CN111747756A - 一种氮化物陶瓷流延浆料及其制备的氮化物陶瓷基片 - Google Patents
一种氮化物陶瓷流延浆料及其制备的氮化物陶瓷基片 Download PDFInfo
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- CN111747756A CN111747756A CN201910230703.6A CN201910230703A CN111747756A CN 111747756 A CN111747756 A CN 111747756A CN 201910230703 A CN201910230703 A CN 201910230703A CN 111747756 A CN111747756 A CN 111747756A
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Abstract
本发明涉及一种氮化物陶瓷流延浆料及其制备方法和应用。所述氮化物陶瓷流延浆料包括复合陶瓷粉体、混合溶剂、分散剂、增塑剂和粘结剂;其中所述粘结剂包括聚乙烯醇缩丁醛(PVB)和聚氯乙烯(PVC),聚乙烯醇缩丁醛和聚氯乙烯的质量比为20:1~4:1;以所述复合陶瓷粉体的质量为基准,所述粘结剂的质量为所述复合陶瓷粉体质量的3%~10%。本发明提供的所述氮化物陶瓷流延浆料,固含量在32%以上,氮化物粉体在浆料中分散均匀;该浆料经过流延工艺可以连续成膜,得到的流延坯体表面光滑均匀,无裂纹、空隙等缺陷,干燥后厚度可达0.6mm左右,拉伸强度5MPa以上,从而满足了陶瓷基片的力学、热学等方面的性能要求。
Description
技术领域
本发明属于陶瓷材料技术领域,具体涉及一种用于制备氮化物陶瓷基片的流延浆料及其制备的氮化物陶瓷基片。
背景技术
近年来,半导体器件在风力发电、太阳能光伏发电、电动汽车、LED照明等行业占据日益重要的地位,半导体器件也沿着大功率化、高频化、集成化的方向迅速发展。绝缘基片是半导体器件中承载和散热的关键部件。相比于传统的树脂基片材料,陶瓷材料具有更优异的导热性及力学性能,并具有高熔点、高硬度、高耐磨性、耐氧化等优点,是高端半导体器件,特别是大功率半导体器件基片用最佳材料。目前已经投入生产应用的陶瓷基片材料主要包括氧化铍(BeO)、氧化铝(Al2O3)、氧化锆(ZrO2)、氮化铝(AlN)和氮化硅(Si3N4)等,这些物质被称为“陶瓷粉体”。氮化铝、氮化硅等氮化物陶瓷,以其高热导率、优良力学性能等方面的优势日益得到重视,正逐步替代传统的传统氧化物陶瓷材料,成为市场主流和未来的发展方向。
流延成型是公认的陶瓷基片材料批量化生产的最佳成型方法。流延浆料(或称为“烧结浆料”)的制备是该方法的关键工艺之一。流延浆料一般由陶瓷粉体、烧结助剂、溶剂、分散剂、粘结剂、增塑剂(或称“塑性剂”)等混合而成。烧结助剂通常为多元金属化合物组合物,溶剂通常为乙醇、丙醇、丁醇、乙酸乙酯等非苯有机溶剂;分散剂可以选自三油酸甘油酯、聚磷酸盐、聚丙烯酸钠、聚山梨酯和聚乙二醇中的一种或几种;粘结剂有报道采用羧甲基纤维素钠、聚乙烯醇或聚丙烯醇;增塑剂常选自邻苯二甲酸甲苯基丁酯、环氧油酸丁酯、环氧硬脂酸辛酯、环氧化甘油三酸酯、甘油三醋酸酯、偏苯三酸三辛酯和偏苯三酸三己酯或均苯四酸四酯中的一种或几种。如张景贤等报道了:采用高纯Y2O3和MgO作为烧结助剂,三油酸甘油酯作为分散剂,乙醇/丁酮共沸组成作为溶剂,聚乙烯醇缩丁醛(PVB)作为粘结剂,邻苯二甲酸甲苯基丁酯(DBP)作为塑性剂制备氮化硅陶瓷基片材料用流延浆料(张景贤,等.高导热Si3N4陶瓷基片材料的制备研究[J].真空电子技术,2016(5):7-10)。公开号CN105481368A(公开日2016年4月13日)的中国发明专利申请“氮化铝陶瓷流延浆料、陶瓷基板及其制备方法和应用”公开的流延浆料,溶剂选自无水乙醇和乙酸乙酯的组合,或无水乙醇和乙酸丙酯的组合,分散剂选自聚磷酸盐、聚丙烯酸钠、聚山梨酯和聚乙二醇的一种或两种以上,烧结助剂选自氧化钇、氧化钙、氟化钇、氧化锂、碳酸钙或碳酸锂的一种或两种以上,增塑剂选自环氧油酸丁酯、环氧硬脂酸辛酯、环氧化甘油三酸酯、甘油三醋酸酯、偏苯三酸三辛酯、偏苯三酸三己酯或均苯四酸四酯的一种或两种以上,粘结剂选自羧甲基纤维素钠、聚乙烯醇或聚丙烯醇的一种或两种以上。此外,公开号CN108516836A(公开日2018年9月11日)的中国发明专利申请“一种氮化铝陶瓷基板的制备方法及封装材料”公开的流延浆料,以选自乙醇、丙醇、丁醇、乙酸乙酯中的一种或两种以上的混合物为溶剂,以选自Y2O3-CaO、Y2O3-CaF2、YF3-CaF2、Y2O3-CaO-Li2O和Y2O3-CaOLi2O3中的一种或两种以上的混合物为烧结助剂,以聚乙醇缩丁醛、聚乙二醇或聚氨酯为粘结剂。
但是,对于氮化物陶瓷而言,由于氮化物粉体粒径小,粉体表面电化学环境复杂,在溶液中分散困难,因此难以获得高固相含量的流延浆料,影响基板成型。此外,由于粉体分散困难,如果按照常规流延浆料粘结剂占陶瓷粉体(氧化铝和或氧化锆)质量10%以上的用量比例添加粘结剂,浆料粘度过大、流动性差,难以用于流延操作;但若减少粘结剂的添加,流延素坯的强韧性较差,流延成型较厚样时坯体易开裂。流延浆料存在的这些问题都会关系到陶瓷基片的制备和性能,最终影响半导体器件。
发明内容
为了克服现有技术的不足,本发明提供一种氮化物陶瓷流延浆料及其制备方法。本发明提供的所述氮化物陶瓷流延浆料粘度适宜,陶瓷粉体在浆料中分散均匀,固相含量达到32%以上。而且该流延浆料制得的流延素坯表面光滑均匀,可连续成膜,干燥后厚度可达0.6mm以上,具有较好的力学性能,完全满足半导体器件,尤其是大功率半导体器件基片的要求。
为了实现上述发明目的,本发明采用了如下的技术方案:
一种氮化物陶瓷流延浆料,包括:复合陶瓷粉体、混合溶剂、分散剂、增塑剂和粘结剂;其中所述粘结剂包括聚乙烯醇缩丁醛(PVB)和聚氯乙烯(PVC),聚乙烯醇缩丁醛和聚氯乙烯的质量比为20:1~4:1;以所述复合陶瓷粉体的质量为基准,所述粘结剂的质量为所述复合陶瓷粉体质量的3%~10%。
优选地,所述聚乙烯醇缩丁醛和聚氯乙烯的质量比为12:1~6:1。
优选地,所述粘结剂由聚乙烯醇缩丁醛和聚氯乙烯组成。
优选地,所述聚乙烯醇缩丁醛的分子量为1500~10000。
优选地,所述聚氯乙烯的分子量为1500~5000。
还优选地,所述粘结剂的质量为所述复合陶瓷粉体质量的5%~10%。
优选地,所述复合陶瓷粉体的体积占所述氮化物陶瓷流延浆料总体积的32%~42%。
还优选地,复合陶瓷粉体包括氮化物粉体和烧结助剂;所述氮化物粉体和所述烧结助剂的质量比为8:2~9.5:0.5。
还优选地,所述氮化物粉体为氮化硅或氮化铝。
优选地,所述氮化硅的粒度为D50=0.3μm-2μm。
优选地,所述氮化铝的粒度为D50=0.5μm-2μm。
还优选地,所述烧结助剂包括金属氧化物和稀土氧化物,所述金属氧化物和稀土氧化物的质量比为1:1~1:5;所述金属氧化物选自MgO、CaO、TiO2和Al2O3中的一种或一种以上,所述稀土氧化物选自Y2O3、Yb2O3、Er2O3、Ho2O3和CeO2中的一种或一种以上。
更优选地,所述金属氧化物和稀土氧化物的质量比为1:1~1:3。
更优选地,所述金属氧化物选自MgO、CaO、TiO2和Al2O3中的一种;最优选为MgO、CaO和Al2O3中的一种。
更优选地,所述稀土氧化物Y2O3、Yb2O3、Er2O3、Ho2O3和CeO2中的一种;最优选为Y2O3、Yb2O3和Er2O3中的一种。
作为一些优选的实施方案,本发明提供的氮化物陶瓷流延浆料中,烧结助剂选自MgO+Yb2O3、CaO+Er2O3和Al2O3+Y2O3中的一种,其中两种氧化物的质量比如前所定义。
优选地,以复合陶瓷粉体的质量为基准,所述混合溶剂的质量为所述复合陶瓷粉体质量的33%~52%。
还优选地,所述混合溶剂包括乙醇和丁酮,更优选由乙醇和丁酮组成;乙醇和丁酮的质量比为6:4。
优选地,以所述复合陶瓷粉体的质量为基准,所述分散剂的质量为所述复合陶瓷粉体质量的0.5%~5%,更优选为0.5%~2%。
还优选地,所述分散剂选自磷酸三乙酯、蓖麻油和丙烯酸铵中的一种。
更优选地,所述分散剂选自磷酸三乙酯或蓖麻油。
优选地,以所述复合陶瓷粉体的质量为基准,所述增塑剂的质量为所述复合陶瓷粉体质量的0.15%~1.6%;更优选为0.24%~1.2%。
还优选地,所述增塑剂选自聚乙二醇(PEG)和邻苯二甲酸丁苄酯(S160)中的一种。
还优选地,所述聚乙二醇的分子量为400~600。
优选地,所述氮化物陶瓷流延浆料还包括消泡剂,所述消泡剂选自聚醚改性硅、聚二甲基硅氧烷和丙烯酸乳液中的一种;以所述氮化物陶瓷流延浆料的总质量为基准,所述消泡剂的质量占所述氮化物陶瓷流延浆料总质量的0.05%~1%。
作为一个优选的实施方案,本发明提供一种氮化物陶瓷流延浆料,原料组成为:
氮化物粉体:选自氮化硅粉或氮化铝粉;
烧结助剂:由质量比为1:1~1:5的金属氧化物和稀土氧化物组成,其中所述金属氧化物选自MgO、CaO、TiO2和Al2O3中的一种,所述稀土氧化物选自Y2O3、Yb2O3、Er2O3、Ho2O3和CeO2中的一种;
混合溶剂:由质量比为6:4的乙醇和丁酮组成。
分散剂:选自磷酸三乙酯、蓖麻油和丙烯酸铵中的一种;
增塑剂:聚乙二醇和邻苯二甲酸丁苄酯中的一种;
粘结剂:由质量比为20:1~4:1的聚乙烯醇缩丁醛和聚氯乙烯组成;
消泡剂:选自聚醚改性硅、聚二甲基硅氧烷和丙烯酸乳液中的一种;
所述氮化物粉体和所述烧结助剂组成复合陶瓷粉体;所述氮化物粉体和所述烧结助剂的质量比为8:2~9.5:0.5;所述复合陶瓷粉体的体积占所述氮化物陶瓷流延浆料总体积的32%~42%;
以所述复合陶瓷粉体的质量为基准,所述混合溶剂的质量为所述复合陶瓷粉体质量的33%~52%,所述分散剂的质量为所述复合陶瓷粉体质量的0.5%~5%,所述粘结剂的质量为所述复合陶瓷粉体质量的3%~10%,所述增塑剂的质量为所述复合陶瓷粉体质量的0.15%~1.6%;
以所述氮化物陶瓷流延浆料的总质量为基准,所述消泡剂的质量占所述氮化物陶瓷流延浆料总质量的0.05%~1%。
作为一个更优选的实施方案,本发明提供一种氮化物陶瓷流延浆料,原料组成为:
氮化物粉体:选自氮化硅粉或氮化铝粉;
烧结助剂:由质量比为1:1~1:3的金属氧化物和稀土氧化物组成,其中所述金属氧化物选自MgO、CaO和Al2O3中的一种,所述稀土氧化物选自Y2O3、Yb2O3和Er2O3中的一种;
混合溶剂:由质量比为6:4的乙醇和丁酮组成。
分散剂:选自磷酸三乙酯或蓖麻油;
增塑剂:分子量400~600的聚乙二醇和邻苯二甲酸丁苄酯中的一种;
粘结剂:由质量比为12:1~6:1的聚乙烯醇缩丁醛和聚氯乙烯组成;
消泡剂:选自聚醚改性硅、聚二甲基硅氧烷和丙烯酸乳液中的一种;
所述氮化物粉体和所述烧结助剂组成复合陶瓷粉体;所述氮化物粉体和所述烧结助剂的质量比为8:2~9.5:0.5;所述复合陶瓷粉体的体积占所述氮化物陶瓷流延浆料总体积的32%~42%;
以所述复合陶瓷粉体的质量为基准,所述混合溶剂的质量为所述复合陶瓷粉体质量的33%~52%,所述分散剂的质量为所述复合陶瓷粉体质量的0.5%~2%,所述粘结剂的质量为所述复合陶瓷粉体质量的5%~10%,所述增塑剂的质量为所述复合陶瓷粉体质量0.24%~1.2%;
以所述氮化物陶瓷流延浆料的总质量为基准,所述消泡剂的质量占所述氮化物陶瓷流延浆料总质量的0.05%~1%。
本发明的另一个目的在于提供所述氮化物陶瓷流延浆料的制备方法,包括如下步骤:
I.按照配比准备复合陶瓷粉体、混合溶剂、分散剂、增塑剂和粘结剂;
II.将所述分散剂加入所述混合溶剂中,混合均匀,得到液态物料;
III.将所述复合陶瓷粉体加入步骤II得到的液态物料中,转移入球磨设备中,加入球磨介质,进行球磨,得到一次球磨浆料;
IV.向步骤III得到的所述一次球磨浆料中加入所述增塑剂,球磨1~3小时,再加入所述粘结剂,进行二次次球磨,得到二次球磨浆料;
V.筛网过滤去除步骤IV得到的所述二次球磨浆料中的球磨介质,加入所述消泡剂,用除泡设备消泡,即得。
优选地,所述球磨设备为球磨罐。
优选地,所述步骤III中,球磨转速为30转/分钟~200转/分钟,球磨时间根据物料的量决定,一般为2~12小时。
优选地,所述步骤IV中,球磨转速为150转/分钟~480转/分钟。
优选地,所述步骤IV中,所述粘结剂采用分次等量添加的方法加入。
还优选地,所述步骤IV中,二次球磨的时间根据粘结剂的量决定,一般每次添加粘结剂后球磨3~6小时,二次球磨的总时间为12~30小时。
优选地,所述步骤V中,所述消泡设备为真空消泡机,消泡时的真空度为10-1Pa。
本发明还有一个目的在于提供所述氮化物陶瓷流延浆料在制备半导体器件用陶瓷基片中的应用。
此外,本发明还提供一种半导体器件用陶瓷基片的流延坯体,采用上述氮化物陶瓷流延浆料,经过包括流延成型和坯体干燥等步骤制备得到。
优选地,坯体干燥的温度为20℃~70℃。
本发明还提供一种上述流延坯体经过烧结得到的半导体器件用陶瓷基片。
制备上述半导体器件用陶瓷基片的流延坯体,并进一步制备半导体器件用陶瓷基片的基本方法是本领域技术人员熟知的,采用的设备也是本领域常规的。
本申请说明书中,如无特殊说明,所述“乙醇”为无水乙醇。
本发明采用PVB和PVC复配作为粘结剂,得到的所述氮化物陶瓷流延浆料粘度适中,完全适于流延成型工艺。且所述浆料中固含量在32%以上,氮化物粉体在浆料中分散均匀。因此,本发明所述氮化物陶瓷流延浆料经过流延工艺可以连续成膜,得到的湿坯(素坯)表面光滑均匀,无裂纹、空隙等缺陷,干燥后厚度可达0.6mm左右,拉伸强度达到5.0MPa以上,从而保证了陶瓷基片的力学、热学等方面的性能,满足了半导体器件,尤其是大功率半导体器件基片的各项要求。
附图说明
下面结合附图对本发明作进一步说明。
图1示出的是实施例1制备得到的氮化硅流延坯体的照片。
图2示出的是实施例2制备得到的氮化铝流延坯体的照片。
图3示出的是对比例1制备得到的氮化铝流延坯体的照片。
具体实施方式
以下参照具体的实施例来说明本发明。本领域技术人员能够理解,这些实施例仅用于说明本发明,其不以任何方式限制本发明的范围。
下述实施例中的实验方法,如无特殊说明,均为常规方法。下述实施例中所用的原料、试剂材料等,如无特殊说明,均为市售购买产品。
实施例1一种氮化硅陶瓷流延浆料及氮化硅流延坯体
本实施例所述氮化硅陶瓷流延浆料的原料组成,见表1所示,通过如下步骤制备所述流延浆料和流延坯体:
I.按照表1所示,准备各原料;
II.无水乙醇和丁酮混合均匀,得到混合溶剂,将磷酸三乙酯加入所述混合溶剂中,采用磁力搅拌器搅拌2小时,混合均匀,得到液态物料;
III.将氮化硅粉(中位粒径D50=0.5μm)、MgO和Yb2O3加入步骤II得到的液态物料中,转移入球磨罐中,加入1500g氮化硅球,以60转/分钟的速度球磨6小时,得到一次球磨浆料;
IV.向步骤III得到的所述一次球磨浆料中加入PEG,按300转/分钟速度球磨2小时;将PVB和PVC混合均匀,得到粘合剂,平均分为4份,分四次加入,每次球磨6小时,球磨速度为300转/分钟,得到二次球磨浆料;
V.筛网过滤去除步骤IV得到的所述二次球磨浆料中的氮化硅球,加入聚二甲基硅氧烷,用真空除泡机抽真空至10-1Pa,并保持真空30分钟,除去浆料中的气泡,即得所述流延浆料;
VI.调整流延机刮刀厚度为1.2mm,将步骤V制备得到的所述流延浆料导入流延机料槽中,调整传送带速度为3cm/min,底板温度为30℃,流延获得氮化硅流延坯体。
本实施例得到的所述氮化硅流延坯体如图1所示,表面光滑,无裂纹、空隙等缺陷,干燥后坯体厚度达到0.54mm,坯体柔韧,强度良好,拉伸强度达到5.2MPa。
实施例2一种氮化铝陶瓷流延浆料及氮化铝流延坯体
本实施例所述氮化铝陶瓷流延浆料的原料组成,见表1所示,通过如下步骤制备所述流延浆料和流延坯体:
I.按照表1所示,准备各原料;
II.无水乙醇和丁酮混合均匀,得到混合溶剂,将丙烯酸铵加入所述混合溶剂中,采用磁力搅拌器搅拌1小时,混合均匀,得到液态物料;
III.将氮化铝粉(中位粒径D50=1μm)、Al2O3和Y2O3加入步骤II得到的液态物料中,转移入球磨罐中,加入900g氮化铝球,以80转/分钟的速度球磨4小时,得到一次球磨浆料;
IV.向步骤III得到的所述一次球磨浆料中加入PEG,按300转/分钟速度球磨2小时;将PVB和PVC混合均匀,得到粘合剂,平均分为4份,分四次加入,每次球磨6小时,球磨速度为350转/分钟,得到二次球磨浆料;
V.筛网过滤去除步骤IV得到的所述二次球磨浆料中的氮化铝球,加入丙烯酸乳液,用真空除泡机抽真空至10-1Pa,并保持真空20分钟,除去浆料中的气泡,即得所述氮化铝流延浆料;
VI.调整流延机刮刀厚度为1.0mm,将步骤V制备得到的所述流延浆料导入流延机料槽中,调整传送带速度为4cm/min,底板温度为40℃,流延获得氮化铝流延坯体。
本实施例得到的所述氮化铝流延坯体如图2所示,表面光滑,无裂纹、空隙等缺陷,干燥后坯体厚度达到0.62mm,坯体柔韧,强度良好,拉伸强度达到6.4MPa。
实施例3一种氮化硅陶瓷流延浆料及氮化硅流延坯体
该实施例的氮化硅陶瓷流延浆料的原料组成,见表1所示;按照实施例1基本相同的方法和步骤制备所述流延浆料和氮化物流延坯体。得到的坯体表面光滑,无裂纹、空隙等缺陷(照片略),干燥后坯体柔韧且强度良好,拉伸强度达到5.8MPa。
实施例4一种氮化硅陶瓷流延浆料及氮化硅流延坯体
该实施例的氮化硅陶瓷流延浆料的原料组成,见表1所示;按照实施例2基本相同的方法和步骤制备所述流延浆料和氮化物流延坯体。得到的坯体表面光滑,无裂纹、空隙等缺陷(照片略),干燥后坯体柔韧且强度良好,拉伸强度达到7.1MPa。
实施例5一种氮化硅陶瓷流延浆料及氮化硅流延坯体
该实施例的氮化硅陶瓷流延浆料的原料组成,见表1所示;按照实施例1基本相同的方法和步骤制备所述流延浆料和氮化物流延坯体。得到的坯体表面光滑,无裂纹、空隙等缺陷(照片略),干燥后坯体柔韧且强度良好,拉伸强度达到5.3MPa。
对比例1一种氮化硅陶瓷流延浆料及氮化硅流延坯体
该对比例的氮化硅陶瓷流延浆料的原料组成,见表2所示;与实施例1比较,原料组成的不同之处在于粘结剂仅采用PVB,且PVB为复合陶瓷粉体质量的5.6%。通过与实施例1基本相同的步骤和工艺制备流延浆料和流延坯体,不同之处在于:
步骤V中将PVB平均分为4份,分四次加入,进行二次球磨。
但是得到的流延坯体在干燥时发生开裂现象,见图3所示,无法进行后续的烧结步骤。
对比例2一种氮化硅陶瓷流延浆料及氮化硅流延坯体
该对比例的氮化硅陶瓷流延浆料的原料组成,见表2所示;与实施例1比较,原料组成的不同之处在于粘结剂仅采用PVB,且PVB为复合陶瓷粉体质量的7.8%。通过与实施例1基本相同的步骤和工艺制备流延浆料不同之处在于:
步骤V中将PVB平均分为8份,分八次加入,进行二次球磨。
但是得到的二次球磨浆料粘度过高,无法进行后续的真空除泡和流延。
对比例3一种氮化硅陶瓷流延浆料及氮化硅流延坯体
该对比例的氮化硅陶瓷流延浆料的原料组成,见表2所示;与实施例1比较,原料组成的不同之处在于粘结剂(PVB和PVC)为复合陶瓷粉体质量的2.8%,小于本发明优选的粘结剂范围。流延后的得到的氮化硅坯体强度差,无法从流延膜带上顺利剥离,无法进行后续的切片、烧结等步骤。
对比例4一种氮化硅陶瓷流延浆料
该对比例的氮化硅陶瓷流延浆料的原料组成,见表2所示;与实施例1比较,原料组成的不同之处在于粘结剂(PVB和PVC)占复合陶瓷粉体质量的11.2%,大于本发明优选的粘结剂范围。通过与实施例1基本相同的步骤和工艺制备流延浆料不同之处在于:
步骤V中将粘结剂平均分为8份,分8次加入,进行二次球磨。二次球磨浆料粘度过高,丧失流动性,无法进行后续的真空除泡和流延。
对比例5一种氮化硅陶瓷流延浆料及氮化硅流延坯体
该对比例的氮化硅陶瓷流延浆料的原料组成,见表2所示;与实施例1比较,原料组成的不同之处在于粘结剂PVB和PVC的用量比例约为21:1,不在本发明的粘结剂配比范围。流延后的得到的氮化硅坯体在干燥时发生开裂现象。
对比例6一种氮化硅陶瓷流延浆料及氮化硅流延坯体
该对比例的氮化硅陶瓷流延浆料的原料组成,见表2所示;与实施例1比较,原料组成的不同之处在于粘结剂采用PVB和PVC的用量比例约为3:1,不在本发明的粘结剂配比范围。流延后的得到的氮化硅坯体柔韧性差,脆性大,无法进行后续切片等工序。
表1本发明实施例的氮化物流延浆料的原料组成
表2本发明对比例的氮化物流延浆料的原料组成
总之,本发明提供了的氮化物陶瓷流延浆料,通过各组分的配合,尤其是两种粘结剂的配合使用,使该浆料具有适宜的粘度,陶瓷粉体分散均匀,固含量高;由此制备的流延素坯连续成膜,坯体表面光滑均匀,干燥后厚度可达到0.6mm以上,具有良好的力学性能,满足了半导体器件,尤其是大功率半导体器件基片的性能要求。
Claims (10)
1.一种氮化物陶瓷流延浆料,包括:复合陶瓷粉体、混合溶剂、分散剂、增塑剂和粘结剂;其中所述粘结剂包括聚乙烯醇缩丁醛和聚氯乙烯,聚乙烯醇缩丁醛和聚氯乙烯的质量比为20:1~4:1;以所述复合陶瓷粉体的质量为基准,所述粘结剂的质量为所述复合陶瓷粉体质量的3%~10%;
优选地,所述聚乙烯醇缩丁醛和聚氯乙烯的质量比为12:1~6:1。
2.根据权利要求1所述的氮化物陶瓷流延浆料,其特征在于,所述粘结剂由聚乙烯醇缩丁醛和聚氯乙烯组成;
优选地,所述聚乙烯醇缩丁醛的分子量为1500~10000;
优选地,所述聚氯乙烯的分子量为1500~5000;
还优选地,所述粘结剂的质量为所述复合陶瓷粉体质量的5%~10%。
3.根据权利要求1或2所述的氮化物陶瓷流延浆料,其特征在于,所述复合陶瓷粉体的体积占所述氮化物陶瓷流延浆料总体积的32%~42%;
优选地,复合陶瓷粉体包括氮化物粉体和烧结助剂;所述氮化物粉体和所述烧结助剂的质量比为8:2~9.5:0.5;
还优选地,所述氮化物粉体为氮化硅或氮化铝;
优选地,所述氮化硅的粒度为D50=0.3μm-2μm;
优选地,所述氮化铝的粒度为D50=0.5μm-2μm。
4.根据权利要求1至3中任一项所述的氮化物陶瓷流延浆料,其特征在于,所述烧结助剂包括金属氧化物和稀土氧化物,所述金属氧化物和稀土氧化物的质量比为1:1~1:5;所述金属氧化物选自MgO、CaO、TiO2和Al2O3中的一种或一种以上,所述稀土氧化物选自Y2O3、Yb2O3、Er2O3、Ho2O3和CeO2中的一种或一种以上;
优选地,所述金属氧化物和稀土氧化物的质量比为1:1~1:3;
优选地,所述金属氧化物选自MgO、CaO、TiO2和Al2O3中的一种;最优选为MgO、CaO和Al2O3中的一种;
优选地,所述稀土氧化物Y2O3、Yb2O3、Er2O3、Ho2O3和CeO2中的一种;最优选为Y2O3、Yb2O3和Er2O3中的一种;
更优选地,所述烧结助剂选自MgO+Yb2O3、CaO+Er2O3和Al2O3+Y2O3中的一种,其中两种氧化物的质量比为1:1~1:5,更优选为1:1~1:3。
5.根据权利要求1至4中任一项所述的氮化物陶瓷流延浆料,其特征在于,以复合陶瓷粉体的质量为基准,所述混合溶剂的质量为所述复合陶瓷粉体质量的33%~52%;
优选地,所述混合溶剂包括乙醇和丁酮,更优选由乙醇和丁酮组成;乙醇和丁酮的质量比为6:4。
优选地,以所述复合陶瓷粉体的质量为基准,所述分散剂的质量为所述复合陶瓷粉体质量的0.5%~5%,更优选为0.5%~2%;
还优选地,所述分散剂选自磷酸三乙酯、蓖麻油和丙烯酸铵中的一种;
更优选地,所述分散剂选自磷酸三乙酯或蓖麻油;
优选地,以所述复合陶瓷粉体的质量为基准,所述增塑剂的质量为所述复合陶瓷粉体质量的0.15%~1.6%;更优选为0.24%~1.2%;
还优选地,所述增塑剂选自聚乙二醇和邻苯二甲酸丁苄酯中的一种;
还优选地,所述聚乙二醇的分子量为400~600。
6.根据权利要求1至4中任一项所述的氮化物陶瓷流延浆料,其特征在于,所述氮化物陶瓷流延浆料还包括消泡剂,所述消泡剂选自聚醚改性硅、聚二甲基硅氧烷和丙烯酸乳液中的一种;以所述氮化物陶瓷流延浆料的总质量为基准,所述消泡剂的质量占所述氮化物陶瓷流延浆料总质量的0.05%~1%。
7.权利要求1至6中任一项所述氮化物陶瓷流延浆料的制备方法,包括如下步骤:
I.按照配比准备复合陶瓷粉体、混合溶剂、分散剂、增塑剂和粘结剂;
II.将所述分散剂加入所述混合溶剂中,混合均匀,得到液态物料;
III.将所述复合陶瓷粉体加入步骤II得到的液态物料中,转移入球磨设备中,加入球磨介质,进行球磨,得到一次球磨浆料;
IV.向步骤III得到的所述一次球磨浆料中加入所述增塑剂,球磨1~3小时,再加入所述粘结剂,进行二次次球磨,得到二次球磨浆料;
V.筛网过滤去除步骤IV得到的所述二次球磨浆料中的球磨介质,加入所述消泡剂,用除泡设备消泡,即得;
优选地,所述球磨设备为球磨罐;
优选地,所述步骤III中,球磨转速为30转/分钟~200转/分钟,球磨时间为2~12小时;
优选地,所述步骤IV中,球磨转速为150转/分钟~480转/分钟;
优选地,所述步骤IV中,所述粘结剂采用分次等量添加的方法加入;
还优选地,所述步骤IV中,每次添加粘结剂后球磨3~6小时,二次球磨的总时间为12~30小时;
优选地,所述步骤V中,所述消泡设备为真空消泡机,消泡时的真空度为10-1Pa。
8.权利要求1至6中任一项所述氮化物陶瓷流延浆料或根据权利要求7所述制备方法制备得到的氮化物陶瓷流延浆料在制备半导体器件用陶瓷基片中的应用。
9.一种半导体器件用陶瓷基片的流延坯体,采用权利要求1至6中任一项所述氮化物陶瓷流延浆料或根据权利要求7所述制备方法制备得到的氮化物陶瓷流延浆料,经过包括流延成型和坯体干燥的步骤制备得到;
优选地,坯体干燥的温度为20℃~70℃。
10.一种半导体器件用陶瓷基片,由权利要求9所述的流延坯体经过烧结得到。
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