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Monitoring and optimization of the synthesis process of the holographic doped photopolymers
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摘要:
掺杂光致聚合物的合成过程对其性能的影响至关重要。目前掺杂光致聚合物的合成过程优化主要依靠大量实验数据和操作者实验经验。本文提出了一种利用掺杂光致聚合物的吸收光谱定量化分析光致聚合物合成过程的方法。该方法通过对掺杂光致聚合物制备过程中的各个阶段样品进行吸收光谱测量分析，揭示样品制备过程中吸收光谱随制备过程变化的趋势，并利用吸收光谱法定量监测聚合物预聚合过程的程度和速率，为科学定量优化掺杂光致聚合物制备过程提供了新方法。
Abstract:The synthesis process of doped photopolymer has a significant impact on its properties. The tradional optimization method for the synthesis process of doped photopolymers depends on experimental parameters and experimental experience. A method for quantitatively monitoring and optimization of the synthesis process of doped photopolymers by absorption spectrum is presented in this paper. The absorption spectra of samples in different steps of the preparation are measured and analyzed. The change rule of the absorption spectra in preparation process is revealed. Quantitative monitoring of the progress and the synthesis rate of photopolymers could be realized by the proposed method. This method brings new possibility to quantitative optimization in the preparation process of doped photopolymers.
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Key words:
- absorption spectrum /
- photopolymer /
- quantitative monitoring /
- quantitative optimization
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Overview: The photopolymer has the advantages of high sensitivity, high resolution, low cost, simple fabrication and good optical performance. The photopolymer has the disadvantages of high shrinkage and low diffraction efficiency, which limit its applications. The doped photopolymer is an improved holographic material compared to the pure photopolymer because it has lower shrinkage and higher diffraction efficiency. The synthesis process of the doped photopolymer has a significant impact on its properties. The traditional optimization method for the synthesis process of the doped photopolymer depends on experimental parameters and experimental experience. A method for quantitative monitoring and optimization of the synthesis process by absorption spectrum is presented in this paper.
Different substances have different compositions and structures. The absorption spectra of various substances are also different. Therefore, qualitative or quantitative analysis of substances could be carried out according to their absorption spectra. The sample used in this work is nanoparticle doped polymethyl methacrylate (PMMA) photopolymer. The single wavelength electromagnetic wave is obtained by a white light source through the spectroscopic system. After passing through the sample at a certain distance, the single-wavelength electromagnetic wave enters the detector. By comparing the light intensity of transmitted single-wavelength electromagnetic wave with the original intensity, the absorption intensity of the sample under the specific wavelength could be obtained. By measuring the absorption intensities under various wavelengths, the absorption spectra of the sample could be obtained.
The pre-polymerization process is very important for the synthesis of the photopolymer. However, there is no quantitative monitoring technology for the process of pre-polymerization. Because the pre-polymerization process results in strong changes in absorption spectrum, the pre-polymerization process could be monitored by the proposed absorption spectrum method. With the absorption spectrum method, the degree and the rate of the pre-polymerization could be monitored and expressed by absorption intensity. More experimental conditions of pre-polymerization could also be determined. Thus, the synthesis process of doped photopolymer can be optimized.
This optimization method can not only be applied to the preparation of doped PMMA photopolymer, but also has important value for the preparation of other materials synthesized by polymerization. It also provides an effective way to fabricate stable doped photopolymers.
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图 1 金纳米棒掺杂光致聚合物制备流程示意图
Figure 1. Synthesis process of the gold nanoparticles doped photopolymer for volume holography
图 2 吸收光谱法测量掺杂光致聚合物制备过程示意图
Figure 2. The principle of absorption spectroscopy during the preparation of doped photopoly
图 3 掺杂光致聚合物制备过程光谱变化
Figure 3. Spectral changes during the preparation of doped photopolymers
图 4 掺杂光致聚合物制备过程中固化前后1 mm厚度样品吸收光谱变化
Figure 4. Absorption spectra changes before and after curing during the preparation of 1 mm doped photopolymer
图 5 预聚合过程中样品多波长吸收强度变化
Figure 5. Absorption intensity of samples during pre-poly merization at several wavelengths
表 1 预聚合过程中不同时段预聚合速率
Table 1. Average pre-polymerization rate of different phases at three wavelengths
Time/h 400/nm 500/nm 600/nm 0~1 0.066 0.066 0.054 1~1.5 0.198 0.204 0.186 1.5~2 0.011 0.042 -0.018 2~2.5 0.018 0.006 0.012 
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