WO2020149348A1 - 一方向性電磁鋼板の製造方法 - Google Patents
一方向性電磁鋼板の製造方法 Download PDFInfo
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- the present invention relates to a method for producing a unidirectional electrical steel sheet used as an iron core material for a transformer, and particularly to a method for producing a unidirectional electrical steel sheet having no forsterite coating excellent in decarburization.
- the present application claims priority based on Japanese Patent Application No. 2019-005129 filed in Japan on January 16, 2019, the contents of which are incorporated herein by reference.
- the present invention removes the glass film by means such as pickling, or intentionally prevents the production of the finished annealed unidirectional electrical steel sheet, that is, a forsterite film.
- the unidirectional electrical steel sheet is excellent in decarburization for reducing the carbon residual amount even when the sheet thickness is thick and realizing low iron loss. It aims at providing the manufacturing method of.
- the content of the acid-soluble Al exceeds 0.07%, the steel sheet becomes brittle, and particularly in the electrical steel sheet of the present invention containing a large amount of Si, the embrittlement becomes remarkable, so the content of the acid-soluble Al is 0. It should be 07% or less. It is preferably 0.05% or less, more preferably 0.03% or less.
- a cold rolling step for forming a steel sheet, a decarburizing annealing step for decarburizing the cold rolled steel sheet, and a finish annealing step for finish annealing the steel sheet after the decarburizing annealing step are provided.
- the decarburization annealing step the cold rolled steel sheet is decarburized and the crystal grain size is controlled to a size suitable for secondary recrystallization (the grain size before secondary recrystallization is referred to as primary recrystallized grain size). It is a process.
- the decarburization annealing step of this manufacturing method is (I-1) a first heat treatment of heating a temperature range of 550° C. or higher and lower than 720° C. at an average heating rate HR1 of 40 to 500° C./sec; (I-2) Following the first heat treatment, a temperature range of 720° C. or higher and a temperature T1° C. or lower that satisfies the following formula (2) is heated at an average heating rate HR2 of 5 to 50° C./second. Heat treatment; (Ii) a second annealing process, followed by a first annealing process of holding the temperature T1° C. for 50 to 1000 seconds; Have.
- the oxygen partial pressure P1 is set to 0.0010 or more. It is preferably 0.010 or more.
- (I-1) First stage heating (sometimes referred to as first heat treatment) Heating temperature range: 550° C. or higher and lower than 720° C. Average heating rate HR1: 40° C./sec or higher, 500° C./sec or lower.
- the SiO 2 formation behavior that inhibits the decarburization reaction is not limited to the oxygen partial pressure of the atmosphere It also depends on the speed. Therefore, it is important that the heating in the decarburization annealing goes through a thermal cycle that avoids the formation of SiO 2 as much as possible.
- the average heating rate HR3 is set to 5°C/sec or more. It is preferably 10° C./second or more.
- the average heating rate HR3 exceeds 50° C./sec, the temperature reached by heating exceeds the temperature T2° C., the primary recrystallized grain size becomes coarse, causing secondary recrystallization failure, and the magnetic flux density decreases.
- the average heating rate HR3 is 50° C./second or less. It is preferably 20° C./second or less.
- a sample of the evaluation sheet was taken from the secondary recrystallized steel sheet that had undergone the above steps, and the sample was subjected to strain relief annealing at 800° C. for 2 hours in a dry gas atmosphere containing nitrogen and hydrogen, Aging treatment was performed at 150° C. for 300 hours in a nitrogen atmosphere, the magnetic flux density and iron loss were measured by SST, and the residual carbon amount was analyzed.
- the magnetic evaluation method and the residual carbon content analysis method are the same as in Example 1.
- Table 4 also shows the magnetic flux density B8 (T), iron loss (W 17/50 ) and residual carbon content (ppm) of the steel sheet after the aging treatment. It can be seen that the residual carbon amount of 24 ppm or less, the magnetic flux density B8 of 1.89 T or more, and the iron loss W 17/50 (W/kg) of 0.80 or less are obtained. Particularly, in the invention examples D1 to D7 and D14 to D16 that satisfy the preferable conditions of the second annealing treatment and the third heating treatment described in the present embodiment, the residual carbon amount or the iron loss tends to be further reduced. In addition, in D14 and D15, the plate thickness was reduced, and also in this respect, the iron loss was a good value.
- Example 4 In Example 4, the same processes as in Invention Examples D1 to D16 of Example 3 were performed, except that the nitriding treatment was performed between the second annealing treatment and the finish annealing step. Here, the nitriding treatment was performed by holding the steel sheet at 700 to 800° C. for 30 seconds in an ammonia gas atmosphere. The results are shown in Table 5. In each of the invention examples, the residual carbon amount was 25 ppm or less, the magnetic flux density B8 was 1.88 T or more, and the iron loss W 17/50 (W/kg) was 0.85 or less.
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Abstract
Description
本願は、2019年1月16日に日本に出願された特願2019-005129号に基づき優先権を主張し、その内容をここに援用する。
脱炭焼鈍工程は、
(i-1)550℃以上、720℃未満の温度域を、40℃/秒~500℃/秒である平均加熱速度HR1で加熱する第1加熱処理と;
(i-2)前記第1加熱処理に続いて、720℃以上、下記式(2)を満たす温度T1℃以下の温度域を、5℃/秒~50℃/秒である平均加熱速度HR2で加熱する第2加熱処理と;
(ii)前記第2加熱処理に続いて、前記温度T1℃で、50~1000秒保持する第1焼鈍処理と;
を有し、
前記第1加熱処理、前記第2加熱処理及び前記第1焼鈍処理は、下記式(1)を満たす酸素分圧P1の雰囲気下で行われ、
前記第1焼鈍処理後の前記鋼板では、C量が25ppm以下である
ことを特徴とする一方向性電磁鋼板の製造方法。
0.0010≦P1≦0.20 ・・・(1)
770≦T1(℃)≦900 ・・・(2)
P2<P1 ・・・(3)
960≧T2≧T1+10 ・・・(4)
前記脱炭焼鈍工程は、
(i-1)550℃以上、720℃未満の温度域を、40~500℃/秒である平均加熱速度HR1で加熱する第1加熱処理と;
(i-2)前記第1加熱処理に続いて、720℃以上、下記式(2)を満たす温度T1℃以下の温度域を、5~50℃/秒である平均加熱速度HR2で加熱する第2加熱処理と;
(ii)前記第2加熱処理に続いて、前記温度T1℃で50~1000秒保持する第1焼鈍処理と;
を有し、
前記第1加熱処理、前記第2加熱処理及び前記第1焼鈍処理は、下記式(1)を満たす酸素分圧P1の雰囲気下で行われ、
前記第1焼鈍処理後の前記鋼板では、C量が25ppm以下である。
0.0010≦P1≦0.20 ・・・(1)
770≦T1(℃)≦900 ・・・(2)
C:0.10%以下
Cの含有量が0.10%を超えると、二次再結晶焼鈍において鋼が相変態して、二次再結晶が十分に進行せず、良好な磁束密度と鉄損特性が得られないので、Cの含有量は0.10%以下とする。鉄損低減の観点から、好ましくは0.08%以下、より好ましくは0.06%以下である。Cの検出限界が0.001%程度であるので、実用鋼板上、0.001%が実質的な下限である。
Siの含有量が0.80%未満であると、二次再結晶焼鈍において鋼が相変態して、二次再結晶が十分に進行せず、良好な磁束密度と鉄損特性が得られないので、Siの含有量は0.80%以上とする。好ましくは1.00%以上、より好ましくは2.50%以上、より好ましくは3.00%以上である。
本発明電磁鋼板において、酸可溶性Al(sol.Al)は、二次再結晶におけるインヒビターとして必須の元素である。即ち、酸可溶性Alは、AlNを形成し、安定して二次再結晶を起こさせる元素である。
Nの含有量が0.012%を超えると、冷延時、鋼板中にブリスター(空孔)が生じるうえに、鋼板の強度が上昇し、製造時の通板性が悪化するので、Nの含有量は0.012%以下とする。好ましくは0.010%以下、より好ましくは0.009%以下である。
Mnの含有量が1.00%を超えると、二次再結晶焼鈍において鋼が相変態して、二次再結晶が十分に進行せず、良好な磁束密度と鉄損特性が得られないので、Mnの含有量は1.00%以下とする。好ましくは0.50%以下、より好ましくは0.20%以下である。
Sの含有量が0.08%を超えると、熱間脆性が原因となり、熱延が著しく困難になるので、Sの含有量は0.08%以下とする。好ましくは0.04%以下、より好ましくは0.03%以下である。
Crは、一次再結晶の集合組織を改善し、二次再結晶を安定化させ、鉄損低減効果をもたらす元素である。Crの含有量が0.01%未満では、集合組織の改善効果が十分に得られないので、Crの含有量は0.01%以上とする。好ましくは0.03%以上、より好ましくは0.05%以上である。
Cuは、Crと同様に一次再結晶の集合組織を改善し、二次再結晶を安定化させ、鉄損低減効果をもたらす元素である。Cuの含有量が0.01%未満では、集合組織の改善効果が十分に得られないので、Cuの含有量は0.01%以上とする。好ましくは0.03%以上、より好ましくは0.05%以上である。
Snは、Cr及びCuと同様に一次再結晶の集合組織を改善する元素である。Snの含有量が0.01%未満では、鋼板表面の平滑化効果が十分に得られないので、Snの含有量は0.01%以上とする。好ましくは0.02%以上、より好ましくは0.03%以上である。
<製造方法>
本実施形態に係る脱炭性に優れた一方向性電磁鋼板の製造方法は、質量%で、C:0.10%以下、Si:0.80~7.00%、酸可溶性Al:0.01~0.07%、N:0.012%以下、Mn:1.00%以下、S:0.08%以下を含有し、残部Fe及び不純物からなる鋼片を熱間圧延して熱延鋼板とする熱延工程と、熱延鋼板を焼鈍する焼鈍工程と、焼鈍工程後の熱延鋼板を酸洗する酸洗工程と、酸洗工程後の熱延鋼板を冷間圧延して冷延鋼板とする冷延工程と、冷延鋼板を脱炭する脱炭焼鈍工程と、脱炭焼鈍工程後の鋼板を仕上げ焼鈍する仕上げ焼鈍工程と、を備える。
ここで、脱炭焼鈍工程は、冷延鋼板を脱炭するとともに、結晶粒径を二次再結晶に好ましい大きさに制御する(二次再結晶前の粒径を一次再結晶粒径という)工程である。
(i-1)550℃以上、720℃未満の温度域を、40~500℃/秒である平均加熱速度HR1で加熱する第1加熱処理と;
(i-2)第1加熱処理に続いて、720℃以上、下記式(2)を満たす温度T1℃以下の温度域を、5~50℃/秒である平均加熱速度HR2で加熱する第2加熱処理と;
(ii)第2加熱処理に続いて、温度T1℃で50~1000秒保持する第1焼鈍処理と;
を有する。
また、第1加熱処理、第2加熱処理及び第1焼鈍処理は、下記式(1)を満たす酸素分圧P1の雰囲気下で行われる。
さらに、第1焼鈍処理後の前記鋼板では、C量が25ppm以下である。
0.0010≦P1≦0.20・・・・・・(1)
770≦T1(℃)≦900・・・・・・(2)
脱炭焼鈍において、鋼板表面に酸化膜(例えば、Mn、Siに由来する酸化膜)が生成すると、脱炭反応が阻害されるので、酸化膜の生成を制御することは重要である。
加熱温度域:550℃以上、720℃未満
平均加熱速度HR1:40℃/秒以上、500℃/秒以下
脱炭反応を阻害するSiO2の生成挙動は、雰囲気の酸素分圧のみならず、加熱速度にも依存する。そのため、脱炭焼鈍における加熱は、SiO2の生成を極力回避する熱サイクルを経ることが重要である。
加熱温度域:720℃以上、上記式(2)を満たす温度T1℃以下
平均加熱速度HR2:5℃/秒以上、50℃/秒以下
720℃以上、温度T1℃以下の加熱温度域における加熱速度も重要である。加熱到達温度が上記式(2)を満たす温度T1℃を確実に超えない加熱速度を採用する必要がある。そこで、720℃以上、上記式(2)を満たす温度T1℃以下の温度域における平均加熱速度HR2を5℃/秒以上、50℃/秒以下とする。
焼鈍温度T1:上記式(2)を満たす温度T1℃(770℃以上、900℃以下)
保持時間:50秒以上、1000秒以下
鋼板C量:25ppm以下
脱炭反応は、鋼中炭素の拡散速度、即ち、温度と時間に大きく依存する。焼鈍温度T1が770℃以下であると、脱炭反応の進行が困難になるので、焼鈍温度T1は770℃以上とする。好ましくは800℃以上、より好ましくは810℃以上である。
P2<P1 ・・・(3)
960≧T2≧T1+10 ・・・(4)
焼鈍雰囲気の酸素分圧P2:P1未満(上記式(3))
焼鈍温度T2:T1+10℃以上、960℃以下(上記式(4))
保持時間:3秒以上、500秒以下
第2焼鈍処理の焼鈍雰囲気である酸素分圧P2を、第1焼鈍処理の焼鈍雰囲気の酸素分圧P1(0.0010以上、0.20以下)と同じにすると、鋼板表面に酸化膜が生成するので、第2焼鈍処理の焼鈍雰囲気の酸素分圧P2は、上記酸素分圧P1未満とする。好ましくは、P1×0.1以下である。
脱炭焼鈍工程後の鋼板に窒化処理を行ってもよい。この窒化処理の方法は特に限定されず、アンモニア等の窒化能のある雰囲気ガス中で行う方法等が例として挙げられる。窒化処理の処理時間や処理条件は特に限定されず、鋼板中のN量が0.005%以上、好ましくは、鋼板中の(N量)/(酸可溶性Al量)の比率が2/3以上となるように窒化処理を行えばよい。
この窒化処理工程は、鋼片を1300℃未満の温度で加熱した後に熱間圧延工程を行う場合(低温スラブ加熱又は中温スラブ加熱と呼ばれる場合がある)に、特に有効である。一方、鋼片を1300℃以上の温度で加熱してインヒビターと呼ばれる微細析出物をほぼ完全に固溶させた後に熱間圧延工程を行う場合(高温スラブ加熱と呼ばれる場合がある)には、窒化処理工程を行わなくてもよい。
表1に示す化学組成のインゴットを真空溶解して鋳造し、鋼片とした。この鋼片を1150℃に加熱し、熱間圧延に供し、板厚2.3mmの熱延鋼板とした。この熱延鋼板を、1000~1100℃で2分間焼鈍した後、酸洗し、酸洗後、冷間圧延に供し、最終板厚0.23~0.30mmの冷延鋼板とした。
表1に示す化学組成のインゴットを真空溶解して鋳造し、鋼片とした。この鋼片を1150℃に加熱し、熱間圧延に供し、板厚2.3mmの熱延鋼板とした。この熱延鋼板を、1000~1100℃で2分間焼鈍した後、酸洗し、酸洗後、冷間圧延に供し、最終板厚0.23~0.30mmの冷延鋼板とした。
表1に示す化学組成のインゴットを真空溶解して鋳造し、鋼片とした。この鋼片を1150℃に加熱し、熱間圧延に供し、板厚2.3mmの熱延鋼板とした。この熱延鋼板を、1000~1100℃で2分間焼鈍した後、酸洗し、酸洗後、冷間圧延に供し、最終板厚0.23~0.30mmの冷延鋼板とした。
実施例4では、窒化処理を第2焼鈍処理と仕上げ焼鈍工程との間で行った他は実施例3の発明例D1~D16と同様の処理を行った。ここで、窒化処理は、鋼板をアンモニアガス雰囲気中で、700~800℃にて30秒保持することで行った。結果を表5に示す。いずれの発明例でも、残留炭素量は25ppm以下、磁束密度B8は1.88T以上、鉄損W17/50(W/kg)は0.85以下となった。
Claims (5)
- 質量%で、C:0.10%以下、Si:0.80~7.00%、酸可溶性Al:0.01~0.07%、N:0.012%以下、Mn:1.00%以下、S:0.08%以下を含有し、残部Fe及び不純物からなる鋼片を熱間圧延して熱延鋼板とする熱延工程と;
前記熱延鋼板を焼鈍する焼鈍工程と;
前記焼鈍工程後の前記熱延鋼板を酸洗する酸洗工程と;
前記酸洗工程後の前記熱延鋼板を冷間圧延して冷延鋼板とする冷延工程と;
前記冷延鋼板を脱炭する脱炭焼鈍工程と;
前記脱炭焼鈍工程後の鋼板を仕上げ焼鈍する仕上げ焼鈍工程と;
を備え、
前記脱炭焼鈍工程は、
(i-1)550℃以上、720℃未満の温度域を、40~500℃/秒である平均加熱速度HR1で加熱する第1加熱処理と;
(i-2)前記第1加熱処理に続いて、720℃以上、下記式(2)を満たす温度T1℃以下の温度域を、5~50℃/秒である平均加熱速度HR2で加熱する第2加熱処理と;
(ii)前記第2加熱処理に続いて、前記温度T1℃で50~1000秒保持する第1焼鈍処理と;
を有し、
前記第1加熱処理、前記第2加熱処理及び前記第1焼鈍処理は、下記式(1)を満たす酸素分圧P1の雰囲気下で行われ、
前記第1焼鈍処理後の前記鋼板では、C量が25ppm以下である
ことを特徴とする一方向性電磁鋼板の製造方法。
0.0010≦P1≦0.20 ・・・(1)
770≦T1(℃)≦900 ・・・(2) - 前記脱炭焼鈍工程が、前記第1焼鈍処理の後に、下記式(3)を満たす酸素分圧P2の雰囲気下で、下記式(4)を満たす温度T2℃で3~500秒保持する第2焼鈍処理を更に有する
ことを特徴とする請求項1に記載の一方向性電磁鋼板の製造方法。
P2<P1 ・・・(3)
960≧T2≧T1+10 ・・・(4) - 前記第1焼鈍処理と前記第2焼鈍処理との間に第3加熱処理を更に有し、
前記第3加熱処理は、前記T1℃から前記T2℃までの温度域を、5~50℃/秒である平均加熱速度HR3で加熱する
ことを特徴とする請求項2に記載の一方向性電磁鋼板の製造方法。 - 前記鋼片が、質量%で、Cr:0.01~0.50%、Cu:0.01~0.50%、Sn:0.01~0.02%の1種又は2種以上を含有する
ことを特徴とする請求項1~3のいずれか1項に記載の一方向性電磁鋼板の製造方法。 - 前記脱炭焼鈍工程と前記仕上げ焼鈍工程との間に、前記脱炭焼鈍工程後の前記鋼板を窒化処理する窒化処理工程をさらに備え、
前記仕上げ焼鈍工程では、前記窒化処理工程後の鋼板を仕上げ焼鈍する
ことを特徴とする、請求項1~4のいずれか1項に記載の一方向性電磁鋼板の製造方法。
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JP2019005129A (ja) | 2017-06-23 | 2019-01-17 | 株式会社三共 | 遊技機 |
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EP3913078A1 (en) | 2021-11-24 |
JPWO2020149348A1 (ja) | 2021-11-25 |
BR112021013677A2 (pt) | 2021-09-14 |
CN113272457A (zh) | 2021-08-17 |
KR20210110866A (ko) | 2021-09-09 |
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