CN100517068C - 纳米压印光刻胶 - Google Patents
纳米压印光刻胶 Download PDFInfo
- Publication number
- CN100517068C CN100517068C CNB038112094A CN03811209A CN100517068C CN 100517068 C CN100517068 C CN 100517068C CN B038112094 A CNB038112094 A CN B038112094A CN 03811209 A CN03811209 A CN 03811209A CN 100517068 C CN100517068 C CN 100517068C
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- China
- Prior art keywords
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- undercoat
- micro
- printing assembly
- plate printing
- Prior art date
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- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 2
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M potassium chloride Inorganic materials [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims 1
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Abstract
本发明涉及一种电子元件的微结构化方法，其提供高分辨率(≤200纳米)和良好纵横比，但明显比照相平版印刷法更为经济。根据本发明的方法包括下列步骤：i)制备如权利要求1的纳米复合材料组合物的未固化的平面溶胶膜；ii)制备由底涂层b)和载体c)组成的目标底材；iii)借助微结构化的转移压印冲头将得自i)的溶胶膜材料转移至ii)中的底涂层b)上；iv)将转移的溶胶膜材料予以固化；v)移除转移压印冲头，得到压印的微结构作为顶涂层a)。微结构化的半导体材料的制备另外包括下列步骤：vi)等离子体蚀刻残余的纳米复合材料溶胶膜层，优选用CHF3/O2等离子体，vii)等离子体蚀刻底涂层，优选用O2等离子体，viii)蚀刻半导体材料或者在经蚀刻区域掺杂半导体材料。
Description
技术领域
本发明涉及微平版印刷术领域。
现有技术
电子元件的微型化，对其而言分辨率必须降至低于1微米，基本上通过照相平版印刷技术达到。分辨极限在此由用以描绘原图的射线的波长预先确定，使得必须使用短波辐射，如高能量UV辐射、电子束和X-射线。
因为越来越小的结构会发生衍射效应，通过照相平版印刷术而结构化能达到其物理极限，该极限在约150纳米。另一方面，对于分辨率、壁斜度(Kantensteilheit)和纵横比(高度与分辨率的比)的要求越来越高，照相平版印刷法结构化所需设备(如：掩模、掩模校准器和步进器)方面成本暴增。特别地，因为现代步进器的价格为数百万美元，它们在微晶片制备中是巨大的成本因素。
因此，本发明的目的是要提出一种用于电子元件的微结构化的方法，其提供高分辨率(≤200纳米)和良好纵横比，但明显比照相平版印刷法更为经济。
US 5,772,905描述一种纳米压印法，其基于施用于底材的整个表面上的光刻胶通过在硬质压印冲头上存在的浮雕的热塑性变形。使用热塑性塑料(聚甲基丙烯酸甲酯，PMMA)作为热压印的光刻胶。因为整个晶片表面的常用厚度变化约100纳米，所以无法在单一步骤中用硬质压印冲头构造出6、8和12寸晶片。因此，必须使用复杂的“步进和重复”法，但这因为再加热已结构化的邻近区域而不予考虑。
WO99/22849公开了一种微结构化法，其采取不同的途径。此处，将具有期望的微结构的聚二甲基硅氧烷柔性压印冲头置于平的无机底材上。随后通过毛细力，液体吸入结构中。在此，液体是TEOS水溶液。通过渗透移除溶剂，留下多孔SiO2结构。这些层主要用于仿生学(用于牙和骨的复合材料)。
US 5,900,160、US 5,925,259和US 5,817,242中，压印冲头用UV可固化的光刻胶润湿(自组装单层，如烷基硅氧烷)，然后压到平滑的底材上。类似于常规压印过程，压印冲头自底材表面升起时，留下结构化的光刻胶材料。在此所用光刻胶材料显示出对底材足够的润湿度，但不适用于提升(lift-off)法，它们不具有足够的耐蚀刻性。结构尺寸在1微米范围内，因此高出多于一个的数量级。
这些方法都不适用以达到本发明的目的。
发明内容
已发现，如果使用特定纳米复合材料组合物作为转印光刻胶(纳米压印光刻胶)，则通过机械转印法达到前述要求。
本发明提供纳米复合材料组合物用作用于将半导体材料、平面形荧光屏、微机械元件和传感器加以微结构化的光刻胶的用途，此组合物包含：
a)通式(I)和/或(II)的可聚合的硅烷和/或由其衍生的缩合物
SiX4 (I)
其中X基团相同或不同，表示可水解基团或羟基；
R1 aR2 bSiX(4-a-b) (II)
其中R1是非可水解基团，R2是带有官能基的基团，X具有前述意义，a和b具有值为0、1、2或3，其中(a+b)的和具有值为1、2或3，
和
b)纳米级粒子，选自氧化物、硫化物、硒化物、碲化物、卤化物、碳化物、砷化物、锑化物、氮化物、磷化物、碳酸盐、羧酸盐、磷酸盐、硫酸盐、硅酸盐、钛酸盐、锆酸盐、铝酸盐、锡酸盐、高铅酸盐及它们的混合氧化物。
前式中，可水解的X基团是例如氢或卤素，如F、Cl、Br或I；烷氧基，优选C1-6-烷氧基，例如甲氧基、乙氧基、正丙氧基、异丙氧基和丁氧基；芳氧基，优选C6-10-芳氧基，例如苯氧基；酰氧基，例如乙酰氧基或丙酰氧基；烷基羰基，优选C2-7-烷基羰基，例如乙酰基；氨基，单烷基氨基或二烷基氨基，其烷基中优选具有1至12个，特别是1至6个碳原子。
非可水解基团R1是例如烷基，优选C1-6-烷基，如甲基、乙基、正丙基、异丙基、正丁基、异丁基和叔丁基、戊基、己基或环己基；烯基，优选C2-6-烯基，如乙烯基、1-丙烯基、2-丙烯基和丁烯基；炔基，优选C2-6-炔基，如乙炔基和炔丙基；及芳基，优选C6-10-芳基，如苯基和萘基。必要时，所述基团R1和X可以具有一个或多个常用取代基，如卤素或烷氧基。
R2基团的官能基的具体例子有环氧基、羟基、醚基、氨基、单烷基氨基、二烷基氨基、酰胺基、羧基、巯基、硫醚基、乙烯基、丙烯酰氧基、甲基丙烯酰氧基、氰基、卤素、醛、烷基羰基、磺酸基和磷酸基。这些官能基优选经过亚烷基、亚烯基或亚芳基桥连基团(其可由氧或硫原子或-NH-基团中断)连接至硅原子上。该桥连基团衍生自例如前述烷基、烯基或芳基。基团R2的桥连基团优选含有1至18个，特别是1至8个碳原子。
通式(II)中，a优选具有值为0、1或2，b优选具有值为1或2，且(a+b)的和优选具有值为1或2。
特别优选的通式(I)的可水解的硅烷是四烷氧基硅烷，如四乙氧基硅烷(TEOS)和四甲氧基硅烷。特别优选的通式(II)的有机硅烷是环氧基硅烷，如3-缩水甘油氧基-丙基三甲氧基硅烷(GPTS)或3-缩水甘油氧基-丙基三乙氧基硅烷，及具有可反应性聚合的双键的硅烷，如丙烯酰氧基丙基三甲氧基硅烷或3-甲基丙烯酰氧基-丙基三甲氧基硅烷。该硅烷或其官能基是优选的，这是因为(在水解缩聚反应完成之后)它们可引起与例如可聚合的单官能和/或双官能有机单体、低聚物和/或聚合物的聚加成反应或加成聚合反应和/或可与存在于纳米级粒子表面上的反应性基团反应并因此有助于固定(例如，通过捆入网络中)纳米级粒子。
以传统方式进行前述化合物的水解反应和缩聚反应，必要时，在酸性或碱性缩合催化剂，如HCl、HNO3或NH3存在下进行。例如，可在(一般已知的)溶胶-凝胶法条件下进行水解反应和缩聚反应。
纳米复合材料组合物中的纳米级粒子的体积分率适宜地为1至50体积％，优选1至30体积％，特别是5至20体积％。纳米级粒子具有的粒度通常为1至200纳米，优选2至50纳米，特别是5至20纳米。这样的纳米级无机粒子例如由WO96/31572是已知的，例如氧化物，如CaO、ZnO、CdO、SiO2、TiO2、ZrO2、CeO2、SnO2、PbO、Al2O3、In2O3和La2O3；硫化物，如CdS和ZnS；硒化物，如GaSe、CdSe或ZnSe；碲化物，如ZnTe或CdTe；卤化物，如NaCl、KCl、BaCl2、AgCl、AgBr、AgI、CuCl、CuBr、CdI2或PbI2；碳化物，如CeC2；砷化物，如AlAs、GaAs或CeAs；锑化物，如InSb；氮化物，如BN、AlN、Si3N4或Ti3N4；磷化物，如GaP、InP、Zn3P2或Cd3P2；碳酸盐，如Na2CO3、K2CO3、CaCO3、SrCO3和BaCO3；羧酸盐，如醋酸盐，如CH3COONa和Pb(CH3COO)4；磷酸盐；硫酸盐；硅酸盐；钛酸盐；锆酸盐；铝酸盐；锡酸盐；高铅酸盐和相应的混合氧化物，其组成优选相当于热膨胀系数低的常用玻璃的组成，如SiO2、TiO2、ZrO2和Al2O3的二元、三元或四元组合。也适用的是，例如具有钙钛矿结构的混合氧化物，如BaTiO3或PbTiO3。此外，可以使用经有机方式改性的无机粒子，如颗粒状聚甲基硅氧烷、甲基丙烯酰基官能化的氧化物颗粒和甲基磷酸的盐。
这些纳米级颗粒可按常用方法制得，例如通过根据WO96/31 572中已知文献的火焰水解、火焰热解和等离子体法。特别优选经稳定的无机粒子的胶体态纳米分散溶胶，如得自BAYER公司的硅胶、得自Goldschmidt公司的SnO2溶胶、得自MERCK公司的TiO2溶胶、得自Nissan Chemicals公司的SiO2、ZrO2、Al2O3和Sb2O3溶胶或得自DEGUSSA公司的Aerosil分散体。
可通过表面改性而改变此纳米级粒子的粘度特性。适合作为表面改性剂，即作为表面改性用低分子量有机(＝含碳)化合物，其具有至少一个官能基，该官能基能够与存在于粉末粒子表面上的基团和聚合物基体反应和/或(至少)相互作用，特别有分子量不高于500，优选不高于350，特别是不高于200的化合物。这样的化合物优选在标准条件下为液体，并优选具有碳原子总数不多于15个，特别是不多于10个，特别优选不多于8个。这些化合物必须带有的官能基主要视每种情况下所用纳米级材料的表面基团并另外还视所期望的与聚合物基体的相作用而定。例如，可能在表面改性用化合物的官能基和颗粒的表面基团之间发生根据Bronsted或Lewis的酸/碱反应(包括形成配合物和形成加合物)。另一种合适的相互作用的例子是偶极-偶极相互作用。合适官能基的例子是羧酸基，(伯、仲、叔和季)氨基和C-H-酸性基团(如β-二酮)。这些基团中的多种也可同时存在于一个分子中(甜菜碱、氨基酸、EDTA)。
据此，优选表面改性剂的例子是具有1至12个碳原子的饱和或不饱和一元和多元羧酸(优选一元羧酸)(如甲酸、乙酸、丙酸、丁酸、戊酸、己酸、丙烯酸、甲基丙烯酸、巴豆酸、柠檬酸、己二酸、丁二酸、戊二酸、草酸、顺丁烯二酸和反丁烯二酸)及它们的酯(优选C1-C4-烷基酯)和酰胺，如甲基丙烯酸甲酯。
其他合适的表面改性剂的例子有酰亚胺和式N+R10R20R30R40Y-的季铵盐，其中R10至R40是非必要彼此不同的脂族、芳族或环脂族基团，其优选具有1至12个，特别是1至6个碳原子，Y-是无机或有机阴离子，如Cl或醋酸根；一元胺和多胺，特别是通式为R3-nNHn的那些，其中n是0、1或2，R基团彼此独立地是具有1至12个，特别是1至6个，特别优选1至4个碳原子的烷基，如甲基、乙基、正丙基、异丙基和丁基，及亚乙基多胺，如乙二胺、二亚乙基三胺；氨基酸；亚胺；具有4至12个，特别是5至8个碳原子的β-二羰基化合物，如乙酰丙酮、2，4-己二酮、3，5-庚二酮、乙酰乙酸和乙酰乙酸-C1-C4-烷基酯；及经改性的醇化物，其中一部分OR基(R如前面定义)经惰性有机基团取代。
为将纳米级粒子静电稳定化，也可使用对于此目的已知的化合物，如NaOH、NH3、KOH、Al(OH)3或四甲基氢氧化铵。
根据本发明使用的纳米复合材料组合物另外可含有可聚合的单官能和/或双官能有机单体、低聚物和/或聚合物，选自(聚)丙烯酸、(聚)甲基丙烯酸、(聚)丙烯酸酯、(聚)甲基丙烯酸酯、(聚)丙烯酰胺、(聚)甲基丙烯酰胺、(聚)脲、(聚)烯烃、(聚)苯乙烯、(聚)酰胺、(聚)酰亚胺、(聚)乙烯基化合物、(聚)酯、(聚)芳基化物、(聚)碳酸酯、(聚)醚、(聚)醚酮、(聚)砜、(聚)环氧化物、含氟聚合物、有机(聚)硅氧烷、(聚)硅氧烷和杂(聚)硅氧烷。例子有(聚)氯乙烯、(聚)乙烯醇、(聚)乙烯醇缩丁醛，相应的共聚物，如聚(乙烯-乙酸乙烯酯)、聚对苯二甲酸乙二酯、聚甲醛、聚环氧乙烷或聚苯醚，有机聚硅氧烷或与金属和过渡金属形成的杂聚硅氧烷，此描述于如EP-A-36 648和EP-A-223067，及这些聚合物中的两种或多种的混合物，只要它们彼此相容。不用上述聚合物，也可以使用它们的低聚物和/或前体(单体)。这些聚合物中，特别优选可溶解于有机溶剂中的聚合物，如聚丙烯酸酯、聚甲基丙烯酸酯(如PMMA)、缩水甘油醚(如双酚A二缩水甘油醚)和聚乙烯醇缩丁醛。
可聚合的单官能和/或双官能有机单体、低聚物和/或聚合物的含量基于可聚合硅烷计可为0至20摩尔％，优选0.1至15摩尔％，特别是1至10摩尔％。
优选的纳米复合材料组合物另外含有式(III)的氟硅烷
R3(X1)3Si (III)
其中
R3是经部分氟化或全氟化的C2-C20-烷基，
X1是C1-C3-烷氧基、甲基、乙基或氯。
经部分氟化的烷基是指这样的烷基，其中至少一个氢原子被氟原子所替代。优选R3基团是CF3CH2CH2、C2F5CH2CH2、C4F9CH2CH2、正-C6F13CH2CH2、正-C8F17CH2CH2、正-C10F21CH2CH2和异-C3F7O-(CH2)3。
也为市售的式(III)的氟硅烷例如有十三氟-1，1，2，2-四氢辛基-1-三乙氧基硅烷、CF3CH2CH2SiCl2CH3、CF3CH2CH2SiCl(CH3)2、CF3CH2CH2Si(CH3)(OCH3)2、异-C3F7O-(CH2)3SiCl2CH3、正-C6F13CH2CH2SiCl2CH3和正-C6F13CH2CH2SiCl(CH3)2。
式(III)的氟硅烷的含量可以是基于纳米复合材料组合物总重计的0至3重量％，优选0.05至3重量％，特别优选0.1至2.5重量％，特别是0.2至2重量％。当使用玻璃或石英玻璃压印冲头作为转印冲头时，特别需要有氟硅烷存在。
此纳米复合材料组合物适宜地含有加成聚合、聚加成和/或缩聚催化剂，它们能够以热和/或光化学方式引发交联和固化(合称为“交联引发剂”)。
所用光引发剂可以是例如，市售引发剂。这些物质的例子有184(1-羟基环己基苯基酮)，
(1-羟基环己基苯基酮，二苯甲酮)及其他可得自Ciba公司的
型光引发剂；
1173、1116、1398、1174和1020(可得自Merck公司)，二苯甲酮、2-氯噻吨酮、2-甲基噻吨酮、2-异丙基噻吨酮、苯偶姻、4，4’-二甲氧基苯偶姻、苯偶姻乙基醚、苯偶姻异丙基醚、苄基二甲醛缩苯乙酮、1，1，1-三氯乙酰苯、二乙氧基乙酰苯和二苯并环庚酮。
合适的热引发剂特别是过氧化二酰基、过氧二碳酸酯、过酸烷基酯、二烷基过氧化物、过缩酮、酮过氧化物和烷基过氧化氢形式的有机过氧化物。这样的热引发剂的具体例子有过氧化二苯甲酰、过苯甲酸叔丁酯和偶氮双异丁腈。
如果使用，交联引发剂的用量通常是基于纳米复合材料组合物计的0.1至5重量％，优选0.5至3重量％。
本发明此外提供微平版印刷组装体(Anordnung)，其包含
a)纳米复合材料组合物的微结构化层作为顶涂层；
b)由含有线性酚醛清漆、苯乙烯、(聚)羟基苯乙烯和/或(甲基)丙烯酸酯的含芳族化合物的(共)聚合物组成的底涂层；
c)底材。
此底材优选是要结构化的半导体材料，如在玻璃上的硅晶片或氧化铟锡层。存在于其上的底涂层应与顶涂层a)和底材都具有良好的粘附性，并优选具有层厚度为约0.1至20微米。
本发明另外提供一种用以制备这样的微平版印刷组装体的方法，其包括如下步骤：
i)制备前述纳米复合材料组合物的未固化的溶胶膜；
ii)制备目标底材，其由底涂层b)和底材c)组成；
iii)借助微结构化的转移压印冲头将得自i)的溶胶膜材料转移至ii)中的底涂层b)上；
iv)将转移的溶胶膜材料予以固化；
v)移除转移压印冲头，得到压印的微结构作为顶涂层a)。
未固化的溶胶膜i)适当地施用于平面组装体上，该组装体由载体(如玻璃、石英玻璃、塑料或硅晶片)和/或粘附促进膜组成。此粘附促进膜包含有机聚合物，其确保对载体及要沉积于其上的纳米复合材料溶胶膜的良好润湿。粘附促进膜可例如由含有线性酚醛清漆、苯乙烯、(聚)羟基苯乙烯和/或(甲基)丙烯酸酯的含芳族化合物的聚合物或共聚物组成。此粘附促进膜可用已知方法(如旋涂)施用到载体上。
随后，根据本发明的纳米复合材料组合物可通过已知方法(如旋涂、喷涂或滚涂)以溶胶膜形式施用于粘附促进膜上，适宜地膜厚度是0.5至1微米。此溶胶膜优选具有粘度为80mPas至2Pas，优选100mPas至1Pas，特别优选200mPas至600mPas。此纳米复合材料组合物可以此形式施用或者优选以在有机溶剂中的溶液形式施用。合适的溶剂例如有醇(如丁醇)、酮(如丙酮)、酯(如乙酸乙酯)、醚(如四氢呋喃)和脂族、芳族及卤代烃(如己烷、苯、甲苯和氯仿)。
此纳米复合材料组合物可例如通过如下方式制备：例如在搅拌下或借助超音波，将纳米级粒子分散于前述溶剂中的一种和/或所述可聚合的化合物中的一种中。然后，将得到的分散体与纳米复合材料组合物中的剩余组分混合，必要时用溶剂稀释。用于稀释的溶剂与分散体所用溶剂相同或是可与其混溶。如果所用溶剂在施用纳米复合材料溶胶膜期间内没有已蒸发，适宜地是在施用膜之后通过合适的措施，如加热，而基本上移除溶剂，因为否则溶胶膜材料借助转移压印冲头的转移是有问题的。
可按相同方法制备目标底材。底涂层的组成可与起始底材的前述粘附促进膜相同或类似。
施用纳米复合材料溶胶并且溶剂风干之后，氟硅烷分子富积于表面上，这时玻璃或石英玻璃转移压印冲头压入该表面约5至300秒钟，优选10至60秒钟(浸没时间)。此转移压印冲头还可以由硅酮橡胶构成。在此情况下，不需式(III)的氟硅烷。氟硅烷分子的经氟化的侧链原则上排斥玻璃或石英玻璃压印冲头的亲水表面，且与粘附促进膜或底材的表面只微弱吸引，因此扩散成浓度梯度。在所述浸没时间之后，将转移压印冲头从过剩的纳米复合材料溶胶膜中抽出。溶胶膜材料的粘附作用在压印冲头的30至500纳米，优选100至200纳米的深且宽的微通道中由于毛细力和通过从(石英)玻璃表面部分移除氟硅烷分子而足够大，使得溶胶膜材料被压印冲头携带出。在未超出浸没时间时，转移会不完全。微结构至目标底材上的转移通过空气，优选在10至300秒钟内进行。在此，氟硅烷富积于与空气的界面，使得压印冲头的润湿度非常好，溶胶一滴也不会集中在转移压印冲头中。
转移压印冲头置于目标底材的底涂层b)上之后，用10至100kPa压力将压印冲头压向底涂层b)上约10至合适地300秒钟，优选20至50秒钟，特别是30至40秒钟。在此，氟硅烷再次扩散向(石英)玻璃表面方向，使得在固化之后，对底涂层的粘附性足够好而对转移压印冲头足够差。转移材料的层厚度是由50至1000纳米，优选150至500纳米。
如果使用相同的纳米复合材料溶胶并用石英玻璃压印冲头转移，则没有结构会沉积于目标底材上。溶胶完全留在压印冲头中。在转移压印冲头平放在底涂层上期间，进行热固化或UV固化。对于UV透明的转移压印冲头，优选通过UV射线固化。加热至约80至150℃约1至10分钟和/或UV照射约5至20钟之后，转移的溶胶膜材料固化，移开转移压印冲头，得到压印的微结构(顶涂层a)。借助扫描电子显微镜，此微结构化的组装体的研究显示，不仅压印的微结构保留在目标底材上，也留下厚度低于30纳米的纳米复合物材料溶胶膜的未结构化的残余层。为随后用于微电子方面，纳米复合材料溶胶膜和底涂层必须具有不同耐蚀刻性，以达到高壁斜度和高纵横比(空白边的高度与两空白边之间的间距的比)。例如，根据本发明使用的纳米复合材料组合物可以用CHF3/O2气体混合物蚀刻，而非以氧等离子体蚀刻。在底涂层方面则相反。
本发明因此还包括一种用以制备微结构化的半导体材料的方法，包括前述步骤i)至v)，其中载体c)是要结构化的半导体材料，及步骤
vi)等离子体蚀刻残余的纳米复合材料溶胶膜层，优选用CHF3/O2等离子体，
vii)等离子体蚀刻底涂层，优选用O2等离子体，
viii)在经蚀刻区域掺杂半导体材料，或者蚀刻半导体材料。
蚀刻过程之后，可用常规溶剂(如四甲基氢氧化铵)移除光刻胶涂层。
扫描电子显微镜照片显示，根据本发明的方法，压印上具有边缘长度为约150纳米且壁斜度为约90度的纳米结构。
具体实施方式
实施例
1)纳米复合材料组合物的制备
236.1克(1摩尔)缩水甘油氧基丙基三甲氧基硅烷(GPTS)与27克(1.5摩尔)水回馏蒸煮24小时。然后在旋转蒸发器中抽除形成的甲醇。
搅拌下，向这样制得的GPTS缩合物中，添加345克经四己基氢氧化铵改性的硅胶(SiO2胶体，直径约10纳米，在异丙醇中约30重量％浓度，每克硅胶用2.4毫克四己基氢氧化铵溶液(40重量％水溶液)改性)。然后在旋转蒸发器中移除异丙醇。每种情况下，基于溶胶计的1重量％的阳离子光引发剂(UVI 6974，Union Carbide)和十三氟-1，1，2，2-四氢辛基-1-三乙氧基硅烷及22.3克(0.0714摩尔)双酚A二缩水甘油醚加至无溶剂的溶胶中。此溶胶通过添加异丙氧基乙醇而稀释，直到得到粘度为约300mPas的纳米复合材料组合物。
2)用于起始底材和目标底材的线性酚醛清漆的制备
120克间甲酚、60克对甲酚和106.8克37重量％甲醛与4克草酸二水合物一起于100℃加热6小时。为蒸馏移除水和未反应的甲酚、甲醛和草酸，将反应混合物加热至200℃，压力降至50毫巴。得到172克固体形式线性酚醛清漆。
3)起始底材的制备
a)经六甲基二硅氮烷处理的4寸硅晶片在旋涂机中用线性酚醛清漆溶液(17.5克前述制得的线性酚醛清漆在82.3克PGMEA中)涂覆。然后在110℃下轻烘烤90秒钟并在235℃下强烘烤90秒钟，使得所得层厚度为约500纳米(粘附促进层)。
b)前述制得的纳米复合材料组合物通过旋涂法(2000转，30秒钟)施用于如上制得的粘附促进层上。为移除溶剂，将溶胶膜在约25℃下干燥1分钟，而溶胶膜未固化。纳米复合材料溶胶膜的层厚度为约500纳米。
4)目标底材的制备：
以类似于3a)的方式制备目标底材。
5)向目标底材上转移和压印微结构：
压印设备是一个电脑控制的试验机(型号为Zwick 1446)，其能够程序控制加载和卸载速率及维持定义的压力以特定的时间。经过有压印冲头经过节头固定在其上的轴传递力。这使得压印结构准确对准底材。金属卤化物辐射器(UV-S400型号，Panacol-Elosol GmbH公司，UV-A射线325-380纳米)用以进行光化学引发的固化作用。
微结构化的石英玻璃压印冲头(4×4厘米，结构深度200纳米)以40牛顿力压入前述制得的起始底材的未固化的溶胶膜中。等待15秒钟之后，将压印冲头从过剩的溶胶膜中抽出。这时将完全用溶胶膜材料润湿的压印冲头保持在空气中30秒钟之久，然后置于前述制得的目标底材上，并以50牛顿力在底涂层上施压35秒钟，其中转移的膜用UV辐射器固化。压印及照射时间总共为5分钟之后，移开压印冲头，固化的微结构化溶胶膜材料保留在目标底材上。涂层的扫描电子显微镜照片显示，以高壁斜度再现了几何尺寸为150纳米×150纳米的结构。残余的25纳米厚溶胶膜材料层存在于底涂层和转移的结构之间。
6)蚀刻过程
将底材于下列条件下蚀刻：
1)使用CHF3/O2(25∶10)，300瓦特，50毫米汞柱，RIE模式，各向异性；以移除残留的顶涂层；
2)O2，300瓦特，50毫米汞柱，RIE模式，各自异性；以移除底涂层。
纵横比为约3。
Claims (14)
1.一种微平版印刷组装体，其包含
a)纳米复合材料组合物的微结构化层作为顶涂层，该纳米复合材料组合物包含如下a1)和a2)：
a1)通式(I)和/或(II)的可聚合的硅烷和/或由其得到的缩合物
SiX4 (I)
其中X基团相同或不同，表示选自H、卤素、烷氧基、芳氧基、酰氧基、烷基羰基、氨基、单烷基氨基、二烷基氨基的可水解基团，或羟基；
R1 aR2 bSiX(4-a-b) (II)
其中R1是非可水解基团，选自烷基、烯基、炔基和芳基；R2是带有官能基的基团并且该基团选自亚烷基、亚烯基或亚芳基，它们都任选被氧或硫原子或-NH-基团中断，并且所述官能基选自环氧基、羟基、醚基、氨基、单烷基氨基、二烷基氨基、酰胺基、羧基、巯基、硫醚基、乙烯基、丙烯酰氧基、甲基丙烯酰氧基、氰基、卤素、醛基、烷基羰基、磺酸基和磷酸基；X具有前述意义，a和b具有值为0、1、2或3，其中(a+b)的和具有值为1、2或3，
和
a2)纳米级粒子，选自CaO、ZnO、CdO、SiO2、TiO2、ZrO2、CeO2、SnO2、PbO、Al2O3、In2O3、La2O3、CdS、ZnS、GaSe、CdSe、ZnSe、ZnTe、CdTe、NaCl、KCl、BaCl2、AgCl、AgBr、AgI、CuCl、CuBr、CdI2、PbI2；CeC2、AlAs、GaAs、CeAs；InSb、BN、AlN、Si3N4、Ti3N4；GaP、InP、Zn3P2、Cd3P2；Na2CO3、K2CO3、CaCO3、SrCO3、BaCO3；CH3COONa、Pb(CH3COO)4；SiO2、TiO2、ZrO2和Al2O3的二元、三元或四元组合；BaTiO3和PbTiO3；
b)由包含线性酚醛清漆、苯乙烯、羟基苯乙烯和/或(甲基)丙烯酸酯的含芳族化合物的聚合物或共聚物组成的底涂层；
c)底材。
2.如权利要求1的微平版印刷组装体，其中顶涂层a)是溶胶膜。
3.如权利要求1的微平版印刷组装体，其中底材c)是半导体材料。
4.如权利要求1至3中任一项的微平版印刷组装体，其中纳米复合材料组合物含有1至50体积％的纳米级粒子。
5.如权利要求1至3中任一项的微平版印刷组装体，其中纳米级粒子经用如下化合物加以表面改性，该化合物选自羧酸、羧酰胺、羧酸酯、氨基酸、β-二酮、酰亚胺，通式N+R10R20R30R40Y-的季铵盐，其中，R10至R40基团相同或不同，是脂族、芳族和/或环脂族基团，Y-是无机或有机阴离子。
6.如权利要求1至3中任一项的微平版印刷组装体，其中纳米复合材料组合物含有可溶解于有机溶剂中的聚合物，这些聚合物选自聚丙烯酸酯、聚甲基丙烯酸酯、缩水甘油醚和聚乙烯醇缩丁醛。
7.如权利要求1至3中任一项的微平版印刷组装体，其中纳米复合材料组合物含有式(III)的氟硅烷
R3(X1)3Si (III)
其中
R3是经部分氟化或全氟化的C2-C20-烷基，而
X1是C1-C3-烷氧基、氯、甲基或乙基。
8.如权利要求1至3中任一项的微平版印刷组装体，其中纳米复合材料组合物含有交联引发剂。
9.一种制备如权利要求1至3中任一项的微平版印刷组装体的方法，包括下列步骤：
i)制备所述纳米复合材料组合物的未固化的平面溶胶膜；
ii)制备由底涂层b)和载体c)组成的目标底材；
iii)借助微结构化的转移压印冲头将得自步骤i)的溶胶膜材料转移至步骤ii)中的底涂层b)上；
iv)将转移的溶胶膜材料予以固化；
v)移除转移压印冲头，得到压印的微结构作为顶涂层a)。
10.如权利要求9的方法，其中得自步骤i)的未固化的平面溶胶膜施用于由载体和/或粘附促进膜组成的平面起始底材。
11.如权利要求9的方法，其中转移压印冲头由硅酮或玻璃构成。
12.如权利要求9的方法，其中转移压印冲头压入得自步骤i)的未固化的平面溶胶膜中5至300秒钟，然后抽出并置于底涂层b)上10至300秒钟，并以压力为10至100kPa压在底涂层b)上10至300秒钟。
13.如权利要求9的方法，其中在转移压印冲头压在底涂层b)上时，进行热固化或UV固化。
14.一种制备微结构化的半导体材料的方法，包括如权利要求9的步骤i)至v)，其中载体c)是要结构化的半导体材料，及步骤
vi)等离子体蚀刻残余的纳米复合材料溶胶膜层，
vii)等离子体蚀刻底涂层，
viii)蚀刻半导体材料或者在经蚀刻区域掺杂半导体材料。
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- 2003-04-09 DE DE50312189T patent/DE50312189D1/de not_active Expired - Lifetime
- 2003-04-09 KR KR1020047016623A patent/KR100950606B1/ko not_active IP Right Cessation
- 2003-04-09 EP EP03722426A patent/EP1497695B1/de not_active Expired - Lifetime
- 2003-04-09 US US10/511,402 patent/US7431858B2/en not_active Expired - Fee Related
- 2003-04-09 JP JP2003584817A patent/JP4381825B2/ja not_active Expired - Fee Related
- 2003-04-09 WO PCT/EP2003/003666 patent/WO2003087935A2/de active Application Filing
- 2003-04-09 AT AT03722426T patent/ATE450811T1/de not_active IP Right Cessation
- 2003-04-15 TW TW092108686A patent/TWI299108B/zh not_active IP Right Cessation
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Also Published As
| Publication number | Publication date |
|---|---|
| DE50312189D1 (en) | 2010-01-14 |
| US20050224452A1 (en) | 2005-10-13 |
| JP4381825B2 (ja) | 2009-12-09 |
| TW200305781A (en) | 2003-11-01 |
| EP1497695A2 (de) | 2005-01-19 |
| KR100950606B1 (ko) | 2010-04-01 |
| EP1497695B1 (de) | 2009-12-02 |
| CN1653391A (zh) | 2005-08-10 |
| WO2003087935A2 (de) | 2003-10-23 |
| JP2005527110A (ja) | 2005-09-08 |
| WO2003087935A3 (de) | 2004-04-01 |
| US7431858B2 (en) | 2008-10-07 |
| TWI299108B (en) | 2008-07-21 |
| DE10217151A1 (de) | 2003-10-30 |
| ATE450811T1 (de) | 2009-12-15 |
| KR20050007300A (ko) | 2005-01-17 |
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