CN105330275A - 用于电子应用的合成物和材料 - Google Patents

用于电子应用的合成物和材料 Download PDF

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CN105330275A
CN105330275A CN201510474302.7A CN201510474302A CN105330275A CN 105330275 A CN105330275 A CN 105330275A CN 201510474302 A CN201510474302 A CN 201510474302A CN 105330275 A CN105330275 A CN 105330275A
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equal
synthetics
nickel
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zinc
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M.D.希尔
D.B.克鲁克香克
K.M.安德森
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Conexant Systems LLC
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Abstract

本发明涉及用于电子应用的合成物和材料。本文中公开的实施方式涉及使用钴(Co)来精细调整镍-锌铁氧体的磁性质，例如磁导率和磁损耗，以改善在电子应用中的材料性能。方法包括用足够的Co+2代替镍(Ni)使得与Co+2替换有关的弛豫峰和与镍对锌(Ni/Zn)的比率有关的弛豫峰变成近似重合。当所述弛豫峰重叠时，材料磁导率可被基本上最大化且磁损耗被基本上最小化。所得材料是有用的且提供优异的性能，特别是对于在13.56MHz？ISM频段下运行的器件而言。

Description

用于电子应用的合成物和材料
相关申请的交叉引用
本申请是受让人的于2011年9月22日提交的美国申请No.13/241,033的部分继续申请，美国申请No.13/241,033根据35U.S.C.§119(e)要求2010年9月22日提交的美国临时申请No.61/385,327和2010年11月30日提交的美国临时申请No.61/418,367的优先权。各所述申请通过引用完整纳入本文。
任何优先权申请的引用纳入
在本申请的申请数据表中指明的外国或本国优先权的任何和全部申请根据37CFR1.57特此引用纳入。
技术领域
本发明实施方式涉及可用于电子应用、和特别是射频(RF)电子仪器(electronics)中的合成物(组成，composition)和材料。
背景技术
具有磁性质的各种结晶材料已经用作电子器件例如便携式电话、生物医学器件和RFID传感器中的组件。经常期望改变这些材料的组成以改善它们的性能特性。例如，可使用在晶格位点中的离子替换(substitution)或掺杂来调整材料的某些磁性质以改善在射频范围的器件性能。然而，不同的离子引入不同的材料性质变化，这经常导致性能折衷。因此，对精细调整(微调，finetune)结晶材料的组成以优化它们的磁性质(特别是对于RF应用)存在持续的需求。
发明内容
本公开内容的合成物、材料、制备方法、器件和体系各自具有若干方面，它们中的单一一个均不独自地决定(担负)其期望的属性。在不限制本发明范围的情况下，现在将简要地讨论其更突出的特征。
任何本文中未直接定义的术语应被理解为具有本领域中所理解的与其通常有关的所有含义。以下或在说明书的其它地方讨论了某些术语，以在描述各种实施方式的合成物、方法、体系等以及如何制造或使用它们中为实践者提供额外的指引。将领会的是，相同的东西可以多于一种的方式被讲到。因此，对于本文中描述的术语的任一个或多个，可使用替代性语言和同义语。本文中是否对术语进行详述或讨论并不重要。提供一些同义语或替换性方法、材料等。叙述一个或几个同义语或等同物并不排除使用其它同义语或等同物，除非明确地指明。在本说明书中使用实例(包括术语的实例)是仅为了说明的目的且不限制本文中实施方式的范围和含义。
本文中公开的实施方式涉及使用钴(Co)来精细调整镍-锌铁氧体的磁性质，例如磁导率和磁损耗，以改善在电子应用中的材料性能。在一个实施方式中，方法包括用足够的Co+2代替镍(Ni)使得与Co+2替换有关的弛豫峰和与镍对锌(Ni/Zn)的比率有关的弛豫峰变成近似重合。有利地，当所述弛豫峰重叠时，材料磁导率可被基本上最大化且磁损耗被基本上最小化。所得材料是有用的且提供优异的性能，特别是对于在13.56MHzISM频段下运行的器件而言。在一个实施方式中，在13.56MHz下，以相同量级的Q因子实现超过100的磁导率。在另一实施方式中，所述方法包括用Co+2掺杂NiZn尖晶石以制造一系列Zn减少的NiZn+Co材料，其以超过10的磁导率和有利的Q因子覆盖最高达约200MHz。使用Co精细调整NiZn合成物的方法优选通过使用高分辨率X-射线荧光的先进工艺控制而得以实现。
在优选的实施方式中，材料合成物由式Ni1-x-yZnxCoyFe2O4表示，其可通过用Co+2掺杂Ni(1-x)ZnxFe2O4而形成。在某些实施方案中，x＝0.2-0.6，且0<y<0.2。材料合成物的实施方式可具有尖晶石晶体结构且可为单一相。所述材料合成物可用在多种应用中，所述应用包括但不限于具有高的材料含量的天线，例如可用于便携式电话、生物医学器件和RFID传感器的那些。
在一些实施方式中，提供被设计成在13.56MHzISM频段下运行的天线，其包括用Co+2掺杂的镍锌铁氧体。优选地，与Co+2替换有关的弛豫峰和与Ni/Zn比率有关的弛豫峰处于近似重合。在一个实施方案中，用Co+2掺杂的镍锌铁氧体可由式Ni1-x-yZnxCoyFe2O4表示，其中x＝0.2-0.6，且0<y<0.2。在一些其它实施方式中，提供被设计成在13.56MHzISM频段下运行的RFID传感器，其包括用Co+2掺杂的镍锌铁氧体。优选地，与Co+2替换有关的弛豫峰和与Ni/Zn比率有关的弛豫峰处于近似重合。在一个实施方案中，用Co+2掺杂的镍锌铁氧体可由式Ni1-x-yZnxCoyFe2O4表示，其中x＝0.2-0.6，且0<y<0.2。
一些实施方式包括在镍-锌铁氧体中用足够的钴(Co2+)代替镍(Ni)的至少一些的方法。在一个实施方式中，所述方法包括将NiO、Fe2O3、CoOx、MnOx、ZnO和CuOx共混以形成具有预定的Ni对Zn的比率和预定的Co浓度的混合物。该系列材料的式优选为Ni1-w-x-y-zZnwCoxMnyCuzFe2O4。所述方法进一步包括将所述材料干燥，之后煅烧、研磨、以及喷雾干燥所述材料。所述方法进一步包括形成部件(零件，part)，然后将该部件烧结。所述部件可为天线例如可用于便携式电话、生物医学器件和RFID传感器的那些。
附图说明
图1示出镍-锌体系在各种Ni和Zn含量水平下的磁导率(μ)的变化；
图2示出一系列显示第一峰(最低频率)的频率(x轴)的偏移以及复磁导率(y轴)的钴谱图(频谱，spectrum)；
图3示出在材料的磁性磁导率谱图中，在100kHz和1GHz之间观察到两个弛豫峰；
图4示出根据本公开内容的一个实施方式的Ni-Zn铁氧体体系的磁性质的调整方法；
图5示出根据本公开内容的一个实施方式的钴掺杂的镍-锌铁氧体合成物的制造方法；以及
图6显示在一些实施方式中，无线器件可结合如本文中描述的材料合成物。
具体实施方式
本文中公开了用于精细调整镍锌铁氧体的磁性质以改善在各种电子应用中的材料性能的方法。本文中还公开了改性的镍锌铁氧体材料，其特别适合用于各种在13.56MHzISM频段下运行的电子器件中。根据本公开内容中描述的实施方式制备的改性的镍锌铁氧体材料表现出有利的磁性质例如提高的磁导率和降低的磁损耗。
本发明的方面和实施方式涉及用于电子器件中的改善的材料。例如，这些材料可用于形成植入性医疗器件(例如葡萄糖传感器)用的RF天线。这些材料还可用于其它目的，例如用于形成非植入性器件用的天线、或者植入性或非植入性器件的其它组件。有利地，所述材料在13.56MHz工业、医疗和科学频段处或者其附近具有优异的磁性磁导率和磁损耗正切的组合。在各种实施方式中，所述材料通过用钴精细调整NiZn尖晶石的磁导率和磁损耗而形成。如以下更详细地描述的，通过使与Co+2替换有关的弛豫峰和与Ni/Zn比率有关的弛豫峰变成近似重合，磁导率可被最大化且磁损耗可被最小化，使得在13.56MHz下可以相同量级的Q实现超过100的磁导率。可使用相同的技术制造一系列具有减少的Zn的NiZn+Co材料，其以超过10的磁导率和良好的Q覆盖最高达200MHz。
Ni-Zn体系
镍-锌铁氧体可由通式NixZn1-xFe2O4表示，且可用于要求高的磁导率的电磁应用中。图1示出镍-锌铁氧体体系在各种Ni和Zn含量水平下的磁导率(μ)的变化。例如，在约13.56MHz，磁导率随着锌含量减少而降低。磁导率的变化暗示：在其中磁导率不那么重要的应用中，可由具有低或零锌含量的Ni-Zn体系得到低磁损耗(高磁性Q)材料。然而，对于某些RFID标签和传感器，Ni-Zn体系不提供最佳性能，因为磁导率对于具有有利的Q的合成物而言太低，或者Q对于具有高的磁导率的合成物而言太低。
钴掺杂的影响
图2示出一系列显示第一峰的频率(x轴)(最低频率)的偏移以及复磁导率(y轴)的钴谱图。钴对频率的影响在约0.025钴处开始停止，因为磁晶各向异性刚好在复磁导率压平(变平，flattenout)(其然后再次下降)时最终经过极小值。如图2中显示的，受钴驱使的第一峰随着Co+2浓度提高最终与第二峰合并。在图2中，带有“ExtRef”的曲线表示Ni/Zn外参比，且另一曲线表示Co2+掺杂的Ni/Zn体系的频率吸收峰。
图3显示在材料的磁性磁导率谱图中，在100kHz和1GHz之间观察到两个弛豫峰。不束缚于具体的理论，据信较低的频率峰对应于磁畴壁旋转，和较高的频率峰对应于磁畴壁膨胀(鼓突，bulging)。还据信钴氧化物可通过降低尖晶石材料的磁晶各向异性而将与磁损耗有关的较低频率弛豫峰推向较高的频率值。在一些实施方式中，这些较高的频率值高于作为RFID标签和RF医疗传感器应用中经常使用的频率的13.56MHz。还据信锰可用来防止铁从Fe3+还原为Fe2+态，且因此改善材料横跨谱图的介电损耗，并且铜可充当容许烧制温度降低的烧结助剂，因此防止Zn从由材料形成的部件的表面挥发。可对以上提到的两个弛豫峰进行调节以提供在约1MHz-约200MHz的整个范围的高磁导率低损耗材料。
不希望受理论束缚，据信第二峰是由Ni/Zn比率确定的，且因此对于固定的比率是静态的。在较高的Co2+浓度下，Co2+在谱图中不再是有区别的峰。还据信第一峰可由畴移动支配，和第二峰可由旋转支配，并且对于给定的Ni/Zn比率，所述峰可在一些Co2+掺杂水平下合并，且仅畴移动峰强烈地对Co2+敏感。
基于发明人的如下理论，可对Co2+和Ni/Zn的组合进行选择以在给定的频率合并，使得吸收曲线的斜率是使磁损耗最小化的给定的频率距离方式(frequencydistanceway)：畴旋转受Ni/Zn比率驱使且决定特征峰频率，且壁移动(经由磁致伸缩而膨胀)受Co2+浓度驱使，其产生第二独立的特征峰。最佳峰位置可取决于所需的磁导率和损耗而选择。对于一些应用而言，最佳峰位置为约100MHz以在13.56MHz下得到低的损耗、但是高的磁导率。
改性的Ni-Zn体系
本公开内容的某些实施方式提供改性的镍-锌铁氧体材料。基础镍-锌铁氧体材料优选具有由式Ni0.5Zn0.5Fe2O4表示的组成。所述材料具有0.02-0.10式单位(配方单位，formulaunit)的铁缺陷、0-0.05式单位的钴含量(替换Ni)、以及0-0.03式单位的锰(替换Fe)和铜(替换Ni)含量。所述材料的实施方式可具有尖晶石晶体结构和可为单相的。
在一些实施方案中，改性的Ni-Zn铁氧体材料可具有由下式表示的组成：Ni1-w-x-y-zZnwCoxMnyCuzFe2-aO4-1.5a，其中w为0.2-0.6，且x、y和z各自为0-0.2，并且a为0-0.2。在优选的实施方案中，w＝0.4725，x＝0.0225，y＝0.02，z＝0，且a＝0.08，其可导致在13.56MHz下显示出特别期望的磁性质的材料。在另一优选的实施方案中，w＝0.4，x＝0.0275，y＝0.01，z＝0且a＝0.08，其可导致在27MHz下显示出特别期望的磁性质的材料。
以下表1示出在完全致密的5000高斯Ni1-x-yZnxCoyFe2O4尖晶石中Co替换的实施方式对谱图的影响。
制造改性的Ni-Zn材料的方法
图4示出根据本公开内容的一个实施方式的Ni-Zn铁氧体体系的磁性质的调整方法。所述方法首先在步骤100中识别所需的运行频率，之后在步骤110中调节镍对锌的比率。优选地，对Ni/Zn比率进行调节以提供在高于所需低磁损耗频率的所需频率下的弛豫吸收峰。所述方法进一步包括在步骤120中调节钴含量。优选地，将钴含量调节至其中钴支配的弛豫峰合并到Ni/Zn比率峰的低频端的水平。所述方法之后可为在步骤130中以所识别的Ni/Zn比率和Co浓度形成部件。在一些应用中，会期望使用过量的钴，因为钴有可能降低磁性磁导率而不提高磁损耗。钴的期望量可通过识别产生如下频率下的弛豫吸收峰的钴的量而确定：在低频率侧的阻抗分析迹线中，其不能通过眼睛从Ni/Zn比率峰解析出来。例如，如果对在27MHz下的RF应用感兴趣，则材料可以组成Ni0.5725Co0.0275Zn0.4Fe2O4合成，其具有54的磁导率和大于100的磁性Q，其中所述磁性Q是在规定频率下实数磁导率对虚数磁导率的比率。
图5示出根据本公开内容的一个实施方式的钴掺杂的镍-锌铁氧体合成物的制造方法。所述方法以步骤200开始，在步骤200中，将原料氧化物NiO、Fe2O3、CoOx、MnOx、ZnO和CuOx通过剪切混合方法(例如Cowles混合机)或者通过振动磨机共混而共混。步骤210指示将材料干燥。所述方法进一步包括步骤220，在步骤220中，将所述材料在900℃-1200℃的温度下煅烧，以使所述材料的组分反应和形成尖晶石相，之后为其中将所述材料研磨至1-10微米的粒度的步骤230，和在步骤240中与添加的粘结剂一起喷雾干燥。在一些实施方案中，所述方法进一步包括步骤250和步骤260，在步骤250中，将所述材料通过等压或硬模压制而形成为部件，在步骤260中，将所述部件在空气中或在氧气中烧结到1100℃-1400℃的温度。
结合改性的Ni-Zn材料的器件和体系
根据本文中描述的实施方式制成的材料合成物可用于多种应用中，所述应用包括但不限于具有高的材料含量的天线，例如可用于便携式电话、生物医学器件和RFID传感器的那些。图6显示在一些实施方式中，无线器件600可结合如本文中描述的材料合成物。这样的器件600可包括模块602、电池604、接口606和天线608。天线608可配置成促进RF信号的发射和接收，优选在13.56MHz范围内。天线608包括以这样的方式配置的钴掺杂的镍锌铁氧体：将钴含量调节至其中钴支配的弛豫峰合并到Ni/Zn比率峰的低频端的水平。在一个实施方案中，天线608的至少一部分具有可由下式表示的组成：Ni1-x-yZnxCoyFe2O4，其中x＝0.2-0.6且0<y<0.2。在另一实施方案中，天线608的至少一部分具有可由下式表示的组成：Ni1-w-x-y-zZnwCoxMnyCuzFe2-aO4-x，其中0.2≤w≤0.6；0≤x≤0.2；0≤y≤0.2；0≤z≤0.2；且0≤a≤0.2。
虽然已经描述了本发明的某些实施方式，这些实施方式仅以实例的方式提出，且不拟限制本公开内容的范围。实际上，本文中描述的新的合成物、方法和体系可以多种其它形式实施；而且可对本文中描述的合成物、方法和体系的形式作出各种省略、替换和改变，而不偏离本公开内容的精神。所附权利要求和它们的等同物拟覆盖落在本公开内容的范围和精神内的这样的形式或修改。

Claims (20)

1.由下式表示的合成物
Ni1-w-x-y-zZnwCoxMnyCuzFe2-aO4-1.5a，
w大于或等于0.2且小于或等于0.6；
x大于或等于0且小于或等于0.2；
y大于或等于0且小于或等于0.2；
z大于或等于0且小于或等于0.2；且
a大于或等于0且小于或等于0.2。
2.权利要求1的合成物，其中w＝0，x＝0.0225，y＝0.02，z＝0且a＝0.08。
3.权利要求1的合成物，其中z＝0。
4.权利要求1的合成物，其中y＝0。
5.结合权利要求1的合成物的RF器件，其中所述RF器件以13.56MHz频段运行。
6.结合权利要求1的合成物的RF器件，其中所述RF器件为天线。
7.由下式表示的改性的镍-锌铁氧体合成物
Ni1-x-yZnxCoyFe2O4，
x大于或等于0.2且小于0.6，且y大于或等于0且小于0.2。
8.权利要求7的合成物，其中x大于或等于0.1且小于或等于0.3。
9.权利要求7的合成物，其中y等于0.0225。
10.结合权利要求7的合成物的RF器件，其中所述RF器件选自RFID标签、生物医学传感器、和RF天线。
11.结合权利要求7的合成物的RF器件，其中所述RF器件以13.56MHz频段运行。
12.精细调整镍-锌铁氧体材料的方法，所述方法包括：
调节镍对锌的比率以提供在高于所需低磁损耗频率的所需频率处的Ni/Zn弛豫吸收峰；和
用钴(Co2+)掺杂所述材料至其中钴支配的弛豫峰合并到Ni/Zn弛豫吸收峰的低频端的水平。
13.权利要求12的方法，进一步包括以所述镍对锌的比率和Co浓度形成材料。
14.权利要求13的方法，进一步包括对所述材料进行烧结。
15.权利要求13的方法，其中所述材料使天线适用于RF器件。
16.权利要求15的方法，其中所述RF器件以13.56MHz频段运行。
17.权利要求13的方法，其中所述材料由式Ni1-x-yZnxCoyFe2O4表示，x为0.2-0.6，且y为0-0.2。
18.权利要求12的方法，其中所述镍对锌的比率为0.45-0.55。
19.权利要求12的方法，其中与Co+2掺杂有关的弛豫峰和与镍对锌(Ni/Zn)的比率有关的弛豫峰变成近似重合。
20.权利要求12的方法，进一步包括将原料氧化物NiO、Fe2O3、CoOx、MnOx、ZnO和CuOx共混以形成具有已定的Ni对Zn的比率和已定的Co浓度的混合物。
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