CN117326860A - 一种单轴型小线宽六角铁氧体材料及其制备方法 - Google Patents
一种单轴型小线宽六角铁氧体材料及其制备方法 Download PDFInfo
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- 238000000498 ball milling Methods 0.000 claims abstract description 19
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- 238000005245 sintering Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims description 7
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
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- 239000010949 copper Substances 0.000 description 26
- 230000005350 ferromagnetic resonance Effects 0.000 description 15
- 239000013078 crystal Substances 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
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- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- MTRJKZUDDJZTLA-UHFFFAOYSA-N iron yttrium Chemical compound [Fe].[Y] MTRJKZUDDJZTLA-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种单轴型小线宽六角铁氧体材料及其制备方法，属于铁氧体材料制备技术领域。本发明首先预烧生成Cu 18H六角铁氧体粉末，加入SiO2添加剂进行高能球磨，球磨得到的亚微米粉末在磁场成型压机取向后烧结生成高密度、织构化Cu 18H六角铁氧体材料。本发明提供的单轴型小线宽Cu 18H六角铁氧体材料及其制备方法，制备工艺为传统固相反应法，操作简单且工艺成熟；制备的Cu 18H六角铁氧体材料兼具高密度(ρ≥5.3g/cm3)、高饱和磁化强度(4πMs≥1400G)、高剩磁比(Mr/Ms≥0.6)、高磁晶各向异性场(Ha≥9kOe)、低铁磁共振线宽(ΔH≤320Oe)特性，适用于自偏置环形器设计，以减小通信系统收发模块重量和体积。
Description
技术领域
本发明属于铁氧体材料制备技术领域，具体涉及一种单轴型小线宽六角铁氧体材料及其制备方法。
背景技术
随着无线通信技术的迅猛发展，通信系统对小型化、轻量化和低损耗的要求越来越高。作为通信系统收发模块中的关键器件，环行器利用铁氧体材料的旋磁效应实现射频信号通过单一通道同时发送和接收。传统环形器用铁氧体，如钇铁石榴石、Ni系尖晶石铁氧体、Li系尖晶石铁氧体等，具有立方晶体结构和低磁晶各向异性，因此需要外加偏置磁场实现旋磁效应。偏置磁场通常由永磁体提供，这增加了环行器的体积、重量和成本，不利于无线通信系统向扁平化和集成化发展。单轴型六角铁氧体具有较强的磁晶各向异性，可在很小的偏置磁场或无任何外加磁场时使磁矩在微波场作用下围绕其磁晶各向异性场进动。基于单轴型六角铁氧体设计的环形器可摆脱外置磁钢，实现自偏置特性，从而显著减小通信系统收发模块的重量和体积。
环形器的插入损耗与铁氧体的铁磁共振线宽密切相关，通过金属离子取代和制备工艺优化可实现六角铁氧体铁磁共振频率与铁磁共振线宽调控。例如，美国东北大学(Appl.Phys.Let t.,2006,88,62516)使用丝网印刷工艺和磁场取向技术制备了织构化的多晶M型六角铁氧体薄膜，在V波段实现了310Oe的零场铁磁共振线宽。电子科技大学(J.Am.Ceram.Soc.,2022,105,7492)通过控制晶粒和晶界中铜离子分布，将多晶M型六角铁氧体的铁磁共振线宽显著降低至303Oe。专利CN108424137B采用固相反应法制备了高各向异性低铁磁共振线宽M型六角铁氧体，其44GHz的零场铁磁共振线宽小于370Oe。专利CN114409392B公开了一种W型和M型复合的六角铁氧体材料，具有高剩磁比和低损耗特性，最优配方的零场铁磁共振线宽为317Oe。迄今为止报道的多晶六角铁氧体最小零场铁磁共振线宽约为300Oe，这使得基于多晶六角铁氧体自偏置环行器的插入损耗很难进一步降低。
发明内容
本发明提供一种单轴型小线宽六角铁氧体材料及其制备方法，通过调控制备工艺实现较小的零场铁磁共振线宽，对于实现低损耗自偏置器件具有重要意义。
本发明的核心思想：传统环形器用铁氧体具有立方晶体结构和低磁晶各向异性，因此需要外加偏置磁场实现环形功能。单轴型六角铁氧体具有较强的磁晶各向异性，可在很小的偏置磁场或无任何外加磁场时使磁矩在微波场作用下围绕其磁晶各向异性场进动，实现自偏置特性，从而显著减小通信系统收发模块的重量和体积。新型18H六角铁氧体(Ba5Me2Ti3Fe12O31，Me＝Mg、Fe、Co、Ni、Cu、Zn等)有别于传统六角铁氧体的晶体结构，其晶胞可视为向Y型六角铁氧体晶胞的T块中插入一个钛酸钡块构成。首先，引入Cu2+离子可调控其磁晶各向异性，Cu 18H六角铁氧体具有单轴型磁晶各向异性，易磁化轴沿晶体c轴；其次，样品成型过程中的磁场取向技术使晶粒易磁化轴排列一致，进一步提高样品磁各向异性和剩磁比；再次，低熔点CuO和高熔点SiO2添加剂的协同效应，在形成液相烧结，促使样品致密化的同时，抑制晶粒异常生长，使得晶粒尺寸细小且均匀。高阻态SiO2添加剂富集于晶界，可有效提高晶界电阻率，降低材料高频损耗。因此，本发明基于一种具有新型晶体结构的18H六角铁氧体材料，通过Cu2+离子调控18H六角铁氧体材料磁晶各向异性，联合SiO2添加剂和磁场取向技术实现高密度、细晶粒、织构化的多晶显微形貌，有效提高Cu 18H六角铁氧体磁晶各向异性和剩磁比，显著降低由于气孔和各向异性导致的铁磁共振展宽，最终制备高密度、小线宽、低损耗Cu 18H六角铁氧体材料。
本发明采用的技术方案如下：
本发明提供了一种单轴型小线宽六角铁氧体材料及其制备方法，具体步骤如下：
S1.配料；按Cu 18H六角铁氧体化学式Ba5Cu2Ti3Fe12O31的化学计量比计算并称量BaC O3、CuO、TiO2、Fe2O3原料粉末。
S2.一次球磨；将步骤S1所得原料粉末在球磨机内分别混合均匀，球磨时间2～4小时。
S3.预烧；将步骤S2所得一次球磨料烘干，随后在1050～1150℃预烧3～5小时生成Cu 18H六角铁氧体预烧粉末。
S4.掺杂；向步骤S3所得Cu 18H六角铁氧体预烧粉加入占总质量0.5～1.5wt％的SiO2作为掺杂剂。
S5.二次球磨；将步骤S4所得混合粉末在高能球磨机中以去离子水为球磨介质球磨8～16小时，球磨后的目标平均颗粒尺寸为0.4～0.8μm。
S6.成型；将步骤S5所得的脱水浆料在磁场成型机下压制成生坯，脱水浆料含水量控制在30wt％～35wt％之间，成型磁场强度为1.2～1.4T，成型压强为80～120MPa，保压时间为40～60s。
S7.烧结；将步骤S6所得生坯置于烧结炉内，在1100～1150℃烧结3～5小时，生成Cu 18H六角铁氧体。
针对步骤S7所得样品，采用X射线衍射仪分析样品相成分和晶粒取向度；采用扫描电子显微镜观察样品微观形貌；采用阿基米德原理测量样品密度ρ；采用振动样品磁强计测量样品平行于c轴和垂直于c轴的磁滞回线，表征其各向异性；从磁滞回线分析得出饱和磁化强度4πMs、剩余磁化强度4πMr、剩磁比Mr/Ms和矫顽力Hc，采用矢量网络分析仪测量样品零场下铁磁共振频率f0和铁磁共振线宽ΔH，各向异性场Ha通过基特尔公式计算得出。
本发明制备的Cu 18H六角铁氧体材料主要技术指标：ρ≥5.3g/cm3、4πMs≥1400G、Mr/Ms≥0.6、Ha≥9kOe、ΔH≤320Oe。
本发明的有益效果如下：Cu 18H六角铁氧体制备工艺为传统固相反应法，操作简单且工艺成熟；Cu 18H六角铁氧体具有较高的各向异性场和剩磁比，有利于实现自偏置特性；Cu 18H六角铁氧体具有较高的密度和较低的铁磁共振线宽，有利于减小自偏置器件的插入损耗。基于单轴型六角铁氧体设计的环形器可摆脱外置磁钢，实现自偏置特性，从而显著减小通信系统收发模块的重量和体积。
附图说明
图1为实施例1～3所得Cu 18H六角铁氧体材料的X射线衍射图。
图2为实施例1所得Cu 18H六角铁氧体材料的扫描电子显微镜照片。
图3为实施例1所得Cu 18H六角铁氧体材料的平行于c轴和垂直于c轴的磁滞回线。
图4为实施例1～3所得Cu 18H六角铁氧体材料的铁磁共振线宽拟合图。
具体实施方式
下面通过实施例，对本发明的核心思想和技术方案作进一步技术说明，但是本发明并不限于这些实施例。
实施例1～3的具体制备方法包括以下步骤：
1.配料；按Cu 18H六角铁氧体化学式Ba5Cu2Ti3Fe12O31的化学计量比计算并称量BaCO 3、CuO、TiO2、Fe2O3原料粉末。实施例1～3中各原料粉末的摩尔百分比如下表。
2.一次球磨；将步骤1所得Cu 18H六角铁氧体原料粉末在球磨机内分别混合均匀，球磨时间2小时。
3.预烧；将步骤2所得Cu 18H六角铁氧体一次球磨料烘干。随后在1050℃预烧4小时得到Cu 18H六角铁氧体预烧粉末。
4.掺杂；将步骤3所得Cu 18H六角铁氧体预烧粉按质量比加入占总质量1.0wt％的SiO2掺杂剂。
5.二次球磨；将步骤4所得混合粉末在高能球磨机中以去离子水为球磨介质球磨12小时，得到的平均颗粒尺寸为0.7μm。
6.成型；将步骤5所得二次球磨料脱水，脱水后浆料含水量控制在30wt％，然后在磁场成型压机下压制成生坯；成型磁场强度为1.2T，成型压强为100MPa，保压时间为60s。
7.烧结；将步骤6所得生坯置于烧结炉内，在1100～1150℃烧结4小时，生成Cu 18H六角铁氧体；实施例1～3的烧结温度如下表：
对步骤7所得样品的相成分、微观形貌和磁特性进行表征和测试。采用阿基米德原理测量样品密度ρ；采用振动样品磁强计测量样品平行于c轴和垂直于c轴的磁滞回线，表征其各向异性，如图3所示；从磁滞回线分析得出饱和磁化强度4πMs、剩余磁化强度4πMr、剩磁比Mr/Ms和矫顽力Hc；采用矢量网络分析仪测量样品零场下铁磁共振频率f0和铁磁共振线宽ΔH，各向异性场Ha通过基特尔公式计算得出。经以上工艺制备的实施例1～3性能参数如下表。
综上所述，本发明基于18H六角铁氧体，通过Cu2+离子调控磁晶各向异性，联合高熔点SiO2添加剂，采用磁场取向技术，制备了高密度(ρ≥5.3g/cm3)、高饱和磁化强度(4πMs≥1400G)、高剩磁比(Mr/Ms≥0.6)、高磁晶各向异性场(Ha≥9kOe)、低铁磁共振线宽(ΔH≤320Oe)的Cu 18H六角铁氧体材料。其零场下铁磁共振线宽低于大多数已报道的多晶六角铁氧体。这些结果证明了通过传统固相反应法制备高密度、织构化、小线宽18H六角铁氧体的可行性，为设计基于Cu 18H六角铁氧体的低损耗自偏置环形器提供了材料基础，从而使环形器摆脱外置磁钢，显著减小通信系统收发模块的重量和体积。
可以理解，本发明是通过一些实施例进行描述的，本领域技术人员知悉的，在不脱离本发明的精神和范围的情况下，可以对这些特征和实施例进行各种改变或等效替换。另外，在本发明的教导下，可以对这些特征和实施例进行修改以适应具体的情况及材料而不会脱离本发明的精神和范围。因此，本发明不受此处所公开的具体实施例的限制，所有落入本申请的权利要求范围内的实施例都属于本发明所保护的范围内。
Claims (2)
1.一种单轴型小线宽六角铁氧体材料，其特征在于，所述六角铁氧体材料为Cu 18H六角铁氧体材料，具有单轴型磁晶各向异性，其化学表达式为：Ba5Cu2Ti3Fe12O31。
2.一种单轴型小线宽六角铁氧体材料的制备方法，其特征在于，包括以下步骤：
S1.配料；按Cu 18H六角铁氧体化学式Ba5Cu2Ti3Fe12O31的化学计量比计算并称量BaCO3、CuO、TiO2、Fe2O3原料粉末；
S2.一次球磨；将步骤S1所得原料粉末在球磨机内分别混合均匀，球磨时间2～4小时；
S3.预烧；将步骤S2所得一次球磨料烘干，随后在1050～1150℃预烧3～5小时生成Cu18H六角铁氧体预烧粉末；
S4.掺杂；向步骤S3所得Cu 18H六角铁氧体预烧粉加入占总质量0.5～1.5wt％的SiO2作为掺杂剂；
S5.二次球磨；将步骤S4所得混合粉末在高能球磨机中以去离子水为球磨介质球磨8～16小时，球磨后的目标平均颗粒尺寸为0.4～0.8μm；
S6.成型；将步骤S5所得浆料脱水，脱水后浆料含水量控制在30wt％～35wt％之间，脱水浆料在磁场成型机下压制成生坯，成型磁场强度为1.2～1.4T，成型压强为80～120MPa，保压时间为40～60s；
S7.烧结；将步骤S6所得生坯置于烧结炉内，在1100～1150℃烧结3～5小时，生成Cu18H六角铁氧体。
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