CN1636904A - 掺氟的硅酸盐玻璃及其用途 - Google Patents

掺氟的硅酸盐玻璃及其用途 Download PDF

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CN1636904A
CN1636904A CNA2004101019177A CN200410101917A CN1636904A CN 1636904 A CN1636904 A CN 1636904A CN A2004101019177 A CNA2004101019177 A CN A2004101019177A CN 200410101917 A CN200410101917 A CN 200410101917A CN 1636904 A CN1636904 A CN 1636904A
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约亨·阿尔克马佩尔
约尔格·舒马赫尔
乌尔里希·波伊赫特
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Abstract

本发明公开了一种掺氟的至少三元硅酸盐玻璃,该硅酸盐玻璃尤其包含TiO2。它可以有利地用作具有低热膨胀的材料,其中在-50℃至100℃的温度范围内热膨胀系数的斜率为±2×10-9/K2。这种材料特别适合用于微石印术,尤其是用于EUV-石印术。

Description

掺氟的硅酸盐玻璃及其用途
本发明涉及掺氟的硅酸盐玻璃,特别是硅酸钛玻璃,并涉及这样一种玻璃如具有优化热膨胀性能的材料的用途。
具有低的或极低的热膨胀的材料在许多分支技术中扮演主要角色。例如,它们可被用作精密光学中的衬底或机械构造。因其低热膨胀而知名的有例如石英玻璃,其热膨胀系数(CTE)在0℃至50℃的范围内为约500×10-9/K(ppb/K)。
尽管与普通多组分玻璃相比,石英玻璃的平均热膨胀系数和瞬时热膨胀系数CTE较小,但是瞬时热膨胀系数CTE仍具有显著的温度相关性。例如,在-50℃时的瞬时CTE为约300ppb/K,而在+100℃时的瞬时CTE为约600ppb/K。
基于石英玻璃的二元硅酸盐玻璃部分地具有依然较小的热膨胀。根据日本专利JP 64-33030,知道了一种二元硅酸盐玻璃,其掺有ZrO2,且其热膨胀系数CTE据说为石英玻璃CTE的约十分之一。另外,掺钛的硅酸盐玻璃被称为NZTE(近零热膨胀)材料,已知其具有<<100ppb/K的热膨胀系数(参见US 2,326,059;WO 02/088035 Al and P.C.Schultz,H.T.Smyth:″Ultra-Low-Expansion Glasses and Their Structure in theSiO2-TiO2 System″in R.W.Douglas,B.Ellis(editor),Amorphous Materials,pages 453-461,Wiley,London,1972),并早已在市场上销售。另外,这种材料显示热膨胀系数的极大的温度相关性。例如,在0至50℃的范围内,CTE(T)曲线的斜率为约1至2ppb/K2
根据美国专利US 3,498,876,已知体系Cu2O-CuO-ZnO-Al2O3-SiO2的铜锌铝硅酸盐玻璃应具有至多15×10-7/K的低热膨胀系数。
尽管在许多申请中,上述热膨胀系数的温度相关性不是有害的,但是它造成了一个缺点,特别是对于一些最新技术。例如,在微石印术中,特别是在EUV-石印术中,热膨胀系数是精确规定的,远离其绝对值,温度相关性也是很重要的,因为它使热效应的模拟和补偿更困难,或者甚至使其不可能。
因此,本发明的一个目的是分别提供一种材料或公开这种材料的新用途,由此可以尽可能地使热膨胀系数恒定,从而特别地,可以有利地使用微石印术,尤其是EUV-石印术。
通过掺氟的至少三元硅酸盐玻璃,特别是通过掺氟的硅酸钛玻璃,达到了这个目的,在-50℃至100℃的范围内,所述玻璃的热膨胀系数CTE至多在±2×10-9/K2之间变化,因此斜率应为2×10-9/K2至-2×10-9/K2,优选1.5×10-9/K2至-1.5×10-9/K2,更优选1×10-9/K2至-1×10-9/K2
尽管在相关温度范围内,例如掺钛的硅酸盐玻璃的平均CTE没有显著降低,然而令人惊奇地,CTE的温度相关性显著较小。
在现有技术中,在接近室温的温度范围内,通过加入氟(在2wt%的范围内),石英玻璃的热膨胀系数降低了,这已报道了几次(参见I.M.Rabinovich:″On the Structural Role of Fluorine in Silicate Glasses″,Phys.Chem.Glasses 24(1983),pages 54-56;C.M.Smith,L.A.Moore:″FusedSilica for 157nm Transmittance″,Proc.SPIE-INT.Soc.Opt.Eng.3676(1999),pages 834-841;K.Rau et al.:″Characteristics of Fluorine DopedGlasses″,Topical Meet.Optical Fiber Transmission II.Williamsburg(1977);H.Takahashi et al.:″Characteristics of Fluorine-Doped SilicaGlass″,Technical Digest:European Conference on Optical Communication(1986),pages 3-6)。具体地,已指出该效应可有利地用于将掺氟石英玻璃在157nm石印术中用作光掩模的衬底材料,因为减少的热膨胀降低了成像缺陷的危险,所述成像缺陷是由从来不能完全避免的温度变化引起的。
在另一方面,已知附加的氟常常导致玻璃网络的松散,并由此导致CTE的增加(Scholze,Horst,″Glas-Natur,Struktur und Eigenschaften,Springer Verlag,3rd edition)。
因此,对本领域技术人员来说,将一种至少三元掺氟石英玻璃用作如下材料,其热膨胀系数在-50℃至100℃的温度范围内变化很小,这不是显而易见的,因为迄今为止,只有二元掺氟硅酸盐玻璃是已知的,且仅能预计热膨胀系数的绝对降低,而CTE的恒定性不起任何作用。
然而,例如在EUV-石印术中,CTE对于应用温度范围的恒定性起主要作用。
使用本发明的玻璃,例如掺氟和钛的三元石英玻璃,可以达到热膨胀系数的显著高恒定性,尤其是在相关的-50℃至100℃的温度区间内。同时,产生了一个平均热膨胀系数CTE,其为<<100×10-9/K,尤其是<10×10-9/K,在一个实施方案中,其为<1×10-9/K。
作为热膨胀系数恒定性的量度,可以使用CTE(T)曲线的平均或瞬时斜率。
因此,这种硅酸盐玻璃可有利地用于EUV石印术中。
根据本发明的有利进展,在-50℃至100℃的温度范围内,热膨胀系数的斜率dCTE/dT为负值,优选为-1.5×10-9/K2<dCTE/dT<0,尤其为约-0.5×10-9/K2
因此,通过改变氟含量,石英玻璃(例如掺钛的石英玻璃,且其TiO2含量为6.8wt%)热膨胀系数的斜率可被调节到在-1.5ppb/K2(氟含量:约3wt%)和1.5ppb/K2(氟含量:0)之间的特定目标值。本发明的硅酸盐玻璃的主要应用温度范围为约-50℃至100℃,尤其是0至50℃,其中10至30℃的范围是特别有利的。这里,掺氟SiO2-TiO2玻璃热膨胀系数(平均热膨胀系数)CTE的绝对值为<600×10-9/k,这取决于TiO2含量(0<TiO2含量<10wt%)。
优选地,掺杂的氟为至少1wt%、优选至少2wt%的氟。在这个可优选扩展到约5wt%氟的范围内,在目标温度范围内达到了热膨胀系数的所需恒定性。
根据本发明的掺杂氟和可能的附加掺杂剂的硅酸盐玻璃可通过火焰水解法(烟灰法)、等离子体法、或通过溶胶-凝胶法以已知基本已知的方式进行制备(参见例如US 2,326,059的火焰水解)。
优选地,加入附加组分作为其他掺杂剂,其用作玻璃形成体。除了TiO2外,还可以包括ZrO2、V2O5、CuO、Al2O3、Ge2O3和/或B2O3。这里优选将CuO与Al2O3一起加入。
SiO2的含量优选为至少85wt%,优选至少90wt%。
其他玻璃形成体的含量为至少1wt%至最多10wt%,其中含量2至7wt%是优选的。如果加入了TiO2,优选最多加入量为高达10wt%,优选高达7wt%。
氟和其他掺杂剂的加入量总和优选为最多15wt%。
在T1至T2的温度范围内,平均CTE的定义如下:
CTE = l 2 ( T 2 ) - l 1 ( T 1 ) ( T 2 - T 1 ) · l 1
其中11、12为在相应温度的样品主体的长度。对于石英玻璃,在-50至0℃的范围内产生约400ppb/K的平均CTE,在0至50℃的范围内产生约500ppb/K的平均CTE,在500至100℃的范围内产生约550ppb/K的平均CTE。作为温度相关性的量度,使用CTE(T)曲线上任意点的斜率或在温度区间内的平均斜率:
ΔCTE / ΔT = CTE 2 ( T 2 ) - CTE 1 ( T 1 ) T 2 - T 1
或者可以使用CTE对于温度的一阶微分:dCTE/dT。
因此,应理解前提条件,即在给定温度区间例如-50℃至+100℃、或0℃至50℃、或10℃至30℃内,热膨胀系数的斜率dCTE/dT为例如1ppb/K2至-1ppb/K2,使得瞬时斜率在总温度范围内的给定范围内。对于dCTE/dT的另一种优选范围为对于上述温度范围具有最小值-1.5ppb/K2至高达最大值0ppb/K2的区间。
或者,可使用平均斜率ΔCTE/ΔT,其必须在对应的相关温度范围内作为平均值来处理。
对于掺氟的至少三元石英玻璃,可以达到热膨胀瞬时系数的高度恒定性,其中dCTE/dT优选小于0.5ppb/K2,优选为负值。

Claims (21)

1.一种包括SiO2和至少一种附加的玻璃形成体的硅酸盐玻璃,该硅酸盐玻璃被掺杂氟,且其热膨胀系数在-50℃至100℃的温度范围内最多变化±2×10-9/K2
2.如权利要求1所述的硅酸盐玻璃,其中热膨胀系数的斜率dCTE/dT在-50℃至100℃的温度范围内为负值,优选为-1.5×10-9/K2<dCTE/dT<0,尤其为约-0.5×10-9/K2
3.如权利要求1或2所述的硅酸盐玻璃,该硅酸盐玻璃掺杂有至少1wt%的氟、优选至少2wt%的氟。
4.如前述权利要求中任一项所述的硅酸盐玻璃,该硅酸盐玻璃包括至少一种附加组分,其选自TiO2、ZrO2、V2O5、CuO、和Al2O3
5.如权利要求4所述的硅酸盐玻璃,该硅酸盐玻璃包括至少附加组分CuO和Al2O3
6.如前述权利要求中任一项所述的硅酸盐玻璃,该硅酸盐玻璃包括至少一种附加组分,其选自Ge2O3、Al2O3、和B2O3
7.如权利要求4至6中任一项所述的硅酸盐玻璃,其中至少一种附加组分的含量为1至10wt%、优选3至9wt%。
8.如前述权利要求中任一项所述的硅酸盐玻璃,该硅酸盐玻璃被构造为三元硅酸盐玻璃,尤其是体系SiO2-TiO2-F-的硅酸盐玻璃。
9.如权利要求1至7中任一项所述的硅酸盐玻璃,该硅酸盐玻璃被构造为四元硅酸盐玻璃。
10.如前述权利要求中任一项所述的硅酸盐玻璃,其中SiO2的含量为至少85wt%、优选为至少90wt%。
11.如前述权利要求中任一项所述的硅酸盐玻璃,该硅酸盐玻璃除了SiO2之外还包括至少1wt%的至少一种附加的玻璃形成体。
12.如前述权利要求中任一项所述的硅酸盐玻璃,该硅酸盐玻璃除了SiO2之外还包括最多10wt%的附加玻璃形成体。
13.如前述权利要求中任一项所述的硅酸盐玻璃,该硅酸盐玻璃包括2至7wt%的附加玻璃形成体。
14.如权利要求1至12中任一项所述的硅酸盐玻璃,该硅酸盐玻璃包括最多10wt%的TiO2、优选最多7wt%的TiO2
15.如前述权利要求中任一项所述的硅酸盐玻璃,该硅酸盐玻璃除了SiO2之外还包括最多15wt%的F-和其他组分。
16.如前述权利要求中任一项所述的硅酸盐玻璃的用途,其用作制造精密部件和/或光学元件的材料,尤其是用于天文学、微石印术、尤其是EUV-石印术的材料。
17.一种光学元件,尤其是掩模、镜子、滤波器、透镜、棱镜,其包括权利要求1至15中任一项的硅酸盐玻璃。
18.如权利要求17所述的光学元件,其中在0℃至50℃的范围内,硅酸盐玻璃的热膨胀系数的平均斜率ΔCTE/ΔT在±2×10-9/K2的范围内,优选在±1.5×10-9/K2的范围内,优选为负值。
19.如权利要求17所述的光学元件,其中在0℃至50℃的整个温度范围内,硅酸盐玻璃的热膨胀系数的瞬时斜率dCTE/dT在±2×10-9/K2的范围内,优选在±1.5×10-9/K2的范围内,优选为负值。
20.如权利要求17所述的光学元件,其中在10℃至30℃的范围内,硅酸盐玻璃热膨胀系数的平均斜率ΔCTE/ΔT在±2×10-9/K2的范围内,优选在±1.5×10-9/K2的范围内,优选为负值。
21.如权利要求17所述的光学元件,其中在10℃至30℃的整个温度范围内,硅酸盐玻璃的热膨胀系数的瞬时斜率dCTE/dT在±2×0-9/K2的范围内,优选在±1.5×10-9/K2的范围内,优选为负值。
CNA2004101019177A 2003-12-18 2004-12-20 掺氟的硅酸盐玻璃及其用途 Pending CN1636904A (zh)

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CN105683102A (zh) * 2013-11-12 2016-06-15 赫罗伊斯石英玻璃股份有限两合公司 由具有高硅酸含量的钛和氟掺杂玻璃制造坯料的方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102164867A (zh) * 2008-08-28 2011-08-24 Sri国际公司 用于生产氟化物气体和掺氟玻璃或陶瓷的方法和系统
CN105683102A (zh) * 2013-11-12 2016-06-15 赫罗伊斯石英玻璃股份有限两合公司 由具有高硅酸含量的钛和氟掺杂玻璃制造坯料的方法

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