TWI664074B - 陶瓷構造體、基板保持裝置用元件以及陶瓷構造體之製法 - Google Patents

陶瓷構造體、基板保持裝置用元件以及陶瓷構造體之製法 Download PDF

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TWI664074B
TWI664074B TW104126954A TW104126954A TWI664074B TW I664074 B TWI664074 B TW I664074B TW 104126954 A TW104126954 A TW 104126954A TW 104126954 A TW104126954 A TW 104126954A TW I664074 B TWI664074 B TW I664074B
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electrode
substrate
ceramic
ceramic structure
thermal expansion
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TW104126954A
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TW201622998A (zh
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勝田祐司
西村昇
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日商日本碍子股份有限公司
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Abstract

本發明的陶瓷構造體10係在圓盤狀陶瓷基體12的內部內建有電極14。陶瓷基體12係主成分為氧化鋁或稀土族金屬氧化物的燒結體，熱膨脹係數在40~1200℃下為7.5~9.5ppm/K。電極14的主成分係金屬釕。電極14係可形成片狀，亦可依擴展於面全體的方式依照一筆畫要領形成圖案。

Description

陶瓷構造體、基板保持裝置用元件以及陶瓷構造體之製法
本發明係關於陶瓷構造體、基板保持裝置用元件以及陶瓷構造體之製法。
當將例如矽基板、玻璃基板、各種單晶基板等板狀材料施行精密加工，而製造半導體等元件、裝置之時，大多採用基板保持裝置。該基板保持裝置係有例如：具有會吸附基板功能的靜電吸盤或真空夾具、具有加熱功能的加熱器、或該等的組合等各式種類。其中，靜電吸盤、加熱器係在設有基板保持面的基體內部，以導電性物質為電極並呈圖案狀埋設，具有使產生靜電力、或供加熱用的焦耳熱等功能。
例如專利文獻1有揭示包括有：各種陶瓷基體、與在其內部埋設之電極的靜電吸盤。陶瓷基體的材料係可例示如：氧化鋁、氮化鋁、氮化矽、氧化矽、氧化鋯、氧化鈦、矽鋁氮氧化物(Sialon)、氮化硼、碳化矽或該等的混合物。另一方面，電極的材料係可例示如：鋁、鐵、銅、銀、金、鈦、鎢、鉬、白金等金屬；石墨、碳、碳化矽、氮化鈦、碳化鈦等陶瓷；或該等的混合物。
[先行技術文獻] [專利文獻]
[專利文獻1]日本專利特開平7-297265號公報
但是，近年使用主成分為氧化鋁或稀土族氧化物之陶瓷基體的基板保持裝置，期待厚度能再薄一點。然而，此種基板保持裝置例如當陶瓷基體與電極係依高溫施行一體煅燒進行製造的情況，厚度較薄的部分會有因陶瓷基體與電極間之熱膨脹差而發生翹曲的問題。
本發明係為解決此種課題而完成，主目的在於提供：在主成分為氧化鋁或稀土族金屬氧化物的陶瓷基體之表面或內部，設有電極的陶瓷構造體，於製造時不易發生翹曲者。
本發明的陶瓷構造體係在主成分為氧化鋁或稀土族金屬氧化物的陶瓷基體之表面或內部，設有電極的陶瓷構造體；其中，上述陶瓷基體的熱膨脹係數係40~1200℃下為7.5~9.5ppm/K；上述電極的主成分係金屬釕。另外，所謂「主成分」係指體積比例佔50體積%以上的成分或所有成分中，體積比例最高的成分。
本發明的基板保持裝置用元件係包括有上述陶瓷構造體。
本發明陶瓷構造體之製法，係在主成分為氧化鋁或稀土族金屬氧化物的成形體、初燒體或燒結體之第1基體其中一面上，配置主成分為金屬釕之電極或電極前驅物，並再於 其上面積層主成分為與上述第1基體相同氧化物之成形體、初燒體或燒結體的第2基體，而形成積層體，再將該積層體施行熱壓煅燒而獲得陶瓷構造體。
本發明的陶瓷構造體中，陶瓷基體的熱膨脹係數係在40~1200℃下為7.5~9.5ppm/K。另一方面，電極的主成分係金屬釕，金屬釕的熱膨脹係數係在40~1200℃下為7.9ppm/K。依此因為陶瓷基體與電極間之熱膨脹係數差較小，因而本發明的陶瓷構造體即便在製造時依高溫將陶瓷基體與電極施行一體煅燒，仍不易發生翹曲。
本發明的基板保持裝置用元件因為包括有上述陶瓷構造體，因而可獲得與利用該陶瓷構造體所獲得效果為同樣的效果。
本發明的陶瓷構造體之製法係適用於製造上述陶瓷構造體。
10‧‧‧陶瓷構造體
12‧‧‧陶瓷基體
14‧‧‧電極
20‧‧‧積層體
21‧‧‧第1基體
22‧‧‧第2基體
24‧‧‧電極圖案
圖1係陶瓷構造體10的立體示意圖。
圖2係圖1的A-A切剖圖。
圖3係陶瓷構造體10之製造步驟圖。
本發明的陶瓷構造體係在陶瓷基體的表面或內部設有電極。
陶瓷基體係主成分為氧化鋁或稀土族金屬氧化物 的燒結體，熱膨脹係數係40~1200℃下為7.5~9.5ppm/K、較佳8~9ppm/K。主成分為氧化鋁的情況，除氧化鋁之外尚可含有源自燒結助劑的成分。氧化鋁的燒結助劑係可例如鹼土族金屬的氟化物(MgF2、CaF2等)或氧化物(MgO、CaO等)。當氧化鋁的燒結助劑係使用鹼土族金屬的氟化物時，經燒結後亦會有直接依構成相存在的成分、或經反應而成為氫氟酸的成分。當氧化鋁的燒結助劑係使用鹼土族金屬之氧化物的情況，經燒結後會成為以其氧化物與氧化鋁之反應物為主的構成相。例如，當氧化鋁的燒結助劑係使用MgO的情況，構成相係含有MgAl2O4。主成分為稀土族金屬氧化物的情況，亦是除稀土族金屬氧化物之外尚可含有源自燒結助劑的成分。稀土族金屬氧化物的燒結助劑係可例如稀土族金屬或鹼土族金屬的氟化物(YF3、YbF3、CaF2等)。
電極的主成分係金屬釕。金屬釕的熱膨脹係數係40~1200℃下為7.9ppm/K。所以，陶瓷基體與電極在40~1200℃下的熱膨脹係數差之絕對值便成為較小值。又，因為金屬釕在室溫下的電阻率係6~10×10-6Ωcm的偏低值，因而例如將電極使用為加熱器電極時便容易精度佳地控制發熱量。特別係因為欲削薄基板保持裝置的情況，亦最好能削薄在陶瓷基體上所形成電極的厚度，因而電極要求較低的電阻率。電阻率並無特別的下限，但可認為5×10-6Ωcm已屬現實極限。
電極係除金屬釕之外，尚亦可含有：填料成分、其他金屬元素、釕與其他金屬的合金中之至少1種。此情況，最好依陶瓷基體與電極在40~1200℃下的熱膨脹係數差之絕對 值變小之方式，含有填料成分、釕以外的金屬、釕與其他金屬的合金。依此絕對值較佳係在1.0ppm/K以下。依此的話，因為40~1200℃下的陶瓷基體與電極之熱膨脹係數差非常小，因而即便削薄陶瓷構造體的厚度，仍幾乎不會發生翹曲。
填料成分較佳係從二氧化鋯、氮化鈦及構成陶瓷基體的主成分物質所構成群組中選擇至少1種。因為二氧化鋯的熱膨脹係數在40~1200℃下係12~12.5ppm/K，因而可有效使用為欲提高電極的熱膨脹係數時的填料成分。即，二氧化鋯係盡量少量添加於電極中便可提高電極的熱膨脹係數。又，二氧化鋯係即便高溫但仍不會(或較難)與金屬釕產生反應，因而對金屬釕的電阻率影響較小，就此點而言亦是屬於較佳的填料成分。因為氮化鈦的熱膨脹係數在40~1200℃下係9~9.5ppm/K，因而可有效使用為欲提高電極的熱膨脹係數時的填料成分。因為氮化鈦係屬於導電性物質，因而可有效使用為欲抑低電極電阻率時的填料成分。因為氮化鈦係即便高溫但仍不會(或較難)與金屬釕產生反應，因而對金屬釕的電阻率影響較小，就此點而言亦是屬於較佳的填料成分。藉由將構成陶瓷基體的主成分物質添加於電極中，便可縮小電極與陶瓷基體間之熱膨脹係數差。另外，填料成分亦可使用熱膨脹係數較高的MgO，但當陶瓷基體的主成分係氧化鋁之情況，在高溫下會與氧化鋁產生反應而生成尖晶石。尖晶石必需注意下述事項：熱膨脹係數與氧化鋁同等、絕緣性亦是與氧化鋁同等均較高、以及電極內的尖晶石體積量會較所添加MgO的體積量增加。
釕以外的其他金屬最好係鈦及鈮中之至少一者。 因為鈦、鈮的熱膨脹係數較高於釕，因而可有效使用為欲提高電極之熱膨脹係數時的添加物。又，因為鈦、鈮係屬於具導電性的成分，因而可有效使用為欲抑低電極電阻率時的添加物。又，因為鈦、鈮的磁化率較小，因而即便將陶瓷構造體使用於利用磁場的磁控式裝置，仍不會對磁場造成不良影響。
釕與其他金屬的合金較佳係RuAl合金。因為RuAl合金的熱膨脹係數在40~1200℃下為11ppm/K前後，較高於釕，因而可有效使用於欲提高電極熱膨脹係數時的添加物。又，因為RuAl合金的導電性較高，因而可有效使用為欲抑低電極電阻率時的添加物。當將此種合金添加於電極時，預估會與釕生成合金的其他金屬，在煅燒時會與釕產生反應並生成合金，故可先預估決定其添加量之後再添加於釕中。
電極較佳係室溫下的電阻率在3.0×10-5Ωcm以下。依此的話，當將電極利用為加熱器電極時便可輕易地精度佳控制發熱量。所以，最好依電極在室溫下的電阻率成為該數值範圍的方式，使金屬釕含有填料成分、釕以外的金屬、釕與其他金屬的合金。當將電極使用為加熱器電極的情況，室溫下的電阻率較佳係2.5×10-5Ωcm以下、更佳係2.0×10-5Ωcm以下。
本發明陶瓷構造體一實施形態，如圖1及圖2所示。圖1所示係陶瓷構造體10的立體示意圖，圖2所示係A-A切剖圖。陶瓷構造體10係在圓盤狀陶瓷基體12的內部內建有電極14。陶瓷基體12係主成分為氧化鋁或稀土族金屬氧化物的燒結體，熱膨脹係數係40~1200℃下為7.5~9.5ppm/K。電極14的主成分係金屬釕。電極14係可形成片狀，亦可依擴展於 面全體的方式依照一筆畫要領形成圖案。又，形成片狀或圖案狀的電極亦可形成複數個。此種陶瓷構造體10的製法一例，如圖3所示。該製法中，首先第1基體21係準備陶瓷燒結體(參照圖3(a))。接著，在第1基體21的上面形成電極圖案24(參照圖3(b))。接著，依覆蓋該電極圖案24的方式，積層著屬於第2基體22的陶瓷成形體而形成積層體20(參照圖3(c))。然後，將該積層體20施行熱壓煅燒。經熱壓煅燒後，第1基體21與第2基體22呈一體而成為陶瓷基體12，電極前驅物24成為電極14，便完成陶瓷構造體10(參照圖3(d))。當第1基體21及第2基體22的主成分係氧化鋁的情況，熱壓煅燒的煅燒溫度最好設定在1500℃以下(例如1100℃以上且1500℃以下)。又，當第1基體21及第2基體22的主成分係稀土族金屬氧化物的情況，熱壓煅燒的煅燒溫度最好設定在1600℃以下(例如1400℃以上且1600℃以下)。在該製法中，第1基體21係可為陶瓷成形體、亦可為陶瓷初燒體。又，第2基體22係可為陶瓷初燒體、亦可為陶瓷燒結體。又，當電極14在熱壓煅燒的前後並沒有變化時，電極前驅物24便與電極14為相同物。又，取代第1基體21，改為使用陶瓷構造體10、積層體20，便可製作多層含有電極的陶瓷構造體。另外，陶瓷構造體10係例示在陶瓷基體12的內部有內建電極14者，但亦可在陶瓷基體12的表面上配置電極14。
但是，國際公開第2013/54806號公報所揭示的陶瓷構造體，係包括有：以在氧化鎂中固溶有Al、N成分的Mg(Al)O(N)為主相之陶瓷基體、以及在其內部埋設的電極。該 文獻揭示電極係在金屬釕中摻和MgO者。但是，該文獻的陶瓷基體係以Mg(Al)O(N)為主相，熱膨脹係數係10.2~12.8ppm/K。所以，就此點而言不同於本發明的陶瓷構造體。又，電極係為配合陶瓷基體的熱膨脹係數而在金屬釕中摻和多量MgO。因為MgO係屬於絕緣體，因而經大量摻合其的電極便成為高電阻。所以，將電極使用為加熱器電極的情況，產生必需增加電極截面積的情形，故會有無法精度佳控制發熱量的可能性，且造成必需對加熱器施加高電壓，因而加熱器控制用的電源要求非常大功率等可能性。
本發明的基板保持裝置用元件係包括有上述陶瓷構造體。基板保持裝置用元件係除保持例如半導體用Si基板、SiC基板、GaN基板等半導體用基板的裝置所使用元件之外，尚亦可例如保持照明用或顯示器用玻璃基板的裝置所使用之元件等。
[實施例]
以下，針對本發明實施例進行說明。另外，本發明並不受以下實施例的任何限定。又，純度、雜質含有量的「%」係指「質量%」。
(1)陶瓷構造體之製法
(1-1)第1基體之準備
(1-1-1)原料粉末之調整
Al2O3粉末係使用市售高純度Al2O3(純度99.99%以上、平均粒徑0.5μm)。為使Al2O3成形體燒結的燒結助劑係使用MgF2粉末與MgO粉末。MgF2粉末係使用由市售MgF2(純度99.9% 以上)粉碎而形成平均粒徑1μm以下者。MgO粉末係使用市售MgO粉末(純度99.95%以上、平均粒徑1μm)。MgF2粉末及MgO粉末的添加量，相對於Al2O3：100質量%分別設為0.3質量%及0.1質量%。秤量成為上述組成的Al2O3粉末、MgF2粉末及MgO粉末，以異丙醇為溶劑，使用尼龍製瓶、直徑5mm的Al2O3卵石依濕式進行4小時混合便形成漿料。從瓶中取出的漿料在氮氣流中依110℃施行乾燥，並將乾燥物通過30篩目的篩，再將過篩的粉末設為第1基體(Al2O3燒結體)製作用的原料粉末。
(1-1-2)圓盤狀成形體之製作
將上述原料粉末依200kgf/cm2壓力施行單軸加壓成形，便製得直徑50mm、厚20mm左右的圓盤狀成形體。
(1-1-3)圓盤狀成形體之煅燒
將上述圓盤狀成形體收容於熱壓用石墨模具中之後，安裝於熱壓爐中，將壓合壓力設為200kgf/cm2，依煅燒溫度(最高溫度)1200℃保持4小時便製得燒結體。升溫速度及降溫速度均設為300℃/hr，升溫中在達1000℃時便施行抽真空，然後導入氮氣。經導入後的氣體壓力維持呈1.5atm左右。降溫時在1000℃停止溫度控制，並施行爐冷卻。所獲得燒結體加工呈直徑50mm、厚10mm左右，將其設為當作第1基體使用的Al2O3燒結體。
以上針對實驗例1~8、10~30的第1基體所使用Al2O3燒結體進行說明，但實驗例9係將Al2O3初燒體使用為第1基體。Al2O3初燒體係使用根據1-1-2的方法所製作圓盤狀成形體，在氬環境下、依900℃施行熱處理後，再調整為直 徑50mm、厚20mm左右的形狀者。又，相關實驗例31、32中使用為第1基體的Y2O3燒結體及Yb2O3燒結體，係依如下述製作。實驗例31係除使用市售高純度Y2O3粉末，並將煅燒溫度設為1575℃之外，其餘均依據上述(1-1)的方法製作Y2O3燒結體。又，實驗例32係除使用市售高純度Yb2O3粉末，並將煅燒溫度設為1500℃之外，其餘均依據上述(1-1)的方法製作Yb2O3燒結體。另外，Y2O3粉末、Yb2O3粉末係使用純度99.9%以上、平均粒徑1μm以下者。
(1-2)電極糊膏之印刷
原料粉末係使用由市售Ru粉末(純度99.9%)粉碎形成平均粒徑4μm左右者。相關Ru電極中所導入的填料成分、以及除Ru以外的金屬成分，係使用下述。另外，所謂「填料成分」係指與Ru的反應性較低之成分，在本發明中係指導入陶瓷成分的情況。例如將Al2O3、ZrO2、TiN、Y2O3、Yb2O3等稱為填料成分。另一方面，屬於金屬成分的Al、Ti、Nb相較於就填料成分所舉例的陶瓷成分之下，較容易與Ru產生反應，例如Al的情況會成為RuAl合金(依莫耳比計為Ru：Al=1：1)，又當Nb的情況會明顯發現固溶於Ru中的成分，因而統籌稱為Ru以外的金屬成分。填料成分所使用的Al2O3、Y2O3、Yb2O3係使用與第1基體所使用者為相同物。ZrO2係使用純度99.9%、平均粒徑1μm以下的市售物。TiN係使用除氧外的雜質含有量在0.1%以下、且平均粒徑0.9μm的市售物。Al係使用高純度Al粉末、且#500以下的市售物。Ti係使用純度99.9%、平均粒徑10μm的市售物。Nb係使用純度99%、且平 均粒徑20μm的市售物。依成為表1所記載比例的方式，秤量Ru粉末與各種填料成分或除Ru以外的金屬成分，且黏結劑係使用聚甲基丙烯酸正丁酯，有機溶劑係使用丁基卡必醇，形成印刷用的電極糊膏。
在依上述(1-1-3)所獲得燒結體的上面，使印刷用的電極糊膏通過網版而印刷為寬5mm×長15mm大小(實驗例1~8、10~32)。此時，電極糊膏的印刷厚度設為50~100μm，經印刷後，在大氣中，依100℃施行1小時乾燥。另外，實施例9中，第1基體係使用將混合粉末的圓盤狀成形體在惰性環境中依900℃施行熱處理者，在該成形體其中一面上印刷電極糊膏。
(1-3)第2基體之配置
在依上述(1-2)所製作第1基體的電極糊膏印刷面上，重疊第2基體而形成積層體。實驗例1~9、11~30中，第2基體係使用上述(1-1-2)所獲得Al2O3成形體。實驗例10中，第2基體係使用上述(1-1-3)所獲得Al2O3燒結體。實驗例31、32中，第2基體係使用獲得上述(1-1-3)的Y2O3燒結體及Yb2O3燒結體前的成形體。
(1-4)煅燒一體化
將上述(1-3)所製作的積層體收容於熱壓爐中，依照與上述(1-1-3)基本相同的條件施行熱壓煅燒，藉由將積層體施行一體化，便獲得在陶瓷基體內部包括有燒結電極的陶瓷構造體。其中，各實驗例的煅燒溫度(最高溫度)係如表1所記載。
(2)陶瓷構造體之評價項目
‧單體之熱膨脹係數
Ru單體的熱膨脹係數係製作Ru粉碎粉末的燒結體，藉由根據JIS-R1618的方法進行測定。此處，將陶瓷基體與電極糊膏藉由煅燒而一體化之後，因熱膨脹係數的不一致而生成之應變會構成問題，因而將熱膨脹係數的溫度範圍設為40~1200℃(1200℃係實驗例1~30的最低煅燒溫度)。依超過1200℃的煅燒溫度所製作構造體，若在此種高溫下，陶瓷材料因熱壓而被施加荷重負荷，不僅以Ru為主成分的金屬系電極材料，就連陶瓷材料多少亦會出現塑性變形，認為因熱膨脹係數的不一致等所生成應變會被緩和。所以，將熱膨脹係數的溫度範圍設為40~1200℃。Al2O3的熱膨脹係數係使用從Al2O3的陶瓷基體所切取Al2O3燒結體試料，根據JIS-R1618的方法進行測定。另外，Al2O3填料的熱膨脹係數亦設為與此同值。填料成分、除Ru以外的金屬之熱膨脹係數，係使用文獻所報告的數值，或使用與Al2O3同樣地製作燒結體，再根據JIS-R1618的方法所測定之數值。該等單體的熱膨脹係數係如表1所記載。
‧電極之熱膨脹係數
各個電極在40~1200℃下的熱膨脹係數，係從所使用材料單體在40~1200℃下的熱膨脹係數、與電極的調配比例計算求得。結果如表1所記載。
‧熱膨脹係數差
陶瓷基體與電極在40~1200℃下的熱膨脹係數差，係依絕對值計算出。
‧電極之電阻率
從所製作的陶瓷構造體，依寬9mm×長9mm×厚6mm程度的立方體狀、且在中央處內建有寬5mm×長9mm程度之電極的方式，切取試驗片。另外，電極的端面係呈試驗片的二端面露出寬5mm狀態，利用顯微鏡測量電極的寬度與厚度，求取電極端面的截面積S(cm2)。又，利用游標卡尺測量電極的長度L(cm)，並使用於電阻率計算。電阻測定用的電路係在電極二端面塗佈導電性糊膏，再連接導線而構成，在大氣中，於室溫下依0~150mA範圍流通微小電流I(mA)，測定此時所發生的微小電壓值V(mV)，並利用R=V/I求取電極的電阻R(Ω)。然後，利用ρ=R×S/L計算出電極的電氣電阻率ρ(Ωcm)。
‧微構造
所獲得元件的切剖面經施行鏡面研磨後，使用掃描式電子顯微鏡(SEM)及電子微探分析儀(EPMA)，觀察電極、陶瓷基體的界面、以及周邊等的微構造。
‧燒結體密度、開氣孔率
使用經切取為棒狀的試料，利用以純水為介質的阿基米德法進行測定。
(3)陶瓷構造體之評價結果
以下，針對各實驗例的評價結果進行說明。
‧實驗例1
將從上側起依序依Al2O3成形體(第2基體)/Ru100%電極/Al2O3燒結體(第1基體)的方式積層之積層體，於1200℃下施行4小時熱壓煅燒，而製作陶瓷構造體的例子。陶瓷基體與電 極的熱膨脹係數差係0.7ppm/K的較小值，當截面觀察時在界面或其附近亦均沒有發現龜裂發生等異常現象。電極的電阻率係1.3×10-5Ωcm的非常小值，得知具有當作加熱器用電極的充分機能。另外，從第1基體、第2基體所切取的Al2O3燒結體，容積密度3.97g/cm3以上、開氣孔率0.02%以下，具有充分緻密性。
‧實驗例2~4
實驗例2中，除在電極中添加Al2O3填料，並將電極組成設為Ru：90vol%、Al2O3：10vol%之外，其餘均依照與實驗例1同樣的條件製作元件。實驗例3、4中，Al2O3填料的添加量較實驗例2增加。因為Al2O3填料的熱膨脹係數較大於Ru，因而隨Al2O3填料添加量的增加，電極的熱膨脹係數亦會隨之變大，接近Al2O3基體的熱膨脹係數。該等例中，電極的熱膨脹係數係8.0~8.2ppm/K、且與Al2O3間之熱膨脹係數差縮小至0.6~0.4ppm/K。電極的電阻率係1.6×10-5~2.8×10-5Ωcm，隨填料添加量的增加亦會提高，但即便實驗例4的40vol%仍是2.8×10-5Ωcm的非常小值較佳狀態。又，與實驗例1同樣，在電極的界面或其附近並沒有龜裂發生等異常現象，且Al2O3基體的緻密性亦良好。
‧實驗例5~8
實驗例5~8中，除改變Al2O3填料的添加量、煅燒溫度之外，其餘均依照與實驗例2同樣的方法製作陶瓷構造體。實驗例5係Al2O3填料設為20vol%，並依1300℃施行煅燒的例子，電極的電阻率係1.6×10-5Ωcm，略低於同組成1200℃煅燒材料 (實驗例3)，呈良好狀態。實驗例6係未添加Al2O3填料，且依1500℃施行煅燒的例子，電極的電阻率係1.0×10-5Ωcm，在實驗例1~30中係屬於最低電阻。Al2O3填料添加20、40vol%的實驗例7、8，電阻率分別係1.5×10-5、2.1×10-5Ωcm，呈良好狀態。又，實驗例5~8均與實驗例1同樣地在電極的界面或其附近均沒有發現龜裂發生等異常現象，Al2O3基體的緻密性亦良好。另外，若實驗例6~8與實驗例1、3、4比較，則燒結溫度1500℃的實驗例6~8之電極電阻率較低於燒結溫度1200℃的實驗例1、3、4，理由係在1500℃時會充分進行電極的燒結，且各個粒子變大，推測減少晶界的電阻。
‧實驗例9、10
在實驗例9係使用Al2O3初燒體作為第1基體，而在實驗例10係使用Al2O3燒結體作為第2基體，除此之外，其餘均依照與實驗例5同樣的方法製作陶瓷構造體。實驗例9、10的電極電阻率分別係1.6×10-5、1.5×10-5Ωcm，屬於低電阻呈良好狀態。如實驗例9當第1基體係使用初燒體的情況，為製作陶瓷構造體的高溫下煅燒(正式煅燒)只要1次便可，具有能縮短製造步驟的優點。如實驗例10當第2基體係使用燒結體的情況，可更加提高電極面的平坦性。所以，當將實驗例10的陶瓷構造體利用為保持晶圓的陶瓷加熱器時，便可期待更加提升溫度均勻性。
‧實驗例11~13
實驗例11中，除填料係使用ZrO2之外，其餘均依照與實驗例2同樣的方法製作陶瓷構造體。從文獻推定ZrO2的熱膨脹係數係12.2ppm/K。因為ZrO2的熱膨脹係數較高，因而如實 驗例11藉由添加16vol%便可將熱膨脹係數差形成0.0ppm/K，能使電極的熱膨脹係數與Al2O3基體的熱膨脹係數呈完全一致。實驗例12係除煅燒溫度設為1300℃之外，其餘均依照與實驗例11同樣的方法製作陶瓷構造體之例子，此處亦是能製作使熱膨脹係數呈完全一致的陶瓷構造體。實驗例13係除將ZrO2添加量設為22vol%、煅燒溫度設為1300℃之外，其餘均依照與實驗例11同樣的方法製作陶瓷構造體。該實驗例13係電極的熱膨脹係數較大於Al2O3熱膨脹係數的例子。實驗例11~13均係在電極的界面或其附近均沒有發現龜裂發生等異常現象，且Al2O3基體的緻密性亦良好。電極的電阻亦是1.5×10-5~1.8×10-5Ωcm的較低值，屬良好狀態。
‧實驗例14,15
實驗例14中，除填料係使用TiN之外，其餘均依照與實驗例2同樣的方法製作陶瓷構造體。實驗例15中，除將TiN的添加量設為30vol%之外，其餘均依照與實驗例14同樣的方法製作陶瓷構造體。經利用所製作燒結體的測定，TiN的熱膨脹係數係9.4ppm/K。因為TiN係屬於導電性物質，因而實驗例14的電極電阻率係1.4×10-5Ωcm，較低於同添加量Al2O3填料的實驗例2之情況。又，實驗例15的電極電阻率係1.8×10-5Ωcm，較低於Al2O3填料20vol%較少狀態的實驗例3之電阻率。實驗例14、15亦均是在電極的界面或其附近均沒有發現龜裂發生等異常現象，且Al2O3基體的緻密性亦良好。
‧實驗例16~22
實驗例16~22中，為調整電極熱膨脹係數的金屬成分Al 添加於Ru中，利用Al與Ru的反應使電極內生成RuAl合金，形成Ru/RuAl電極。陶瓷構造體的基本製作方法係根據實驗例2。RuAl合金的熱膨脹係數及密度經利用燒結體實測係10.9ppm/K、7.97g/cm3，在假設所添加的Al全部均會與Ru產生反應而形成RuAl合金前提下，設定Al的添加量。表1的備註欄中，電極中的RuAl合金量係依「vol%」表示。因為RuAl合金係導電性高、且熱膨脹係數亦較大的材料，因而如實驗例16~22，利用少量的Al添加便可接近Al2O3基體的熱膨脹係數，且可使電極的電阻率成為1×10-5~2×10-5Ωcm的較低狀態。特別係實驗例16、18、21中，藉由添加11vol%的Al使生成RuAl合金18vol%，便可使電極的熱膨脹係數與Al2O3基體的熱膨脹係數差接近至0.2ppm/K。實驗例16~22均係在電極的界面或其附近均沒有發現龜裂發生等異常現象，且Al2O3基體的緻密性亦良好。
‧實驗例23~30
實驗例23~28的金屬成分係添加Ti，實驗例29、30的金屬成分係添加Nb。實驗例23~30係根據實驗例2的方法製作陶瓷構造體。實驗例23~30亦是可使電極的熱膨脹係數接近Al2O3基體的熱膨脹係數，且因為Ti與Nb係屬於熱膨脹係數高並具有導電性的成分，因而可獲得低電阻率的電極。特別係實驗例24、27可使電極的熱膨脹係數與Al2O3基體的熱膨脹係數呈完全一致。Ti與Nb係屬於容易固溶於Ru中的成分，但由電極利用EPMA進行的元素分佈解析，發現到特別係Nb廣泛擴散於Ru內。電極的電阻率係有添加Ti的實驗例23~28 為1×10-5Ωcm~2×10-5Ωcm的較低值，但經添加Nb的電阻則略高於該等，實驗例30因添加30vol%便成為1.6×10-4Ωcm。另外，實驗例23~30亦均在電極的界面或其附近均沒有發現龜裂發生等異常現象，且Al2O3基體的緻密性亦良好。
‧實驗例31,32
實驗例31、32係陶瓷基體主成分設為稀土族金屬氧化物的例子，除將煅燒溫度分別設為1575℃、1500℃之外，其餘均依照與實驗例2同樣的方法製作陶瓷構造體。陶瓷基體的熱膨脹係數係使用由陶瓷構造體切取的試料進行實測。二實驗例均係在電極中添加與第1基體同種成分的填料20vol%，但電極與陶瓷基體的熱膨脹係數差係0.3~0.5ppm/K的較小值，且電極的電阻率為1.4×10-5之較小值，可獲得良好狀態。由陶瓷構造體切取的陶瓷基體試料，Y2O3的容積密度達5.00g/cm3以上、Yb2O3的容積密度達9.17g/cm3以上，且開氣孔率均在0.03%以下，緻密性呈良好。又，在電極的界面與其附近亦沒有發現龜裂等異常現象。
‧比較例1~5
比較例1~5係在Al2O3基體中埋設習知所使用電極的例子。分別在表2所記載導電成分中添加既定量Al2O3填料，並根據實驗例1的方法製作陶瓷構造體。另外，在WC電極中分別添加為促進燒結用之助劑的Ni、Co各5vol%。又，各導電成分的熱膨脹係數係採用文獻值。比較例1~5雖Al2O3基體、電極的緻密性均良好，但因為電極的熱膨脹係數較小，因而即便在電極中添加相當量的Al2O3填料，但Al2O3基體與電極的 熱膨脹係數差仍較大於1ppm/K。且，因添加相當量的Al2O3填料，導致電極的電阻率高於3.0×10-5Ωcm。
由比較例1~5的結果得知，習知技術針對如氧化鋁、稀土族金屬氧化物(氧化釔等)所代表的熱膨脹係數7.5~9.5ppm/K(特別係8~9ppm/K)陶瓷基體，較難達成與陶瓷基體的熱膨脹係數差在1ppm/K以內、且電阻率在3×10-5Ωcm以下之低電阻率的電極組合。又，非常難獲得當作加熱器電極時能顯現出更高性能、電極電阻率在2.5×10-5Ωcm以下、或1×10-5Ωcm左右、且電極的熱膨脹係數能調整為適當的陶瓷構造體。又，比較例所示電極中，Ni、Co係屬於磁化率非常高的元素。容易帶此種磁性的元素在利用磁場的磁控式裝置中，因為會有對磁場環境造成影響的顧慮，因而電極中最好儘量避免含有。另外，實驗例1~32所示電極均係磁化率小，不會有對磁場造成影響的擔憂。
‧實驗例33、34
實驗例33係與實驗例16~22同樣地，在Ru中添加金屬成分的Al，而製作Ru/RuAl電極的例子。除將Al的添加量設為14vol%之外，其餘均依照與實驗例21同樣的條件製作陶瓷構造體，進行特性評價。本例中，藉由將電極中的Al添加量設為14vol%，便能獲得Ru/RuAl電極的熱膨脹係數與Al2O3基體的熱膨脹係數呈完全一致、且在電極與Al2O3的界面處沒有龜裂等經埋設良好電極的Al2O3基體。電極的電阻率係1.3×10-5Ωcm的較低值，屬良好狀態。實驗例34係除在Al2O3粉末中所添加的燒結助劑僅設定為MgO粉末0.25質量%，且熱壓煅燒溫度係在第1基材製作、積層體製作時均設為1500℃之外，其餘均依照與實驗例33同樣的方法，製作埋設 Ru/RuAl電極的Al2O3基體。本例亦是能獲得Al2O3與電極材的熱膨脹係數差為零、且沒有龜裂的良好構造體。電極電阻率係1.1×10-5Ωcm的較低值，屬良好狀態。。
本申請案係在根據2014年9月16日所提出申請日本專利申請案第2014-187868號主張優先權基礎下，爰引其所有內容融入於本說明書中。
另外，當然本發明並不因上述實施例而受任何限定。
[產業上之可利用性]
本發明係可利用於製造半導體等元件、裝置時所使用的基板保持裝置。

Claims (8)

  1. 一種陶瓷構造體，在主成分為氧化鋁或稀土族金屬氧化物的陶瓷基體之表面或內部，設有電極；其中，上述陶瓷基體的熱膨脹係數係40~1200℃下為7.5~9.5ppm/K；上述電極的主成分係金屬釕，並且，上述電極除金屬釕之外，尚含有釕以外的金屬、或釕與其他金屬的合金，上述釕以外的金屬係鈦及鈮中之至少一者，上述釕與其他金屬的合金係釕鋁合金。
  2. 如申請專利範圍第1項之陶瓷構造體，其中，上述陶瓷基體與上述電極在40~1200℃下的熱膨脹係數差之絕對值係1.0ppm/K以下。
  3. 如申請專利範圍第1或2項之陶瓷構造體，其中，上述電極係除金屬釕以外之外，尚含有填料成分。
  4. 如申請專利範圍第3項之陶瓷構造體，其中，上述填料成分係從二氧化鋯、氮化鈦、及構成上述陶瓷基體的主成分物質所構成群組中選擇至少1者。
  5. 如申請專利範圍第1或2項之陶瓷構造體，其中，上述電極在室溫下的電阻率係3.0×10-5Ωcm以下。
  6. 一種基板保持裝置用元件，包括有申請專利範圍第1至5項中任一項之陶瓷構造體。
  7. 一種陶瓷構造體之製法，在主成分為氧化鋁或稀土族金屬氧化物的成形體、初燒體或燒結體之第1基體其中一面上，配置主成分為金屬釕之電極或電極前驅物，並再於其上面積層主成分為與上述第1基體相同氧化物之成形體、初燒體或燒結體的第2基體，而形成積層體，再將該積層體施行熱壓煅燒而獲得陶瓷構造體。
  8. 如申請專利範圍第7項之陶瓷構造體之製法，其中，當上述第1基體及上述第2基體的主成分係氧化鋁的情況，便將上述熱壓煅燒的煅燒溫度設定在1500℃以下；當上述第1基體及上述第2基體的主成分係稀土族金屬氧化物的情況，便將上述熱壓煅燒的煅燒溫度設定在1600℃以下。
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