液晶/聚合物光栅激光器的制备研究
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摘要
液晶/聚合物光栅是通过液晶中光敏单体的定域光聚合而形成的折射率周期变化结构。如果在光栅形成之前将激光染料混合到材料中，就能制作出染料掺杂的分布反馈激光器：在泵浦光激发下染料能级实现粒子数反转，再由光栅的选模、增益放大后，出射激光。该激光器制作成本低，阈值低，线宽窄，具有出射波长可调谐的特点，因而有巨大潜力应用在材料研究的特种光源与高分辨率光谱仪领域。
由于染料的浓度淬灭现象，只能以低浓度掺杂到液晶/聚合物光栅中，使得增益介质层对泵浦光吸收效率低下，激光的能量转化率很低。另外，液晶/聚合物分布反馈激光器的阈值较高，模式多，激光光斑发散角大且无法控制，严重阻碍了器件的实用化进展。针对以上问题，本论文进行了以下几方面的研究工作。
首先对液晶/聚合物光栅的制备条件进行了深入研究，发现在低强度曝光时相分离出来的液晶能够形成均匀层结构，而不是像通常人们报道的那样以液滴形状出现，由此使光栅散射损失小于4%，符合激光器谐振腔的要求。通过分别实时监测液晶/聚合物光栅形成过程中的S偏振光和P偏振光衍射效率，证实在制备完成的光栅中，相分离的液晶分子沿着光栅矢量取向排列。据此设计了光延迟实验定量给出光栅的相分离度，进一步的以该测量方法为依据，系统研究了照射光偏振，强度以及光栅周期对相分离度的影响，获得了一些制备理想光栅谐振腔的普适规律。光栅矢量方向是激光器中光子的谐振方向，按照初衷谐振腔的设计，液晶分子须沿垂直光栅矢量方向排列，以使光栅界面△n最大、光子的谐振效率最高。依据进一步的实验现象分析得出，液晶分子沿着光栅矢量自取向是缘于来不及到达聚合物层的光敏单体丝状聚合产生的体锚定作用，要克服这种丝状聚合，有效的办法是提高制备光栅时的温度至清亮点以上，令液晶分子在光栅中混乱取向，相对提高光栅界面△n。实验结果表明，通过这一改进使得激光能量效率从0.3%上升到了0.9%，说明了光栅界面△n对于分布式反馈激光器非常重要。
进一步探讨了液晶/聚合物光栅激光器的选模机理，发现这种DFB激光器所支持的模式由两个机理决定，一是以HPDLC层为导芯层的波导机理，使谐振光子在两基板间全反射传播；二是光子在光栅中的布拉格衍射机理，使光子在行进中有效撞击染料中心而反馈增益。基于此理论，通过减小光栅介质与基板间的折射率差、控制光子全反射振荡周期，得到了单模出射的激光器；并对激光器施加电场，改变液晶层的分子取向，得到出射波长8nm变化的连续调谐。
为大幅提高能量转化效率，将高吸光效率的有机半导体增益介质引入到液晶/聚合物激光器中，由于其与液晶不互溶，所以设计成外反馈DFB腔，即液晶/聚合物光栅位于该增益薄膜之上，光栅反馈腔不但触发MEH-PPV膜层激射、同时对激射波产生布拉格衍射作用，形成沿光栅槽出射的截面为直线状的激光束。MEH-PPV薄膜的最佳厚度为75nm，采用S偏振光泵浦，器件出射TE偏振单模激光。在周期590nm的液晶/聚合物三级衍射DFB腔中，工作阈值低至21μJ/cm2，仅为染料光栅激光器的十分之一，能量效率达到6.5%，上升了七倍。采用周期为390nm的液晶/聚合物光栅，实现了二级布拉格反馈条件，工作阈值进一步降至13μJ/cm2，且激光近乎垂直于基板表面发射。出射光斑在平行光栅槽方向呈线状光束，发散角在垂直光栅槽方向近于衍射极限。
本论文系统研究了液晶/聚合物光栅激光器的制备方法，大幅提高了能量转化效率、减小发散角，为可调谐DFB激光器的实用化打下了坚实基础。
Holographic polymer dispersed liquid crystal (HPDLC) gratings are formedthrough photo-polymerization induced anisotropic phase separation of liquid crystal(LC) from the polymer matrix. Distributed feedback (DFB) lasers can be made bydoping the laser dye at a suitable concentration into the HPDLC prepolymer syrup.The HPDLC grating film not only provides coherent Bragg scattering at eachcorrugation for positive optical feedback, but also works as the gain medium forlight amplification. Lasing can be obtained once input pump energy exceeds thelaser threshold. These organic lasers have advantages of simple fabrication, lowworking threshold, narrow linewidth and wavelength tunability across the wholevisible range. Thus they are very promising in using as optical sources for highsensitivity spectroscopic analysis.
However, the current output lasing from dye-doped HPDLC lasers ismulti-mode with a large divergence. The reported lasing threshold is high and theslope efficiency is ultra-low. In order to address these problems, the correlationsbetween parameters of HPDLC gratings and laser device working performance haveto be considered and the studies into enhancing lasing properties throughoptimization of HPDLC cavities should be put forward. Besides, novel gain mediumshould be introduced to replace the laser dye, as it suffers severely from concentration quenching and provides low absorption efficiency. The mainresearches of this dissertation are listed as follows:
1. We successfully fabricated polymer scaffolding morphologic HPDLCtransmission gratings from common acrylate monomers. The phase separated LCsform homogeneous layers instead of spherical domains. Transmittance measurementshows the grating exhibits little scattering which is less than4%. We also show thatdue to the anchoring effect of polymer filaments across the pure LC layer, thesephase separated LC molecules are well aligned along the grating vector. We furtherdesigned a birefringence experiment to measure the LC phase separation degree inHPDLC gratings, so all structural parameters can be obtained. Based on aboveunderstandings of the grating structure, we then analyzed the effect of fabricationconditions, such as polarization state of the writing beams, exposure intensity andgrating period on LC phase separation degree and obtained some fabrication rulesfor efficient HPDLC gratings. At last, the phase separated LC director configurationis altered by recording the grating at a high temperature. In this way, the refractiveindex modulation for light propagating along the grating vector can be increased andthe slope efficiency for output lasing is enhanced from0.3%to0.9%.
2. We investigated the mode selection mechanism and found it was based ontwo principles. First, the resonant modes should fulfill the waveguide conditions inthe core layer which is the grating layer in dye-doped HPDLC DFB lasers. So thelaser modes could not leak out through the two glass substrates, and light could beeffectively confined inside the grating layer. Second, the resonant mode shouldfulfill the Bragg condition of the grating, so positive optical feedback can beobtained through coherent Bragg scattering at each corrugation. The mode couldthen be amplified through stimulated emission when it is travelling around. Themode emits lasing when the pump energy reaches the working threshold. Based onthe mode selection mechanism, we modulate or optimize the output lasing modesaccordingly. We show that the lasing wavelength could be continuously tuned over8nm by applying an electrical field. The homogenously aligned LC molecules along the grating vector could be reoriented to the cell normal, thereby increasing theeffective refractive index experiencing by the laser mode. The electrical tunability oflasing wavelength from HPDLC based DFB lasers is an attracting advantage and canbe used in optical spectroscopy. The DFB working structure is optimized from theperspective of refractive index difference between the cladding layer and the corelayer to allow only one lasing mode being resonated.
3. Organic semiconductor has been introduced as gain medium to HPDLC basedDFB lasers. Unlike the dye molecules, organic semiconductor is immiscible withHPDLC prepolymer syrup. So we have designed a new DFB working structure inwhich the grating layer is fabricated separately on top of the gain medium layer. Thetwo layers interact with each other by evanescent wave spread into the claddinglayer. We show that the thickness of the organic semiconductor layer has to bearound75nm to balance optical feedback and light amplification in order to obtain ahigh performance lasing output. The output lasing shows single-mode, linearpolarization performance, and can be tuned in the gain spectrum of the gain medium.The working threshold is21μJ/cm2(one tenth that of dye-doped HPDLC lasers) andthe slope efficiency is increased to5.9%(six times that of dye doped HPDLC lasers).We further show the effect of pump polarization on working performance and finds-polarization guarantees best working performance. We then made verticallysurface-emitting organic lasers by employing second-order Bragg scattering. Theperiod of the HPDLC grating is just394nm and emitted lasing is coupled outthrough first-order scattering. Thanks to more efficient light coupling insecond-order Bragg scattering, the laser threshold of this surface-emitting laser isreduced to13μJ/cm2. We also investigate the effect of pump length on laserthreshold, and show the refractive index modulation HPDLC grating is sufficient forefficient feedback as long as the pump length is longer than0.03cm.
由于染料的浓度淬灭现象，只能以低浓度掺杂到液晶/聚合物光栅中，使得增益介质层对泵浦光吸收效率低下，激光的能量转化率很低。另外，液晶/聚合物分布反馈激光器的阈值较高，模式多，激光光斑发散角大且无法控制，严重阻碍了器件的实用化进展。针对以上问题，本论文进行了以下几方面的研究工作。
首先对液晶/聚合物光栅的制备条件进行了深入研究，发现在低强度曝光时相分离出来的液晶能够形成均匀层结构，而不是像通常人们报道的那样以液滴形状出现，由此使光栅散射损失小于4%，符合激光器谐振腔的要求。通过分别实时监测液晶/聚合物光栅形成过程中的S偏振光和P偏振光衍射效率，证实在制备完成的光栅中，相分离的液晶分子沿着光栅矢量取向排列。据此设计了光延迟实验定量给出光栅的相分离度，进一步的以该测量方法为依据，系统研究了照射光偏振，强度以及光栅周期对相分离度的影响，获得了一些制备理想光栅谐振腔的普适规律。光栅矢量方向是激光器中光子的谐振方向，按照初衷谐振腔的设计，液晶分子须沿垂直光栅矢量方向排列，以使光栅界面△n最大、光子的谐振效率最高。依据进一步的实验现象分析得出，液晶分子沿着光栅矢量自取向是缘于来不及到达聚合物层的光敏单体丝状聚合产生的体锚定作用，要克服这种丝状聚合，有效的办法是提高制备光栅时的温度至清亮点以上，令液晶分子在光栅中混乱取向，相对提高光栅界面△n。实验结果表明，通过这一改进使得激光能量效率从0.3%上升到了0.9%，说明了光栅界面△n对于分布式反馈激光器非常重要。
进一步探讨了液晶/聚合物光栅激光器的选模机理，发现这种DFB激光器所支持的模式由两个机理决定，一是以HPDLC层为导芯层的波导机理，使谐振光子在两基板间全反射传播；二是光子在光栅中的布拉格衍射机理，使光子在行进中有效撞击染料中心而反馈增益。基于此理论，通过减小光栅介质与基板间的折射率差、控制光子全反射振荡周期，得到了单模出射的激光器；并对激光器施加电场，改变液晶层的分子取向，得到出射波长8nm变化的连续调谐。
为大幅提高能量转化效率，将高吸光效率的有机半导体增益介质引入到液晶/聚合物激光器中，由于其与液晶不互溶，所以设计成外反馈DFB腔，即液晶/聚合物光栅位于该增益薄膜之上，光栅反馈腔不但触发MEH-PPV膜层激射、同时对激射波产生布拉格衍射作用，形成沿光栅槽出射的截面为直线状的激光束。MEH-PPV薄膜的最佳厚度为75nm，采用S偏振光泵浦，器件出射TE偏振单模激光。在周期590nm的液晶/聚合物三级衍射DFB腔中，工作阈值低至21μJ/cm2，仅为染料光栅激光器的十分之一，能量效率达到6.5%，上升了七倍。采用周期为390nm的液晶/聚合物光栅，实现了二级布拉格反馈条件，工作阈值进一步降至13μJ/cm2，且激光近乎垂直于基板表面发射。出射光斑在平行光栅槽方向呈线状光束，发散角在垂直光栅槽方向近于衍射极限。
本论文系统研究了液晶/聚合物光栅激光器的制备方法，大幅提高了能量转化效率、减小发散角，为可调谐DFB激光器的实用化打下了坚实基础。
Holographic polymer dispersed liquid crystal (HPDLC) gratings are formedthrough photo-polymerization induced anisotropic phase separation of liquid crystal(LC) from the polymer matrix. Distributed feedback (DFB) lasers can be made bydoping the laser dye at a suitable concentration into the HPDLC prepolymer syrup.The HPDLC grating film not only provides coherent Bragg scattering at eachcorrugation for positive optical feedback, but also works as the gain medium forlight amplification. Lasing can be obtained once input pump energy exceeds thelaser threshold. These organic lasers have advantages of simple fabrication, lowworking threshold, narrow linewidth and wavelength tunability across the wholevisible range. Thus they are very promising in using as optical sources for highsensitivity spectroscopic analysis.
However, the current output lasing from dye-doped HPDLC lasers ismulti-mode with a large divergence. The reported lasing threshold is high and theslope efficiency is ultra-low. In order to address these problems, the correlationsbetween parameters of HPDLC gratings and laser device working performance haveto be considered and the studies into enhancing lasing properties throughoptimization of HPDLC cavities should be put forward. Besides, novel gain mediumshould be introduced to replace the laser dye, as it suffers severely from concentration quenching and provides low absorption efficiency. The mainresearches of this dissertation are listed as follows:
1. We successfully fabricated polymer scaffolding morphologic HPDLCtransmission gratings from common acrylate monomers. The phase separated LCsform homogeneous layers instead of spherical domains. Transmittance measurementshows the grating exhibits little scattering which is less than4%. We also show thatdue to the anchoring effect of polymer filaments across the pure LC layer, thesephase separated LC molecules are well aligned along the grating vector. We furtherdesigned a birefringence experiment to measure the LC phase separation degree inHPDLC gratings, so all structural parameters can be obtained. Based on aboveunderstandings of the grating structure, we then analyzed the effect of fabricationconditions, such as polarization state of the writing beams, exposure intensity andgrating period on LC phase separation degree and obtained some fabrication rulesfor efficient HPDLC gratings. At last, the phase separated LC director configurationis altered by recording the grating at a high temperature. In this way, the refractiveindex modulation for light propagating along the grating vector can be increased andthe slope efficiency for output lasing is enhanced from0.3%to0.9%.
2. We investigated the mode selection mechanism and found it was based ontwo principles. First, the resonant modes should fulfill the waveguide conditions inthe core layer which is the grating layer in dye-doped HPDLC DFB lasers. So thelaser modes could not leak out through the two glass substrates, and light could beeffectively confined inside the grating layer. Second, the resonant mode shouldfulfill the Bragg condition of the grating, so positive optical feedback can beobtained through coherent Bragg scattering at each corrugation. The mode couldthen be amplified through stimulated emission when it is travelling around. Themode emits lasing when the pump energy reaches the working threshold. Based onthe mode selection mechanism, we modulate or optimize the output lasing modesaccordingly. We show that the lasing wavelength could be continuously tuned over8nm by applying an electrical field. The homogenously aligned LC molecules along the grating vector could be reoriented to the cell normal, thereby increasing theeffective refractive index experiencing by the laser mode. The electrical tunability oflasing wavelength from HPDLC based DFB lasers is an attracting advantage and canbe used in optical spectroscopy. The DFB working structure is optimized from theperspective of refractive index difference between the cladding layer and the corelayer to allow only one lasing mode being resonated.
3. Organic semiconductor has been introduced as gain medium to HPDLC basedDFB lasers. Unlike the dye molecules, organic semiconductor is immiscible withHPDLC prepolymer syrup. So we have designed a new DFB working structure inwhich the grating layer is fabricated separately on top of the gain medium layer. Thetwo layers interact with each other by evanescent wave spread into the claddinglayer. We show that the thickness of the organic semiconductor layer has to bearound75nm to balance optical feedback and light amplification in order to obtain ahigh performance lasing output. The output lasing shows single-mode, linearpolarization performance, and can be tuned in the gain spectrum of the gain medium.The working threshold is21μJ/cm2(one tenth that of dye-doped HPDLC lasers) andthe slope efficiency is increased to5.9%(six times that of dye doped HPDLC lasers).We further show the effect of pump polarization on working performance and finds-polarization guarantees best working performance. We then made verticallysurface-emitting organic lasers by employing second-order Bragg scattering. Theperiod of the HPDLC grating is just394nm and emitted lasing is coupled outthrough first-order scattering. Thanks to more efficient light coupling insecond-order Bragg scattering, the laser threshold of this surface-emitting laser isreduced to13μJ/cm2. We also investigate the effect of pump length on laserthreshold, and show the refractive index modulation HPDLC grating is sufficient forefficient feedback as long as the pump length is longer than0.03cm.
引文
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