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How does resistivity change during curing?

Abstract: 文章探讨了在固化过程中电阻率的变化及其对过程控制的应用。图1展示了在等温固化过程中电阻率随玻璃化转变温度(Tg)变化的情况,表明微介质传感器在涂层监测和过程控制中的有效性。通过实时监测电阻率,结合温度或压力变化,可以实现精确的反应控制。文章详细介绍了两种过程控制方法:1) 介电反馈控制,通过监测和调节电阻率(或粘度)来保持固化过程中的稳定性;2) 介质-热反馈控制,使用微介质传感器与石墨环氧材料接触,防止过固化,并优化反应时间。图2展示了如何通过这些反馈技术实现有效的固化过程控制。

Figure 1 depicts the change in resistivity as a function of glass transition temperature during isothermal curing. These data demonstrate the use of micromedia sensors for coating monitoring and process control.

Using the techniques described earlier, ionic conductivity (or its inverse, resistivity) can be obtained in real time by continuously monitoring a series of frequencies. It can then control the reaction by changing the temperature or pressure. There are several ways to use dielectric feedback. Some of these examples are as follows:

•The temperature can be kept constant or controlled until the desired viscosity is reached (medium measurement).

• Viscosity can be kept constant or changed at will by controlling temperature changes.

Fig.1 Ion resistivity data and Tg during isothermal epoxy-amine curing

1. Process control via dielectric feedback

Figure 2 shows an example of process-controlled curing of graphite epoxy resin using micromedia feedback. Using improved Micromet Instruments dielectric software and hardware, the control is realized on IBM PC. Curing is carried out on a heat press with computer controlled temperature. The sequence of process control software is as follows:

1. Heat and hold at 250° until log resistivity reaches 7.0 (allows degassing while preventing premature curing).

2. Maintain resistivity (viscosity) at 7.0 until 350°F (allows controlled cure, prevents second viscosity minimum).

3. Hold at 350°F until the dielectric reaction rate approaches zero (allow the reaction to complete).

4. Cool down and notify the operator that the cycle is complete.

Fig. 2 The process of controlling the curing of epoxy graphite by microdielectric feedback

2. Medium-thermal feedback process control

Curing in Figure 2 is fully controlled by media and thermal feedback. The micro-media sensor is in contact with a graphite epoxy material. Note that the secondary viscosity (resistivity) minima for these materials are completely eliminated by using viscosity control. This technique is useful for limiting excessive emissions from composite materials prone to this type of problem. Finally, detect the end point, stop the reaction, and save unnecessary over-curing time.

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