CN106882967A - 一种含内置电极的陶瓷体的热压烧结方法 - Google Patents
一种含内置电极的陶瓷体的热压烧结方法 Download PDFInfo
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Abstract
本发明提供了一种含内置电极的陶瓷体的热压烧结方法,包括以下步骤:步骤一、将陶瓷粉体和分散剂加入溶剂中,制成混合浆料,初次球磨后加入增塑剂和粘结剂,进行二次球磨,制备成陶瓷浆料;步骤二、真空条件下对陶瓷浆料进行除泡,并流延成陶瓷生片;步骤三、陶瓷生片干燥后,在陶瓷生片表面印刷电极浆料;步骤四、印刷电极浆料的陶瓷生片烘干后,置于热压烧结模具中,进行排胶处理;步骤五、排胶后,在陶瓷生片表面铺洒陶瓷粉体;步骤六、对陶瓷生片热压烧结处理。本发明简化了含内置电极层的陶瓷体的制备工艺,省去了印刷电极后的层压等工艺,保证了电极层与陶瓷体上下表面的平行度,适用于小批量、多尺寸的含内置电极层陶瓷体的制备。
Description
技术领域
本发明涉及陶瓷体制备领域,尤其是一种工序简单、适于小批量、多尺寸的陶瓷体热压烧结方法。
背景技术
AlN陶瓷由于具有优异的热传导性能,可以作为加工晶圆的静电卡盘。静电卡盘通常含有内置电极层,为保证其在一定的电流电压下对晶圆的吸附脱附能力均匀稳定,因此电极层与陶瓷体上下表面的平行度须达到20μm左右。
含内置电极层的陶瓷体中,电极层本身十分平整,与陶瓷体的上下表面平行度较高(一般在20μm范围内)。制备含内置电极的陶瓷体,一般需要一体化烧结内置电极与陶瓷体。无压烧结过程中陶瓷体会发生径向收缩和横向收缩,对于电极浆料与陶瓷生坯烧结收缩的一致性要求较高;另一方面无压烧结过程中无外加压力,更易出现电极层与陶瓷体的分层,因此无压烧结工艺烧结前需对电极层和陶瓷坯体进行层压以保证电极层与陶瓷体之间结合紧密无分层现象。相比而言,热压烧结过程中径向压力使得其仅有径向收缩,因此电极层与陶瓷体的结合更紧密不易分层,更重要的是,采用热压烧结工艺不需温水静压机等层压设备,可省去层压工序,大大简化了工艺。因此含内置电极的陶瓷体烧结优选热压烧结。
而热压烧结过程中如何保证电极层与陶瓷的平行度是难以解决的关键问题。
发明内容
本发明的目的是提供一种含内置电极的陶瓷体的层压与烧结一体化工艺,解决内置电极层陶瓷体易分层、不能保证电极层与上下陶瓷表面的平行度的问题。
一种含内置电极的陶瓷体的热压烧结方法,包括以下步骤:
步骤一、将陶瓷粉体和分散剂加入溶剂中,制成混合浆料,初次球磨后加入增塑剂和粘结剂,进行二次球磨,制备成陶瓷浆料;
步骤二、真空条件下对陶瓷浆料进行除泡,并流延成陶瓷生片;
步骤三、陶瓷生片干燥后,在陶瓷生片表面印刷电极浆料;
步骤四、印刷电极浆料的陶瓷生片烘干后,置于热压烧结模具中,进行排胶处理;
步骤五、排胶后,在陶瓷生片表面铺洒陶瓷粉体;
步骤六、对陶瓷生片热压烧结处理。
进一步地,所述步骤一中,陶瓷粉体为AlN或AlN与Y2O3、La2O3、CeO2、CaO、CaF2的一种或几种组成的复合材料。
进一步地,所述步骤一中,分散剂为磷酸三乙酯,分散剂质量为陶瓷粉体质量的0.5%~2%;
粘结剂为PVB,粘结剂质量为陶瓷粉质量的3%~7%;
增塑剂为DBP,粘结剂与增塑剂加入量质量比为0.6:1~1.6:1。
进一步地,所述步骤一中,溶剂为无水乙醇与异丙酮或丁酮或甲苯的混合溶液,混合质量比为1:1~2:1。
进一步地,所述步骤一中,初次球磨过程为:向混合浆料中加入磨球,磨球与陶瓷粉体的质量比为1:1~3:1,球磨时间为2~10h;二次球磨时间为2~10h。
进一步地,所述步骤一中,陶瓷浆料的固相含量为40%~50%(体积),粘度为1000~10000mPa·s。
进一步地,所述步骤二中,真空度为100~300Pa时进行除泡,除泡时间为0.5~2h。
进一步地,所述步骤三中,电极浆料印刷厚度为5~25μm。
进一步地,所述步骤四中,排胶过程在N2气氛下加热进行,加热时升温速率为0.5~3℃/min,升温至600~800℃,保温1~4h。
进一步地,所述步骤六中,烧结过程升温速率不超过20℃/min,升温至1700~1900℃,保持压力8~25MPa,保温时间为1~8h。
优选地,电极浆料的具体制备方法为:
取钨98~100份、乙基纤维素1.5~4份,松油醇12~18份混合均匀,以上各份为质量份。
优选地,所述步骤四中,印刷电极浆料的陶瓷生片在60~90℃条件下烘干,烘干时间为3~20min后置于热压烧结模具中,在N2气氛下进行排胶。
优选地,所述步骤五中,排胶后,在陶瓷生片表面铺洒陶瓷粉体,所铺陶瓷粉体的厚度为0.5~3mm为宜,便于后期加工。
本发明的含内置电极的陶瓷体烧结方法简化了含内置电极的陶瓷体的制备工艺,省去了印刷电极后的层压等工艺,保证了电极层与陶瓷体上下表面的平行度,适用于小批量、多尺寸的含内置电极陶瓷体的制备。
附图说明
附图仅用于示出具体实施例的目的,而并不认为是对本发明的限制,在整个附图中,相同的参考符号表示相同的部件。
图1是本发明的热压烧结制备陶瓷体的流程示意图。
具体实施方式
下面结合附图和具体实施方式对本发明作进一步详细的说明。
实施例1
步骤一、称取500g的AlN陶瓷粉体,添加5g磷酸三乙酯为分散剂、以无水乙醇和异丙醇的混合溶液为溶剂,混合比例为1:1,加入磨球,磨球与陶瓷粉体的质量比为1:1,球磨混合6h后,加入15gPVB粘结剂、以18gDBP(邻苯二甲酸二丁酯)为增塑剂,继续进行二次球磨,球磨时间3h,混合均匀后,制备出固相含量为40%(体积),粘度为5200mPa·s的AlN陶瓷浆料。
步骤二、真空度160Pa除泡30min后,流延出厚度为220μm的AlN陶瓷生片。
步骤三、干燥后在生片上表面印刷电极浆料,印刷电极浆料厚度为10μm。
电极浆料的具体制备方法为:
取质量份为:钨100份、乙基纤维素2份,松油醇16.5份混合均匀。
步骤四、以70℃保温10min烘干后,印刷电极浆料的表面形成钨电极,将未印刷浆料的生片置于底层,然后放置印刷浆料的生片(印刷面朝上),于石墨模具中在氮气气氛下排胶:以0.8℃/min升温至600℃,保温2h,排胶。
步骤五、排胶后于钨电极表面铺洒1000g的AlN复合粉体,厚度为3mm。
步骤六、以10℃/min的速率升温至1850℃,压力25MPa,保温3h,热压烧结最后获得含钨的特殊陶瓷体,AlN陶瓷致密度达98.8%,钨电极层与陶瓷体无分层现象,经平行度检测,钨电极层与陶瓷体上下表面的平行度分别为16μm和10μm。
实施例2
步骤一、称取475g的AlN陶瓷粉体,25gY2O3粉体,添加6g磷酸三乙酯为分散剂、以无水乙醇和丁酮的混合溶液为溶剂,混合质量为1:1,加入磨球,磨球与陶瓷粉体的质量比为2:1,球磨混合5h后,加入17.5gPVB粘结剂、以20gDBP(邻苯二甲酸二丁酯)为增塑剂,继续进行二次球磨,球磨时间3h,混合均匀后,制备出固相含量为43%(体积)的AlN陶瓷浆料,粘度6000mPa·s。
步骤二、真空度200Pa除泡1h后,流延出厚度为260μm的AlN陶瓷生片。
步骤三、在乙醇浓度为25%的环境中干燥后在生片表面印刷电极浆料,电极浆料厚度为15μm。
电极浆料为:取质量份为:钨98份、乙基纤维素2份,松油醇14.5份混合均匀。
步骤四、以75℃保温12min烘干后,印刷电极浆料的表面形成钨电极,将未印刷浆料的生片置于底层,然后放置印刷浆料的生片(印刷面朝上),于石墨模具中在氮气气氛下排胶:以1℃/min的速率升温至650℃,保温2h,进行排胶。
步骤五、排胶后于钨电极表面铺洒400g的AlN复合粉体,厚度为0.8mm。
步骤六、以10℃/min的速率升温至1810℃,压力15MPa,保温2.5h,热压烧结最后获得含钨的特殊陶瓷体,AlN复合陶瓷致密度达99.2%,钨电极层与陶瓷体未发生分层现象,经平行度检测,钨电极层与上下表面的平行度分别为17μm和14μm。
实施例3
步骤一、称取475g的AlN陶瓷粉体,1.5gY2O3粉体,2.5gCeO2,2.5gCaO,添加9g磷酸三乙酯为分散剂、以无水乙醇和甲苯的混合溶液为溶剂,混合质量比为3:2,加入磨球,磨球与陶瓷粉体的质量比为3:1,球磨混合4h后,加入14.5gPVB粘结剂、以22gDBP(邻苯二甲酸二丁酯)为增塑剂,继续进行二次球磨,球磨时间2h,混合均匀后,制备出固相含量为40%(体积)的AlN复合陶瓷浆料。
步骤二、真空度180Pa除泡40min后,流延出厚度为300μm的AlN陶瓷生片。
步骤三、在乙醇浓度为35%的环境中干燥后在生片表面印刷电极浆料,电极浆料厚度为20μm。
电极浆料为:取质量份为:钨99份、乙基纤维素2.4份,松油醇15份混合均匀。
步骤四、以80℃保温9min烘干后,印刷电极浆料的表面形成钨电极,将未印刷浆料的生片置于底层,然后放置印刷浆料的生片(印刷面朝上),于石墨模具中在氮气气氛下排胶:以1.5℃/min的速率升温至650℃,保温2.5h,进行排胶。
步骤五、排胶后于钨电极表面铺洒300g的AlN复合粉体,厚度为0.5mm。
步骤六、热压烧结处理。以12℃/min的速率升温至1780℃,压力18MPa,保温3h,热压烧结最后获得含钨的特殊陶瓷体,AlN复合陶瓷致密度达99.3%,钨电极层与陶瓷体无分层现象,经平行度检测,上下表面的平行度分别为18μm和16μm。
综上所述,本发明利用流延成型制备陶瓷生片本身平整度较好的特性,在流延后生片上印刷电极浆料,置于石墨模具后进行排胶,然后在电极层上面铺洒陶瓷粉体,整体热压烧结获得含电极层的陶瓷体。该工艺方法简化了含内置电极层的陶瓷体的制备工艺,省去了印刷电极后的层压等工艺,保证了电极层与陶瓷体上下表面的平行度,适用于小批量、多尺寸的含内置电极层陶瓷体的制备。
尽管已经结合优选的实施例对本发明进行了详细地描述,但是本领域技术人员应当理解的是在不违背本发明精神和实质的情况下,各种修正都是允许的,它们都落入本发明的权利要求的保护范围之中。
Claims (10)
1.一种含内置电极的陶瓷体的热压烧结方法,其特征在于,包括以下步骤:
步骤一、将陶瓷粉体和分散剂加入溶剂中,制成混合浆料,初次球磨后加入增塑剂和粘结剂,进行二次球磨,制备成陶瓷浆料;
步骤二、真空条件下对陶瓷浆料进行除泡,并流延成陶瓷生片;
步骤三、陶瓷生片干燥后,在陶瓷生片表面印刷电极浆料;
步骤四、印刷电极浆料的陶瓷生片烘干后,置于热压烧结模具中,进行排胶处理;
步骤五、排胶后,在陶瓷生片表面铺洒陶瓷粉体;
步骤六、对陶瓷生片热压烧结处理。
2.根据权利要求1所述的一种含内置电极的陶瓷体的热压烧结方法,其特征在于,所述步骤一中,陶瓷粉体为AlN或AlN与Y2O3、La2O3、CeO2、CaO、CaF2的一种或几种组成的复合材料。
3.根据权利要求2所述的一种含内置电极的陶瓷体的热压烧结方法,其特征在于,所述步骤一中,分散剂为磷酸三乙酯,分散剂质量为陶瓷粉体质量的0.5%~2%;
粘结剂为PVB,粘结剂质量为陶瓷粉质量的3%~7%;
增塑剂为DBP,粘结剂与增塑剂加入量质量比为0.6:1~1.6:1。
4.根据权利要求3所述的一种含内置电极的陶瓷体的热压烧结方法,其特征在于,所述步骤一中,溶剂为无水乙醇与异丙酮或丁酮或甲苯的混合溶液,混合质量比为1:1~2:1。
5.根据权利要求1-4任一所述的一种含内置电极的陶瓷体的热压烧结方法,其特征在于,所述步骤一中,初次球磨过程为:向混合浆料中加入磨球,磨球与陶瓷粉体的质量比为1:1~3:1,球磨时间为2~10h;二次球磨时间为2~10h。
6.根据权利要求1-4任一所述的一种含内置电极的陶瓷体的热压烧结方法,其特征在于,所述步骤一中,陶瓷浆料的固相含量为40%~50%(体积),粘度为1000~10000mPa·s。
7.根据权利要求6所述的一种含内置电极的陶瓷体的热压烧结方法,其特征在于,所述步骤二中,真空度为100~300Pa时进行除泡,除泡时间为0.5~2h。
8.根据权利要求7所述的一种含内置电极的陶瓷体的热压烧结方法,其特征在于,所述步骤三中,电极浆料印刷厚度为5~25μm。
9.根据权利要求8所述的一种含内置电极的陶瓷体的热压烧结方法,其特征在于,所述步骤四中,排胶过程在N2气氛下加热进行,加热时升温速率为0.5~3℃/min,升温至600~800℃,保温1~4h。
10.根据权利要求9所述的一种含内置电极的陶瓷体的热压烧结方法,其特征在于,所述步骤六中,烧结过程升温速率不超过20℃/min,升温至1700~1900℃,保持压力8~25MPa,保温时间为1~8h。
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