JP2634847B2 - Method of drying annealing separator for grain-oriented electrical steel sheets - Google Patents
Method of drying annealing separator for grain-oriented electrical steel sheetsInfo
- Publication number
- JP2634847B2 JP2634847B2 JP63085335A JP8533588A JP2634847B2 JP 2634847 B2 JP2634847 B2 JP 2634847B2 JP 63085335 A JP63085335 A JP 63085335A JP 8533588 A JP8533588 A JP 8533588A JP 2634847 B2 JP2634847 B2 JP 2634847B2
- Authority
- JP
- Japan
- Prior art keywords
- grain
- steel sheet
- oriented electrical
- annealing
- annealing separator
- 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.)
- Expired - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
- C21D8/1283—Application of a separating or insulating coating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Thermal Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Electromagnetism (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
- Heat Treatment Of Sheet Steel (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は方向性電磁鋼板の焼鈍分離剤乾燥方法に係わ
り、欠陥がなく均一ですぐれたグラス被膜とともに、磁
気特性もすぐれた方向性電磁鋼板が得られる焼鈍分離剤
乾燥方法に関する。Description: TECHNICAL FIELD The present invention relates to a method for drying an annealing separator for grain-oriented electrical steel sheets, and a grain-oriented electrical steel sheet having excellent and uniform glass coating without defects and excellent magnetic properties. And a method for drying an annealing separator.
［従来の技術］ 方向性電磁鋼板は、Si4wt％（以下％と略す）以下を
含有する珪素鋼スラブを熱延し、必要に応じて熱延板応
を焼鈍し、１回又は中間焼鈍をはさんで２回以上の冷延
工程により、最終仕上厚みの冷延板を得、次に脱炭焼鈍
を行った後、MgOを主成分とする焼鈍分離剤を水に溶か
してスラリー状とし、これを塗布し乾燥し、仕上焼鈍を
施して、Goss方位をもった２次再結晶粒を発達させ、更
にS,Nなどの不純物を除去するとともに、グラス被膜を
形成する一連の工程を経て製造される。[Prior art] A grain-oriented electrical steel sheet is obtained by hot-rolling a silicon steel slab containing Si4wt% (hereinafter abbreviated as%) or less, annealing the hot-rolled sheet as needed, and performing one or intermediate annealing. In two or more cold-rolling steps, a cold-rolled sheet with a final finish thickness is obtained, and then decarburization annealing is performed, and an annealing separator mainly containing MgO is dissolved in water to form a slurry. It is manufactured through a series of steps of applying, drying and finish annealing to develop secondary recrystallized grains having Goss orientation, further removing impurities such as S and N, and forming a glass film. You.
方向性電磁鋼板のグラス被膜は、密着性がよく、シモ
フリやスパングル等と称されるような欠陥がなく、外観
が均一で光沢があり、また鋼板への付与張力が大である
等の特性を有することが望まれる。The glass coating of grain-oriented electrical steel sheet has properties such as good adhesion, no defects such as shimofuri and spangles, uniform appearance and gloss, and high applied tension to the steel sheet. It is desirable to have.
焼鈍分離剤は方向性電磁鋼板への付着性を高め、また
鋼板板面に一様に塗布されるために、前述の如くスラリ
ー状にして塗布されるが、焼鈍分離剤のMgOは水と反応
し水酸化マグネシウムが生成され、これが鋼板への持込
み水分となり、グラス被膜の形成に悪影響を及ぼしてい
る。Since the annealing separator enhances the adhesion to grain-oriented electrical steel sheets and is uniformly applied to the steel sheet surface, it is applied as a slurry as described above, but the MgO of the annealing separator reacts with water. Then, magnesium hydroxide is generated, which becomes the water carried into the steel sheet, and adversely affects the formation of the glass film.
ところで、従来から方向性電磁鋼板のグラス被膜の改
善と向上について検討されている。例えば特開昭53−15
205号公報では水和水分を１〜４％としたMgOに、TiO2と
Al2S3またはZnSを添加した焼鈍分離剤を用いて、鉄損の
改善とグラス被膜の向上を図ることが提案されている。By the way, conventionally, the improvement and improvement of the glass coating of the grain-oriented electrical steel sheet have been studied. For example, JP-A-53-15
The hydration moisture 1-4% and the MgO in 205 discloses a TiO 2
It has been proposed to improve the iron loss and the glass coating by using an annealing separator containing Al 2 S 3 or ZnS.
また、特開昭58−189374号公報では、MgOを1300℃以
上の高温で焼成して不活性化し、これをスラリーとする
さいは温水中で水和させて、450℃以上の温度での灼熱
減量率を2.0〜10％とし、これを鋼板に塗布し、外観が
均一で密着性のよいグラス被膜の形成を図ることが提案
されている。Further, in JP-A-58-189374, MgO is inactivated by firing at a high temperature of 1300 ° C. or more, and when it is converted into a slurry, it is hydrated in warm water and burnt at a temperature of 450 ° C. or more. It has been proposed to set the weight loss rate to 2.0 to 10%, apply this to a steel plate, and to form a glass coating having a uniform appearance and good adhesion.
これらによって、グラス被膜と磁気特性とも幾分改善
された方向性電磁鋼板が得られるようになっている。As a result, a grain-oriented electrical steel sheet having somewhat improved glass coating and magnetic properties can be obtained.
［発明が解決しようとする課題］ しかし、焼鈍分離剤を塗布した方向性電磁鋼板の仕上
焼鈍は、コイル上で約1000〜1250℃温度にて行なわれる
が、コイル内に温度偏差が生じる。とくに加熱時にはコ
イル半径方向、軸方向とも温度偏差が大きく、例えば昇
温時の500〜600℃間には100〜200℃にもなる。[Problems to be Solved by the Invention] However, finish annealing of a grain-oriented electrical steel sheet coated with an annealing separating agent is performed at a temperature of about 1000 to 1250 ° C on a coil, but a temperature deviation occurs in the coil. In particular, during heating, the temperature deviation is large in both the coil radial direction and the axial direction. For example, the temperature deviation between 500 and 600 ° C. during heating increases to 100 to 200 ° C.
一方、鋼板に塗布された焼鈍分離剤は、仕上焼鈍の加
熱時にまず水和分が乾燥作用を受けるが、前記温度偏差
に起因してコイル内で水分の放出程度に偏差が生じ、板
間の露点が異なる。On the other hand, the annealing separator applied to the steel sheet, the hydration first undergoes a drying action at the time of heating for finish annealing, but due to the temperature deviation, a deviation occurs in the degree of water release in the coil, and between the plates Dew point is different.
また、焼鈍分離剤は方向性電磁鋼板の表面に脱炭焼鈍
で生じたSiO2を含む酸化膜と反応し、グラス被膜を形成
するが、このさい、板間の露点が異なることに起因して
部分的に鋼板は追加酸化され、グラス被膜に欠陥例えば
シモフリ，スパングル，変色等が生じる。In addition, the annealing separator reacts with the oxide film containing SiO 2 generated by the decarburizing annealing on the surface of the grain-oriented electrical steel sheet, and forms a glass film, but due to the difference in the dew point between the sheets. Partially the steel sheet is additionally oxidized, causing defects in the glass coating, for example, shimofuri, spangles, discoloration and the like.
これらの問題は、十分に満足できるまで解決されてい
るとはいえない。These problems have not been solved until fully satisfactory.
本発明はこれらの問題を解決するもので、方向性電磁
鋼板のコイルの全福，全長にわたって、密着性、外観と
もすぐれたグラス被膜を形成し、あわせて磁気特性がす
ぐれたものを得ることを目的とする。The present invention solves these problems, and forms a glass coating with excellent adhesion and appearance over the entire length and length of a coil of grain-oriented electrical steel sheet, and at the same time, obtains a coil having excellent magnetic properties. Aim.
［課題を解決するための手段］ 以下に本発明について詳細に説明する。[Means for Solving the Problems] Hereinafter, the present invention will be described in detail.
本発明者達は、仕上焼鈍における方向性電磁鋼板コイ
ルの板間の露点の差異発生防止について検討した。The present inventors have studied how to prevent the occurrence of a difference in dew point between sheets of a grain-oriented electrical steel sheet coil in finish annealing.
これまでは焼鈍分離剤を高温焼成して不活性化し、水
分との反応を少なくして、板間の露点の変動防止策がと
られたり、あるいは焼鈍分離剤をスラリーとするさい、
水の温度を下げることがなされていた。Until now, the annealing separator was fired at a high temperature to deactivate it and reduce the reaction with moisture to prevent the fluctuation of the dew point between plates, or when the annealing separator was turned into a slurry,
The water temperature had been reduced.
ところで本発明者達は焼鈍分離剤を水に混溶してスラ
リー状として、方向性電磁鋼板に塗布した後の乾燥を急
速加熱すると、焼鈍分離剤は鋼板に強く付着したまま水
和分の生成が抑制され、仕上焼鈍での板間の露点に差異
が生ぜず、被膜特性，磁気特性ともすぐれることを知見
した。By the way, the present inventors mixed the annealed separating agent in water to form a slurry, applied the coated steel to the grain-oriented electrical steel sheet, and rapidly heated the drying. Was found to be suppressed, and there was no difference in the dew point between the plates during the finish annealing, and the coating properties and magnetic properties were excellent.
本発明はこの知見に基づいてなされたものである。即
ち脱炭焼鈍までの製造条件としては珪素鋼スラブを熱間
圧延し、焼鈍して１回または中間焼鈍をはさんで２回以
上の冷間圧延により所定最終板厚とし脱炭焼鈍される如
何なるものでもよい。The present invention has been made based on this finding. That is, the production conditions up to the decarburizing annealing are any conditions in which the silicon steel slab is hot-rolled, annealed once, or cold-rolled two or more times after intermediate annealing to obtain a predetermined final thickness and decarburizing annealing. It may be something.
脱炭焼鈍により方向性珪素鋼板は脱炭されるととも
に、その鋼板表面にはSiO2を含むサブスケールが形成さ
れる。次にMgOを主成分とする焼鈍分離剤を水に懸濁さ
せスラリー状とし、ロールコーター等の塗布手段により
上述の鋼板上に塗布する。The directional silicon steel sheet is decarburized by the decarburization annealing, and a subscale containing SiO 2 is formed on the surface of the steel sheet. Next, an annealing separator containing MgO as a main component is suspended in water to form a slurry, and the slurry is applied onto the above-described steel sheet by an application means such as a roll coater.
焼鈍分離剤はMgOを主成分とする他にTiO2、硫化物あ
るいはSiO2のコロイダル粒子などの添加物を配合したも
のが用いられるが、その配合添加物を特定する必要はな
い。As the annealing separator, a mixture of additives such as TiO 2 , sulfide, or colloidal particles of SiO 2 in addition to MgO as a main component is used, but it is not necessary to specify the additive.
塗布のちに乾燥させるが、加熱乾燥においての昇温速
度が重要である。加熱温度は200〜300℃であり、その温
度に80℃／秒以上の速度で急速加熱する。Drying is performed after coating, and the rate of temperature rise in heating and drying is important. The heating temperature is 200 to 300 ° C, and the temperature is rapidly increased to 80 ° C / sec or more.
昇温速度が80℃／秒以上になるとMgOと水分の化合を
ほぼ完全に抑え、化合水量を減少させることができる。
化合水は、100℃に加熱され蒸発を完了するまでの間の
沸とう水に、MgOが浸漬した状態において、MgO粒内への
水分の侵入により生成する。When the temperature rise rate is 80 ° C./sec or more, the compound of MgO and water is almost completely suppressed, and the amount of compound water can be reduced.
Compound water is generated by infiltration of water into MgO particles in a state in which MgO is immersed in boiling water heated to 100 ° C. until evaporation is completed.
従って水分が蒸発を完了するまでの時間を短縮し、水
分の粒内への侵入を抑えることにより化合水量を減少し
得るが、第１図に示すように、鋼板を80℃／秒以上の加
熱速度にて加熱，乾燥を行えば、水分がMgO粒内へ侵入
する時間を与えず、化合水の生成をほぼ完全に抑えるこ
とが可能である。Therefore, the amount of compounded water can be reduced by shortening the time until the completion of the evaporation of the water and suppressing the penetration of the water into the grains. However, as shown in FIG. 1, the steel sheet is heated at 80 ° C./sec or more. If heating and drying are performed at a speed, it is possible to almost completely suppress the generation of compound water without giving time for water to enter the MgO particles.
鋼板は80℃／秒以上の加熱速度を得るために、誘導加
熱等の急速加熱法を用いて加熱，乾燥される。なお従来
の加熱速度は20〜40℃／分であった。The steel sheet is heated and dried using a rapid heating method such as induction heating in order to obtain a heating rate of 80 ° C./sec or more. The conventional heating rate was 20 to 40 ° C./min.
乾燥の後はコイルに捲取られ、仕上焼鈍される。仕上
焼鈍はH2,N2の単独または混合雰囲気、あるいはさらに
必要に応じてO2やAr微量添加された雰囲気下で、例えば
1000〜1200℃に加熱されて行なわれる。After drying, it is wound on a coil and finish-annealed. The finish annealing is performed under an atmosphere of H 2 or N 2 alone or in a mixed atmosphere, or further, if necessary, in an atmosphere in which a small amount of O 2 or Ar is added.
It is performed by heating to 1000 to 1200 ° C.
この焼鈍において加熱時に方向性電磁鋼板のコイル内
に温度偏差が不可避的に生じるが、鋼板に塗布した焼鈍
分離剤の乾燥を前述の如くして行っているので、過酸化
が生じる程の板間の露点変動がない。During this annealing, a temperature deviation inevitably occurs in the coil of the grain-oriented electrical steel sheet during heating. However, since the annealing separator applied to the steel sheet is dried as described above, the gap between the sheets is large enough to cause peroxidation. No fluctuation of dew point.
このため、密着性，色調，コイル内における均一さに
ともにすぐれたグラス被膜が形成される。また磁気特性
もすぐれる。For this reason, a glass film having excellent adhesion, color tone, and uniformity in the coil is formed. Also, the magnetic properties are excellent.
［実 施 例］ Si3.2％,S0.02％,Al0.030％,N0.006％を含み、残部が
鉄および不可避的不純物からなる方向性珪素鋼板のスラ
ブを3mm厚に熱間圧延し、1120℃で３分間の熱延板焼鈍
を施した後、冷間圧延し、最終板厚を0.3mmとした。[Example] A slab of grain-oriented silicon steel sheet containing 3.2% of Si, 0.02% of S, 0.030% of Al, and 0.006% of N and the balance of iron and unavoidable impurities was hot-rolled to a thickness of 3mm. After hot-rolled sheet annealing at 1120 ° C. for 3 minutes, the sheet was cold-rolled to a final sheet thickness of 0.3 mm.
次に850℃で３分間露点60℃、H270％からなる雰囲気
下で連続焼鈍し、この方向性珪素鋼板にMgOを主成分と
する焼鈍分離剤に水を添加し懸濁させてスラリー状とし
ロールコーターにて塗布した。Then 3 min dew point 60 ° C. at 850 ° C., continuously in an atmosphere composed of H 2 70% annealed, water was added and suspended in a slurry form in the annealing separator composed mainly of MgO to the grain-oriented silicon steel sheet It was applied by a roll coater.
次に焼鈍分離剤を塗布した該鋼板は乾燥炉で200,100,
80,50℃／秒の昇温速度で300℃に加熱して乾燥した。Next, the steel sheet coated with the annealing separator was placed in a drying oven for 200, 100,
It was heated to 300 ° C. at a heating rate of 80,50 ° C./sec and dried.
次にコイル状に捲取り、仕上焼鈍を1210℃で行なっ
た。焼鈍後の鋼板について磁気特性、グラス被膜特性を
調査し、その結果を第１表に示す。Next, it was wound into a coil and finish annealing was performed at 1210 ° C. The magnetic properties and glass coating properties of the annealed steel sheet were investigated, and the results are shown in Table 1.
［発明の効果］ 以上のように、本発明によるとグラス被膜、磁気特性
ともすぐれた方向性電磁鋼板が得られる効果がある。 [Effects of the Invention] As described above, according to the present invention, there is an effect that a grain-oriented electrical steel sheet having excellent glass coating and magnetic properties can be obtained.
第１図は方向性電磁鋼板の焼鈍分離剤乾燥における昇温
速度による化合水生成率を示す図表である。FIG. 1 is a chart showing a compound water generation rate depending on a heating rate in drying an annealing separator of a grain-oriented electrical steel sheet.
Claims (1)
脱炭焼鈍し、鋼板表面にSiO2を含む酸化膜を形成し、該
酸化膜上に酸化マグネシアを主成分とする焼鈍分離剤を
塗布し、乾燥し、仕上焼鈍する方向性電磁鋼板の製造に
おいて、酸化マグネシアを主成分とする焼鈍分離剤を水
に混溶して方向性電磁鋼板に塗布した後、該鋼板を昇温
速度80℃／秒以上で加熱し、焼鈍分離剤を乾燥せしめる
ことを特徴とする方向性電磁鋼板の焼鈍分離剤乾燥方
法。(1) cold-rolling a grain-oriented electrical steel to a predetermined thickness;
Decarburizing annealing, forming an oxide film containing SiO 2 on the surface of the steel sheet, applying an annealing separator containing magnesia oxide as a main component on the oxide film, drying, and finish annealing. After mixing an annealing separator mainly composed of magnesia oxide in water and applying it to a grain-oriented electrical steel sheet, the steel sheet is heated at a heating rate of 80 ° C./sec or more to dry the annealing separator. A method for drying an annealing separator for grain-oriented electrical steel sheets.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63085335A JP2634847B2 (en) | 1988-04-08 | 1988-04-08 | Method of drying annealing separator for grain-oriented electrical steel sheets |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63085335A JP2634847B2 (en) | 1988-04-08 | 1988-04-08 | Method of drying annealing separator for grain-oriented electrical steel sheets |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01259126A JPH01259126A (en) | 1989-10-16 |
| JP2634847B2 true JP2634847B2 (en) | 1997-07-30 |
Family
ID=13855769
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63085335A Expired - Lifetime JP2634847B2 (en) | 1988-04-08 | 1988-04-08 | Method of drying annealing separator for grain-oriented electrical steel sheets |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2634847B2 (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5911670A (en) * | 1982-07-12 | 1984-01-21 | Toshiba Corp | Semiconductor integrated circuit device |
-
1988
- 1988-04-08 JP JP63085335A patent/JP2634847B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01259126A (en) | 1989-10-16 |
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