CN100499018C - 用于从物体的微结构中清除残余物的方法和组合物 - Google Patents
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Abstract
本发明提供一种从物体的微结构中清除残余物的方法，其包括下述步骤：制备包括二氧化碳、用于清除残余物的添加剂、在加压流体条件下将添加剂溶解在所说的二氧化碳中的共溶剂的清除剂，使物体和所说的清除剂接触以清除物体中残余物。本发明还提供一种用于从物体的微结构中清除残余物的组合物。
Description
技术领域
本发明涉及用于从物体的微结构中清除残余物的方法和组合物。具体来说，本发明涉及用于从具有凸凹部分的精细结构的半导体晶片表面上清除残余物如在半导体生产过程中产生的抗蚀剂的方法和组合物。
发明背景
在生产半导体晶片时，需要一个清除其它生产步骤中产生的残余物如光致抗蚀剂、UV-硬化抗蚀剂、X-射线硬化抗蚀剂、灰化抗蚀剂(ashedresist)、含碳-氟(carbon-fluorine)的聚合物、等离子体蚀刻残余物及有机或无机污染物。通常使用干和湿清除方法。在湿清除方法中，将半导体晶片浸渍在试剂如包括清除剂的水溶液中以清除半导体晶片表面上的残余物。
近来有人提出用超临界二氧化碳作为这样的试剂，这是因为超临界二氧化碳具有低粘度和高扩散性。因为具有这样的性能，所以用超临界二氧化碳进行清除在处理微结构中具有多种优点，例如，因为超临界相中没有液-液界面，所以其在微结构之间的小区域内具有高渗透性，并且能够成功地干燥微结构。
但是，超临界二氧化碳本身并不足以清除半导体晶片表面上的多种残余物。为了解决这一问题，有人提出向超临界二氧化碳中加入几种添加剂。如日本未审公开专利10-125644所述，将甲烷或具有CFx基团的表面活性剂作为添加剂加入超临界二氧化碳中。在日本未审公开专利8-191063中，用二甲亚砜或二甲基甲酰胺作为这样的添加剂。但是，基于本发明的发明人研究，这些添加剂并不总能有效地清除残余物。具体来说，当清洁物体是由低介电常数的材料组成的晶片时，通过用碱性化合物和水的这些方法处理后，这些晶片的质量下降。因为碱性化合物和水能够破坏低介电常数的材料，特别是介电常数低于4的材料(后面称为低k材料)，所以这种情况很可能发生。因此，本发明的目的是提供一种在不会对低k材料造成很大破坏的条件下的新颖而有效的清洁方法。
发明内容
因此，本发明的目的是提供一种在不会对低k材料造成很大破坏的条件下有效地清除物体的微结构中的残余物的方法和组合物。
本发明提供一种从物体中清除残余物的方法，其包括下述步骤：制备包括二氧化碳、用于清除残余物的添加剂、用于防止低k破坏的抑制剂和在加压流体条件下将所说的添加剂溶解在所说的二氧化碳中的共溶剂的清除剂(remover)，并使物体和所说的清除剂接触以清除物体中残余物。
本发明还提供一种用于从物体中清除残余物的组合物，其包括二氧化碳、含氟化物的添加剂、能够溶解含氟化物的添加剂的共溶剂或多种所述共溶剂的混合物、和抑制剂。
附图简述
参考附图并结合下面的详述部分能够更清楚地看出本发明的上述特点和特征及其它特点和特征，在附图中，类似的参考数字表示类似的部件，其中：
图1是本发明用于清除残余物的装置的示意图。
具体实施方式
本发明适用于物体的微结构，如其表面上具有凸凹部分的精细结构的半导体晶片，本发明还适用于由形成或保持其它不同材料的连续或不连续层的金属、塑料或陶瓷制成的基片。
首先说明本发明使用的所说的清除剂。清除剂包括二氧化碳、用于清除残余物的添加剂、用于抑制残余物的抑制剂、和用于在加压流体条件下将所说的添加剂和所说的抑制剂溶解在所说的二氧化碳中的共溶剂。加压的二氧化碳具有高的分散率，并且能够使溶解的残余物分散在其中。如果二氧化碳转换成超临界状态，则它可以更有效地渗入物体的精细图案部分。因为二氧化碳的粘度低，所以利用这一性能可以使添加剂进入物体表面上的孔或凹面部分。将二氧化碳加压至5MPa或更大，但在31℃下不能低于7.1MPa，将二氧化碳转换成超临界流体状态。
尽管可以使用所有能够清除微结构中残余物的添加剂，但是本发明优选使用氟化季铵盐(quaternaryammoniumfluoride)，因为氟化季铵盐具有有效的清洁能力。优选的氟化物包括至少一种选自下述物质中的化合物：氟化四甲铵、氟化四乙铵、氟化四丙铵、氟化四丁铵、胆碱氟酸盐(cholinefluoride)。在这些化合物中最优选氟化四甲铵(TMAF)。
如果添加剂的浓度太低，则清洁残余物的效果不充分。添加剂的下限是0.001wt％，优选0.005wt％，更优选0.01wt％。但是，当浓度大于0.1wt％时，由于低k材料的过度蚀刻而使低k材料受到破坏。因此，添加剂的上限是0.1wt％，优选0.05wt％，更优选0.03wt％。
本发明的清除剂还包括多元醇。多元醇用作抑制剂，防止诸如氟化物的添加剂过多破坏低k材料。在本发明的研究进程中，对含微结构的低k膜进行一些清洁试验后出现一些液体状残余物。可以认为这些“液体状残余物”是清除剂中的一些化合物与部分低k材料之间发生蚀刻反应的副产品。因为这些来自低k材料的产品不易于溶入超临界二氧化碳，所以这些副产品不能被清除，并且看起来是液体状残余物。
进一步研究后发现：当用多元醇作为所说的清除剂中的一种组分时，可以减少这些液体状残余物的量。因此，本发明的清除剂包括多元醇，多元醇用作抑制剂，防止低k材料受到破坏。尽管多元醇对低k材料的保护机理尚在研究之中，但是多元醇可以吸附在低k材料的表面上，并防止化学物质攻击其表面。
多元醇可以是二元醇，如乙二醇、丙二醇、亚丙基二醇、二甘醇、双丙甘醇、1，2-、1，3-、1，4-或2，3-丁二醇、亚戊基二醇、己二醇、辛二醇，多元醇还可以是三元醇如甘油、三羟甲基丙烷、1，2，6-己三醇和四元醇如季戊四醇。还可以使用聚乙二醇或聚丙二醇。在这些化合物中，优选二元醇，更优选乙二醇和丙二醇。
如果多元醇的浓度太低，则对低k材料的保护不充分，液体状残余物的量增加。多元醇的下限是0.005wt％，优选0.007wt％，更优选0.01wt％。但是，当浓度大于0.1wt％时，保护功效达到饱和。因此，多元醇的上限是0.1wt％，优选0.07wt％，更优选0.05wt％。
因为加压二氧化碳本身并不足以溶解添加剂和抑制剂如TMAF和多元醇，所以本发明用共溶剂将其溶入二氧化碳。本发明的共溶剂是对二氧化碳和添加剂均有亲和力的化合物。这样的共溶剂将添加剂均匀地溶解或分散在流体状态的加压二氧化碳中。尽管可以使用任何能够将添加剂和多元醇溶入加压二氧化碳中的共溶剂，但优选使用醇。醇可以是任何醇，如乙醇、甲醇、正丙醇、异丙醇、正丁醇、异丁醇、二甘醇单甲醚(diethyleneglycolmonomethyleter)、二甘醇单乙醚和六氟异丙醇。在这些醇中，优选甲醇、乙醇和异丙醇，因为它们可以作为很多化合物的良好的共溶剂。
共溶剂的种类和用量的选择取决于加入二氧化碳的添加剂的种类和用量。共溶剂的用量优选是添加剂用量的5倍或更多，因为这样易于使清除剂均匀而透明。一种替代方案是，清除剂可以包括1wt％-50wt％的共溶剂。如果加入的共溶剂超过50wt％，则由于二氧化碳的量较少将使得清除剂的渗透率下降。使用的清除剂优选包括二氧化碳、作为共溶剂的醇、作为添加剂的氟化季铵盐和/或季铵氢氧化物，因为醇能够使这些添加剂很好地溶入二氧化碳，并且这些添加剂是亲CO2的。
当用TMAF作为添加剂时，应当首先将TMAF溶入所说的共溶剂，因为TMAF在环境温度下是固体。此时可以加入二甲基乙酰胺(DMAC)或去离子水(DIW)，以使TMAF更容易地溶入二氧化碳。这些溶剂的用量优选低于TMAF的20倍。特别是应当使DIW的浓度最小化，因为DIW能够破坏低k材料。
下面用附图说明实际工序。在下面的说明中，除二氧化碳之外的清除剂组分—添加剂混合物、抑制剂、共溶剂简称为“清洁试剂”。图1示出本发明用于清除残余物的装置的简单示意图。在图中，1是二氧化碳钢瓶，2是二氧化碳的高压泵，3是清洁试剂的储槽，4是清洁试剂泵，5是阀，6是清洁试剂的储槽，7是漂洗试剂泵，8是阀，9是高压容器，10是恒温箱。首先引入微结构如其表面上有残余物的半导体晶片，将其置放在高压容器9中，然后用高压泵2将二氧化碳从二氧化碳钢瓶1供给高压容器9。为了使高压容器9中的加压二氧化碳保持超临界状态，用恒温箱10将高压容器9恒温在规定温度。可以用具有加热单元的容器代替高压容器9。用高压泵4将清洁试剂从储槽3供给高压容器9。当清洁试剂从储槽3供给高压容器9时开始清洁步骤。二氧化碳和清洁试剂的供应可以是连续的，也可以是间歇的。
在下述条件下进行清除工序：温度为31℃-120℃，压力为5MPa-30MPa，优选7.1MPa-20MPa。清除残余物需要的时间取决于物体大小、残余物的种类和数量，时间范围通常是1分钟至几十分钟。
清洁步骤后面是漂洗步骤。清洁步骤完成后，在清洁过程中从表面上除掉的残余物仍保留在容器9中。如果在这种条件下加入纯二氧化碳，则部分残余物将沉积在物体表面上。因此，在清洁步骤后用二氧化碳和漂洗试剂的混合物进行第一次漂洗步骤。第一次漂洗步骤后，用纯二氧化碳进行第二次漂洗步骤。
第一次漂洗步骤中优选使用的漂洗试剂是能够清除液体状残余物的那些试剂。本发明的发明人在研究后发现：比介电常数与水类似的化合物可以有效地达到该目的。因为水在25℃和1个大气压下的比介电常数是78，所以使用比介电常数不小于78的化合物。要求比介电常数与水类似的原因是作为低k蚀刻副产品的液体状残余物具有高极性，导致与极性溶剂的高亲和力。
另一方面，如前一部分所述，本发明需要多元醇。但是，如果清洁试剂的用量少到足以抑制由于低k材料的破坏所造成的副产品的生产，则可以在不向清洁步骤中加入任何多元醇的情况下用比介电常数不小于78的漂洗试剂处理较长时间。但是，为了降低第一次漂洗步骤的工艺时间(例如，5分钟或更少)，优选通过加入多元醇减少液体状残余物这样的副产品的生成。
实际上可以通过下述方式实施第一次漂洗步骤：用阀5停止清洁试剂的供料，然后将二氧化碳和漂洗试剂供给高压容器9，以除去容器9的内容物。可以用流量计12控制流速。在第一次漂洗步骤中，优选用阀8逐渐降低或者逐步降低漂洗试剂的供料速度，然后在第二次漂洗步骤中用纯二氧化碳置换容器9的内容物。
例如，可以用包括液气分离器的二氧化碳再循环工艺将从清洁步骤和第一次漂洗步骤中排出的流体分成气态二氧化碳和液体部分，从而将其再循环和再利用。
在第二次漂洗步骤后，通过用压力控制阀11卸压使二氧化碳蒸发成气相。从而使微结构如半导体晶片干燥，而不会留下水斑，也不会使图案受到任何破坏。
下面参照试验描述本发明。尽管已经通过参考附图的实施例详尽地描述了本发明，但是应当理解的是，对于本领域普通技术人员来说进行各种变化和改进是显而易见的。因此，只要这些变化和改进没有背离本发明的范围，它们就应当处于本发明的保护范围之内。
实施例
实施例1
为了研究清洁试剂对低k材料的破坏程度，首先测量低k膜的蚀刻速度。通过涂布由有机硅组成的材料，然后进行加热和干燥的方法在硅片上制备低k膜。低k膜的膜厚约为500
，k值是2-3。用图1所示的清洁工具将涂布有低k膜的晶片放入高压容器9。盖住容器9的盖子后，通过泵2将二氧化碳钢瓶中的二氧化碳导入。用恒温箱10将容器9的温度恒温在50℃，用控制阀11控制压力。压力达到15MPa后，通过泵4将储槽4中的清洁试剂供入容器9。处理10分钟后，进行5分钟的第一次漂洗步骤，然后用纯二氧化碳进行10分钟的第二次漂洗步骤。第一次漂洗步骤中使用的漂洗试剂是0.5wt％的去离子水、4.5wt％的乙醇和95wt％的二氧化碳。
第二次漂洗步骤后，用压力控制阀11卸压后取出晶片进行进一步评价。用处理前后的膜厚差除以10分钟，计算出蚀刻速度(/min)。用光学测量工具测量膜厚。结果示于表1。
表1中的缩写词如下：
TMAF：氟化四甲铵，DMAC：二甲基乙酰胺，DIW：去离子水，EG：乙二醇，PG：丙二醇，EtOH：乙醇
表1
实施例2
用实施例1所述的同样的方法制备涂布有低k膜的晶片。用平版印刷术在表面上加工线条和空间图案(180nm宽)后，用碳氟化合物气体进行普通蚀刻，用氧气等离子体进行灰化。在与实施例1相同的条件下用表2列出的清洁试剂清洁1分钟后，用表2列出的组分进行5分钟或10分钟的第一次漂洗步骤，然后用纯二氧化碳进行10分钟的第二次漂洗步骤。使用的第一次漂洗试剂是0.5wt％的列举组分、4.5wt％的乙醇和95wt％的二氧化碳。通过打开压力控制阀11卸压后取出处理后的晶片进行进一步评价。通过用振幅为50000的扫描电镜(SEM)观察评价清洁性能。检测清洁性能时既要观察线条表面上的残余物又要观察液体状残余物。检测的标准如下：
优秀：不再有残余物
良好：晶片的图案侧上残余物的量小于1％面积
NG(不好)：残余物的量大于1％面积
表2中的缩写词如下：
TMAF：氟化四甲铵，DMAC：二甲基乙酰胺，H2O：水(ε＝78)，DIW：去离子水，EG：乙二醇，PG：丙二醇，EtOH：乙醇，FA：甲酰胺(ε＝111)，MF：甲基甲酰胺(ε＝182)，DMF：二甲基甲酰胺(ε＝36.7)，MeOH＝甲醇(ε＝42)，AC：丙酮(ε＝21)
根据本发明所述的清洁方法，通过使用加入二氧化碳中的包括抑制剂如多元醇的清洁试剂可以保护易于被清洁试剂破坏的低k材料。另外，通过选择合适的漂洗试剂可以清除由于清洁试剂破坏低k材料产生的残余物。因此，本发明所述的清洁方法提供了一种适用于微结构如半导体晶片的优化清洁方法。
Claims (13)
1、一种从物体的微结构中清除残余物的方法，其包括下述步骤：
制备清除剂，所述清除剂包括超临界流体状态的二氧化碳、0.001至0.1wt％的用于清除残余物的添加剂、0.005至0.1wt％的丙二醇和用于在所述超临界流体条件下将所说的添加剂和丙二醇溶解在所说的二氧化碳中的共溶剂；和
使物体和所说的清除剂接触以清除物体中残余物。
2、根据权利要求1所述的方法，其中，所说的添加剂包括氟化季铵盐。
3、根据权利要求1所述的方法，其中，所说的添加剂包括氟化四甲铵。
4、一种从物体的微结构中清除残余物的方法，其包括下述步骤：
制备清除剂，所述清除剂包括超临界流体状态的二氧化碳、0.001至0.1wt％的用于清除残余物的添加剂、0.005至0.1wt％的丙二醇和用于在所述超临界流体条件下将所说的添加剂溶解在所说的二氧化碳中的共溶剂；和
使物体和所说的清除剂接触，以从物体中除去残余物，然后进行包括漂洗试剂的漂洗步骤，所述漂洗试剂在25℃和latm的温度和压力下的介电常数为78或更大。
5、根据权利要求4所述的方法，其中，所说的漂洗试剂选自包括水、甲酰胺、甲基甲酰胺和甲基乙酰胺的化合物中的至少一种。
6、根据权利要求4所述的方法，其中，所说的添加剂包括氟化季铵盐。
7、根据权利要求4所述的方法，其中，所说的添加剂包括氟化四甲铵。
8、一种用于从物体的微结构中清除残余物的组合物，其包括超临界流体状态的二氧化碳、0.001至0.1wt％的含氟化物的添加剂、能够溶解含氟化物的添加剂的共溶剂或多种所述共溶剂的混合物和0.005至0.1wt％的丙二醇。
9、根据权利要求8所述的组合物，其中，所说的含氟化物的添加剂是氟化季铵盐。
10、根据权利要求9所述的组合物，其中，氟化季铵盐是氟化四甲铵。
11、根据权利要求8所述的组合物，其中，共溶剂是乙醇、甲醇、正丙醇、异丙醇、正丁醇或二甲基乙酰胺。
12、根据权利要求11所述的组合物，其中，共溶剂是乙醇和二甲基乙酰胺的混合物。
13、一种用于从物体的微结构中清除残余物的组合物，其包括
超临界流体状态的二氧化碳、
乙醇、
二甲基乙酰胺、
0.001至0.1wt％的氟化四甲铵和
0.005至0.1wt％的丙二醇。
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-
2002
- 2002-05-23 US US10/152,782 patent/US20030217764A1/en not_active Abandoned
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2003
- 2003-05-19 SG SG200402532A patent/SG128463A1/en unknown
- 2003-05-21 CN CNA2004100621728A patent/CN1563315A/zh active Pending
- 2003-05-21 CN CNB031378153A patent/CN100499018C/zh not_active Expired - Fee Related
- 2003-05-22 DE DE60304389T patent/DE60304389T2/de not_active Expired - Lifetime
- 2003-05-22 TW TW092113865A patent/TWI231824B/zh not_active IP Right Cessation
- 2003-05-22 EP EP03011130A patent/EP1365441B1/en not_active Expired - Lifetime
- 2003-05-22 KR KR1020030032526A patent/KR100562597B1/ko not_active IP Right Cessation
- 2003-05-22 TW TW093118357A patent/TWI249573B/zh not_active IP Right Cessation
- 2003-05-22 AT AT03011130T patent/ATE322740T1/de not_active IP Right Cessation
- 2003-05-22 DE DE60306617T patent/DE60306617T2/de not_active Expired - Fee Related
- 2003-05-22 EP EP04010688A patent/EP1453080B1/en not_active Expired - Fee Related
- 2003-05-23 JP JP2003146503A patent/JP4256722B2/ja not_active Expired - Fee Related
-
2004
- 2004-04-13 US US10/822,804 patent/US7220714B2/en not_active Expired - Lifetime
- 2004-04-27 KR KR1020040028938A patent/KR100551864B1/ko not_active IP Right Cessation
- 2004-08-27 JP JP2004249222A patent/JP2005089746A/ja active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| JP2004047980A (ja) | 2004-02-12 |
| EP1453080B1 (en) | 2006-07-05 |
| SG128463A1 (en) | 2007-01-30 |
| CN1563315A (zh) | 2005-01-12 |
| TWI249573B (en) | 2006-02-21 |
| KR20040040425A (ko) | 2004-05-12 |
| CN1494954A (zh) | 2004-05-12 |
| EP1365441A1 (en) | 2003-11-26 |
| TWI231824B (en) | 2005-05-01 |
| US20030217764A1 (en) | 2003-11-27 |
| JP2005089746A (ja) | 2005-04-07 |
| TW200424307A (en) | 2004-11-16 |
| US20040192572A1 (en) | 2004-09-30 |
| DE60306617D1 (de) | 2006-08-17 |
| TW200400258A (en) | 2004-01-01 |
| KR20030091746A (ko) | 2003-12-03 |
| KR100551864B1 (ko) | 2006-02-13 |
| US7220714B2 (en) | 2007-05-22 |
| DE60304389D1 (de) | 2006-05-18 |
| ATE322740T1 (de) | 2006-04-15 |
| EP1453080A1 (en) | 2004-09-01 |
| DE60306617T2 (de) | 2007-07-05 |
| JP4256722B2 (ja) | 2009-04-22 |
| EP1365441B1 (en) | 2006-04-05 |
| KR100562597B1 (ko) | 2006-03-17 |
| DE60304389T2 (de) | 2007-02-01 |
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