有机硅杂化光波导材料的制备及性能研究
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摘要
光子技术和光子器件的迅猛发展对光子材料提出更高的要求,在众多的光电材料中,有机/无机杂化材料由于兼具有机聚合物材料的易加工和无机材料的耐高温等多种特性,成为近年来研究的热点。但是目前大多的有机/无机杂化材料存在易开裂、固化周期长和光学损耗大等缺陷,限制了其应用。
本文首先以苯基三乙氧基硅烷和甲基丙烯酰氧丙基三甲氧基硅烷为前驱体,制备出可紫外固化聚倍半硅氧烷PSQ-S15。PSQ-S15结构中含有C=C和Si-OH两种可交联基团,分别以过氧化苯甲酰和1-羟基环己基苯基甲酮(IHT-PI 184)为C=C键的热和光引发剂,应用二甲基甲酰胺(DMF)为溶剂旋涂成膜并固化后,得到不发生开裂的高平整度(均方根表面粗糙度Rq小于0.5nm)薄膜。所得固化膜在1310nm和1550nm的光学损耗分别约为0.31dB·cm~(-1)和0.60dB·cm~(-1),折射率分别为1.535和1.532,双折射小于0.0005,热光系数均为-2.2×10~(-4)℃~(-1)。PSQ-S15固化膜在40～300℃范围内未出现玻璃化转变温度,并且在氮气氛围中热失重1.0wt%的温度大于370℃。
为改善DMF在空气中吸水可能导致PSQ-S15薄膜表面破坏的问题,制备出可直接旋涂成膜的液态有机硅杂化材料PSQ-Ls(包括PSQ-LH和PSQ-LL)。PSQ-Ls类材料是以苯基三甲氧基硅烷、甲基三甲氧基硅烷和甲基丙烯酰氧丙基三甲氧基硅烷为前驱体,室温酸性水解缩聚得到。PSQ-Ls结构中含有C=C、Si-OH和Si-OCH_3三种活性基团,应用复合光引发剂体系(光阳离子引发剂IHT-PI 820+IHT-PI 184)和单光引发剂体系(IHT-PI 184)分别进行紫外(UV)辐照和加热两步固化并对固化工艺进行优化。对于单光引发剂固化体系可获得光学损耗较低的固化膜(在1550nm处约0.70～0.80dB·cm~(-1),在1310nm处约0.20～0.30dB·cm~(-1))。通过PSQ-LH和PSQ-LL以不同比例混合实现固化薄膜折射率在约1.450～1.520范围连续准确调节,且双折射均小于0.0005。PSQ-LH固化膜的热光系数在1310nm和1550nm处均为-2.4×10~(-4)℃~(-1),PSQ-LL固化膜的热光系数在1310nm和1550nm处均为-2.2×10~(-4)℃~(-1)。所得固化膜的均方根表面粗糙度Rq小于0.6nm,且折射率和薄膜厚度均具有很好的均一性。PSQ-LH和PSQ-LL固化膜的耐热性能优异,在氮气下热失重1.0wt%的温度分别出现在330～347℃和365～376℃,在40～300℃范围内均未出现玻璃化转变温度。
为进一步提高该类材料的折射率和力学强度,分别以六氟双酚A(6FDA),4',4-联苯二酚(DP)和4-(4-羟基-苯基)-2H-二氮杂萘-1-酮(DHPZ)为原料经二丙烯基醚化合物,合成出三种桥连型硅氧烷单体,进而以该三种桥连硅氧烷单体分别与二苯基硅二醇和甲基丙烯酰氧丙基三甲氧基硅烷为前驱体,制备出三种含芳环桥连结构的杂化材料P-6FDA、P-DP和P-DHPZ。经紫外和加热两步固化后所得薄膜同时具有较高的折射率和低损耗,在1310nm处的光学损耗分别为0.39dB·cm~(-1)、0.25dB·cm~(-1)和0.39dB·cm~(-1);在1550nm处,光学损耗分别为0.63dB·cm~(-1)、0.62dB·cm~(-1)和0.82dB·cm~(-1)。三种固化膜在1310nm处的折射率分别为1.525(TE)、1.550(TE)和1.558(TE),双折射分别为＜0.0005、0.0012和0.0028,热光系数均为-3.0×10~(-4)℃~(-1);在1550nm处的折射率分别为1.522(TE)、1.548(TE)和1.556(TE),双折射分别为＜0.0005、0.0010和0.0027,热光系数均为-2.9×10~(-4)℃~(-1)。三种固化膜在氮气中热失重1.0wt%的温度分别为333℃、334℃和366℃,在40～300℃的范围均未出现玻璃化转变温度。
PSQ-Ls类材料基本满足制作集成光波导的性能要求。应用PSQ-LH为波导芯层,采用光刻刻蚀工艺、硬压印光刻和软压印光刻等方法制作出集成光波导结构,得到具有很好表面平整度和拐角垂直度的光波导结构,并实现直波导的导光(光刻刻蚀工艺)。应用PSQ-LH薄膜制作出非本征型Fabry-Perot光纤压力传感器,并得到很好的结果。
The rapid development of photonic technology and photonic components in telecom and datacom industries need advanced photic material with low-cost waveguide fabrication urgently.Optical polymer will play a key role in integrated photonics fileld due to their easier processibility and integration over inorganic counterparts.Organic silicone polymers can be viewed as organic-inorganic hybrids that combine many desirable properties of conventional organic and inorganic components,such as good thermal stability,rigidity, transparency to UV and visible light,and photostability.
In this thesis,three hybrid materal systems have been developed for waveguides.The first one is solid UV curable polysilisesquoxane(PSQ-S15) derived from phenyltriethoxylsilane andγ-Methacryloxypropyltfimethoxysilane.Films with low surface roughness(Rq＜0.5nm) can be obtained by spin-coating using dimethyl formamide(DMF) as solvent.Curing behavior and optical properties(at 1310nm and 1550nm) are discussed.Double bonds(C=C) and Si-OH as curable chemical groups are introduced to PSQ-S15.The optical losses of the films which are cured with different initiators(BPO or IHT-PI 184) are about 0.60dB·cm~(-1) at 1550nm and 0.31dB·cm~(-1) at 1310nm cured films.The refractive indexes of the cured film are 1.535 at 1550nm,and 1.533 at 1310nm,the thermal-optic coefficients are -2.2×10~(-4)℃~(-1) both at 1310nm and 1550nm,and the birefringence are lower than 0.0005.Besides,the cured films shows outstanding thermal stability(no Tg in the range of 40～300℃,and Td with 1.0wt% weight loss are above 370℃in nitrogen).
To overcome possible defect of PSQ-S15 films because of the water absorption as using DMF at spin coating procedure,solvent-free liquid hybrid materials(named as PSQ-LH and PSQ-LL) are prepared base on sol-gel process using phenyltrimethoxylsilane, methyltrimethoxylsilane andγ-methacryloxypropyltrimeth-oxysilane as precursors.PSQ-Ls crack-free films with one to ten or more micrometers thickness which possess low surface roughness(Rq＜0.5nm) can be obtained by spin coating without solvent.The refractive index of PSQ-Ls can be exactly tuned from 1.450 to 1.520 by blending PSQ-LH and PSQ-LL at room temperature.There are there reactive groups in PSQ-Ls,C=C,Si-OH and Si-OCH_3.In the simplex photoinitiator curing system,a majority of Si-OCH_3 is reserved but hardly find Si-OH in the films which undergo UV curing and thermal curing processes.And the optical loss of the corresponding waveguide film is as low as 0.70dB·cm~(-1).The curing process is optimized for the simplex photoinitiator system,and the dependence of optical properties on water feed,UV exposure time,thermal curing temperature and time is discussed.Optical losses of cured PSQ-LH films are about 0.70～0.80dB·cm~(-1) at 1550nm and 0.20～0.30dB·cm~(-1) and birefringence are lower than 0.0005 at both wavelength.The thermal-optic coefficients are-2.2×10~(-4)℃~(-1) for PSQ-LL cured films both at 1310nm and 1550nm,and -2.4×10~(-4)℃~(-1) for PSQ-LH cured films both at 1310nm and 1550nm.In addition,the cured films aren't exist Tg in the range of 40～300℃,and Td with 1.0wt%weight loss are 330～347℃for PSQ-LH films, and 322～328℃for PSQ-LL films in nitrogen.
In order to increase refractive index and improve mechanical property of above hybrid materials,three hybrid materials containing bridged structures(P-6FDA,P-DP and P-DHPZ) are synthesized from(6FDA-Si,DP-Si,and DHPZ-Si),diphenylsilanediol andγ-methacryloxypropyltrimethoxysilane respectively.After UV(IHT-PI 184 as photoinitiator) and thermal curing process,the optical losses of P-6FDA,P-DP and P-DHPZ films are 0.39, 0.25,and 0.39dB·cm~(-1) at 1310nm respectively,and 0.63,0.62 and 0.82dB·cm~(-1) at 1550nm respectively,the refractive index are 1.525(TE),1.550(TE),and 1.558(TE) at 1310nm respectively,and 1.522(TE),1.548(TE) and 1.556(TE) at 1550nm respectively. Birefringences are＜0.0005,0.0012 and 0.0028 at 1310nm respectively,and＜0.0005,0.0010 and 0.0027 at 1550nm respectively.Three cured films also show outstanding thermal stability (Td with 1.0wt%weight loss are 333℃,334℃and 366℃in nitrogen,and no Tg in the range of 40～300℃).
PSQ-Ls material system can satisfy requirements for integrated optical waveguide. Conventional lithographic patterning,hard nanoimprint and soft nanoimprint are applied to fabricate optical waveguides using PSQ-Ls.And high quality sidewalls of waveguides are obtained,and achieve propagation light by a straight waveguide.In addition,PSQ-Ls also applied to fabricate Fabry-Perot fiber pressure sensor successfully.
本文首先以苯基三乙氧基硅烷和甲基丙烯酰氧丙基三甲氧基硅烷为前驱体,制备出可紫外固化聚倍半硅氧烷PSQ-S15。PSQ-S15结构中含有C=C和Si-OH两种可交联基团,分别以过氧化苯甲酰和1-羟基环己基苯基甲酮(IHT-PI 184)为C=C键的热和光引发剂,应用二甲基甲酰胺(DMF)为溶剂旋涂成膜并固化后,得到不发生开裂的高平整度(均方根表面粗糙度Rq小于0.5nm)薄膜。所得固化膜在1310nm和1550nm的光学损耗分别约为0.31dB·cm~(-1)和0.60dB·cm~(-1),折射率分别为1.535和1.532,双折射小于0.0005,热光系数均为-2.2×10~(-4)℃~(-1)。PSQ-S15固化膜在40～300℃范围内未出现玻璃化转变温度,并且在氮气氛围中热失重1.0wt%的温度大于370℃。
为改善DMF在空气中吸水可能导致PSQ-S15薄膜表面破坏的问题,制备出可直接旋涂成膜的液态有机硅杂化材料PSQ-Ls(包括PSQ-LH和PSQ-LL)。PSQ-Ls类材料是以苯基三甲氧基硅烷、甲基三甲氧基硅烷和甲基丙烯酰氧丙基三甲氧基硅烷为前驱体,室温酸性水解缩聚得到。PSQ-Ls结构中含有C=C、Si-OH和Si-OCH_3三种活性基团,应用复合光引发剂体系(光阳离子引发剂IHT-PI 820+IHT-PI 184)和单光引发剂体系(IHT-PI 184)分别进行紫外(UV)辐照和加热两步固化并对固化工艺进行优化。对于单光引发剂固化体系可获得光学损耗较低的固化膜(在1550nm处约0.70～0.80dB·cm~(-1),在1310nm处约0.20～0.30dB·cm~(-1))。通过PSQ-LH和PSQ-LL以不同比例混合实现固化薄膜折射率在约1.450～1.520范围连续准确调节,且双折射均小于0.0005。PSQ-LH固化膜的热光系数在1310nm和1550nm处均为-2.4×10~(-4)℃~(-1),PSQ-LL固化膜的热光系数在1310nm和1550nm处均为-2.2×10~(-4)℃~(-1)。所得固化膜的均方根表面粗糙度Rq小于0.6nm,且折射率和薄膜厚度均具有很好的均一性。PSQ-LH和PSQ-LL固化膜的耐热性能优异,在氮气下热失重1.0wt%的温度分别出现在330～347℃和365～376℃,在40～300℃范围内均未出现玻璃化转变温度。
为进一步提高该类材料的折射率和力学强度,分别以六氟双酚A(6FDA),4',4-联苯二酚(DP)和4-(4-羟基-苯基)-2H-二氮杂萘-1-酮(DHPZ)为原料经二丙烯基醚化合物,合成出三种桥连型硅氧烷单体,进而以该三种桥连硅氧烷单体分别与二苯基硅二醇和甲基丙烯酰氧丙基三甲氧基硅烷为前驱体,制备出三种含芳环桥连结构的杂化材料P-6FDA、P-DP和P-DHPZ。经紫外和加热两步固化后所得薄膜同时具有较高的折射率和低损耗,在1310nm处的光学损耗分别为0.39dB·cm~(-1)、0.25dB·cm~(-1)和0.39dB·cm~(-1);在1550nm处,光学损耗分别为0.63dB·cm~(-1)、0.62dB·cm~(-1)和0.82dB·cm~(-1)。三种固化膜在1310nm处的折射率分别为1.525(TE)、1.550(TE)和1.558(TE),双折射分别为＜0.0005、0.0012和0.0028,热光系数均为-3.0×10~(-4)℃~(-1);在1550nm处的折射率分别为1.522(TE)、1.548(TE)和1.556(TE),双折射分别为＜0.0005、0.0010和0.0027,热光系数均为-2.9×10~(-4)℃~(-1)。三种固化膜在氮气中热失重1.0wt%的温度分别为333℃、334℃和366℃,在40～300℃的范围均未出现玻璃化转变温度。
PSQ-Ls类材料基本满足制作集成光波导的性能要求。应用PSQ-LH为波导芯层,采用光刻刻蚀工艺、硬压印光刻和软压印光刻等方法制作出集成光波导结构,得到具有很好表面平整度和拐角垂直度的光波导结构,并实现直波导的导光(光刻刻蚀工艺)。应用PSQ-LH薄膜制作出非本征型Fabry-Perot光纤压力传感器,并得到很好的结果。
The rapid development of photonic technology and photonic components in telecom and datacom industries need advanced photic material with low-cost waveguide fabrication urgently.Optical polymer will play a key role in integrated photonics fileld due to their easier processibility and integration over inorganic counterparts.Organic silicone polymers can be viewed as organic-inorganic hybrids that combine many desirable properties of conventional organic and inorganic components,such as good thermal stability,rigidity, transparency to UV and visible light,and photostability.
In this thesis,three hybrid materal systems have been developed for waveguides.The first one is solid UV curable polysilisesquoxane(PSQ-S15) derived from phenyltriethoxylsilane andγ-Methacryloxypropyltfimethoxysilane.Films with low surface roughness(Rq＜0.5nm) can be obtained by spin-coating using dimethyl formamide(DMF) as solvent.Curing behavior and optical properties(at 1310nm and 1550nm) are discussed.Double bonds(C=C) and Si-OH as curable chemical groups are introduced to PSQ-S15.The optical losses of the films which are cured with different initiators(BPO or IHT-PI 184) are about 0.60dB·cm~(-1) at 1550nm and 0.31dB·cm~(-1) at 1310nm cured films.The refractive indexes of the cured film are 1.535 at 1550nm,and 1.533 at 1310nm,the thermal-optic coefficients are -2.2×10~(-4)℃~(-1) both at 1310nm and 1550nm,and the birefringence are lower than 0.0005.Besides,the cured films shows outstanding thermal stability(no Tg in the range of 40～300℃,and Td with 1.0wt% weight loss are above 370℃in nitrogen).
To overcome possible defect of PSQ-S15 films because of the water absorption as using DMF at spin coating procedure,solvent-free liquid hybrid materials(named as PSQ-LH and PSQ-LL) are prepared base on sol-gel process using phenyltrimethoxylsilane, methyltrimethoxylsilane andγ-methacryloxypropyltrimeth-oxysilane as precursors.PSQ-Ls crack-free films with one to ten or more micrometers thickness which possess low surface roughness(Rq＜0.5nm) can be obtained by spin coating without solvent.The refractive index of PSQ-Ls can be exactly tuned from 1.450 to 1.520 by blending PSQ-LH and PSQ-LL at room temperature.There are there reactive groups in PSQ-Ls,C=C,Si-OH and Si-OCH_3.In the simplex photoinitiator curing system,a majority of Si-OCH_3 is reserved but hardly find Si-OH in the films which undergo UV curing and thermal curing processes.And the optical loss of the corresponding waveguide film is as low as 0.70dB·cm~(-1).The curing process is optimized for the simplex photoinitiator system,and the dependence of optical properties on water feed,UV exposure time,thermal curing temperature and time is discussed.Optical losses of cured PSQ-LH films are about 0.70～0.80dB·cm~(-1) at 1550nm and 0.20～0.30dB·cm~(-1) and birefringence are lower than 0.0005 at both wavelength.The thermal-optic coefficients are-2.2×10~(-4)℃~(-1) for PSQ-LL cured films both at 1310nm and 1550nm,and -2.4×10~(-4)℃~(-1) for PSQ-LH cured films both at 1310nm and 1550nm.In addition,the cured films aren't exist Tg in the range of 40～300℃,and Td with 1.0wt%weight loss are 330～347℃for PSQ-LH films, and 322～328℃for PSQ-LL films in nitrogen.
In order to increase refractive index and improve mechanical property of above hybrid materials,three hybrid materials containing bridged structures(P-6FDA,P-DP and P-DHPZ) are synthesized from(6FDA-Si,DP-Si,and DHPZ-Si),diphenylsilanediol andγ-methacryloxypropyltrimethoxysilane respectively.After UV(IHT-PI 184 as photoinitiator) and thermal curing process,the optical losses of P-6FDA,P-DP and P-DHPZ films are 0.39, 0.25,and 0.39dB·cm~(-1) at 1310nm respectively,and 0.63,0.62 and 0.82dB·cm~(-1) at 1550nm respectively,the refractive index are 1.525(TE),1.550(TE),and 1.558(TE) at 1310nm respectively,and 1.522(TE),1.548(TE) and 1.556(TE) at 1550nm respectively. Birefringences are＜0.0005,0.0012 and 0.0028 at 1310nm respectively,and＜0.0005,0.0010 and 0.0027 at 1550nm respectively.Three cured films also show outstanding thermal stability (Td with 1.0wt%weight loss are 333℃,334℃and 366℃in nitrogen,and no Tg in the range of 40～300℃).
PSQ-Ls material system can satisfy requirements for integrated optical waveguide. Conventional lithographic patterning,hard nanoimprint and soft nanoimprint are applied to fabricate optical waveguides using PSQ-Ls.And high quality sidewalls of waveguides are obtained,and achieve propagation light by a straight waveguide.In addition,PSQ-Ls also applied to fabricate Fabry-Perot fiber pressure sensor successfully.
引文
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