has a uniform composition and is promoted to be densified by diffusion annealing, and exhibits intended electromagnetic characteristics. Make it thicker. Skin pass rolling for finishing not only improves the thickness accuracy of the obtained silicon steel sheet, but also has the advantage of increasing the flexibility of the product. The improvement in flexibility is an unexpected benefit, and improved workability increases punchability and allows for the manufacture of products with complex shapes or narrow parts.
【００１８】簡略化された態様は、焼結工程より高い温
度に加熱する拡散焼鈍を行ない、拡散による合金組成の
ミクロ的な均一化とともに、薄板材料の強度の発現、お
よび磁気特性の改善を、同時に進行させる製造方法であ
る。In a simplified embodiment, diffusion annealing is performed by heating to a temperature higher than that of the sintering step, and the microscopic uniformization of the alloy composition by diffusion, the development of the strength of the sheet material, and the improvement of the magnetic properties are achieved. This is a manufacturing method that proceeds simultaneously.
【００１９】いずれの態様に従うにせよ、各工程の具体
的な条件は、上記の意図に適合するように選択すべきこ
とになる。まず、Ｆｅの粉末と混合するＦｅ−Ｓｉ合金
の粉末中のＳｉ含有量は、前記のとおり重量で８〜６５
％の広い範囲から選択可能であるが、Ｓｉ量は高すぎて
も低くすぎても好ましくない。たとえば、Ｆｅ−６．５
％Ｓｉ鋼を製造する場合、Ｓｉ量が８％Ｓｉより低い合
金は、磁気特性にとって有害な酸素の含有量が高くなり
がちであり、かつ、成分調整に必要な鉄粉の添加量が過
少になるため、粉末混合物の成形性が低くなって、とく
に薄い珪素鋼板の製造に不適当である。一方で、高いＳ
ｉ量の合金は、Ｆｅ粉末に対するＦｅ−Ｓｉ合金粉末の
配合量が過少となるため、粉末混合物の均一さが得にく
く、やはり不適当である。Regardless of which embodiment, the specific conditions for each step should be selected to meet the above intent. First, the content of Si in the powder of the Fe—Si alloy mixed with the powder of Fe is 8 to 65 by weight as described above.
% Can be selected from a wide range, but it is not preferable that the amount of Si is too high or too low. For example, Fe-6.5
When producing% Si steel, alloys having a Si content lower than 8% Si tend to have a high oxygen content which is harmful to magnetic properties, and the amount of iron powder required for component adjustment is too small. As a result, the compactability of the powder mixture is reduced, which is unsuitable for producing particularly thin silicon steel sheets. On the other hand, high S
In the case of the alloy having the amount i, the amount of the Fe-Si alloy powder relative to the Fe powder is too small, so that it is difficult to obtain a uniform powder mixture, which is also unsuitable.
【００２０】本発明は、従来技術で実現困難であった高
いＳｉ含有量、すなわち５％以上のＳｉを含有する珪素
鋼板を製造することに意義があるから、Ｆｅ−Ｓｉ合金
中のＳｉ量は当然に、ある限度以上でなければならない
が、他方で、電磁材料としてのＦｅ−Ｓｉ合金が含有す
べきＳｉ量は、実用上１１〜１２％を上限とするという
現状にかんがみれば、あまり高いＳｉ含有量もまた不利
である。Ｆｅの粉末とＦｅ−Ｓｉ合金の粉末との混合割
合に関して、一方が圧倒的に多い組み合わせ、たとえば
重量比で９５：５またはそれ以上の比率は、混合の均一
さを確保するという観点から好ましいものではなく、９
０：１０またはそれより５０：５０に近づいた比率が好
ましい。Since the present invention is significant in producing a silicon steel sheet containing a high Si content, which is difficult to realize by the conventional technology, that is, containing 5% or more of Si, the amount of Si in the Fe—Si alloy is reduced. Naturally, it must be above a certain limit, but on the other hand, the amount of Si that the Fe—Si alloy as the electromagnetic material should contain is practically high, considering the current state that the upper limit is 11 to 12%. Content is also disadvantageous. With respect to the mixing ratio between the Fe powder and the Fe-Si alloy powder, a combination in which one is overwhelmingly large, for example, a ratio of 95: 5 or more by weight is preferable from the viewpoint of ensuring uniform mixing. Not 9
A ratio of 0:10 or closer to 50:50 is preferred.
【００２１】上記の条件を満たすには、一般に、Ｓｉ含
有量が１０％以上で３０％をあまり上回らないものが使
いやすい。Ｆｅ−Ｓｉ系は、１８％Ｓｉの点にひとつの
共晶点（Ｆｅ3Ｓｉ、融点１２００℃）があるので、こ
の合金の粉末を利用することが得策である。In order to satisfy the above conditions, it is generally easy to use those having an Si content of 10% or more and not exceeding 30%. Since the Fe-Si system has one eutectic point (Fe 3 Si, melting point 1200 ° C.) at a point of 18% Si, it is advisable to use a powder of this alloy.
【００２２】２種の粉末の組み合わせについては、つぎ
の極端な典型例の間でさまざまな態様があり得るが、 ・Ｆｅ粉末を多量＋高Ｓｉ含有量のＦｅ−Ｓｉ合金粉末
を少量 ・Ｆｅ粉末を少量＋低Ｓｉ含有量のＦｅ−Ｓｉ合金粉末
を多量 経済性と粉末成形性の観点からは、どちらかといえば、
前者が有利であり、とくに薄い製品を得ようとする場合
には成形性を確保すべきであるから、Ｆｅ粉末を多量に
使用することが推奨される。拡散焼鈍においては、ミク
ロな成分の偏りが小さい方が、つまり後者の方が、均一
な組成の実現を容易にする。そのほかに、製造を意図す
る珪素鋼板のＳｉ含有量の値も重要であり、それらの諸
因子を考え合わせて、具体的な組成の組み合わせを決定
すればよい。The combination of the two powders can have various aspects between the following extreme typical examples: a large amount of Fe powder + a small amount of Fe-Si alloy powder having a high Si content; and a small amount of Fe powder. A small amount + a large amount of Fe-Si alloy powder with a low Si content From the viewpoint of economy and powder moldability, if anything,
The former is advantageous. In particular, when a thin product is to be obtained, the formability should be ensured. Therefore, it is recommended to use a large amount of Fe powder. In diffusion annealing, the smaller the deviation of the micro components, that is, the latter makes it easier to achieve a uniform composition. In addition, the value of the Si content of the silicon steel sheet intended for production is also important, and a specific composition combination may be determined in consideration of those factors.
【００２３】焼結工程は、拡散をあまり進行させず、か
つ後続の冷間圧延において空孔が効果的につぶされる焼
結体を得ることを目的とする工程である。温度範囲の下
限９５０℃に達しない温度では焼結が実用的な速度で進
行しないためであり、上限の１４００℃は、これ以上の
温度では合金粉末が溶融してしまうため設けた。この工
程は、上述したように後続の工程における加工性を確保
するため、Ｓｉ含有率が５．５％以下の部分が面積率で
３０％以上８０％以下を占めるような条件で実施すべき
である。「Ｓｉ含有率が５．５％以下の部分」は、いう
までもなく加工性を保っている部分であり、その割合が
３０％に達しないほど拡散を進めてしまうと、加工性が
著しく低下する。一方、８０％を超えるほど未拡散部分
が残っている焼結では、焼結体の強度が不充分であっ
て、圧延加工そのものが困難である。Ｓｉ含有率は、当
業者によく知られている手段、ＥＰＭＡによって測定す
ることができる。The sintering step is a step for obtaining a sintered body which does not progress diffusion much and in which the pores are effectively crushed in the subsequent cold rolling. This is because sintering does not proceed at a practical rate at a temperature below the lower limit of 950 ° C. of the temperature range, and the upper limit of 1400 ° C. is provided because alloy powder melts at temperatures higher than this. As described above, this step should be performed under the condition that a portion having a Si content of 5.5% or less occupies an area ratio of 30% or more and 80% or less in order to secure workability in a subsequent step as described above. is there. The “portion where the Si content is 5.5% or less” is, of course, a portion that maintains workability. If the diffusion proceeds so that the ratio does not reach 30%, the workability is significantly reduced. I do. On the other hand, in the case of sintering in which the undiffused portion remains as it exceeds 80%, the strength of the sintered body is insufficient and the rolling itself is difficult. The Si content can be measured by EPMA, a means well known to those skilled in the art.
【００２４】この段階では、焼結途上で空孔が多数存在
するため拡散速度が高く、焼結パラメータＰは次式で表
され、 Ｐ＝Ｔ×（２０＋Log10ｔ） Ｔ：絶対温度 ｔ：
時間（min） 焼結パラメータＰとＳｉの拡散の面積率との関係は、図
７によって、わりあいよく整理されることがわかった。
図７において、「Ｓｉ含有率が５．５％以下の部分」の
面積率が上記３０〜８０％の適正範囲に入るような焼結
パラメータＰの値は、（２３０〜３１０）×１０2であ
り、これに対応する焼結条件は、それぞれ、９５０℃×
３０分間および１３５０℃×１０分間である。したがっ
て、実際の操業条件は、この範囲内の温度と時間の組み
合わせとして選択すればよい。とくに好ましいＰの値
は、図７に明らかなように、約（２７０〜２８０）×１
０2である。At this stage, the diffusion rate is high because there are many vacancies during the sintering, and the sintering parameter P is represented by the following equation: P = T × (20 + Log 10 t) T: absolute temperature t:
Time (min) The relationship between the sintering parameter P and the area ratio of Si diffusion was found to be relatively well-ordered according to FIG.
In FIG. 7, the value of the sintering parameter P such that the area ratio of the “portion having a Si content of 5.5% or less” falls within the appropriate range of 30 to 80% is (230 to 310) × 10 2 . The corresponding sintering conditions are 950 ° C. ×
30 minutes and 1350 ° C. × 10 minutes. Therefore, the actual operating conditions may be selected as a combination of temperature and time within this range. Particularly preferable value of P is approximately (270 to 280) × 1 as apparent from FIG.
0 2 .
【００２５】上述の焼結に対し、拡散焼結は、Ｓｉの拡
散による組成の均一化を図り、かつ密度の向上を目指す
工程であるから、１１５０℃以上の高い温度に加熱する
ことが必要である。これより低い温度でも、拡散はある
程度進行するが、密度の上昇がほとんど望めず、製品鋼
板の磁気特性が向上しない。磁気特性向上の効果は、加
熱温度を高めるとともに高まるが、１３５０℃付近で飽
和する。１４００℃以上の温度では、合金が溶融してし
まう。拡散焼結は、バッチ炉、連続炉のどちらでも実施
することができるが、バッチ炉の場合は、重なり合った
材料が焼き付きを起こさないように、アルミナのような
焼き付き防止剤を塗布しておく必要がある。In contrast to the above-mentioned sintering, diffusion sintering is a process aimed at uniforming the composition by diffusion of Si and improving the density, so that it is necessary to heat to a high temperature of 1150 ° C. or more. is there. Even at a lower temperature, the diffusion proceeds to some extent, but almost no increase in density is expected, and the magnetic properties of the product steel sheet are not improved. The effect of improving the magnetic properties increases as the heating temperature increases, but saturates around 1350 ° C. At temperatures above 1400 ° C., the alloy will melt. Diffusion sintering can be performed in either a batch furnace or a continuous furnace, but in the case of a batch furnace, it is necessary to apply an anti-seizure agent such as alumina so that overlapping materials do not seize. There is.
【００２６】この工程は、磁気特性を確保するため、Ｓ
ｉ含有率が６％以上７％以下の部分が面積率で５０％以
上を占めるとともに、結晶粒を過度に粗大化させず、次
工程における加工性を確保することができるような条件
で実施すべきである。拡散焼結の段階における焼結パラ
メータＰは、つぎの式で表され、 Ｐ＝Ｔ×（１０＋Log10ｔ） Ｔ：絶対温度 ｔ：
時間（min） 焼結パラメータＰとＳｉの拡散の面積率との関係は、図
８によって整理されることがわかった。図８において、
「Ｓｉ含有率が６％以上７％以下の部分」の面積率が上
記した５０％以上という適正範囲に入るような焼結パラ
メータＰの値は、（１７０〜２００）×１０2であり、
これに対応する焼結条件は、それぞれ、１２００℃×３
０分間（または１１５０℃×６０分）および１３５０℃
×１２０分間である。したがって、実際の操業条件は、
この範囲内の温度と時間の組み合わせとして選択すれば
よい。とくに好ましいＰの値は、図８からわかるとお
り、約（１８０〜２００）×１０2である。In this step, in order to secure magnetic characteristics, S
The portion having an i content of 6% or more and 7% or less occupies 50% or more in terms of area ratio, does not excessively coarsen the crystal grains, and is carried out under conditions that can ensure workability in the next step. Should. The sintering parameter P in the diffusion sintering stage is represented by the following equation: P = T × (10 + Log 10 t) T: absolute temperature t:
Time (min) The relationship between the sintering parameter P and the area ratio of Si diffusion was found to be summarized by FIG. In FIG.
The value of the sintering parameter P such that the area ratio of the “portion having a Si content of 6% or more and 7% or less” falls within the above-described appropriate range of 50% or more is (170 to 200) × 10 2 ,
The corresponding sintering conditions are 1200 ° C. × 3
0 minutes (or 1150 ° C x 60 minutes) and 1350 ° C
× 120 minutes. Therefore, the actual operating conditions are:
What is necessary is just to select as a combination of the temperature and time in this range. A particularly preferable value of P is about (180 to 200) × 10 2 as can be seen from FIG.
【００２７】焼鈍工程は、圧延による歪を開放して、つ
ぎの冷間圧延を容易にする作業であり、この工程で製品
の強度の向上を図ることはできない。６００℃に達しな
い温度では加工歪の緩和が進まないが、９５０℃以上の
温度に上げても加工性の向上はそれ以上望めず、いたず
らにエネルギーを消費するだけである。The annealing step is an operation for releasing the distortion caused by the rolling and facilitating the next cold rolling, and it is impossible to improve the strength of the product in this step. If the temperature does not reach 600 ° C., the relaxation of the processing strain does not progress. However, even if the temperature is raised to 950 ° C. or more, the improvement of the workability cannot be expected any more, and energy is simply consumed unnecessarily.
【００２８】上述した方法により、Ｓｉ含有量が５〜１
２重量％で、厚さが０．０５〜０．５０ｍｍ、実用的な
範囲は０．１０〜０．３５mmの、組成が均一で加工性の
高い珪素鋼板を製造することができ、この製品も本発明
の範囲に包含される。According to the method described above, the Si content is 5 to 1
At 2% by weight, a silicon steel sheet having a uniform composition and high workability with a thickness of 0.05 to 0.50 mm and a practical range of 0.10 to 0.35 mm can be manufactured. Included within the scope of the invention.
【００２９】[0029]
【実施例】原料粉末として、Ｆｅ粉末および１８％Ｓｉ
−Ｆｅ粉末を、いずれも水噴霧法により製造し、１００
メッシュ通過粉を採取した。平均粒径は、どちらも約４
０μｍである。これらの粉末を、混合物中のＳｉ量が
６．５重量％になるように、重量比で６６:３４の割合
で、タンブラーにより混合した。この粉末混合物を、下
に記すNo.１〜No.９の、種々のバラエティをもつ工程で
加工し、珪素鋼板を製造した。EXAMPLES As raw material powders, Fe powder and 18% Si were used.
-Fe powder was manufactured by water spraying method,
The powder that passed through the mesh was collected. The average particle size is about 4
0 μm. These powders were mixed by a tumbler at a ratio of 66:34 by weight so that the amount of Si in the mixture was 6.5% by weight. This powder mixture was processed in the following No. 1 to No. 9 processes having various varieties to produce silicon steel sheets.
【００３０】粉末圧延は、直径２００mm、長さ２４０mm
のロール２本をもつ水平方向圧延ロールを使用し、これ
に振動板上から粉末を供給して、圧力７０トンの一定値
でキスロール方式で圧延することにより実施した。各工
程において、拡散焼鈍は、バッチ炉（No.１ないしNo.
６）または連続炉（No.７ないしNo.９）を使用して行な
い、張力下焼鈍は、とくに条件の記載がない限り、７５
０℃×２分間、張力３kg/mm2の条件で実施した。仕上圧
延（スキンパス圧延）の圧下率は、０．５〜５％であ
る。Powder rolling, diameter 200mm, length 240mm
This was carried out by using a horizontal rolling roll having two rolls, supplying the powder from above the diaphragm to the kiss roll system at a constant pressure of 70 tons. In each process, diffusion annealing is performed in a batch furnace (No. 1 to No. 1).
6) or using a continuous furnace (No. 7 to No. 9), and annealing under tension is performed at 75% unless otherwise specified.
The test was performed at 0 ° C. for 2 minutes under a tension of 3 kg / mm 2 . The rolling reduction of the finish rolling (skin pass rolling) is 0.5 to 5%.
【００３１】［比較例］ No.１（在来技術） 粉末混合−粉末圧延（板厚０．１０mm）−焼結（バッチ
炉、１２５０℃×１時間、製品板厚０．１０mm）[Comparative Example] No. 1 (conventional technology) Powder mixing-powder rolling (sheet thickness 0.10 mm)-sintering (batch furnace, 1250 ° C x 1 hour, product sheet thickness 0.10 mm)
【００３２】［基本的な態様の実施例］ No.２（図１） Ａ．粉末混合−Ｂ．粉末圧延（板厚０．１１mm）−Ｃ．
焼結（バッチ炉、１０５０℃×１時間）−Ｄ．冷間圧延
（板厚０．１０５mm）−Ｅ．拡散焼鈍（バッチ炉、１２
００℃×１時間）−Ｆ．仕上圧延（製品板厚０．１０m
m） No.３（No.２に焼鈍−冷間圧延を加えたもの） Ａ．粉末混合−Ｂ．粉末圧延（板厚０．１２mm）−Ｃ．
焼結（バッチ炉、１０５０℃×１時間）−Ｄ．冷間圧延
（板厚０．１１mm）−Ｈ．焼鈍（８５０℃×１時間）−
冷間圧延（板厚０．１０５mm）−Ｅ．拡散焼鈍（バッチ
炉、１２００℃×１時間）−Ｆ．仕上圧延（製品板厚
０．１０mm） No.４（No.３に平坦化処理を加えたもの、図５） Ａ．粉末混合−Ｂ．粉末圧延（板厚０．１２mm）−Ｃ．
焼結（１０５０℃×１時間）−Ｈ．冷間圧延（板厚０．
１１mm）−焼鈍（８５０℃×１時間）−冷間圧延（板厚
０．１０５mm）−Ｅ．拡散焼鈍（バッチ炉、１２００℃
×１時間）−仕上圧延（製品板厚０．１０mm）−Ｇ．平
坦化処理 No.５（図３） Ａ．粉末混合−Ｂ．粉末圧延（板厚０．１１mm）−Ｃ．
焼結（連続炉、１０５０℃×６分間）−Ｄ．冷間圧延
（板厚０．１０５mm）−Ｅ．拡散焼鈍（連続炉、１２８
５℃×８分間）−Ｆ．仕上圧延（製品板厚０．１０mm）
−Ｇ．平坦化処理[Example of Basic Embodiment] No. 2 (FIG. 1) Powder mixing-B. Powder rolling (sheet thickness 0.11 mm) -C.
Sintering (batch furnace, 1050 ° C. × 1 hour) -D. Cold rolling (sheet thickness 0.105 mm) -E. Diffusion annealing (batch furnace, 12
00 ° C. × 1 hour) -F. Finish rolling (product thickness 0.10m
m) No. 3 (No. 2 with annealing and cold rolling added) Powder mixing-B. Powder rolling (sheet thickness 0.12 mm) -C.
Sintering (batch furnace, 1050 ° C. × 1 hour) -D. Cold rolling (sheet thickness 0.11 mm) -H. Annealing (850 ° C x 1 hour)
Cold rolling (sheet thickness 0.105 mm) -E. Diffusion annealing (batch furnace, 1200 ° C. × 1 hour) -F. Finish rolling (product thickness 0.10mm) No. 4 (No. 3 with flattening treatment, Fig. 5) Powder mixing-B. Powder rolling (sheet thickness 0.12 mm) -C.
Sintering (1050 ° C. × 1 hour) -H. Cold rolling (plate thickness 0.
11 mm)-annealing (850 ° C x 1 hour)-cold rolling (sheet thickness 0.105 mm)- Diffusion annealing (batch furnace, 1200 ° C
X 1 hour)-Finish rolling (product thickness 0.10mm)- Flattening treatment No. 5 (FIG. 3) A. Powder mixing-B. Powder rolling (sheet thickness 0.11 mm) -C.
Sintering (continuous furnace, 1050 ° C. × 6 minutes) -D. Cold rolling (sheet thickness 0.105 mm) -E. Diffusion annealing (continuous furnace, 128
5 ° C. × 8 minutes) -F. Finish rolling (product thickness 0.10mm)
-G. Flattening process
【００３３】［簡略化された態様の実施例］ No.６（図２） Ａ．粉末混合−Ｂ．粉末圧延（板厚０．１０５mm）−
Ｅ’．拡散焼鈍（バッチ炉、１２００℃×１時間）−
Ｆ．仕上圧延（製品板厚０．１０mm） No.７（No.６に焼鈍−冷間圧延を加えたもの、図６） Ａ．粉末混合−Ｂ．粉末圧延（板厚０．１１mm）−焼鈍
（８５０℃×０．５時間）−Ｈ．焼結（バッチ炉、１２
００℃×１時間、真空中で）−冷間圧延（板厚０．１０
５mm）−Ｅ’拡散焼鈍（バッチ炉、１２００℃×１時
間）−Ｆ．仕上圧延（製品板厚０．１０mm） No.８（図４） Ａ．粉末混合−Ｂ．粉末圧延（板厚０．１０５mm）−
Ｅ’．拡散焼鈍（連続炉、１２８５℃×８分間）−Ｆ．
仕上圧延（製品板厚０．１０mm）−Ｇ．平坦化処理 No.９（図４） Ａ．粉末混合−Ｂ．粉末圧延（板厚０．１０５mm）−
Ｅ’．拡散焼鈍（連続炉、１３２５℃×２分間）−Ｆ．
仕上圧延（製品板厚０．１０mm）−Ｇ．平坦化処理[Example of Simplified Embodiment] No. 6 (FIG. 2) Powder mixing-B. Powder rolling (board thickness 0.105mm)
E '. Diffusion annealing (batch furnace, 1200 ° C x 1 hour)
F. Finish rolling (product thickness 0.10 mm) No. 7 (No. 6 with annealing and cold rolling added, Fig. 6) Powder mixing-B. Powder rolling (sheet thickness 0.11 mm) -annealing (850 ° C. × 0.5 hour) Sintering (batch furnace, 12
Cold rolling (sheet thickness 0.10)
5 mm) -E 'diffusion annealing (batch furnace, 1200 ° C. × 1 hour) -F. Finish rolling (product thickness 0.10mm) No. 8 (Fig. 4) Powder mixing-B. Powder rolling (board thickness 0.105mm)
E '. Diffusion annealing (continuous furnace, 1285 ° C. × 8 minutes) -F.
Finish rolling (product thickness 0.10 mm) -G. Flattening process No. 9 (FIG. 4) A. Powder mixing-B. Powder rolling (board thickness 0.105mm)
E '. Diffusion annealing (continuous furnace, 1325 ° C. × 2 minutes) -F.
Finish rolling (product thickness 0.10 mm) -G. Flattening process
【００３４】No.１ないし４およびNo.６，７の製品珪素
鋼板について密度を測定し、下の表１に示す結果を得
た。No.１およびNo.２については、比抵抗を測定した。
その結果も、あわせて表１に掲げた。 表 １No. 密度ρ(g/cm3 ) 比抵抗(μΩｃｍ) １ ７．３２ ８０ ２ ７．３１ ８０ ３ ７．３８ ４ ７．４２ ６ ７．３６ ７ ７．３３The densities of the silicon steel products Nos. 1 to 4 and Nos. 6 and 7 were measured, and the results shown in Table 1 below were obtained. For No. 1 and No. 2, the specific resistance was measured.
The results are also shown in Table 1. Table 1 No. Density ρ (g / cm 3 ) Specific resistance (μΩcm) 1 7.32 80 2 7.31 803 7.38 4 7.42 6 7.36 7 7.33
【００３５】直流磁気特性の値は、つぎの表２に示すと
おりである。 表 ２ No. Ｂ１ Ｂ２ Ｂ１０ Ｂ２５ Ｈｃ(Ｏｅ) １ 8200 9350 11800 12700 ０．３２ ２ 9800 10900 11200 12600 ０．２５ ３ 8750 9780 11850 13010 ０．２８ ４ 8860 9840 11800 12930 ０．２７ ５ 8750 9580 11700 12900 ０．３８ ６ 8700 9480 11500 12700 ０．４６ ７ 8100 9250 11700 12800 ０．３０ ８ 8710 9500 11600 12600 ０．５２ ９ 8680 9460 11300 12600 ０．４０The values of the DC magnetic characteristics are as shown in Table 2 below. Table 2 No. B1 B2 B10 B25 Hc (Oe) 1 8200 9350 11800 12700 0.32 2 9800 10900 11200 12600 0.25 3 8750 9780 11850 13010 0.28 4 8860 9840 11800 12930 0.27 5 8750 9580 11700 12900 0 .38 6 8700 9480 11500 12700 0.46 7 8100 9250 11700 12800 0.30 8 8710 9500 11600 12600 0.52 9 8680 9460 11300 12600 0.40
【００３６】交流磁気特性の値は、つぎの表３のとおり
である。 表 ３ No. Ｗ10/50 Ｗ10/100 Ｗ10/400 Ｗ10/1K Ｗ10/2K Ｗ10/5K Ｗ10/10K １ 0.81 1.86 8.52 33.8 70.3 261.1 714.3 ２ 0.74 1.84 8.00 31.6 68.6 253.6 710.2 ３ 0.85 1.95 9.10 35.5 73.5 280.5 784.4 ４ 0.82 1.91 8.86 34.7 71.9 277.9 778.8 ５ 0.80 1.90 9.00 36.0 77.8 288.4 804.2 ６ 0.88 2.13 10.04 51.1 92.3 341.9 981.7 ７ 0.78 1.88 8.81 34.2 70.8 274.9 771.8 ８ 0.90 2.15 10.50 52.3 98.6 364.6 1005.9 ９ 0.85 2.00 9.80 49.5 87.3 320.9 960.6 Ｂｍ＝１０ＫＧのときの値、単位ｗ／ｋｇThe values of the AC magnetic characteristics are as shown in Table 3 below. Table 3 No. W10 / 50 W10 / 100 W10 / 400 W10 / 1K W10 / 2K W10 / 5K W10 / 10K 1 0.81 1.86 8.52 33.8 70.3 261.1 714.3 2 0.74 1.84 8.00 31.6 68.6 253.6 710.2 3 0.85 1.95 9.10 35.5 73.5 280.5 784.4 4 0.82 1.91 8.86 34.7 71.9 277.9 778.8 5 0.80 1.90 9.00 36.0 77.8 288.4 804.2 6 0.88 2.13 10.04 51.1 92.3 341.9 981.7 7 0.78 1.88 8.81 34.2 70.8 274.9 771.8 8 0.90 2.15 10.50 52.3 98.6 364.6 1005.9 9 0.85 2.00 9.80 49.5 87.3 320.9 960.6 Bm At the time of, unit w / kg
【００３７】平坦化処理の効果を、No.３とNo.４の製品
の幅８５mm、長さ１ｍのものを平定盤上に乗せ、最大高
さを測定して平坦度を比較することによって確認した。
その結果は、つぎの表４のとおりであった。 表 ４No. 平坦度（μｍ／ｍ） ３ ８３６ ４ ２３５The effect of the flattening process was confirmed by placing No. 3 and No. 4 products having a width of 85 mm and a length of 1 m on a flat surface plate, measuring the maximum height, and comparing the flatness. did.
The results are as shown in Table 4 below. Table 4 No. Flatness (μm / m) 3 836 4 235
【００３８】No.５の製品について、張力下焼鈍の条件
を変えて、得られる平坦度を比較した。その結果をつぎ
の表５に示す。 表 ５ No. 温度 張力 平坦度 （℃） （kgf/mm２） （μｍ／ｍ） イ 張力下焼鈍前 １０４０ ロ ６００ ４ ９６５ ハ ７００ ２ ７８４ ニ ７００ ３ ６６９ ホ ７００ ４ ２３０ ヘ ７５０ ２ ３２０ ト ７５０ ３ １６８ チ ８００ ３ ２４６ リ １０００ ２ 切 断With respect to the product of No. 5, the obtained flatness was compared by changing the conditions of annealing under tension. The results are shown in Table 5 below. Table 5 No. Temperature Tension Flatness (° C) (kgf / mm2) (μm / m) A Before annealing under tension 1040 B 600 4965 C 700 2 784 D 700 3 669 E 700 4 230 F 750 2 320 G 750 3 168 h 800 3 246 ri 1000 2 cutting
【００３９】仕上圧延工程のスキンパス圧延がもたらす
前記の利益、すなわち可撓性の向上は、No.１におい
て、抗折試験の結果が、下記の値を示したことから明ら
かである： 抗折力（Ｍｐａ） 撓み（ｍｍ） 拡散焼鈍後 ９９８ ０．８０ スキンパス圧延後 １９８６ １．９８ 試験片サイズは、３×５×４０ｍｍ、標点間距離２５ｍ
ｍ。[0039] The benefit of skin pass rolling finish rolling process results, i.e. improved flexibility, in No.1, the results of bending tests, it is apparent from the fact indicated the following values: transverse rupture strength (Mpa) Deflection (mm) After diffusion annealing 998 0.80 After skin pass rolling 1986 1.98 Test specimen size is 3 × 5 × 40 mm, distance between gauges 25 m
m.
【００４０】[0040]
【発明の効果】本発明により、Ｆｅ−Ｓｉ合金の難点で
ある加工性の低さを、Ｆｅ粉末の高い加工性でカバーす
ることができ、従来製造が困難であった５重量％以上１
１〜１２％に及ぶ高いＳｉ含有量の珪素鋼板薄板が、容
易に製造できる。板厚は、仕上工程のスキンパス圧延に
より、０．０５〜０．５ｍｍの範囲において高い精度が
実現できる。スキンパス圧延は、製品である珪素鋼板の
可撓性と加工性を高め、打ち抜きを容易にし、これは珪
素鋼板の主たる用途である変圧器鉄心の製造にとって好
都合である。テンションアニ−リングを施した好適態様
の製品は、高い平坦度を示す。According to the present invention, the low workability, which is a disadvantage of the Fe-Si alloy, can be covered by the high workability of the Fe powder, and it has been difficult to manufacture 5% by weight or more of 1%.
A silicon steel sheet having a high Si content ranging from 1 to 12% can be easily manufactured. The plate thickness can achieve high accuracy in the range of 0.05 to 0.5 mm by skin pass rolling in the finishing step. Skin pass rolling increases the flexibility and workability of the product silicon steel sheet and facilitates punching, which is advantageous for the manufacture of transformer cores, which is the main use of silicon steel sheet. Products of the preferred embodiment that have been subjected to tension annealing exhibit high flatness.
【００４１】[0041]
【図１】 本発明に従う珪素鋼板の製造方法の、基本的
な態様の工程を示すフローチャート。FIG. 1 is a flowchart showing the steps of a basic embodiment of the method for manufacturing a silicon steel sheet according to the present invention.
【図２】 本発明に従う珪素鋼板の製造方法の、簡略化
された態様の工程を示すフローチャート。FIG. 2 is a flowchart showing the steps of a simplified embodiment of the method for manufacturing a silicon steel sheet according to the present invention.
【図３】 図１に示した珪素鋼板の製造方法の、変更態
様を示すフローチャート。FIG. 3 is a flowchart showing a modification of the method for manufacturing the silicon steel sheet shown in FIG.
【図４】 図２に示した珪素鋼板の製造方法の、変更態
様を示すフローチャート。FIG. 4 is a flowchart showing a modification of the method for manufacturing the silicon steel sheet shown in FIG.
【図５】 図１に示した珪素鋼板の製造方法の、別の変
更態様を示すフローチャート。FIG. 5 is a flowchart showing another modification of the method of manufacturing the silicon steel sheet shown in FIG.
【図６】 図２に示した珪素鋼板の製造方法の、別の変
更態様を示すフローチャート。FIG. 6 is a flowchart showing another modification of the method for manufacturing the silicon steel sheet shown in FIG. 2;
【図７】 本発明の工程（Ｃ）、すなわち焼結工程の実
施条件を確立するために利用したデータであって、焼結
パラメータＰと、焼結体のＳｉ含有率が５．５％以下の
部分が占める面積率との関係を実測したグラフ。FIG. 7 shows data used to establish the process (C) of the present invention, that is, the conditions for performing the sintering step, wherein the sintering parameter P and the Si content of the sintered body are 5.5% or less. The graph which measured the relationship with the area ratio which a part occupies.
【図８】 本発明の工程（Ｅ）、すなわち拡散焼結工程
の実施条件を確立するために利用したデータであって、
焼結パラメータＰと、焼結体のＳｉ含有率が６％以上７
％以下の部分が占める面積率との関係を実測したグラ
フ。FIG. 8 shows data used for establishing the conditions for carrying out the step (E) of the present invention, ie, the diffusion sintering step,
The sintering parameter P and the Si content of the sintered body are 6% or more 7
The graph which measured the relationship with the area ratio which a part below% occupies.
─────────────────────────────────────────────────────
────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成１２年１０月６日（２０００．１０．
６）[Submission date] October 6, 2000 (2000.10.
6)
【手続補正１】[Procedure amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】請求項６[Correction target item name] Claim 6
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ２２Ｃ 38/00 ３０３ Ｃ２２Ｃ 38/00 ３０３Ｕ 38/02 38/02 Ｈ０１Ｆ 1/16 Ｈ０１Ｆ 1/16 Ａ ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C22C 38/00 303 C22C 38/00 303U 38/02 38/02 H01F 1/16 H01F 1/16 A
Claims (7)
法： Ａ）Ｆｅの粉末と、８〜６５重量％のＳｉを含有するＦ
ｅ−Ｓｉ合金の粉末とを、混合物中のＳｉが５〜１２重
量％を占める割合で混合する粉末混合工程、 Ｂ）この混合物を粉末圧延法により厚さ０．０５〜０．
５mmの薄板に成形する粉末圧延工程、 Ｃ）粉末圧延によって得た薄板を、９５０℃以上１４０
０℃未満の温度で焼結する焼結工程、 Ｄ）焼結した薄板を冷間圧延して、板厚を所定の厚さに
するとともにカサ密度を９８％以上に高める冷間圧延工
程、 Ｅ）冷間圧延後の薄板を１１５０℃以上１４００℃未満
の温度で非酸化性雰囲気下に加熱して、合金組成を均一
化する拡散焼鈍工程、および Ｆ）拡散焼鈍をへて合金組成が均一化された薄板に、圧
下率０．５〜５％のスキンパス圧延を行って板厚を所定
の厚さにする仕上圧延工程。1. A method for producing a silicon steel sheet comprising the following steps: A) Fe powder and F containing 8 to 65% by weight of Si
a powder mixing step of mixing the powder of the e-Si alloy with Si in the mixture at a ratio of 5 to 12% by weight, and B) a thickness of 0.05 to 0.
A powder rolling step of forming into a 5 mm thin plate; C) a thin plate obtained by powder rolling
A sintering step of sintering at a temperature lower than 0 ° C., D) a cold rolling step of cold rolling the sintered thin plate to a predetermined thickness and a bulk density of 98% or more; D) a diffusion annealing step of heating the cold-rolled sheet at a temperature of 1150 ° C. or more and less than 1400 ° C. in a non-oxidizing atmosphere to make the alloy composition uniform, and F) making the alloy composition uniform by diffusion annealing A finish rolling step of subjecting the thin sheet to skin pass rolling at a draft of 0.5 to 5% to reduce the sheet thickness to a predetermined thickness.
程を行なう請求項１に記載の珪素鋼板の製造方法： Ｇ）薄板に対しその長手方向に張力を加えつつ焼鈍を行
なう平坦化処理。2. The method for producing a silicon steel sheet according to claim 1, wherein the following steps are performed subsequent to the finish rolling step (F): G) Flattening the thin sheet by annealing while applying tension in its longitudinal direction. processing.
工程のいずれかを行なう請求項１に記載の珪素鋼板の製
造方法：Ｈ）６００℃以上９５０℃未満の温度に加熱す
る焼鈍と、それに後続する冷間 圧延との組み合わせ、または Ｉ）６００以上９００℃以下の温度における温間圧延。3. The method for producing a silicon steel sheet according to claim 1, wherein one of the following steps is performed prior to the diffusion annealing step (E): H) annealing to a temperature of 600 ° C. or more and less than 950 ° C. Or a combination with subsequent cold rolling, or I) warm rolling at a temperature of 600 to 900 ° C.
法： Ａ）Ｆｅの粉末と、８〜６５重量％のＳｉを含有するＦ
ｅ−Ｓｉ合金の粉末とを、混合物中のＳｉが５〜１２重
量％を占める割合で混合する粉末混合工程、 Ｂ）この混合物を粉末圧延法により厚さ０．０５〜０．
５mmの薄板に成形する粉末圧延工程、 Ｅ’）粉末圧延によって得た薄板を、１１５０℃以上１
４００℃未満の温度で非酸化性雰囲気下に加熱して、密
度を高めるとともに合金組成を均一化する拡散焼鈍工
程、および Ｆ）拡散焼鈍をへて合金組成が均一化された薄板に、圧
下率０．５〜５％のスキンパス圧延を行って板厚を所定
の厚さにする仕上圧延工程。4. A method for producing a silicon steel sheet comprising the following steps: A) Fe powder and F containing 8 to 65% by weight of Si.
a powder mixing step of mixing the powder of the e-Si alloy with Si in the mixture at a ratio of 5 to 12% by weight, and B) a thickness of 0.05 to 0.
A powder rolling step of forming into a 5 mm thin plate; E ′) a thin plate obtained by powder rolling is heated to 1150 ° C. or higher;
A diffusion annealing step of increasing the density and homogenizing the alloy composition by heating in a non-oxidizing atmosphere at a temperature of less than 400 ° C., and F) applying a reduction rate to the sheet having a uniform alloy composition through the diffusion annealing. A finish rolling step of performing a 0.5 to 5% skin pass rolling to make the sheet thickness to a predetermined thickness.
程を行なう請求項４に記載の珪素鋼板の製造方法： Ｇ）薄板に対しその長手方向に張力を加えつつ焼鈍を行
なう平坦化処理。5. The method for producing a silicon steel sheet according to claim 4, wherein the following steps are performed subsequent to the finish rolling step (F): G) Flattening the thin sheet by performing annealing while applying tension in the longitudinal direction. processing.
の工程のいずれかを行なう請求項２に記載の珪素鋼板の
製造方法： Ｈ）６００℃以上９５０℃未満の温度に加熱する焼鈍
と、それに後続する冷間圧延との組み合わせ、または Ｉ）６００以上９００℃以下の温度における温間圧延。6. The method for producing a silicon steel sheet according to claim 2, wherein one of the following steps is performed prior to the diffusion annealing step (E ′): H) Annealing by heating to a temperature of 600 ° C. or more and less than 950 ° C. Or a combination of the subsequent cold rolling, or I) warm rolling at a temperature of 600 to 900 ° C.
法により製造した、Ｓｉ含有量が５〜１２重量％で、厚
さが０．０５〜０．３５mmの珪素鋼板。7. A silicon steel sheet having a Si content of 5 to 12% by weight and a thickness of 0.05 to 0.35 mm, produced by the method according to any one of claims 1 to 6.
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| JP11372351A JP2001026822A (en) | 1999-05-10 | 1999-12-28 | Silicon steel sheet and its manufacture |
| EP00109188A EP1052043A3 (en) | 1999-05-10 | 2000-05-09 | Silicon steel plate and method for producing the same |
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|---|---|---|---|
| JP11-129250 | 1999-05-10 | ||
| JP12925099 | 1999-05-10 | ||
| JP11372351A JP2001026822A (en) | 1999-05-10 | 1999-12-28 | Silicon steel sheet and its manufacture |
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|---|---|
| JP2001026822A true JP2001026822A (en) | 2001-01-30 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100457359B1 (en) * | 2002-09-12 | 2004-11-16 | 한국과학기술연구원 | Pressing Device and Method for Sintering Substrates |
| KR100900662B1 (en) * | 2002-11-11 | 2009-06-01 | 주식회사 포스코 | Coating composition and, method for manufacturing high silicon grain-oriented electrical steel sheet with superior core loss property using thereof |
| KR100946069B1 (en) * | 2002-11-27 | 2010-03-10 | 주식회사 포스코 | Method for manufacturing high silicon grain-oriented electrical steel sheet with superior magnetic properties |
| KR101060913B1 (en) | 2003-12-20 | 2011-08-30 | 주식회사 포스코 | Manufacturing method of high silicon oriented electrical steel sheet with excellent iron loss characteristics |
| CN103273043A (en) * | 2013-05-24 | 2013-09-04 | 北京科技大学 | Method for preparing pure iron/columnar crystal high-silicon electrical steel composite plate blank |
| KR101865256B1 (en) * | 2009-04-13 | 2018-06-11 | 한국생산기술연구원 | High silicon containing extremely thin electrical steel sheets and method for manufacturing the same |
| KR20220089154A (en) * | 2020-12-21 | 2022-06-28 | 재단법인 포항산업과학연구원 | Method for manufacturing electrical steel sheet from powder |
-
1999
- 1999-12-28 JP JP11372351A patent/JP2001026822A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100457359B1 (en) * | 2002-09-12 | 2004-11-16 | 한국과학기술연구원 | Pressing Device and Method for Sintering Substrates |
| KR100900662B1 (en) * | 2002-11-11 | 2009-06-01 | 주식회사 포스코 | Coating composition and, method for manufacturing high silicon grain-oriented electrical steel sheet with superior core loss property using thereof |
| KR100946069B1 (en) * | 2002-11-27 | 2010-03-10 | 주식회사 포스코 | Method for manufacturing high silicon grain-oriented electrical steel sheet with superior magnetic properties |
| KR101060913B1 (en) | 2003-12-20 | 2011-08-30 | 주식회사 포스코 | Manufacturing method of high silicon oriented electrical steel sheet with excellent iron loss characteristics |
| KR101865256B1 (en) * | 2009-04-13 | 2018-06-11 | 한국생산기술연구원 | High silicon containing extremely thin electrical steel sheets and method for manufacturing the same |
| CN103273043A (en) * | 2013-05-24 | 2013-09-04 | 北京科技大学 | Method for preparing pure iron/columnar crystal high-silicon electrical steel composite plate blank |
| KR20220089154A (en) * | 2020-12-21 | 2022-06-28 | 재단법인 포항산업과학연구원 | Method for manufacturing electrical steel sheet from powder |
| KR102530028B1 (en) * | 2020-12-21 | 2023-05-04 | 재단법인 포항산업과학연구원 | Method for manufacturing electrical steel sheet from powder |
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