CN1012071B - 含有环状氟化磺酸盐表面活性剂蚀刻溶液 - Google Patents
含有环状氟化磺酸盐表面活性剂蚀刻溶液Info
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Abstract
本发明提供了具有可溶性表面添加剂的二氧化硅蚀刻溶液。改进的二氧化硅蚀刻剂是由把可溶性表面添加剂添加到集成电路制作中的标准的氧化物蚀刻剂中而获得的。本发明的有效表面活性剂称为氟化环烷烃磺酸盐和氟化环烯烃磺酸盐，一般式如下：
式中：X是F、H、Cl、OH、SO3A或R，Y是F、H、OH、R或略去，从而给予双键；其中R是1-4氟烷基；其中n值小于等于6。A表示阳离子组，可以是NH4 +、H+、Na+、K+、Li+、R+或有机胺阳离子。
Description
本申请案是我们在1984年4月26日提出的流水号为604112的共同待批的，现在是美国专利第4517106号的部分继续申请。
本发明涉及改进含有可溶性表面活性添加剂的蚀刻溶液的组分。这些添加剂能够降低基片的表面张力以改进湿润，并且可用于集成电路制作。具体地说，本发明涉及用氟化环烷烃磺酸盐和（或）氟化环烯烃磺酸盐作抑制表面张力的添加剂的应用。
随着集成电路元件尺寸的小型化，基片表面用蚀刻溶液作物理润湿也变得越来越困难了。特别是本发明可作为二氧化硅蚀刻中所用的氟化铵/氢氟酸氧化物蚀刻溶剂的缓冲剂，因为这些溶液在典型的蚀刻温度下，呈现极高的表面张力，其数值为85-90达因/厘米。由于所用的掩蔽材料的表面能量相当低，光刻外形，存在的杂质的类型以及从其他加工工序中来的残留污染物，所以难以完完全全地润湿基片，从而导致蚀刻不均以及线条复制不好。
为了解决这些问题，集成电路工业的大部分均已采用至少二种公知技术中的一种技术。第一种是把基片置于蚀刻剂前，先在表面活性剂水溶液中预浸，而第二种是把表面活性剂直接添加在蚀刻剂溶液中。然而，由于该项工业是朝着较无颗粒的系统发展。而该系统是使用再度过滤箱的，并且还要求较精确蚀刻且偏差较小的线条，所以现有的方法有一些不足之处。对于采用预浸的方法来说，除了增添了一个额外的处理工序之外，还需要两只箱。此外，因为要预浸薄片，就会有物质从预浸箱带到蚀刻箱的趋势，这样就改变了蚀刻剂的性能并且缩短了其使用寿命。更为严重的是，这些方法主要缺点均与上述的两个方面有关，正如经验所指出的那样，工业上通常所用的大多数表面活性剂都是不溶于氟化铵/氢氟酸氧化物蚀刻剂溶液，这就引起表面活性剂分离而覆在基片表面，从而使循环蚀刻槽
中通常所用的过滤器（大约为0.2微米）堵塞，这样，使得蚀刻剂溶液中几乎没有表面活性剂存在。另外，所用的表面活性剂可包含一些金属离子杂质;由于蚀刻剂中有氢氟酸而引起表面活性剂降解，这些杂质可损害集成电路的性能或者使之丧失作用。一些蚀刻剂制备已试图把表面活性剂溶合到其氧化物蚀刻溶液里。然而，这些物质的分析表明几乎没有，如果有，表面活性剂也仅按表面张力测定所指示是存在的。故而，需要一种经改进的、有效的且具有低表面张力的二氧化硅蚀刻剂溶液是显而易见的，其中表面活性剂在通过0.2微米独立过滤器过滤之后在氟化胺/氢氟酸溶液中保持表面活性，并且基本上无金属离子。
在我们的1984年4月26日提交的流水号为604112的在先申请案中，曾叙述了应用线性和高度支化的氟化烷基磺酸盐作为氟化铵/氢氟酸氧化物蚀刻剂缓冲溶液中的可溶性添加剂，其后业已弄清楚某些氟化环类物质可提供极好的润湿。因此，这些添加剂在0.2微米过滤之后仍留在溶液中，并且金属离子污染低，具有这些添加剂的蚀刻剂的表面张力一般小于30达因/厘米，而没有表面活性添加剂的蚀刻剂的表面张力为85-90达因/厘米。
本发明的有效的表面活性剂是氟化环烷烃磺酸盐和氟化环烯烃磺酸盐，它们具有以下的一般式：
式中：X可以是F、H、Cl、OH、SO3A或R，Y可以是F、H、OH、R或略去R，从而给予双键;其中R是1-4氟环基;其中n为小于等于6的一个数值。这些物质具有良好的可溶性，不会被0.2微米过滤去除。A表示阳离子组，可以是NH+ 4、H+、Na+、K+、Li+、R+或有机胺阳离子，即NR+ 4、其中R是1-4个碳的烷基。此处金属离子，例如Na、K及Li的盐可能有害于集成电路的电性能，比如首先应略去Li、Na、K、Ca及Mg的离子。值得注意的是，看来这些物质在连续过滤槽中并未被去除，也不堵塞过滤器或者分离覆在基片表面上。
因此，本发明的目的旨在提供一系列二氧化硅蚀刻溶液，这些溶液具有所要求的蚀刻速率和优于已有技术的蚀刻溶液的润湿性，这些经改进的蚀刻剂在过滤之后仍保持其表面活性。
本发明的另一个目的旨在提供一系列这样的蚀刻溶液，即这些溶液在0.2微米过滤之后基本上无金属离子，在相同的蚀刻温度下，具有与已有技术溶液相同的蚀刻速率，并具有较好的改善蚀刻均匀性的润湿性，以及不留下残余作物或者不有害于光刻粘合。
本发明的目的是这样实现的：本发明所提供的蚀刻溶液包含氟化氢和氟化铵的水溶液，其中氟化氢（HF）大约为1-12（重量）%，氟化铵（NH4F）大约为13.5-40.5（重量）%以及少量表面活性剂，大约为25-20000ppm。
最佳实施例
本发明的有效的表面活性剂被称为氟化环烷烃磺酸盐和氟化环烯烃磺酸盐，其一般式如下：
式中：X可以是F、H、Cl、OH、SO3A或R，Y可以是F、H、OH、R或略去R，从而给予双键;其中R是1-4氟烷基;n为小于等于6的一个数值。最佳化合物含有4-9个碳。这些物质具有良好的可溶性，经0.2微米过滤不被去除。典型的阳离子组，可以是NH+ 4、H+、Na+、K+、Li+、R+或者有机胺阳离子，即NR+ 4、其中R是1-4个碳的烷基。然而，此处离子含量相当高的盐，比如Na、K、Li盐可能有害于电路的电性能，所以包含这种离子的物质应当略去，“低金属离子含量”一词指的是略去周期表中Ⅰ和Ⅱ族的任何大量的金属离子，主要是Li、Na、K、Ca及Mg离子。
本发明的新型蚀刻溶液在0.2微米过滤之后，甚至在连续过滤的条件下均能保持其表面活性。因此，尽管经过滤，本发明的新型溶液仍较有效地具有润湿基片的性能，并且在没有对已有技术的溶液附加任何有害影响的情况下，以相同的速率，通过
蚀刻绘有图形的保护层中的小几何形状（1-5微米）和大几何形状（＞5微米）的氧化物获得较均匀的效果。
本发明的NF-NF4F溶液可以通过把规定比例的组分溶解在水中的任何方法制备。然而，我们优先采用分别混合HF和NH4F
单个组分的水溶液。我们发现含有氟化氢大约49（重量）%的标准HF溶液很适合此目的。很清楚，可以应用HF浓度高的醚溶液。当应用这种含HF49%的溶液时，必需使用NH4F浓度大约为15-40（重量）%的氟化铵溶液，经混合，溶液含有二种组分的所要求的相对比例。可以应用1重量份的49（重量）%的氟化氢水溶液与4-100体积份的15-48（重量）%的氟化铵的水溶液的掺合物。这种掺合物形成含有大约1-11（重量）%的HF和大约13.5-40.5（重量）%的NH4F
以及其余为水的混合物，再把一种低金属离子型的可溶解的优先采用的氟化环烷烃磺酸盐和（或）氟化环烯烃磺酸盐添加到该混合物中，该溶液经0.2微米过滤器过滤。当然，也可以制备不同浓度的HF和NH4F。
作为有效的表面活性剂添加的所确定的有效浓度范围是20-20000ppm。可以以固体或者以含水的极性溶剂的混合的溶液添加。所要求的浓度范围是200-5000ppm的有效表面活性剂。
在有些应用范围中，可以添加合适的稀释剂以抑制腐蚀作用。合适的稀释剂包括诸如醋酸、乙二醇以及低级烷基醇等，它们具有1-3个碳原子。
以下用具体的实施例进一步叙述本发明。但是，应当认为，虽然这些实施例可以详细地叙述本发明的一些最佳的操作条件，然而，这些主要是为了说明，本发明的范围并不限于此。
实施例1-6
将250ppm表面活性剂添加到氟化铵27（重量）%、氢氟酸6（重量）%以及其余为水的溶液中。采用F19-核磁共振和质谱测定法完成表面活性剂的分析。表面张力使用杜诺林张力计（Du Nouy Ring tensiometer）在25℃下测定。溶液（如表Ⅰ所示）通过0.2μm坦弗隆（Te FLo N）碳氟聚合物过滤，并且再用相同的方法测定表面张力。
表Ⅰ中的测定结果表明，全氟环己基磺酸及其全氟辛基衍生物钾盐和支化的全氟辛基磺酸的钾盐如表面张力测定所示并未显著地去除。然而，表面张力测定结果表明，线性全氟辛基磺酸的钾盐在过滤时基本上自溶液中被去除。
由此可见，具有C8链长的线性氟化磺酸盐被除去，反之，同样质量的氟化环烷基磺酸盐和支化的全氟烷基磺酸盐仍留在溶液中。
Claims (10)
1、一种包含可溶性表面活性剂且阻止表面活性剂沉淀的蚀刻溶液，其特征在于所说的溶液包括氟化铵和表面活性剂的一种水状混合物，所说混合物含有氟化铵(NH4F)13.5-40.5(重量)%以及具有以下结构式的氟化环烷烃磺酸盐和(或)氟化环烯烃磺酸盐25-2000ppm，
式中：n为小于等于6的一个数值，X可以是F、Cl、H、OH、SO4A、R或者可略去R，Y可以是F-、Cl、H、OH-、R或者可略去R、A可以是H+、NH+、Na+、K+、Li+、R+或者NR+ 4，其中R为1-4个碳原子的烷基和(或)氟烷基及它们的混合物，其余为水。
2、如权利要求1所说的一种蚀刻溶液，其特征在于所说的溶液含有高达11（重量）%的氟化氢。
3、如权利要求1所说的一种蚀刻溶液，其特征在于所说的氟化环类表面活性剂中“n”为小于等于6的一个数值。
4、如权利要求1所说的一种蚀刻溶液，其特征在于所说的氟化环类表面活性剂是具有低金属离子含量的铵盐。
5、如权利要求1所说的一种蚀刻溶液，其特征在于所说的氟化环烷烃或者环烯烃磺酸盐是氟化环烷烃或者环烯烃磺酸。
6、如权利要求1所说的一种蚀刻溶液，其特征在于所说的氟化环表面活性剂的存在量为200-5000ppm，并以干燥固体或者以极性水溶剂混合的溶液添加到蚀刻溶液中。
7、如权利要求1所说的一种蚀刻溶液，其特征在于所说的溶液含有高达11（重量）%的氟化氢、200-500ppm的氟化环类表面活性剂以及减少腐蚀的稀释剂。
8、如权利要求2所说的一种蚀刻溶液，其特征在于所说的溶液含有高达50（重量）%的用于降低腐蚀的稀释剂，所说稀释剂是由醋酸、乙二醇以及1-3个碳原子的醇组成的组中选择的。
9、一种制备蚀刻溶液的方法，其特征在于所说的方法包括将49（重量）%的氟化氢水溶液和15-40（重量）%的氟化铵水溶液掺合，并添加200-5000ppm的有效的氟化环类表面活性剂。
10、如权利要求9所说的方法，其特征在于所说的氟化铵水溶液含有大约30（重量）%的NH4F。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US733568 | 1985-05-13 | ||
| US06/733,568 US4620934A (en) | 1984-04-26 | 1985-05-13 | Soluble fluorinated cycloalkane sulfonate surfactant additives for NH4 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86103055A CN86103055A (zh) | 1986-11-26 |
| CN1012071B true CN1012071B (zh) | 1991-03-20 |
Family
ID=24948178
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86103055A Expired CN1012071B (zh) | 1985-05-13 | 1986-04-29 | 含有环状氟化磺酸盐表面活性剂蚀刻溶液 |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US4620934A (zh) |
| EP (1) | EP0201808B1 (zh) |
| JP (1) | JPH0694596B2 (zh) |
| KR (1) | KR900003980B1 (zh) |
| CN (1) | CN1012071B (zh) |
| CA (1) | CA1276530C (zh) |
| DE (1) | DE3689962T2 (zh) |
Families Citing this family (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4761244A (en) * | 1987-01-27 | 1988-08-02 | Olin Corporation | Etching solutions containing ammonium fluoride and an alkyl polyaccharide surfactant |
| US4863563A (en) * | 1987-01-27 | 1989-09-05 | Olin Corporation | Etching solutions containing ammonium fluoride and a nonionic alkyl amine glycidol adduct and method of etching |
| US4761245A (en) * | 1987-01-27 | 1988-08-02 | Olin Corporation | Etching solutions containing ammonium fluoride and an alkylphenol polyglycidol ether surfactant |
| EP0416012B1 (en) * | 1988-05-16 | 1993-11-24 | Olin Corporation | Etching solutions containing anionic sulfate esters of alkylphenol polyglycidol ethers |
| EP0691676B1 (en) * | 1993-02-04 | 1999-05-12 | Daikin Industries, Limited | Wet-etching composition for semiconductors excellent in wettability |
| US5320709A (en) * | 1993-02-24 | 1994-06-14 | Advanced Chemical Systems International Incorporated | Method for selective removal of organometallic and organosilicon residues and damaged oxides using anhydrous ammonium fluoride solution |
| GB9621949D0 (en) * | 1996-10-22 | 1996-12-18 | Molloy Malachy J | Floor and tile anti-slip treatment |
| DE19805525C2 (de) * | 1998-02-11 | 2002-06-13 | Sez Semiconduct Equip Zubehoer | Verfahren zum Naßätzen von Halbleiterscheiben zum Erzeugen eines definierten Randbereichs durch Unterätzen |
| US5939336A (en) * | 1998-08-21 | 1999-08-17 | Micron Technology, Inc. | Aqueous solutions of ammonium fluoride in propylene glycol and their use in the removal of etch residues from silicon substrates |
| US6670281B2 (en) * | 1998-12-30 | 2003-12-30 | Honeywell International Inc. | HF etching and oxide scale removal |
| US6248704B1 (en) | 1999-05-03 | 2001-06-19 | Ekc Technology, Inc. | Compositions for cleaning organic and plasma etched residues for semiconductors devices |
| AU2001274038A1 (en) * | 2000-05-25 | 2001-12-03 | Max Braun | Etching process |
| ES2195770B1 (es) * | 2002-02-21 | 2005-02-16 | Jon Imanol Murua Fuertes | Compuesto antideslizante. |
| US6740571B2 (en) * | 2002-07-25 | 2004-05-25 | Mosel Vitelic, Inc. | Method of etching a dielectric material in the presence of polysilicon |
| US6890452B2 (en) * | 2002-11-08 | 2005-05-10 | 3M Innovative Properties Company | Fluorinated surfactants for aqueous acid etch solutions |
| JP4816250B2 (ja) * | 2006-05-25 | 2011-11-16 | 三菱瓦斯化学株式会社 | エッチング液組成物及びエッチング方法 |
| US7779744B2 (en) * | 2006-09-20 | 2010-08-24 | Gm Global Technology Operations, Inc. | Vehicular hydraulic system with priority valve |
| KR100891255B1 (ko) * | 2007-01-05 | 2009-04-01 | 주식회사 하이닉스반도체 | 커패시터의 리닝 방지용 식각액 조성물 및 이를 이용한커패시터 제조 방법 |
| KR20090109198A (ko) * | 2008-04-15 | 2009-10-20 | 주식회사 동진쎄미켐 | 액정디스플레이 장치용 유리기판의 세정 및 식각 조성물 및이를 이용한 유리기판의 식각 방법 |
| CN101840964B (zh) * | 2009-03-18 | 2012-04-25 | 中国科学院半导体研究所 | 低阻p-GaN欧姆接触电极制备方法 |
| CN108384548A (zh) * | 2018-02-24 | 2018-08-10 | 苏州晶瑞化学股份有限公司 | 一种非金属氧化物膜用缓冲蚀刻液 |
| CN115231864B (zh) * | 2022-08-10 | 2023-06-20 | 安徽理工大学 | 一种利用二氧化硅基体蚀刻废液制备的碱激发混凝土及其应用 |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1228083A (zh) * | 1968-06-10 | 1971-04-15 | ||
| US3650960A (en) * | 1969-05-06 | 1972-03-21 | Allied Chem | Etching solutions |
| US4040897A (en) * | 1975-05-05 | 1977-08-09 | Signetics Corporation | Etchants for glass films on metal substrates |
| US4055458A (en) * | 1975-08-07 | 1977-10-25 | Bayer Aktiengesellschaft | Etching glass with HF and fluorine-containing surfactant |
| JPS5616129A (en) * | 1979-07-18 | 1981-02-16 | Hitachi Ltd | Pattern forming method |
| JPS5639027A (en) * | 1979-09-08 | 1981-04-14 | Mitsui Petrochem Ind Ltd | Cyclopropenium salt and its preparation |
| JPS59974A (ja) * | 1982-06-25 | 1984-01-06 | Fujitsu Ltd | 半導体受光装置の製造方法 |
| JPS6039176A (ja) * | 1983-08-10 | 1985-02-28 | Daikin Ind Ltd | エッチング剤組成物 |
| US4517106A (en) * | 1984-04-26 | 1985-05-14 | Allied Corporation | Soluble surfactant additives for ammonium fluoride/hydrofluoric acid oxide etchant solutions |
-
1985
- 1985-05-13 US US06/733,568 patent/US4620934A/en not_active Expired - Lifetime
-
1986
- 1986-04-29 CN CN86103055A patent/CN1012071B/zh not_active Expired
- 1986-04-30 DE DE3689962T patent/DE3689962T2/de not_active Expired - Fee Related
- 1986-04-30 EP EP86105979A patent/EP0201808B1/en not_active Expired - Lifetime
- 1986-05-10 KR KR1019860003650A patent/KR900003980B1/ko not_active IP Right Cessation
- 1986-05-12 CA CA000508873A patent/CA1276530C/en not_active Expired - Fee Related
- 1986-05-13 JP JP61109370A patent/JPH0694596B2/ja not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0694596B2 (ja) | 1994-11-24 |
| EP0201808B1 (en) | 1994-07-13 |
| CN86103055A (zh) | 1986-11-26 |
| DE3689962T2 (de) | 1995-01-05 |
| JPS61266581A (ja) | 1986-11-26 |
| KR900003980B1 (ko) | 1990-06-07 |
| US4620934A (en) | 1986-11-04 |
| EP0201808A2 (en) | 1986-11-20 |
| DE3689962D1 (de) | 1994-08-18 |
| CA1276530C (en) | 1990-11-20 |
| KR860009100A (ko) | 1986-12-20 |
| EP0201808A3 (en) | 1988-03-23 |
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