High-throughput measurement of polymer blend phase behavior
High-throughput measurement of polymer blend phase behavior
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DOI：
10.1021/ma0004662
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发表时间：
2000-08-08
期刊：
影响因子：
5.5
通讯作者：
Amis, EJ
中科院分区：
文献类型：
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作者：
Meredith, JC;Karim, A;Amis, EJ
导言。由于药物研究的成功，组合和高通量方法在合成和发现新的无机材料、4-6催化剂、7、8和有机聚合物方面受到越来越多的关注。组合方法还可以快速扫描参数空间，以进行基本测量和开发聚合物的物理模型。一个限制是用常规仪器和样品制备制备并行文库和进行高通量筛选的难度。最近，我们开发了一种研究聚合物薄膜去湿现象的组合技术，通过使用具有厚度和温度垂直梯度的样本库，在几个小时的实验中创建了一个大型的去湿信息数据库。3，11本报告描述了利用一种新的样品沉积方法高通量测量聚合物共混物的浊点，以创建二维组成(φ)、温度(T)库。在样品库中，T和φ是正交变化的，光学显微镜用来检测相分离和微观结构。用这种高通量方法测定的浊点通过与常规光散射结果和单组分控制的比较进行了验证。制备组成梯度膜涉及三个步骤：梯度混合(图1a)、沉积(图1b)和膜铺展(图1c)。两个注射器泵(哈佛PHD2000)12(图1a)分别以速度I和W将聚合物溶液引入混合瓶和从混合瓶中取出聚合物溶液，其中I)W)1.7毫升/分钟。泵I在甲苯中含有质量分数为0.080的聚苯乙烯(PS，MR)96.4 kg/m ol，MR/Mn 1.01，Tosoh)13。从泵W中装入质量分数为0.080的聚甲基乙烯基醚的初始质量分数为2.0mLPVME，mR/mN为2.514。在大力搅拌小瓶溶液的同时启动输液和退出注射泵，并使用第三个注射器S手动从小瓶中提取溶液。瞬时混合过程的质量平衡得出在任何时间t(分钟)瓶中PS、XPS的质量分数为
Introduction. Because of successes in pharmaceuticals research, combinatorial and high-throughput methods for searching composition space1-3 have received increasing attention for the synthesis and discovery of new inorganic materials, 4-6 catalysts, 7, 8 and organic polymers. 9, 10 Combinatorial methods can also allow rapid scanning of parameter space to make fundamental measurements and develop physical models for polymers. One limitation is the difficulty of preparing parallel libraries and performing highthroughput screening with conventional instrumentation and sample preparation. Recently, we developed a combinatorial technique for investigating polymer thin film dewetting phenomena by using sample libraries with orthogonal gradients in thickness and temperature to create a large database of dewetting information in a few hours of experiments. 3, 11 This report describes high-throughput measurement of cloud points for polymer blends utilizing a novel sample deposition method for creating two-dimensional composition (φ), temperature (T) libraries. In the sample libraries, T and φ are varied orthogonally, and optical microscopy is used to detect phase separation and microstructure. The cloud points determined with this high-throughput method are validated by comparison to conventional light scattering results and singlecomposition controls.Library Preparation. Three steps are involved in preparing composition gradient films: gradient mixing (Figure 1a), deposition (Figure 1b), and film spreading (Figure 1c). Two syringe pumps (Harvard PHD2000) 12 (Figure 1a) introduce and withdraw polymer solutions to and from a mixing vial at rates I and W, respectively, where I) W) 1.7 mL/min. Pump I contained mass fraction xPS, O) 0.080 of polystyrene (PS, Mr) 96.4 kg/mol, Mr/Mn) 1.01, Tosoh) 13 in toluene. The vial was loaded with an initial M0) 2.0 mL of mass fraction xPVME, O) 0.080 of poly (vinyl methyl ether)(PVME, Mr) 119 kg/mol, Mr/Mn) 2.5) 14 in toluene from pump W. The infusion and withdrawal syringe pumps were started simultaneously while vigorously stirring the vial solution, and a third syringe, S, was used to manually extract solution from the vial. A mass balance of the transient mixing process gives the mass fraction of PS, xPS, in the vial at any time t (minutes) as