CN111825853A - 一种半导体行业掺杂用复合浆料及固化成膜加工方法 - Google Patents

一种半导体行业掺杂用复合浆料及固化成膜加工方法 Download PDF

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CN111825853A
CN111825853A CN202010716882.7A CN202010716882A CN111825853A CN 111825853 A CN111825853 A CN 111825853A CN 202010716882 A CN202010716882 A CN 202010716882A CN 111825853 A CN111825853 A CN 111825853A
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崔恩密
王毅
崔乐珅
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Sihong Red Core Semiconductor Co ltd
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Abstract

一种半导体行业掺杂用复合浆料及固化成膜加工方法。本发明属于高分子材料领域，尤其涉及半导体行业掺杂用复合浆料及后续固化成型制作方法。本发明一种半导体行业掺杂用复合浆料的固化成膜加工方法，将所述掺杂用复合浆料采用湿法造纸设备加工，其特征在于，在投入所述湿法造纸设备之前，对所述掺杂用复合浆料进行水洗，所述水洗采用去离子水或超纯水。本发明的复合浆料及其成型膜，硬度适中，强度适中，掺杂均匀一致，在国内著名半导体厂家和进口产品做平行对比试验，皆满足产品良率大于99.999%的苛刻指标要求。对实现该类产品进口替代，摆脱对国外进口产品的依赖，起到积极意义。

Description

一种半导体行业掺杂用复合浆料及固化成膜加工方法
技术领域
本发明属于高分子材料领域，尤其涉及半导体行业掺杂用复合浆料及后续固化成型制作方法。
背景技术
现有半导体行业掺杂（扩散工艺），主要采用复合浆料及后续固化成型膜产品，属于小众产品，应用范围极其狭窄。全国饱和市场份额也不过几千万元人民币，同时其又属于高端电子化学品，存在进入门槛高、认证周期漫长、出现质量问题索赔费用大等不利因素。所以罕有大规模资金投入该领域进行研发和生产的行为，故而造成该产品一直长期被国外公司垄断。目前国内市场上是美国进口的FILMTRONICS产品，相关该产品的专利技术在涉及复合浆料配方方面，目前处于保密状态。国内专利仅有CN200510045330.3中提到用喷、涂或粘的方法将浆料至于某一平面之上，待其自然干燥后，再喷、涂或粘一次，如此不断循环，直至涂层达到理想厚度，最终将成膜取下。目前此专利代表该掺杂膜产品行业国内水平，按照这样的工艺流程，是可以制造出膜成品出来，但存在工艺繁琐，溶剂浪费严重，环境污染严重的问题，尤其在狠抓环保的今天，大量的VOC排入大气，哪怕是经过废气处理，也必然会有大量溶剂逃逸，进入大气层，造成经济、环境双方面损失。因此，国内率先开发复合浆料配方及后续固化成型制造技术就显得很有必要。
发明内容
本发明针对以上问题，提供了一种适用于扩散工艺的半导体行业掺杂用复合浆料及固化成膜加工方法。
本发明的技术方案是：掺杂用复合浆料包括以下重量份的组分：
主体树脂30-50，
分散剂3-15，
分散介质15-35，
固体填料20-30，和
掺杂源5-15。
所述的主体树脂为：天然橡胶、聚异戊烯橡胶、端羟基聚丁二烯-苯乙烯橡胶、羟甲基纤维素醚、乙基纤维素、可溶性淀粉、聚乙烯醇、聚乙烯醇缩丁醛、聚乙烯醇缩甲醛或热塑性线性聚氨酯。
所述的分散剂为：聚乙二醇、甲基戊醇或脂肪酸聚乙二醇酯。
所述的分散介质为：甲苯、二甲苯、水、乙醇、丙醇、丁醇、丙酮、醋酸乙酯、醋酸丁酯、二氯甲烷、三氯甲烷、二氯乙烯、三氯乙烯、二甘醇、三甘醇、二甘醇乙醚、二甘醇丁醚中的一种或几种复配。
所述的固体填料为碳酸钙、二氧化硅、二氧化钛、氮化硅、氧化铝、云母粉、高岭土、膨润土、硅藻土或凹凸棒土。
所述的掺杂源为硼源，包括硼单质、硼砂、硼酐、硼酸、三溴化硼、硼酸三甲酯、硼酸三乙酯中的一种或几种复配。
所述的掺杂源为磷源，包括五氧化二磷、磷酸铵、磷单质、聚合磷酸铵、磷酸三甲酯、磷酸三乙酯、磷酸三丁酯、磷酸三苯酚酯、三苯基膦、TCEP、TCPP中的一种或几种复配。
本发明一种半导体行业掺杂用复合浆料的固化成膜加工方法，将所述掺杂用复合浆料采用湿法造纸设备加工，其特征在于，在投入所述湿法造纸设备之前，对所述掺杂用复合浆料进行水洗，所述水洗采用去离子水或超纯水。
本发明的复合浆料及其成型膜，硬度适中，强度适中，掺杂均匀一致，在国内著名半导体厂家和进口产品做平行对比试验，皆满足产品良率大于99.999%的苛刻指标要求。对实现该类产品进口替代，摆脱对国外进口产品的依赖，起到积极意义。
附图说明
图1是本发明成型膜的工作原理示意图；
图中1是高纯单晶硅基材，2是膜材质。
图中箭头方向代表膜中掺杂元素扩散方向。
具体实施方式
下面结合附图1详细表述本发明，本发明采用的掺杂用复合浆料包括以下重量份的组分：
主体树脂30-50，
分散剂3-15，
分散介质15-35，
固体填料20-30，和
掺杂源5-15。
所述的主体树脂为：天然橡胶、聚异戊烯橡胶、端羟基聚丁二烯-苯乙烯橡胶、羟甲基纤维素醚、乙基纤维素、可溶性淀粉、聚乙烯醇、聚乙烯醇缩丁醛、聚乙烯醇缩甲醛或热塑性线性聚氨酯（TPU）。
所述的分散剂为：聚乙二醇、甲基戊醇或脂肪酸聚乙二醇酯。其作用是促进其他成分的均匀分散。
所述的分散介质为：甲苯、二甲苯、水、乙醇、丙醇、丁醇、丙酮、醋酸乙酯、醋酸丁酯、二氯甲烷、三氯甲烷、二氯乙烯、三氯乙烯、二甘醇、三甘醇、二甘醇乙醚、二甘醇丁醚中的一种或几种复配。作为溶剂用。
所述的固体填料为碳酸钙、二氧化硅、二氧化钛、氮化硅、氧化铝、云母粉、高岭土、膨润土、硅藻土或凹凸棒土。
所述的掺杂源为硼源，包括硼单质、硼砂、硼酐、硼酸、三溴化硼、硼酸三甲酯、硼酸三乙酯中的一种或几种复配。主要作为掺入三价元素（如硼、镓），成P型。
所述的掺杂源为磷源，包括五氧化二磷、磷酸铵、磷单质、聚合磷酸铵、磷酸三甲酯、磷酸三乙酯、磷酸三丁酯、磷酸三苯酚酯、三苯基膦、TCEP、TCPP中的一种或几种复配。掺入五价元素（如磷、砷），成N型。
包括一个按照重量比称取主体树脂、分散剂、液体分散介质、固体填料、掺杂源等组份，各成分的重量比如下：
主体树脂30-50
分散剂3-15
分散介质15-35
固体填料20-30
掺杂源5-15
包括一个将上述各组分搅拌均匀，成一定粘度流体的步骤。将上述各组分按重量比称量好，加入带有搅拌功能的匀质釜中，搅拌分散均匀后，即成为掺杂用复合浆料。
浆料制备实施例一：
称取30kg橡胶类材料（天然橡胶、聚异戊烯橡胶或端羟基聚丁二烯-苯乙烯橡胶）作为主体，
称取15kg聚乙二醇作为分散剂；
称取35kg水和乙醇作为分散介质，水和乙醇比例为1:2；
称取30kg碳酸钙作为固体填料，
称取15kg硼砂，
将上述物料均匀搅拌，成粘稠流体状。
浆料制备实施例二：
称取40kg橡胶类材料（羟甲基纤维素醚、乙基纤维素或可溶性淀粉）作为主体，
称取9kg甲基戊醇作为分散剂；
称取25kg甲苯作为分散介质；
称取25kg二氧化钛作为固体填料，
称取10kg硼酸三甲酯，
将上述物料均匀搅拌，成粘稠流体状。
浆料制备实施例三：
称取50kg橡胶类材料（聚乙烯醇、聚乙烯醇缩丁醛、聚乙烯醇缩甲醛或热塑性线性聚氨酯（TPU））作为主体，
称取3kg脂肪酸聚乙二醇酯作为分散剂；
称取15kg三氯乙烯和二甘醇作为分散介质，三氯乙烯和二甘醇比例为1:1；
称取20kg硅藻土作为固体填料，
称取5kg磷单质，
将上述物料均匀搅拌，成粘稠流体状。
本发明一种半导体行业掺杂用复合浆料的固化成膜加工方法，将所述掺杂用复合浆料采用湿法造纸设备加工，在投入所述湿法造纸设备之前，对所述掺杂用复合浆料进行水洗，所述水洗采用去离子水或超纯水。
具体制作时,将上述浆料经抄片机浸入18兆欧以上纯水中，再进入压榨机，随后经干燥成型，成型后的膜片经脱模后，再按客户需要剪裁成相应的尺寸和形状即可。使用过的超纯水通过精馏，可以分别回收分散介质及溶剂，并可循环使用，既减低了成本，也保护了环境，实现资源和社会可持续发展。
上述所得成品膜材料表征参数如下（按四英寸晶圆产品类型计）：
硬度（邵氏硬度）：5-6,
膜厚（微米）：16-18,
PH值（膜材浸入30倍质量纯水中，30分钟后测）：6.8-7.2,
拉伸强度（兆帕）：0.08-0.09,
断裂伸长率（%）：6-9。
本发明制得后具体应用时，如图1所示，将膜2贴附在硅基材1表面，高温扩散，使膜2中目标元素扩散至硅基材1的表面内。
本发明并不局限于上述实施例，在本发明公开的技术方案的基础上，本领域的技术人员根据所公开的技术内容，不需要创造性的劳动就可以对其中的一些技术特征做出一些替换和变形，这些替换和变形均在本发明的保护范围内。

Claims (8)

1.一种半导体行业掺杂用复合浆料，其特征在于，掺杂用复合浆料包括以下重量份的组分：
主体树脂30-50，
分散剂3-15，
分散介质15-35，
固体填料20-30，和
掺杂源5-15。
2.根据权利要求1所述的一种半导体行业掺杂用复合浆料，其特征在于，所述的主体树脂为：天然橡胶、聚异戊烯橡胶、端羟基聚丁二烯-苯乙烯橡胶、羟甲基纤维素醚、乙基纤维素、可溶性淀粉、聚乙烯醇、聚乙烯醇缩丁醛、聚乙烯醇缩甲醛或热塑性线性聚氨酯。
3.根据权利要求1所述的一种半导体行业掺杂用复合浆料，其特征在于，所述的分散剂为：聚乙二醇、甲基戊醇或脂肪酸聚乙二醇酯。
4.根据权利要求1所述的一种半导体行业掺杂用复合浆料，其特征在于，所述的分散介质为：甲苯、二甲苯、水、乙醇、丙醇、丁醇、丙酮、醋酸乙酯、醋酸丁酯、二氯甲烷、三氯甲烷、二氯乙烯、三氯乙烯、二甘醇、三甘醇、二甘醇乙醚、二甘醇丁醚中的一种或几种复配。
5.根据权利要求1所述的一种半导体行业掺杂用复合浆料，其特征在于，所述的固体填料为碳酸钙、二氧化硅、二氧化钛、氮化硅、氧化铝、云母粉、高岭土、膨润土、硅藻土或凹凸棒土。
6.根据权利要求1所述的一种半导体行业掺杂用复合浆料，其特征在于，所述的掺杂源为硼源，包括硼单质、硼砂、硼酐、硼酸、三溴化硼、硼酸三甲酯、硼酸三乙酯中的一种或几种复配。
7.根据权利要求1所述的一种半导体行业掺杂用复合浆料，其特征在于，所述的掺杂源为磷源，包括五氧化二磷、磷酸铵、磷单质、聚合磷酸铵、磷酸三甲酯、磷酸三乙酯、磷酸三丁酯、磷酸三苯酚酯、三苯基膦、TCEP、TCPP中的一种或几种复配。
8.权利要求1所述一种半导体行业掺杂用复合浆料的固化成膜加工方法，将所述掺杂用复合浆料采用湿法造纸设备加工，其特征在于，在投入所述湿法造纸设备之前，对所述掺杂用复合浆料进行水洗，所述水洗采用去离子水或超纯水。
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