CN105683125A - 铁氧体烧结体、铁氧体烧结板和铁氧体烧结片材 - Google Patents
铁氧体烧结体、铁氧体烧结板和铁氧体烧结片材 Download PDFInfo
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Abstract
本发明的技术课题在于提供一种μˊ高,μ"低,而且μˊ因温度的变化小,铁氧体的微细结构致密的铁氧体烧结片材。本发明涉及一种铁氧体烧结体、铁氧体烧结板和铁氧体烧结片材,该铁氧体烧结体的特征在于,其为以氧化物换算,具有包括47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO的组成的铁氧体烧结板,并含有0.2~1.4wt%的SnO2和0.005~0.03wt%的S,密度为5.05~5.30g/cm3;该铁氧体烧结片材的特征在于,在该铁氧体烧结板的表面设置槽,还设置粘合层和/或保护层。
Description
技术领域
本发明提供铁氧体烧结体、铁氧体烧结板以及在该铁氧体烧结板的表面设置粘合层和/或保护层的铁氧体烧结片材。
背景技术
移动电话、智能手机等的通信设备中,配备有如NFC(近距离无线通信)、支付系统这样的能够使用平面状线圈天线交换信息的系统。该天线靠近线路基板、电池等的含有金属的部件配置,因此,这样直接配置会使信息交换灵敏度显著降低。因此,为了提高信息交换灵敏度,在该天线和含有金属的部件之间配置铁氧体烧结片材。
在这些系统中,为了提高其信息交换灵敏度,公开有通过向Ni-Zn-Cu铁氧体中添加CoO,控制铁氧体烧结片材的导磁率的技术(专利文献1、2)。
另一方面,在感应器部件的领域中,公开有通过添加SnO2、Co氧化物、Bi氧化物,得到导磁率的温度特性优异,密度高的感应器部件的方法(专利文献3)。另外,公开有将铁氧体中的S和Cl的含量设在规定范围内,由此对Ag向铁氧体中的扩散进行控制的方法(专利文献4)。另外,已知将含有SnO2的铁氧体用于感应器的方法(专利文献5)。
现有技术文献
专利文献
专利文献1:日本特开2005-340759号公报
专利文献2:日本特开2013-133263号公报
专利文献3:日本特开2002-255637号公报
专利文献4:日本特开平5-258937号公报
专利文献5:日本特开2002-124408号公报
发明内容
发明要解决的课题
为了通信设备的小型化、高功能化,要求进一步提高平面状线圈天线的信息交换灵敏度,为此,需要通过增大铁氧体烧结片材的导磁率的实数部(μ′),增大天线的电感。然而,铁氧体烧结片材具有如下性质:在作为交换信息频率的13.56MHz,若μ′变大,则导磁率的虚数部(μ″)所表示的损失增大,该损失使天线的信息交换灵敏度降低。因此,要求μ″尽量小并且μ′尽量大的铁氧体烧结片材。
在专利文献1中,公开了添加CoO的技术,但是μ′低,对于提高信息交换灵敏度是不充分的。
在专利文献2中,提出了含有Co,具有包括粒成长进行中的晶粒和空穴的微细结构的铁氧体烧结片材,但是,由于具有空穴,存在制造过程中操作时易碎的缺点。因此,为了使其不容易碎,需要提高烧结密度,去除空穴。
在专利文献3中,没有考虑到使铁氧体具有S。专利文献4中,为了控制内部导体中的Ag的扩散,对S成分和Cl成分的含量进行控制,但是,不含Sn,μ′因温度的变化大。专利文献5所述的铁氧体不含Co,μ″大。
另外,铁氧体烧结片材组装在移动设备中,在户外使用的情况较多。因此,为了对于外界气温的变化,使天线的特性稳定,需要减小相对于温度的导磁率的温度变化。
于是,本发明的技术课题在于,提供一种烧结密度高,μ′大,μ″小,而且μ′因温度的变化小的铁氧体烧结片材。
用于解决课题的方法
上述技术课题可以通过以下的本发明实现。
即,本发明为一种铁氧体烧结体,其特征在于,以氧化物换算,具有包括47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO的组成,并且含有0.2~1.4wt%的SnO2和0.005~0.03wt%的S(本发明1)。
即,本发明为一种铁氧体烧结板,其特征在于,以氧化物换算,具有包括47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO的组成,并且含有0.2~1.4wt%的SnO2和0.005~0.03wt%的S(本发明2)。
即,本发明为一种铁氧体烧结板,其特征在于,以氧化物换算,具有包括47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO的组成,并且含有0.2~1.4wt%的SnO2和0.005~0.03wt%的S,该铁氧体烧结板的密度为5.05~5.30g/cm3(本发明3)。
另外,本发明为一种铁氧体烧结片材,其在本发明2或3所述的铁氧体烧结板的一侧的表面设置粘合层,在相反侧的表面设置保护层(本发明4)。
另外,本发明为一种铁氧体烧结片材,其在本发明2或3所述的铁氧体烧结板的两面设置粘合层(本发明5)。
另外,本发明为一种铁氧体烧结片材,其在本发明2或3所述的铁氧体烧结板的两面设置保护层(本发明6)。
另外,本发明为一种铁氧体烧结片材,其在本发明4~6中任一项所述的铁氧体烧结片材中,在铁氧体烧结板的至少一侧的表面形成有至少一个槽(本发明7)。
另外,本发明为一种铁氧体烧结片材,其在本发明4~6中任一项所述的铁氧体烧结片材中,铁氧体烧结板被分割为小片状(本发明8)。发明的效果
本发明的铁氧体烧结体、铁氧体烧结板和铁氧体烧结片材的μ′大、μ″小,而且μ′因温度的变化小,因此适合在NFC等的系统中作为使信息交换灵敏度提高并且使其稳定的部件。
附图说明
图1是表示在实施例1中得到的铁氧体烧结板的微细结构的扫描型电子显微镜照片。
图2是表示在比较例1中得到的铁氧体烧结板的微细结构的扫描型电子显微镜照片。
具体实施方式
本发明的构成的更详细的说明如下。
以氧化物换算,本发明的铁氧体烧结体和铁氧体烧结板的组成如下:含有47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO,总计为100mol%。对此,还含有0.2~1.4wt%的SnO2和0.005~0.03wt%的S。即,本发明为包括Fe2O3、NiO、ZnO、CuO、CoO的铁氧体和SnO2和S的混合物。
在本发明的铁氧体烧结体和铁氧体烧结板中的Fe2O3的组成小于47.5mol%的情况下,μ′变小。在超过49.8mol%的情况下,不能烧结。更优选的Fe2O3的组成为48~49.5mol%。
在本发明的铁氧体烧结体和铁氧体烧结板中的NiO的组成小于13.5mol%的情况下,μ″变大。在超过19.5mol%的情况下,μ′变小。更优选的NiO的组成为14.5~18.5mol%。
在本发明的铁氧体烧结体和铁氧体烧结板中的ZnO的组成小于21mol%的情况下,μ′变小。在超过27mol%的情况下,μ″变大。更优选的ZnO的组成为22~26mol%。
在本发明的铁氧体烧结体和铁氧体烧结板中的CuO的组成小于7.5mol%的情况下,不能烧结。在超过12.5mol%的情况下,CuO析出,μ′变小。更优选的CuO的组成为8.5~11.5mol%。
在本发明的铁氧体烧结体和铁氧体烧结板中的CoO的组成小于0.2mol%的情况下,μ″变大。在超过0.8mol%的情况下,μ′变小,而且μ′因温度的变化变大。更优选的CoO的组成为0.2~0.7mol%。
在本发明的铁氧体烧结体和铁氧体烧结板中的SnO2的含量小于0.2wt%的情况下,μ′因温度的变化变大。在超过1.4wt%的情况下,μ′变小。更优选的SnO2的含量为0.2~1.3wt%。
在本发明的铁氧体烧结体和铁氧体烧结板中的S的含量小于0.005wt%的情况下,烧结性变差,μ′变小。在超过0.03wt%的情况下,μ′因温度的变化变大,μ″变大。更优选的S的含量为0.007~0.025wt%。
在本发明的铁氧体烧结板的密度小于5.05g/cm3的情况下,其微细结构中生成数μm以下的空穴,成为不均匀的微细结构,因此,操作时易碎。由于铁氧体的理论密度为5.30g/cm3左右,本发明中的密度的上限为5.30g/cm3。如本发明,如果铁氧体烧结板的密度在5.05~5.30g/cm3的范围内,则在微细结构不生成空穴,能够得到致密的微细结构,因此,在操作时不容易碎,生产性提高。为了使铁氧体烧结板的密度在上述范围内,可以通过使各构成成分的比例在上述范围内的同时,控制烧结温度,从而实现。
本发明的铁氧体烧结板的厚度优选为0.01~0.7mm。更优选为0.02~0.7mm。
在本发明的铁氧体烧结板的至少一侧的表面能够设置粘合层。粘合层的厚度优选为0.001~0.1mm。
在本发明的铁氧体烧结板的至少一侧的表面能够设置保护层。保护层的厚度优选为0.001~0.1mm。
本发明的铁氧体烧结片材的μ′(25℃时的)优选为90~180。更优选为100~170。
本发明的铁氧体烧结片材的μ″(25℃时的)优选为0.05~5。更优选为0.1~4.5。
本发明的铁氧体烧结片材的μ′因温度的变化(85℃时的导磁率的实数部μ′85和25℃时的导磁率的实数部μ′25的差相对于μ′25的比((μ′85-μ′25)/μ′25))优选为5~30%。更优选为5~25%。
作为本发明的粘合层,可以列举双面胶带。作为双面胶带没有特别限制,可以使用公知的双面胶带。另外,作为粘合层,可以是如下粘合层,其为在铁氧体烧结板的单面依次叠层粘合层、具有弯曲性和伸缩性的膜或片材、粘合层和脱模片材而得的粘合层。
通过设置本发明中的保护层,能够提高对于分割铁氧体烧结板时的落粉的可靠性和耐久性。作为该保护层,只要是弯曲铁氧体烧结片材时不发生断裂而能够拉伸的树脂,则没有特别限制,可以例示PET膜等。
本发明的铁氧体烧结片材为了与弯曲的部分紧密贴附,可以是如下构成:能够以预先设在铁氧体烧结板的至少一侧的表面的至少一个槽作为起点,分割铁氧体烧结板。上述槽可以以连续的方式形成,也可以以断续的方式形成,另外,还可以形成多个微小的凹部,由此替代槽。优选的槽的截面为U字型或V字型。
本发明的铁氧体烧结片材为了与弯曲的部分紧密贴附,并且为了防止在使用时破裂,优选为预先将铁氧体烧结板分割为小片状。例如可以采取如下中的任意方法:以预先设在铁氧体烧结板的至少一侧的表面的至少一个槽为起点,分割铁氧体烧结板,或者,不形成槽而将铁氧体烧结板分割为小片状。
铁氧体烧结板由槽划分为任意大小的三角形、四边形、多角形或这些的组合。例如,三角形、四边形、多角形的一边的长度通常为1~12mm,被附着物的粘接面为曲面的情况下,优选为1mm以上且其曲率半径的1/3以下,更优选为1mm以上且曲率半径的1/4以下。在形成有槽的情况下,在槽以外的位置不发生不定形的破裂,能够密合或实质上密合在平面、圆柱状的侧曲面和具有一些凹凸的面上。
形成在铁氧体烧结板的槽的开口部的宽度,通常优选为250μm以下,更优选为1~150μm。开口部的宽度超过250μm的情况下,铁氧体烧结板的导磁率大幅降低,不作为优选。另外,槽的深度通常为铁氧体烧结板的厚度的1/20~3/5。另外,厚度为0.01mm~0.2mm的薄的铁氧体烧结板的情况下,槽的深度优选为铁氧体烧结板的厚度的1/20~1/4,更优选为1/20~1/6。
接下来,对于本发明的铁氧体烧结板和铁氧体烧结片材的制造方法进行说明。
首先,铁氧体粉末能够通过以下方法获得:对于将构成铁氧体的各元素的氧化物、碳酸盐、氢氧化物、草酸盐等的原料以规定的组成比例混合得到的原料混合物或者使各元素在水溶液中沉淀得到的沉淀物,在大气中以700~900℃的温度范围进行1~20小时的预烧制后,进行粉碎。此时,即使在制造铁氧体的原料混合物中进一步混合SnO2,进行预烧制,SnO2也不成为铁氧体的构成要素,因此优选将SnO2预先与制造铁氧体的原料混合物混合。或者,也可以向通过预烧制制造的Ni-Zn-Cu-Co铁氧体中添加SnO2,进行粉碎混合,制成混合粉末,或者,也可以向经预烧制,粉碎制造的Ni-Zn-Cu-Co铁氧体粉末中添加SnO2制成混合粉末。
特别是,成为铁元素的供给源的氧化铁优选如下的氧化铁,该氧化铁对在水溶液中由硫酸铁与氢氧化钠得到的沉淀物进行烧结而得到。该氧化铁以硫酸铁作为原料,因此含有通过水洗等未能够完全去除干净的S,其含量能够在制造过程中适当调整。另外,以该氧化铁作为原料的铁氧体粉末中,必然含有S。
将得到的铁氧体粉末与粘结剂树脂混合后,通过粉末压缩成型法、注射成型法、压延法、挤出法等,成型铁氧体板,根据需要进行脱脂处理后,进行烧结处理,由此能够制造铁氧体烧结板。另外,将铁氧体粉末和粘结剂树脂和溶剂混合后,通过刮片等涂布在膜或片材上,得到生片,根据需要进行脱脂处理后,对得到的生片进行烧结处理,由此能够制造铁氧体烧结板。另外,也可以叠层多张所得到的生片后,进行烧结。
按照需要,在铁氧体烧结板形成槽的情况下,能够在铁氧体板的成型过程中、成型后或烧结处理后形成槽。例如,通过粉末压缩成型法或注射成型法进行成型的情况下,优选在成型过程中形成槽,通过压延法或挤出法进行成型的情况下,优选在成型后且烧结前形成槽,经由生片制造烧结铁氧体板的情况下,优选在生片形成槽。
脱脂处理通常以150~500℃的温度进行。烧结温度通常为850~970℃,优选为860~960℃。烧结时间通常为30~180分钟,优选为30~120分钟。在烧结温度小于850℃的情况下,颗粒的烧结变得困难,得到的烧结铁氧体板的强度不充分,μ′也低。另外,若烧结温度超过970℃,则颗粒的成长进行,μ′因温度的变化变大,μ″变大,因而不优选。在烧结时间小于30分钟的情况下,颗粒的烧结变得困难,得到的烧结铁氧体板的强度不充分,μ′也低。另外,烧结时间为180分钟时,颗粒的烧结充分进行,因此不需要超过180分钟延长烧结时间。
在本发明中,使各构成成分的比例在规定的范围内的同时,控制烧结温度,由此能够制造具有所要求的特性(导磁率μ′、μ″和μ′因温度的变化率、密度)的铁氧体烧结体。
接着,按照需要,对得到的铁氧体烧结板的表面设置粘合材料层,例如,设置双面胶带。粘合材料层可以在铁氧体烧结板的单面或两面形成。
另外,按照需要,对得到的铁氧体烧结板的表面,设置保护层。粘合材料层可以在铁氧体烧结板的单面或两面形成。保护层的形成能够通过如下方法进行:将构成保护层的树脂的膜或片材,根据需要经由粘接剂粘接在烧结铁氧体板的表面,或者将含有构成保护层的树脂的涂料涂布在烧结铁氧体板的表面。通过形成保护层,能够防止铁氧体烧结板的落粉。
另外,在本发明中,能够在铁氧体烧结板的一侧的表面形成粘合层,在另一侧的表面形成保护层。
将铁氧体烧结板沿着槽分割的情况下,在形成粘合层和/或保护层后,利用辊进行分割即可。
<作用>
在本发明中最重要的点为如下事实:包括特定的组成的铁氧体烧结体、铁氧体烧结板或铁氧体烧结片材的μ′高,μ″低,而且μ′因温度的变化小。因此,天线的电感变大,其损失变小,从而能够提高信息交换灵敏度。而且,μ′因温度的变化小,因此在户外使用时,外界气温的变化导致的电感的变化变小,使稳定的信息交换成为可能。另外,本发明的铁氧体烧结板由于其密度高,具有致密的微细结构,因此在操作时不易碎,能够提高生产效率。
实施例
本发明的代表性的实施方式如下。
铁氧体烧结板的组成利用荧光X射线分析装置3530(理学电机工业(株)制造)和碳/硫分析装置EMIA-920V2((株)堀场制作所制造)进行测定。
铁氧体烧结板的密度由利用游标卡尺和千分尺测定的外部尺寸和重量计算求得。
铁氧体烧结板和铁氧体烧结片材的厚度利用千分尺测定。
铁氧体烧结片材的μ′和μ″是对冲压成外径为20mm、内径为10mm的环,利用阻抗/材料分析仪E4991A(AgilentTechnologies(株)制造)在13.56MHz的频率测定的。
通过将85℃时的导磁率的实数部μ′85和25℃时的导磁率的实数部μ′25的差相对于μ′25的比((μ′85-μ′25)/μ′25)以百分比的形式表示的值,评价铁氧体烧结片材的μ′因温度的变化Δμ′。
铁氧体烧结板的微细结构利用S-4800型场发射型扫描电子显微镜((株)日立高新技术制造),以倍率8000倍观察。
实施例1:
以铁氧体的组成成为规定的组成的方式,将各氧化物原料称量,使用球磨机进行20小时湿式混合后,将混合浆料过滤、干燥,得到原料混合粉末。将该原料混合粉末以720℃烧制3小时得到的预烧制物使用球磨机进行粉碎,得到本发明的Ni-Zn-Cu-Co铁氧体粉末。另外,S来自在制造原料Fe2O3时所使用的硫酸铁。
对于得到的Ni-Zn-Cu-Co铁氧体粉末100重量份,加入作为结合材料的聚乙烯醇缩丁醛8重量份、作为增塑剂的邻苯二甲酸苄基正丁酯3重量份、作为溶剂的3甲基-3甲氧基-1丁醇50重量份后,充分混合,得到浆料。将该浆料利用刮片式涂布机涂布在PET膜上,形成涂膜后,使其干燥,由此得到厚度120μm的生片。
在该生片的表面使用刀刃为V字型的刀模,使深度为50μm的槽以3mm的间隔形成为格子状。
将得到的生片以400℃进行脱脂后,以920℃烧结2小时,由此,得到铁氧体烧结板。该铁氧体烧结板的组成如下:Fe2O3为48.37mol%、NiO为16.95mol%、ZnO为23.43mol%、CuO为10.97mol%、CoO为0.28mol%、SnO2为0.40wt%、S为0.01wt%,厚度为98μm,密度为5.17g/cm3。另外,推测S以氧化物(SO2、SO3等)的形式存在。该铁氧体烧结板的微细结构示于图1。由该图可知,该铁氧体烧结板的微细结构中没有空穴,是致密的结构。
在得到的铁氧体烧结板的一侧的表面贴附PET膜,在另一侧的表面上贴附两面胶带,得到铁氧体烧结片材。厚度为118μm。
将得到的铁氧体烧结片材分割后,在13.56MHz的μ′为148,μ″为2.8,Δμ′为14%。
实施例2~9:
通过与实施例1相同的方法,得到铁氧体烧结板和铁氧体烧结片材。此时的制造条件以及得到的铁氧体烧结板和铁氧体烧结片材的诸特性示于表1。
比较例1:
通过与实施例1相同的方法,得到铁氧体烧结板和铁氧体烧结片材。此时的制造条件以及得到的铁氧体烧结板和铁氧体烧结片材的诸特性示于表1。铁氧体烧结板的微细结构示于图2。由该图可知,在该铁氧体烧结板的微细结构中,能够确认到较多的空穴。
比较例2~7:
通过与实施例1相同的方法,得到铁氧体烧结板和铁氧体烧结片材。此时的制造条件以及得到的铁氧体烧结板和铁氧体烧结片材的诸特性示于表1。
[表1]
工业上的可利用性
本发明的铁氧体烧结片材的μ′大,μ″小,而且μ′因温度的变化小,因此对于外界气温的变化能够使天线的特性稳定,能够将本发明的铁氧体烧结片材组装在便携设备中使用。
Claims (6)
1.一种铁氧体烧结体,其特征在于:
以氧化物换算,具有包括47.5~49.8mol%的Fe2O3、13.5~19.5mol%的NiO、21~27mol%的ZnO、7.5~12.5mol%的CuO、0.2~0.8mol%的CoO的组成,还含有0.2~1.4wt%的SnO2和0.005~0.03wt%的S。
2.如权利要求1所述的铁氧体烧结体,其特征在于:
铁氧体烧结体为铁氧体烧结板。
3.如权利要求2所述的铁氧体烧结板,其特征在于:
铁氧体烧结板的密度为5.05~5.30g/cm3。
4.一种铁氧体烧结片材,其特征在于:
在权利要求2或3所述的铁氧体烧结板的一侧的表面设置粘合层或保护层,在相反侧的表面设置粘合层或保护层。
5.如权利要求4所述的铁氧体烧结片材,其特征在于:
在铁氧体烧结板的至少一侧的表面形成有至少一个槽。
6.如权利要求4所述的铁氧体烧结片材,其特征在于:
铁氧体烧结板被分割为小片状。
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