CN111675190A - 一种微型实心硅针的制备方法 - Google Patents

一种微型实心硅针的制备方法 Download PDF

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CN111675190A
CN111675190A CN202010560946.9A CN202010560946A CN111675190A CN 111675190 A CN111675190 A CN 111675190A CN 202010560946 A CN202010560946 A CN 202010560946A CN 111675190 A CN111675190 A CN 111675190A
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silicon nitride
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朱红飞
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Suzhou Hengzhiqing Biotechnology Co ltd
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Abstract

本发明提供一种微型实心硅针的制备方法,首先在单晶硅的表面生长一层二氧化硅，然后在二氧化硅的表面淀积一层氮化硅保护膜，接着在氮化硅保护膜的表面涂覆光刻胶，并对其进行曝光显影、蚀刻等步骤，保护膜采用氮化硅，在蚀刻硅的过程中能够加快蚀刻反应，使得硅针的基座直径更小。本发明工艺简单，实心硅针的耐用性好，适用于生物大分子药物的透皮药物渗透。

Description

一种微型实心硅针的制备方法
技术领域
本发明涉及半导体硅材料表面微加工和制造技术领域，特别涉及一种微型实心硅针的制备方法。
背景技术
由于药物在肠胃中的降解和肝脏的首过效应，绝大部分口服药物在达到作用部位之前就已经大部分或全部失效。此外，患者的用药适应性也是问题，大部分口服给药在治疗期间需要以一定的间隔服药，给患者带来诸多不便。
除此，另一种常见的给药方式是能够使得药物穿透生物屏障的注射给药，包括皮下注射和静脉输入。该种方法虽然有效，但是注射通常都会给患者带来额外的痛感，在注射点也容易造成皮肤局部损伤、出血，增加了疾病传染的风险。
现有一种新型给药技术，即透皮给药。头皮给药指在皮肤表面给药，使得药物以接近恒定速度通过皮肤各层，经毛细血管吸收进入循环产生全身或局部治疗作用的剂型。
中国发明专利CN1569271A公开的微型实心硅针阵列芯片及其制备方法和用途。在该专利中，采用金属膜作为保护膜，制成的微型实心硅针的微针尖部直径为10nm-10μm，微针的底部直径为20-300μm。众所周知，在控制好微针折断率的同时，微针针体直径越小，对人体皮肤造成的创口就越小，也越容易穿透皮肤。
所以，针对以上问题，提出了一种微型实心硅针的制备方法，以制取针体更细，更便于穿透皮肤，造成的创口更小的微型实心硅针。
发明内容
为克服上述现有技术中的不足，本发明目的在于提供一种微型实心硅针的制备方法。
为实现上述目的及其他相关目的，本发明提供的技术方案是：一种微型实心硅针的制备方法，其特征在于，包括以下步骤：
（1）选取单面或双面抛光的单晶硅片，进行清洗及干燥；
（2）先在单晶硅片上生长一层二氧化硅；
（3）然后在二氧化硅上淀积一层氮化硅；
（4）再在氮化硅上旋涂光刻胶，通过光刻工艺将掩膜板上的图案转移至光刻胶上，掩膜板的图案为阵列状圆形斑点，光刻后的光刻胶形成阵列状的圆形遮挡胶膜；
（5）依次去除位于遮挡胶膜外的氮化硅以及下方的二氧化硅，露出单晶硅片；
（6）利用电感耦合等离子体刻蚀系统，采用深硅刻蚀Bosch工艺，对步骤5露出的单晶硅片进行各向异性刻蚀，在单晶硅片上刻蚀出阵列状的圆柱体；
（7）依次去除圆柱体顶端的遮挡胶膜、氮化硅和二氧化硅，通过KOH对圆柱体顶端进行各向同性刻蚀，形成实心微针尖锥针头，并得到微型实心硅针阵列芯片；
（8）然后在微型实心硅针阵列芯片的针体面上涂覆光刻胶，通过光刻工艺将掩膜板上的图案转移至光刻胶上，掩膜版的图案为棋盘状方块，光刻后光刻胶形成方块状遮挡胶膜，然后刻蚀，并于硅针之间形成网格状导流槽，然后去除遮挡胶膜。
优选的技术方案为：所述步骤1中，单晶硅片为N型，电阻率范围为1-10Ω•cm，厚度为700±10μm。
优选的技术方案为：所述步骤2中，单晶硅片按照湿氧-干氧的顺序进行氧化生长一层二氧化硅，氧化温度控制在1100℃以下，湿氧和干氧时间均为5h。
优选的技术方案为：所述步骤3中，PECVD淀积的衬底温度为300-450℃，压强在10-270Pa。
优选的技术方案为：所述PECVD淀积的衬底温度为400℃。
优选的技术方案为：所述步骤3中，采用PECVD在二氧化硅的表面淀积一层200nm厚的氮化硅。
优选的技术方案为：所述步骤5中，通过干法刻蚀掉暴露在遮挡胶膜外的氮化硅，露出二氧化硅，再用湿法蚀刻掉二氧化硅。
优选的技术方案为：所述步骤5中，还可采用离子束对暴露在遮挡胶膜外的氮化硅以及位于氮化硅下方的二氧化硅进行刻蚀。
优选的技术方案为：先采用反应离子刻蚀机对氮化硅进行干法刻蚀，待露出二氧化硅后，再用氟化氢和氢氟酸的混合液湿法蚀刻二氧化硅，直至露出单晶硅片。
优选的技术方案为：所述步骤7中，选用40-80度的KOH溶液进行蚀刻，蚀刻时间30-70min。
由于上述技术方案运用，本发明和现有技术相比具有的优点是：
同样是利用电感耦合等离子体刻蚀系统，采用深硅刻蚀Bosch工艺，对露出的单晶硅片进行各向异性刻蚀，在单晶硅片上刻蚀出阵列状的圆柱体。背景技术中使用金属层作为保护层，而本发明使用氮化硅作为保护层，在深硅蚀刻过程中，氮化硅能够加快内部蚀刻反应，使得圆柱体更细，最终得到的针体直径就更细。
附图说明
图1为采用背景技术方案制成的实心硅针照片。
图2为采用本发明技术方案支撑的实心硅针照片。
图3为本发明技术流程示意图。
图4为本发明步骤4中的掩膜板图案。
图5为本发明步骤8中的掩膜板图案。
具体实施方式
以下由特定的具体实施例说明本发明的实施方式，熟悉此技术的人士可由本说明书所揭露的内容轻易地了解本发明的其他优点及功效。
请参阅图1-图5。须知，在本发明的描述中，需要说明的是，术语“中心”、“上”、“下”、“左”、“右”、“竖直”、“水平”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，或者是该发明产品使用时惯常摆放的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。此外，术语“第一”、“第二”、“第三”等仅用于区分描述，而不能理解为指示或暗示相对重要性。术语“水平”、“竖直”、“悬垂”等术语并不表示要求部件绝对水平或悬垂，而是可以稍微倾斜。如“水平”仅仅是指其方向相对“竖直”而言更加水平，并不是表示该结构一定要完全水平，而是可以稍微倾斜。
在本发明的描述中，还需要说明的是，除非另有明确的规定和限定，术语“设置”、“安装”、“相连”、“连接”应做广义理解，例如，可以是固定连接，也可以是可拆卸连接，或一体地连接，可以是机械连接，也可以是电连接，可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通。对于本领域的普通技术人员而言，可以具体情况理解上述术语在本发明中的具体含义。
实施例：
如图3所示，本实施例中微型实心硅针的制备方法，包括以下步骤：
1）选取（100）晶面，单面或双面抛光的单晶硅片，所选取的单晶硅片为N型，电阻率为5Ω·cm（在实际操作中，选择电阻率范围在1-10Ω·cm，厚度为700±10μm均可）。经标准清洗液RCA1（水:氨水:双氧水的摩尔比为5:1:1）和RCA2（水:盐酸:双氧水的摩尔比为5:1:1）清洗后，用去离子水清洗干净并脱水干燥。
2）将单晶硅片按照湿氧-干氧的顺序进行氧化生长一层二氧化硅，氧化温度控制在1100℃以下，湿氧和干氧时间均为5h。
3）在二氧化硅的表面采用PECVD淀积一层200nm厚的氮化硅，PECVD淀积的衬底温度为300-450℃，压强在10-270Pa。
4）再在氮化硅上旋涂光刻胶，通过光刻工艺将掩膜板上的图案转移至光刻胶上，掩膜板的图案为阵列状圆形斑点（参见图4），光刻后的光刻胶形成阵列状的圆形遮挡胶膜；本实施例中，采用AZ9260型光刻胶，旋涂光刻胶的转速为2500r/min，时间35s，光刻胶膜厚度10μm；然后，将单晶硅片在95℃环境中前烘9min，待单晶硅片自然冷却后进行掩模图形光刻，曝光120s，剂量为1530mJ/cm2，然后在浓度为2 .38％的NMD-W显影液中显影10min，用去离子水冲洗1min，再在100℃环境中坚膜15min，把掩模板图形转移到光刻胶上；掩膜版的图形的圆形斑点的直径为200μm，相邻的圆形斑点的圆心间距为500μm。
5）先采用反应离子刻蚀机对氮化硅进行干法刻蚀，待露出二氧化硅后，再用氟化氢和氢氟酸的混合液湿法蚀刻二氧化硅，直至露出单晶硅片。本实施例中，反应离子刻蚀机功率为100W，CHF3气流量为100sccm，真空度为2.5Pa，刻蚀时间106min。用氟化氢:氢氟酸的混合液（BOE液，6份量40wt%氟化氢和1重量49wt%氢氟酸）湿法蚀刻。
或用离子束对暴露在遮挡胶膜外的氮化硅以及位于氮化硅下方的二氧化硅进行刻蚀，露出单晶硅片。
6）利用电感耦合等离子体刻蚀系统，采用深硅刻蚀Bosch工艺，对步骤5露出的单晶硅片进行各向异性刻蚀，在单晶硅片上刻蚀出阵列状的圆柱体。本实施例中，电感耦合等离子体刻蚀系统功率为1000W，刻蚀与钝化时间6s/4s为一个循环，刻蚀速率为0.4μm/循环，单晶硅片与遮挡胶膜抗刻蚀比为42:1；刻蚀个循环后圆柱体高度为160μm，直径45μm，侧壁与单晶硅片角度为90度。
7）依次去除圆柱体顶端的遮挡胶膜、氮化硅和二氧化硅，通过KOH对圆柱体顶端进行各向同性刻蚀，形成实心微针尖锥针头，并得到微型实心硅针阵列芯片。本实施例中，选用40-80度的KOH溶液进行蚀刻，蚀刻时间30-70min。
8）然后在微型实心硅针阵列芯片的针体面上涂覆光刻胶，光刻胶涂覆厚度超过微针高度，再通过光刻工艺将掩膜板上的图案转移至光刻胶上，掩膜版的图案为棋盘状方块（参见图5），光刻后的光刻胶形成方块状遮挡胶膜，然后刻蚀，并于硅针之间形成网格状的导流槽，最后除去遮挡胶膜，得到带有导流槽的微型实心硅针阵列芯片。
原理：
本发明选用氮化硅作为保护膜，在蚀刻硅的过程中，能够加剧底部硅蚀刻反应，从而使得硅针的基座直径更细。
所以，本发明具有以下优点：
采用深硅刻蚀Bosch工艺，对露出的单晶硅片进行各向异性刻蚀，在单晶硅片上刻蚀出阵列状的圆柱体。背景技术中使用金属层作为保护层，而本发明使用氮化硅作为保护层，在深硅蚀刻过程中，氮化硅能够加快内部蚀刻反应，使得圆柱体更细，最终得到的针体直径就更细。
上述实施例仅例示性说明本发明的原理及其功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神和技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。

Claims (10)

1.一种微型实心硅针的制备方法，其特征在于，包括以下步骤：
（1）选取单面或双面抛光的单晶硅片，进行清洗及干燥；
（2）先在单晶硅片上生长一层二氧化硅；
（3）然后在二氧化硅上淀积一层氮化硅；
（4）再在氮化硅上旋涂光刻胶，通过光刻工艺将掩膜板上的图案转移至光刻胶上，掩膜板的图案为阵列状圆形斑点，光刻后的光刻胶形成阵列状的圆形遮挡胶膜；
（5）依次去除位于遮挡胶膜外的氮化硅以及下方的二氧化硅，露出单晶硅片；
（6）利用电感耦合等离子体刻蚀系统，采用深硅刻蚀Bosch工艺，对步骤5露出的单晶硅片进行各向异性刻蚀，在单晶硅片上刻蚀出阵列状的圆柱体；
（7）依次去除圆柱体顶端的遮挡胶膜、氮化硅和二氧化硅，通过KOH对圆柱体顶端进行各向同性刻蚀，形成实心微针尖锥针头，并得到微型实心硅针阵列芯片；
（8）然后在微型实心硅针阵列芯片的针体面上涂覆光刻胶，通过光刻工艺将掩膜板上的图案转移至光刻胶上，掩膜版的图案为棋盘状方块，光刻后光刻胶形成方块状遮挡胶膜，然后刻蚀，并于硅针之间形成网格状导流槽，然后去除遮挡胶膜。
2.根据权利要求1所述的一种微型实心硅针的制备方法，其特征在于：所述步骤1中，单晶硅片为N型，电阻率范围为1-10Ω·cm，厚度为700±10μm。
3.根据权利要求1所述的一种微型实心硅针的制备方法，其特征在于：所述步骤2中，单晶硅片按照湿氧-干氧的顺序进行氧化生长一层二氧化硅，氧化温度控制在1100℃以下，湿氧和干氧时间均为5h。
4.根据权利要求1所述的一种微型实心硅针的制备方法，其特征在于：所述步骤3中，PECVD淀积的衬底温度为300-450℃，压强在10-270Pa。
5.根据权利要求4所述的一种微型实心硅针的制备方法，其特征在于：所述PECVD淀积的衬底温度为400℃。
6.根据权利要求1所述的一种微型实心硅针的制备方法，其特征在于：所述步骤3中，采用PECVD在二氧化硅的表面淀积一层200nm厚的氮化硅。
7.根据权利要求1所述的一种微型实心硅针的制备方法，其特征在于：所述步骤5中，通过干法刻蚀掉暴露在遮挡胶膜外的氮化硅，露出二氧化硅，再用湿法蚀刻掉二氧化硅。
8.根据权利要求1所述的一种微型实心硅针的制备方法，其特征在于：所述步骤5中，还可采用离子束对暴露在遮挡胶膜外的氮化硅以及位于氮化硅下方的二氧化硅进行刻蚀。
9.根据权利要求7所述的一种微型实心硅针的制备方法，其特征在于：先采用反应离子刻蚀机对氮化硅进行干法刻蚀，待露出二氧化硅后，再用氟化氢和氢氟酸的混合液湿法蚀刻二氧化硅，直至露出单晶硅片。
10.根据权利要求1所述的一种微型实心硅针的制备方法，其特征在于：所述步骤7中，选用40-80度的KOH溶液进行蚀刻，蚀刻时间30-70min。
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