TWI704120B - 鐵氧體燒結體及使用其的電子部件 - Google Patents

鐵氧體燒結體及使用其的電子部件 Download PDF

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TWI704120B
TWI704120B TW107147661A TW107147661A TWI704120B TW I704120 B TWI704120 B TW I704120B TW 107147661 A TW107147661 A TW 107147661A TW 107147661 A TW107147661 A TW 107147661A TW I704120 B TWI704120 B TW I704120B
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sintered body
oxide
ferrite
ferrite sintered
component
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TW201932434A (zh
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芝山武志
高橋幸雄
鈴木孝志
田之上寬之
下保真志
加藤昌弘
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日商Ｔｄｋ股份有限公司
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Abstract

本發明提供一種可以在900℃左右下燒成且具有高導磁率及高居里溫度(Tc)的鐵氧體材料及使用其的電子部件。一種鐵氧體燒結體，其具有主成分與副成分，前述主成分由以Fe2 O3 換算為48.65~49.45莫耳%的氧化鐵、以CuO換算為2~16莫耳%的氧化銅、以ZnO換算為28.00~33.00莫耳%的氧化鋅、剩餘部分為氧化鎳而構成，作為前述副成分，相對於前述主成分100重量份，含有以B2 O3 換算為5~100ppm的氧化硼，且平均結晶粒徑為2~30μm。

Description

鐵氧體燒結體及使用其的電子部件
本發明關於一種適於層疊型電感器等的製造的鐵氧體燒結體與具有該燒結體的電子部件。
近年來，伴隨自動運轉技術及電動汽車的發展，汽車的電氣化急劇地發展。在汽車的電氣化中，電子部件在低頻帶區的噪音對策成為必須。並且，車載用電子部件被要求可耐受超過100℃的環境溫度。由於這樣的背景，而要求耐受超過100℃的環境溫度的層疊型噪音濾波器。
可以適用於這樣的噪音濾波器的鐵氧體材料，較佳為導磁率及居里溫度高。並且，能用於這樣的噪音濾波器的鐵氧體材料，被要求能在900℃左右的低溫下燒成。為了提高生產率及可靠性，將鐵氧體材料與內部電極同時燒成而製造能用於噪音濾波器的層疊型電子部件。此時，如果使用能在低溫下燒成的鐵氧體材料，則可以使用熔點比較低的材料作為內部電極。
專利文獻1中公開一種藉由將組成設為規定的範圍內而具有高導磁率、高居里溫度的鐵氧體材料。但是，專利文獻1中，藉由在1000~1200℃這樣的比較高的燒成溫度下使粒生長而實現高導磁率。因此，若將這樣的鐵氧體材料與熔點低的內部電極同時燒成，則有可靠性降低之虞。
專利文獻2中公開一種以含有玻璃為特徵的磁性鐵氧體材料。並且，公開燒成溫度為800~930℃。但是，專利文獻2的磁性鐵氧體材料含有源自玻璃的Na2 O。Na2 O抑制燒成時的粒生長。因此，在將專利文獻2的鐵氧體材料用於車載用噪音濾波器的情況下，有可靠性降低之虞。
專利文獻3中公開一種由Ni-Zn-Cu系鐵氧體粉末與Zn-B系玻璃粉末而構成的鐵氧體粉體。專利文獻3中公開這樣的鐵氧體粉體的低頻帶區下的導磁率，但近年來，要求更高的性能。 [先前技術文獻] [專利文獻]
專利文獻1：日本特開2004-338997號公報 專利文獻2：日本專利第3343813號 專利文獻3：日本專利第4753016號
[發明所要解決的技術問題]
本發明是鑒於這樣的實際情況而完成的，其目的在於，提供一種可以在900℃左右下燒成且具有高的導磁率及高的居里溫度(Tc)的鐵氧體材料及使用其的電子部件。 [用於解決問題的技術方案]
為了實現上述目的，本發明的鐵氧體燒結體的特徵在於：具有主成分與副成分；前述主成分由氧化鐵以Fe2 O3 換算為48.65~49.45莫耳%的氧化鐵、以CuO換算為2~16莫耳%的氧化銅、以ZnO換算為28.00~33.00莫耳%的氧化鋅、剩餘部分為氧化鎳而構成；作為前述副成分，相對於前述主成分100重量份，含有以B2 O3 換算為5~100ppm的氧化硼；且平均結晶粒徑為2~30μm。
上述鐵氧體燒結體，較佳為，作為前述副成分，相對於前述主成分100重量份，含有以SiO2 換算為5~500ppm的氧化矽。
上述鐵氧體燒結體，較佳為，作為前述副成分，相對於前述主成分100重量份，含有以ZrO2 換算為5~1100ppm的氧化鋯。
本發明的電子部件具有上述的鐵氧體燒結體。
此外，本發明的鐵氧體燒結體適合用於層疊型電感器、層疊型L-C濾波器、層疊型共模濾波器、由其它的層疊方法所致之複合電子部件等。例如在LC複合電子部件、NFC線圈、層疊型阻抗元件、層疊型變壓器中也適合使用本發明的鐵氧體燒結體。 [發明效果]
根據本發明，可以提供一種能夠在900℃左右下燒成且具有高導磁率及高居里溫度(Tc)的鐵氧體材料及使用其的電子部件。
以下，基於圖式所示的實施形態說明本發明。 首先，作為本發明的電子部件的一個實施形態，針對層疊型電感器進行說明。如圖1所示，本發明的一個實施形態的層疊型電感器1具有元件2與端子電極3。元件2是將經由鐵氧體層4而三維地且螺旋狀地形成有線圈導體5的坯料的層疊體進行燒成而得到。鐵氧體層4由本發明的一個實施形態的鐵氧體燒結體而構成。在元件2的兩端形成端子電極3，藉由經由引出電極5a、5b與端子電極3連接，而可得到層疊型電感器1。對元件2的形狀沒有特別限制，但通常為長方體狀。並且，對其尺寸也沒有特別限制，只要根據用途製成適當的尺寸即可。
作為線圈導體5及引出電極5a、5b的材質，沒有特別限定，可使用Ag、Cu、Au、Al、Pd、Pd/Ag合金等。此外，也可以添加Ti化合物、Zr化合物、Si化合物等。
本實施形態的鐵氧體燒結體為Ni-Cu-Zn系鐵氧體，作為主成分，含有氧化鐵、氧化銅、氧化鋅及氧化鎳。
主成分100莫耳%中，氧化鐵的含量以Fe2 O3 換算為48.65~49.45莫耳%，較佳為49.00~49.45莫耳%，更佳為49.10~49.30莫耳%，再佳為49.25~49.35莫耳%。藉由將氧化鐵的含量設為上述範圍，可得到具有高導磁率的鐵氧體燒結體。並且，氧化鐵的含量過多之情形，存在燒結性劣化、特別是低溫燒結時的燒結密度降低、同時電阻率降低的傾向。氧化鐵的含量過少之情形，有無法得到高導磁率之虞。
主成分100莫耳%中，氧化銅的含量以CuO換算為2~16莫耳%，較佳為4~14莫耳%，更佳為6~12莫耳%，再佳為8~10莫耳%。藉由將氧化銅的含量設為上述範圍，可得到能以900℃左右燒成的鐵氧體燒結體。若氧化銅的含量過少，則有燒結性降低，特別是低溫燒結時的燒結密度降低之虞。
主成分100莫耳%中，氧化鋅的含量以ZnO換算為28.00~33.00莫耳%，較佳為28.50~32.00莫耳%，更佳為29.00~31.00莫耳%，再佳為29.90~30.20莫耳%。藉由將氧化鋅的含量設為上述範圍，可得到具有高居里溫度(Tc)與高導磁率的鐵氧體燒結體。存在氧化鋅的含量越多，初導磁率越上升的傾向；初導磁率變得越高，越適於電感器。但是，若氧化鋅的含量過多，則存在居里溫度降低的傾向。
主成分的剩餘部分由氧化鎳構成。
本實施形態的鐵氧體燒結體，除上述的主成分之外，更含有氧化硼作為副成分，進一步亦可含有氧化矽及氧化鋯等化合物。
相對於主成分100重量份，氧化硼的含量以B2 O3 換算為5~100ppm，較佳為5~85ppm，更佳為5~60ppm，再佳為10~50ppm。藉由將氧化硼的含量設為上述範圍，可得到具有高導磁率的鐵氧體燒結體。若氧化硼的含量過多，則有在燒成時抑制粒生長而導磁率降低之虞。
相對於主成分100重量份，氧化矽的含量以SiO2 換算較佳為5~500ppm，更佳為5~350ppm，再佳為5~200ppm。藉由將氧化矽的含量設為上述範圍，可得到燒結性良好的鐵氧體燒結體。若矽化合物的含量過多，則有燒結性劣化，特別是低溫燒結時的燒結密度降低之虞。
相對於主成分100重量份，氧化鋯的含量以ZrO2 換算較佳為5~1100ppm，更佳為5~900ppm，再佳為5~700ppm。藉由將氧化鋯的含量設為上述範圍，可得到燒結性良好且具有高導磁率的鐵氧體燒結體。
在本實施形態的鐵氧體燒結體中，除了構成主成分的各成分的含量被控制在上述的範圍之外，還在規定範圍內含有氧化硼等化合物作為副成分。其結果，可以使燒結溫度降低，作為同時被燒成的內部導體，可以使用例如Ag等比較低熔點的金屬。進而，藉由低溫燒成所得到的鐵氧體燒結體，其初導磁率高，居里溫度Tc高。
並且，本實施形態的鐵氧體燒結體，也可以進一步在不阻礙本發明的效果的範圍內含有與上述副成分不同的Mn3 O4 等錳氧化物、氧化錫、氧化鎂、玻璃化合物等附加的成分。此等附加的成分的含量沒有特別限定，但例如為0.05~10重量%左右。
進而，在本實施形態的鐵氧體組合物中，可含有不可避免的雜質元素或其氧化物。
具體而言，作為不可避免的雜質元素，可列舉：C、S、Cl、As、Se、Br、Te、I、或Li、Na、Mg、Al、Ca、Ga、Ge、Sr、Cd、In、Sb、Ba、Pb等典型金屬元素、或Sc、Ti、V、Cr、Y、Nb、Mo、Pd、Ag、Hf、Ta等過渡金屬元素。並且，不可避免的雜質元素的氧化物可以在鐵氧體組合物中含有0.05重量%以下左右。
特別是若大量地含有Na，則有抑制燒結時的粒生長且導磁率降低之虞。因此，Na的含量較佳為以NaO換算為200ppm以下。
在本實施形態的鐵氧體燒結體中，結晶粒子的平均結晶粒徑為2~30μm，較佳為3~20μm，更佳為4~10μm。 此外，平均結晶粒徑是指由規定數的結晶粒子的結晶粒徑所算出的體積分布中的中位數粒徑(D50粒徑，50%粒徑)。具體而言，將根據需要而以化學蝕刻等適當地處理過的鐵氧體燒結體的切斷面，利用例如光學顯微鏡或SEM進行觀察，並由規定數的結晶粒子的結晶粒徑算出體積分布。此外，各結晶粒子的粒徑例如可以作為假定為相當於各結晶粒子的面積的圓之圓當量徑(Heywood徑)求出。並且，進行平均結晶粒徑的測定的粒子數目通常為100個以上。
本實施形態的鐵氧體燒結體的密度較佳為4.90~5.30g/cm3 ，更佳為5.00~5.30g/cm3 ，再佳為5.10~5.30g/cm3 。 此外，鐵氧體燒結體的密度係由將盤形的成型體在900℃下燒成所得到的燒結體的尺寸及重量而算出。
本實施形態的鐵氧體燒結體的居里溫度Tc較佳為100℃以上，更佳為125℃以上，再佳為150℃以上。 此外，居里溫度Tc基於JIS-C-2560-1、2進行測定。
本實施形態的鐵氧體燒結體的電阻率ρ較佳為106 Ω・m以上，更佳為107 Ω・m以上，較佳為108 Ω・m以上。 此外，電阻率ρ可以測定附有In-Ga電極的鐵氧體燒結體的直流電阻值而求出。電阻率ρ可以使用IR計進行測定。
本實施形態的鐵氧體燒結體的頻率100kHz中的導磁率μ’較佳為1000以上，更佳為1100以上，再佳為1200以上。 此外，就導磁率μ’而言，在環形鐵芯形狀的鐵氧體燒結體上將銅線電線捲繞10匝而進行測定。導磁率μ’可以使用LCR計進行測定。測定條件為頻率100kHz、溫度25℃。
接著，針對本實施形態的鐵氧體燒結體的製造方法的一例進行說明。首先，以成為規定的組成比之方式秤量起始材料(主成分的原料及副成分的原料)而進行混合，得到原料混合物。作為混合的方法，可列舉例如使用球磨機進行的濕式混合、或使用乾式混合器進行的乾式混合。此外，較佳使用平均粒徑為0.05~1.0μm的起始材料。
作為主成分的原料，可以使用氧化鐵(α-Fe2 O3 )、氧化銅(CuO)、氧化鋅(ZnO)、氧化鎳(NiO)、或複合氧化物等。進而，此外可以使用藉由燒成而成為上述的氧化物或複合氧化物的各種化合物等。作為藉由燒成而成為上述的氧化物的化合物，可列舉例如：金屬單體、碳酸鹽、草酸鹽、硝酸鹽、氫氧化物、鹵化物、有機金屬化合物等。
作為副成分的原料，可以使用含有氧化硼的軟化點低的玻璃。作為此種玻璃，可以使用B-Zn-Si系玻璃。在B-Zn-Si系玻璃中，除氧化硼之外，亦可含有氧化鋅、氧化矽、其它的微量成分。此種玻璃中所含的成分的一部分有時會在後述的鍛燒步驟及燒成步驟中消失。
接著，進行原料混合物的鍛燒，得到鍛燒材料。鍛燒是為了引起原料的熱分解、成分的均質化、鐵氧體的生成、由燒結所致之超微粉的消失與朝向適當的粒子尺寸的粒生長並且將原料混合物轉換為適於後步驟的形態而進行的。如此的鍛燒，較佳在500~900℃的溫度下、通常進行2~15小時左右。鍛燒通常在大氣(空氣)中進行，但也可以在與大氣中相比氧分壓更低的氣體環境下進行。此外，主成分的原料與副成分的原料的混合可以在鍛燒之前進行，也可以在鍛燒後進行。
接著，進行鍛燒材料的粉碎，得到粉碎材料。粉碎是為了將鍛燒材料的凝集破壞而製成具有適當的燒結性的粉體而進行。在鍛燒材料形成大的塊時，進行粗粉碎之後，使用球磨機或超微磨碎機等進行濕式粉碎。濕式粉碎進行直至粉碎材料的平均粒徑成為較佳0.1~1.0μm左右。
使用所得到的粉碎材料，製造本實施形態的層疊型電感器。針對製造該層疊型電感器的方法沒有限制，但以下針對片材法進行說明。
首先，將所得到的粉碎材料與溶劑或黏合劑等添加劑同時漿料化，製作膏體。然後，使用此膏體形成生胚片(green sheet)。接著，將所形成的生胚片加工成規定的形狀，經過脫黏合劑步驟、燒成步驟，可得到例如經由如圖1所示的鐵氧體層4而三維地且螺旋狀地形成有線圈導體5的層疊型電感器1。鐵氧體層4由本發明的一實施形態的鐵氧體燒結體構成。燒成在線圈導體5及引出電極5a、5b的熔點以下的溫度下進行。例如，線圈導體5及引出電極5a、5b為Ag(熔點962℃)的情況下，較佳為在850~920℃的溫度下進行。燒成時間通常進行1~5小時左右。並且，燒成可以在大氣(空氣)中進行，也可以在與大氣中相比氧分壓更低的氣體環境下進行。然後，在元件2的兩端形成端子電極3，藉由經由引出電極5a、5b而與端子電極3連接，從而可得到層疊型電感器1。
以上，針對本發明的實施形態進行了說明，但本發明並不受限於如此的實施形態，在不脫離本發明的要旨的範圍內當然能以各種的態樣實施。例如，作為圖2所示的LC複合電子部件10中的鐵氧體層4，亦可使用本發明的鐵氧體組合物。此外，圖2中，符號12所示的部分為電感部，符號14所示的部分為電容部。 [實施例]
以下，基於更詳細的實施例說明本發明，但本發明並不受限於此等實施例。
首先，作為主成分的原料，準備Fe2 O3 、NiO、CuO、ZnO。作為副成分的原料，準備B-Zn-Si系玻璃。
接著，將所準備的主成分作為燒結體以成為表1中記載的組成之方式進行秤量後，以球磨機進行濕式混合16小時而得到原料混合物。
接著，在將所得到的原料混合物進行乾燥後，在空氣中以500℃~ 900℃進行鍛燒而製成鍛燒粉。將鍛燒粉及副成分的原料粉末以鋼鐵製球磨機進行濕式粉碎72小時而得到粉碎粉。
接著，將此粉碎粉進行乾燥後，在粉碎粉100重量份中添加作為黏合劑的6wt%濃度的聚乙烯醇水溶液10.0重量份並進行造粒而製成顆粒。將此顆粒進行加壓成形，以成為成形密度3.20Mg/m3 之方式，得到環形(尺寸＝外徑13mm×內徑6mm×高度3mm)的成形體、及盤形(尺寸＝外徑12mm×高度2mm)的成形體。
接著，將此等各成形體在空氣中，在為Ag的熔點(962℃)以下的900℃，進行燒成2小時，得到作為燒結體的環形鐵芯樣品。進一步對樣品進行以下的特性評價。將試驗結果示於表1。此外，帶有底線的樣品No.為比較例。
平均結晶粒徑 將鐵氧體燒結體的切斷面根據需要以化學蝕刻等適當地進行處理，以光學顯微鏡或SEM進行觀察，由100個以上的結晶粒子的結晶粒徑算出體積分布。然後，將該體積分布中的中位數粒徑(D50粒徑，50%粒徑)設為平均結晶粒徑。此外，各結晶粒子的粒徑基於假定為相當於各結晶粒子的面積的圓之圓當量徑(Heywood徑)而求出。
成分的含量的測定 關於樣品中所含的成分的含量，針對Fe、Cu、Zn、Ni使用螢光X射線分析裝置(XRF)進行測定，針對B、Si、Zr，使用ICP發光光譜分析法(ICP-AES)或ICP質量分析計(ICP-MS)進行測定。此外，表1中記載的各成分的含量分別為換算成Fe2 O3 、CuO、ZnO、NiO、B2 O3 、SiO2 、ZrO2 的值。
密度 鐵氧體燒結體的密度係由將盤形的成型體以900℃進行燒成所得到的燒結體的尺寸及重量而算出。
導磁率μ’ 在環形鐵芯樣品上將銅線電線捲繞10匝，使用LCR計(Hewlett-Packard公司製4285A)測定導磁率μ’。作為測定條件，設定為測定頻率100kHz、測定溫度25℃。
電阻率ρ 在盤樣品的兩面塗敷In-Ga電極，測定直流電阻值，求出電阻率ρ(單位：Ω・m)。測定使用IR計(HEWLETT PACKARD公司製4329A)而進行。
居里溫度(Tc) 居里溫度Tc基於JIS-C-2560-1、2進行測定。
[表1]
Figure 02_image001
由表1可知：含有以Fe2 O3 換算為48.65~49.45莫耳%的氧化鐵、以CuO換算為2~16莫耳%的氧化銅、以ZnO換算為28.00~33.00莫耳%的氧化鋅、進一步含有以B2 O3 換算為5~100ppm的氧化硼的鐵氧體燒結體(樣品No.1~8、13~17、20~25)，在100kHz的導磁率良好。
另一方面，氧化鐵的含量在以Fe2 O3 換算為48.65~49.45莫耳%的範圍之外的情況(樣品No.9~12)下，在100kHz的導磁率降低。並且，氧化硼的含量以B2 O3 換算小於5ppm的情況(樣品No.18)下，在100kHz的導磁率降低，大於100ppm的情況(樣品No.19)下，電阻率ρ降低。
1‧‧‧層疊型電感器2‧‧‧元件3‧‧‧端子電極4‧‧‧層疊體5‧‧‧線圈導體5a、5b‧‧‧引出電極10‧‧‧LC複合電子部件12‧‧‧電感部14‧‧‧電容部
圖1為本發明的一實施形態的層疊型電感器的剖視圖。 圖2為本發明的一實施形態的LC複合電子部件的剖視圖。
1‧‧‧層疊型電感器
2‧‧‧元件
3‧‧‧端子電極
4‧‧‧層疊體
5‧‧‧線圈導體
5a、5b‧‧‧引出電極

Claims (3)

  1. 一種鐵氧體燒結體，其具有主成分與副成分，前述主成分由以Fe2O3換算為48.65~49.45莫耳%的氧化鐵、以CuO換算為2~16莫耳%的氧化銅、以ZnO換算為28.00~33.00莫耳%的氧化鋅、剩餘部分為氧化鎳而構成，作為前述副成分，相對於前述主成分100重量份，含有以B2O3換算為5~100ppm的氧化硼，相對於前述主成分100重量份，含有以SiO2換算為5~500ppm的氧化矽，所述鐵氧體燒結體的平均結晶粒徑為2~30μm。
  2. 如申請專利範圍第1項所述的鐵氧體燒結體，其中，作為前述副成分，相對於前述主成分100重量份，含有以ZrO2換算為5~1100ppm的氧化鋯。
  3. 一種電子部件，具有如申請專利範圍第1或2項所述的鐵氧體燒結體。
TW107147661A 2018-01-17 2018-12-28 鐵氧體燒結體及使用其的電子部件 TWI704120B (zh)

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