CN1202284C - 用退火隔离剂涂覆电炉钢带的方法 - Google Patents
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Abstract
本发明涉及用氧化物粉末作为退火隔离剂涂覆电炉钢带的一种方法，它通过涂覆一种主要含有氧化镁和至少一种添加剂的水溶液来进行，添加剂包括一种含氯化合物。本发明的特征在于加入到水溶液中的添加剂是氯化铵(NH4Cl或NH4Cl·nH2O)。
Description
本发明涉及用氧化物粉末作为退火隔离剂(Gluehseparator)涂覆电炉钢带的一种方法，它通过涂覆一种主要含有氧化镁和至少一种添加剂的水溶液来进行，添加剂包括一种含氯化合物，其特征在于加入到水溶液中的添加剂是氯化铵或氯化铵水合物。
常规地，电炉钢带通过熔化合金，铸成钢板，将板热轧，将热钢条退火以建立抑制剂相，将热钢条冷轧，将冷钢条脱碳退火，涂覆一种主要含有氧化镁的粘合隔离剂作为在紧接着的为实现二次再结晶而进行的卷绕成卷材的电炉钢带的最后退火过程中的粘合保护。
由硅钢条制成的晶粒定向的电工钢片，因其在变压器中的应用，必须具有一种允许在轧制方向可容易地磁化的结构(Goss结构)，因此将它们与晶粒生长抑制剂，例如铝和氮、锰和硫、铜和硫、锰和硒熔合。这些物质生成化合物例如氮化铝、硫化锰、硫化铜、硒化锰，它们以微粒分散的形式沉淀，阻碍了晶粒在再结晶退火期间的过早生长。其结果是，优选的Goss取向的晶粒生长在二次再结晶期间产生。
颗粒物细分散的分布尽可能均匀，这对抑制剂的颗粒生长抑制效应是非常重要的。这在热钢条退火过程中和/或在紧跟着脱碳进行的氮含量增加过程中发生。抑制剂的分布仍然可以受影响，直至在选择性的晶粒生长刚开始之前。已被确认的共识是退火隔离剂的组成对晶粒生长抑制剂的分布也特别重要。因此将少量的其它物质加入到基本上由氧化镁组成的退火隔离剂中，以便改善表面，提高极化和降低反复磁化损耗。
DE 29 47 945 C2建议加入硼和钠的化合物，而EP 0 232 537 B1建议加入钛、硼或硫的化合物。刚开始，加入氯化物通常被认为是有害的。但是，按照DE 34 40 344，将硫酸锑与锑、锶、钛或锆的氯化物相结合加入，导致在磁性方面获得改善。但是，硫酸锑在水中难溶，而且是有毒的。按照DE 44 09 691 A1的教导，应该加入可很好地溶于水的钠的化合物或细分散的氧化铝化合物，在此可以额外加入金属氯化物。EP 0 789 093 A1揭示了卤素或卤化物用作添加剂。按照EP 0416 420 A2，明确限定的氯的含量应该通过在退火隔离剂中加入镁、钙、钠和/或钾的氯化物来进行调节。在该文献中所列出的氯化物的缺点是与它们同时引入了一些元素，在长时间退火之后，它们在钢条表面上留下了干扰固体残余物。
本发明的目的是防止氮化物和/或硫化物抑制剂在最后退火过程的加热阶段过早降解，或者在此阶段重新生成氮化物抑制剂。在此阶段通过退火气体与基材或者与包含在其中的抑制剂的反应，抑制剂被决定性地影响。在此退火隔离剂的组成起重要的作用。
为解决这个问题，在按照本发明明确类型的方法中，加入到水溶液中的添加剂是氯化铵(NH4Cl或NH4Cl·nH2O)。添加剂的量应如此选择，以使氯浓度，基于在退火隔离剂中的氧化镁的重量比例，为0.01～0.10％重量百分比，优选为0.02～0.05％重量百分比。
按照本发明的另一种添加剂可以是焦磷酸钠，优选以这样的量加入，以使钠浓度，基于在退火隔离剂中的氧化镁的比例，被调节为0.02～0.05％重量百分比。
通过按照本发明加入到退火隔离剂中的物质如此控制层的形成，以使玻璃薄膜在低温下形成，并且其具有如此高的密度以至阻碍在电炉钢带中退火气体和抑制剂之间相互作用。
通过实施按照本发明的方法不仅改善了反复磁化损耗，而且明显提高了取向锐度-也就是说获得了一个显著的Goss结构，并由此通过在制成的钢条上进行区域精炼(Domaenenfeinung)例如通过激光处理获得大大改善的电势。所提供的添加剂还有以下优点，即它们容易获取，具有令人满意的水溶性、便宜和简单的可行性，还有毒性和生态方面的相容性。
在按照本发明的方法中，氯和钠在退火隔离剂中的浓度被相互独立地调节。氯和钠以不同化合物的形式被引入水溶液中，从而确保氯或钠各自的浓度分别最佳化。
在高度可渗透的电工钢片的情况下，按照本发明在退火隔离剂中添加氯和必要的话钠的一个特别的优点是磁性对最后退火过程中的条件差异的响应明显弱得多。因为最后的退火在卷材中进行，不可避免地，在钢条的横向和纵向方向上，退火条件将产生差异。退火条件的差异尤其涉及退火气体的露点。以含水浆体的形式涂覆然后干燥的氧化镁不可避免地含有一定比例的氢氧化镁。在最后退火过程中的加热阶段，氢氧化镁被热分解成氧化镁和水。释放的水使退火气体的露点升高。不利的露点可能对抑制剂的分布产生负面效应。
选择氯化铵作为退火隔离剂的氯源(Chlorspender)特别重要，与其它已知的氯化合物相比较具有两个决定性的优点。一方面，在最后的退火过程中的加热条件下，氯的键合伙伴应以一种对环境友好的方式经气相送走，而不留下固体残余物。此外，正如前面所提到的，必须防止氮化物抑制剂在电炉钢带中过早降解。氯化铵以一种杰出的方式满足这两个条件。NH3基团在最后的退火过程中被热分离掉。此外，作为避免钢条中的氮化物抑制剂降解的先决条件，此气体提高了卷材绕组之间的氮气分压，并且被分解成无害的氮气和氢气。
磁性的进一步改进可以通过应用焦磷酸钠作为加至退火隔离剂中附加的添加剂而获得。焦磷酸钠促进了氯添加剂的性能改进效应。它还阻碍了钢条中氮含量的明显提高。
现在通过下面的实施例更详细地说明本发明。
实施例1
在厚度为0.23毫米的高渗透性的晶粒定向的电工钢片的工业生产中，氯的浓度通过氯化铵调节，与氯化锑作为退火隔离剂中的添加剂进行比较。
表1
氯浓度(ppm)，基于在退火隔离剂中的氧化镁
| NH4Cl | SbCl3 | |
| 在氧化镁中的比例 | 200 | 200 |
| 来自添加剂 | 120/240 | 170 |
| 总氯量 | 320/440 | 370 |
图1显示了以反复磁化损耗P1，7.为基础的结果。通过按照本发明应用氯化铵调节氯浓度，与应用氯化锑相比较，磁性明显改善。
实施例2
在厚度为0.30毫米的高渗透性的晶粒定向的电工钢片的工业生产中，通过添加剂氯化铵和焦磷酸钠，氯和钠的浓度被调节到以下值：
表2
氯和钠的浓度(ppm)
| Cl | Na | |
| 在氧化镁中的比例 | 200 | 20 |
| 来自NH4Cl | 144 | |
| 来自Na4P2O7 | 280 | |
| 总量 | 344 | 300 |
表3显示了以反复磁化损耗P1，7.为基础的结果。
表3
反复磁化损耗P1，7(瓦/千克)
| 制成的钢条的激光处理 | 无添加剂 | 有钠和氯 |
| 无 | 1.06 | 0.99 |
| 有 | 1.02 | 0.89 |
通过按照本发明调节钠和氯的浓度，磁性明显改善。反复磁化损耗大约降低7％。在按照本发明调节钠和氯在退火隔离剂中的浓度时，在制成的钢条上进行的用于区域精炼的激光处理，其有效性特别明显。
实施例3
在厚度为0.27毫米的高渗透性的晶粒定向的电工钢片的工业生产中，通过加入氯化铵和焦磷酸钠，氯和钠在退火隔离剂中的浓度被相继调节到以下值：
表4
氯和钠的浓度(ppm)
| Cl | Na | |
| 在氧化镁中的比例 | 200 | 20 |
| 来自NH4Cl | 275 | |
| 来自Na4P2O7 | 280 | |
| 总量 | 475 | 300 |
表5显示了以反复磁化损耗P1，7.为基础的结果。
表5
反复磁化损耗P1，7.(瓦/千克)
| 制成的钢条的激光处理 | 有氯(来自NH4Cl) | 有Cl和Na(来自NH4Cl及Na4P2O7) |
| 无 | 0.91 | 0.88 |
| 有 | - | 0.77 |
通过按照本发明调节氯浓度，反复磁化的损耗大约降低2％。按照本发明额外调节钠的浓度，可再降低损耗3％。激光处理的有效性明显提高，正如图2所证实的。
Claims (5)
1.用退火隔离剂涂覆电炉钢带的方法，它通过涂覆一种含有氧化镁和至少一种添加剂的水溶液来进行，添加剂包括含氯的化合物，其特征在于加入到水溶液中的添加剂是氯化铵或氯化铵水合物。
2.根据权利要求1的方法，其特征在于氯化铵被加入到水溶液中，以使氯在退火隔离剂中的浓度为0.01～0.10％，基于退火隔离剂中的氧化镁的重量。
3.根据权利要求2的方法，其特征在于氯的浓度被调节为0.02～0.05％，基于退火隔离剂中的氧化镁的重量。
4.根据权利要求1～3之任一项的方法，其特征在于焦磷酸钠或焦磷酸钠水合物作为另一种添加剂也被加入水溶液中。
5.根据权利要求4的方法，其特征在于钠的浓度被调节到0.02～0.05％，基于退火隔离剂中的氧化镁的重量。
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| DE19750066A DE19750066C1 (de) | 1997-11-12 | 1997-11-12 | Verfahren zum Beschichten von Elektrostahlbändern mit einem Glühseparator |
| DE19750066.8 | 1997-11-12 |
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| US (1) | US6423156B1 (zh) |
| EP (1) | EP1029113B1 (zh) |
| JP (1) | JP4194753B2 (zh) |
| KR (1) | KR100560178B1 (zh) |
| CN (1) | CN1202284C (zh) |
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| AU (1) | AU730568B2 (zh) |
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| ID (1) | ID27132A (zh) |
| PL (1) | PL187121B1 (zh) |
| RU (1) | RU2198958C2 (zh) |
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| IT1306157B1 (it) * | 1999-05-26 | 2001-05-30 | Acciai Speciali Terni Spa | Procedimento per il miglioramento di caratteristiche magnetiche inlamierini di acciaio al silicio a grano orientato mediante trattamento |
| CN102443736B (zh) * | 2010-09-30 | 2013-09-04 | 宝山钢铁股份有限公司 | 一种高磁通密度取向硅钢产品的生产方法 |
| KR101480498B1 (ko) * | 2012-12-28 | 2015-01-08 | 주식회사 포스코 | 방향성 전기강판 및 그 제조방법 |
| EP4027357A1 (de) | 2020-12-18 | 2022-07-13 | Vacuumschmelze GmbH & Co. KG | Fecov-legierung und verfahren zum herstellen eines bands aus einer fecov-legierung |
| DE102020134301A1 (de) | 2020-12-18 | 2022-06-23 | Vacuumschmelze Gmbh & Co. Kg | Weichmagnetische Legierung und Verfahren zum Herstellen einer weichmagnetischen Legierung |
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| US3950575A (en) * | 1973-01-23 | 1976-04-13 | Nippon Steel Corporation | Heat treatment of metals in a controlled surface atmosphere |
| IT1127263B (it) * | 1978-11-28 | 1986-05-21 | Nippon Steel Corp | Sostanza di separazione da utilizzare nella fase di ricottura di strisce di acciaio al silicio a grani orientati |
| JPS60145382A (ja) * | 1984-01-09 | 1985-07-31 | Nippon Steel Corp | 磁気特性、皮膜特性とも優れた方向性電磁鋼板の製造方法 |
| JPS62156226A (ja) * | 1985-12-27 | 1987-07-11 | Nippon Steel Corp | 均一なグラス皮膜を有し磁気特性が優れた方向性電磁鋼板の製造方法 |
| JPS62288116A (ja) * | 1986-06-03 | 1987-12-15 | Mitsui Mining & Smelting Co Ltd | 硫化マンガン（２）粉末の製造方法 |
| EP0416420B1 (en) * | 1989-09-08 | 1994-12-14 | Armco Inc. | Magnesium oxide coating for electrical steels and the method of coating |
| JP3399969B2 (ja) * | 1992-01-10 | 2003-04-28 | 川崎製鉄株式会社 | 磁気特性の優れた方向性電磁鋼板の製造方法 |
| JPH06192732A (ja) * | 1992-12-24 | 1994-07-12 | Kawasaki Steel Corp | 磁気特性に優れた一方向性電磁鋼板の製造方法 |
| RU2069237C1 (ru) * | 1992-12-30 | 1996-11-20 | Предприятие "Виктор" | Состав для получения антифрикционных покрытий на поверхности стальных изделий |
| DE4409691A1 (de) * | 1994-03-22 | 1995-09-28 | Ebg Elektromagnet Werkstoffe | Verfahren zur Herstellung von Elektroblechen mit einem Glasüberzug |
| CN1043056C (zh) * | 1994-05-13 | 1999-04-21 | 新日本制铁株式会社 | 用于硅钢片的具有良好反应性的退火隔离物及其使用方法 |
| JPH08165525A (ja) * | 1994-12-13 | 1996-06-25 | Nippon Steel Corp | グラス被膜が均一で優れ、磁気特性の極めて良好な方向性電磁鋼板の製造方法 |
| JP2749783B2 (ja) * | 1994-11-16 | 1998-05-13 | 新日本製鐵株式会社 | グラス被膜性能と磁気特性の極めて優れる方向性電磁鋼板の製造方法 |
| CN1065004C (zh) * | 1994-11-16 | 2001-04-25 | 新日本制铁株式会社 | 具有优良玻璃膜及磁性能的晶粒取向电工钢板的生产工艺 |
| JPH08193257A (ja) * | 1995-01-17 | 1996-07-30 | Nippon Steel Corp | 高温雰囲気炉の内張り用金属板 |
| JPH09256068A (ja) * | 1996-03-25 | 1997-09-30 | Nippon Steel Corp | 優れたグラス被膜を得るための方向性電磁鋼板の製造方法 |
| JPH1180909A (ja) * | 1997-09-04 | 1999-03-26 | Kawasaki Steel Corp | 張力付加型被膜の密着性の良い低鉄損方向性珪素鋼板 およびその製造方法 |
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| Publication number | Publication date |
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| WO1999024639A1 (de) | 1999-05-20 |
| KR100560178B1 (ko) | 2006-03-13 |
| TW416994B (en) | 2001-01-01 |
| US6423156B1 (en) | 2002-07-23 |
| SK285304B6 (sk) | 2006-10-05 |
| RU2198958C2 (ru) | 2003-02-20 |
| KR20010031919A (ko) | 2001-04-16 |
| AU730568B2 (en) | 2001-03-08 |
| JP4194753B2 (ja) | 2008-12-10 |
| PL187121B1 (pl) | 2004-05-31 |
| AU1023999A (en) | 1999-05-31 |
| ID27132A (id) | 2001-03-01 |
| CN1278872A (zh) | 2001-01-03 |
| SK6762000A3 (en) | 2001-08-06 |
| DE19750066C1 (de) | 1999-08-05 |
| RU2000115302A (ru) | 2005-01-10 |
| EP1029113A1 (de) | 2000-08-23 |
| DE59800806D1 (de) | 2001-07-05 |
| BR9814038A (pt) | 2000-09-26 |
| CZ295684B6 (cs) | 2005-09-14 |
| ZA989390B (en) | 1999-04-15 |
| JP2001522942A (ja) | 2001-11-20 |
| CZ20001647A3 (en) | 2001-05-16 |
| ATE201723T1 (de) | 2001-06-15 |
| PL340454A1 (en) | 2001-02-12 |
| EP1029113B1 (de) | 2001-05-30 |
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