CN110759734B - 一种单晶硅片背面减薄用砂轮及其制备方法 - Google Patents

一种单晶硅片背面减薄用砂轮及其制备方法 Download PDF

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CN110759734B
CN110759734B CN201911057003.8A CN201911057003A CN110759734B CN 110759734 B CN110759734 B CN 110759734B CN 201911057003 A CN201911057003 A CN 201911057003A CN 110759734 B CN110759734 B CN 110759734B
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grinding wheel
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nitrate
abrasive
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史冬丽
马尧
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Hangzhou Xinyanke Semiconductor Materials Co ltd
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Abstract

本发明公开了一种单晶硅片背面减薄用砂轮及其制备方法，先把结合剂原材料溶解于去离子水中，再分别加入磨料、分散剂、单体、交联剂、引发剂,在一定的温度下形成凝胶，再经过干燥、煅烧形成结合剂包覆磨料的混合粉体。再分别加入造孔剂、润湿剂，制备成型料，冷压成型成具有一定形状的成型块，在一定温度下烧结，制成砂轮块。将砂轮块体进行精加工，然后经过粘结，制成硅片减薄砂轮。采用该方法制备的陶瓷结合剂砂轮具有结合剂对磨料的润湿性好、能够显著降低细粒度及超细粒度磨料的团聚、磨料在结合剂中的分散性好、砂轮对硅片的损伤层小等特点。

Description

一种单晶硅片背面减薄用砂轮及其制备方法
技术领域
本发明属于磨具制备技术领域，涉及一种砂轮及其制备方法，具体涉及一种单晶硅片背面减薄用砂轮及其制备方法。
背景技术
对于IC器件所需的单晶硅片，其背面需被磨削达到规定的厚度，然后被分割成各个元件。属于硬脆材料的单晶硅片，由于其脆性高，容易出现崩边、划伤等问题，为了降低其损伤层，一般通过细粒度或超细粒度砂轮进行精密磨削来实现硅片由脆性去除转变为塑性去除。但是，采用传统工艺制造超细粒度砂轮具有很大的难度，陶瓷结合剂砂轮的常用制造工艺是将磨料、结合剂、造孔剂等在混料机中搅拌均匀后，再加入润湿剂，然后冷压成型，烧结、粘结、加工，最终制备出砂轮。使用传统方法制备细粒度砂轮，容易出现以下问题：一方面，当磨料达到细粒度及超细粒度料时，由于其表面活性高，容易出现团聚体，与结合剂难以均匀混合，容易造成硅片表面的划伤；另一方面，由于磨料粒度较细，结合剂粒度也应与其匹配，而且超细粒度的结合剂不易制备且成本较高，同样也容易团聚且难以分散。因此，陶瓷结合剂的制备及超细磨料的分散问题制约着高精密磨具的发展。而本发明就是为了解决这一问题，一方面，通过原材料在去离子水中的溶解，实现了结合剂自身的均匀混合，达到分子水平的均匀混合，另一方面，通过分散剂的加入，降低了磨料间的聚集，同时通过吸附作用，结合剂也能够均匀包裹在磨料的周围，进一步降低了磨料的团聚。
发明内容
本发明的目的是针对硅片减薄过程中，砂轮中磨料的团聚体会对硅片表面进行划伤的问题，提供了一种降低磨料团聚，改善磨料的分散性的一种细粒度及超细粒度陶瓷结合剂砂轮的制备方法。
本发明为解决其技术问题所采用的技术方案为：
一种硅片背面减薄砂轮的制备方法，其特征在于，所述方法包括以下步骤：
SS1.将正硅酸乙酯、无水乙醇、去离子水在容器中水解，形成氧化硅水溶胶；
SS2.将硝酸钠、硝酸钙、硝酸镁、硝酸锂、硝酸铝、硼酸溶解于水中，搅拌均匀后形成盐溶液；
SS3.将步骤SS1制备的氧化硅水溶胶加入到步骤SS2制备的盐溶液中，搅拌均匀；
SS4.将磨料、分散剂加入到步骤SS3制备的混合溶液中，超声分散均匀，形成悬浮液；
SS5.将单体、交联剂、引发剂分别加入到步骤SS4制备的悬浮液中形成凝胶；
SS6.将步骤SS5制备的凝胶在一定的温度下干燥，形成干凝胶；
SS7.将步骤SS6制备的干凝胶在一定的温度下煅烧，形成陶瓷粉体；
SS8.将步骤SS7制备的陶瓷粉体分别加入造孔剂、润湿剂，得到成型料；
SS9.将步骤SS8制备的成型料冷压成型后，在一定的温度下烧结，形成具有一定形状的块体；
SS10.将步骤SS9烧结的块体进行精加工，制成所需尺寸的砂轮块体；
SS11.将步骤SS10的砂轮块粘结在基体上，制备成砂轮；
SS12.将步骤SS11制备的砂轮进行精加工后得到成品。
优选地，以体积计，所述步骤SS1中制备的氧化硅水溶胶所需的各成分组成如下：正硅酸乙酯体积分数50-60％、无水乙醇体积分数26-35％、去离子水体积分数15-25％。
优选地，以质量计，所述步骤SS2中盐溶液中各组分的组成如下：硝酸钠8-15％、硝酸钙9-16％、硝酸镁12-18％、硝酸锂12-20％、硝酸铝29-38％、硼酸8-15％。
优选地，以质量计，所述步骤SS4中悬浮液的组成是：磨料3-8％、分散剂1-6％、盐溶液75-85％、氧化硅溶胶8-15％。
优选地，所述步骤SS5中，单体为丙烯酰胺、交联剂为N,N-亚甲基双丙烯酰胺、引发剂为过硫酸铵。
优选地，以质量计，所述步骤SS5中形成凝胶的各成分组成：单体6-12％、交联剂1-4％、引发剂0.2-1.2％、悬浮液86-95％。
优选地，所述步骤SS6中，凝胶的干燥温度120-180℃，干燥时间5-8h。
优选地，所述步骤SS7中，凝胶的煅烧温度为580-630℃，煅烧时间为3-8h。
优选地，所述步骤SS8中，以质量计，成型料的各成分如下：含磨料及结合剂的混合粉体80-90％、造孔剂2-8％、润湿剂8-10％。
优选地，所述步骤SS9中，烧结温度为650-750℃，保温时间2-6h。
优选地，所述步骤SS4中，所述磨料为：普通金刚石、含硼金刚石、碳化硅、立方碳化硅的任一种或几种。
优选地，所述步骤SS8中，所述造孔剂为树脂粉、树脂空心球、精萘、糊精粉。
优选地，所述步骤SS8中，所述润湿剂为石蜡、糊精液、聚乙烯醇溶液、水玻璃液。
优选地，所述步骤SS4中，所述磨料的粒度为0.1-10μm。
根据本发明的另一方面，还提供了一种硅片背面减薄砂轮，所述砂轮根据本发明上述的方法制备得到。
同现有技术相比，本发明的单晶硅片背面减薄用砂轮及其制备方法，先把结合剂原材料溶解于去离子水中，再分别加入磨料、分散剂、单体、交联剂、引发剂,在一定的温度下形成凝胶，再经过干燥、煅烧形成结合剂包覆磨料的混合粉体。再分别加入造孔剂、润湿剂，制备成型料，冷压成型成具有一定形状的成型块，在一定温度下烧结，制成砂轮块。将砂轮块体进行精加工，然后经过粘结，制成硅片减薄砂轮。采用该方法制备的陶瓷结合剂砂轮具有结合剂对磨料的润湿性好、能够显著降低细粒度及超细粒度磨料的团聚、磨料在结合剂中的分散性好、砂轮对硅片的损伤层小等特点。
具体实施方式
为了更好的理解本发明，下面结合实施例进一步阐明本发明的内容，以使本发明的优点和特征能更易于被本领域技术人员理解。需要说明的是，以下所述仅为本发明的较佳实施例，但本发明的内容不局限于下面的实施例。实际上，在未背离本发明的范围或精神的情况下，可以在本发明中进行各种修改和变化，这对本领域技术人员来说将是显而易见的。例如，作为一个实施例的一部分示出或描述的特征可以与另一个实施例一起使用来产生又一个实施例。因此，意图是本发明将这样的修改和变化包括在所附的权利要求书和它们的等同物的范围内。
实施例1
SS1.将40ml正硅酸乙酯、20ml无水乙醇、12ml去离子水，在烧杯中水解，形成氧化硅溶胶；
SS2.将11.65g硝酸钠、13.12g硝酸钙、13.89g硝酸镁、14.68g硝酸锂、34.59g硝酸铝、12.07g硼酸溶解于500ml水中，搅拌均匀后形成盐溶液；
SS3.将步骤SS1的制备的氧化硅溶胶加入到步骤SS2制备的盐溶液中，搅拌均匀；
SS4.将25g金刚石、22g聚乙烯醇加入到步骤SS3制备的混合溶液中，超声分散均匀，形成悬浮液；
SS5.将55g丙烯酰胺、10.5g N,N-亚甲基双丙烯酰胺、2.5g过硫酸铵加入到步骤SS4制备的悬浮液中形成凝胶；
SS6.将步骤SS5制备的凝胶在150℃的干燥箱中干燥8h，形成干凝胶；
SS7.将步骤SS6制备的干凝胶在600℃下煅烧4h，形成粉体；
SS8.按照上述方法制备100g含磨料及结合剂的粉体，分别加入8g造孔剂、10g石蜡，得到成型料；
SS9.将步骤SS8制备的成型料冷压成型，烧结温度720℃，保温时间2h，制成具有一定形状的块体；
SS10.将步骤SS9烧结的块体的进行精加工，制成所需尺寸的砂轮块体；
SS11.将步骤SS10的砂轮块粘结在基体上，制备成砂轮；
SS12.将步骤SS11制备的砂轮进行精加工，再检查，合格后得到成品。
所述磨料为金刚石，粒度为2.5μm，所述造孔剂为树脂微球本。
实施例2
SS1.将40ml正硅酸乙酯、20ml无水乙醇、12m去离子水，在烧杯中水解，形成氧化硅溶胶；
SS2.将11.65g硝酸钠、13.12g硝酸钙、13.89g硝酸镁、14.68g硝酸锂、34.59g硝酸铝、12.07g硼酸溶解于500ml水中，搅拌均匀后形成盐溶液；
SS3.将步骤1的制备的氧化硅溶胶加入到步骤2制备的盐溶液中，搅拌均匀；
SS4.将31.5g含硼金刚石、3.5g立方碳化硅、35g聚乙烯醇加入到步骤3制备的混合溶液中，超声分散均匀，形成悬浮液；
SS5.将55g丙烯酰胺、10.5g N,N-亚甲基双丙烯酰胺、2.5g过硫酸铵加入到步骤4制备的悬浮液中形成凝胶；
SS6.将步骤5制备的凝胶在150℃的干燥箱中干燥8h，形成干凝胶；
SS7.将步骤6制备的干凝胶在600℃下煅烧4h，形成粉体；
SS8.按照上述方法制备100g含磨料及结合剂的粉体，分别加入8g造孔剂、10g石蜡，得到成型料；
SS9.将步骤8制备的成型料冷压成型，烧结温度750℃，保温时间2h，制成具有一定形状的块体；
SS10.将步骤9烧结的块体的进行精加工，制成所需尺寸的砂轮块体；
SS11.将步骤10的砂轮块粘结在基体上，制备成砂轮；
SS12.将步骤SS11制备的砂轮进行精加工，再检查，合格后得到成品。
所述磨料为金刚石和碳化硅，金刚石粒度为7μm，立方碳化硅粒度为5μm，所述造孔剂为树脂微球。
实施例3
SS1.将40ml正硅酸乙酯、20ml无水乙醇、12m去离子水，在烧杯中水解，形成氧化硅溶胶；
SS2.将11.65g硝酸钠、13.12g硝酸钙、13.89g硝酸镁、14.68g硝酸锂、34.59g硝酸铝、12.07g硼酸溶解于500ml水中，搅拌均匀后形成盐溶液；
SS3.将步骤SS1的制备的氧化硅溶胶加入到步骤2制备的盐溶液中，搅拌均匀；
SS4.将18g金刚石、20g聚乙烯醇加入到步骤3制备的混合溶液中，超声分散均匀，形成悬浮液；
SS5.将55g丙烯酰胺、10.5g N,N-亚甲基双丙烯酰胺、2.5g过硫酸铵加入到步骤4制备的悬浮液中形成凝胶；
SS6.将步骤SS5制备的凝胶在150℃的干燥箱中干燥8h，形成干凝胶；
SS7.将步骤SS6制备的干凝胶在600℃下煅烧4h，形成粉体；
SS8.按照上述方法制备100g含磨料及结合剂的粉体，分别加入6g造孔剂、10g石蜡，得到成型料；
SS9.将步骤SS8制备的成型料冷压成型，烧结温度720℃，保温时间2h，制成具有一定形状的块体；
SS10.将步骤SS9烧结的块体的进行精加工，制成所需尺寸的砂轮块体；
SS11.将步骤SS10的砂轮块粘结在基体上，制备成砂轮；
SS12.将步骤SS11制备的砂轮进行精加工，再检查，合格后得到成品。
所述磨料为金刚石，粒度为0.5μm，所述造孔剂为树脂微球。
为了比较本发明所制备砂轮的使用性能，同时使用传统方法按照实施例1、实施例2、实施例3同样的配方分别制备了对比例1、对比例2、对比例3砂轮。使用这六种砂轮分别磨削8英寸单晶硅片，减薄厚度200μm。为了表征硅片的表面质量，在硅片磨削面取6个不同位置，分别测试其表面粗糙度，实施例1～3及对比例1～3中硅片磨削面各测试位置的表面粗糙度结果如下表1所示。根据表1示出的磨削结果可以看到，使用本发明制备的砂轮对单晶硅片进行背面减薄后硅片表面的粗糙度要优于对比例，粗糙度的最大偏差也小于对比例。实施例制备的砂轮磨削硅片后会有轻微的磨削纹，对比例磨削后会有明显的磨削纹。
表1硅片磨削面各测试位置的表面粗糙度结果
Figure BDA0002256799700000081
以上所述的具体实施例，对本发明的目的、技术方案和有益效果进行了进一步详细说明。所应理解的是，以上所述仅为本发明的具体实施例而已，并不用于限制本发明，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (2)

1.一种硅片背面减薄砂轮的制备方法，其特征在于，所述方法包括以下步骤：
SS1.将正硅酸乙酯、无水乙醇、去离子水在容器中水解，形成氧化硅水溶胶，其中，以体积计，正硅酸乙酯的体积分数为50-60％、无水乙醇的体积分数为26-35％、去离子水的体积分数为15-25％，各组分用量百分数之和等于100％；
SS2.将硝酸钠、硝酸钙、硝酸镁、硝酸锂、硝酸铝、硼酸溶解于水中，搅拌均匀后形成盐溶液，其中，以质量计，硝酸钠8-15％、硝酸钙9-16％、硝酸镁12-18％、硝酸锂12-20％、硝酸铝29-38％、硼酸8-15％；
SS3.将步骤SS1制备的氧化硅水溶胶加入到步骤SS2制备的盐溶液中，搅拌均匀得氧化硅水溶胶与盐溶液的混合溶液；
SS4.将磨料、分散剂加入到步骤SS3制备的混合溶液中，超声分散均匀，形成悬浮液，其中，以质量计，磨料3-8％、分散剂1-6％、盐溶液75-85％、氧化硅水溶胶8-15％，所述磨料为普通金刚石、含硼金刚石、碳化硅、立方碳化硅中的任一种或几种，所述磨料的粒度为0.1-10μm；
SS5.将单体、交联剂、引发剂分别加入到步骤SS4制备的悬浮液中形成凝胶，其中，以质量计，单体6-12％、交联剂1-4％、引发剂0.2-1.2％、悬浮液86-95％，各组分用量百分数之和等于100％；所述单体为丙烯酰胺、交联剂为N,N-亚甲基双丙烯酰胺、引发剂为过硫酸铵；
SS6.将步骤SS5制备的凝胶在一定的温度下干燥，形成干凝胶，其中，凝胶的干燥温度120-180℃，干燥时间5-8h；
SS7.将步骤SS6制备的干凝胶在580-630℃的温度下煅烧3-8h，形成含磨料及结合剂且结合剂包覆磨料的混合陶瓷粉体；
SS8.将步骤SS7制备的陶瓷粉体分别加入造孔剂、润湿剂，得到成型料，其中，以质量计，成型料的各成分如下：含磨料及结合剂的混合陶瓷粉体80-90％、造孔剂2-8％、润湿剂8-10％，各组分用量百分数之和等于100％，所述造孔剂为树脂粉、树脂空心球、精萘或糊精粉，所述润湿剂为石蜡、糊精液、聚乙烯醇溶液或水玻璃液；
SS9.将步骤SS8制备的成型料冷压成型后，在650-750℃的温度下烧结2-6h，形成具有一定形状的块体；
SS10.将步骤SS9烧结的块体进行精加工，制成所需尺寸的砂轮块体；
SS11.将步骤SS10的砂轮块粘结在基体上，制备成砂轮；
SS12.将步骤SS11制备的砂轮进行精加工后得到成品。
2.一种硅片背面减薄砂轮，所述砂轮根据权利要求1所述的方法制备得到。
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