TWI291936B - - Google Patents

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Publication number
TWI291936B
TWI291936B TW091108705A TW91108705A TWI291936B TW I291936 B TWI291936 B TW I291936B TW 091108705 A TW091108705 A TW 091108705A TW 91108705 A TW91108705 A TW 91108705A TW I291936 B TWI291936 B TW I291936B
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Taiwan
Prior art keywords
powder
single crystal
ceramics
ceramic
ceramic powder
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TW091108705A
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English (en)
Inventor
Takaya Minoru
Akachi Yoshiaki
Kobuke Hisashi
uematsu Hiroyuki
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Tdk Corp
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C30B13/16—Heating of the molten zone
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/018—Dielectrics
    • H01G4/06—Solid dielectrics
    • H01G4/08—Inorganic dielectrics
    • H01G4/12—Ceramic dielectrics
    • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
    • H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
    • H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
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    • C01G23/003—Titanates
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    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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1291936 A7 — _ B7 ___ 五、發明説明（彳） [技術領域] 本發明有關一種單晶陶瓷粉末及其製造方法。 [背景技術] 以往’電介質粉末或磁性鐵酸鹽粉末等陶瓷粉末使用於 許多領域。例如，作為電介質粉末，鈦酸鋇、氧化鈦等之 介電性、壓電性及熱電性優異，而一直被用作瓷器電容 器、滤波器、感測器等的材料。 將陶瓷粉末作為瓷電容器用的材料使用時，希望其介電 常數高、損失小。此外，當作為磁性鐵酸鹽材料使用時， 希望其損失小、導磁率平緩地向高頻區域延伸。這些特性 依賴於陶瓷粉末的形狀、粒徑、純度、反應性等物性。例 如，如果陶瓷粉末為多結晶或不定形粉末時，容易引起局 部兴常顆粒成長，容易產生組成不均句，導致磁特性和電 氣特性劣化。因此，陶瓷粉末較好不含有結晶粒界或不純 物’為單相或單晶。此外，為了獲得更加優異的特性，陶 竞粉末較好為2種或以上的金屬與氧的化合物。 [發明欲解決之課題] 但疋’難以製造具有優異特性的陶瓷粉末。例如，在固 相反應法中，藉由在空氣或惰性氣體中對與對應於最終生 成物組成的金屬氧化物的混合粉末進行燒結，可製得2種 以上的金屬與氧的化合物的金屬氧化物電介質，但難以製 得單相的粉末。此外，在共沈澱法等液相法中，從金屬鹽 的水溶液或有機溶劑溶液中製造水合物等形式的金屬氧化 物的前驅物（1次粒子），將該前驅物在空氣或惰性氣體中 ___ -4- 本紙張尺度it用巾H g家標準(CNS) M規格(⑽χ 297公复) 1291936
進2燒結製得陶瓷粉末。但是，難於製得具有優異結晶性 的電介質粉末，而且由於金屬氧化物的前驅物具有很強的 結合，最終得到大塊物質，因此為了得到電介質粉末必須 對燒結後的電介質進行粉碎。如此得到的粉末中，每個粒 子的形狀為不定形，粒度分佈也宽，而且不純物混入的可 能性高。 因此’提出了改善粉末中粒子形狀及粒度分佈的水熱合 成法和氣相反應法等，但在生產性和成本方面，這些方法 均難於在工業上咼效製造。此外，特開平7_33579號公報 中揭不一種藉由對於將原料溶解於溶液中所形成的物質進 行水解或共沈澱的方法等，形成氧化物的微粉末，藉由使 微粉末進行熱處理而使其結晶並使粒子成長，進而將製得 的物質中含有的玻璃溶解去除，製得粒徑相同的單晶粉末 的方法。但疋，咸方法程序複雜，工業上量產困難。 此外，特開平9-263496號公報揭示一種將平均粒徑為1 〇 4政米或以下的鈥故鋇在12 0 〇。〇至16 18 °C下進行燒結，製得 單曰曰鈥故鋇的方法。在該方法中，在比鈥酸鋇溶點低的溫 度下’在燒結時產生溫度梯度，產生異常粒生長，從而形 成單晶鈦酸鋇。但是，在該方法中，製得的鈦酸鋇粒徑 大，為500微米左右，因此無法製得微粒子。此外，由於 單晶是在含於多晶體中的狀態下製得，因此為了取出單 晶，需要有將多晶體浸潰於濃鹽酸中以破壞多晶部分的程 序。 陶瓷;粉末’有時只將粉末作為單體使用，有時將其分散 -5-本紙張尺度適用中國國家標準(CNS) A4規格(210X297公釐) 1291936
1291936 A7 B7 五、發明説明（4 ) '' ---- 的溫度，具體而言是加熱到該粉體的、溶·點以上，在冷卻程 序中U吉晶化程序將在加熱處理程序中製得的生成物冷 卻’從而製得單晶陶瓷粉末。 採用該製造方& ’可製得球形度09心乂上的單晶陶资 粉末。 、在孩製造方法的加熱處理程序中，由於將由陶瓷成分組 成的粉體熔融形成熔融物後，在冷卻程序中使其結晶化， 因旎夠製造球形度高、結晶性優異的單晶陶瓷粉末。在 加熱處理程序中經過熔融處理後，經由隨後之冷卻程序進 行結晶化，可用少的能量製造單晶粉末。此時，加熱處理 私序較好在電氣管狀爐中進行。由於在電氣管狀爐中進 行’溫度及溫度輪廓的控制變得容易，因此在製造上較 佳0 由陶資:成分組成的粉體，如果是由5〇微米或以下的粒子 所形成，則可製造粒徑30微米或以下的單晶陶瓷粉末。 此外’由陶瓷成分組成的粉體，如果是由平均粒徑1微 米或以下的1次粒子所形成的顆粒，則可製造粒徑小的單 晶陶瓷粉末，因此較佳。 如果用其他觀點來詮釋本發明所涉及的單晶陶瓷粉末的 製造方法’可以捕捉到該製造方法的特徵，即，邊使由陶 竞成分組成的粉體浮游，邊使其在加熱爐中移動，藉由冷 卻製得的生成物，可製得球形度為〇·9或以上的單晶陶瓷 粉末。由於如此邊使由陶瓷成分組成的粉體浮游邊進行加 熱，因此可製造球形度高的單晶陶瓷粉末。 本紙張尺度適财國®家科(CNS)織格( χ 297公憂) 1291936 A7 ______B7 五、發明説明（5 ) 根據本發明所製得的單晶陶瓷粉末，為平均粒徑〇1至 3〇微米、且球形度為〇·9或以上的單晶陶瓷粉末。由於該 單晶陶瓷粉末粒徑小且球形度高，因此具有優異特性，特 別是對樹脂等的填充性高。 該單晶陶瓷粉末，由例如氧化物磁性材料或氧化物電介 質材料構成，成為顯示出優異的磁特性、電氣特性的物 質。 如果該單晶陶瓷粉末的平均粒徑為1至2〇微米，則成為 具有更為優異填充性的物質。 本發明為適用於由磁性體或電介質材料組成的單晶球狀 氧化物粉末與分散並保持有上述球狀氧化物粉末的結合材 料組成的複合材料。而且，在該複合材料中，其特徵在於 球狀氧化物粉末的平均粒徑為0.1至30微米，球形度為〇 9 或以上。精由使用球形度南的微細粉末，可提高其在與樹 脂材料的複合材料中的填充性，並且能夠有效發揮粉末所 具有的特性。 以上的複合材料中，可以用樹脂作為結合材料。此時， 較好球狀氧化物粉末含量在30至98重量％範圍内。 此外，以上的複合材料中，可以由電介質材料構成球狀 氧化物粉末。而且，在本發明中，可以由比構成球狀氧化 物粉末的電介質材料熔點低的電介質材料構成結合材料。 此時，較好球狀氧化物粉末含量在30至70體積％的範圍 内。 此外，在以上的複合材料中，可以由磁性體材料構成球 -8 - 本紙張尺度適用中國國家標準(CNS) Α4規格(210 X 297公釐） A7 B7
1291936 五、發明説明（6 狀氧化物粉末。而且，在本發明中，可、 化物粉末的磁性體材料熔點低的磁構成球狀氧 料。此時，較好球狀氧化物粉末本景 "^ ^ 圍内。 。里在30至7〇體積％的箣 本發明提供-種使用以上複合材料的電子零件。該 零件的特徵在於電介質層中配置有内部金屬電極"*· 介質層為由電介質材料組成的球狀氧化物粉末與分散並： 持有該球狀氧化物粉末的結合材料組成的複合材料所組 成，球狀氧化物粉末的平均粒徑為〇1至3〇微米，球形度 為0.9或以上。此外，本發明提供一種電子零件，其特二 在於’在磁性體層中配置有内部金屬電極，磁性體層為由 磁性材料組成的球狀氧化物粉末與分散並保持有該球狀氧 化物粉末的結合材料組成的複合材料组成，球狀氧化物粉 末的平均粒徑為0.1至30微米，球形度為〇 9或以上。 [圖式簡單說明] 圖1 :表示陶瓷粉末製造程序簡要實施例的說明圖。 圖2 :表示實施例1製造的陶瓷粉末的X射線繞射結果的 圖譜。 圖3 :表示實施例1製造的陶瓷粉末的SEM照片圖。 圖4 :表示實施例1製造的陶瓷粉末的電子射線繞射像的 照片。 圖5 ··表示比較例1製造的陶瓷粉末的SEM照片圖。 圖6 ··表示比較例1製造的陶瓷粉末的電子射線繞射像的 照片。 -9- ___ 本紙張尺度適用中國國家標準(CNS) A4規格(210X 297公釐）
裝 訂
% 1291936 A7 •_____B7 五、發明説明（7 ) —--- 圖7:表示實施例4製造的陶瓷粉末的SEM照片圖。 圖8 :1示實施例4製造的陶资粉末的磁特性曲線圖。 圖9:表示比較例2製造的陶瓷粉末的磁特性曲線圖。 圖表示用實施例4及比較例2製得的陶究粉末所形成 的基板導磁率的曲線圖。 圖11:表示本發明所適用的高頻模組的透視斜視圖。 圖12:表示本發明所適用的晶片線圈的透視斜視圖。
/13:表示實施例6製造的複合磁性材料的感應系數值L k:化率的曲線圖。
广4:表示比較例4製造的複合磁性材料的感應系數值L fe：化率的曲線圖。 [具體實施方式] 以下就本發明的實施形態進行說明。 杂、據圖1對本發明有關的單晶陶瓷粉末的製造程序簡要 實施例進行說明。如圖1所示，本發明的製造方法係由將 原料粉砰而製造1次粒子的1次粒子形成程序、由1次粒子 二：顆粒的顆粒形成程序、供給由顆粒組成的粉體的粉體 h%序、使供給的粉體加熱到所需溫度的加熱處理程 序、將加熱處理製得之生成物冷卻的冷卻程序以及後處理 程序所構成。 彤首先，在1次粒子形成程序中，由陶瓷成分組成的原料 形成1次粒子。在i次粒子形成程序中，將由陶瓷成分組成 =原料粉碎，較好調整平均粒徑達到丨微米或以下。該粒 /不僅決定最終製造的單晶陶瓷粉末的粒徑，而且藉由使
1291936 A7
用具有此粒徑的1次粒子，可 ^ 、、 于 了以使單晶陶瓷粉末的品質優 化。粉碎方法並無特別限定 4疋例如可以使用球磨機等。 本發明中所謂的陶咨忐八 , ^ . 刀 匕含被認為是陶瓷：的氧化 物、氮化物、碳化物等化人％ ^ 物。此外，不僅包含單-的陶 ΐ複：=:數陶究的混合物、複合氧化物、複合氮化物 不口 口 。陶瓷成分具體例為電介質材料、磁性材 料0 私介質材料可以包括，例如鈥酸鋇省系陶資、欽酸相^ 錫峨、錯,系陶資、二氧化職、鈦酸鋇系陶 瓷、鈦酸鉛系陶瓷、鈦酸鳃系陶冑、鈦酸鈣 峨究、欽酸…毫等，以及Caw04=^^ Ba(Mg、Nb)〇3系陶瓷、Ba(Mg、Ta)〇3系陶瓷、Ba(c〇、 Mg、Nb) 03系陶瓷、Ba( c〇、Mg、叫〇3系陶瓷等。這些 :質可以單獨或2種以上混合使用。又，二氧化鈦系陶 瓷，係指其在組成上只含有二氧化鈦的體系，或在二氧化 鈦=又含有其他少量添加物的體系，但保持作為主成分的 一氧化鈦的結晶構造。對於其他體系的陶瓷亦如此。此 外，一氧化鈦為以Ti〇2表示的物質，且具有各種結晶構 造，但作為電介質陶瓷使用的為具有金紅石構造的物質。 至於磁性材料，可使用具有磁性的氧化物。例如可使用 Μη Zn系鐵酸鹽、Ni-Zn系鐵酸鹽、Mn-Mg-Zn系鐵酸鹽、
Ni-Cu-Zn系鐵酸鹽等。此外，也可以使用、以〕&等 氧化鐵。 這些陶瓷成分亦可使用市售陶瓷，此外，可以藉燒結用 尽紙浪尺⑽料a B家標準(CNS^^(摩297公爱) 1291936 五、發明説明（v 於形成陶瓷成分的組合物、材料來製造陶瓷成分。例如， 1氧化鋇和鈦酸混合，製得顆粒狀的複合氧化物，將該複 合氧化物粉碎成適當大小的物質，然後進行燒結反應，由 此製得欽酸鋇等的陶瓷成分。 隨後，在顆粒形成程序中，使上述製造的丨次粒子形成 =粒。具體而言，製造用於使丨次粒子藉噴嘴進行噴霧的 水液。漿液可藉由將丨次粒子適量添加到溶劑後，用球磨 機等混合機進行混合而製造。溶劑可以使用水或乙醇，為 了提高1次粒子的分散性，推薦添加分散劑。分散劑的添 加量為，例如1次粒子重量的1%左右。亦可添加使i次粒 子間機械結合的結合劑，例如PVA(聚乙烯醇）。製得的裝 液藉由噴嘴進行噴霧，而形成液滴。 本文，噴嘴是指用於對上述漿液和壓縮氣體進行噴霧的 裝置，可以使用2流體噴嘴或4流體噴嘴等。與壓縮氣體 (例如2氣、氮氣等）一起從喷嘴噴出的漿液被顆粒化並形 成噴務。噴霧中液滴的粒徑可藉由漿液與壓縮氣體的比率 加以控制。藉控制液滴粒徑，可以控制最終製得的單晶陶 瓷粉末粒徑。藉由噴嘴進行的噴霧程序在所定的腔室内進 仃。適罝使用在加熱下兼有乾燥的噴霧乾燥法製造顆粒。 使用噴霧乾燥法，由於幾乎沒有如粉碎粉末般巨大的粉末 混入，因此可以確保最終製得的製品品質可靠性。 如此，藉由使用噴嘴，可以製造適於本發明中使用的粒 徑小顆粒粉，例如，可以製造丨至2〇微米左右的微細顆粒 粉。該粒徑決定最終製得的單晶陶瓷粉末的粒徑。如上所 12- 本紙張尺度適财S ®家標準(CNS)A4規格(210X297公釐） 1291936 五、發明説明（ 述，粒徑可以藉由控制漿液與壓縮氣體的比 t制ί由使漿液間發生碰撞’也可製得小液滴。於θ ’ :匕 此製侍的顆粒被輸送到粉體供給程序。 、疋如 在粉體供給程序中，將顆粒形成程序中 、 =陶瓷成分組成的粉體與載氣一起供給到加熱區:或粒：為 貫施f體供給程序的具體構成，圖1記載由不同的 備載氣和顆粒，通過噴嘴N，將供=仫午 ，理程:的形態。載氣可以使用各種氣 孔ΑγΛ及Ne氣等。對於需要加熱到i3〇〇c>c以 ：： J慮到加熱處理程序中產生Ν〇χ，因此較好使二科Ne 程岸中，將由陶資成分組成的粉體供給到加 …處里•王序的万法不限於圖！所記載的方式。例如 成分組成的粉體吹送含有載氣的壓縮氣體， ^將八供給到加熱處理程序的方法。此外，也可以 分散機供給’利用分級機和粉碎機輸出供給，亦即由於八 級或粉碎，將從輸出侧製造的粉末供給到加熱處理程序;7 、在本發明實施形態中，由陶變成分組成的粉體的噴霧可 以j乾燥狀怨，也可以為含有水分等的濕潤狀態。 a Ik後在加熱處理程序中，將從粉體供給程序用噴嘴供 之由陶瓷成分組成的粉體在加熱區域進行燒結處理， 而製得單晶的陶瓷粉末。 加扁處理程序在加熱爐中進行。至於加熱方式，可以採 用私加A、利用氣體的燃燒熱進行加熱及高頻加熱等已知 本紙張尺奴财® ® -13· 1291936 A7 __ B7 五、發明説明（u ) 方式。尤其，與燃燒氣體的方法相比，使用電氣管狀爐易 於對爐内氛圍氣進行控制。由陶瓷成分組成的粉體在爐内 與形成氣流的載氣一同浮游於加熱爐内，在此狀態下進行 單晶化及球狀化。由陶瓷成分組成的粉體的流速根據收集 效率、熱分解溫度進行適當決定，大致在〇〇5至1〇 111/8的 範圍内，特佳1至5 m/s。粉末流速可藉由控制載氣流速進 饤改變。此時，較好控制使陶瓷成分組成的粉體在加熱爐 内的滯留時間為1至10秒。但是，較好至少要比陶瓷粉末 不成為非晶質的臨界冷卻速度慢。臨界冷卻速度依物質不 同而兴，例如，當為鈦酸鋇時，臨界冷卻速度為1. h 1Μ (k/sec)。如果比孩速度快，製得的陶瓷粉末為玻璃（非晶 貝）。單晶化所需的時間依賴於粒徑，粒徑越小則該時間 越短。 加熱條件，特別是溫度及時間係根據陶瓷組成進行適當 決足。至於加熱條件，加熱爐内的氛圍氣可以根據例如電 介質材料、磁性材料等、作為目的最終生成物的單晶陶瓷 粉末的種類，選擇氧化性氛圍氣、還原性氛圍氣或非活性 乳圍氣加以選擇。可以根據所選擇的氛圍氣選擇載氣， 將必要的氣體供給到加熱爐内。 $ 扣至於加熱溫度，可以設定為由陶瓷成分組成的粉體進广 早晶化的溫度。具體而言，設定為由陶瓷成分組成的粉： 的‘點以上。藉加熱到熔點以上，陶瓷成分的粉體熔融 從而得到單晶。料，陶資成分的粉末一旦溶㉟，由於表 面張力的原因，製得的陶瓷粉末形狀更接近真球。
本紙張尺度適财國國家料(CNS) 1291936 A7 B7
五、發明説明（13 〇·9Μ，更好0.95M。球形度如果為〇9或以上，當將级 晶陶瓷粉末分散於樹脂材料中以複合材料使用肖，單心 资粉末易於均㈣分散於樹脂材料中，進而在燒結時^ 產生由於不均勾性而引起的龜裂。 據此，根據本實施形態製得的單晶陶瓷粉末不含有結晶 粒界以及不純物，為單相且為單晶。因此，該單晶陶 末，作為電介質材料、磁性材料時，可使磁性或介電特^ 提高，顯示出優異的特性。 此外，用根據本實施形態中記載的方法形成的單晶陶瓷 粉末，由於沒有使用以往方法中所使用的酸以及有機溶 封J因此不產生有害的氣體等，而且，可用較便宜的設備 製造。在本實施形態中，粉體供給程序中所供給的由陶瓷 成分組成的粉體，包含粉末、顆粒粉、粉碎粉等、由不局 限於遠形悲的粒子構成的各種形態。因此，在粉體供給^ 序中供給的粉體不限於上述實施形態般的顆粒，亦可為例 如使陶资成分粉碎的粉體。此時，由於使用具有較大粒徑 的粉體，因此可以形成較大的單晶陶瓷粉末。具體而言， 如果使用50微米或以下的粒子，則可以形成3〇 μ^或以下 的單晶陶瓷粉末。 進而，在本實施形態中，可以製造粒徑小且為球狀的單 晶陶瓷粉末。此單晶陶瓷粉末，其凝集性低，分散性和填 充性優異。因此，可以將製得的單晶陶瓷粉末與分散並保 持有該單晶陶备粉末的結合材料混合，形成複合材料。 結合材料可以使用樹脂。此時，複合材料中單晶陶究粉 -16- 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公嫠)
訂
線 14 1291936 五、發明説明（ 末的含量較好在30至98重量％的範 二：熱塑性樹脂、熱固性樹脂兩•，且二:該樹脂可 用的樹脂包括含有環氧樹脂、酚酸樹二而…以使 聚醯亞胺樹脂、聚酷樹脂、聚苯：：„系樹脂、 氰酸酯系樹脂、鄰苯二甲酸二 /二水讯胺樹脂、 化合物樹脂、液晶聚合物、氟系樹月:，脂、聚苯乙埽魅 脂、聚乙埽醇樹γ ^桌乙烯醇縮丁醛樹 丙旨中至少一種以上的樹脂等。㈣、准素树脂、 當早晶陶瓷粉末由電介質材料構 可以使用比上述電介質材料且右否M f為、，。口材科， -方面使在更低的心低溶點的電介質材料。 裝 能，另、：製造複合電介質材料成為可 ^ 万面’藉由在此低溫燒結，可獲得原本在高 材:f才能得到的特性。構成複合材料的低炫點電介質 ^ ’較好使用比單晶陶资粉末具有更小粒徑的粉末供达 二原因在於，藉由在單晶陶資粉末的間隙填 的粉末，可使單晶陶瓷粉末均勻地分散。 以上的觀點也適用於單晶陶资粉末由磁性材料構成 合。亦即，可製得在相對低溶點的磁性材料中分散並保持 有由相對高㈣的磁性材料構成的單晶㈣粉末而 複合磁性材料。 、 本發明中，可使以上複合材料適用於各種電子零件。其 中1個實施例示於圖11及圖12。圖1丨為表示作為電子零件 的1個實施例的高頻模組的斜視圖。該高頻模組在複合電 介質層4的表面上裝有二極體6、晶體三極管7及晶片電阻 17- 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐） 15 1291936 五、發明説明（ 8。此外，高頻模組在複合電介質層5的裏面及内部配置有 ，，電極〗。進而，高頻模組在其内部配置有通孔導體〕、 電客器形成電極3。而且以上說明的複合電介質材料適用 於該複合電介質層4。此外，圖12為表示作為電子零件的1 個實施例的晶片線圈的斜視圖。該晶片線圈在複合磁性體 層丨4的内部配置有線圈形成導體n和通孔導體12。並且^ 晶片線圈在複合磁性體層14的側面形成有外部端子電= 11。而且上述複合磁性材料適用於該複合磁性體層。以 上為電子零件的部分例示，本發明的複合磁性材^還適用 於基板等其他電子零件。 [實施例] 以下結合具體實施例對本發明進行說明。 (實施例1) 漿 比 在以1:1的莫耳比稱量的氧化鋇（Ba〇)粉末及氧化鈦 (Τι〇2)粉末中添加水，用球磨機混合12小時，由此製得 液（以下稱第1漿液）。混合前，按相對於粉末重量1%白$ 例添加分散劑（東亞合成社製a_30SL)。 噴 的 七第1漿液經噴霧乾燥機乾燥，進行顆粒化。此時的 霧、乾燥條件並無特別限定，最好設定的條件使顆粒粉 粒徑達到200微米或以下。 作 並 製 所得的顆粒粉在l25(rc的溫度燒結丨小時，從而製得 為複合氧化物燒結體的鈦酸鋇。在該燒結體中添加水， 作 按相對於燒結體重量1%的比例添加分散劑（東亞合成社 A-30SL)後，用球磨機進行48小時粉碎，從而製成含有 1291936 A7 ______B7 五、發明説明（16 ) ~~" 為1次粒子的平均粒徑0.3微米的粉末漿液（第2漿液）。相 對於粉末總重，於該第2漿液中添加2重量％的稀釋為1〇重 量％濃度的PVA(聚乙缔醇），進而進行調整以使第2裝液 中的粉末含量達到40重量％。 對第2聚液使用喷霧乾燥法製成顆粒粉。所使用的噴霧 乾燥機為藤崎電機（株）製的MDL_〇5〇，採用4流體方式的 噴嘴，使^送液量為40 cc/分鐘，噴嘴氣量為16〇 NL/分鐘， 給氣溫度為19(TC。所得顆粒粉的平均粒徑為9 7微米。 並且涊識到，改變製造丨次粒子時球磨機的條件，除了 使用平均粒徑為1.5微米的粉末作為！次粒子外，其他與上 述相同地製造顆粒粉，顆粒粉的平均粒徑達到58微米，難 以平均粒徑達到30微米或以下。 以氮氣作為載氣，將製得的顆粒粉供給到由陶瓷管構成 且以電為加熱源的加熱爐中。爐内溫度（加熱處理溫度）為 1650 C。此外，進行調節以使載氣流量達到丨升/分鐘，顆 粒粉在陶瓷管中的滯留時間調節在丨至…秒左右。 對於通過陶瓷管的粉末，使用螢光又射線分析裝置的X 射線繞射觀察組織。X射線繞射結果示於圖2。如圖2所 示，由於只觀察到鈦酸鋇（BaTl〇3)的峰，因此確認所製得 的粉末為由鈦酸鋇（BaTl〇3)單相構成的陶瓷粉末。鈦酸鋇 (BaTi03)的熔點為丨^?^。 此外，以SEM(掃描電子顯微鏡）觀察製得的鈦酸鋇粉 末。結果確認，該粉末的粒徑為0」至1〇微米左右，非常 接近真球狀，而且這些粉末沒有凝集。進而判明所測定的 ____-19- 本紙張尺度適用中國國家標準(CNS) A4規格(21〇χ 297公爱) 1291936 A7 ______B7 五、發明説明（17 ) 平均粒徑為2.5微米左右，且球形度約為】。進而，SEM獲 知的粉末擴大照片示於圖3，對每個粒子進行詳細觀察， 發現在整個粒子表面存在具有對稱性的結晶面的小平面 (7 7七7卜），為在粒子内不含粒界的單晶粒子。 此外，藉由TEM(透射電子顯微鏡）觀察製得的粉末。電 子束繞射像示於圖4，可以確認其具有粉末單晶特有的規 則性。， (比較例1) •除了加熱溫度變為1400°C以外，其餘與實施例！相同， 製得鈦酸鋇粉末。製得的粉末經SEM獲得的粉末放大照片 示於圖5。從圖5可以觀察到，鈦酸鋇粒子表面存在著粒 界。進而，電子束繞射像示於圖6中，從該電子束解析像 的結果可以確認其不為單晶。 (實施例2) 除了使用莫耳比為13.8: 54.7: 3 1.4: 0.1稱量的氧化鋇（Ba〇) 敉末、氧化鈦（Ti〇2)粉末、氧化钕（Nd2〇3)粉末和氧化錳 (MnO)粉末外，其餘與實施例相同，製得陶瓷粉末。 構成所得粉末的粒子平均粒徨為2 5微米，其為形狀非 常接近真球狀的微粒子。此外，觀察到整個粒子表面存在 具有對稱性的結晶面的小平面，為在粒子内不含粒界的單 晶粒子。 (實施例3) 除了在顆粒粉形成時，藉由噴嘴方式形成顆粒粉以使顆 粒私具有儘可能小的形狀外，其餘與實施例2相同，製得 -20- 1291936 A7 ---- - B7 五、發明説明（18 ) 陶資粉末。顆粒粉的平均粒徑為9丨微米。 對製得的粒子進行觀察，可以確認其生成了與實施例2 基本相同的單晶粒子。 、 (實施例4) 於旲耳比45.3: 47.1:7.6稱量的氧化鐵（ρ^2〇3)粉末、氧化 鎳（Ν1〇2)粉末及氧化鋅（Ζη〇)粉末中加入水，用球磨機混 合12小時，由此製造得到漿液（以下稱第丨漿液）。曰入 前，按相對於粉末重量1%的比例添加分散劑（東亞合二^ 製 A-30SL)。 第1漿液經喷霧乾燥機乾燥，進行顆粒化。此時的喷 霧、乾燥條件並無特麻定，最好設定的條件使顆粒粉的 粒徑達到200微米或以下。 ，所得顆粒粉在lOOOt的溫度燒結i小時，從而製得複合 氧=物燒結體。於該燒結體中添加水’並按相對於燒結二 重量1%的比例添加分散劑（東亞合成杜製A_30SL)後，以 球磨機粉碎48小時，從而製成含有作為^欠粒子的平均粒 徑0.3微米的粉末的漿液（第2漿液）。相對於粉末總重，於 該第2漿液中添加2重量％的稀#為1〇重量％濃度的pvA(聚 乙婦醇）溶液，進而進行調整以使第2漿液中粉末含量達到 60重量％。 第2漿液使用噴霧乾燥法製成顆粒粉。所用的喷霧乾 機為藤崎電機（株）製的MDL_050，採用4流體方式的噴 嘴，使送液量為40 CC/分鐘，噴嘴氣量為π。nl/分鐘，給 氣溫度為190°C。所得顆粒粉的平均粒徑為8 9微米。 -21-
1291936 A7 _________ 五、發明説明（19 ) ^ ~--- 以氮氣作為載氣’將製得的顆粒粉供給到由陶资管構成 且以電為加熱源的加熱爐中。爐内溫度（加熱處理溫度）為 15〇〇C。此外’進行調節以使載氣流量達到0.8升/分鐘， 顆粒粉在陶瓷管中的滯留時間達到丨至1〇秒左右。如此， 由顆粒粉製得陶瓷粉末（磁性鐵酸鹽材料）。 所得的陶€粉末藉#螢光⑽、線分析裝置的乂射線繞 射，對組織進行觀察。結果並未觀察到Fe2〇3、、 ,NiFe2C>4 ZnFe2〇4、CuFe2〇4的峰，因此確認所製得 的粉末為由Ni-Cu-Zn鐵酸鹽單相構成的陶瓷粉末。 此外，以SEM觀察所製得的Ni_Cu-Zn鐵酸鹽粉末。結果 確認，該粉末粒徑為O.iSiO微米左右，非常接近真球 狀且這些勃末沒有凝集。進而測定其平均粒徑為2.5微 米左右，且球形度約為1。進而，藉SEM獲得的粉末擴大 照片示於圖7，對每個粒子進行詳細的觀察，發現在整個 粒子表面存在具有對稱性的結晶面的小平面，為在粒子内 不含粒界的單晶粒子。 此外’以振動磁力計測定單晶陶瓷粉末的磁特性。結果 示於表1和圖8。該磁特性如後述。 進而’將製得的單晶陶瓷粉末以含有率為4〇體積。/(>混合 於環氧樹脂中，製得漿液（以下稱第3漿液）。此時，作為 ¥氧樹脂’其主成分含有··作為多官能環氧樹脂的 epibis(工（£匕只）型環氧樹脂（油化蜆殼環氧公司 製 epicot 1001及epicot 1007)，平均含量為Μ.9重量。/。；雙酚a型高 分子環氧樹脂（油化蜆殼環氧公司製epicot 1225)，含量為 •22- 1291936 A7 ____B7 五、發明説明（2〇 ) 23.1重量％，作為含有特殊骨架的環氧樹脂的四苯驗基乙 院型環氧樹脂（油化蜆殼環氧公司製epic〇t 1〇31s)，含量 為23.1重量％ ’作為固化劑的雙酚a型酚醛清漆樹脂（油化 規殼環氧公司製YLH129B65)，作為固化促進劑的咪唑化 合物（四國化成工業社製2E4MZ)溶解於甲苯及甲基乙基酮 中。於其中添加鐵酸鹽單晶粒子，以球磨機分散、混合。 所得的第3漿液塗覆於玻璃布上，製成半固化狀態的聚 酯預浸膠，作為基板的原材料。使聚酯預浸膠成為半固化 狀態的熱處理條件為·· 1〇〇。(：加熱2小時。此外，玻璃布為 Η玻璃、E玻璃、D玻璃等’並無特別限定，可以根據不同 要求特性分別使用，但此處使用Ε玻璃。此外，玻璃厚度 可以根據要求使用所需的適宜厚度，此處使用的厚度為 100微米。製得的半固化狀態的聚酯膠片按規定片數重 疊’在加壓、加熱條件下製成厚度約〇4毫米的複合磁性 材料。測定該基板的頻率特性-導磁率。結果示於圖丨〇。 (比較例2) 於莫耳比45.3:47.1:7.6稱量的氧化鐵（Fe2〇3)粉末、氧化 鎳（Ni〇2)粉末及氧化鋅（Zn0)粉末中加入水，以球磨機混 合12小時，製得漿液（以下稱第丨漿液）。混合前，按相對 於粉末重量1%的比例添加分散劑（東亞合成社製冬 30SL)。 第1漿液經噴霧乾燥機乾燥，進行顆粒化。 所得顆粒粉在1000°C的溫度燒結丨小時，從而製得複合 氧化物燒結體。以球磨機粉碎該燒結體丨2小時，從而製得 -23- 本紙張尺度適财81國$標準(CNS) A4規格(210 X 297公釐) 1291936
千均粒徑3¼米的粉末。與實施例4相同，對 杜α ， 了邊粉末進行磁 特性測足。結果示於表1及圖9。 除了使用製得的粉末外，其餘與實施例4相同，製造複 合磁性材料，並測定其頻率特性-導磁率。沾 ΊΠ 、、、。果示於圖 [表1] 尤施例4 比較例2 飽和磁通量密度Bs(G) 3125 2978 (實施例4及比較例2中測定的磁特性） 從表1可看出，與比較例2製造的粉末相比，命、 μ 男她例4中 衣侍的鐵酸鹽粉末，其飽和磁通量密度提高。此外，實施 例4及比較例2製得的粉末的磁滞曲線示於圖8及圖9中只= 藉由實施例4和比較例2的比較結果，可看出實施例*的磁 滯損失降低，作為磁性鐵酸鹽材料，其為低損失物質。此 外，如圖10所tf，藉由實施例4和比較例2中的頻率特性_ 導磁率比較，可看出實施例4的複合磁性材料超過ι〇〇〇 MHz的區域高達20%。 (實施例5) 首先於依1: 1莫耳比分別稱量的氧化鎂（Mg〇)粉末、氧 化鈦（Ti〇2)粉末中添加水，以球磨機混合12小時，由此製 仔漿液（第1漿液）。混合時按相對於粉末總重量的比例 添加分散劑（東亞合成社製A-30SL)。 該第1漿液經噴霧乾燥機進行乾燥、顒粒化，製得複合 -24-
1291936 A7 —·~— _B7 五、發明説明（22 ) 氧化物顆粒。此時的乾燥噴霧條件並無限定，可以設定條 件使顆粒徑達到200微米或以下。 該顆粒在1250°C的溫度燒結1小時，使複合氧化物反應 並燒結。其後，於該複合氧化物中添加水及分散劑（東亞 合成社製A-30SL)，再次用球磨機粉碎48小時，製得由平 均粒徑為0.5微米的微粉末構成的漿液（第2漿液）。相對於 粉末的'總重，於該第2漿液中添加2重量％的濃度稀釋為1〇 重量％的PVA(聚乙晞醇）溶液，進一步調整使第2漿液中 粉末重量比達到40重量％。 對第2漿液使用噴霧乾燥法，製得顆粒粉。使用的噴霧 乾燥機為藤崎電機（株）製的MDL-050，採用4流體方式的 噴嘴，送液量為40 cc/分鐘，噴嘴氣量為16〇 NL/分鐘，給 氧μ度為190 C。製造的顆粒粉平均粒徑為9 7微米。 隨後，以氮氣和氧氣的混合氣體作為載氣，將上述製得 的顆粒粉供給到加熱至1600它的陶瓷管中。藉由調節載氣 的流量，使生成粉末的滯留時間達到1至1〇秒左右。 對通過陶瓷管的粉末，以螢光又射線分析裝置獲得的χ 射、、泉繞射結果可以看到鈦酸鎂的單相。此外，以SEM觀察 ^製得的鈦酸鎂粉末，可以確認該粉末沒有凝集。此外， 可以看到，各粉末的粒徑為〇 1至1 〇微米左右，由非常接 近真球狀的微粒子組成，平均粒徑約為丨5微米，球形度 、’、勺為1。對每個粒子進行仔細觀察，可以發現整個粒子表 面存在具有對稱性的結晶面的小平面，為在粒子内不含有 介面的單晶粒子。 -25- 1291936 A7 B7
五、發明説明（23 稱1與上述單晶粉末燒結溫度不同的玻璃材料（日本兩 氣硝子製Mg〇· b2〇3 · Si02系玻璃GA-60、平均粒徑：^ 微米），使上述單晶粉末含量達到65體積％，將聚乙缔酵 縮丁醛（積水化學ESLESK(工只b y夕）bh-3)溶解於甲苯^ 乙醇的混合溶劑中，然後混入漿液中，製得電介質漿液。 混合使用球磨機，可使混合分散均句。將其用刮刀塗裝 法成型為厚度約200微米的生膜。其後，將生膜積層成約 1300微米厚度，在9〇(rc保持2小時的條件下進行燒結，製 得燒結體。進而，將該燒結體製成長8毫米、寬1毫米、厚 1愛米的帶狀試料，測定其介電常數及品質係數Q(=1/tan 5 )。 至於比較例3，在900°C下保持2小時的條件下只對上述玻 璃材料進行燒結，測定燒結體的特性，結果示於表2。 實施例5雖然在9〇〇。(：的低溫燒結，但與玻璃單體相比， 可製得具有大Q的複合材料。此外，實施例5由於使用單 晶鈥酸鎂粉末，在燒結程序中，鈦酸鎂粉末與玻璃的反應 被控制在表面，因此可將鈦酸鎂所具有的Q降低控制在最 小限度内。結果製得具有高q值的複合材料。 [表2] £ Q 實施例5 5.2 458 比較例3 5.1 281 測定頻率：2 GHz (實施例6) 準備好實施例4中製得的單晶鐵酸鹽粉末。另一方面 ---：__-26- 本紙張尺度適用中g國*標準(CNS) ^規格(⑽X 297公

Claims (1)

  1. 95·汍1 知‘]c 年ρ ^4」Λ1 補充1 1291势莎砂〇87〇5號專利申請案 ^Ψ文申铸專产範圍替換本(95年10月)
    1· 一種單晶陶瓷粉末的製造方法，其特徵在於包括：將 由陶资成分組成的粉體與載氣一起供給到加熱處理區 域的粉體供給程序、將供給到上述加熱處理區域中的 上述粉體加熱到該粉體的熔點以上，並將該粉體保持 於前述加熱處理區域i至i 0秒的加熱處理程序、以及藉 由使上述加熱處理程序中製得的生成物冷卻而製得單 晶陶資粉末的冷卻程序，上述由陶瓷成分組成的粉體 係由平均粒徑為1微米或以下的1次粒子所形成的顆 粒。 2 ·如申請專利範圍第丨項之單晶陶瓷粉末的製造方法，其 特徵在於上述單晶陶瓷粉末的球形度為〇·9或以上。 3 ·如申請專利範圍第1項之單晶陶瓷粉末的製造方法，其 特徵在於上述加熱處理程序中，係將上述由陶瓷成分 組成的粉體溶融而形成溶融物。 4 ·如申請專利範圍第3項之單晶陶瓷粉末的製造方法，其 特徵在於上述加熱處理程序係在電氣管狀爐中進行 者。 5 ·如申請專利範圍第1項之單晶陶瓷粉末的製造方法，其 特徵在於上述由陶瓷成分組成的粉體是由5〇微米或以 下的粒子所形成者。 6· —種單晶陶瓷粉末的製造方法，其特徵在於藉由使由 陶資成分組成的粉體浮游同時使其在加熱爐中移動， 然後冷卻所製得的生成物，從而製得球形度為〇·9或以 上的單晶陶瓷粉末，上述由陶瓷成分組成的粉體係由 1291936 平均粒控為1微米或以下的1次粒子所形成的顆粒。
    7 . —種單晶陶瓷粉末，其特徵為其實質上由單晶非磁性 鐵酸鹽陶瓷粉末所構成，該非磁性鐵酸鹽陶資粉末之 平均粒後為1至20微米，具有0.9或以上的球形度，且係 由鈦酸鋇-敍系陶瓷、鈦酸鋇_錫系陶瓷、鉛_鈣系陶 瓷、二氧化鈦陶瓷、鈦酸鋇系陶瓷、鈦酸鉛系陶瓷、 鈦酸鳃系陶瓷、鈦酸鈣系陶瓷、鈦酸鉍系陶瓷、鈦酸 鎂系陶瓷等、CaW04系陶瓷、Ba(Mg、训）〇3系陶瓷、 Ba(Mg、Ta)〇3系陶資、Ba(c。、Mg、Nb)〇3 系陶資、 Ba(Co、Mg、Ta)〇3系陶瓷所成群中所選出之至一 種0 8 4申哨專利範圍第7項之單晶陶瓷粉末，其特徵在於 述單晶陶瓷粉末係由氧化物磁性材料所構成。 、 9·如申請專利範圍第7項之單晶陶㈣末，其特徵在於 述早晶陶竞粉末係由氧化物電介質材料所構成。
    1〇.^請專利範圍第7項之單晶陶资粉末，其特徵在於 述早晶陶瓷粉末的平均粒徑為丨至“微米。 11.:種複合材料，其特徵在於其係由磁性體材 負材料組成的單晶球狀44 、十、# t产 欠狀虱化物粉末與分散並保持有 =氧化物粉末的結合材料组成的複合材料，上 早卵球狀氧化物粉末的 為0.9或以上者。 千均粒徑為0.1至30微米球形 I2·如申請專利範圍第丨i項 处人妯拉尨A 1 ”<複合材料，其特徵在於上: 〜a材科係由樹脂所構成。 -2- 1291936 13. 如申請專利範園第12項之複合材料，其特徵在 球狀氧化物粉末含量在30至98重量％的範圍内。 14. 如申請專利範圍第11項之複合材科，其特徵在於上述 球狀氧化物粉末係由電介質材料所構成，上述社A材 料係由比構成上述球狀氧化物粉末的電介質材^溶 點低的電介質材料所構成。 15·如申請專利範圍第u項之複合材料，其特徵在於上述 球狀氧化物粉末的量為3〇至7〇體積％。 申請專利範圍第u項之複合材料〇，°其特徵在於上述 球狀氧化物粉末係由磁性體材料所構成，上述結合材 料係由比構成上述球狀氧化物格古 虱化物4末的磁性體材料熔點 低的磁性體材料所構成。 申請專利範圍第16項之複合材料，其特徵在於上述 琢狀氧化物粉末量為30至70體積％。 18.:申請專利範圍第η項之複合材料，其係用於在電介 負層中配置有内邵金屬電極的電子零件。 19·ΐ!請專利範圍第U項之複合材料，其係'用於在磁性 滑中配置有内部金屬電極的電子零件。
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