CN1102485C - 高密度铁氧体基元和用于制造该基元的铁氧体珠粒组合物 - Google Patents
高密度铁氧体基元和用于制造该基元的铁氧体珠粒组合物 Download PDFInfo
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- CN1102485C CN1102485C CN99120552A CN99120552A CN1102485C CN 1102485 C CN1102485 C CN 1102485C CN 99120552 A CN99120552 A CN 99120552A CN 99120552 A CN99120552 A CN 99120552A CN 1102485 C CN1102485 C CN 1102485C
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- ferrite bead
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
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- Inorganic Chemistry (AREA)
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- Powder Metallurgy (AREA)
Abstract
这里公开的是适合于压塑加工成压塑铁氧体的铁氧体珠粒组合物的制备方法,该压塑铁氧体进行烧结热处理得到可用作电磁材料的烧结铁氧体基元。该方法包括以下步骤:从铁氧体颗粒和有机粘结剂化合物形成铁氧体珠粒;和将铁氧体珠粒与有限量的脱水己糖醇化合物的高级脂肪酸酯如脱水山梨糖醇单-或倍半油酸酯均匀地混合。本发明的铁氧体珠粒组合物不仅理想地表现于压塑性能如压塑体的高密度、从金属模具中的低的抽出压力和回弹现象的减少,而且表现于烧结后铁氧体的性能。
Description
本发明涉及高密度铁氧体基元和用于制造该基元的铁氧体珠粒组合物以及涉及制备铁氧体珠粒组合物的方法。更具体地说,本发明涉及可用作电气和电子装置的组件的高密度铁氧体基元和用于通过压塑方法制备铁氧体基元的铁氧体珠粒组合物以及制备该铁氧体珠粒组合物的方法。
众所周知的是,各种类型的铁氧体一般广泛地用作制备铁氧体基元的材料,该铁氧体基元可用作各种电子装置如电绝缘元件等的结构或功能部分,通过利用它们的高耐热性、化学稳定性、机械强度、电绝缘性能、磁性能等的高性能。
此类铁氧体基元在大多数情况下是由包括例如铁氧体材料和粘结剂化合物的细颗粒的铁氧体粉末型组合物的干法压塑过程得到压塑体,然后进行烧结热处理而最终制得。也就是说,铁氧体颗粒与粘结剂化合物和水掺混得到含水的料浆,后者在喷雾干燥器中进行喷雾干燥得到适合于干法压塑的铁氧体珠粒组合物。此外,该铁氧体组合物可通过反复干燥和振荡式挤出以使铁氧体颗粒和粘结剂化合物的含水溶液的混合物粒化而制备。
为了令人满意地用于压塑加工中,铁氧体珠粒组合物需要具有良好的流动性以确保快速和完全填充金属模腔来进行压塑以及从铁氧体基元的质量和压塑过程的生产率考虑该珠粒在压制下有良好的崩解能力。在日本专利申请公开5-159918和日本专利公告7-17460中建议了有良好流动性和显示出良好的珠粒崩解能力的陶瓷珠粒组合物的制备方法,其中用于制备陶瓷珠粒的含水料浆与分散剂混合。此外,在日本专利申请公开3-31660和日本专利公开10-59776中提出了一些建议,其中通过采取降低粘结剂化合物的偏析的措施来制备陶瓷珠粒组合物。日本专利申请公开10-29871公开了一种用于制造具有优异机械性能的烧结陶瓷体的、在压塑过程中有良好模塑性的陶瓷珠粒组合物,其中陶瓷颗粒在含水料浆中与包括聚乙烯醇、聚乙二醇和多羟基醇的高级脂肪酸酯如硬脂酸脱水山梨醇酯等的三种类型的粘结剂化合物的混合物进行掺混。
虽然当由含水料浆的喷雾干燥造粒方法制备陶瓷珠粒组合物时在一定程度上有效,但是当振荡挤出造粒方法用于从陶瓷颗粒的含水料浆制备陶瓷珠粒组合物时,现有技术的方法不是非常令人满意。还有,现有技术的方法具有就以下几个方面而言的诸多问题:从陶瓷珠粒组合物制备的陶瓷基元的密度的不可再现性,压塑加工体从金属模具中的脱模能力,因模塑体的所谓回弹现象而在陶瓷基元中形成裂纹以及金属模具的耐久性,尽管在陶瓷珠粒组合物的流动性和陶瓷珠粒在较低压制力下的崩解性能上获得一定程度的改进。
本发明的主要目的因此是提供陶瓷材料或尤其高均匀性的铁氧体材料的压塑高密度基元,后者能够得到显示出优异电磁性能的烧结铁氧体基元,该基元可通过铁氧体珠粒组合物的压塑加工来制备,有良好的从金属模具中脱模的性能且没有因回弹现象所导致的任何模塑缺陷如裂纹。
本发明的第二个目的是提供在压塑过程中显示出优异流动性和压力传递性且适合于压塑(在压塑过程中没有任何麻烦和不会降低金属模具的寿命)得到压塑基元的铁氧体珠粒组合物,以及提供制备该铁氧体珠粒组合物的方法。
因此,本发明的制备铁氧体珠粒组合物的方法包括以下步骤:
(a)将平均粒径在0.5-5微米范围内的铁氧体的颗粒与0.2-10wt%的有机粘结剂化合物均匀掺混制备铁氧体粉末混合物;
(b)将铁氧体粉末混合物造粒成平均粒径在0.05-0.5mm范围内的铁氧体珠粒;和
(c)将铁氧体颗粒的珠粒与脱水己糖醇例如脱水山梨糖醇和脱水甘露糖醇的高级脂肪酸例如油酸、硬脂酸和棕榈酸的酯均匀地混合,以在铁氧体珠粒上形成涂层,高级脂肪酸脱水己糖醇酯的量是在0.1-3wt%范围内,基于由铁氧体颗粒和有机粘结剂化合物组成的铁氧体珠粒的量。
铁氧体珠粒组合物因此包括:
(A)平均粒径在0.05-0.5mm范围内的铁氧体珠粒,它是由包括平均粒径在0.5-5微米范围内的铁氧体颗粒和含量相当于铁氧体颗粒的0.2-10wt%的有机粘结剂化合物的铁氧体粉末混合物进行凝集所形成的;和
(B)在铁氧体珠粒上形成涂层的高级脂肪酸脱水己糖醇酯,高级脂肪酸脱水己糖醇酯的量是相当于铁氧体珠粒的0.1-3wt%范围内。作为本发明的主要目的的高密度铁氧体基元能够容易地由以上所定义的铁氧体珠粒组合物在金属模具中以至少0.5吨/厘米2的压制力下进行压塑而获得。
图1A和1B各自是显示了在实施例1-5和对比实施例1-5的一些中制备的压塑体的密度作为压塑加工压力的函数的曲线图。
图2A和2B各自是显示了在实施例1-5和对比实施例1-5的一些中模塑体从金属模具中抽出的压力作为模塑体的密度的函数的曲线图。
图3A和3B各自是显示了在实施例1-5和对比实施例1-5的一些中从金属模具中取出的模塑体的膨胀比率作为模塑体的密度的函数的曲线图。
图4A,4B和4C各自是显示了分别在实施例1,对比实施例1和对比实施例2中在不同模塑压力下制备的模塑棒形体的密度分布的曲线图。
图5A和5B各自是显示了在实施例6和对比实施例6中,从实施例1-5和对比实施例1-5中制得的铁氧体珠粒组合物制备的烧结铁氧体的密度作为烧结温度的函数的曲线图。
图6A和6B各自是显示了在实施例6和对比实施例6中,从实施例1-5和对比实施例1-5的一些中制得的铁氧体珠粒组合物制备的烧结铁氧体的初始磁通量作为烧结温度的函数的曲线图。
图7A和7B各自是显示了在实施例7和对比实施例7中,从实施例1-5和对比实施例1-5中制得的铁氧体珠粒组合物制备的烧结铁氧体的挠曲强度作为烧结温度的函数的曲线图。
在制备铁氧体珠粒的本发明方法的步骤(a)中,铁氧体颗粒与有机粘结剂化合物掺混得到铁氧体粉末混合物。有机粘结剂化合物没有特别的限制并能够选自通常用于制备陶瓷珠粒的供压塑用的那些,其中包括聚乙烯醇,聚丙烯酸,纤维素衍生物如甲基纤维素,聚丙烯酰胺等等,其中聚乙烯醇是优选的。与铁氧体粉末掺混的有机粘结剂化合物的量是0.2-10重量份,或优选0.5-8重量份或更优选0.7-5重量份/每100重量份的铁氧体颗粒。
本发明的方法不受特别限制地适用于任何类型的铁氧体材料,取决于模塑的铁氧体基元的预定特殊用途。如果需要,两种或多种不同的铁氧体粉未能够混合使用。铁氧体的颗粒应该具有0.5-5微米,优选0.7-3微米的平均粒径。
根据需要还选择的是,造粒用的铁氧体粉末混合物与各种有限用量的已知添加剂混合。选择性使用的添加剂的实例包括分散剂如聚羧酸的盐类,缩合萘磺酸的盐类和类似物,增塑剂如甘油,二醇化合物,三醇化合物和类似物,润滑剂如蜡、硬脂酸、硬脂酸盐和类似物,有机聚结剂如聚醚,脲烷改性聚醚,聚丙烯酸,改性聚丙烯酸和类似物以及无机聚结剂如硫酸铝,氯化铝,硝酸铝和类似物,等等。
铁氧体粉末与有机粘结剂化合物的掺混是通过添加水或通过使用单独制备的水溶液形式的有机粘结剂化合物来进行。从铁氧体粉末和已用水润湿的有机粘结剂化合物制得的铁氧体粉末混合物在步骤(b)中由已知的造粒方法如使用喷雾干燥器的喷雾干燥方法和振荡挤出造粒方法造粒成铁氧体珠粒。如此制得的铁氧体珠粒应该具有0.05-0.5mm或优选0.07-0.3mm的平均粒径。
在制备铁氧体珠粒组合物的本发明方法的步骤(c)中,按以上所述方式制备的铁氧体珠粒与脱水己糖醇化合物的高级脂肪酸酯按照特定比例进行掺混。以上提及的高级脂肪酸,它可以是饱和或不饱和的,优选包括硬脂酸,油酸和棕榈酸(虽然并不特定的限于它们),以及在分子中具有12-18个碳原子的脂肪酸(其中包括月桂酸,豆蔻酸,棕榈酸,硬脂酸和油酸)都能够使用。脱水己糖醇化合物例如有脱水山梨糖醇,脱水甘露糖醇和脱水半乳糖醇,其中脱水山梨糖醇和脱水甘露糖醇是优选的和脱水山梨糖醇是更优选的。这里的术语“脱水己糖醇”是指己糖醇或己糖的糖醇消除水分子所形成的内醚化合物。可选择性的使用两种或多种不同的高级脂肪酸脱水己糖醇酯的混合物。脱水己糖醇与高级脂肪酸的酯化反应是对脱水己糖醇化合物分子中部分或所有的羟基进行的。当然也可选择的是,脱水己糖醇是部分和全部酯化产物的混合物。
与铁氧体珠粒掺混的脱水己糖醇化合物的高级脂肪酸酯的量是在0.1-3wt%,或优选0.2-2wt%或更优选0.3-1.5wt%范围内,基于由铁氧体颗粒和有机粘结剂化合物组成的铁氧体珠粒的量。将铁氧体珠粒与高级脂肪酸脱水己糖醇酯掺混的方法能够通过以下方法来进行,虽然并不特别地限于这些方法。例如,铁氧体珠粒与由高级脂肪酸脱水己糖醇酯溶于合适的有机溶剂如醇类、甲苯和类似物中所制备的溶液混合,它们一起在转鼓混合机中进行掺混,随后干燥。此外,铁氧体珠粒在合适的流化装置中保持流化,通过喷雾将该溶液喷涂在珠粒上来进行铁氧体珠粒的涂敷。还可以使用合适的掺混机器将铁氧体珠粒和所述脱水己糖醇酯进行干混。
实施本发明方法的一种优选方案如下所述,通过已知的造粒方法,例如使用喷雾干燥器的喷雾造粒法和振荡挤出造粒法将铁氧体粉末造粒成平均粒径为0.1至0.3mm的珠粒。然后,通过上述工序使铁氧体珠粒和脱水己糖醇化合物的脂肪酸酯化合物掺混,从而在铁氧体珠粒的至少30%的表面上涂敷一层上述脱水己糖醇酯化合物,当然最好是使铁氧体珠粒的全部表面均涂覆一层上述的脱水己糖醇酯。即使部分形成上述涂层的脱水己糖醇酯化合物渗入所述铁氧体珠粒的表层也不会产生特别的缺点。
按以上方式制备的铁氧体珠粒组合物能够在金属模具中由压塑方法成形为模塑的铁氧体,后者可用作由烧结形成的电磁材料的前体。在该压塑方法中的模塑压力是在0.5-5吨/厘米2或优选在1-4吨/厘米2范围内。如此获得的模塑铁氧体的密度是(虽然取决于铁氧体材料的类型和其它因素)在3.0-4.0g/cm2范围内,当铁氧体材料是镍/铜/锌基铁氧体时。该模塑的铁氧体显示出良好的从金属模具中脱出的能力,需要较低的从金属模具中抽出的压力。还有,从金属模具中抽出的模塑体显示出减少的回弹现象,因此模塑体不存在裂纹、裂沟和其它模塑缺陷,以确保高的电磁性能。这一未曾预料到的优点归因于脂肪酸脱水己糖醇酯的表面活性,导致铁氧体珠粒的润滑性、流动性和压力传递性的改进而确保了对金属模腔的良好浸润性能和降低的模塑压力,进而导致金属模具的耐久性的延长连同从金属模具中抽出的压力的降低以及回弹现象(在从金属模具中取出模塑体时或多或少不可避免)的减少。
压塑的铁氧体可通过在800-1400℃范围内,或优选在1000-1300℃范围内的温度下进行热处理来烧结。
在下面,本发明将通过实施例和对比实施例来详细地描述,然而,决不限制本发明的范围。
实施例1
通过在湿法研磨-混合机中均匀掺混66重量份的具有平均粒径1微米的镍/铜/锌-基铁氧体颗粒,34重量份的水,1.0重量份作为粘结剂的聚乙烯醇和0.25重量份作为分散剂的聚羧酸铵盐来制备料浆化的铁氧体粉末混合物。该铁氧体粉末料浆在喷雾干燥器中进行喷雾造粒得到球形颗粒构型的平均粒径为0.125mm的铁氧体珠粒。
该铁氧体珠粒然后与用量相当于铁氧体珠粒的1.0wt%的浓度为50wt%的倍半油酸脱水山梨糖醇酯/乙醇溶液混合,然后在转鼓混合机中进行旋转掺混而得到不含任何粗的团聚物的铁氧体珠粒组合物。
将1.2g一份的铁氧体珠粒组合物在直径6.0mm的金属模具的腔内通过施加在0.5-4吨/厘米2范围内变化的压力进行压塑,得到没有裂纹和其它模塑缺陷的12-14mm长的圆柱形模塑体。模塑体然后在明显降低的抽出压力下从金属模具中脱出。
单独地,金属模具的耐久性试验被用来在金属模具中在约3吨/厘米2的压力下使用同样的铁氧体珠粒组合物来模塑1.3mm直径和1.5mm高度的粒料,结果发现,通过使用单只金属模具能够进行多大1.2百万次的压塑且没有任何明显的损坏或金属模具的磨损。
图1A,2A和3A各自由曲线I分别显示了在模塑压力和模塑的铁氧体的密度之间,在模塑的铁氧体的密度和从金属模具中抽出的压力之间以及在模塑的铁氧体的密度和模塑体的膨胀比(即回弹程度)之间的关系。
为了检查模塑体的密度分布上的变化,从2.0g一份的铁氧体珠粒组合物分别在0.5、1.0或2.0吨/厘米2的模塑压力下制备直径为6mm和长度为20-22mm的棒形模塑体。图4A显示了模塑体的密度沿着棒的长度方向分成5个等同部分A、B、C、D和E的分布,分别由对应于0.5、1.0和2.0吨/厘米的模塑压力的曲线I、II和III表示。
实施例2
实验程序基本上与实施例1中相同,只是脱水山梨糖醇酯溶液的量从1.0wt%减少至0.6wt%。
图2A中由曲线II显示了在模塑体的密度和从金属模具中抽出的压力之间的关系。显示了在模塑压力和模塑体密度之间和在模塑体的密度和膨胀比之间关系的曲线图各自非常接近于和基本上分别重叠了实施例1的图1A和3A中的各自曲线I。
实施例3
实验程序基本上与实施例1中相同,只是脱水山梨糖醇倍半油酸酯溶液被同样量的50%浓度脱水山梨糖醇单油酸酯/乙醇溶液代替。
在图1A、2A和3A的每一个中对应于曲线I的曲线图非常接近于和基本上重叠了实施例1的各自曲线I。
实施例4
实验程序基本上与实施例3中相同,只是脱水山梨糖醇酯溶液的量从1.0wt%减少至0.6wt%。
显示了在模塑压力和模塑体密度之间和在模塑体的密度和膨胀比之间的关系的曲线图各自非常接近于和基本上分别重叠了实施例1的图1A中的曲线I和图3A中的曲线I。显示了在模塑体的密度和抽出压力之间的关系的曲线图非常接近于和基本上重叠了实施例2的图2A中的曲线II。
对比实施例1
实验程序与实施例1中基本相同,只是所制备的铁氧体珠粒原样进行压塑成形为模塑的铁氧体。
图1A,2A和3A各自由曲线C-I显示了在模塑压力和模塑体的密度之间,在模塑体的密度和从金属模具中抽出的压力之间以及在模塑体的密度和模塑体的膨胀比(即回弹程度)之间的关系。类似于图4A,图4B显示了在0.5、1.0或2.0吨/厘米2的各种模塑压力下制备的模塑体的密度分布,并沿着棒形模塑体的长度方向分成5个部分,分别由曲线I、II和III表示。
这些结果表明,所制得的铁氧体珠粒在润滑性和压力传递性上比较逊色,使得模塑体的密度下降,尤其当模塑压力较低且密度分布的变化大时。还有,模塑体从金属模具中抽出的压力明显高于实施例1且附带金属模具的吱吱声,尤其当模塑压力较高导致产生层状裂纹。
对比实施例2
实验程序基本上与实施例1中相同,只是浓度50wt%的倍半油酸脱水山梨糖醇酯/乙醇溶液被用量相当于铁氧体珠粒的0.1wt%的硬脂酸锌的细干燥粉末所代替。
图2A由曲线C-II显示了在模塑体的密度和从金属模具中抽出的压力之间的关系。显示了在模塑压力和模塑体密度之间和在模塑体的密度和模塑体的膨胀比(即回弹程度)之间的关系的曲线图各自非常接近于和基本上分别重叠了在对比实施例1的图1A和图3A的每一个中的曲线C-I。
从以上结果可理解,硬脂酸锌的添加可用于改进模塑的铁氧体的脱模性能而同时降低抽出压力,但是模塑体仍然遭遇密度下降的问题,且在密度分布中有较大的不均匀性。
按照与实施例1中同样的方式通过重复铁氧体粒料的模塑加工来进行金属模具的耐久性试验无法继续重复进行到800千次以上,因为模塑的粒料由于金属模具的磨损已经无法再通过外观和尺寸的测试,即使金属模具没有肉眼观察到的明显损坏。
实施例5
通过使用搅拌造粒机(型号TM混合机,由Mitsui Kozan Co.制造)将100重量份的平均粒径为1微米的镍/铜/锌-基铁氧体粉末和17重量份的6wt%聚乙烯醇水溶液的掺混物造粒成粒状粉末。在带式干燥机上干燥后,粒化的粉末在振荡-造粒离解机(由Nippon Seiki Co.制造)中进行振荡-挤出造粒过程,随后在移位器(Shifter)上进行筛选而得到平均粒径为0.250mm的铁氧体珠粒。通过使用转鼓混合机将铁氧体珠粒与用量相当于干燥铁氧体珠粒量的1.0wt%的50wt%浓度倍半油酸脱水山梨糖醇酯/乙醇溶液混合,得到不含团聚物的铁氧体珠粒组合物。
将1.2克一份的铁氧体珠粒组合物在金属模具内通过施加0.5-4.0吨/厘米2的压制力进行压塑,得到直径6mm和长度12-14mm的圆柱形模塑体。
图1B,2B和3B各自由曲线V分别显示了在模塑压力和模塑体的密度之间,在模塑体的密度和从金属模具中抽出的压力之间以及在模塑体的密度和在从金属模具中抽出之后模塑体的膨胀比之间的关系。
对比实施例3
实验程序基本上与实施例5中相同,只是没有添加倍半油酸脱水山梨糖醇酯的乙醇溶液,从平均粒径为0.250mm的铁氧体珠粒直接制备圆柱形模塑体。
图1B,2B和3B各自由曲线C-III分别显示了在模塑压力和模塑体的密度之间,在模塑体的密度和从金属模具中抽出的压力之间以及在模塑体的密度和模塑体的膨胀比之间的关系。
通过与实施例5比较可清楚的看出,倍半油酸脱水山梨糖醇酯的添加可有效地提高模塑体的密度,降低抽出压力和降低膨胀比,当然同时还在从金属模具中抽出模塑体的过程中抑制了金属模具发出吱吱声和在模塑体中形成层状裂沟,尤其当模塑压力较高时出现的这些情况。
对比实施例4
实验程序基本上与实施例5中相同,只是倍半油酸脱水山梨糖醇酯的乙醇溶液被用量相当于铁氧体珠粒量的0.1wt%的硬脂酸锌细干燥粉末所代替。
显示了在模塑压力和模塑体的密度之间的曲线图非常接近于和基本上重叠了在对比实施例3的图1B中的曲线C-III。图2B和3B各自由曲线C-IV分别显示了在模塑体的密度和从金属模具中抽出的压力之间和在模塑体的密度和模塑体的膨胀比之间的关系。
对比实施例5
实验程序基本上与实施例5中相同,只是圆柱形模塑体的压塑是通过使用铁氧体珠粒来进行,该珠粒是通过掺混100重量份铁氧体粉末,17重量份的6%聚乙烯醇水溶液和1.0重量份的倍半油酸脱水山梨糖醇酯来制备。
显示了在模塑压力和模塑体的密度之间的曲线图非常接近于和基本上重叠了在实施例5的图1B中的曲线V。图2B和3B各自由曲线C-V分别显示了在模塑体的密度和从金属模具中抽出的压力之间和在模塑体的密度和模塑体的膨胀比之间的关系。
实施例6和对比实施例6
在实施例1-5和对比实施例1-5中制备的铁氧体珠粒组合物各自在1.0吨/厘米2的模塑压力下压塑成外直径21mm、内直径12mm和高度7mm的环形模塑体。
模塑体在1030℃、1050℃、1070℃或1090℃的温度下在空气中进行烧结热处理2小时,得到线性收缩率约15%的环形磁芯。
根据阿基米德方法,这些烧结的芯样品进行密度的测量。结果作为烧结温度的函数以曲线方式示于图5A和5B中,对于实施例1-5的铁氧体珠粒组合物分别由曲线I-V表示,和对于对比实施例1-5所使用的铁氧体珠粒或珠粒组合物分别由曲线C-I至C-V表示。
此外,初始磁通量的测量是通过使用LCR计(型号4274A,由HewlettPackard Co.制造)在100KHz的频率下对这些样品进行的。结果作为烧结温度的函数以曲线方式示于图6A和6B中,对于实施例1-5和对比实施例1,2,3和5的铁氧体珠粒组合物分别由曲线I-V,C-I,C-II,C-III和C-V表示。实施例2-4的曲线非常接近于和基本上重叠了实施例1的曲线I。对比实施例4的曲线非常接近于和基本上重叠了对比实施例3的曲线C-III。
实施例7和对比实施例7
烧结铁氧体的挠曲强度的测量是根据JIS R 1601中规定的操作程序对试样来进行,试样是由实施例1-5和对比实施例1-5中制得的铁氧体珠粒组合物的压塑和烧结获得的。因此,铁氧体珠粒组合物中的每一种在1.0吨/厘米2的压力下压塑成55mm长度、12mm宽度和5mm厚度的模塑体。模塑体在1030℃、1060℃或1090℃下进行烧结热处理2小时。测量的结果作为烧结温度的函数以曲线方式示于图7A和7B中,对于实施例1-5的珠粒组合物分别由曲线I-V表示和对于对比实施例1-5的珠粒组合物分别由曲线C-I至C-V表示。
Claims (16)
1、制备铁氧体珠粒组合物的方法,包括以下步骤:
(a)将平均粒径在0.5-5微米范围内的铁氧体的颗粒与0.2-10wt%的有机粘结剂化合物均匀掺混制备铁氧体粉末混合物;
(b)将铁氧体粉末混合物造粒成平均粒径在0.05-0.5毫米范围内的铁氧体珠粒;和
(c)将铁氧体颗粒的珠粒与脱水己糖醇化合物的高级脂肪酸酯均匀地混合,以在铁氧体珠粒上形成涂层,高级脂肪酸脱水己糖醇酯的量是在0.1-3wt%范围内,基于由铁氧体颗粒和有机粘结剂化合物组成的铁氧体珠粒的量。
2、根据权利要求1的制备铁氧体珠粒组合物的方法,其中在步骤(a)中使用的有机粘结剂化合物选自聚乙烯醇,聚乙酸乙烯酯的部分皂化产物,聚丙烯酸,甲基纤维素和聚丙烯酰胺。
3、根据权利要求2的制备铁氧体珠粒组合物的方法,其中在步骤(a)中使用的有机粘结剂化合物是聚乙烯醇。
4、根据权利要求1的制备铁氧体珠粒组合物的方法,其中在步骤(a)中使用的有机粘结剂化合物的量是基于铁氧体颗粒的0.7-5wt%。
5、根据权利要求1的制备铁氧体珠粒组合物的方法,其中铁氧体颗粒具有0.7-3微米的平均粒径。
6、根据权利要求1的制备铁氧体珠粒组合物的方法,其中在步骤(b)中制备的铁氧体珠粒具有0.07-0.3mm的平均粒径。
7、根据权利要求1的制备铁氧体珠粒组合物的方法,其中与脱水己糖醇形成酯的脂肪酸在分子中具有12-18个碳原子。
8、根据权利要求7的制备铁氧体珠粒组合物的方法,其中与脱水己糖醇形成酯的脂肪酸选自月桂酸,豆蔻酸,棕榈酸,硬脂酸和油酸。
9、根据权利要求1的制备铁氧体珠粒组合物的方法,其中脱水己糖醇选自脱水山梨糖醇,脱水甘露糖醇和脱水半乳糖醇。
10、根据权利要求9的制备铁氧体珠粒组合物的方法,其中脱水己糖醇是脱水山梨糖醇。
11、根据权利要求1的制备铁氧体珠粒组合物的方法,其中脱水己糖醇化合物的脂肪酸酯的量是基于铁氧体珠粒的0.2-2wt%。
12、铁氧体珠粒组合物,它包括:
(A)平均粒径在0.05-0.5mm范围内的铁氧体珠粒,它是由包括平均粒径在0.5-5微米范围内的铁氧体颗粒和含量相当于铁氧体颗粒的0.2-10wt%的有机粘结剂化合物的铁氧体粉末混合物进行凝集所形成的;和
(B)在铁氧体珠粒上形成涂层的高级脂肪酸脱水己糖醇酯,高级脂肪酸脱水己糖醇酯的量是相当于铁氧体珠粒的0.1-3wt%范围内。
13、根据权利要求12的铁氧体珠粒组合物,其铁氧体珠粒具有0.07-0.3mm的平均粒径。
14、根据权利要求12的铁氧体珠粒组合物,其中铁氧体颗粒具有0.7-3微米的平均粒径。
15、根据权利要求12的铁氧体珠粒组合物,其中与脱水己糖醇形成酯的脂肪酸选自月桂酸,豆蔻酸,棕榈酸,硬脂酸和油酸。
16、根据权利要求12的铁氧体珠粒组合物,其中脱水己糖醇选自脱水山梨糖醇,脱水甘露糖醇和脱水半乳糖醇。
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