CN106190616A - 频率片的腐蚀方法 - Google Patents

频率片的腐蚀方法 Download PDF

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CN106190616A
CN106190616A CN201610549209.2A CN201610549209A CN106190616A CN 106190616 A CN106190616 A CN 106190616A CN 201610549209 A CN201610549209 A CN 201610549209A CN 106190616 A CN106190616 A CN 106190616A
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徐亮
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SUZHOU JING RUI PU TECHNOLOGY Co Ltd
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Abstract

本发明公开了一种频率片的腐蚀方法,首先利用高效清洗液对频率片表面洁净处理,去除脂类、微生物类污渍,为腐蚀打下良好基础;再设计性质温和的腐蚀体系,结合旋转腐蚀工艺,有效对频率片进行腐蚀,腐蚀速度提高到0.3μm/min,远高于现有0.18μm/min,腐蚀后的频率片频率偏差范围从±50KHz下降到±10KHz。

Description

频率片的腐蚀方法
技术领域
本发明属于频率片制备技术,具体涉及一种频率片的腐蚀方法。
背景技术
如今电子产品的功能越来越多,这就要求水晶振动子的精度不断提高,客户对于频率片的频率偏差范围也越来越严格。产品若腐蚀后频率偏差范围越大,产生的不良就越多。频率片的腐蚀后频率偏差范围主要和腐蚀速度、腐蚀体系成分有关,由于每片频率片的密度不一样,腐蚀速度越快则腐蚀后的频率偏差范围越小,反之,则越大。现有腐蚀方法主要是将频率片放入特氟龙网通中,在腐蚀体系中进行上下摇动腐蚀。虽然在上下摇动过程中频率片会散开,但散开的程度并不充分,此时若加快腐蚀速度的话,由于频率片有轻微的重叠现象,会造成有些频率片的腐蚀不均匀,从而造成频率片表面产生厚度差,直接影响客户的CI、DLD等特性不良;腐蚀速度低的话,虽然不会形成厚度差,但会造成腐蚀后频率片的频率偏差过大。若是频率片表面有脏污,即使是很小很淡的脏污,也会影响到客户产品的精度,现有腐蚀将频率片进行上下摇动,这样频率片在摇动过程中无法有效的完全去除频率片表面的异物,干燥后腐蚀体系会残留在频率片的表面,形成脏污。
发明内容
本发明的目的是公开一种频率片的腐蚀方法,配制腐蚀体系体系,配合旋转式腐蚀工艺,腐蚀速度提高到0.3μm/min,远高于现有0.18μm/min,腐蚀后的频率片频率偏差范围从±50KHz下降到±10KHz。
为达到上述发明目的,本发明采用的技术方案是:一种频率片的腐蚀方法,包括以下步骤:
(1)将频率片置入清洗液中,清洗10~15分钟;然后置入酒精中浸泡1~2分钟,红外烘干,得到清洗后的频率片;所述清洗液由萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水组成;
(2)将过氧化钠加入水中,混匀后加入醋酸;搅拌3分钟后再加入离子液体;搅拌15~20分钟后再加入偶氮二异庚腈,搅拌3~5分钟后再加入酒石酸钾钠,搅拌4~6分钟后再加入多孔硅球,搅拌得到腐蚀体系;所述多孔硅球的平均粒径为620纳米;所述离子液体的化学结构式如下:
(3)将腐蚀体系加入腐蚀桶中,然后加入频率片,旋转腐蚀体系;3~3.5分钟后加入絮凝液,继续旋转腐蚀体系,得到腐蚀后的频率片,即完成频率片的腐蚀;所述絮凝液由丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水混合后,于70℃反应1~1.5小时得到。
上述技术方案中,步骤(1)中,清洗是频率片腐蚀的重要基础,如果清洗不彻底的话,残留的污渍,尤其是油脂类、微生物类对极大影响腐蚀体系活性,而且会造成频率片表面腐蚀不均匀。萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水的质量比为3:5:8:3:6:3:100;整体清洗液呈碱性,可以有效去除频率片表面污渍,尤其添加了萘酚化合物、噻唑化合物对去除微生物体系特别有效,关键其活性不受其他成分的影响,通过叔丁基锂、有机钠化合物增加了碱性体系的咬合活性,高分子的聚丙烯酸化合物能够以长链形式去除频率片表面的油脂类污渍;再结合酒精后处理,红外烘干,避免烘箱加热干燥对频率片的损伤,从而可以得到洁净的频率片。
上述技术方案中,步骤(2)中,腐蚀体系腐蚀性平和,腐蚀环境温和,可以克服传统强酸强碱对频率片造成的影响;结合腐蚀工艺,适用于频率片的腐蚀要求,腐蚀后的频率片频率偏差范围从±50KHz下降到±10KHz,此外,利用离子液体(水体系)可以回收的特性,腐蚀体系可以循环利用。现有方法主要是将频率片放入特氟龙网通中,在腐蚀体系中进行上下摇动腐蚀,腐蚀体系多为强酸、强碱体系,否则不能腐蚀频率片,同时腐蚀效率还较低0.18μm/min;本发明配制的腐蚀体系性温和,但是可以对频率片有效腐蚀,添加离子液体与偶氮二异庚腈可以充分发挥腐蚀活性,利用纳米级多孔硅球增加频率片表面的摩擦力,提高腐蚀液的咬合能力,同时硅球质软,不会造成频率片损伤。优选的,过氧化钠、醋酸、离子液体、偶氮二异庚腈、酒石酸钾钠、多孔硅球、水的质量比为8:12:8:1:11:1:100。
上述技术方案中,步骤(3)中,腐蚀体系的高度为腐蚀桶高度的55~65%,不仅防止腐蚀体系溅出,更主要对频率片产生一定的旋转力,使其片片分开而且悬浮在腐蚀体系中;采用旋转方式腐蚀的工艺,将现有摇动腐蚀改为旋转腐蚀的方式,通过旋转使腐蚀体系在腐蚀桶中形成漩涡,利用漩涡的离心力将频率片充分的散开,不会有重叠现象,提高腐蚀速度后也不会造成频率片的腐蚀不均匀,并能大大降低腐蚀后的频率偏差范围,克服了现有技术要么腐蚀厚度不均匀、要么腐蚀后频率误差太大的缺陷。
上述技术方案中,旋转腐蚀体系的方式可以为磁力旋转,比如在腐蚀桶底部设置磁力转子,将腐蚀桶置于磁力盘上,通过转子转动带动腐蚀体系旋转,防止频率片有干扰,可以在桶下部设置大孔滤网以阻隔磁力转子与频率片;还可以为机械旋转,比如将腐蚀桶置入转轴上,转动转轴,从而带动腐蚀桶旋转,进而使得桶内腐蚀体系旋转,也可以将腐蚀桶置于转盘上,通过转盘旋转带动腐蚀桶旋转,进而使得桶内腐蚀体系旋转;还可以为吹气旋转,最能体现本发明的创造性,在腐蚀桶侧壁下部设置进气管,进气管连接气泵,从而可以将气流吹向腐蚀桶内,促使腐蚀体系产生周向运动,从而旋转腐蚀体系,带动频率片转动,此方式最能达到腐蚀均匀的效果,而且不会对频率片产生损伤。
上述技术方案中,絮凝液中,丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水质量比为6:2:4:3:100;频率片的腐蚀开始很快,逐步放平缓,为了避免腐蚀物对频率片的干扰,同时提高腐蚀体系的效率,而且提高腐蚀体系的再利用程度,本发明采用絮凝液,在前期腐蚀后加入,有效提高腐蚀效率以及改善腐蚀效果。
上述技术方案中,频率片的最终腐蚀时间根据对频率片的频率要求而设计,加入腐蚀体系质量0.8~1%的絮凝液后,根据不同产品要求,选择不同的结束腐蚀时间。优选腐蚀桶为圆柱形,防止频率片损伤,而且腐蚀更加均匀,提高产品良率。
本发明首先利用高效清洗液对频率片表面洁净处理,去除脂类、微生物类污渍,为腐蚀打下良好基础;再设计性质温和的腐蚀体系,结合旋转腐蚀工艺,有效对频率片进行腐蚀,腐蚀速度提高到0.3μm/min,远高于现有0.18μm/min,腐蚀后的频率片频率偏差范围从±50KHz下降到±10KHz。
具体实施方式
实施例一
一种频率片的腐蚀方法,包括以下步骤:
(1)将频率片置入清洗液中,清洗15分钟;然后置入酒精中浸泡1分钟,红外烘干,得到清洗后的频率片;所述清洗液由萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水组成;萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水的质量比为3:5:8:3:6:3:100。
(2)将过氧化钠加入水中,混匀后加入醋酸;搅拌3分钟后再加入离子液体;搅拌15分钟后再加入偶氮二异庚腈,搅拌5分钟后再加入酒石酸钾钠,搅拌4分钟后再加入多孔硅球,搅拌得到腐蚀体系;所述多孔硅球的平均粒径为620纳米;过氧化钠、醋酸、离子液体、偶氮二异庚腈、酒石酸钾钠、多孔硅球、水的质量比为8:12:8:1:11:1:100。
(3)将腐蚀体系加入腐蚀桶中,然后加入频率片,旋转腐蚀体系; 3.5分钟后加入腐蚀体系质量0.8%的絮凝液,继续旋转腐蚀体系,得到腐蚀后的频率片,即完成频率片的腐蚀;在腐蚀桶底部设置磁力转子,将腐蚀桶置于磁力盘上,通过转子转动带动腐蚀体系旋转,防止频率片有干扰,在桶下部设置大孔滤网以阻隔磁力转子与频率片;所述絮凝液由丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水混合后,于70℃反应1.5小时得到;丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水质量比为6:2:4:3:10。
实施例二
一种频率片的腐蚀方法,包括以下步骤:
(1)将频率片置入清洗液中,清洗10分钟;然后置入酒精中浸泡2分钟,红外烘干,得到清洗后的频率片;所述清洗液由萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水组成;萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水的质量比为3:5:8:3:6:3:100。
(2)将过氧化钠加入水中,混匀后加入醋酸;搅拌3分钟后再加入离子液体;搅拌20分钟后再加入偶氮二异庚腈,搅拌5分钟后再加入酒石酸钾钠,搅拌4分钟后再加入多孔硅球,搅拌得到腐蚀体系;所述多孔硅球的平均粒径为620纳米;过氧化钠、醋酸、离子液体、偶氮二异庚腈、酒石酸钾钠、多孔硅球、水的质量比为8:12:8:1:11:1:100。
(3)将腐蚀体系加入腐蚀桶中,然后加入频率片,旋转腐蚀体系;将腐蚀桶置于转盘上,通过转盘旋转带动腐蚀桶旋转,进而使得桶内腐蚀体系旋转;3分钟后加入腐蚀体系质量1%的絮凝液,继续旋转腐蚀体系,得到腐蚀后的频率片,即完成频率片的腐蚀;在腐蚀桶底部设置磁力转子,将腐蚀桶置于磁力盘上,通过转子转动带动腐蚀体系旋转,防止频率片有干扰,在桶下部设置大孔滤网以阻隔磁力转子与频率片;所述絮凝液由丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水混合后,于70℃反应1小时得到;丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水质量比为6:2:4:3:10。
实施例三
一种频率片的腐蚀方法,包括以下步骤:
(1)将频率片置入清洗液中,清洗12分钟;然后置入酒精中浸泡2分钟,红外烘干,得到清洗后的频率片;所述清洗液由萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水组成;萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水的质量比为3:5:8:3:6:3:100。
(2)将过氧化钠加入水中,混匀后加入醋酸;搅拌3分钟后再加入离子液体;搅拌18分钟后再加入偶氮二异庚腈,搅拌5分钟后再加入酒石酸钾钠,搅拌4分钟后再加入多孔硅球,搅拌得到腐蚀体系;所述多孔硅球的平均粒径为620纳米;过氧化钠、醋酸、离子液体、偶氮二异庚腈、酒石酸钾钠、多孔硅球、水的质量比为8:12:8:1:11:1:100。
(3)将腐蚀体系加入腐蚀桶中,然后加入频率片,旋转腐蚀体系;在腐蚀桶侧壁下部设置进气管,进气管连接气泵,从而可以将气流吹向腐蚀桶内,促使腐蚀体系产生周向运动,从而旋转腐蚀体系,带动频率片转动,此方式最能达到腐蚀均匀的效果,而且不会对频率片产生损伤;3分钟后加入腐蚀体系质量0.8%的絮凝液,继续旋转腐蚀体系,得到腐蚀后的频率片,即完成频率片的腐蚀;在腐蚀桶底部设置磁力转子,将腐蚀桶置于磁力盘上,通过转子转动带动腐蚀体系旋转,防止频率片有干扰,在桶下部设置大孔滤网以阻隔磁力转子与频率片;所述絮凝液由丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水混合后,于70℃反应1小时得到;丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水质量比为6:2:4:3:10。
本发明设计性质温和的腐蚀体系,结合旋转腐蚀工艺,有效对频率片进行腐蚀,腐蚀速度提高到0.3μm/min,远高于现有0.18μm/min,腐蚀后的频率片频率偏差范围从±50KHz下降到±10KHz。

Claims (9)

1.一种频率片的腐蚀方法,包括以下步骤:
(1)将频率片置入清洗液中,清洗10~15分钟;然后置入酒精中浸泡1~2分钟,红外烘干,得到清洗后的频率片;所述清洗液由萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水组成;
(2)将过氧化钠加入水中,混匀后加入醋酸;搅拌3分钟后再加入离子液体;搅拌15~20分钟后再加入偶氮二异庚腈,搅拌3~5分钟后再加入酒石酸钾钠,搅拌4~6分钟后再加入多孔硅球,搅拌得到腐蚀体系;所述多孔硅球的平均粒径为620纳米;所述离子液体的化学结构式如下:
(3)将腐蚀体系加入腐蚀桶中,腐蚀体系的高度为腐蚀桶高度的55~65%,然后加入频率片,旋转腐蚀体系;3~3.5分钟后加入絮凝液,继续旋转腐蚀体系,得到腐蚀后的频率片,即完成频率片的腐蚀;所述絮凝液由丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水混合后,于70℃反应1~1.5小时得到。
2.根据权利要求1所述频率片的腐蚀方法,其特征在于:步骤(1)中,萘酚化合物、叔丁基锂、异构十三醇聚氧乙烯醚、聚丙烯酸钠、十二水磷酸氢二钠、2-巯基苯并噻唑、水的质量比为3:5:8:3:6:3:100。
3.根据权利要求1所述频率片的腐蚀方法,其特征在于:步骤(2)中,过氧化钠、醋酸、离子液体、偶氮二异庚腈、酒石酸钾钠、多孔硅球、水的质量比为8:12:8:1:11:1:100。
4.根据权利要求1所述频率片的腐蚀方法,其特征在于:步骤(3)中,腐蚀体系的高度为腐蚀桶高度的55~65%。
5.根据权利要求1所述频率片的腐蚀方法,其特征在于:旋转腐蚀体系的方式为磁力旋转。
6.根据权利要求1所述频率片的腐蚀方法,其特征在于:旋转腐蚀体系的方式为机械旋转。
7.根据权利要求1所述频率片的腐蚀方法,其特征在于:旋转腐蚀体系的方式为吹气旋转。
8.根据权利要求1所述频率片的腐蚀方法,其特征在于:丙烯酸、双(2,3-环氧基环戊基)醚、2-丙烯酰胺基-2-甲基丙磺酸、十六烷基三甲基氯化铵、水质量比为6:2:4:3:10。
9.根据权利要求1所述频率片的腐蚀方法,其特征在于:加入腐蚀体系质量0.8~1%的絮凝液。
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