CN107129757A - 用于形成二氧化硅层的组成物、二氧化硅层及其制造方法以及包含二氧化硅层的电子装置 - Google Patents

用于形成二氧化硅层的组成物、二氧化硅层及其制造方法以及包含二氧化硅层的电子装置 Download PDF

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CN107129757A
CN107129757A CN201610835603.2A CN201610835603A CN107129757A CN 107129757 A CN107129757 A CN 107129757A CN 201610835603 A CN201610835603 A CN 201610835603A CN 107129757 A CN107129757 A CN 107129757A
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silicon dioxide
dioxide layer
constituent
chemical formula
solvent
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CN107129757B (zh
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韩权愚
郭泽秀
卢健培
徐珍雨
沈秀姸
尹熙灿
李知虎
张俊英
黄丙奎
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Samsung SDI Co Ltd
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Samsung SDI Co Ltd
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Abstract

本发明提供一种用于形成二氧化硅层的组成物、二氧化硅层及其制造方法以及包含二氧化硅层的电子装置。用于形成二氧化硅层的组成物包含含硅的聚合物和作为溶剂的由化学式1表示的化合物。在化学式1中，L1、L2、m、n、X1以及X2与说明书中所定义相同。本发明可将二氧化硅层中缺陷的产生降到最低并且确保涂布特性。

Description

用于形成二氧化硅层的组成物、二氧化硅层及其制造方法以 及包含二氧化硅层的电子装置
相关申请案的交叉引用
本申请要求2016年2月26日在韩国知识产权局提交的韩国专利申请第10-2016-0023589号的优先权和权益，其全部内容以引用的方式并入本文中。
技术领域
本发明涉及一种用于形成二氧化硅层的组成物，一种用于制造二氧化硅层的方法，以及一种通过所述方法制造的二氧化硅层。
背景技术
平板显示器使用包含栅极电极、源极电极、漏极电极以及半导体的薄膜晶体管(thin film transistor，TFT)作为切换装置，并且配备有传递用于控制薄膜晶体管的扫描信号的栅极线和传递施加到像素电极的信号的数据线。此外，在半导体与若干电极之间形成绝缘层以将其隔开。绝缘层可为包含硅组分的二氧化硅层。
一般来说，通过涂布聚硅氮烷、聚硅氧氮烷或其混合物并且将涂层转化成氧化物膜来形成二氧化硅层，其中膜材料应确保产生较少缺陷的特征(涂布特性)，即膜中较少粒子并且同时容易涂布于衬底上以便获得均匀氧化物膜。
发明内容
一个实施例提供用于形成二氧化硅层的组成物，其可将层中缺陷的产生降到最低并且确保涂布特性。
另一个实施例提供一种使用用于形成二氧化硅层的组成物制造二氧化硅层的方法。
另一个实施例提供一种通过所述方法制造的二氧化硅层。
另一个实施例提供一种电子装置，包含所述二氧化硅层。
根据一个实施例，用于形成二氧化硅层的组成物包含含硅的聚合物，和作为溶剂的由化学式1表示的化合物。
[化学式1]
在化学式1中，
L1和L2独立地是单键或C1到C5亚烷基，
m和n独立地是0到2范围内的整数，以及
X1和X2独立地是C1到C10烷基，
其限制条件为当m和n都是零(0)时，X1和X2中的至少一个为C3到C10异烷基或C4到C10叔烷基(tert-alkyl group)。
由化学式1表示的化合物在其结构中可包含7个到14个碳。
由化学式1表示的化合物在其结构中可包含8个到12个碳。
溶剂可包含异丁醚(isobutylether)、异戊醚(isoamylether)、双-(2，2-二甲基丙基)-醚(bis-(2，2-dimethyl propyl)-ether)、双-(1，1-二甲基丙基)-醚(bis-(1，1-dimethyl propyl)-ether)或其组合。
溶剂的沸点可以小于或等于200℃。
含硅聚合物可包含聚硅氮烷(polysilazane)、聚硅氧氮烷(polysiloxazane)或其组合。
按用于形成二氧化硅层的组成物的量计，含硅的聚合物可以0.1重量％到30重量％的量包含在内。
根据一个实施例，制造二氧化硅层的方法包含在衬底上涂布用于形成二氧化硅层的组成物，干燥涂布有用于形成二氧化硅层的组成物的衬底，并且在250℃到1,000℃下固化组成物形成二氧化硅层。
固化可包含首先在250℃到1,000℃的水蒸气气氛下固化，并且其次在600℃到1,000℃下在氮气气氛下固化。
用于形成二氧化硅层的组成物的涂布可以通过旋涂法进行。
根据一个实施例，提供使用所述方法制造的二氧化硅层。
根据一个实施例，提供一种包含二氧化硅层的电子装置。
根据一个实施例的用于形成二氧化硅层的组成物包含具有预定结构的化合物作为溶剂。因此，使用用于形成二氧化硅层的组成物制造的二氧化硅层可具有均匀膜特性。
具体实施方式
本发明的示范性实施例将在下文中进行详细描述，并且可以容易由具有相关领域中常识的人员执行。然而，本发明可以许多不同形式实施，并且不应理解为限于本文所阐述的示范性实施例。
如本文所用，当未另外提供定义时，术语‘取代’是指化合物的至少一个氢经选自以下的取代基置换：卤素原子(F、Br、Cl或I)、羟基、烷氧基、硝基、氰基、氨基、叠氮基、甲脒基、肼基、亚肼基、羰基、氨甲酰基、硫醇基、酯基、羧基或其盐、磺酸基或其盐、磷酸或其盐、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杂烷基、C2到C20杂芳基、C3到C20杂芳烷基、C3到C30环烷基、C3到C15环烯基、C6到C15环炔基、C2到C30杂环烷基以及其组合。
如本文所用，当未另外提供定义时，术语‘杂’是指包含1个到3个选自N、O、S以及P的杂原子。
另外，在说明书中，标志“＊”是指某物与相同或不同的原子或化学式连接的位置。
在下文中，描述一种根据一个实施例的用于形成二氧化硅层的组成物。
根据一个实施例的用于形成二氧化硅层的组成物包含含硅的聚合物，和作为溶剂的由化学式1表示的化合物。
[化学式1]
在化学式1中，
L1和L2独立地是单键或C1到C5亚烷基，
m和n独立地是0到2范围内的整数，以及
X1和X2独立地是C1到C10烷基，
其限制条件为当m和n都是零(0)时，X1和X2中的至少一个为C3到C10异烷基或C4到C10叔烷基。
根据一个实施例的用于形成二氧化硅层的组成物的溶剂由化学式1表示，并且在其结构中包含一个氧且包含三种类型的原子，即氧原子、碳原子和氢原子。
由化学式1表示的化合物在结构中包含至少一个叔碳。此处，叔碳指示四个连接点中有三个连接点经除了氢以外的其它基团取代的碳。
举例来说，在化学式1中，m和n指示位于氧原子左侧和右侧的-CH3CH-部分的数目，并且-CH3CH-部分在结构中包含一个叔碳。举例来说，当化学式1中的m和n为1时，由化学式1表示的化合物在氧的左侧和右侧分别包含一个叔碳。
在化学式1中，末端处由X1和X2表示的官能团为C1到C10烷基，并且所述烷基可例如具有多种结构，例如正烷基、异烷基、仲烷基、叔烷基等。然而，当化学式1中的m和n都是0时，X1和X2中的至少任一个是C3到C10异烷基或C4到C10叔烷基。当X1和X2是C3到C10异烷基或C4到C10叔烷基时，X1和X2分别在结构中包含至少一个叔碳。当X1或X2是C3到C10异烷基时，X1或X2可以是例如异丙基、异丁基或异戊基，并且当X1或X2是C4到C10叔烷基时，X1或X2可以是例如(但不限于)叔丁基。
因为半导体在较低温度下集成，所以重要的是控制用于形成二氧化硅层的组成物中所包含的聚合物的特性以在所述低温下形成致密和均匀二氧化硅层。一般来说，当聚合物的重量平均分子量增加时，聚合物具有较大吸湿性，并且因此可以在低温下形成相对致密二氧化硅层。然而，当聚合物的重量平均分子量增加时，可以从旋涂器的喷嘴尖端产生更多粒子。因此，重要的是选择用于形成二氧化硅层的组成物中所用的溶剂。
根据一个实施例，用于形成二氧化硅层的组成物包含具有化学式1的结构的化合物作为溶剂，并且因此可确保与底层的亲和力并且可以控制缺陷(例如空隙或空穴缺陷)的产生。为了确保与底层的亲和力，可使用具有氧原子的溶剂，但溶剂中的氧原子与空气中的水分具有相对足够反应性并且因此可吸收相对更多水分。因此，根据一个实施例的用于形成二氧化硅层的组成物使用例如异烷基、叔烷基等溶剂由于位阻而抵消氧原子与空气中的水分的反应。
举例来说，表示化学式1中的连接基团的L1和L2可以独立地是单键(即直接键)或C1到C2亚烷基。
由化学式1表示的化合物可具有中心是氧的对称结构或不对称结构。举例来说，由化学式1表示的化合物在结构中可以例如包含7个到14个碳和例如8个到12个碳。当碳的数目超出所述范围时，层可能具有缺陷，但当碳的数目在所述范围内时，溶剂可能更具挥发性并且在薄膜形成期间引起涂布问题。
举例来说，溶剂可以包含(但不限于)异丁醚、异戊醚、双-(2，2-二甲基丙基)-醚(bis-(2，2-dimethyl propyl)-ether)、双-(1，1-二甲基丙基)-醚(bis-(1，1-dimethylpropyl)-ether)或其组合。
举例来说，溶剂的沸点可以小于或等于200℃，例如(但不限于)90℃到190℃范围。
溶剂在室温下可以液体形式存在，例如由化学式1本身表示的碳化合物、超过两种由化学式1表示的化合物的混合物或由化学式1表示的化合物与其它组分的混合物。
下文中，描述用于形成二氧化硅层的组成物的含硅的聚合物。
含硅的聚合物包含聚硅氮烷、聚硅氧氮烷或其组合，并且可具有例如1,000到100,000的重量平均分子量。
含硅的聚合物可包含例如由化学式A表示的部分。
[化学式A]
在化学式A中，R1到R3独立地是氢、经取代或未经取代的C1到C30烷基、经取代或未经取代的C3到C30环烷基、经取代或未经取代的C6到C30芳基、经取代或未经取代的C7到C30芳基烷基、经取代或未经取代的C1到C30杂烷基、经取代或未经取代的C2到C30杂环烷基、经取代或未经取代的C2到C30烯基、经取代或未经取代的烷氧基、羧基、醛基、羟基或其组合，以及
“*”表示连接点。
举例来说，含硅的聚合物是通过使卤代硅烷(halosilane)与氨反应产生的聚硅氮烷。
举例来说，除了由化学式A表示的部分之外，用于形成二氧化硅层的组成物中所包含的含硅的聚合物可以更包含由化学式B表示的部分。
[化学式B]
在化学式B中，R4到R7独立地是氢、经取代或未经取代的C1到C30烷基、经取代或未经取代的C3到C30环烷基、经取代或未经取代的C6到C30芳基、经取代或未经取代的C7到C30芳基烷基、经取代或未经取代的C1到C30杂烷基、经取代或未经取代的C2到C30杂环烷基、经取代或未经取代的C2到C30烯基、经取代或未经取代的烷氧基、羧基、醛基、羟基或其组合，以及
“*”表示连接点。
在这一情形下，除了硅-氮(Si-N)结合部分之外，含硅的聚合物在其结构中包含硅-氧-硅(Si-O-Si)结合部分，并且由此硅-氧-硅(Si-O-Si)结合部分可减弱通过热处理和缩减收缩固化期间的应力。
举例来说，含硅的聚合物包含由化学式A表示的部分和由化学式B表示的部分，并且可以更包含由化学式C表示的部分。
[化学式C]
*-SiH3
由化学式C表示的部分具有末端用氢封端的结构，并且按聚硅氮烷或聚硅氧氮烷结构的Si-H键的总量计，可以15重量％到35重量％的量包含在内。当化学式C的部分在所述范围内包含于聚硅氮烷或聚硅氧氮烷结构中时，会防止SiH3部分分散到SiH4，同时在热处理期间充分进行氧化反应，并且可以防止填料图案中出现裂纹。
举例来说，按用于形成二氧化硅层的组成物的总量计，所述含硅的聚合物可以0.1重量％到30重量％的量包含在内。
用于形成二氧化硅层的组成物可以更包含热酸产生剂(thermal acidgenerator，TAG)。
热酸产生剂可以是改善用于形成二氧化硅层的组成物的显影特性的添加剂，并且由此使得所述组成物的聚合物在相对低温度下显影。
如果所述热酸产生剂通过加热产生酸(H+)，那么其可以包含任何化合物而不受特定限制。具体来说，其可以包含在90℃或高于90℃下活化并且产生足够酸并且还具有低挥发性的化合物。
热酸产生剂可以例如选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)以及其组合。
按用于形成二氧化硅层的组成物的总量计，热酸产生剂可以0.01重量％到25重量％的量包含在内。在所述范围内，聚合物可以在低温下显影并且同时具有改善的涂布特性。
用于形成二氧化硅层的组成物可还包含表面活性剂。
表面活性剂不受特定限制，并且可能是例如非离子表面活性剂，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、聚氧乙烯鲸蜡基醚、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；聚氧乙烯脱水山梨醇脂肪酸酯，例如脱水山梨醇单月桂酸酯、脱水山梨糖醇单棕榈酸酯、脱水山梨糖醇单硬脂酸酯、脱水山梨糖醇单油酸酯、聚氧乙烯脱水山梨糖醇单硬脂酸酯、聚氧乙烯脱水山梨糖醇三油酸酯、聚氧乙烯脱水山梨糖醇三硬酯酸酯等；EFTOP EF301、EFTOPEF303、EFTOP EF352的氟类表面活性剂(托化工制品有限公司(Tochem Products Co.，Ltd.))、麦格菲斯孔71(MEGAFACEF171)、麦格菲斯F173(大日本油墨和化学有限公司(Dainippon Ink&Chem.，Inc.))、氟罗拉FC430(FLUORAD FC430)、氟罗拉FC431(住友3M(Sumitomo 3M))、朝日防护AG710(Asahi guardAG710)、索龙S-382(Surflon S-382)、索龙SC101、索龙SC102、索龙SC103、索龙SC104、索龙SC105、索龙SC106(朝日玻璃有限公司(Asahi Glass Co.，Ltd.))等；其它硅酮类表面活性剂，例如有机硅氧烷聚合物KP341(信越化学有限公司(Shin-Etsu Chemical Co.，Ltd.))等。
按用于形成二氧化硅层的组成物的总量计，表面活性剂可以0.001重量％到10重量％的量包含在内。在所述范围内，可以改善溶液的分散性，并且同时可以改善层的均匀厚度。
根据另一实施例，用于制造二氧化硅层的方法包含涂布用于形成二氧化硅层的组成物，干燥涂布有组成物的衬底以形成二氧化硅层，并且固化用于形成二氧化硅层的组成物。
用于形成二氧化硅层的组成物可以经例如旋涂、狭缝涂布、喷墨印刷等溶液法进行涂布。
衬底可以是例如装置衬底，例如(但不限于)半导体、液晶等。
当用于形成二氧化硅层的组成物完成涂布时，随后将衬底干燥并且固化。干燥和固化可以例如在大于或等于100℃下通过施加例如能量(例如热、紫外光(UV)、微波、声波、超声波等)进行。
举例来说，可以在100℃到200℃下进行干燥，并且可以通过干燥从用于形成二氧化硅层的组成物去除溶剂。另外，固化可以在250℃到1,000℃下进行，并且通过固化，用于形成二氧化硅层的组成物可以转化成薄氧化物膜。固化可以首先例如在250℃到1,000℃下在水蒸气气氛下进行，并且其次在600℃到1,000℃下在氮气气氛下进行。
根据另一实施例，提供一种包含根据所述方法制造的二氧化硅层的电子装置。二氧化硅层可以是(但不限于)例如绝缘层、分离层或保护层，例如硬涂层。
根据另一实施例，提供一种包含由上述方法制造的二氧化硅层的电子装置。电子装置可以是例如显示装置，例如LCD或LED；或半导体装置。
以下实例更详细地说明本发明的实施例。然而，这些实例是示范性的，并且本发明并不限于此。
制备用于形成二氧化硅层的组成物
聚合实例1：合成聚硅氮烷
配备有搅拌器和温度控制器的2升反应器内部用干燥氮气替代。随后，将1,500克干燥吡啶注入其中，充分混合，并且在20℃下保温。随后，历经一小时将100克二氯硅烷缓慢注入其中。接着，将70克氨气经3小时缓慢注入其中。随后，将干燥氮气注入其中持续30分钟，并且去除反应器中剩余的氨气。在干燥氮气气氛下，通过1微米铁氟龙过滤器(Teflonfilter)过滤白色浆料相产物，获得1,000克过滤溶液。接着，向其中添加1,000克无水二甲苯，并且通过使用旋转蒸发器总共重复三次用吡啶代替二甲苯将混合物调整到具有20重量％的固体浓度，并且接着使用孔径为0.03微米的铁氟龙过滤器过滤。获得的聚硅氮烷的氧含量为3.8％，SiH3/SiH(总)为0.22，并且重量平均分子量为4,000。
制备用于形成二氧化硅层的组成物
实例1
根据聚合实例1的聚硅氮烷与异戊醚溶剂混合以制备固体含量15±0.1重量％的用于形成二氧化硅层的组成物。
实例2
根据与实例1相同的方法制备用于形成二氧化硅层的组成物，但使用混合溶剂二丁醚和异戊醚(体积比＝50∶50)代替异戊醚。
实例3
用于形成二氧化硅层的组成物根据与实例1相同的方法制备，但使用异丁醚作为溶剂。
实例4
用于形成二氧化硅层的组成物根据与实例1相同的方法制备，但使用双-(2，2二甲基丙基)醚作为溶剂。
比较例1
用于形成二氧化硅层的组成物根据与实例1相同的方法制备，但使用二丙醚作为溶剂。
比较例2
用于形成二氧化硅层的组成物根据与实例1相同的方法制备，但使用二甲苯作为溶剂。
比较例3
用于形成二氧化硅层的组成物根据与实例1相同的方法制备，但使用二丁醚作为溶剂。
评估1：溶剂的吸湿性
评估实例1到实例4和比较例1到比较例3中所用的各溶剂的吸湿性。
在23℃±2℃下，在40％±10％相对湿度下，根据计算等式1评估实例1到实例4和比较例1到比较例3中所用的各溶剂的吸湿性。
[计算等式1]
溶剂的吸湿性＝(静置12小时时溶剂中吸附的水分重量)/(静置12小时时二甲苯中吸附的水分重量)
参考比较例2中所用的二甲苯溶剂(二甲苯的吸湿性＝1.0)，使用计算等式1评估各溶剂的相对吸湿性。
评估2：薄膜的空穴缺陷
从旋转器的喷嘴尖端施配3毫升根据实例1到实例4和比较例1到比较例3的各用于形成二氧化硅层的组成物，并且使用旋涂器(K-SPIN8设备)以1，500转/分钟在直径为8英寸的图案化硅晶圆的中心旋涂。在150℃下预烘烤经涂布的薄膜。随后，在300℃下在供应水蒸气的锅炉中固化经涂布的薄膜并且转化成氧化物膜。接着，通过蚀刻去除大于或等于1,000埃的氧化物膜，并且通过使用缺陷检查(KLA Tencor)设备计数薄膜中以凹陷或凸出盘(直径：大于或等于50纳米)形式存在的空穴缺陷的数目。
评估1到评估2的结果提供于表1中。
[表1]
比较例1 比较例2 比较例3 实例1 实例2 实例3 实例4
溶剂的吸湿性 7.4 1.0(参考) 4.5 2.0 3.4 2.3 1.9
空穴缺陷数目 104 247 85 91 87 94 89
参看表1，相较于比较例1到比较例3中所用溶剂的吸湿性，显示实例1到实例4中所用的溶剂的吸湿性相对小。
另外，参看表1，当在评估2中测量时，显示根据实例1到实例4的用于形成二氧化硅层的组成物的空穴缺陷数目比根据比较例1到比较例3的用于形成二氧化硅层的组成物的空穴缺陷数目少。
虽然已经结合目前视为实用示范性实施例的内容来描述本发明，但应理解本发明不限于所披露的实施例，而是相反，本发明旨在涵盖包含在所附权利要求书的精神和范围内的各种修改和等效配置。

Claims (12)

1.一种用于形成二氧化硅层的组成物，其特征在于包括：
含硅的聚合物，以及
作为溶剂的由化学式1表示的化合物：
[化学式1]
其中在化学式1中，
L1和L2独立地是单键或C1到C5亚烷基，
m和n独立地是0到2范围内的整数，以及
X1和X2独立地是C1到C10烷基，
其限制条件为当m和n都是零时，X1和X2中的至少一个为C3到C10异烷基或C4到C10叔烷基。
2.根据权利要求1所述的用于形成二氧化硅层的组成物，其中所述由化学式1表示的化合物在其结构中包含7个到14个碳。
3.根据权利要求2所述的用于形成二氧化硅层的组成物，其中所述由化学式1表示的化合物在其结构中包含8个到12个碳。
4.根据权利要求1所述的用于形成二氧化硅层的组成物，其中所述溶剂包含异丁醚、异戊醚、双-(2，2-二甲基丙基)-醚、双-(1，1-二甲基丙基)-醚或其组合。
5.根据权利要求1所述的用于形成二氧化硅层的组成物，其中所述溶剂的沸点小于或等于200℃。
6.根据权利要求1所述的用于形成二氧化硅层的组成物，其中所述含硅的聚合物包含聚硅氮烷、聚硅氧氮烷或其组合。
7.根据权利要求1所述的用于形成二氧化硅层的组成物，其中按所述用于形成二氧化硅层的组成物的量计，所述含硅的聚合物以0.1重量％到30重量％的量包含在内。
8.一种制造二氧化硅层的方法，其特征在于包括：
将根据权利要求1到权利要求7中的一项所述的用于形成二氧化硅层的组成物涂布于衬底上，
干燥涂布有所述用于形成二氧化硅层的组成物的所述衬底，以及
在250℃到1,000℃下固化所述用于形成二氧化硅层的组成物。
9.根据权利要求8所述的制造二氧化硅层的方法，其中所述固化包含首先在250℃到1,000℃的水蒸气气氛下固化，其次在600℃到1,000℃的氮气气氛下固化。
10.根据权利要求8所述的制造二氧化硅层的方法，其中通过旋涂法进行所述用于形成二氧化硅层的组成物的涂布。
11.一种二氧化硅层，其特征在于所述二氧化硅层根据权利要求8所述的制造二氧化硅层的方法制造。
12.一种电子装置，其特征在于所述电子装置包括根据权利要求11所述的二氧化硅层。
CN201610835603.2A 2016-02-26 2016-09-20 用于形成二氧化硅层的组成物、二氧化硅层及其制造方法以及包含二氧化硅层的电子装置 Active CN107129757B (zh)

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