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TWI833031B - 摻雜釕的z型六方晶系鐵氧體、包含彼之複合物與製品、以及彼之製備方法 - Google Patents

摻雜釕的z型六方晶系鐵氧體、包含彼之複合物與製品、以及彼之製備方法 Download PDF

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TWI833031B
TWI833031B TW109125753A TW109125753A TWI833031B TW I833031 B TWI833031 B TW I833031B TW 109125753 A TW109125753 A TW 109125753A TW 109125753 A TW109125753 A TW 109125753A TW I833031 B TWI833031 B TW I833031B
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ferrite
ghz
ferrite composition
composition
frequency
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TW109125753A
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TW202110772A (zh
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李啟帆
亞杰 陳
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美商羅傑斯公司
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Abstract

在一態樣中，包含具有下式之Ru-Co2 Z鐵氧體的鐵氧體組合物：(Ba3-x Mx )Co2 (M'Ru)y Fe24-2y-z O41 ，其中，M係Sr、Pb、或Ca之至少一者；M' 係Co、Zn、Mg、或Cu之至少一者；x 係 1至3；y 係大於0至2；以及z 係 -4至4。在另一態樣中，製品係包含該鐵氧體組合物。在其他態樣中，製備該鐵氧體組合物的方法係包含：混合包含Fe、Ba、Co、及Ru之鐵氧體的前驅化合物；以及將該鐵氧體的前驅化合物於氧氣氣氛中進行燒結，以形成Ru-Co2 Z鐵氧體。

Description

摻雜釕的Z型六方晶系鐵氧體、包含彼之複合物與製品、以及彼之製備方法
本文係揭露摻雜釕的Z型六方晶系鐵氧體。
為滿足在各種商業及國防相關產業中特別令人感興趣之超高頻（UHF）、L-波段、及S-波段應用中所用裝置不斷增長的需求，需要經改良的性能且微型化。作為雷達及現代無線通訊系統中的重要組件，不斷地開發具有小型尺寸的天線元件。然而，開發用於該些高頻應用的鐵氧體材料係具有挑戰性的，因為大部分的鐵氧體材料在高頻下展現相對高的磁損耗（magnetic loss）。一般而言，六方晶系鐵氧體（hexagonal ferrite 或 hexaferrite）為一種鐵–氧化物陶瓷化合物，具有六方晶體結構並展現磁性。已知數種六方晶系鐵氧體家族，包括Z型鐵氧體（Ba3 Me2 Fe24 O41 ）及Y型鐵氧體（Ba2 Me2 Fe12 O22 ），其中Me可為小的2+陽離子（例如Co、Ni、或Zn）、以及Sr可被Ba取代。其他六方晶系鐵氧體的種類包括M型鐵氧體（(Ba,Sr)Fe12 O19 ）、W型鐵氧體（(Ba,Sr)Me2 Fe16 O27 ）、X型鐵氧體（(Ba,Sr)2 Me2 Fe28 O46 ）、及U型鐵氧體（(Ba,Sr)4 Me2 Fe36 O60 ）。
部分六方晶系鐵氧體（例如經鈷取代之鋇Y型（Co2 Y）及Z型（Co2 Z）六方晶系鐵氧體）可具有相較於尖晶石鐵氧體更高的鐵磁共振頻率及磁導率，使其在高頻應用中具有吸引力。儘管有這些改良，它們在高頻及微波裝置中的用途仍受限制，因為這些替代也會導致磁損耗提升。雖然Z型鐵氧體為高阻抗磁介電複合物（magneto-dielectric composite）的候選者，但高磁損耗限制了它們的用途。因此，需要經改良的Z型鐵氧體。
在一態樣中，一種鐵氧體組合物，包含具有下式之Ru-Co2 Z鐵氧體：(Ba3-x Mx )Co2 (M'Ru)y Fe24-2y-z O41 ，其中M係Sr、Pb、或Ca之至少一者；M' 係Co、Zn、Mg、或Cu之至少一者；x 係 1至3；y 係大於0至2；以及，z 係 -4至4。
在另一態樣中，一種製品，其包含該鐵氧體組合物或鐵氧體複合物之至少一者。
在其他態樣中，製造該鐵氧體組合物的方法係包含：混合包含Fe、Ba、Co、及Ru之鐵氧體的前驅化合物（precursor compound）；以及，將該鐵氧體的前驅化合物於氧氣氣氛中進行燒結，以形成Ru-Co2 Z鐵氧體。
本發明之上述及其他特徵係透過以下附圖、詳細說明、及申請專利範圍進行例示。
經發現，將Z型六方晶系鐵氧體中至少一部分之鐵離子以釕進行取代，可以產生具有經改良之性質的Ru-Co2 Z鐵氧體。具體地，該Ru-Co2 Z鐵氧體可具有以下通式： (Ba3-xMx)Co2 (M'Ru)y Fe24-2y-z O41 其中，M係Sr、Pb、或Ca之至少一者；M'係Co、Zn、Mg、或Cu之至少一者；x係1至3；y係大於0至2、或0.001至2；以及z係-4至4。M'可為Co。Ru與M'的比值可為0.01至3、或0.01至1。可將該變量z修改為非零，以包括非化學計量的組合物。
該Ru-Co2 Z鐵氧體可具有平面易磁化作用（c-平面）。該Ru-Co2 Z鐵氧體可具有高磁導率、高操作頻率、或低磁損耗之至少一者，使其可適用於在S-L波段頻率下作為天線或感應器。該Ru-Co2 Z鐵氧體可於固態陶瓷形式下在1至2吉赫（gigahertz）、或在2至4吉赫之頻率下具有大於或等於3.5、或者大於或等於5、或者5至10的磁導率。該Ru-Co2 Z鐵氧體可於固態陶瓷形式下在1至2吉赫之頻率下具有小於或等於0.4、小於或等於0.2、或者小於或等於0.1、或者小於或等於0.08、或者0.04至0.4的磁損耗正切（tanδµ ）。 該Ru-Co2 Z鐵氧體可於固態陶瓷形式下在1至2吉赫之頻率下具有6至15、或6至12、或10至14的介電係數。該Ru-Co2 Z鐵氧體可於固態陶瓷形式下在1至2吉赫之頻率下具有小於或等於0.15、小於或等於0.009、或者小於或等於0.008、或者0.002、或者0.001至0.15的介電損耗正切（tanδɛ ）。該Ru-Co2 Z鐵氧體可於固態陶瓷形式下具有0.1至4吉赫、或0.5至2吉赫、或1至2吉赫的操作頻率。
該Ru-Co2 Z鐵氧體可在超高頻率範圍中具有低介電損耗正切（tanδɛ ）或磁損耗正切（tanδµ ）之至少一者。舉例言之，該Ru-Co2 Z鐵氧體可於固態陶瓷形式下具有以下至少一者：在1至2吉赫之頻率下小於或等於0.01、或小於或等於0.008、或0.006至0.01的介電損耗正切（tanδɛ ）、或者小於或等於0.12、或小於或等於0.08、或0.05至0.12的磁損耗正切（tanδµ ）。
如本文中使用，磁及介電性質係於同軸空氣線（coaxial airline）中使用Nicholson-Ross-Weir（NRW）法透過向量網路分析儀（vector network analyzer，VNA）進行測量，並且磁導率及介電係數之數值分別為相對磁導率及相對介電係數。
該Ru-Co2 Z鐵氧體可使用任何合適的方法進行製備。一般而言，該Ru-Co2 Z鐵氧體可透過先形成包含前驅化合物的混合物來形成，該前驅化合物係包括至少Ba、M、Co、Ru、及Fe的氧化物，其中M係Sr、Pb、或Ca。舉例言之，該混合物可至少包含BaCO3 、 MCO3 、Co3 O4 、RuO2 、及Fe2 O3 。基於該混合物的總重量計，該混合物可包含5至20重量%之BaCO3 。基於該混合物的總重量計，該混合物可包含5至50重量%之MCO3 。基於該混合物的總重量計，該混合物可包含2至15重量%之Co3 O4 。基於該混合物的總重量計，該混合物可包含0.1至10重量%之RuO2 。基於該混合物的總重量計，該混合物可包含50至80重量%之Fe2 O3 。該混合物可進一步包含Zn、Mg、或Cu之至少一者的氧化物。需注意該混合物之重量百分比可基於在混合物中之氧化物的總重量計。
該混合物可於空氣中進行鍛燒，以形成包含Z型鐵氧體的鐵氧體。該鍛燒可在800至1,300攝氏溫度（°C）的鍛燒溫度下進行。該鍛燒可進行0.5至20小時、1至10小時、或2至5小時的鍛燒時間。需注意該鍛燒步驟為視需要的，並且唯一的加熱步驟可為燒結，以形成鐵氧體。
該鐵氧體可經粉碎並視需要過篩，以形成顆粒。該過篩可包含藉由10至100網目之篩網進行過篩。粗顆粒可進一步進行研磨以降低顆粒尺寸。該顆粒可具有0.5至50微米（micrometer）、或0.5至10微米的體積中位數D50顆粒尺寸。該顆粒尺寸可使用Horiba LA-910雷射光散射PSD分析儀進行測定、或者根據ASTM D4464-15進行測定。可將該鐵氧體與黏結劑（binder）混合。該黏結劑可包含聚乙烯醇、甲基纖維素、聚乙烯醇縮丁醛、聚乙二醇、或聚碳酸伸烴酯（poly(alkylene carbonate)）之至少一者。基於該鐵氧體及黏結劑之總重量計，該黏結劑可以8至12重量%之含量存在。該黏結劑可促進鐵氧體成形並可於燒結期間完全燒盡。經黏結之鐵氧體可具有10至300微米、或50至300微米的體積中位數D50顆粒尺寸。
可視需要地對該鐵氧體進行成形或燒結，以形成Ru-Co2 Z鐵氧體。成形方法並無限制且可包含單軸壓縮、等壓壓製（isostatic pressing）、鑄造、壓製、或類似者的至少一種。該壓製可在每平方公分0.5至2公噸之壓力下進行。該燒結可在1,000至1,300°C、或1,200至1,250°C之燒結溫度下進行。升高至該燒結溫度、及自該燒結溫度降低的斜升溫／斜降溫（ramping temperature）可各自獨立地於每分鐘1至5°C之斜升溫／斜降溫速率下進行。該燒結可進行1至20小時或5至12小時之燒結時間。該燒結可於氧氣環境中進行，以協助減少介電損耗。氧氣可以每分鐘0.1至10公升之流速引入燒結室中。經燒結之Ru-Co2 Z鐵氧體可依其應用而以任何所欲方式進行最終加工，例如：切割或拋光。
在燒結之前，可將一含量之氧化鉍添加至鐵氧體中。基於鐵氧體之總重量計，該氧化鉍可以0.2至5重量%之含量進行添加。可存在於Z型鐵氧體相晶界之Bi2 O3 的添加可以幫助獲得具有相同或實質上相同之磁導率及介電係數數值且維持低磁及介電損耗正切的組合物。
該Ru-Co2 Z鐵氧體可具有1至100微米、或5至50微米之平均晶粒尺寸。該晶粒尺寸可使用穿透式電子顯微鏡、場發射掃瞄式電子顯微鏡、或X光繞射之至少一者進行測量。
該Ru-Co2 Z鐵氧體可為塊體陶瓷、或可存在於複合物中，例如：包含該Ru-Co2 Z鐵氧體及聚合物的複合物。該聚合物可包含熱塑性聚合物或熱固性聚合物。如本文中使用，所謂「熱塑性（thermoplastic）」係指可塑或可變形、於加熱時熔成液態、且於充分冷卻時凍結成脆性之玻璃態的材料。可使用之熱塑性聚合物的例子包括環狀烯烴聚合物（包括聚降冰片烯（polynorbornene）及含有降冰片烯基單元之共聚物，例如：如降冰片烯之環狀聚合物與如乙烯或丙烯之非環狀烯烴的共聚物）、氟聚合物（例如：聚氟乙烯（PVF）、聚偏二氟乙烯（PVDF）、氟化乙烯丙烯共聚物（FEP）、聚四氟乙烯（PTFE）、聚（乙烯- 四氟乙烯）（PETFE）、或全氟烷氧基（PFA））、聚縮醛（例如：聚氧乙烯及聚甲醛）、聚（C1-6 烷基）丙烯酸酯、聚丙烯醯胺（包括未經取代及單-N-或二-N-（C1-8 烷基）丙烯醯胺）、聚丙烯腈、聚醯胺（例如：脂族聚醯胺、聚鄰苯二甲醯胺、或聚芳醯胺）、聚醯胺醯亞胺、聚酸酐、聚芳醚（例如：聚苯醚）、聚芳醚酮（例如：聚醚醚酮（PEEK）及聚醚酮酮（PEKK））、聚芳酮、聚芳硫醚（例如：聚苯硫醚（PPS））、聚芳碸（聚醚碸（PES）、聚苯碸（PPS）、及其類似物）、聚苯並噻唑、聚苯並噁唑、聚苯並咪唑、聚碳酸酯（包括均聚碳酸酯、或者如聚碳酸酯–矽氧烷、聚碳酸酯–酯、或聚碳酸酯–酯–矽氧烷的聚碳酸酯共聚物）、聚酯（例如：聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、聚芳香酯、或如聚酯醚的聚酯共聚物）、聚醚醯亞胺（例如：如聚醚醯亞胺–矽氧烷共聚物的共聚物）、聚醯亞胺（例如：如聚醯亞胺–矽氧烷共聚物的共聚物）、聚甲基丙烯酸（C1-6 烷基）酯、聚烷基丙烯醯胺（例如：未經取代、及單-N-或二-N-（C1-8 烷基）丙烯醯胺）、聚烯烴（例如：如高密度聚乙烯（HDPE）、低密度聚乙烯（LDPE）、及線性低密度聚乙烯（LLDPE）之聚乙烯、聚丙烯、及其鹵代衍生物（例如聚四氟乙烯）、及其共聚物（例如乙烯-α-烯烴共聚物））、聚噁二唑、聚甲醛、聚鄰苯二甲內酯、聚矽氮烷、聚矽氧烷（聚矽氧）、聚苯乙烯（例如：如丙烯腈–丁二烯–苯乙烯（ABS）或甲基丙烯酸甲酯–丁二烯–苯乙烯（MBS）之共聚物）、多硫化物、聚磺醯胺、聚磺酸酯（polysulfonate）、聚碸、聚硫酯、聚三嗪、聚尿素、聚胺甲酸酯、乙烯基聚合物（例如：聚乙烯醇、聚乙烯酯、聚乙烯醚、聚乙烯鹵化物（例如聚氯乙烯）、聚乙烯酮、聚乙烯腈、或聚乙烯硫醚）、石蠟、或其類似物。可使用包含前述熱塑性聚合物之至少一者的組合。
熱固性聚合物係衍生自能夠隨聚合反應或固化而不可逆地硬化且變得不可溶的熱固性單體或預聚物（樹脂），其中該聚合反應或固化係透過熱或暴露於輻射（例如紫外光、可見光、紅外光、或電子束（e–束）輻射）而誘導。熱固性聚合物包括醇酸、雙馬來亞醯胺聚合物、雙馬來亞醯胺三嗪聚合物、氰酸酯聚合物、苯並環丁烯聚合物、苯並噁嗪（benzoxazine）聚合物、鄰苯二甲酸二烯丙酯（diallyl phthalate）聚合物、環氧樹脂、羥甲基呋喃聚合物、三聚氰胺–甲醛聚合物、酚類（包括酚–甲醛聚合物，例如酚醛樹脂及可溶酚醛樹脂）、苯並噁嗪、如聚丁二烯（包括均聚物及其共聚物，例如：聚（丁二烯–異戊二烯））的聚二烯、聚異氰酸酯、聚尿素、聚胺甲酸酯、三聚氰酸三烯丙酯聚合物、三聚異氰酸三烯丙酯（triallyl isocyanurate）聚合物、某些聚矽氧烷、及可聚合之預聚物（例如：如不飽和聚酯、聚醯亞胺之具有烯鍵不飽和的預聚物）、或其類似物。該預聚物可例如與反應性單體進行聚合、共聚合、或鍵結，其中該反應性單體例如為苯乙烯、α-甲基苯乙烯、乙烯基甲苯（vinyltoluene）、氯苯乙烯、丙烯酸、（甲基）丙烯酸、丙烯酸（C1-6 烷基）酯、甲基丙烯酸（C1-6 烷基）酯、丙烯腈、乙酸乙烯酯、乙酸烯丙酯、三聚氰酸三烯丙酯、三聚異氰酸三烯丙酯、或丙烯醯胺。
形成複合物的方法並無限制且可包含射出成型、反應射出成型、層壓、擠出、壓縮成型、壓延、鑄造、及其類似者。該複合物可沒有空隙。
製品可包含該Ru-Co2 Z鐵氧體。製品可為天線或感應器核心。該製品可用於頻率0.1至4吉赫範圍、或於0.5至2吉赫範圍。製品可用於可在超高頻範圍內操作之多種裝置，例如高頻或微波的天線、過濾器、感應器、循環器、或移相器。製品可在大於或等於0.1 GHz之頻率下、或者在大於或等於0.3 GHz之頻率下操作。製品可用於商業及軍事應用、天氣雷達、科學通訊、無線通訊、自動駕駛車輛、飛機通訊、太空通訊、衛星通訊、或監控。
如本文中所揭露，鐵氧體組合物可包含具有下式之Ru-Co2 Z鐵氧體：(Ba3-x Mx )Co2 (M'Ru)y Fe24-2y-z O41 ，其中M係Sr、Pb、或Ca之至少一者；M'係Co、Zn、Mg、或Cu之至少一者；x係1至3；y係大於0至2、或0.001至2；以及z係-4至4。M'可至少為Co。Ru與M'的比值可為0.01至3。基於該鐵氧體組合物之總重量計，該鐵氧體組合物可進一步包含0.2至5.0重量%的Bi2 O3 。該鐵氧體組合物可於固態陶瓷形式下在1至2吉赫之頻率下具有大於或等於3.5的磁導率。該鐵氧體組合物可於固態陶瓷形式下在1至2吉赫之頻率下具有6至15的介電係數。該鐵氧體組合物於固態陶瓷形式下在1至2吉赫之頻率下具有小於或等於0.12、或0.08的磁損耗正切（tanδµ ）。該鐵氧體組合物於固態陶瓷形式下在1至2吉赫之頻率下具有小於或等於0.01、或者小於或等於0.008的介電損耗正切（tanδɛ ）。複合物可包含該鐵氧體組合物及聚合物。製品可包含該鐵氧體組合物或該複合物。該製品可為天線、過濾器、感應器、循環器、或移相器。該製品可為微波天線。該天線可在大於或等於0.1吉赫、或者大於或等於0.3吉赫、或者0.1至4吉赫之頻率下操作。
製造該鐵氧體組合物的方法可包含：混合包含Fe、Ba、Co、及Ru之鐵氧體的前驅化合物；以及，將該鐵氧體的前驅化合物於氧氣氣氛中進行燒結，以形成Ru-Co2 Z鐵氧體。該鐵氧體前驅化合物可包含BaCO3 、MCO3 、Co3 O4 、RuO2 、及Fe2 O3, ，其中M係Sr、Pb、或Ca之至少一者。該鐵氧體的前驅化合物可包含5至20重量%之BaCO3 、5至20重量%之MCO3 、2至15重量%之Co3 O4 、0.1至10重量%之RuO2 、及50至80重量%之Fe2 O3 ；皆係基於該混合物的總重量計。該燒結可在1,000至1,300°C、或1,200至1,250°C之溫度下進行1至20小時、或5至12小時之燒結時間。該方法可在燒結之前，進一步包含於空氣中對該鐵氧體的前驅化合物進行鍛燒。該方法可在燒結之前，進一步包含將該鐵氧體的前驅化合物與黏結劑混合。該方法可在燒結之前，進一步包含形成該鐵氧體的前驅化合物。
以下實施例係提供以說明本發明。該實施例僅作為說明，並非欲將根據本發明製造之裝置限制於本文所列之材料、條件、或製程參數。實施例
在此實施例中，所獲鐵氧體樣品的磁導率係於同軸空氣線中使用Nicholson-Ross-Weir（NRW）法透過向量網路分析儀（VNA）在0.1至10 GHz之頻率下進行測量。實施例 1-8 ： Ru-Co2 Z 鐵氧體樣品 的製備
Ru-Co2 Z鐵氧體樣品係於通式(Ba1.5 Sr1.5 )Co2 (CoRu)y Fe22.4-2y O41 中透過不同含量之釕、y，來形成如表1所示之鐵氧體組合物。該Ru-Co2 Z鐵氧體係於濕式行星式研磨機（wet planetary mill）中透過混合適量的BaCO3 、SrCO3 、Co3 O4 、Fe2 O3 、及RuO2 以形成混合物而製備。將該混合物於空氣中以1,200°C之鍛燒溫度進行鍛燒，歷時4小時之持溫時間，以形成鐵氧體。該鐵氧體係經粉碎並透過40網目之篩網進行過篩。將該粗顆粒於濕式行星式研磨機中進行研磨，以形成具有0.5至10微米之體積中位數D50顆粒尺寸的顆粒。粒狀混合物係透過將該顆粒與0.5至5重量%之聚乙烯醇（基於該粒狀混合物之總量計）混合而形成。然後，將該粒狀混合物在每平方公分1公噸之壓力下進行壓縮，以形成具有7毫米之外徑、3毫米之內徑、及3至3.5毫米之厚度的環狀顆粒（toroid granule）。將環狀顆粒於氧氣氣氛中在1,200°C、1,220°C、或1,240°C之燒結溫度下進行燒結10小時，其係透過在每分鐘0.5公升之速率下流入氧氣、且使用每分鐘3°C之升溫速率及每分鐘-3°C之冷卻速率進行。
表1
y 式
0 Ba1.5 Sr1.5 Co2 Fe22.4 O41
0.1 Ba1.5 Sr1.5 Co2.1 Ru0.1 Fe22.2 O41
0.2 Ba1.5 Sr1.5 Co2.2 Ru0.2 Fe22 O41
0.3 Ba1.5 Sr1.5 Co2.3 Ru0.3 Fe21.8 O41
在表2及3所示之燒結溫度及y值下製備各式鐵氧體組合物。該磁導率（實線）及磁損耗正切（虛線）係以頻率的函數示於圖1、圖2、及圖3，並且不同組合物的特定數值係顯示於表2。需注意在圖3中，具有星號之樣品為重複樣品。數個樣品之介電係數（實線）及介電損耗正切（虛線）係以頻率的函數示於圖4，並且不同組合物的特定數值係顯示於表3。
表2
鐵氧體樣品 1 2 3 4 5 6 7 8
y 0 0.1 0.1 0.2 0.2 0.3 0.3 0.3
燒結溫度（°C） 1,200 1,200 1,220 1,200 1,220 1,200 1,220 1,240
於1 GHz下的μ' 15.6 6.7 7.7 4.6 5.4 3.5 4.1 4.8
於1.6 GHz下的μ' 7.2 7.4 8.6 4.9 5.8 3.6 4.3 4.9
於2 GHz下的μ' 3.4 7.7 9.3 5.1 6.1 3.6 4.4 5.1
於3 GHz下的μ' - - 6.0 - 7.1 - 4.8 5.8
於1 GHz下的tanδµ 0.380 0.099 0.094 0.068 0.065 0.066 0.067 0.061
於1.6 GHz下的tanδµ 0.240 0.210 0.201 0.121 0.102 0.132 0.102 0.087
於2 GHz下的tanδµ 3.171 0.352 0.355 0.187 0.141 0.189 0.134 0.112
於3 GHz下的tanδµ - - 1.370 - 0.415 - 0.291 0.242
該結果顯示提升釕含量造成磁損耗正切的顯著下降，同時仍在1至2吉赫下維持大於或等於3之磁導率（μ'）。該結果亦顯示僅透過提升燒結溫度，該磁導率可被提升且同時進一步降低磁損耗正切。
表3
鐵氧體樣品 4 6 8
y 0.2 0.3 0.3
燒結溫度（°C） 1,200 1,200 1,240
於1 GHz下的ε' 10.8 10.5 13.8
於1.6 GHz下的ε' 10.8 10.5 13.8
於2 GHz下的ε' 10.8 10.5 13.9
於3 GHz下的ε' 10.9 10.6 13.9
於1 GHz下的tanδɛ 0.005 0.004 0.009
於1.6 GHz下的tanδɛ 0.006 0.006 0.008
於2 GHz下的tanδɛ 0.005 0.006 0.008
於3 GHz下的tanδɛ 0.008 0.008 0.010
表3及圖4顯示提升燒結溫度可造成介電係數的提升且同時維持低介電損耗正切數值。實施粒 9-10 ：使用 1- 步驟燒結加工之 Ru-Co2 Z 鐵氧體樣品 的製備
Ru-Co2 Z鐵氧體樣品係於通式(Ba1.5 Sr1.5 )Co2 (CoRu)y Fe22.4-2y O41 中透過不同含量之釕、y，來形成如表1所示之鐵氧體組合物。該Ru-Co2 Z鐵氧體係於濕式行星式研磨機中透過混合適量的BaCO3 、SrCO3 、Co3 O4 、RuO2 及Fe2 O3 以形成混合物而製備。該混合物係透過將該顆粒與0.5至5重量%之聚乙烯醇（基於該混合物之總量計）混合而形成。然後，將該混合物在每平方公分1公噸之壓力下進行壓縮，以形成具有7毫米之外徑、3毫米之內徑、及3至3.5毫米之厚度的環狀顆粒。將該環狀顆粒於氧氣氣氛中在1,220°C、或1,240°C之燒結溫度下進行燒結10小時，其係透過在每分鐘0.5公升之速率下流入氧氣、且使用每分鐘3°C之升溫速率及每分鐘-3°C之冷卻速率進行。
在表4及5所示之燒結溫度及y值下製備各式鐵氧體組合物。該磁導率（實線）及磁損耗正切（虛線）係以頻率的函數示於圖5，並且不同組合物的特定數值係顯示於表4。數個樣品之介電係數（實線）及介電損耗正切（虛線）係以頻率的函數示於圖6，並且不同組合物的特定數值係顯示於表5。
表4
鐵氧體樣品 9 10
y 0.2 0.3
燒結溫度（°C） 1,200 1,240
於1 GHz下的μ' 4.6 4.2
於1.6 GHz下的μ' 4.9 4.3
於2 GHz下的μ' 5.2 4.5
於3 GHz下的μ' 5.7 5.0
於1 GHz下的tanδµ 0.061 0.057
於1.6 GHz下的tanδµ 0.096 0.079
於2 GHz下的tanδµ 0.135 0.101
於3 GHz下的tanδµ 0.404 0.215
表5
鐵氧體樣品 9 10
y 0.2 0.3
燒結溫度（°C） 1,200 1,240
於1 GHz下的ε' 4.6 4.2
於1.6 GHz下的ε' 4.9 4.3
於2 GHz下的ε' 5.2 4.5
於3 GHz下的ε' 5.7 5.0
於1 GHz下的tanδɛ 0.061 0.057
於1.6 GHz下的tanδɛ 0.096 0.079
於2 GHz下的tanδɛ 0.135 0.101
於3 GHz下的tanδɛ 0.404 0.215
該結果顯示使用1-步驟燒結加工維持了良好的磁導率及磁損耗正切數值。實施例 11-14 ：包含鐵氧體組合物之複合物的製備
Ru-Co2 Z鐵氧體樣品係於通式(Ba1.5 Sr1.5 )Co2 (CoRu)y Fe22.4-2y O41 中透過不同含量之釕、y，來形成如表1所示之鐵氧體組合物。該Ru-Co2 Z鐵氧體係於濕式行星式研磨機中透過混合適量的BaCO3 、SrCO3 、Co3 O4 、Fe2 O3 、及RuO2 以形成混合物而製備。將該混合物於空氣中以1,200°C之鍛燒溫度進行鍛燒，歷時4小時之持溫時間，以形成鐵氧體。該鐵氧體係經粉碎並透過100網目之篩網進行過篩。對該粗顆粒進行以下步驟：於空氣中在1,240°C下進行燒結10小時；於濕式行星式研磨機中研磨以形成顆粒；以及，於每分鐘0.4公升之速率的氧氣流中在900°C下進行退火2小時，以形成鐵氧體粉末。該鐵氧體粉末具有3至6微米之中位數D50顆粒尺寸。將該鐵氧體粉末與石蠟混合，以形成包含40體積%之鐵氧體粉末與60體積%之石蠟的複合物。該複合物係成型為具有7毫米之外徑、3毫米之內徑、及2.5毫米之壁厚的環，並測量磁及介電性質。
磁性質係顯示於表6，以及介電性質係顯示於表7。
表6
實施例 11 12 13 14
y 0 0.1 0.2 0.3
於1 GHz下的μ' 1.62 1.59 1.50 1.39
於1.6 GHz下的μ' 1.62 1.59 1.49 1.40
於2 GHz下的μ' 1.63 1.59 1.49 1.40
於3 GHz下的μ' 1.64 1.63 1.51 1.40
於4 GHz下的μ' 1.61 1.64 1.52 1.42
於5 GHz下的μ' 1.51 1.58 1.50 1.43
於1 GHz下的tanδµ 0.037 0.044 0.027 0.002
於1.6 GHz下的tanδµ 0.055 0.051 0.037 0.023
於2 GHz下的tanδµ 0.068 0.056 0.043 0.027
於3 GHz下的tanδµ 0.129 0.097 0.069 0.046
於4 GHz下的tanδµ 0.227 0.179 0.123 0.077
於5 GHz下的tanδµ 0.305 0.267 0.187 0.119
表7
實施例 11 12 13 14
y 0 0.1 0.2 0.3
於1 GHz下的ε' 6.45 6.63 6.42 6.42
於1.6 GHz下的ε' 6.43 6.62 6.41 6.41
於2 GHz下的ε' 6.42 6.61 6.41 6.41
於3 GHz下的ε' 6.41 6.59 6.4 6.39
於4 GHz下的ε' 6.39 6.57 6.37 6.37
於5 GHz下的ε' 6.37 6.55 6.36 6.36
於1 GHz下的tanδɛ 0.013 0.013 0.009 0.009
於1.6 GHz下的tanδɛ 0.011 0.012 0.009 0.008
於2 GHz下的tanδɛ 0.012 0.013 0.01 0.009
於3 GHz下的tanδɛ 0.011 0.013 0.011 0.008
於4 GHz下的tanδɛ 0.012 0.013 0.109 0.008
於5 GHz下的tanδɛ 0.011 0.013 0.01 0.007
該結果顯示包含鐵氧體顆粒之複合物有良好的磁導率及磁損耗正切。
如下所列為本發明之非限制性的態樣。
態樣1：包含具有下式之Ru-Co2 Z鐵氧體的鐵氧體組合物：(Ba3-x Mx )Co2 (M'Ru)y Fe24-2y-z O41 ，其中，M係Sr、Pb、或Ca之至少一者；M'係Co、Zn、Mg、或Cu之至少一者；x係1至3；y係大於0至2；以及，z係-4至4。
態樣2：態樣1之鐵氧體組合物，其中y係0.001至2。
態樣3：前述態樣之任一或多個鐵氧體組合物，其中M'係至少為Co。
態樣4：前述態樣之任一或多個鐵氧體組合物，其中Ru與M'的比值係0.01至3。
態樣5：前述態樣之任一或多個鐵氧體組合物，基於該鐵氧體組合物之總重量計，係進一步包含0.2至5.0重量%的Bi2 O3 。
態樣6：前述態樣之任一或多個鐵氧體組合物，其中該鐵氧體組合物於固態陶瓷形式下在1至2吉赫之頻率下具有大於或等於3.5的磁導率。
態樣7：前述態樣之任一或多個鐵氧體組合物，其中該鐵氧體組合物於固態陶瓷形式下在1至2吉赫之頻率下具有6至15的介電係數。
態樣8：前述態樣之任一或多個鐵氧體組合物，其中該鐵氧體組合物於固態陶瓷形式下在1至2吉赫之頻率下具有小於或等於0.12、或者0.08的磁損耗正切（tanδµ ）。
態樣9：前述態樣之任一或多個鐵氧體組合物，其中該鐵氧體組合物於固態陶瓷形式下在1至2吉赫之頻率下具有小於或等於0.01、或者小於或等於0.008的介電損耗正切（tanδɛ ）。
態樣10：包含前述態樣之任一或多個鐵氧體組合物的製品。
態樣11：態樣10之製品，其中該製品係天線、過濾器、感應器、循環器、或移相器。
態樣12：態樣10至11之任一或多個製品，其中該製品係微波天線。
態樣13：態樣10至12之任一或多個製品，其中該製品係可在大於或等於0.1吉赫、或者大於或等於0.3吉赫、或者0.1至4吉赫之頻率下操作的天線。
態樣14：製造例如前述態樣之任一或多個鐵氧體組合物的方法，包含：混合包含Fe、Ba、Co、及Ru之鐵氧體的前驅化合物；以及，將該鐵氧體的前驅化合物於氧氣氣氛中進行燒結，以形成Ru-Co2 Z鐵氧體。
態樣15：態樣14之方法，其中該鐵氧體前驅化和物係包含BaCO3 、MCO3 、Co3 O4 、RuO2 、及Fe2 O3, ，其中M係Sr、Pb、或Ca之至少一者。
態樣16：態樣15之方法，其中該鐵氧體的前驅化合物包含5至20重量%之BaCO3 、5至20重量%之MCO3 、2至15重量%之Co3 O4 、0.1至10重量%之RuO2 、及50至80重量%之Fe2 O3 ；皆係基於該混合物的總重量計。
態樣17：態樣14至16之任一或多種方法，其中該燒結係在1,000至1,300°C、或1,200至1,250°C之燒結溫度下進行1至20小時、或5至12小時之燒結時間。
態樣18：態樣14至16之任一或多種方法，其係在燒結之前，進一步包含於空氣中對該鐵氧體的前驅化合物進行鍛燒。
態樣19：態樣14至18之任一或多種方法，其係在燒結之前，進一步包含將該鐵氧體的前驅化合物與黏結劑混合。
態樣20：態樣14至19之任一或多種方法，其係在燒結之前，進一步包含形成該鐵氧體的前驅化合物。
態樣21：包含前述態樣之任一或多個鐵氧體組合物的複合物。
本申請案係要求於2019年8月5日提出申請之第62/882,681號美國臨時專利申請案的權益。該相關申請案之全文併入本文供參考。
該組合物、方法、及製品可替代地包含任何本文中所揭露之適當的材料、步驟、或組分，或者由或實質上由任何本文中所揭露之適當的材料、步驟、或組分構成。該組合物、方法、及製品可額外地或替代地經配製為不含或實質上不含對於實現該組合物、方法、及製品之功能或目的而言非必需的任何材料（或種類）、步驟、或組分。
除非文中有明確指出，否則本所中所使用之「一」、「該」、以及「至少一」並不表示數量的限制且欲涵蓋單數及複數形式。舉例言之，除非文中有明確指出，否則「一元素（an element）」與「至少一元素（at least one element）」具有相同涵義。所謂「組合（combination）」包括摻合物（blend）、混合物、合金、反應產物、及類似物。以及，「至少一（at least one of）」係指包括所列舉之各個獨立元素與任二或多個元素的組合、以及所列舉之至少一個元素與未列舉之相似元素的組合。
除非文中有明確指出，否則所謂「或（or）」係指「及／或（and/or）」。整個說明書中對「一態樣」、「另一態樣」、「部分態樣」等的引用係指與該態樣連結所描述的特定元素（例如：特徵、結構、步驟、或性質）係包括在本文中描述的至少一態樣中，並且可存在或可不存在於其他態樣中。此外，應當理解所述元素可在各式態樣中以任何合適的方式進行組合。
除非本文中有相反說明，否則全部的測試標準皆為本申請案之申請日期起生效的最新標準、或者是出現於最早優先權申請案之申請日期的測試標準（若有要求優先權）。
所有針對相同組分或性質之範圍的端點係包括該端點、可獨立地組合、以及包括全部的中間點與範圍。舉例言之，「高達25體積%、或5至20體積%」係包括該端點、以及「5至25體積%」範圍的全部中間值，例如：10至23體積%等。
除非有額外定義，否則本文中使用之技術與科學術語係具有與本發明所屬領域技藝人士通常理解的相同涵義。
引用之專利、專利申請案、及其他參考文獻之全文係全部併入本文供參考。然而，若本申請案中的術語與併入之參考文獻中的術語有矛盾或衝突，則本申請案中的術語將優先於併入之參考文獻中所衝突的術語。
儘管已經描述了特定的實施態樣，但申請人或其他本領域技藝人士可能想到目前無法預見或可能無法預見的替代、修飾、變化、改良、及實質相等物。因此，所提交的及可能被修正的後附申請專利範圍欲包含全部這樣的替代、修飾、變化、改良、及實質相等物。
以下附圖係為闡述本發明而提供的例示性實施態樣。這些附圖為實施例的說明，並非欲將根據本發明製造之裝置限制於本文所列之材料、條件、或處理參數。
圖1為實施例1、2、4、及6之磁導率及磁損耗正切對頻率（f）的圖示說明；
圖2為實施例3、5、及7之磁導率及磁損耗正切對頻率（f）的圖示說明；
圖3為實施例4、6、及8之磁導率及磁損耗正切對頻率（f）的圖示說明；
圖4為實施例4、6、及8之介電係數及介電損耗正切對頻率（f）的圖示說明；
圖5為實施例9及10之之磁導率及磁損耗正切對頻率（f）的圖示說明；以及
圖6為實施例9及10之之介電係數及介電損耗正切對頻率（f）的圖示說明。

Claims (20)

  1. 一種鐵氧體組合物，包含具有下式之Ru-Co2Z鐵氧體：(Ba3-xMx)Co2(M'Ru)yFe24-2y-zO41其中M係Sr、Pb、或Ca之至少一者；M'係Co、Zn、Mg、或Cu之至少一者；x係1至3；y係大於0至2；以及，z係-4至4。
  2. 如請求項1之鐵氧體組合物，其中y係0.001至2。
  3. 如請求項1或2之鐵氧體組合物，其中M'係至少為Co。
  4. 如請求項1或2之鐵氧體組合物，基於該鐵氧體組合物之總重量計，該鐵氧體組合物進一步包含0.2至5.0重量%的Bi2O3。
  5. 如請求項1或2之鐵氧體組合物，其中該鐵氧體組合物於固態陶瓷形式下在1至2吉赫(gigahertz)之頻率下具有大於或等於3.5的磁導率(permeability)。
  6. 如請求項1或2之鐵氧體組合物，其中該鐵氧體組合物於固態陶瓷形式下在1至2吉赫之頻率下具有6至15的介電係數(permittivity)。
  7. 如請求項1或2之鐵氧體組合物，其中該鐵氧體組合物於固態陶瓷形式下在1至2吉赫之頻率下具有小於或等於0.12的磁損耗正切(magnetic loss tangent，tanδμ)。
  8. 如請求項1或2之鐵氧體組合物，其中該鐵氧體組合物於固態陶瓷形式下在1至2吉赫之頻率下具有小於或等於0.01的介電損耗正切(dielectric loss tangent，tanδε)。
  9. 一種具鐵氧體組合物之複合物，其包含如請求項1或2之鐵氧體組合物、以及聚合物。
  10. 一種具鐵氧體組合物之製品，其包含如請求項1或2之鐵氧體組合物。
  11. 如請求項10之製品，其中該製品係天線、過濾器、感應器、循環器、或移相器。
  12. 如請求項10之製品，其中該製品係微波天線。
  13. 如請求項10之製品，其中該製品係可在大於或等於0.1吉赫之頻率下操作的天線。
  14. 一種製造如請求項1或2之鐵氧體組合物的方法，包含：混合包含Fe、Ba、Co、Ru、M及M’之鐵氧體的前驅化合物(precursor compound)；以及將該鐵氧體的前驅化合物於氧氣氣氛中進行燒結，以形成Ru-Co2Z鐵氧體，其中，M係Sr、Pb、或Ca之至少一者；及M'係Co、Zn、Mg、或Cu之至少一者。
  15. 如請求項14之方法，其中該鐵氧體的前驅化合物係包含BaCO3、MCO3、Co3O4、RuO2、及Fe2O3,，其中M係Sr、Pb、或Ca之至少一者。
  16. 如請求項15之方法，其中該鐵氧體的前驅化合物包含5至20重量%之BaCO3、5至20重量%之MCO3、2至15重量%之Co3O4、0.1至10重量%之RuO2、及50至80重量%之Fe2O3；皆係基於該混合物的總重量計。
  17. 如請求項14之方法，其中該燒結係在1,000至1,300℃之溫度下進行1至20小時之燒結時間。
  18. 如請求項14之方法，在燒結之前，係進一步包含於空氣中對該鐵氧體的前驅化合物進行鍛燒。
  19. 如請求項14之方法，在燒結之前，係進一步包含將該鐵氧體的前驅化合物與黏結劑混合。
  20. 如請求項14之方法，在燒結之前，係進一步包含形成該鐵氧體的前驅化合物。
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