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国防科技大学理学院化学与生物系,长沙,410073
纸质出版日期:2012-1-20,
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方庆玲, 李效东, 李义和, 金东杓. 由光敏性全氢聚硅氮烷制备透明高硬SiO微/纳米结构压印模板[J]. 高分子学报, 2012,(1):56-62.
FANG Qingling, LI Xiaodong, LI Yihe, JIN Dongbiao. HIGH RESOLUTION SILICA IMPRINTING MOLD FABRICATED FROM A PHOTOCURABLE PERHYDROPOLYSILAZANE[J]. Acta Polymerica Sinica, 2012,(1):56-62.
方庆玲, 李效东, 李义和, 金东杓. 由光敏性全氢聚硅氮烷制备透明高硬SiO微/纳米结构压印模板[J]. 高分子学报, 2012,(1):56-62. DOI: 10.3724/SP.J.1105.2012.11062.
FANG Qingling, LI Xiaodong, LI Yihe, JIN Dongbiao. HIGH RESOLUTION SILICA IMPRINTING MOLD FABRICATED FROM A PHOTOCURABLE PERHYDROPOLYSILAZANE[J]. Acta Polymerica Sinica, 2012,(1):56-62. DOI: 10.3724/SP.J.1105.2012.11062.
面向可用作压印模板的透明高硬微/纳米结构的低成本制备
无机高分子全氢聚硅氮烷用甲基丙烯酸(2-异氰酸基乙酯)进行光敏改性
经FTIR
1H-NMR
13C-NMR等手段表征
推断获得的是甲基丙烯酸酯化的全氢聚硅氮烷(MPHPS)
并以此为原料
用一种含氟聚合物(FP)模板
施加0.1~0.4 MPa的压力
紫外压印制备MPHPS的微结构
发现增加压力
压印复制效果提高
0.23 MPa可以完全复制FP模板的微结构.此外
在0.4 MPa的压力下也制备了分辨率为90 nm
70 nm的纳米级结构.随后在碱性条件下室温水解
MPHPS聚合物结构转化为SiO无机结构
最终获得透明高硬结构
硬度4.5103 MPa
弹性模量115103 MPa.
Towards the low-cost fabrication of a hard imprinting mold with micro-and nanostructures
a novel photocurable inorganic polymer was modified from perhydropolysilazane (PHPS) by grafting with 2-isocyanatoethyl methacrylate (ICMA) in this paper.The as-modified product was characterized by the methods of FTIR
1H-NMR
13C-NMR and 2D-1H-1H-NMR (COSY).The new peaks at =3.2~3.8 on1H-NMR spectra of the product were assigned to be the NHCH2 group
and =152~158 on 13C-NMR spectra was assigned to be the CONH group.In the FTIR spectra
the absorbing peaks at 2153 and 1363 cm-1(N=C=O)
1117 cm-1(CN C) of PHPS were obviously consumed after chemical modification
and the new peaks at 1690
1530 and 1314 cm-1(CONH)were appeared.Combined with the COSY analysis
it was concluded that the UV sensitive methacrylyate group was successfully grafted to PHPS
and methacrylated perhydropolysilazane (MPHPS) was used to name the as-modified product here.MPHPS was then used to fabricate the micro-and nanostructures via UV imprinting lithography using a fluoropolymer (FP) mold with microstructures
adding a pressure ranged in 0.1~0.4 MPa.The efficiency of the pattern transfer from FP mold was increased by the pressure increasing
and the thoroughly pattern copy was realized at 0.23 MPa.Besides
nanostructures with 90 nm
70 nm feature sizes were obtained at the pressure of 0.4 MPa.Then the as-prepared micro-and nanostructures were converted into SiO inorganic phase by a followed hydrolysis treatment.The converted product was concluded to be a composition of SiO1.5 from XPS depth profile.The final obtained mold was optical transparent
and with a hardness of 4.5103 MPa and a elastic modulus of 115103 MPa.
全氢聚硅氮烷光敏水解微/纳米结构压印模板
PerhydropolysilazanePhotocurableHydrolysisMicro-and nanostructuresImprinting mold
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