CN114423723A - 用于制造氮化硅基底的方法 - Google Patents

用于制造氮化硅基底的方法 Download PDF

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CN114423723A
CN114423723A CN202080065937.0A CN202080065937A CN114423723A CN 114423723 A CN114423723 A CN 114423723A CN 202080065937 A CN202080065937 A CN 202080065937A CN 114423723 A CN114423723 A CN 114423723A
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Prior art keywords
silicon nitride
mixture
sheet
ceramic additive
slurry
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CN202080065937.0A
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李承沿
李承官
池银玉
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OCI Holdings Co Ltd
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OCI Co Ltd
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Abstract

本发明涉及一种用于制造氮化硅基底的方法，并且更具体地，包括以下步骤：通过混合氮化硅粉末、陶瓷添加剂和溶剂来形成浆料；使浆料成型以形成片材；将片材中的至少一个夹在下板与上板之间以形成堆叠结构；将堆叠结构脱脂；以及烧结堆叠结构。下板和上板中的至少一个包括设置在其一个表面的多个突起，并且突起在一个方向上彼此平行地延伸。

Description

用于制造氮化硅基底的方法
技术领域
本发明涉及一种用于制造氮化硅基底的方法。
背景技术
具有高电绝缘性和高导热性的陶瓷材料可以用作快速传递从装置产生的热量的热介质。陶瓷材料被用于用来传送机器的装置的基底、用于高度集成电子电路的基底、用于激光振荡部的散热组件、用于半导体制造设备的反应容器组件和精密机器组件。
具体地，用于高输出功率装置的陶瓷基底需要具有高绝缘性、高耐压性(voltageresistance)、高导热率、高强度和低介电常数。适用于上述需要的陶瓷基底包括氮化铝基底、氧化铝基底和氮化硅基底。
氮化硅(Si3N4)基底具有高强度(500MPa至800MPa)、高延展性(5MPa·m至8MPa·m)以及热膨胀系数与硅(Si)的优异一致性。此外，氮化硅(Si3N4)基底具有高导热率(70W/mK至170W/mK)。也就是说，氮化硅(Si3N4)基底适用于下一代高输出功率装置的材料。
发明内容
技术问题
本发明提供了一种用于制造高质量氮化硅基底的方法。
技术方案
根据本发明的构思，用于制造氮化硅基底的方法包括：通过混合氮化硅粉末、陶瓷添加剂和溶剂形成浆料；使浆料成型以形成片材；将片材中的至少一个夹在下板与上板之间以形成堆叠结构；对堆叠结构进行脱脂；以及烧结堆叠结构。这里，下板和上板中的至少一个包括设置在其一个表面的多个突起，并且突起在一个方向上彼此平行地延伸。
有益效果
用于制造氮化硅基底的方法可以通过使用下板和上板来夹持氮化硅片材，下板和上板中的每个具有图案化表面。由于对如上所述形成的堆叠结构执行脱脂工艺和烧结工艺，因此可以进一步有效地执行脱脂工艺和烧结工艺。结果，本发明可以提供高质量的氮化硅基底。
附图说明
图1是用于说明根据本发明的实施例的用于制造氮化硅基底的方法的流程图。
图2是用于说明图1的第一步骤的示意图。
图3a至图3e是用于说明图1的第二步骤的示意图。
图4是用于说明图1的第三步骤的示意图。
图5是用于说明图1的第四步骤的示意图。
图6是用于说明图1的第五步骤的示意图。
图7是用于说明图1的第六步骤的示意图。
图8是用于说明图1的第七步骤的示意图。
具体实施方式
在下文中，将参照附图描述本发明的实施例，以便充分理解本发明的构成和效果。然而，本发明可以以不同的形式实施，并且不应被解释为限于在这里阐述的实施例。相反，提供这些实施例使得本公开将是彻底的和完整的，并且将向本领域技术人员充分传达本发明的范围。此外，本发明仅由权利要求的范围限定。
此外，尽管在发明构思的各种实施例中使用如第一、第二和第三的术语来描述各种区域和层，但是区域和层不限于这些术语。这些术语仅用于将一个组件与另一组件区分开。在这里描述和例示的实施例包括其互补实施例。
在以下描述中，技术术语仅用于说明特定示例性实施例，而不限制本发明。在说明书中，除非相反地提及，否则单数形式的术语可以包括复数形式。此外，“包括”、“包含”及其变型的含义说明了性质、区域、固定数量、步骤、工艺、元件和/或组件，但不排除其它性质、区域、固定数量、步骤、工艺、元件和/或组件。
图1是用于说明根据本发明的实施例的用于制造氮化硅基底的方法的流程图。
参照图1，根据本发明的实施例的用于制造氮化硅基底的方法可以包括：制备陶瓷添加剂的第一步骤S110；通过混合氮化硅粉末、陶瓷添加剂和溶剂来形成浆料的第二步骤S120；通过流延成型工艺使浆料成型以形成片材的第三步骤S130；堆叠片材并对其执行层压工艺以形成层压片材的第四步骤S140；将层压片材夹在下板与上板之间以形成堆叠结构的第五步骤S150；对堆叠结构执行脱脂工艺的第六步骤S160；以及对堆叠结构执行烧结工艺的第七步骤S170。
图2是用于说明图1的第一步骤的示意图。
参照图1和图2，可以在第一容器CON1中设置第一球BA1和第一混合物MI1。第一混合物MI1可以包括陶瓷粉末和溶剂。具体地，可以将第一球BA1和溶剂放入第一容器CON1中。可以将陶瓷粉末放入溶剂中。第一球BA1可以包括诸如氧化锆的陶瓷。溶剂可以是有机溶剂(例如乙醇)。陶瓷粉末可以包括氧化钇(Y2O3)、氧化镁(MgO)和氧化锆(ZrO2)。根据本发明的另一实施例，可以省略陶瓷粉末中的氧化锆(ZrO2)。
通过使用混合器混合第一混合物MI1，陶瓷粉末可以均匀地混合在第一混合物MI1中。第一球BA1可以物理地帮助陶瓷粉末被均匀地混合。具体地，可以在第一混合物MI1中均匀地混合氧化钇、氧化镁和氧化锆。
在混合完成之后，可以去除第一球BA1。可以通过干燥第一混合物MI1来蒸发全部溶剂。结果，可以在步骤S110中获得粉末形式的陶瓷添加剂SA。陶瓷添加剂SA可以包括氧化钇(Y2O3)、氧化镁(MgO)和氧化锆(ZrO2)。根据本发明的另一实施例，可以省略陶瓷添加剂SA中的氧化锆(ZrO2)。
氧化钇与陶瓷添加剂SA的重量比可以是0.5至0.8。氧化镁与陶瓷添加剂SA的重量比可以为0.1至0.4。氧化锆与陶瓷添加剂SA的重量比可以是0至0.3(即，等于或小于0.3)。当陶瓷添加剂SA不包含氧化锆时，氧化锆的重量比可以为0。根据本发明的实施例，氧化锆与陶瓷添加剂SA的重量比可以为0.1至0.3。
例如，在陶瓷添加剂SA中，氧化钇可以具有约56wt％的重量比，氧化镁可以具有约22wt％的重量比，氧化锆可以具有约22wt％的重量比。
图3a至图3e是用于说明图1的第二步骤的示意图。
参照图1和图3a，可以在第二容器CON2中设置第二球BA2和溶剂SV。溶剂SV可以是例如异丙醇和甲苯的有机溶剂。异丙醇和甲苯可以以4:6的体积比混合。第二球BA2可以包括氮化硅。
可以通过将氮化硅(Si3N4)粉末SNP、陶瓷添加剂SA和分散剂DIS放入第二容器CON2中的溶剂SV中来制备第二混合物MI2。陶瓷添加剂SA可以通过先前的第一步骤S110制备。分散剂DIS可以包括市场上可买到的分散剂DIS，例如BYK-111。
溶剂SV可以具有相对于第二混合物MI2的整个体积的40vol％至60vol％的体积比。氮化硅粉末SNP可以具有相对于第二混合物MI2的整个体积的15vol％至25vol％的体积比。陶瓷添加剂SA可以具有相对于第二混合物MI2的重量的5wt％至10wt％的重量比。
参照图1和图3b，可以通过对第二混合物MI2执行第一球磨工艺来均匀地混合第二混合物MI2。第二球BA2可以物理地帮助第二混合物MI2均匀地混合。
具体地，第一球磨工艺可以包括通过使用球磨机以预定的速度旋转其中储存有第二混合物MI2的第二容器CON2的工艺。当第二容器CON2旋转时，可以通过第二容器CON2中的第二球BA2执行机械研磨和均匀混合。球磨机可以具有100rpm至500rpm的旋转速度。
参照图1和图3c，在第一球磨工艺之后，可以通过添加粘合剂BI和增塑剂PL来制备第三混合物MI3。粘合剂BI可以包括纤维素衍生物(诸如乙基纤维素、甲基纤维素、硝基纤维素和羧基纤维素)、树脂(诸如聚乙烯醇、丙烯酸酯、甲基丙烯酸酯、聚乙烯醇缩丁醛)以及衍生物和树脂的混合物中的至少一种。例如，粘合剂BI可以包括聚乙烯醇缩丁醛(PVB)。增塑剂PL可以包括邻苯二甲酸二丁酯或邻苯二甲酸二辛酯。添加的增塑剂PL可以具有粘合剂BI的重量的约50％的重量。另外，可以将溶剂进一步添加到第二混合物MI2中。
参照图1和图3d，可以通过对第三混合物MI3执行第二球磨工艺来均匀地混合第三混合物MI3。当通过第二球磨工艺均匀地混合第三混合物MI3时，可以在步骤S120中形成浆料SL。第二球磨工艺可以与上述第一球磨工艺基本上相同或相似。此后，可以去除第二球BA2。
参照图1和图3e，可以通过老化通过第二球磨工艺形成的浆料SL而从浆料SL中去除挥发性气体。在老化浆料SL的同时，可以通过使用搅拌器SIT搅拌浆料SL。可以在约24小时期间执行老化。
图4是用于说明图1的第三步骤的示意图。
参照图1和图4，可以通过在流延成型工艺中使在第二步骤120中制备的浆料SL成型来形成片材SH。具体地，流延成型工艺可以包括：将浆料SL倾倒至被设定为预定的坝高度的刀片；以及将浆料SL施加在移动的基底膜上。当溶剂从施加在基底膜上的浆料SL中挥发并剥离基底膜时，可以获得成型的片材SH。可以使用不锈钢带、油纸带或聚合物带(诸如聚酯)作为基底膜。例如，可以将浆料倾倒至被设定在约0.3mm的坝高度的刮刀处，并且可以将浆料施加在以预定的速度(例如，0.1m/min至1m/min)移动的基底膜上。此后，当执行干燥工艺和剥离基底膜的工艺时，可以获得片材SH。
流延成型工艺可以在30℃至80℃的温度下执行。可以将通过流延工艺形成的片材SH切割成适当的尺寸。片材SH可以具有0.1mm至0.16mm的厚度。
图5是用于说明图1的第四步骤的示意图。
参照图1和图5，可以堆叠在第三步骤S130中制备的多个片材SH。当对堆叠的片材SH执行层压工艺时，可以在步骤S140中形成层压片材SSH。例如，可以通过层压三个至五个片材SH来构造层压片材SSH。层压工艺可以在约60℃的温度和约10MPa的压力下执行。
可以压制层压片材SSH。压制工艺可以使用温等静压机(WIP)。压制工艺可以在约70℃的温度和约30MPa的压力下执行。最后，层压片材SSH可以具有0.3mm至4mm的厚度TH。
图6是用于说明图1的第五步骤的示意图。
参照图1和图6，可以制备堆叠结构SS。堆叠结构SS可以包括下板PLT1、上板PLT2和设置在下板PLT1与上板PLT2之间的层压片材SSH。制备堆叠结构SS的工艺可以包括将在第四步骤S140中制备的层压片材SSH夹在下板PLT1与上板PLT2之间。尽管一个层压片材SSH设置在下板PLT1与上板PLT2之间作为图6中的示例，但本发明不限于此。例如，两个或更多个层压片材SSH可以设置在下板PLT1与上板PLT2之间。
在制备堆叠结构SS之前，可以将氮化硼BN均匀地施加到层压片材SSH上。下板PLT1和上板PLT2中的每个可以包括氮化硼。下板PLT1和上板PLT2中的每个可以具有1.4g/cm3至1.7g/cm3的密度。下板PLT1和上板PLT2中的每个可以具有层压片材SSH的面积的1.00倍至1.02倍的面积。
下板PLT1和上板PLT2中的至少一个可以包括设置在其一个表面的多个突起PP。层压片材SSH的一个表面可以接触突起PP。突起PP可以在一个方向上彼此平行地延伸。凹陷RS可以限定在彼此相邻的突起PP之间。换句话说，下板PLT1和上板PLT2中的至少一个可以具有图案化表面。在本发明的另一实施例中，可以省略突起PP。
每个突起PP可以具有第一宽度W1。凹陷RS可以具有第二宽度W2。第一宽度W1和第二宽度W2可以彼此相等或不同。第一宽度W1可以是0mm至15mm，优选地是0.1mm至15mm，更优选地是4mm至15mm。第二宽度W2可以是0mm至15mm，优选地是0.1mm至15mm，更优选地是4mm至15mm。突起PP可以以预定的节距PI布置。突起PP的节距PI可以是第一宽度W1和第二宽度W2的总和。
突起PP可以具有圆形的剖面形状。对于另一示例，突起PP可以具有多边形(三角形或矩形)剖面形状。
堆叠结构SS可以包括在下板PLT1与层压片材SSH之间的第一间隙GA1和在上板PLT2与层压片材SSH之间的第二间隙GA2。第一间隙GA1可以由下板PLT1的相邻的突起PP和限定在其间的凹陷RS限定。第二间隙GA2可以由上板PLT2的相邻的突起PP和限定在其间的凹陷RS限定。
图7是用于说明图1的第六步骤的示意图。
参照图1和图7，可以在步骤S160中对在第五步骤S150中制备的堆叠结构SS执行脱脂工艺(例如，粘合剂烧尽(B.B.O.))。因此，可以燃烧并去除层压片材SSH中的诸如粘合剂、分散剂和增塑剂的所有有机材料。脱脂工艺可以在大气炉(AF)中在约600℃的温度下执行12小时。也就是说，脱脂工艺可以在大气(空气)下执行。
如上所述，可以在层压片材SSH的底表面上确保第一间隙GA1，可以在层压片材SSH的顶表面上确保第二间隙GA2。尽管层压片材SSH被下板PLT1和上板PLT2夹在中间，但是可以通过第一间隙GA1和第二间隙GA2顺利执行脱脂工艺。例如，加热的气体(即，空气)可以穿过第一间隙GA1和第二间隙GA2。加热的气体可以通过第一间隙GA1和第二间隙GA2接触层压片材SSH的底表面和顶表面。
图8是用于说明图1的第七步骤的示意图。
参照图1和图8，在第六步骤S160之后，可以在坩埚CRU中设置堆叠结构SS。当将垫粉末BNP放入坩埚CRU中时，堆叠结构SS可以埋在垫粉末BNP中。垫粉末BNP可以包括氮化硼粉末、氮化硅粉末或其混合物。当垫粉末BNP是氮化硼粉末和氮化硅粉末的混合物时，氮化硼粉末和氮化硅粉末可以以1:1的比例混合。
在步骤S170中，可以通过加热坩埚CRU来对堆叠结构SS执行烧结工艺。因此，当层压片材SSH被烧结时，可以形成氮化硅基底。烧结工艺可以在约1900℃的温度下执行6小时。烧结工艺可以在氮气气氛下执行。
如上所述，可以在层压片材SSH的底表面上确保第一间隙GA1，可以在层压片材SSH的顶表面上确保第二间隙GA2。尽管层压片材SSH被下板PLT1和上板PLT2夹在中间，但是烧结工艺可以通过第一间隙GA1和第二间隙GA2顺利执行。
本发明的描述意图是说明性的，并且本发明的技术领域的普通技术人员将理解的是，本发明可以以其它特定的形式实现而不改变技术思路或基本特征。因此，应当理解的是，上述实施例包括各方面的示例并且不是限制性的。

Claims (12)

1.一种用于制造氮化硅基底的方法，所述方法包括：
通过混合氮化硅粉末、陶瓷添加剂和溶剂形成浆料；
使所述浆料成型以形成片材；
通过将所述片材中的至少一个夹在下板与上板之间来形成堆叠结构；
对所述堆叠结构执行脱脂工艺；以及
对所述堆叠结构执行烧结工艺，
其中，所述下板和所述上板中的至少一个包括设置在其一个表面的多个突起，并且
所述突起在一个方向上彼此平行地延伸。
2.根据权利要求1所述的方法，其中，所述陶瓷添加剂包括氧化钇(Y2O3)、氧化镁(MgO)和氧化锆(ZrO2)，
所述氧化钇与所述陶瓷添加剂的重量比为0.5至0.8，
所述氧化镁与所述陶瓷添加剂的重量比为0.1至0.4，并且
所述氧化锆与所述陶瓷添加剂的重量比为0.3或更小。
3.根据权利要求1所述的方法，其中，形成所述浆料的步骤包括添加粘合剂和增塑剂。
4.根据权利要求1所述的方法，其中，形成所述浆料的步骤包括：
通过向所述溶剂中添加氮化硅粉末、所述陶瓷添加剂和分散剂来形成第一混合物；
对所述第一混合物执行第一球磨工艺；
通过向完成所述第一球磨工艺的第一混合物添加粘合剂和增塑剂来形成第二混合物；以及
对所述第二混合物执行第二球磨工艺。
5.根据权利要求1所述的方法，其中，使所述浆料成型的步骤包括流延成型工艺。
6.根据权利要求1所述的方法，所述方法还包括：在形成所述堆叠结构之前，通过堆叠所述片材并对其执行层压工艺来形成层压片材。
7.根据权利要求1所述的方法，其中，所述下板和所述上板中的每个具有1.4g/cm3至1.7g/cm3的密度。
8.根据权利要求1所述的方法，其中，所述下板和所述上板中的每个具有所述片材的面积的1.00倍至1.02倍的面积。
9.根据权利要求1所述的方法，其中，凹陷限定在彼此相邻的突起之间，并且
所述堆叠结构包括由所述相邻的突起、凹陷和片材的一个表面限定的间隙。
10.根据权利要求9所述的方法，其中，所述突起具有第一宽度，所述凹陷具有第二宽度，
所述第一宽度为0mm至15mm，并且
所述第二宽度为0mm至15mm。
11.根据权利要求9所述的方法，其中，在脱脂工艺期间，加热的气体通过所述间隙接触所述片材的所述一个表面。
12.根据权利要求1所述的方法，其中，所述突起以预定的节距布置。
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Application publication date: 20220429