TWI227744B - Electroconductive oxide sintered compact, sputtering target comprising the sintered compact and methods for producing them - Google Patents

Electroconductive oxide sintered compact, sputtering target comprising the sintered compact and methods for producing them Download PDF

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TWI227744B
TWI227744B TW092116229A TW92116229A TWI227744B TW I227744 B TWI227744 B TW I227744B TW 092116229 A TW092116229 A TW 092116229A TW 92116229 A TW92116229 A TW 92116229A TW I227744 B TWI227744 B TW I227744B
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sintered compact
sintered body
target
relative density
oxide sintered
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TW092116229A
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TW200402476A (en
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Ryo Suzuki
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Nikko Materials Co Ltd
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Description

1227744 玫、發明說明： [發明所屬之技術領域] 本發明係關於對DRAM、FRAM等之介電體薄膜記 十思體之電極為適宜之導電性氧化物燒結體、該燒結體 所構成之濺鍍靶及其等之製造方法。 [先前技術] 以往’在DRAM、FRAM等之介電體薄膜記憶體之 電極方面係使用Pt電極，惟受人質疑Pt電極之觸媒 作用會造成強介電體薄膜之氫惡化，乃有人提出幾種 導電性氧化物來取代此pt：電極。在此種導電性氧化 物方面，有 SrRu〇3、Srlr03、CaRu03、BaRu〇3、 Sr2Ru04 、 Sr2Ir04 等。 另一方面，在介電體材料方面係使用 PTZ(PbZrxTll-x〇3)或是 BST(BaSrTi3)，而上述導電性 氧化物對此等材料為適合之材質，且體電阻 極度受到期盼。 -故乃 但是，上面所舉出之導電性氧化物，由於皆為燒 結性不良之物’而存有燒結密度顯著不足之問題。： 此種低密度燒結體所得到之濺鍍靶，由於該靶中之氣 孔形態為開氣孔，戶斤以靶加工時會殘留切削粉等，: 利用濺鑛形成電極剌膜之際粒子的產生會顯著择 ’此為問題所在。 又，燒結密度低的濺錢歡，於製造過 A操作日矣 甚至於進行濺鍍時容易發生破裂或碎片，良 ^ 千不向， 1227744 所以量產成本居高不下 又錢鍍時無法提昇賤鑛功率 基於此種情況，乃提出 ® Γ添加燒結助劑來提昇婷 結岔度之方法。例如在日I 70 承專利特開2000-247739文 獻中，即嘗試添加〇. 〇〇 lml〜 01 0.5mol 之 Bi2〇3 來提昇 相對密度至85%〜90%。 但是， 90%以下， 該文獻雖可提升相對密度，但最大也不過 未能說可將靶密度提升至令人滿意之程度 疋以JiU主進行濺錢來形成薄膜之際仍會產生許 多的粒子’無法有效地控制品質並減少良率的下降。 [發明内容] 本毛明為了解決上述問題，乃提供一種導電性氧 化物纟7〇、、Ό體、忒燒結體所構成之賤鍍無及其等之製造 方法藉由改善Βΐ2〇3之添加量與燒結條件，來謀求
SrRu〇3系導電性氧化物燒結體之相對密度的提升，抑 制利用濺鍍形成薄膜之際所產生之粒子，來提升品質 與良率。 本發明係提供： 1 ·種$Γ^〇3系導電性氧化物燒結體，其特徵在 於，相對密度在93%以上。 2.如上述1記載之SrRU〇3系導電性氧化物燒結體 ’其中，比電阻在500 // Ωαη以下。 3·如上述1記載之SrRu〇3系導電性氧化物燒結體 1227744 ’其中，比電阻在300 " Ωε(η以下。 4.如上述1〜3中任一記載之SrRu〇3系導電性氧化 物燒結體，其中，人古β Λ ^ 3 有 Βι2〇3 〇·3m〇l〜1.2mol 。 5·如上述1〜3中任一 物燒結體，其中，含有 記載之SrRu03系導電性氧化 Bi2〇3 〇.5mol (超過）〜l.Omol 又’本發明係提供： 6· 一種SrRu〇3系導電性氧化物燒結體所構成之濺 鍍靶，其特徵在於，相對密度在93%以上。 7. 如上述6 3己載之srRu〇3系導電性氧化物燒結體 所構成之濺鍍靶，其中，比電阻在500 " Qcm以下。 8. 如上述6 5己載之SrRu〇3系導電性氧化物燒結體 所構成之濺録，其中，比電阻在3叫^以下。 9·如上述6〜8中任-記載之SrRu〇3系導電性氧化 :勿燒結體所構成之濺鍍靶，其中，含有W爪 〇.3mo1〜1·2mo1 。 1 〇 .如上述6〜8中任>Ο Π r\ γ仕δ己載之SrRu〇3系導電性氧 化物燒結體所構成之濺鍍靶，其中，含有 〇· 5mol (超過）〜1· Om〇1。 2 3 11. -種™3系導電性氧化物燒結體之製造方 其特徵在於，於製造糾u03系導電性氧化物燒結 體之際，添加Bl2〇3〇.3m〇K2mol做為燒結助劑。 12. -種SrRu〇3系導電性氧化物燒結體之製造方 1227744
法，^寺徵在於，於製造SrRu〇3系導電性氧化物燒結 體之際，添加β“〇3 0.5moI (超過)~h〇m〇"故為燒J 助劑。 几、、口 H 一種SrRu〇3系導電性氧化物燒結體之製造方 法其特徵在於，於製造SrRu〇3系導電性氧化物燒結 體之際，以燒結溫度1400〜1 700°C進行燒結。 14_如上述U或12記載之SrRu〇3系導電性氧化 ㈣結體之製造方法’其中’於製造SrRu〇3系導電性 虱化物燒結體之際，以燒結溫度1400〜170(TC進行燒 [實施方式] 本發明係關於一種做為濺鍍靶材料之可利用來形 成DRAM、FRAM等之介電體薄膜記憶體用薄膜電極之 鈣鈦礦（perovskite)型SrRu〇3系導電性氧化物，以 SrRu〇3系導電性氧化物之密度提升為目標而不斷改良 的結果，乃可得到相對密度93%以上之SrRu〇3系導電 性氧化物燒結體及濺鍍靶。本發明進一步提供該等物 質之製造方法。 本發明之SrRu〇3系導電性氧化物燒結體以及濺鍍 靶可得到比電阻500 // QCm以下、甚至是比電阻3〇〇 //Qcm以下之材料，在電極材料方面可得到良好的導 電性。若相對密度提升則比電阻有更為減少的傾向。 於習知技術中，未曾見到比電阻5〇〇/z Qcm以下 、且相對密度為93%以上之SrRu〇3系導電性氧化物， 1227744 本發明則是首先達成者。 於製造本發明之SrRu〇3系導電性氧化物燒結體之 際，燒結助劑係添加Β^〇3 0.3m〇1〜12m〇1。較佳為添 加Bi2〇3 〇.5mol (超過）〜;i.0m〇1進行燒結。藉此，於 SrRu〇3系導電性氧化物燒結體以及濺鐘靶中會含有 Βι 203 0· 3mo卜 1· 2mol、較佳為含有 Bi2〇3 〇. 5m〇1 (超過 )〜1·Omol 。 為了改善燒結性，得到高密度之SrRu〇3系導電性 氧化物燒結體’必須添加BigO3 〇· 3mol以上，更佳為 添加Bi2〇3超過0.5mol。若Β^〇3未滿〇.3mol，則無 法達成密度93%以上。 但疋’若SrRu〇3系導電性氧化物燒結體以及濺鍍 靶中之Β“〇3增加，則濺鍍膜中之Bi2〇3會增加，比電 阻有增高之傾向。又，若超過1.2m〇l，在濺鍍膜中會 出現第2層’其與BST0膜或PZT膜之界面會產生Bi 化合物，而會發生介電特性降低之問題。基於此情形 ’添加量之上限定為1· 2mol，更佳為1· Om〇1。 再者，於SrRu〇3系導電性氧化物燒結體之製造中 ’以燒結溫度14 0 0〜1 7 0 0 C進行燒結為佳。藉由將燒 結溫度定於1400°C，可更顯著地改善燒結性，可製造 高密度靶。 若燒結溫度超過1701TC，則Ru〇2之蒸發變得顯 著，會產生SqRuO4，降低導電性，所以必須設定在 1 7 0 0 °C 以下。 1227744 S r η 所得之相對密度9⑽以上之… 咖〇3系導電性氧化物燒結體乾，由 度 -呈密閉氣孔(未殘存開放氣孔）， 之卿 殘存切削粉等，以減鍍形成電 ；…會 減少粒子產生。 存胰之際，可顯著 過程==所述有減少比電阻之效果，於製造 ，可二時不會發生破裂或碎片 時可提升 +㈣生產成本’此亦為其效果。 C實施例與比較例） 以下說明實施例。又，本實施例僅為發明之一例 ’本發明不因為這些實施例而受到限制。#即，包含 本發明之技術思想所包含之其他態樣以及變形。 (貫施例1〜3、比較例1〜2 ) 以純度5Ν(99·999%)之SrC〇3粉以及純度 4Ν(99·99%)之Ru〇2粉做為起始原料，將兩粉末以莫爾 比1 ·· 1做秤取之後，以純水做為介質進行球磨混合 。將所得之漿料乾燥之後，於大氣中，以1⑽t χΐ〇 小時之條件進行熱合成，製作出SrRu〇；3單相粉末。 其次，對SrRu〇3粉末分別添加Β“〇3粉末〇(無添 加）、0.2、0.5、0.8、1·〇以及1.2莫爾％，做為個別 之減樣’將其再度以球磨機實施混合、粉碎。
將此混合漿料乾燥之後，添加有機黏合劑以單軸 加壓成形做預成形之後，以1 500kg/cm2之壓力做ciP 1227744 成形。各成形體係安置於半密閉之氧化鋁容器内，以 1 300°C (比較例 1)、1400°C (實施例 1)、1 600°C (實施 例2)、1 700°C (實施例3)、1750。(：（比較例2)進行燒 成。 燒結後，自燒結體表面去除Ru02缺陷層，測定密 度以及比電阻。其結果係示於表1。 1227744 i
Bi203 添加量(mol%) (N 〇 σί 〇 On 〇 〇\ 〇 (N 〇\ X 〇 Os 〇 〇 〇 〇\ 〇 Η 〇\ X 〇〇 o 〇 (Γ) Os 〇 Ό Ο 〇 〇\ 〇 (Τ) 〇\ 〇 ^T) o 00 00 〇 〇 in C\ 〇 〇\ 〇 (Ν 〇\ X cn o s 〇 〇 〇 〇 τ-Η 〇\ X (N 〇 X JO X § 〇 m 00 〇 in X o o un X (N X 00 ^sO X X 〇\ Ό X 相對密度(％) 比電阻判定 相對密度(％) 比電阻判定 相對密度(％) 比電阻判定 相對密度(％) 比電阻判定 相對密度(％) 比電阻判定 燒成溫度 P 1300 1400 1600 1700 1750 比較例1 實施例1 實施例2 實施例3 比較例2 l^«x^#T^§as^00T^«〇K1#H-^§GST/00e^Bq:i :wM^ltfq:i 1227744 於表1中’〇係表示比電阻3〇〇//πιΩαη以下，即使是 比較例1之燒成溫度1300。〇，當Bi2〇3之添加量多的情況 下’也可成為3 0 0 // m Ω cm以下，但是無法得到9 3 %以上之 充分的密度。 但是，實施例卜3之1400°C〜1 700°C則可得到93%以上 充分之密度。如比較例2所示般，以1 750°C之燒結溫度雖 部分可得到93%之高密度燒結體，但如上所述般，燒結溫 度旦起過1700C則Ru〇2的条發會變得顯著，會產生 Si^RuO4 k成膜性質變化，故有避免之必要。 以1 700 C燒成時之β^Ο3添加量與相對密度之關係係 如圖1所示般，相對密度在添加量0·3ιη〇1%以上時成為93% 以上’隨Βΐ2〇3添加量之增加，相對密度有上升之傾向。 又以1 7〇 〇 C燒成時之B i2〇3添加量與比電阻之關係 亦同樣示於圖1。如圖i所示般，當Bi2〇3添加量0 2m〇i% 以上’可達成比電阻3 〇 〇 # m Ω cm以下。 其次’將以1 700°C燒成之Bi 203添加量〇·2、〇·3、 〇.8moU之燒結體以機械加工製作成^〇〇_X6_t之靶。 使用所製作出之靶進行濺鍍，測定於6吋晶圓上之粒 子數。結果，尺寸〇.3//m以上之粒子分別為89、14、Μ 個。 落於本發明範圍内之靶的相對密度皆為93%以上，又 粒子數在20個以下。再者，於14〇〇t〜17〇(rc之最佳之燒 結條件之下可達成相對密度之提升。 相對於此，超出本發明範圍之密度低的靶，會產生許 13 1227744 多的粒子。 由以上可知，太又 g . ^ H , w. 么月之貝施例的優越性是很明顯的， 具有優異的特性。 發明效果^ ,4:月之相對密度93%以上之高密度訃 …燒結體I由於”之氣孔形態呈密閉氣= 存開放#ί多丨、，Μ # 山剛孔札（未殘 仔閉敌矾孔），所以靶加工時不會 形成電極：薄膜之際，可顯著減少粒子產生？ ’以濺鑛 又’局遂度無有減少比電 作時甚至於進㈣鍵時不會二於製造過程或操 良率，此為其顧著優點。再者生片’可提升製品 降低生產成本，此亦為其優異效果。 干 [圖式簡單說明] 圖1所示係以170(TC燒成時 阻及相對密度的關係圖。 ^ 3之添加量與比電
14

Claims (1)

1227744 導電性氧化 7，於製造 燒結溫度 10.如申請專利範圍第9項之由SrRu03系 物燒結體所構成之濺鍍靶之製造方法，其1 SrRu03系導電性氧化物燒結體之際，以 1 400〜1 700°C進行燒結。 拾壹、圖式： 如次頁 16
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TWI402862B (zh) * 2006-03-15 2013-07-21 Sumitomo Metal Mining Co 氧化物燒結體、其製法、使用它之透明導電膜之製法與所得到的透明導電膜

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