TW201706228A - 氧化鋁燒結體的製法及氧化鋁燒結體 - Google Patents
氧化鋁燒結體的製法及氧化鋁燒結體 Download PDFInfo
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Abstract
本發明,係氧化鋁燒結體的製法,係包含:(a)將含有Al2O3粉末、MgO粉末、MgF2粉末、溶劑、分散劑及凝膠劑之懸浮液投入成形模中,藉由在前述成形模內使前述凝膠劑化學反應而使前述懸浮液凝膠化後而得到成形體之工程、(b)藉由使該成形體乾燥後脫脂更預燒結,得到預燒結體之工程、(c)藉由在1150~1350℃熱壓燒成前述預燒結體,得到陶瓷燒結體之工程。在前述工程(a),關於調製前述懸浮液,做為Al2O3粉末,使用純度99.9質量%以上者,對於Al2O3粉末100質量分,使用0.1~0.2質量分之MgO粉末,0.13質量分以下之MgF2粉末。
Description
本發明係關於氧化鋁燒結體的製法及氧化鋁燒結體。
從以往,在半導體晶圓上施以成膜或蝕刻等之表面處理時,有使用靜電吸盤之情況。做為靜電吸盤,已知在圓板狀之氧化鋁基板埋設靜電電極,氧化鋁基板之一面成為晶圓載置面者。將半導體晶圓載置於此靜電吸盤之晶圓載置面之狀態下對靜電電極通電,則在靜電電極與半導體晶圓之間發生靜電力,藉由該靜電力,半導體晶圓被吸附保持於該晶圓載置面。又,在氧化鋁基板,也有與靜電電極一同埋設加熱電極之情況。在此情況,若在將半導體晶圓載置於晶圓載置面之狀態對於加熱電極通電,則半導體晶圓會由於加熱電極而被加熱。做為如此之靜電吸盤所使用之氧化鋁基板之製法,已知專利文獻1所記載之方法。根據該製法,首先,製作含有純度99.7%之氧化鋁粉末、少量的MgO原料粉、黏結劑、水及分散劑之懸浮液。接著,將該懸浮液噴霧乾燥,在500℃除去黏結劑製作氧化鋁顆粒。將該氧化鋁顆粒充填於模具,加壓成形做為成
形體。將該成形體設置於碳製之套管中,藉由熱壓燒成而做為氧化鋁燒結體,熱壓燒成,例如,係在100kg/cm2之加壓下,在氮氣氣氛(150kPa)中,在1600℃保持2小時之條件來進行。將如此所得到之氧化鋁燒結體研磨加工而做為氧化鋁基板。
[先前技術文獻]
[專利文獻]
專利文獻1:日本專利特開2008-53316號公報
然而,上述靜電吸盤,有在高溫之解吸響應性之差異很大的問題。解吸響應性,已知與體積電阻率或耐電壓有相關。因此,相較於以往,在高溫之體積電阻率或耐電壓高,每批次之這些的差異小之氧化鋁燒結體之開發被期待。
本發明係為了解決如此之課題而做成,以提供在高溫之體積電阻率或耐電壓高,每批次之這些的差異小之氧化鋁燒結體為目的。
本發明之氧化鋁燒結體之製法,係包含:(a)將含有Al2O3粉末、MgO粉末、MgF2粉末、溶劑、分散劑及凝膠劑之懸浮液投入成形模中,藉由在前述成形模內使前述凝膠劑化學反應而使前述懸浮液凝膠化後而得到成形體之工程、(b)藉由使該成形體乾燥後脫脂更預燒結,得到預燒結體之工程、(c)藉由在1150~1350℃熱壓燒成前述預燒結體,得到陶瓷燒結體之工程。在前述工程(a),關於調製前述懸浮液,做為Al2O3粉末,使用純度99.9質量%以上者,對於Al2O3粉末100質量分,使用0.1~0.2質量分之MgO粉末,0.13質量分以下之MgF2粉末。
根據此氧化鋁燒結體之製法,可得到在高溫之體積電阻率或耐電壓高,每批次之這些的差異小之氧化鋁燒結體。之所以可得到如此之氧化鋁燒結體,係由於在懸浮液中,做為助燒結劑而作用之MgF2粉末與做為粒成長抑制劑而作用之MgO粉末之添加量為適當之範圍之故。若MgF2粉末過多,則粒徑變的過大而成為諸特性惡化之原因,若過少則變得難以燒結。MgO粉末若過少,則粒徑變得過大而成為諸特性惡化之原因。若MgO粉末或MgF2粉末過多,則在氧化鋁中生成導電率相對較高之異相(MgAl2O4)等,因此體積電阻率會變低。又,藉由此製法所得到之氧化鋁燒結體之在高溫之體積電阻率或耐電壓,跟批次無關而安定。特性安定,係由於採用所謂凝膠鑄造法(將懸浮液凝膠化而成形之方法),因此Al2O3粉末或MgF2粉末、MgO粉末容易均一分散之故。
又,若考慮在高溫之解吸響應性,氧化鋁燒結體,在400℃之體積電阻率在1.0×1015Ω‧cm以上,耐電壓在130kV/mm以上為佳。平均粒徑以0.5~10μm為佳。粒徑之3 σ(σ為標準差)在1~20μm為佳。做為組成,含有0.9~0.17質量%之Mg元素,0.03~0.04質量%之F元素為佳。本發明之製法,適合製造如此之氧化鋁燒結體。
1‧‧‧半導體製造裝置用構件
10‧‧‧靜電吸盤
12‧‧‧氧化鋁基板
12a‧‧‧晶圓載置面
14‧‧‧加熱電極
16‧‧‧靜電電極
18‧‧‧冷卻板
20‧‧‧冷媒通路
W‧‧‧晶圓
51‧‧‧第1成形體
52‧‧‧第2成形體
53‧‧‧第3成形體
61‧‧‧第1預燒結體
62‧‧‧第2預燒結體
63‧‧‧第3預燒結體
71‧‧‧加熱電極用糊料
72‧‧‧靜電電極用糊料
第1圖係半導體製造裝置用構件1之剖面圖。
第2圖係表示靜電吸盤10之製造程序之工程圖。
參照圖式,如以下說明本發明之較佳的實施形態。第1圖係半導體製造裝置用構件1之剖面圖。
半導體製造裝置構件1,係具有:可吸附施以電漿處理之矽製之晶圓W之靜電吸盤10,與配置在此靜電吸盤10之做為支持台之冷卻板18。
靜電吸盤10,係具有圓盤狀之氧化鋁基板12,與埋設於此氧化鋁基板12之加熱電極14及靜電電極16。氧化鋁基板12之上面,係成為晶圓載置面12a。加熱電極14,係使其佈滿氧化鋁基板12之全面而配線,例如以一筆劃圖之要領形成圖樣,若施加電壓則發熱加熱晶圓W。此加熱電極14,係鉬與氧化鋁之混合物。對於加熱器電極14,可從冷卻板18之反面,藉由分別到達加熱電極14之一端及另一端之棒狀端子(無圖示)而施加電壓。靜電電極16,係藉由無圖示之外部電源而可施加直流電壓之平面狀的電極。若對於此靜電電極16施加直流電壓,晶圓W會由於庫倫力或約翰生-拉別克效應而吸附固定在載置面12a,若解除直流電壓之施加,則晶圓W之對於晶圓載置面12a之吸附固定解除。
冷卻板18,係金屬製(例如鋁製)之圓盤構件,係介在無圖示之接合層而與靜電吸盤10之晶圓載置面12a相反側之面接合。此冷卻板18,係具有以無圖示之外部冷卻裝置所冷卻之冷媒(例如水)循環之冷媒通路20。此冷媒通路,係使冷媒可經過冷卻板18之全面而通過,例如以一筆劃圖之要領所形成。
接著,說明關於如此而構成之半導體製造裝置用構件1之使用例。半導體製造裝置用構件1,係配置於無圖示
之反應室內,藉由在此反應室內所發生之電漿而用於蝕刻晶圓W之表面。此時,藉由調節供給於加熱電極14之電力量,或是循環於冷卻板18之冷媒通路20之冷媒的流量,使晶圓W之溫度成為一定而控制。
接著,說明關於構成半導體製造裝置用構件1之靜電吸盤10之製造程序。以下,一邊說明靜電吸盤10之製造程序,一邊也說明氧化鋁基板12之製造程序。
1.成形體之製作(參照第2圖(a),本發明之工程(a)之一例)
製作第1~第3之成形體51~53。成形體51~53,首先係在分別之成形模(第1~第3之成形模)中投入含有Al2O3粉末、做為粒成長抑制劑之MgO粉末、做為助燒結劑之MgF2粉末、溶劑、分散劑及凝膠劑之懸浮液,在成形模內使凝膠劑化學反應而使懸浮液凝膠化後,藉由脫模而製作。
做為溶劑,只要可溶解分散劑及凝膠劑者,並沒有特別限定,例如,可舉出:碳氫系溶劑(甲苯、二甲苯、溶劑石腦油等);醚系溶劑(乙二醇單乙基迷、二甘醇丁醚、丁基甘醇丁醚醋酸酯等);醇系溶劑(異丙醇、1-丁醇、乙醇、2-乙基己醇、松油醇、乙二醇、甘油等);酮系溶劑(丙酮、甲基乙基酮等);酯系溶劑(醋酸丁酯、戊二酸二甲酯、三醋酸甘油酯等);多元酸系溶劑(戊二酸等)。特別是,以使用多元酸酯(例如:戊二酸二甲酯等)、多元醇之酸酯(例如:三醋酸甘油酯等)等之具有2以上之酯鍵結之溶劑為佳。
做為分散劑,只要可使Al2O3粉末在溶劑中均一地
分散者即可,並沒有特別限定。例如,可舉出聚羧酸系共聚物、聚羧酸鹽、山梨糖醇脂肪酸酯、聚甘油脂肪酸酯、磷酸酯鹽系共聚物、磺酸鹽系共聚物、具有3級胺之聚氨酯聚酯系共聚物等。特別是以使用聚羧酸系共聚物、聚羧酸鹽等為佳。藉由添加此分散劑,可使成形前之懸浮液為低黏度且為具有高濃度之物。
做為凝膠劑,可為含有異氰酸酯類、多元醇類及觸媒之物。在其中,做為異氰酸酯類,只要為具有異氰酸酯基做為官能基之物質即可而沒有特別限定,例如,可舉出甲苯二異氰酸酯(TDI)、二苯基甲烷二異氰酸酯(MDI)或是這些的變性體等。又,在分子內,也可含有異氰酸酯基以外之反應性官能基,更且,如聚異氰酸酯般,也可含有多數反應官能基。做為多元醇類,只要為具有2個以上可與異氰酸酯基反應之氫氧基之物質即可而沒有特別限定,例如,可舉出乙二醇(EG)、聚乙二醇(PEG)、丙二醇(PG)、聚丙二醇(PPG)、聚丁二醇(PTMG)、聚己二醇(PHMG)、聚乙烯醇(PVA)等。做為觸媒,只要為可促進異氰酸酯類與多元醇類之聚氨酯反應之物質即可而沒有特別限定,例如,可舉出三乙烯二胺、己二胺、6-二甲基氨基-1-己醇等。
在此工程,首先,對於Al2O3粉末與MgO粉末與MgF2粉末,依照既定比率添加溶劑及分散劑,藉由將這些混合經過既定時間,調製懸浮液前驅體,之後,對於此懸浮液前驅體,添加凝膠劑,混合‧真空脫泡而做為懸浮液為佳。Al2O3粉末,係使用純度99.9質量%以上者,對於Al2O3粉末100質量分,使用0.1~0.2質量分之MgO粉末,0.13質量分(以0.09~0.13質量分為佳)以下之MgF2粉末。調製懸浮液前驅體或懸浮液時
之混合方法,並沒有特別限定,例如可使用球磨、自公轉式攪拌、振動式攪拌、螺旋槳式攪拌等。又,對於懸浮液前驅體添加凝膠劑之懸浮液,由於隨著時間的經過,凝膠劑之化學反應(聚氨酯反應)開始進行,因此以迅速流入成形模內為佳。流入成形模內之懸浮液,會由於懸浮液所含有之凝膠劑化學反應而凝膠化。凝膠化劑之化學反應,係指異氰酸酯類與多元醇類發生聚氨酯反應而成為聚氨酯樹脂(聚氨酯)之反應。藉由凝膠劑之反應,懸浮液凝膠化,聚氨酯樹脂做為有機黏結劑作用。
2.預燒結體之製作(參照第2圖(b),本發明之工程(b)之一例)
將第1~第3之成形體51~53乾燥後脫脂,更藉由預燒結,而得到第1~第3之預燒結體61~63。成形體51~53之乾燥,係為了使含有於成形體51~53之溶劑蒸發而進行。乾燥溫度或乾燥時間,跟根據所使用之溶劑而適當設定即可。但是,乾燥溫度,須注意使乾燥中之成形體51~53不會產生裂縫而設定。又,氣氛為大氣氣氛、惰性氣氛、真空氣氛之任一種皆可。乾燥後之成形體51~53之脫脂,係為了分解‧除去分散劑或觸媒或黏結劑等之有機物而進行。脫脂溫度,可根據所含有之有機物之種類而適當設定,例如可設定在400~600℃。又,氣氛為大氣氣氛、惰性氣氛、真空氣氛之任一種皆可。脫脂後之成形體51~53之預燒結,係為了使強度變高容易操作而進行。預燒結溫度,雖沒有特別限定,例如可設定750~900℃。又,氣氛為大氣氣氛、惰性氣氛、真空氣氛之任一種皆可。
3.電極用糊料之印刷(參照第2圖(c))
在第1之預燒結體61之單面上使加熱電極用糊料71成為既定之加熱電極用圖樣印刷,在第3之預燒結體63之單面上使靜電電極用糊料72成為既定之靜電電極用圖樣印刷。兩糊料71、72,皆為含有氧化鋁粉末與鉬粉末之物。做為黏結劑,例如,可舉出纖維素系黏結劑(乙基纖維素等)或丙烯酸系(聚甲基丙烯酸甲酯等)或乙烯系黏結劑(聚乙烯醇縮丁醛等)。做為溶劑,例如,可舉出松油醇等。印刷方法,例如可舉出網版印刷法等。
4.熱壓燒成(參照第2圖(d),本發明之工程(c)之一例)
如夾住印刷後之加熱電極用糊料71般,將第1預燒結體61與第2預燒結體62重疊之同時,如夾住印刷後之靜電電極用糊料72般,將第2預燒結體62與第3預燒結體63重疊,在該狀態熱壓燒成。藉由此,加熱電極用糊料71被燒成而成為加熱電極14,靜電電極用糊料72被燒成而成為靜電電極16,各預燒結體61~63燒結一體化而成為氧化鋁基板12,可得到靜電吸盤10。在熱壓燒成,至少在最高溫度(燒成溫度),使加壓壓力為30~300kgf/cm2為佳,而以50~250kgf/cm2更佳。又,最高溫度,由於在Al2O3粉末中添加了助燒結劑之MgF2粉末,因此可設定成較不添加MgF2粉末之情況低溫(1150~1350℃)。氣氛可從大氣氣氛、惰性氣氛、真空氣氛中適當選擇。又,若將最高溫度設定成未滿1150℃,則Al2O3粉末之燒結無法充分進行而不佳,若設定超過1350℃,則氧化鋁燒結粒變得過大而諸特性惡化之故因此不佳。
在以上詳述之本實施形態,所得到之氧化鋁基板12,會成為在高溫之體積電阻率或耐電壓高之物。之所以可得
到如此之氧化鋁基板12,係由於在懸浮液中,做為助燒結劑而作用之MgF2粉末與做為粒成長抑制劑而作用之MgO粉末之添加量為適當的範圍之故。又,如此所得到之氧化與基板12之在高溫之體積電阻率或耐電壓,跟批次無關而安定。特性安定,係由於採用所謂凝膠鑄造法(將懸浮液凝膠化而成形之方法),因此Al2O3粉末或MgF2粉末、MgO粉末容易均一分散之故。
若考慮在高溫之解吸響應性,氧化鋁燒結體12,在400℃之體積電阻率在1.0×1015Ω‧cm以上,耐電壓在130kV/mm以上為佳。平均粒徑以0.5~10μm為佳。粒徑之3 σ(σ為標準差)在1~20μm為佳。做為組成,含有0.9~0.17質量%之Mg元素,0.03~0.04質量%之F元素為佳。上述之製法,適合製造如此之氧化鋁燒結體12。
又,本發明並非限定於上述實施形態,只要在屬於本發明之技術範圍內,可以各種形態實施是不在話下的。
例如,在上述實施形態,係舉例將加熱電極14與靜電電極16埋設於氧化鋁基板12之靜電吸盤10,但也可僅將加熱電極14與靜電電極16之任一方埋設於氧化鋁基板12,又也將電漿產生用之高頻電極取代這些電極或和這些電極一起埋設。
在上述實施形態,係在第1預燒結體61之單面印刷加熱電極用糊料71,在第3預燒結體63之單面印刷靜電電極用糊料72後,在將第1~第3之預燒結體61~63層積之狀態下熱壓燒成,但也可採用以下的程序。亦即,也可在第1之成形體51之單面印刷加熱電極用糊料,在第3成形體53之單面印刷靜電電極用糊料72。接著,將第1~第3成形體51~53乾
燥後脫脂,藉由更預燒結,而成為第1~第3之預燒結體,將其層積熱壓燒成。
在上述實施形態,係舉例表示靜電吸盤10之製法之一例,但也可省略加熱電極14與靜電電極16,做為沒有內藏電極之氧化鋁基板之製法。在該情況,可將3個預燒結體層積者熱壓燒成,也可僅對1個成形體乾燥‧脫脂‧預燒結後藉由熱壓燒成而製造氧化鋁基板。
[實施例]
以下,對於本發明之實施例說明。又,以下之實施例並非對本發明做任何限定。
[實驗例1]
依照上述製造程序(參照第2圖),如以下製作靜電吸盤10。
(a)成形體之製作
秤量Al2O3粉末(平均粒徑0.5μm,純度99.99%)100質量分、MgO粉末0.1質量分、MgF2粉末0.09質量分,做為分散劑之聚羧酸系共聚物3質量分,做為溶劑之多鹽基酸酯20質量分,將此以球磨(滾筒)混合14小時,做為懸浮液前驅體。對於此懸浮液前驅體,添加凝膠劑,亦即4,4’-二苯基甲烷二異氰酸酯3.3質量分做為異氰酸酯類,乙二醇0.3質量分做為多元醇類,6-二甲基氨基-1-己醇0.1質量分做為觸媒,以自公轉式攪拌機混合12分鐘,得到懸浮液。將所得到之懸浮液分別流入在實施形態1所使用之第1~第3成形模。之後,藉由在22℃放置2小時,在各成形模內使凝膠劑化學反應而使懸浮液凝膠化後脫模。藉由此,從第1~第3成形模分別得到第1~第
3之成形體51~53(參照第2圖(a))。
(b)預燒結體之製作
將第1~第3之成形體51~53在100℃乾燥10小時後,在最高溫度550℃、大氣氣氛下脫脂1小時,更在最高溫度820℃、大氣氣氛下預燒結1小時,而得到第1~第3之預燒結體61~63(參照第2圖(b))。
(c)電極用糊料之印刷
將鉬粉末與Al2O3粉末,使氧化鋁含有量成為10%質量%,藉由添加混合聚甲基丙烯酸甲酯做為黏結劑,松油醇做為溶劑,而調製電極用糊料。此電極用糊料,係使其用於靜電電極用、加熱電極用之兩方。然後,在第1預燒結體61之單面網版印刷加熱電極用糊料71,在第3預燒結體63之單面網版印刷加熱電極用糊料72(參照第2圖(c))。
(d)熱壓燒成
如夾住加熱電極用糊料71般,將第1及第2預燒結體61、62重疊之同時,如夾住靜電電極用糊料72般,將第2及第3預燒結體62、63重疊。然後,在該狀態下進行熱壓燒成。藉由此,加熱電極糊料71被燒成而成為加熱電極14,靜電電極用糊料72被燒成而成為靜電電極16,各預燒結體61~63燒結一體化而成為氧化鋁基板12(參照第2圖(d))。熱壓燒成,係在真空氣氛下,藉由在壓力250kgf/cm2,最高溫度1260℃保持2小時來進行。之後,將陶瓷燒結體表面以鑽石研磨石進行平面研磨加工,使從靜電電極16至晶圓載置面12a之厚度為350μm,從加熱電極14至另一方的表面之厚度為750μm。之後,
施以側面加工,開孔加工,進行端子的裝配,而得到內藏加熱電極14及靜電電極16之直徑300mm之靜電吸盤10。
對於所得到之靜電吸盤10中之氧化鋁基板12,測定以下的特性。其結果示於表1。又,根據特性,另外以同於試驗例1之製造程序製作氧化鋁試驗片(無電極)。
‧相對密度
假設在製造時所混合之各原料(Al2O3或MgO、MgF2)全部以該狀態存在於氧化鋁燒結體內,由各原料的理論密度與各原料的使用量(質量分)求得燒結體的理論密度。之後,以阿基米斯法所求得的體積密度除以燒結體的理論密度,將其乘以100之值做為燒結體的相對密度(%)。因此,若各原料之使用量相同,體積密度約大則相對密度愈大。
‧強度
根據JIS R1601進行4點彎曲試驗,算出強度。
‧平均粒徑及3 σ
以線性分析法求得。具體而言,係對於以電子顯微鏡觀察各燒結體之剖面而得到之SEM照片畫任意數量的線,求得平均切片長度。與線相交之粒子數愈多精密度愈高,因此該線數,雖會根據粒徑而不同。但畫約可與60個程度的粒子相交之程度的線數。由該平均切片長度推定平均粒徑。又,推定平均粒徑時所使用之各粒徑求得標準偏差σ,將其乘以3做為3 σ。
‧體積電阻率
根據JIS C2141之方法,在大氣中,在400℃測定。試驗片形狀為□50mm(50mm四方)×厚度0.2mm,使主電極成為直徑
20mm,保護電極成為內徑30mm,外徑40mm,施加電極成為直徑40mm而以銀形成各電極。施加電壓為2kV/mm,讀取電壓施加後30分時之電流值,由該電流值算出體積電阻率。又,製作5個實驗例1,求得其在400℃之體積電阻率之標準偏差。
‧耐電壓
使試驗片形狀為□50mm×厚度0.2mm。使用此,根據JIS C2110,測定耐電壓。又,製作5個實驗例1,求得其之耐電壓之標準偏差。
‧化學分析
Mg之含有量,係藉由感應耦合電漿(ICP)原子發射光質譜儀分析而求得。又,Mg含有量之測定下限為1ppm。又,F之含有量,係熱解分離-離子色譜儀法所求得(JIS R9301-3-11)。又,F含有量之測定下限為10ppm。
[實驗例2~9]
在實驗例2~9,除了使對於Al2O3粉末100質量分之MgO粉末及MgF2粉末之質量分變更如表1以外,同於實驗例1製作靜電吸盤10。又,同於實驗例1,測定實驗例2~9之氧化鋁基板12之各特性。其結果示於表1。
[實驗例10]
在實驗例10,製作沒有埋設電極氧化鋁基板。首先,將純度99.5%之Al2O3粉末與MgO粉末與CaO粉末,對於氧化鋁100質量分,使MgO粉末成為0.05質量分,CaO成為0.03質量分而混合。對於此混合粉末添加黏結劑之聚乙烯醇(PVA)、水及分散劑,以滾筒混合16小時製作懸浮液。使用噴霧乾燥機將此懸浮液噴霧乾燥,之後,在450℃保持5小時除去黏結劑,製作平均粒徑80μm之氧化鋁顆粒。將此氧化鋁顆粒充填於模具,以200kg/cm2之壓力進行加壓成形,得到成形體。接著,將此成形體設置在碳製的套筒,使用熱壓燒成法燒成。燒成係在100kg/cm2之加壓下,且在氮氣加壓氣氛(150kPa)進行,以300℃/h升溫,在1620℃保持2小時,得到氧化鋁燒結體。將此氧化鋁燒結體研磨加工,製作 300mm,厚6mm之氧化鋁基板。同於實驗例1,測定實驗例10之氧化鋁基板之各特性。其結果示於表1。
[評價]
在實驗例1、2、5、6,可得到在400℃之體積電阻率高至1.0×1015Ω‧cm以上,耐電壓高至130kV/mm以上之氧化鋁基板。又,關於實驗例1、2、5、6,製作複數個的情況,由這些
的特性的標準偏差為小的值來看,可知批次間的差異也小。氧化鋁燒結粒之平均粒徑為1~2μm,粒徑之3 σ(σ為標準差)為1~2μm。在這些的實驗例,做為Al2O3粉末,使用純度99.9質量%以上者,對於Al2O3粉末100質量分,使用0.1~0.2質量分之MgO粉末,0.13質量分以下之MgF2粉末。
另一方面,在實驗例3、4、7、8,由於助燒結劑之MgF2粉末之使用量多,因此粒成長過於進行,氧化鋁燒結粒之平均粒徑成長過大至8μm以上,在400℃之體積電阻率或耐電壓低下。又,批次間之差異也變大。
在實驗例9,由於粒成長抑制劑之MgO之使用量過多,因此氧化鋁燒結粒之平均粒徑雖小,但相對密度沒有充分增加,在400℃之體積電阻率或耐電壓低下。又,批次間的差異也變大。
在實驗例10,由成形方法並非採用凝膠鑄造法而採用加壓成形,在高溫燒成,因此在400℃之體積電阻率或耐電壓低下。又,批次間之差異也變大。氧化鋁燒結粒之平均粒徑也超過15μm,且3 σ也很大,因此可知粒度分布的範圍變大。
又,實驗例1、2、5、6相當於本發明之實施例,其他的實驗例相當於比較例。
此申請書,係以2015年3月26日申請之日本國專利申請第2015-063671號為優先權主張的基礎,藉由引用,其內容全部包含於本說明書。
[產業上之可利用性]
本發明,係可做為半導體製造裝置用構件而利用。
1‧‧‧半導體製造裝置用構件
10‧‧‧靜電吸盤
12‧‧‧氧化鋁基板
12a‧‧‧晶圓載置面
14‧‧‧加熱電極
16‧‧‧靜電電極
18‧‧‧冷卻板
20‧‧‧冷媒通路
W‧‧‧晶圓
Claims (4)
- 一種氧化鋁燒結體的製法,包含:(a)將含有Al2O3粉末、MgO粉末、MgF2粉末、溶劑、分散劑及凝膠劑之懸浮液投入成形模中,藉由在前述成形模內使前述凝膠劑化學反應而使前述懸浮液凝膠化後而得到成形體之工程;(b)藉由使該成形體乾燥後脫脂更預燒結,得到預燒結體之工程;及(c)藉由在1150~1350℃熱壓燒成前述預燒結體,得到陶瓷燒結體之工程,在前述工程(a),關於調製前述懸浮液,做為Al2O3粉末,使用純度99.9質量%以上者,對於Al2O3粉末100質量分,使用0.1~0.2質量分之MgO粉末,0.13質量分以下之MgF2粉末。
- 如申請專利範圍第1項之氧化鋁燒結體的製法,其中,在前述工程(a),使用0.09~0.13質量分之MgF2粉末。
- 一種氧化鋁燒結體,係氧化鋁燒結體,含有Mg元素0.09~0.17質量%、F元素0.03~0.04質量%,在400℃之體積電阻率為1.0×1015Ω‧cm以上,耐電壓130kV/mm以上,平均粒徑0.5~10μm,粒徑之3 σ(σ為標準差)為1~20μm。
- 如申請專利範圍第3項之氧化鋁燒結體,其中,平均粒徑為1~2μm,粒徑之3 σ(σ為標準差)為1~2μm。
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