TW201733962A - 含富鋁紅柱石燒結體、其製法及複合基板 - Google Patents

含富鋁紅柱石燒結體、其製法及複合基板 Download PDF

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TW201733962A
TW201733962A TW106109502A TW106109502A TW201733962A TW 201733962 A TW201733962 A TW 201733962A TW 106109502 A TW106109502 A TW 106109502A TW 106109502 A TW106109502 A TW 106109502A TW 201733962 A TW201733962 A TW 201733962A
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Prior art keywords
mullite
sintered body
less
substrate
containing sintered
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TW106109502A
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English (en)
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TWI718275B (zh
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Yoshinori Isoda
Yoshio Suzuki
Katsuhiro Inoue
Yuji Katsuda
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Ngk Insulators Ltd
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/185—Mullite 3Al2O3-2SiO2
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Abstract

本發明提供一種含富鋁紅柱石燒結體，係除了富鋁紅柱石(mullite)之外，尚含有至少1種選自由氮化矽、氧氮化矽及賽隆(SIALON)所成群組。此含富鋁紅柱石燒結體，以在40~400℃的熱膨脹係數未達4.3ppm/℃，孔隙率為0.5%以下，平均結晶粒徑為1.5μm以下為佳。

Description

含富鋁紅柱石燒結體、其製法及複合基板
本發明係關於一種含富鋁紅柱石燒結體、其製法及複合基板。
富鋁紅柱石燒結體，一般為將氧化鋁(Al2O3)與二氧化矽(SiO2)以3比2的比例燒結成為耐熱衝擊性佳的材料，以3Al2O3．2SiO2表示。作為此類富鋁紅柱石燒結體，例如專利文獻1所揭示，將在富鋁紅柱石粉末中混合30質量%氧化釔安定化二氧化鋯(YSZ)粉末而成的粉末成形，將其成形體進行燒結者。專利文獻1中，從富鋁紅柱石燒結體切出富鋁紅柱石基板，藉由對此富鋁紅柱石基板的主表面研磨，成為可用於與GaN基板貼合的基底基板。GaN的熱膨脹係數在室溫至1000℃的範圍內為6.0ppm/K，富鋁紅柱石的熱膨脹係數為5.2ppm/K。因此，當考慮到將兩者貼合使用時，以提高富鋁紅柱石的熱膨脹係數至接近GaN基板的熱膨脹係數較佳，故於富鋁紅柱石粉末中混合YSZ粉末並使其燒結。
另一方面，專利文獻2中記載將由鉭酸鋰或鈮酸鋰等構成的機能性基板與富鋁紅柱石燒結體製的支撐基板藉由直接接合使其接合的複合基板應用於表面聲波元件等聲波裝置的例子。此等聲波裝置，由於作為支撐基板的富鋁紅柱石 基板的熱膨脹係數為4.4ppm/℃(40~400℃)左右，楊氏模數為220GPa以上，能夠使因聲波裝置本身的溫度變化所造成的膨脹或收縮變小，藉此大幅改善頻率的溫度依存性。為了使機能性基板與支撐基板直接接合，於各接合面要求有高的平坦性。例如，專利文獻2中記載，中心線平均粗度Ra為3nm以下為較佳。
【先前技術文獻】
專利文獻
專利文獻1：日本特許5585570號公報
專利文獻2：日本特許5861016號公報
然而，雖然專利文獻1中記載在富鋁紅柱石中添加相當量的其他成分，提高熱膨脹係數的富鋁紅柱石燒結體，於專利文獻2中記載富鋁紅柱石的純度高的富鋁紅柱石燒結體，卻完全未提及降低熱膨脹係數的富鋁紅柱石燒結體，更不用說知曉作為此類低熱膨脹的富鋁紅柱石燒結體的經研磨精緻化的面的表面平坦性高一事。此外，即使將低熱膨脹的低剛性富鋁紅柱石燒結體作為複合基板的支撐基板使用時，複合基板也會因些微的溫度差而造成捲曲。
本發明的主要目的係為了解決此等課題，使含有富鋁紅柱石的燒結體，相較於單獨的富鋁紅柱石，熱膨脹係數降低、剛性提高，同時提高研磨面的平坦性。
本發明的含富鋁紅柱石燒結體，係除了富鋁紅柱石之外，尚含有至少1種選自由氮化矽、氧氮化矽及賽隆所成群組之含富鋁紅柱石燒結體，其中，40~400℃的熱膨脹係數未達4.3ppm/℃，孔隙率為0.5%以下，平均結晶粒徑(燒結粒子的平均粒徑)為1.5μm以下者。此含富鋁紅柱石燒結體相較於單獨的富鋁紅柱石，熱膨脹係數低且剛性高。此外，可提高研磨面的平坦性。
本發明的含富鋁紅柱石燒結體的製法，係包含：(a)將平均粒徑1.5μm以下的富鋁紅柱石粉末50~90體積%與平均粒徑1μm以下的氮化矽粉末10~50體積%，以合計成為100體積%的方式混合，獲得混合原料粉末的步驟；及(b)將上述混合原料粉末成形為預定形狀的成形體，藉由將上述成形體在加壓壓力20~300kgf/cm2，燒成溫度1525~1700℃進行熱壓燒成，獲得含富鋁紅柱石燒結體的步驟。此製法適於製造上述本發明的含富鋁紅柱石燒結體。且，粉末的平均粒徑係由雷射繞射法所測定的值(以下皆同)。
本發明的複合基板係將機能性基板與支撐基板予以接合的複合基板，上述支撐基板係上述含富鋁紅柱石燒結體。此複合基板，由於作為支撐基板的含富鋁紅柱石燒結體的研磨面平坦性高，故能與機能性基板良好地接合。此外，此複合基板應用於表面聲波裝置時，頻率溫度依存性大幅改善。此外，即使在光波導裝置、LED裝置、切換裝置中，因支撐基板的熱膨脹係數小而提升性能。
10‧‧‧複合基板
12‧‧‧壓電基板
14‧‧‧支撐基板
30‧‧‧電子裝置
32,34‧‧‧IDT電極
36‧‧‧反射電極
第1圖係含富鋁紅柱石燒結體的製造步驟流程圖。
第2圖係複合基板10的斜視圖。
第3圖係使用複合基板10所製作的電子裝置30的斜視圖。
以下，具體說明本發明的實施的形態，然而，本發明不限定於以下的實施的形態，在不脫離本發明要旨的範圍內，基於所屬領域者的通常知識，應可理解而加以適當變更、改良等。
本實施形態的含富鋁紅柱石燒結體係除了富鋁紅柱石之外，尚含有至少1種選自由氮化矽、氧氮化矽及賽隆所成群組。以富鋁紅柱石成為燒結體中含有最多的成分(主成分)為佳，然而即使選自上述群組成分成為主成分也無妨。此含富鋁紅柱石燒結體，以40~400℃的熱膨脹係數未達4.3ppm/℃，孔隙率為0.5%以下，平均結晶粒徑為1.5μm以下為佳。此含富鋁紅柱石燒結體，相較於單獨的富鋁紅柱石，熱膨脹係數低，楊氏模數(剛性)高。此外，此含富鋁紅柱石燒結體，由於幾乎沒有孔隙率為0.5%以下之氣孔、平均結晶粒徑小至1.5μm以下，因此研磨精緻化的面(研磨面)的平坦性變高。
本實施形態的含富鋁紅柱石燒結體，以存在於研磨面100μm×100μm每單位面積上的最大長度1μm以上的氣孔數為10個以下為佳。若氣孔數為10個以下，研磨精緻化的面的平坦性變得更高。此類氣孔數以3個以下為較佳，以零則更佳。
本實施形態的含富鋁紅柱石燒結體，以楊氏模數為240GPa以上為佳，以4點抗彎強度為300MPa以上為佳。氮化矽或來自於該等的成分比富鋁紅柱石有更高的楊氏模數或強度，藉由對富鋁紅柱石調節氮化矽的添加比例，可使含富鋁紅柱石燒結體的楊氏模數達240GPa以上，4點抗彎強度達300MPa以上。且，以4點抗彎強度為320MPa以上為較佳。
本實施形態的含富鋁紅柱石燒結體，以研磨面的中心線平均粗度Ra為1.5nm以下為佳。於聲波裝置等作為複合基板應用時，將機能性基板與支撐基板接合為已知，然而，像這樣使用研磨面的Ra為1.5nm以下的含富鋁紅柱石燒結體作為支撐基板使用，可使支撐基板與機能性基板的接合性變良好。例如，接合界面之間實際接合的面積的比例(接合面積比例)達到80%以上(較佳為90%以上)。研磨面的中心線平均粗度Ra以1.1nm以下為較佳，以1.0nm以下為更佳。
本實施形態的含富鋁紅柱石燒結體，以40~400℃的熱膨脹係數3.8ppm/℃以下為更佳，像這樣將含富鋁紅柱石燒結體作為支撐基板的複合基板應用於聲波裝置中，當彈性波裝置的溫度上昇時，由於機能性基板變得比原來熱膨脹更小的熱膨脹，而改善彈性波裝置的頻率溫度依存性。40~400℃的熱膨脹係數以3.5ppm/℃以下為更佳。
接著，說明本發明的含富鋁紅柱石燒結體的製造方法的一實施形態。含富鋁紅柱石燒結體的製造流程如第1圖所示，包含：(a)調製混合原料粉末的步驟；(b)製作含富鋁紅柱石燒結體的步驟。
‧步驟(a)：調製混合原料粉末
混合原料粉末係藉由將富鋁紅柱石粉末與氮化矽粉末混合而調製。作為富鋁紅柱石原料，以使用純度高、平均粒徑小的粉末為佳。純度以99.0%以上為佳，以99.5%以上為較佳，以99.8%以上為更佳。純度的單位為質量%。此外，平均粒徑(D50)以1.5μm以下為佳，以0.1~1.5μm為較佳。富鋁紅柱石原料可使用市售品，亦可使用高純度的氧化鋁或二氧化矽粉末所製作者。作為製作富鋁紅柱石原料的方法，例如可列舉專利文獻2中記載的方法。作為氮化矽原料，以使用平均粒徑小的粉末為佳。平均粒徑以1μm以下為佳，以0.1~1μm為更佳。富鋁紅柱石原料與氮化矽原料的混合比例，例如，以富鋁紅柱石原料50~90體積%(較佳為70~90體積%)與氮化矽原料10~50體積%(較佳為10~30體積%)合計100體積%的方式秤量，藉由球磨機等混合機混合，必要時藉由噴霧乾燥機乾燥，獲得混合原料粉末。
‧步驟(b)：製作含富鋁紅柱石燒結體
將步驟(a)所得的混合原料粉末成形為預定形狀的成形體。成形的方法並無特別限制，可使用一般的成形法。例如，可將混合原料粉末直接藉由模具加壓成形。加壓成形時，將混合原料粉末藉由噴霧乾燥機成為顆粒狀，成形性變得良好。另外，添加有機結合劑，製作生坯進行擠出成形，或是製作料漿進行板狀成形亦可。此等程序在燒成步驟前或是燒成步驟中必須去除有機結合劑成分。此外，亦可藉由冷均壓(CIP,cold isostatic press)進行高壓成形。
接著，將所得的成形體燒成，製作含富鋁紅柱石燒 結體。此時，維持燒結粒子的微細，在燒結中將氣體排出，使含富鋁紅柱石燒結體的表面平坦性提高為佳。作為其手段，熱壓法非常有效。因為使用此熱壓法，相較於常壓燒結，在低溫以微細粒的狀態朝向緻密化邁進，可抑制常壓燒結常見的殘留粗大的氣孔。此熱壓時的燒成溫度(最高溫度)以1525~1700℃為佳。此外，熱壓時的加壓壓力以達到20~300kgf/cm2為佳。特別是低的加壓壓力，由於可使熱壓治具的小型化或長壽命化而較佳。在燒成溫度的維持時間，可考慮成形體的形狀或大小、加熱爐的特性等，選擇合適、適當的時間。具體的較佳維持時間，例如1~12小時，更好為2~8小時。燒成環境氣體並無特別限制，熱壓時的環境氣體一般為氮、氬等惰性環境氣體。昇溫速度或降溫速度，考慮成形體的形狀或大小、加熱爐的特性等，適當地設定即可，例如可設定在50~300℃/小時的範圍。
接著，說明關於本發明的複合基板的一實施形態。本實施態的複合基板係將機能性基板與上述含富鋁紅柱石燒結體製的支撐基板接合而成者。此複合基板因兩基板的接合面積比例變大而顯示良好的接合性。作為機能性基板，並無特別限制，例如可列舉鉭酸鋰、鈮酸鋰、氮化鎵、矽等。接合方法以直接接合為佳。直接接合時，機能性基板與支撐基板之各別的接合面經研磨後活化，以兩接合面面對面對齊的狀態擠壓兩基板。接合面的活化，例如對接合面進行惰性氣體(氬等)的離子束的照射之外，尚有電漿或中性原子束的照射等。機能性基板與支撐基板的厚度比(機能性基板的厚度/支撐基板的厚度)以0.1以下為佳。第2圖表示複合基板的一例。複合基板10 係作為機能性基板的壓電基板12與支撐基板14經直接接合而接合而成者。
本實施形態的複合基板，可應用於電子裝置等。作為此類電子裝置，除了聲波裝置(表面聲波裝置或藍姆波(Lamb wave)元件、薄膜共振器(FBAR)等)之外，尚可列舉如LED裝置、光波導裝置、切換裝置等。於聲波裝置中利用上述複合基板時，由於作為支撐基板的含富鋁紅柱石燒結體的熱膨脹係數小至未達4.3ppm/K(40~400℃)，因此大幅改善頻率溫度依存性。第3圖表示使用複合基板10所製作的電子裝置30的一例。電子裝置30係1埠(port)SAW共振器亦即表面聲波裝置。首先，於複合基板10的壓電基板12使用一般的光微影技術，形成多數個電子裝置30的圖案，之後，藉由切割將一個一個的電子裝置30切出。電子裝置30係藉由光微影技術，在壓電基板12的表面形成IDT(Interdigital Transducer)電極32,34與反射電極36者。
又，本發明不限定於上述實施形態的任何一者，在本發明所屬技術範圍內，可實施各種態樣。
1. 製作混合原料粉末
作為富鋁紅柱石原料，使用市售純度99.9%以上，平均粒徑1.5μm的富鋁紅柱石粉末，作為氮化矽原料，使用市售純度97%以上，平均粒徑0.8μm的氮化矽粉末。將富鋁紅柱石原料與氮化矽原料如表1的實驗例1~3所示比例秤量，使用 5mm的氧化鋁圓石以球磨機混合，藉由噴霧乾燥機製作混合原料粉末。
2. 製作含富鋁紅柱石燒結體。
將實驗例1~3的混合原料粉末倒入直徑約125mm的模具中，在厚度10~15mm左右的圓盤狀以200kgf/cm2的壓力成形，獲得含富鋁紅柱石成形體。接著將含富鋁紅柱石成形體收容於內徑約125mm的熱壓用的石墨模具中，以熱壓爐製作直徑約125mm、厚度5~8mm左右的含富鋁紅柱石燒結體。且，燒成時的最高溫度(燒成溫度)為1650℃，在燒成溫度的維持時間為5小時，昇溫速度、降溫速度皆為100℃/小時。加壓負荷在昇溫中的900℃以上達到200kgf/cm2，爐內環境氣體至900℃為止呈真空，到達900℃後導入N2，在N2下進行燒結。在燒成溫度維持預定時間後，降溫至1200℃，停止控制加壓負荷與爐內環境氣體，自然冷卻至室溫。此外，實驗例4僅用富鋁紅柱石粉末同樣地形成成形體，製作燒結體。
3. 特性評估
從實驗例1~4的燒結體切出測試片(4×3×40mm尺寸的抗折棒等)，評估各種特性。此外，燒結體的研磨面係對4×3×10mm左右測試片的一面經研磨而精緻化成鏡面狀者。研磨依序以3μm的鑽石粗粒，0.5μm的鑽石粗粒進行，最終精緻化使用0.1μm以下的鑽石粗粒進行拋光研磨。評估的特性如下。
(1)結晶性
將燒結體粉碎，藉由X線繞射裝置，進行結晶相的認定。測定條件為CuKα、50kV、300mA、2θ=5-70°，使用旋轉靶陰 極型X線繞射裝置(理學電機製RINT)。
(2)結晶相比率
從上述(1)的X線繞射剖析，算出各結晶相的峰值面積比率。將富鋁紅柱石(210)面(2θ=26.2°)的峰值面積當作1，相對於此的各結晶相的峰值面積作為結晶相比率。在此，作為各結晶相的代表峰值，氮化矽使用(101)面(2θ=20.6°)，賽隆使用Si2Al3O7N的(3-20)面(2θ=24.6°)及Si5AlON7的(200)面(2θ=26.9°)。
(3)容積密度、孔隙率
使用抗折棒，藉由使用純水的阿基米德法，測定容積密度、孔隙率。
(4)楊氏模數
依JIS R1602為準則，以靜止彎曲法測定。測試片形狀為3mm×4mm×40mm抗折棒。
(5)抗彎強度
依JIS R1601為準則，測定4點抗彎強度。測試片形狀為3mm×4mm×40mm抗折棒或其一半的尺寸。
(6)熱膨脹係數(40~400℃)
依JIS R1618為準則，以推桿示差式測定。測試片形狀為3mm×4mm×20mm。
(7)氣孔數
如上述精緻化燒結體的研磨面以SEM觀察，計測存在於每100μm×100μm，最大長度為1μm以上的氣孔數。
(8)表面平坦性(Ra)
對如上述精緻化燒結體的研磨面，使用AFM，測定中心線平均粗度Ra。測定範圍為10μm×10μm。
(9)燒結粒子的平均粒徑
如上述的精緻化燒結體的研磨面以磷酸進行化學蝕刻，以SEM測定200個以上燒結粒子的大小，使用線性分析算出平均粒徑。線性分析的係數為1.5，將SEM實測的長度乘以1.5的值作為平均粒徑。
(10)接合性
從實驗例1~4的燒結體切出直徑100mm、厚度600μm左右的圓板。此圓板經如上述的研磨精緻化後，洗淨去除表面的微粒或污染物質等。接著，將此圓板作為支撐基板，對支撐基板與機能性基板實施直接接合，獲得複合基板。換言之，首先將支撐基板與機能性基板之各別的接合面以氬的離子束活化，之後將兩接合面對向貼合，以10tonf擠壓，獲得經接合的複合基板。作為機能性基板，使用鈮酸鋰(LN)基板。接合性的評估，從IR穿透影像判定，接合面積比例為90%以上者為「最佳」，80%以上未達90%者為「佳」，未達80%者為「不佳」。
4. 評估結果
實驗例1~3的含富鋁紅柱石燒結體係混合富鋁紅柱石原料與氮化矽原料的混合原料粉末經燒成而成者，氮化矽的一部份因燒成而變化成賽隆。實驗例1~3的含富鋁紅柱石燒結體由於含氮化矽等，相較於實驗例4的僅含富鋁紅柱石的燒結體，楊氏模數及4點抗彎強度提升。亦即，楊氏模數提升 至240GPa以上，4點抗彎強度提升至320MPa以上。此外，實驗例1~3的含富鋁紅柱石燒結體，40~400℃的熱膨脹係數未達4.3ppm/℃(3.5~4.1ppm/℃)，較實驗例4的僅含富鋁紅柱石的燒結體成為更低的值。再者，由於實驗例1~3的含富鋁紅柱石燒結體或實驗例4的僅含富鋁紅柱石的燒結體，孔隙率為0.5%以下(未達0.1%)，平均結晶粒徑為1.5μm以下(1.0~1.2μm)，研磨面的中心平均粗度Ra小至1.1nm以下(0.9~1.1nm)。因此，從實驗例2~4的燒結體所切出的圓板與機能性基板直接接合時的接合性，任一者接合面積比例皆達90%以上的「最佳」，從實驗例1的燒結體所切出的圓板與機能性基板直接接合時的接合性，接合面積比例為80%以上未達90%的「佳」。且，由於研磨面的中心平均粗度Ra到達如此小的值，故賦予氣孔數為3個以下(零)。
又，實驗例1~3相當於本發明的實施例，實驗例4相當於比較例。本發明並不限定於此等實驗例。
本申請案以主張2016年3月23日申請的日本專利申請第2016-058970號優先權的基礎，經由引用將其內容全部包含於本說明書中。

Claims (7)

  1. 一種含富鋁紅柱石燒結體，係除了富鋁紅柱石之外，尚含有至少1種選自由氮化矽、氧氮化矽及賽隆(SIALON)所成群組之含富鋁紅柱石燒結體，其中，40~400℃的熱膨脹係數未達4.3ppm/℃，孔隙率為0.5%以下，平均結晶粒徑為1.5μm以下者。
  2. 根據申請專利範圍第1項之含富鋁紅柱石燒結體，其中，在研磨面100μm×100μm每單位面積所存在的最大長度1μm以上的氣孔數為10個以下。
  3. 根據申請專利範圍第1或2項之含富鋁紅柱石燒結體，其中，楊氏模數為240GPa以上。
  4. 根據申請專利範圍第1至3項中任一項之含富鋁紅柱石燒結體，其中，4點抗彎強度為320MPa以上。
  5. 根據申請專利範圍第1至4項中任一項之含富鋁紅柱石燒結體，其中，研磨面的中心線平均粗度Ra為1.5nm以下。
  6. 一種含富鋁紅柱石燒結體的製造方法，係包含以下步驟：(a)將平均粒徑1.5μm以下的富鋁紅柱石粉末50~90體積%與平均粒徑1μm以下的氮化矽粉末10~50體積%混合成為合計100體積%，獲得混合原料粉末的步驟；及(b)將上述混合原料粉末成形為預定形狀的成形體，藉由將上述成形體在加壓壓力20~300kgf/cm2、燒成溫度1525~1700℃進行熱壓燒成，獲得含富鋁紅柱石燒結體的步驟。
  7. 一種複合基板，係接合機能性基板與支撐基板的複合基 板，上述支撐基板係申請專利範圍第1至5項中任一項之含富鋁紅柱石燒結體。
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