CN101711418A - 用于在基材上制备磁性层的方法和可印刷的可磁化漆料 - Google Patents
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Abstract
在基材上制备磁性层的方法,包括制备可印刷的漆料,该漆料包括60重量%的钕铁硼粉末;10重量%的铁氧体粉末,优选锶六方晶系铁氧体粉末;1.4重量%的催化剂;1.1重量%的分散剂;以及余量的基质,优选环氧化物多元醇基质。所述材料通过搅拌和捏合混合并在三辊轧制机中滚轧。优选以丝网印刷施加在基材上,并随后在80-120℃预硬化6-12小时,并随后在200℃-220℃硬化1-3小时。
Description
本发明涉及用于在基材上制备磁性层的方法以及涉及可印刷的可磁化漆料。
在测量、自动控制和控制技术中,非接触式操作的传感器被越来越多的用于测量构件的位置、排列、旋转角等等。在汽车技术中,一些例子是减震器中的线性移动传感器、用于测量转向角(Lenkwinkel)的旋转角传感器(Drehwinkelsensor)、或者节流阀位置传感器,这里仅仅举出很少几个例子。
与带有滑触电刷(Schleiferabgriff)的电位器相比,非接触式操作的传感器所具有的显著优点是它们事实上不经历任何的磨损,并且对于机械震动是显著更不敏感。因此它们是非常可靠的,并且具有更长的使用寿命。
一种形式的非接触式操作的传感器是使用磁性传感层来工作的,该磁性传感层通过磁场敏感性传感器来扫描。其例子描述在DE10038296A1,DE19536433C2或者DE102004057901中。
磁活性的传感器层可以通过不同的方式施加到基材上。DE19911186A1提出了将磁性层电镀施加到基材上。这需要高的电流密度以及在使用之后对所用电解质高的处理成本。
DE3111657C2将待涂覆的基材浸入到熔融物中。这个熔融物需要例如960℃的工作温度,这导致了在装置和能量方面更大的开支。
DE2429177A1描述一种通过金属原料组合的分解产物来生产磁性薄层的方法。在这个方法中,高毒性的铁和钴的金属羰基化合物在高温热分解,并重新沉积到固体基底上。这些方法需要大量的能量消耗,技术上复杂的加工步骤,并且涉及有害化学品的处理。
因此,有人也提出了制作由磁性材料制成的可印刷的糊。DE3915446A1提出了使用钕铁硼永磁体(其中向该磁体配备有α-Fe2O3涂料来防止腐蚀),其中使该磁体在600℃到烧结温度之间的温度在氧化性气氛中进行退火处理(Glühbehandlung)。
DE10038296A1和DE10309027A1提出了将具有尽可能高剩磁和高的矫顽磁场强度的硬磁性(hartmagnetisch)粉末作为磁体材料,为此,测试了Sr六方晶系铁氧体粉末和NdFeB粉末。在防腐蚀和有利的粒度分布方面,Sr六方晶系铁氧体优于钕铁硼。市售可得的NdFeB粉末的平均(durchschnittlich)粒度是200μm。它们因此是太粗的粒子,并且在使用前必须研磨,以使得能够获得大约1μm的平均(mittler)粒径。为此目的,提出了粉末的耗费的预处理,该粉末随后被结合到聚合物基质来生产印刷糊(Druckpast),以及主要提出了将基于双酚F的胺硬化的环氧化物用于此目的。后者允许印刷结构的低收缩性硬化并且与基于双酚A的环氧树脂相比,其具有更低的粘度,这被认为有利于混入高含量的固体。粘度的进一步降低是通过使用反应性稀释剂来实现的。然后将这样的材料主要借助丝网印刷(Schablonendruck)施加到基底材料上。其中,特别建议了刚玉浮法玻璃(Korund-Float-Glas)、具有低线性膨胀系数的玻璃陶瓷和非磁性的精炼钢(Edelstahl)以及合成材料。
DE3921146A1提出了高矫顽磁条,在其中将磁性层以流延技术施加到载体箔上,该磁性层是由基于六方晶系铁氧体的可磁化粒子的分散体制成的。
除了这些技术方法之外,还描述了磁阻(magnetoresistive)材料,其的特征在于纳米尺寸的层结构。其中GMR、AMR或者TMR成分属于这样的公知材料,在其中各层之间的距离小于电子的平均自由行程长度。因而实现了电子与相邻层的耦合效应,由此改变了材料的电阻(参见DE3820475C1)。
这种效应还可以用于路程或者角度的测量(参见DE10108760A1,DE10214946A1,DE102267A1)。
但是,这些层结构只能用技术上复杂的涂覆工艺例如旋涂或者溅射来实现。
另外,平板印刷和蚀刻技术也被使用(DE19830343C1)。
DE69720206T2(WO97/03842;EP0898778B1)描述一种由磁性粉末和粘合剂制成的复合磁体材料,其中基本上使用钕铁硼粉末,环氧化物被用作粘合剂。铌或者其他金属例如钨、铬、镍、铝、铜、镁和锰、镓、钒、钼、钛、钽、锆和锡被提出作为其他的添加成分,以及加入了碳、钙、硅、氧和氮。
由锶六方晶系铁氧体(Strontiumhexaferrit)生产的永磁体更详细的方法描述在DE4330197A1中。DE4041962A1还描述了基于细颗粒六方晶系铁氧体和环氧化物胺加成聚合物的聚合物结合的各向异性磁体材料。
具有低钴含量的钕铁硼合金在US5411608以及在US2003/0217620A1中被提及。由锶六方晶系铁氧体粉末制备磁体还描述在EP0351775B1(DE68905251T2)以及DE3921146A1中。
用于测量旋转角或者直线路程(Linearweg)的、用磁活性材料来工作的传感器的实际应用描述在下面的文献中:DE19911702C2(旋转角传感器),DE19903490C2(节流阀位置传感器),DE19956361A1(带有GMR磁场传感器的旋转角传感器),DE10038296A1(角度测量装置),DE202004004455U1(加速踏板用的线性传感器),DE19751519C2(线性传感器),US6154025(线性传感器)和DE3214794A1(长度和角度测量装置)。
本发明的目标是提供用于在基材上制备磁性层的方法以及可印刷的可磁化漆料(Lack),该漆料尽可能好地满足下面的标准:
-硬化的漆料应当具有良好的磁性,特别是高的矫顽磁场强度和高剩磁;
-漆料应当尽可能均匀;
-漆料应当耐长期存储;
-漆料应当能够用已知的施加方法(即使层厚大也以精确的轮廓)进行施加;和
-漆料应当能成本有益地生产。
本发明借助专利的权利要求1和10的特征而解决了这些问题。所述权利要求有利的实施方案和进一步的推展可以在从属权利要求中找到。
本发明的漆料具有如下组成:
-大约60重量%的钕铁硼粉末;
-大约10重量%的铁氧体粉末,优选锶六方晶系铁氧体粉末;
-大约1.4重量%的催化剂;
-大约1.1重量%的分散剂;
-余量的基质,优选是环氧化物多元醇基质。
所列出的重量百分比每一个被理解为具有大约+/-3%的波动幅度(Bandbreit),这产生了下面的组成:
-58.2-61.8重量%的钕铁硼粉末;
-9.7-10.3重量%的铁氧体粉末,优选锶六方晶系铁氧体粉末;
-1.35-1.44重量%的催化剂;
-1.07-1.13重量%的分散剂;
-29.68-25.33重量%的基质,优选是环氧化物多元醇基质。
该漆料在基质中包含溶剂,其在硬化过程中蒸发。所以,由于因此所失去的溶剂,硬化的漆料具有更低的百分比份额的基质和更高份额的钕铁硼粉末,并且后者在硬化的漆料中的份额为至多70重量%。
基于本发明人广泛的试验,根据目标要求,确定了上述的最佳组成。硬化的和磁化的漆料的饱和极化强度是430mT,剩磁是202mT,矫顽磁场强度是625KA/m,能量乘积(Energieprodukt)(B×H)是6.78mJ/cm3,其中施加了磁极宽度(Polbreit)2.5mm,层厚25μm的磁化条。此外,以这种方式生产的尚未硬化的漆料在冷藏下能够耐几周的存储,并且存储后具有优异的可印刷性。没有发生脱混和沉降。
用于在基材上制备磁性层的本发明的方法具有下面的连续(aufeinanderfolgend)步骤:
a)通过搅拌或者捏合来混合上述组分;
b)滚轧(Walzen)该混合物;
c)将以这种方式生产的漆料施加到基材上,优选借助丝网印刷(Schablonendruck)来施加;
f)磁化该硬化的层。
在步骤b)之后,再加工该滚轧过的混合物可能是需要的,根据粘度再一次加入分散剂,并且进行重复(nochmalig)的滚轧。该滚轧在步骤b)之后,以及如果需要,该重复的滚轧优选是在三辊轧制机(Drei-Walzenstuhl)上进行的。
预硬化进行达6-12个小时,并且促进了基质中溶剂受控的蒸发,由此防止了任何溶剂夹杂物的残留和在材料中形成密度梯度。在预硬化之后,获得了一个没有完全硬化的层,其仍然能够容易地成形。该预硬化以及随后的硬化将产生光滑的层,其甚至在逐步顶铣中也不表现出任何的孔洞或者夹杂物。
钕铁硼粉末是球形Nd2Fe14B类型的合金,其在MQP-S-11-9名称下获自Magnequench公司。该混合物的粒径是40μm,并且粒径分布是35-55μm。
这种磁体粉末的一个问题是,在聚合物基质中不足的分散性。为此原因,该铁氧体粉末是以所示的量混入的,并且在一个具体的工作实施例中,加入粒度为5μm的烧结粒子形式的锶六方晶系铁氧体粉末(Sr-Fe3O4)。
在一种具体的工作实施例中,在上述组分通过搅拌或者捏合进行混合之后,将该混合物在三辊轧制机上进行滚轧。在这个加工中,由于更大的簇的解聚集,因此粒子被粉碎。在该滚轧之后,甚至在长期存储之后也检测不到金属粒子的沉降,并且该漆料即使在并向中存放12小时之后仍然能够流动并因而是可加工的。因此,在冷藏过程中没有发生交联。
施加到基材上的磁性层在40℃的温度和95%的空气湿度经历100小时的潮湿存储过程。吸湿量小于0.1%。并且在该磁性层中也没能检测到视觉变化。所以,该磁性层也是耐腐蚀性。
市售的合成树脂例如环氧化物、聚酯或者聚氨酯可以与胺类或酚类硬化剂一起用作聚合物基质。环氧化物用于该具体的实施方案中。在此,基质还包含催化剂形式的用于加速所述反应的其他添加剂以及分散剂,分散剂可以使用市售的表面活性剂。将溶剂例如醇或者酮加入到该混合物中,来调整所需的漆料印刷性能。
Al2O3陶瓷或者市售的合成材料例如层压的环氧化物/玻璃织物板(Glasgewebe-Platte)优选用作基材。
对于实际应用的传感器的情况而言,选择至少200μm的层厚度,并且其可以至多为1000μm。这些层厚度可以通过丝网印刷来最佳地实现。
在印刷步骤之后在80-120℃进行预硬化6-12小时。更短的干燥时间或者更高的温度将导致不期望的空洞或者气泡的形成。获得了受控的溶剂蒸发。随后的硬化在200-220℃进行达1-3个小时,该硬化产生了所述物质的完全交联。
Claims (13)
1.用于在基材上制备磁性层的方法,其具有下面的连续步骤:
a)通过搅拌或者捏合来制备下列的混合物:60重量%的钕铁硼粉末、10重量%的铁氧体粉末、1.4重量%的催化剂、1.1重量%的分散剂和17.5重量%的基质,其中该催化剂充当该基质的反应加速剂;
b)滚轧该混合物;
c)将该混合物施加到基材上;
d)将该施加到该基材上的混合物在80℃-120℃的温度预硬化6-12个小时;
e)在200℃-220℃的温度硬化1-3个小时;和
f)磁化该硬化的层。
2.根据权利要求1的方法,特征在于步骤b)的滚轧该混合物是在三辊轧制机上进行的。
3.根据权利要求1或2的方法,特征在于权利要求1的步骤c)的施加到基材上是借助丝网印刷来进行的。
4.根据权利要求1-3中之一的方法,特征在于权利要求1的步骤a)中所述的重量%是在+/-3%的波动幅度内可变的。
5.根据权利要求1-4中之一的方法,特征在于该铁氧体粉末是锶六方晶系铁氧体粉末。
6.根据权利要求1-5中之一的方法,特征在于该基质是环氧化物多元醇基质。
7.根据权利要求1-6中之一的方法,特征在于在权利要求1的步骤b)之后,通过进一步添加分散剂来对该混合物进行再加工。
8.根据权利要求7的方法,特征在于该混合物的再加工还包括重复地滚轧。
9.根据权利要求1-8中之一的方法,特征在于在权利要求1的步骤e)之后,通过铣或磨对该硬化的层进行机械再加工。
10.可印刷的可磁化漆料,其具有下面的组成:
-60重量%的钕铁硼粉末;
-10重量%的铁氧体粉末;
-1.4重量%的催化剂;
-1.1重量%的分散剂;
-余量的基质;
其中该催化剂是基质的反应加速剂。
11.根据权利要求10的漆料,特征在于所述铁氧体粉末是锶六方晶系铁氧体粉末。
12.根据权利要求10的漆料,特征在于所述基质是环氧化物多元醇基质。
13.根据权利要求10的漆料,特征在于权利要求10所述的重量%是在+/-3%的波动幅度内可变的。
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DE102007026503.6 | 2007-06-05 | ||
DE102007026503A DE102007026503B4 (de) | 2007-06-05 | 2007-06-05 | Verfahren zur Herstellung einer Magnetschicht auf einem Substrat und druckbarer magnetisierbarer Lack |
PCT/EP2008/004108 WO2008148467A1 (de) | 2007-06-05 | 2008-05-23 | Verfahren zur herstellung einer magnetschicht auf einem substrat und druckbarer magnetisierbarer lack |
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US (1) | US20100129540A1 (zh) |
EP (1) | EP2158595A1 (zh) |
JP (1) | JP2010529661A (zh) |
KR (1) | KR20100018492A (zh) |
CN (1) | CN101711418A (zh) |
DE (1) | DE102007026503B4 (zh) |
MX (1) | MX2009012852A (zh) |
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DE102009010248A1 (de) | 2009-02-24 | 2010-09-02 | Dürr Systems GmbH | Beschichtungsvorrichtung und Beschichtungsverfahren zur Beschichtung eines Werkstücks |
RU2476939C1 (ru) * | 2011-08-30 | 2013-02-27 | Учреждение Российской академии наук Институт металлургии и материаловедения им. А.А. Байкова РАН | Способ получения текстурированных покрытий с анизотропной коэрцитивной силой на основе магнитных соединений |
KR101376076B1 (ko) * | 2012-08-09 | 2014-03-19 | 한국수력원자력 주식회사 | 노외 노심용융물 냉각설비 희생 콘크리트 조성물 및 이의 제조방법 |
US9596755B2 (en) * | 2014-10-15 | 2017-03-14 | Rogers Corporation | Magneto-dielectric substrate, circuit material, and assembly having the same |
CA2995067A1 (en) * | 2015-08-07 | 2017-02-16 | Evolva Sa | Production of steviol glycosides in recombinant hosts |
US11508503B2 (en) | 2018-04-12 | 2022-11-22 | Rogers Corporation | Textured planar m-type hexagonal ferrites and methods of use thereof |
JP7298568B2 (ja) | 2020-08-25 | 2023-06-27 | 株式会社村田製作所 | 磁性粉の製造方法および圧粉成形体の製造方法 |
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2007
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- 2008-05-23 KR KR1020097021891A patent/KR20100018492A/ko not_active Application Discontinuation
- 2008-05-23 WO PCT/EP2008/004108 patent/WO2008148467A1/de active Application Filing
- 2008-05-23 MX MX2009012852A patent/MX2009012852A/es active IP Right Grant
- 2008-05-23 EP EP08749496A patent/EP2158595A1/de not_active Withdrawn
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WO2008148467A1 (de) | 2008-12-11 |
EP2158595A1 (de) | 2010-03-03 |
JP2010529661A (ja) | 2010-08-26 |
DE102007026503B4 (de) | 2009-08-27 |
MX2009012852A (es) | 2009-12-11 |
US20100129540A1 (en) | 2010-05-27 |
DE102007026503A1 (de) | 2008-12-11 |
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