TWI580815B - 用於形成二氧化矽層的組成物、二氧化矽層及其製造方法以及包含二氧化矽層的電子裝置 - Google Patents

用於形成二氧化矽層的組成物、二氧化矽層及其製造方法以及包含二氧化矽層的電子裝置 Download PDF

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TWI580815B
TWI580815B TW105129013A TW105129013A TWI580815B TW I580815 B TWI580815 B TW I580815B TW 105129013 A TW105129013 A TW 105129013A TW 105129013 A TW105129013 A TW 105129013A TW I580815 B TWI580815 B TW I580815B
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composition
forming
chemical formula
cerium oxide
layer according
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TW201730372A (zh
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韓權愚
郭澤秀
盧健培
徐珍雨
沈秀姸
尹熙燦
李知虎
張俊英
黃丙奎
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三星Ｓｄｉ股份有限公司
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Description

用於形成二氧化矽層的組成物、二氧化矽層及其製造方法以及包含二氧化矽層的電子裝置
本發明涉及一種用於形成二氧化矽層的組成物，一種用於製造二氧化矽層的方法，以及一種藉由所述方法製造的二氧化矽層。
平板顯示器使用包含閘極電極、源極電極、汲極電極以及半導體的薄膜電晶體（thin film transistor，TFT）作爲切換裝置，並且配備有傳遞用於控制薄膜電晶體的掃描信號的閘極線和傳遞施加到像素電極的信號的數據線。此外，在半導體與若干電極之間形成絕緣層以將其隔開。絕緣層可爲包含矽組分的二氧化矽層。
一般來說，藉由塗佈聚矽氮烷、聚矽氧氮烷或其混合物並且將塗層轉化成氧化物膜來形成二氧化矽層，其中膜材料應確保產生較少缺陷的特徵（塗佈特性），即膜中較少粒子並且同時容易塗佈於基底上以便獲得均勻氧化物膜。
一個實施例提供用於形成二氧化矽層的組成物，其可將層中缺陷的產生降到最低並且確保塗佈特性。
另一個實施例提供一種使用用於形成二氧化矽層的組成物製造二氧化矽層的方法。
另一個實施例提供一種藉由所述方法製造的二氧化矽層。
另一個實施例提供一種電子裝置，包含所述二氧化矽層。
根據一個實施例，用於形成二氧化矽層的組成物包含含矽的聚合物，和作爲溶劑的由化學式1表示的化合物。 [化學式1] 在化學式1中， L 1和L 2獨立地是單鍵或C1到C5伸烷基， m和n獨立地是0到2範圍內的整數，以及 X 1和X 2獨立地是C1到C10烷基， 其限制條件爲當m和n都是零（0）時，X 1和X 2中的至少一個爲C3到C10異烷基或C4到C10叔烷基（tert-alkyl group）。
由化學式1表示的化合物在其結構中可包含7個到14個碳。
由化學式1表示的化合物在其結構中可包含8個到12個碳。
溶劑可包含異丁醚(isobutylether)、異戊醚(isoamylether)、雙-(2,2-二甲基丙基)-醚(bis-(2,2-dimethyl propyl)-ether)、雙-(1,1-二甲基丙基)-醚(bis-(1,1-dimethyl propyl)-ether)或其組合。
溶劑的沸點可以小於或等於200℃。
含矽聚合物可包含聚矽氮烷(polysilazane)、聚矽氧氮烷(polysiloxazane)或其組合。
按用於形成二氧化矽層的組成物的量計，含矽的聚合物可以0.1重量%到30重量%的量包含在內。
根據一個實施例，製造二氧化矽層的方法包含在基底上塗佈用於形成二氧化矽層的組成物，乾燥塗佈有用於形成二氧化矽層的組成物的基底，並且在250℃到1,000℃下固化組成物形成二氧化矽層。
固化可包含首先在250℃到1,000℃的水蒸氣氣氛下固化，並且其次在600℃到1,000℃下在氮氣氣氛下固化。
用於形成二氧化矽層的組成物的塗佈可以藉由旋塗法進行。
根據一個實施例，提供使用所述方法製造的二氧化矽層。
根據一個實施例，提供一種包含二氧化矽層的電子裝置。
根據一個實施例的用於形成二氧化矽層的組成物包含具有預定結構的化合物作爲溶劑。因此，使用用於形成二氧化矽層的組成物製造的二氧化矽層可具有均勻膜特性。
本發明的示範性實施例將在下文中進行詳細描述，並且可以容易由具有相關領域中常識的人員執行。然而，本發明可以許多不同形式實施，並且不應理解爲限於本文所闡述的示範性實施例。
如本文所用，當未另外提供定義時，術語‘取代’是指化合物的至少一個氫經選自以下的取代基置換：鹵素原子（F、Br、Cl或I）、羥基、烷氧基、硝基、氰基、氨基、疊氮基、甲脒基、肼基、亞肼基、羰基、氨甲醯基、硫醇基、酯基、羧基或其鹽、磺酸基或其鹽、磷酸或其鹽、C1到C20烷基、C2到C20烯基、C2到C20炔基、C6到C30芳基、C7到C30芳烷基、C1到C30烷氧基、C1到C20雜烷基、C2到C20雜芳基、C3到C20雜芳烷基、C3到C30環烷基、C3到C15環烯基、C6到C15環炔基、C2到C30雜環烷基以及其組合。
如本文所用，當未另外提供定義時，術語‘雜’是指包含1個到3個選自N、O、S以及P的雜原子。
另外，在說明書中，標志“＊”是指某物與相同或不同的原子或化學式連接的位置。
在下文中，描述一種根據一個實施例的用於形成二氧化矽層的組成物。
根據一個實施例的用於形成二氧化矽層的組成物包含含矽的聚合物，和作爲溶劑的由化學式1表示的化合物。 [化學式1] 在化學式1中， L 1和L 2獨立地是單鍵或C1到C5伸烷基， m和n獨立地是0到2範圍內的整數，以及 X 1和X 2獨立地是C1到C10烷基， 其限制條件爲當m和n都是零（0）時，X 1和X 2中的至少一個爲C3到C10異烷基或C4到C10叔烷基。
根據一個實施例的用於形成二氧化矽層的組成物的溶劑由化學式1表示，並且在其結構中包含一個氧且包含三種類型的原子，即氧原子、碳原子和氫原子。
由化學式1表示的化合物在結構中包含至少一個叔碳。此處，叔碳指示四個連接點中有三個連接點經除了氫以外的其它基團取代的碳。
舉例來說，在化學式1中，m和n指示位於氧原子左側和右側的-CH 3CH-部分的數目，並且-CH 3CH-部分在結構中包含一個叔碳。舉例來說，當化學式1中的m和n爲1時，由化學式1表示的化合物在氧的左側和右側分別包含一個叔碳。
在化學式1中，末端處由X 1和X 2表示的官能團爲C1到C10烷基，並且所述烷基可例如具有多種結構，例如正烷基、異烷基、仲烷基、叔烷基等。然而，當化學式1中的m和n都是0時，X 1和X 2中的至少任一個是C3到C10異烷基或C4到C10叔烷基。當X 1和X 2是C3到C10異烷基或C4到C10叔烷基時，X 1和X 2分別在結構中包含至少一個叔碳。當X 1或X 2是C3到C10異烷基時，X 1或X 2可以是例如異丙基、異丁基或異戊基，並且當X 1或X 2是C4到C10叔烷基時，X 1或X 2可以是例如（但不限於）叔丁基。
因爲半導體在較低溫度下集成，所以重要的是控制用於形成二氧化矽層的組成物中所包含的聚合物的特性以在所述低溫下形成緻密和均勻二氧化矽層。一般來說，當聚合物的重量平均分子量增加時，聚合物具有較大吸濕性，並且因此可以在低溫下形成相對緻密二氧化矽層。然而，當聚合物的重量平均分子量增加時，可以從旋塗器的噴嘴尖端產生更多粒子。因此，重要的是選擇用於形成二氧化矽層的組成物中所用的溶劑。
根據一個實施例，用於形成二氧化矽層的組成物包含具有化學式1的結構的化合物作爲溶劑，並且因此可確保與底層的親和力並且可以控制缺陷（例如空隙或電洞缺陷）的產生。爲了確保與底層的親和力，可使用具有氧原子的溶劑，但溶劑中的氧原子與空氣中的水分具有相對足夠反應性並且因此可吸收相對更多水分。因此，根據一個實施例的用於形成二氧化矽層的組成物使用例如異烷基、叔烷基等溶劑由於位阻而抵消氧原子與空氣中的水分的反應。
舉例來說，表示化學式1中的連接基團的L 1和L 2可以獨立地是單鍵（即直接鍵）或C1到C2伸烷基。
由化學式1表示的化合物可具有中心是氧的對稱結構或不對稱結構。舉例來說，由化學式1表示的化合物在結構中可以例如包含7個到14個碳和例如8個到12個碳。當碳的數目超出所述範圍時，層可能具有缺陷，但當碳的數目在所述範圍內時，溶劑可能更具揮發性並且在薄膜形成期間引起塗佈問題。
舉例來說，溶劑可以包含（但不限於）異丁醚、異戊醚、雙-(2,2-二甲基丙基)-醚（雙-(2,2-二甲基丙基)-醚）、雙-(1,1-二甲基丙基)-醚（雙-(1,1-二甲基丙基)-醚）或其組合。
舉例來說，溶劑的沸點可以小於或等於200℃，例如（但不限於）90℃到190℃範圍。
溶劑在室溫下可以液體形式存在，例如由化學式1本身表示的碳化合物、超過兩種由化學式1表示的化合物的混合物或由化學式1表示的化合物與其它組分的混合物。
下文中，描述用於形成二氧化矽層的組成物的含矽的聚合物。
含矽的聚合物包含聚矽氮烷、聚矽氧氮烷或其組合，並且可具有例如1,000到100,000的重量平均分子量。
含矽的聚合物可包含例如由化學式A表示的部分。 [化學式A] 在化學式A中，R 1到R 3獨立地是氫、經取代或未經取代的C1到C30烷基、經取代或未經取代的C3到C30環烷基、經取代或未經取代的C6到C30芳基、經取代或未經取代的C7到C30芳基烷基、經取代或未經取代的C1到C30雜烷基、經取代或未經取代的C2到C30雜環烷基、經取代或未經取代的C2到C30烯基、經取代或未經取代的烷氧基、羧基、醛基、羥基或其組合，以及
“*”表示連接點。
舉例來說，含矽的聚合物是藉由使鹵代矽烷(halosilane)與氨反應產生的聚矽氮烷。
舉例來說，除了由化學式A表示的部分之外，用於形成二氧化矽層的組成物中所包含的含矽的聚合物可以更包含由化學式B表示的部分。 [化學式B]
在化學式B中，R 4到R 7獨立地是氫、經取代或未經取代的C1到C30烷基、經取代或未經取代的C3到C30環烷基、經取代或未經取代的C6到C30芳基、經取代或未經取代的C7到C30芳基烷基、經取代或未經取代的C1到C30雜烷基、經取代或未經取代的C2到C30雜環烷基、經取代或未經取代的C2到C30烯基、經取代或未經取代的烷氧基、羧基、醛基、羥基或其組合，以及
“*”表示連接點。
在這一情形下，除了矽-氮（Si-N）結合部分之外，含矽的聚合物在其結構中包含矽-氧-矽（Si-O-Si）結合部分，並且由此矽-氧-矽（Si-O-Si）結合部分可減弱藉由熱處理和縮減收縮固化期間的應力。
舉例來說，含矽的聚合物包含由化學式A表示的部分和由化學式B表示的部分，並且可以更包含由化學式C表示的部分。 [化學式C]
由化學式C表示的部分具有末端用氫封端的結構，並且按聚矽氮烷或聚矽氧氮烷結構的Si-H鍵的總量計，可以15重量%到35重量%的量包含在內。當化學式C的部分在所述範圍內包含於聚矽氮烷或聚矽氧氮烷結構中時，會防止SiH 3部分分散到SiH 4，同時在熱處理期間充分進行氧化反應，並且可以防止填料圖案中出現裂紋。
舉例來說，按用於形成二氧化矽層的組成物的總量計，所述含矽的聚合物可以0.1重量%到30重量%的量包含在內。
用於形成二氧化矽層的組成物可以更包含熱酸產生劑（thermal acid generator，TAG）。
熱酸產生劑可以是改善用於形成二氧化矽層的組成物的顯影特性的添加劑，並且由此使得所述組成物的聚合物在相對低溫度下顯影。
如果所述熱酸產生劑藉由加熱產生酸（H +），那麽其可以包含任何化合物而不受特定限制。具體來說，其可以包含在90℃或高於90℃下活化並且產生足夠酸並且還具有低揮發性的化合物。
熱酸產生劑可以例如選自甲苯磺酸硝基苯甲酯（nitrobenzyl tosylate）、苯磺酸硝基苯甲酯（nitrobenzyl benzenesulfonate）、苯酚磺酸酯（phenol sulfonate）以及其組合。
按用於形成二氧化矽層的組成物的總量計，熱酸產生劑可以0.01重量%到25重量%的量包含在內。在所述範圍內，聚合物可以在低溫下顯影並且同時具有改善的塗佈特性。
用於形成二氧化矽層的組成物可更包含表面活性劑。
表面活性劑不受特定限制，並且可能是例如非離子表面活性劑，例如聚氧乙烯烷基醚，例如聚氧乙烯月桂基醚、聚氧乙烯硬脂基醚、聚氧乙烯鯨蠟基醚、聚氧乙烯油醇醚等；聚氧乙烯烷基烯丙基醚，例如聚氧乙烯壬基酚醚等；聚氧乙烯·聚氧丙烯嵌段共聚物；聚氧乙烯脫水山梨醇脂肪酸酯，例如脫水山梨醇單月桂酸酯、脫水山梨糖醇單棕櫚酸酯、脫水山梨糖醇單硬脂酸酯、脫水山梨糖醇單油酸酯、聚氧乙烯脫水山梨糖醇單硬脂酸酯、聚氧乙烯脫水山梨糖醇三油酸酯、聚氧乙烯脫水山梨糖醇三硬酯酸酯等；EFTOP EF301、EFTOP EF303、EFTOP EF352的氟類表面活性劑（托化工製品有限公司（Tochem Products Co., Ltd.））、麥格菲斯F171（MEGAFACE F171）、麥格菲斯F173（大日本油墨和化學有限公司（Dainippon Ink & Chem., Inc.））、氟羅拉FC430（FLUORAD FC430）、氟羅拉FC431（住友3M（Sumitomo 3M））、朝日防護AG710（Asahi guardAG710）、索龍S-382（Surflon S-382）、索龍SC101、索龍SC102、索龍SC103、索龍SC104、索龍SC105、索龍SC106（朝日玻璃有限公司（Asahi Glass Co., Ltd.））等；其它矽酮類表面活性劑，例如有機矽氧烷聚合物KP341（信越化學有限公司（Shin-Etsu Chemical Co., Ltd.））等。
按用於形成二氧化矽層的組成物的總量計，表面活性劑可以0.001重量%到10重量%的量包含在內。在所述範圍內，可以改善溶液的分散性，並且同時可以改善層的均勻厚度。
根據另一實施例，用於製造二氧化矽層的方法包含塗佈用於形成二氧化矽層的組成物，乾燥塗佈有組成物的基底以形成二氧化矽層，並且固化用於形成二氧化矽層的組成物。
用於形成二氧化矽層的組成物可以經例如旋塗、狹縫塗佈、噴墨印刷等溶液法進行塗佈。
基底可以是例如裝置基底，例如（但不限於）半導體、液晶等。
當用於形成二氧化矽層的組成物完成塗佈時，隨後將基底乾燥並且固化。乾燥和固化可以例如在大於或等於100℃下藉由施加例如能量（例如熱、紫外光（UV）、微波、聲波、超聲波等）進行。
舉例來說，可以在100℃到200℃下進行乾燥，並且可以藉由乾燥從用於形成二氧化矽層的組成物去除溶劑。另外，固化可以在250℃到1,000℃下進行，並且藉由固化，用於形成二氧化矽層的組成物可以轉化成薄氧化物膜。固化可以首先例如在250℃到1,000℃下在水蒸氣氣氛下進行，並且其次在600℃到1,000℃下在氮氣氣氛下進行。
根據另一實施例，提供一種包含根據所述方法製造的二氧化矽層的電子裝置。二氧化矽層可以是（但不限於）例如絕緣層、分離層或保護層，例如硬塗層。
根據另一實施例，提供一種包含由上述方法製造的二氧化矽層的電子裝置。電子裝置可以是例如顯示裝置，例如LCD或LED；或半導體裝置。
以下實例更詳細地說明本發明的實施例。然而，這些實例是示範性的，並且本發明並不限於此。
製備用於形成二氧化矽層的組成物
聚合實例 1 ： 合成聚矽氮烷
配備有攪拌器和溫度控制器的2升反應器內部用乾燥氮氣替代。隨後，將1,500克乾燥吡啶注入其中，充分混合，並且在20℃下保溫。隨後，歷經一小時將100克二氯矽烷緩慢注入其中。接著，將70克氨氣經3小時緩慢注入其中。隨後，將乾燥氮氣注入其中持續30分鐘，並且去除反應器中剩餘的氨氣。在乾燥氮氣氣氛下，通過1微米鐵氟龍過濾器（Teflon filter）過濾白色漿料相產物，獲得1,000克過濾溶液。接著，向其中添加1,000克無水二甲苯，並且藉由使用旋轉蒸發器總共重複三次用吡啶代替二甲苯將混合物調整到具有20重量%的固體濃度，並且接著使用孔徑爲0.03微米的鐵氟龍過濾器過濾。獲得的聚矽氮烷的氧含量爲3.8%，SiH 3/SiH（總）爲0.22，並且重量平均分子量爲4,000。
製備用於形成二氧化矽層的組成物
實例 1
根據聚合實例1的聚矽氮烷與異戊醚溶劑混合以製備固體含量15±0.1重量%的用於形成二氧化矽層的組成物。
實例 2
根據與實例1相同的方法製備用於形成二氧化矽層的組成物，但使用混合溶劑二丁醚和異戊醚（體積比=50:50）代替異戊醚。
實例 3
用於形成二氧化矽層的組成物根據與實例1相同的方法製備，但使用異丁醚作爲溶劑。
實例 4
用於形成二氧化矽層的組成物根據與實例1相同的方法製備，但使用雙-(2,2二甲基丙基)醚作爲溶劑。
比較例 1
用於形成二氧化矽層的組成物根據與實例1相同的方法製備，但使用二丙醚作爲溶劑。
比較例 2
用於形成二氧化矽層的組成物根據與實例1相同的方法製備，但使用二甲苯作爲溶劑。
比較例 3
用於形成二氧化矽層的組成物根據與實例1相同的方法製備，但使用二丁醚作爲溶劑。
評估 1 ：溶劑的吸濕性
評估實例1到實例4和比較例1到比較例3中所用的各溶劑的吸濕性。
在23℃±2℃下，在40%±10%相對濕度下，根據計算等式1評估實例1到實例4和比較例1到比較例3中所用的各溶劑的吸濕性。 [計算等式1] 溶劑的吸濕性= (靜置12小時時溶劑中吸附的水分重量) / (靜置12小時時二甲苯中吸附的水分重量)
參考比較例2中所用的二甲苯溶劑（二甲苯的吸濕性=1.0），使用計算等式1評估各溶劑的相對吸濕性。
評估 2 ： 薄膜的電洞缺陷
從旋轉器的噴嘴尖端施配3毫升根據實例1到實例4和比較例1到比較例3的各用於形成二氧化矽層的組成物，並且使用旋塗器（K-SPIN8設備）以1,500轉/分鐘在直徑爲8英寸的圖案化矽晶圓的中心旋塗。在150℃下預烘烤經塗佈的薄膜。隨後，在300℃下在供應水蒸氣的鍋爐中固化經塗佈的薄膜並且轉化成氧化物膜。接著，藉由蝕刻去除大於或等於1,000埃的氧化物膜，並且藉由使用缺陷檢查（KLA Tencor）設備計數薄膜中以凹陷或凸出盤（直徑：大於或等於50納米）形式存在的電洞缺陷的數目。
評估1到評估2的結果提供於表1中。 [表1] <TABLE border="1" borderColor="#000000" width="85%"><TBODY><tr><td> </td><td> 比較例1 </td><td> 比較例2 </td><td> 比較例3 </td><td> 實例1 </td><td> 實例2 </td><td> 實例3 </td><td> 實例4 </td></tr><tr><td> 溶劑的吸濕性 </td><td> 7.4 </td><td> 1.0 （參考） </td><td> 4.5 </td><td> 2.0 </td><td> 3.4 </td><td> 2.3 </td><td> 1.9 </td></tr><tr><td> 電洞缺陷數目 </td><td> 104 </td><td> 247 </td><td> 85 </td><td> 91 </td><td> 87 </td><td> 94 </td><td> 89 </td></tr></TBODY></TABLE>
參看表1，相較於比較例1到比較例3中所用溶劑的吸濕性，顯示實例1到實例4中所用的溶劑的吸濕性相對小。
另外，參看表1，當在評估2中測量時，顯示根據實例1到實例4的用於形成二氧化矽層的組成物的電洞缺陷數目比根據比較例1到比較例3的用於形成二氧化矽層的組成物的電洞缺陷數目少。
雖然已經結合目前視爲實用示範性實施例的內容來描述本發明，但應理解本發明不限於所披露的實施例，而是相反，本發明旨在涵蓋包含在所附申請專利範圍的精神和範圍內的各種修改和等效配置。
無。

Claims (12)

  1. 一種用於形成二氧化矽層的組成物，包括： 含矽的聚合物，以及 作爲溶劑的由化學式1表示的化合物： [化學式1] 其中在化學式1中， L 1和L 2獨立地是單鍵或C1到C5伸烷基， m和n獨立地是0到2範圍內的整數，以及 X 1和X 2獨立地是C1到C10烷基， 其限制條件爲當m和n都是零時，X 1和X 2中的至少一個爲C3到C10異烷基或C4到C10叔烷基。
  2. 如申請專利範圍第1項所述的用於形成二氧化矽層的組成物，其中所述由化學式1表示的化合物在其結構中包含7個到14個碳。
  3. 如申請專利範圍第2項所述的用於形成二氧化矽層的組成物，其中所述由化學式1表示的化合物在其結構中包含8個到12個碳。
  4. 如申請專利範圍第1項所述的用於形成二氧化矽層的組成物，其中所述溶劑包含異丁醚、異戊醚、雙-(2,2-二甲基丙基)-醚、雙-(1,1-二甲基丙基)-醚或其組合。
  5. 如申請專利範圍第1項所述的用於形成二氧化矽層的組成物，其中所述溶劑的沸點小於或等於200℃。
  6. 如申請專利範圍第1項所述的用於形成二氧化矽層的組成物，其中所述含矽的聚合物包含聚矽氮烷、聚矽氧氮烷或其組合。
  7. 如申請專利範圍第1項所述的用於形成二氧化矽層的組成物，其中按所述用於形成二氧化矽層的組成物的量計，所述含矽的聚合物以0.1重量%到30重量%的量包含在內。
  8. 一種製造二氧化矽層的方法，包括： 將如申請專利範圍第1項到第7項中的一項所述的用於形成二氧化矽層的組成物塗佈於基底上， 乾燥塗佈有所述用於形成二氧化矽層的組成物的所述基底，以及 在250℃到1,000℃下固化所述用於形成二氧化矽層的組成物。
  9. 如申請專利範圍第8項所述的製造二氧化矽層的方法，其中所述固化包含首先在250℃到1,000℃的水蒸氣氣氛下固化，其次在600℃到1,000℃的氮氣氣氛下固化。
  10. 如申請專利範圍第8項所述的製造二氧化矽層的方法，其中藉由旋塗法進行所述用於形成二氧化矽層的組成物的塗佈。
  11. 一種二氧化矽層，所述二氧化矽層如申請專利範圍第8項所述的製造二氧化矽層的方法製造。
  12. 一種電子裝置，所述電子裝置包括如申請專利範圍第11項所述的二氧化矽層。
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