CN108562609B - A method for predicting the effect of thermal cycling on the thermal expansion coefficient of polymer matrix composites based on free radical content - Google Patents
A method for predicting the effect of thermal cycling on the thermal expansion coefficient of polymer matrix composites based on free radical content Download PDFInfo
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- 150000003254 radicals Chemical class 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229920013657 polymer matrix composite Polymers 0.000 title claims abstract description 38
- 239000011160 polymer matrix composite Substances 0.000 title claims abstract description 38
- 238000005382 thermal cycling Methods 0.000 title description 13
- 230000000694 effects Effects 0.000 title 1
- 239000002131 composite material Substances 0.000 claims abstract description 46
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- 238000012360 testing method Methods 0.000 claims description 88
- 239000000463 material Substances 0.000 claims description 44
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 23
- 239000004917 carbon fiber Substances 0.000 claims description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 239000000805 composite resin Substances 0.000 claims description 10
- 239000004643 cyanate ester Substances 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 10
- 229920000647 polyepoxide Polymers 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
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Abstract
一种基于自由基含量预测热循环对聚合物基复合材料热膨胀系数影响的方法，它属于复合材料的尺寸稳定性的评价技术领域，本发明解决了航天器在轨运行期间，由于受到实验条件和设备条件的限制，对结构复杂的聚合物基复合材料的热膨胀系数的测量需要的时间较长，且测量难度较高的问题。本发明在真空度小于1Pa条件下，对需要测定热膨胀系数的聚合物基复合材料进行热循环实验，得出该聚合物基复合材料的自由基含量随着热循环次数的变化规律与热膨胀系数随着热循环次数的变化规律一致，因此，在轨运行期间，可以仅测量自由基含量来预测聚合物基复合材料的热膨胀系数。本发明可以应用于复合材料的尺寸稳定性的评价技术领域用。
A method for predicting the influence of thermal cycle on the thermal expansion coefficient of polymer-based composite materials based on the content of free radicals belongs to the technical field of evaluation of the dimensional stability of composite materials. Due to the limitation of equipment conditions, it takes a long time to measure the thermal expansion coefficient of polymer matrix composites with complex structures, and the measurement is difficult. In the present invention, under the condition that the vacuum degree is less than 1Pa, the thermal cycle experiment is carried out on the polymer-based composite material whose thermal expansion coefficient needs to be measured, and it is obtained that the free radical content of the polymer-based composite material varies with the number of thermal cycles and the thermal expansion coefficient varies with Therefore, the thermal expansion coefficient of polymer matrix composites can be predicted only by measuring the free radical content during on-orbit operation. The present invention can be applied to the technical field of evaluation of the dimensional stability of composite materials.
Description
技术领域technical field
本发明属于复合材料的尺寸稳定性的评价技术领域，具体涉及一种基于自由基含量预测热循环对聚合物基复合材料热膨胀系数影响的方法。The invention belongs to the technical field of evaluation of the dimensional stability of composite materials, in particular to a method for predicting the influence of thermal cycles on the thermal expansion coefficient of polymer-based composite materials based on the content of free radicals.
背景技术Background technique
在航天领域，聚合物基复合材料主要应用于主承力筒、太阳电池阵基板、光学遥感器及抛物面天线等结构中。由于航天器在轨运行期间需反复进出地球阴影区域，所以航天器所处的外界环境温度在-160℃～120℃范围内交替变化。美国航天局、欧空局和我国都明确规定了航天器及其组件验收时的真空热循环实验规范，可见研究真空热循环条件下聚合物基复合材料的行为对于保证航天器在轨安全运行，提高服役的可靠性及使用寿命具有重要的意义。In the aerospace field, polymer-based composite materials are mainly used in structures such as main bearing cylinders, solar cell array substrates, optical remote sensors and parabolic antennas. Since the spacecraft needs to repeatedly enter and exit the shadowed area of the earth during its orbital operation, the external ambient temperature where the spacecraft is located varies alternately within the range of -160°C to 120°C. NASA, ESA and my country have clearly stipulated the vacuum thermal cycle experimental specifications for the acceptance of spacecraft and their components. It can be seen that studying the behavior of polymer matrix composites under vacuum thermal cycling conditions is important to ensure the safe operation of spacecraft on orbit. It is of great significance to improve the reliability and service life of the service.
由于聚合物基复合材料与增强纤维热膨胀系数相差一个数量级，聚合物基复合材料在交变温度场的作用下材料内将产生热应力，随着热应力累积会使材料内产生微裂纹，最终导致材料力学性能和尺寸稳定性下降，因此，预测聚合物基复合材料的热膨胀系数对研究聚合物基复杂材料的结构具有重要意义。然而，航天器在轨运行期间，由于受到目前实验条件和设备条件的限制，对于很多结构复杂的聚合物基复合材料来说，直接测其热膨胀系数需要的测量时间较长，而且，由于热膨胀系数的测量必须将聚合物基复合材料制成标准件才能进行，所以测量难度较高。Since the thermal expansion coefficient of the polymer matrix composite material and the reinforcing fiber differ by an order of magnitude, the polymer matrix composite material will generate thermal stress in the material under the action of the alternating temperature field. The mechanical properties and dimensional stability of materials decrease, therefore, predicting the thermal expansion coefficient of polymer-based composites is of great significance for studying the structure of polymer-based complex materials. However, due to the limitations of the current experimental conditions and equipment conditions during the spacecraft's orbital operation, for many polymer matrix composites with complex structures, it takes a long time to directly measure the thermal expansion coefficient. Moreover, due to the thermal expansion coefficient The measurement of the polymer matrix composite material must be made into a standard part, so the measurement is difficult.
发明内容SUMMARY OF THE INVENTION
本发明的目的是为解决航天器在轨运行期间，由于受到实验条件和设备条件的限制，对结构复杂的聚合物基复合材料的热膨胀系数的测量需要的时间较长，且测量难度较高的问题。The purpose of the present invention is to solve the problem that the measurement of the thermal expansion coefficient of the polymer matrix composite material with complex structure requires a long time and is difficult to measure due to the limitation of experimental conditions and equipment conditions during the orbital operation of the spacecraft. question.
本发明为解决上述技术问题采取的技术方案是：The technical scheme that the present invention takes for solving the above-mentioned technical problems is:
步骤一、选用聚合物基复合材料作为实验样品，在真空度小于1Pa的条件下，对所选用的实验样品进行热循环试验；设定每组热循环试验的热循环次数不少于200次，热循环试验的组数不少于3组；Step 1. Select the polymer matrix composite material as the experimental sample. Under the condition that the vacuum degree is less than 1Pa, carry out the thermal cycle test on the selected experimental sample; The number of groups in the thermal cycle test shall not be less than 3;
步骤二、每次热循环后均取出实验样品，并对取出的实验样品进行热膨胀系数测试；分别记录每组热循环试验的不同热循环次数下的热膨胀系数；计算各组热循环试验的相同热循环次数对应的热膨胀系数的平均值，得到不同热循环次数下的热膨胀系数变化规律；Step 2: After each thermal cycle, the experimental samples are taken out, and the thermal expansion coefficient test is carried out on the taken out experimental samples; the thermal expansion coefficients under different thermal cycle times of each group of thermal cycle tests are respectively recorded; The average value of the thermal expansion coefficient corresponding to the number of cycles is obtained, and the variation law of the thermal expansion coefficient under different thermal cycles is obtained;
步骤三、对步骤二中每次取出的实验样品进行自由基含量测试，计算各组热循环试验的相同热循环次数对应的自由基含量的平均值，得到不同热循环次数下的自由基含量变化规律；Step 3: Carry out the free radical content test on the experimental samples taken out in step 2 each time, calculate the average value of the free radical content corresponding to the same thermal cycle number of each group of thermal cycle tests, and obtain the change of the free radical content under different thermal cycle times. law;
步骤四、对比步骤二中的热膨胀系数随热循环次数的变化曲线和步骤三中的自由基含量随热循环次数的变化曲线，得出自由基含量和热膨胀系数均随着热循环次数的增加而减小，且自由基含量随着热循环次数的变化规律与热膨胀系数随着热循环次数的变化规律一致；Step 4. Comparing the variation curve of the thermal expansion coefficient with the number of thermal cycles in step 2 and the variation curve of the free radical content with the number of thermal cycles in step 3, it is concluded that both the content of free radicals and the thermal expansion coefficient increase with the increase of the number of thermal cycles. decreases, and the change rule of radical content with the number of thermal cycles is consistent with the change rule of the thermal expansion coefficient with the number of thermal cycles;
步骤五、对于某种需要测量热膨胀系数的聚合物基复合材料，按照步骤一至步骤三的方法，得到该聚合物基复合材料的热膨胀系数随热循环次数的变化规律和自由基含量随热循环次数的变化规律；在轨运行期间，只需要按照步骤三的方法测量该聚合物基复合材料的自由基含量；Step 5. For a certain polymer-based composite material that needs to measure the thermal expansion coefficient, according to the methods from steps 1 to 3, obtain the variation law of the thermal expansion coefficient of the polymer-based composite material with the number of thermal cycles and the free radical content with the number of thermal cycles. During the on-orbit operation, it is only necessary to measure the free radical content of the polymer matrix composite material according to the method of step 3;
步骤六、根据步骤五测量得到的自由基含量，通过查该聚合物基复合材料的热膨胀系数随热循环次数的变化规律和自由基含量随热循环次数的变化规律，来预测该聚合物基复合材料的热膨胀系数。Step 6: According to the free radical content measured in step 5, the polymer matrix composite material is predicted by checking the variation law of the thermal expansion coefficient of the polymer matrix composite material with the number of thermal cycles and the variation rule of the free radical content with the number of thermal cycles. The thermal expansion coefficient of the material.
本发明的有益效果是：本发明提供了一种基于自由基含量预测热循环对聚合物基复合材料热膨胀系数影响的方法，本发明选用碳纤维氰酸酯树脂复合材料或碳纤维环氧树脂复合材料作为实验样品，在真空度小于1Pa条件下，对实验样品进行热循环试验，每组热循环试验的热循环次数不少于200次，且每次热循环后均取出实验样品，对取出的实验样品的自由基含量和热膨胀系数进行测试，得出自由基含量随热循环次数的变化规律与热膨胀系数随着热循环次数的变化规律一致；因此，针对某种需要测量热膨胀系数的聚合物基复合材料，我们可以通过模拟在轨运行时的空间条件，来得到该聚合物基复合材料的热膨胀系数和自由基含量随热循环次数的变化规律，在轨运行期间，仅需要测量该聚合物基复合材料的自由基含量，就可以通过查已测得的该聚合物基复合材料的热膨胀系数和自由基含量随热循环次数的变化规律来预测出该聚合物基复合材料的热膨胀系数。The beneficial effects of the present invention are as follows: the present invention provides a method for predicting the influence of thermal cycles on the thermal expansion coefficient of polymer-based composite materials based on the content of free radicals, and the present invention selects carbon fiber cyanate ester resin composite materials or carbon fiber epoxy resin composite materials as For the experimental samples, under the condition that the vacuum degree is less than 1Pa, the thermal cycle test is carried out on the experimental samples. The number of thermal cycles of each group of thermal cycle tests is not less than 200 times, and the experimental samples are taken out after each thermal cycle. The free radical content and thermal expansion coefficient were tested, and it was found that the change rule of the free radical content with the number of thermal cycles was consistent with the change rule of the thermal expansion coefficient with the number of thermal cycles; therefore, for a polymer matrix composite material that needs to measure the thermal expansion coefficient , we can obtain the variation law of thermal expansion coefficient and radical content of the polymer matrix composite with the number of thermal cycles by simulating the space conditions during on-orbit operation. During the on-orbit operation, only the polymer matrix composite needs to be measured. The thermal expansion coefficient of the polymer matrix composite material can be predicted by checking the measured thermal expansion coefficient of the polymer matrix composite material and the variation law of the free radical content with the number of thermal cycles.
采用本发明的方法来预测热循环后聚合物基复合材料的热膨胀系数，可以节约80％的热膨胀系数的测量时间，而且本发明根据自由基含量来预测热膨胀系数，即不必将复杂结构的聚合物基复合材料制成标准件，就能实现对热膨胀系数测量，大大简化了测量的过程，降低了测量的难度。Using the method of the present invention to predict the thermal expansion coefficient of the polymer matrix composite material after thermal cycling can save 80% of the measurement time of the thermal expansion coefficient, and the present invention predicts the thermal expansion coefficient according to the content of free radicals, that is, it is not necessary to use the polymer with complex structure to predict the thermal expansion coefficient. The matrix composite material is made into a standard part, and the thermal expansion coefficient can be measured, which greatly simplifies the measurement process and reduces the difficulty of measurement.
本发明的方法可以应用于航天领域中对复合材料的研究。The method of the invention can be applied to the research on composite materials in the aerospace field.
附图说明Description of drawings
图1为本发明的一种基于自由基含量预测热循环对聚合物基复合材料热膨胀系数影响的方法的流程图；1 is a flow chart of a method for predicting the influence of thermal cycling on the thermal expansion coefficient of polymer matrix composites based on free radical content according to the present invention;
图2为本发明的实验样品为碳纤维氰酸酯树脂复合材料的热循环试验的升、降温速率为1.5℃/min时，不同热循环次数条件下自由基特征峰的变化曲线图；2 is a graph showing the change of free radical characteristic peaks under different thermal cycle times conditions when the heating and cooling rates of the thermal cycle test of the carbon fiber cyanate ester resin composite material are 1.5° C./min as the experimental sample of the present invention;
图3为本发明的实验样品为碳纤维氰酸酯树脂复合材料的热循环试验的升、降温速率为1.5℃/min时，自由基含量随热循环次数的变化曲线图；3 is a graph showing the change of radical content with the number of thermal cycles when the heating and cooling rates of the thermal cycle test of the carbon fiber cyanate ester resin composite material are 1.5°C/min as the experimental sample of the present invention;
图4为本发明的实验样品为碳纤维氰酸酯树脂复合材料的热循环试验的升、降温速率为1.5℃/min时，热膨胀系数随热循环次数的变化曲线图；4 is a graph showing the variation of thermal expansion coefficient with the number of thermal cycles when the heating and cooling rates of the thermal cycle test of the carbon fiber cyanate ester resin composite material are 1.5°C/min as the experimental sample of the present invention;
图5为本发明的实验样品为碳纤维环氧树脂复合材料的热循环试验的升、降温速率为1.5℃/min时，不同热循环次数条件下自由基特征峰的变化曲线图；5 is a graph showing the change of the characteristic peaks of free radicals under different thermal cycle times when the heating and cooling rates of the thermal cycle test of the carbon fiber epoxy resin composite material are 1.5°C/min as the experimental sample of the present invention;
图6为本发明的实验样品为碳纤维环氧树脂复合材料的热循环试验的升、降温速率为1.5℃/min时，自由基含量随热循环次数的变化曲线图；6 is a graph showing the change of the free radical content with the number of thermal cycles when the heating and cooling rates of the thermal cycle test of the carbon fiber epoxy resin composite material as the experimental sample of the present invention are 1.5°C/min;
图7为本发明的实验样品为碳纤维环氧树脂复合材料的热循环试验的升、降温速率为1.5℃/min时，热膨胀系数随热循环次数的变化曲线图；7 is a graph showing the variation of thermal expansion coefficient with the number of thermal cycles when the heating and cooling rates of the thermal cycle test of the carbon fiber epoxy resin composite material as the experimental sample of the present invention are 1.5°C/min;
图8为本发明的实验样品为碳纤维氰酸酯树脂复合材料的热循环试验的升、降温速率为2.5℃/min时，不同热循环次数条件下自由基特征峰的变化曲线图；8 is a graph showing the change of the characteristic peaks of free radicals under different thermal cycle times when the heating and cooling rates of the thermal cycle test of the carbon fiber cyanate ester resin composite material are 2.5°C/min as the experimental sample of the present invention;
图9为本发明的实验样品为碳纤维氰酸酯树脂复合材料的热循环试验的升、降温速率均为2.5℃/min时，自由基含量随热循环次数的变化曲线图；9 is a graph showing the change of free radical content with the number of thermal cycles when the heating and cooling rates of the thermal cycle test of the carbon fiber cyanate ester resin composite material are both 2.5°C/min as the experimental sample of the present invention;
图10为本发明的实验样品为碳纤维氰酸酯树脂复合材料的热循环试验的升、降温速率均为2.5℃/min时，热膨胀系数随热循环次数的变化曲线图；10 is a graph showing the variation of thermal expansion coefficient with the number of thermal cycles when the heating and cooling rates of the thermal cycle test of the carbon fiber cyanate ester resin composite material are both 2.5°C/min as the experimental sample of the present invention;
图11为本发明的实验样品为碳纤维环氧树脂复合材料的热循环试验的升、降温速率均为2.5℃/min时，不同热循环次数条件下自由基特征峰的变化曲线图；11 is a graph showing the change of free radical characteristic peaks under different thermal cycle times when the heating and cooling rates of the thermal cycle test of the carbon fiber epoxy resin composite material are both 2.5°C/min as the experimental sample of the present invention;
图12为本发明的实验样品为碳纤维环氧树脂复合材料的热循环试验的升、降温速率均为2.5℃/min时，自由基含量随热循环次数的变化曲线图；12 is a graph showing the change of radical content with the number of thermal cycles when the heating and cooling rates of the thermal cycle test of the carbon fiber epoxy resin composite material are both 2.5°C/min as the experimental sample of the present invention;
图13为本发明的实验样品为碳纤维环氧树脂复合材料的热循环试验的升、降温速率均为2.5℃/min时，热膨胀系数随热循环次数的变化曲线图；13 is a graph showing the variation of thermal expansion coefficient with the number of thermal cycles when the heating and cooling rates of the thermal cycle test of the carbon fiber epoxy resin composite material are both 2.5°C/min as the experimental sample of the present invention;
具体实施方式Detailed ways
下面结合附图对本发明的技术方案作进一步的说明，但并不局限于此，凡是对本发明技术方案进行修改或者等同替换，而不脱离本发明技术方案的精神和范围，均应涵盖在本发明的保护范围中。The technical solutions of the present invention will be further described below in conjunction with the accompanying drawings, but are not limited thereto. Any modification or equivalent replacement of the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention shall be included in the present invention. within the scope of protection.
具体实施方式一：结合图1说明本实施方式。本实施方式所述的一种基于自由基含量预测热循环对聚合物基复合材料热膨胀系数影响的方法，该方法的具体步骤为：Embodiment 1: This embodiment is described with reference to FIG. 1 . A method for predicting the influence of thermal cycling on the thermal expansion coefficient of polymer-based composite materials based on the content of free radicals described in this embodiment, the specific steps of the method are:
步骤一、选用聚合物基复合材料作为实验样品，在真空度小于1Pa的条件下，对所选用的实验样品进行热循环试验；设定每组热循环试验的热循环次数不少于200次，热循环试验的组数不少于3组；Step 1. Select the polymer matrix composite material as the experimental sample. Under the condition that the vacuum degree is less than 1Pa, carry out the thermal cycle test on the selected experimental sample; The number of groups in the thermal cycle test shall not be less than 3;
步骤二、每次热循环后均取出实验样品，并对取出的实验样品进行热膨胀系数测试；分别记录每组热循环试验的不同热循环次数下的热膨胀系数；计算各组热循环试验的相同热循环次数对应的热膨胀系数的平均值，得到不同热循环次数下的热膨胀系数变化规律；Step 2: After each thermal cycle, the experimental samples are taken out, and the thermal expansion coefficient test is carried out on the taken out experimental samples; the thermal expansion coefficients under different thermal cycle times of each group of thermal cycle tests are respectively recorded; The average value of the thermal expansion coefficient corresponding to the number of cycles is obtained, and the variation law of the thermal expansion coefficient under different thermal cycles is obtained;
步骤三、对步骤二中每次取出的实验样品进行自由基含量测试，计算各组热循环试验的相同热循环次数对应的自由基含量的平均值，得到不同热循环次数下的自由基含量变化规律；Step 3: Carry out the free radical content test on the experimental samples taken out in step 2 each time, calculate the average value of the free radical content corresponding to the same thermal cycle number of each group of thermal cycle tests, and obtain the change of the free radical content under different thermal cycle times. law;
步骤四、对比步骤二中的热膨胀系数随热循环次数的变化曲线和步骤三中的自由基含量随热循环次数的变化曲线，得出自由基含量和热膨胀系数均随着热循环次数的增加而减小，且自由基含量随着热循环次数的变化规律与热膨胀系数随着热循环次数的变化规律一致；Step 4. Comparing the variation curve of the thermal expansion coefficient with the number of thermal cycles in step 2 and the variation curve of the free radical content with the number of thermal cycles in step 3, it is concluded that both the content of free radicals and the thermal expansion coefficient increase with the increase of the number of thermal cycles. decreases, and the change rule of radical content with the number of thermal cycles is consistent with the change rule of the thermal expansion coefficient with the number of thermal cycles;
步骤五、对于某种需要测量热膨胀系数的聚合物基复合材料，按照步骤一至步骤三的方法，得到该聚合物基复合材料的热膨胀系数随热循环次数的变化规律和自由基含量随热循环次数的变化规律；在轨运行期间，只需要按照步骤三的方法测量该聚合物基复合材料的自由基含量；Step 5. For a certain polymer-based composite material that needs to measure the thermal expansion coefficient, according to the methods from steps 1 to 3, obtain the variation law of the thermal expansion coefficient of the polymer-based composite material with the number of thermal cycles and the free radical content with the number of thermal cycles. During the on-orbit operation, it is only necessary to measure the free radical content of the polymer matrix composite material according to the method of step 3;
步骤六、根据步骤五测量得到的自由基含量，通过查该聚合物基复合材料的热膨胀系数随热循环次数的变化规律和自由基含量随热循环次数的变化规律，来预测该聚合物基复合材料的热膨胀系数。Step 6: According to the free radical content measured in step 5, the polymer matrix composite material is predicted by checking the variation law of the thermal expansion coefficient of the polymer matrix composite material with the number of thermal cycles and the variation rule of the free radical content with the number of thermal cycles. The thermal expansion coefficient of the material.
本实施方式设置热循环试验的组数不少于3组，且每组热循环试验的热循环次数不少于200次，且每次热循环后均取出实验样品进行热膨胀系数和自由基含量的测试，因此，可以分别计算出每个热循环次数点处的各组热膨胀系数的均值和自由基含量的均值，将热膨胀系数的均值、自由基含量的均值分别作为各个热循环次数点的热膨胀系数、自由基含量，来绘制热膨胀系数随热循环次数的变化曲线和自由基含量随热循环次数的变化曲线。通过对比得出，热膨胀系数随热循环次数的变化规律与自由基含量随热循环次数的变化规律一致。In this embodiment, the number of thermal cycle tests is set to be no less than 3 groups, and the number of thermal cycles for each thermal cycle test is no less than 200 times, and the experimental samples are taken out after each thermal cycle for thermal expansion coefficient and free radical content. Therefore, the mean value of thermal expansion coefficient and the mean value of radical content of each group at each thermal cycle number point can be calculated separately, and the mean value of thermal expansion coefficient and the mean value of radical content can be used as the thermal expansion coefficient of each thermal cycle number point. , free radical content, to draw the change curve of thermal expansion coefficient with the number of thermal cycles and the change curve of free radical content with the number of thermal cycles. By comparison, it can be concluded that the variation rule of thermal expansion coefficient with the number of thermal cycles is consistent with the variation rule of free radical content with the number of thermal cycles.
因此，对于某种需要测量热膨胀系数的聚合物基复合材料，在轨运行期间，我们只需要测量其自由基的含量，然后通过查实验条件下得到的该聚合物基复合材料的热膨胀系数和自由基含量随热循环次数的变化规律曲线，就可以得出该聚合物基复合材料的热膨胀系数。Therefore, for a polymer matrix composite material that needs to measure the thermal expansion coefficient, we only need to measure the content of its free radicals during the orbital operation, and then check the thermal expansion coefficient and free radical content of the polymer matrix composite material obtained under the experimental conditions. The thermal expansion coefficient of the polymer matrix composite material can be obtained by the curve of the change rule of the content of the polymer matrix with the number of thermal cycles.
本实施方式设置热循环试验的组数不少于3组，目的是对每个热循环次数对应的热膨胀系数和自由基含量取平均值，以提高数据的准确率。In this embodiment, the number of groups of thermal cycle tests is set to be no less than 3 groups, and the purpose is to average the thermal expansion coefficient and the content of free radicals corresponding to each number of thermal cycles, so as to improve the accuracy of the data.
具体实施方式二：本实施方式对实施方式一所述的一种基于自由基含量预估热循环对聚合物基复合材料热膨胀系数影响的方法进行进一步的限定，本实施方式中的步骤一中的实验样品的尺寸为：长度20mm～25mm，宽度5mm～6mm，厚度1mm～3mm；设定每次热循环的温度范围为-150℃～150℃；Embodiment 2: This embodiment further defines a method for estimating the influence of thermal cycling on the thermal expansion coefficient of polymer-based composite materials based on the content of free radicals described in Embodiment 1. Step 1 in this embodiment The size of the experimental sample is: length 20mm～25mm, width 5mm～6mm, thickness 1mm～3mm; set the temperature range of each thermal cycle to be -150℃～150℃;
设定实验样品周围的环境温度从150℃逐步降温至-150℃，降温速率为x，且0.2≥x>0，单位是℃/min，再以升温速率x将环境温度从-150℃逐步升温至150℃；当实验样品周围的环境温度从150℃到-150℃，再从-150℃到150℃的过程即为一次热循环；Set the ambient temperature around the experimental sample to gradually cool down from 150°C to -150°C, the cooling rate is x, and 0.2≥x>0, the unit is °C/min, and then the ambient temperature is gradually raised from -150°C at the heating rate x to 150°C; when the ambient temperature around the experimental sample is from 150°C to -150°C, and then from -150°C to 150°C, it is a thermal cycle;
本实施方式中设定每次热循环的温度范围为-150℃～150℃，以保证实验样品的试验温度与实际在轨运行期间所处的外界环境温度相匹配。In this embodiment, the temperature range of each thermal cycle is set to be -150°C to 150°C to ensure that the test temperature of the experimental sample matches the external ambient temperature during the actual on-orbit operation.
具体实施方式三：本实施方式对实施方式二所述的一种基于自由基含量预估热循环对聚合物基复合材料热膨胀系数影响的方法进行进一步的限定，所述聚合物基复合材料为碳纤维复合材料。Embodiment 3: This embodiment further defines the method for estimating the influence of thermal cycling on the thermal expansion coefficient of a polymer-based composite material based on the content of free radicals described in Embodiment 2. The polymer-based composite material is carbon fiber. composite material.
具体实施方式四：本实施方式对实施方式三所述的一种基于自由基含量预估热循环对聚合物基复合材料热膨胀系数影响的方法进行进一步的限定，本实施方式中的步骤二的对每次热循环后取出的实验样品的热膨胀系数测试的过程需要在流量为50ml/min的氮气或氩气保护下进行；分别记录每组热循环试验的不同热循环次数下的热膨胀系数；Embodiment 4: This embodiment further defines the method for estimating the influence of thermal cycling on the thermal expansion coefficient of polymer-based composite materials based on the content of free radicals described in Embodiment 3. Step 2 in this embodiment The thermal expansion coefficient test process of the experimental samples taken out after each thermal cycle needs to be carried out under the protection of nitrogen or argon with a flow rate of 50ml/min; the thermal expansion coefficient under different thermal cycle times of each thermal cycle test is recorded separately;
为了防止热膨胀系数的测试过程中实验样品被氧化，测试时采用氮气或氩气保护，且氮气或氩气的流量为50ml/min。In order to prevent the experimental sample from being oxidized during the test of thermal expansion coefficient, nitrogen or argon gas was used for protection during the test, and the flow rate of nitrogen or argon gas was 50ml/min.
计算各组热循环试验的相同热循环次数对应的热膨胀系数的平均值，对测得的热膨胀系数进行处理分析，得到热循环试验的不同热循环次数下的热膨胀系数变化规律。Calculate the average value of the thermal expansion coefficient corresponding to the same number of thermal cycles in each group of thermal cycle tests, process and analyze the measured thermal expansion coefficient, and obtain the variation law of thermal expansion coefficient under different thermal cycle times of the thermal cycle test.
具体实施方式五：本实施方式对实施方式四所述的一种基于自由基含量预估热循环对聚合物基复合材料热膨胀系数影响的方法进行进一步的限定，本实施方式中的步骤三通过调整设备的频率、磁场和增益，对取出的实验样品的自由基含量进行测试；Embodiment 5: This embodiment further defines a method for estimating the influence of thermal cycling on the thermal expansion coefficient of polymer-based composite materials based on the content of free radicals described in Embodiment 4. Step 3 in this embodiment is adjusted by adjusting The frequency, magnetic field and gain of the equipment, to test the free radical content of the experimental sample taken out;
计算各组热循环试验的相同热循环次数对应的自由基含量的平均值，对测得的自由基含量进行处理分析，得到热循环试验的不同热循环次数下的自由基含量变化规律。Calculate the average value of the free radical content corresponding to the same number of thermal cycles in each group of thermal cycle tests, and process and analyze the measured free radical content to obtain the change rule of free radical content under different thermal cycle times in the thermal cycle test.
实施例Example
实施例1Example 1
本发明的一种基于自由基含量预估热循环对聚合物基复合材料热膨胀系数影响的方法，按以下步骤进行：A method of the present invention based on the content of free radicals to estimate the influence of thermal cycle on the thermal expansion coefficient of polymer-based composite materials, is carried out according to the following steps:
步骤一、选用碳纤维氰酸酯树脂复合材料作为实验样品，实验样品的尺寸为：长度25mm，宽度5mm，厚度2mm；在真空度小于1Pa的条件下，对选用的实验样品进行热循环实验，根据航天器在轨的任务期限要求和在轨的工作时间，设定热循环实验的温度范围为-150℃～150℃，升温速率和降温速率均为1.5℃/min；Step 1. Select the carbon fiber cyanate ester resin composite material as the experimental sample. The size of the experimental sample is: length 25mm, width 5mm, thickness 2mm; under the condition that the vacuum degree is less than 1Pa, the selected experimental sample is subjected to a thermal cycle test, according to For the spacecraft's on-orbit mission period and on-orbit working time, the temperature range of the thermal cycle experiment is set to be -150°C to 150°C, and the heating rate and cooling rate are both 1.5°C/min;
步骤二、根据实验要求，每次热循环后均取出实验样品，并对取出的实验样品进行热膨胀系数测试，分别计算各组热循环试验的相同热循环次数对应的热膨胀系数的平均值。为了保证测试过程中温度均匀以及防止氧化，测试时采用氩气保护，流量为50ml/min，根据0次、50次、100次和200次热循环对应的热膨胀系数的平均值，绘制出热循环试验的热膨胀系数随着热循环次数的变化规律，如图4所示。Step 2: According to the experimental requirements, the experimental samples are taken out after each thermal cycle, and the thermal expansion coefficient test is carried out on the taken out experimental samples, and the average value of the thermal expansion coefficient corresponding to the same thermal cycle times of each group of thermal cycle tests is calculated respectively. In order to ensure uniform temperature and prevent oxidation during the test, argon protection was used during the test, and the flow rate was 50ml/min. The thermal cycle was drawn according to the average value of the thermal expansion coefficient corresponding to 0, 50, 100 and 200 thermal cycles. The variation law of the thermal expansion coefficient of the test with the number of thermal cycles is shown in Figure 4.
步骤三、对步骤二中每次取出的实验样品进行自由基含量测试，测试时需要调整设备的频率，磁场和增益，如图2所示，为不同热循环次数条件下自由基特征峰的变化曲线图。Step 3: Test the free radical content of the experimental samples taken out in step 2 each time. During the test, the frequency, magnetic field and gain of the equipment need to be adjusted. Graph.
根据0次、50次、100次和200次热循环对应的自由基含量的平均值，绘制出热循环试验的自由基含量随着热循环次数的变化规律，如图3所示。According to the average value of the free radical content corresponding to 0, 50, 100 and 200 thermal cycles, the variation law of the free radical content in the thermal cycle test with the number of thermal cycles was drawn, as shown in Figure 3.
步骤四、利用步骤二和步骤三得出的热循环试验的自由基含量随热循环次数变化的曲线和热膨胀系数随热循环次数变化的曲线；得出自由基含量和热膨胀系数均随着热循环次数的增加而减小，且自由基含量随着热循环次数的变化规律与热膨胀系数随着热循环次数的变化规律一致；Step 4. Use the curve of the free radical content changing with the number of thermal cycles and the curve of the thermal expansion coefficient changing with the number of thermal cycles obtained in steps 2 and 3; it is obtained that the content of free radicals and the coefficient of thermal expansion change with the thermal cycle. The change of free radical content with the number of thermal cycles is consistent with the change of thermal expansion coefficient with the number of thermal cycles;
步骤五、对于某种需要测量热膨胀系数的聚合物基复合材料，我们可以模拟其在轨运行时的环境条件，按照步骤一至步骤三的方法，得到该聚合物基复合材料的热膨胀系数随热循环次数的变化规律和自由基含量随热循环次数的变化规律；所以，在轨运行期间，只需要按照步骤三的方法测量该聚合物基复合材料的自由基含量；就可以通过查该聚合物基复合材料的热膨胀系数随热循环次数的变化规律和自由基含量随热循环次数的变化规律，来预测该聚合物基复合材料的热膨胀系数。Step 5. For a polymer matrix composite material that needs to measure the thermal expansion coefficient, we can simulate the environmental conditions of its on-orbit operation, and obtain the thermal expansion coefficient of the polymer matrix composite material according to the methods from steps 1 to 3 with thermal cycling. The change law of the number of times and the change law of the free radical content with the number of thermal cycles; therefore, during the on-orbit operation, it is only necessary to measure the free radical content of the polymer matrix composite material according to the method in step 3; The thermal expansion coefficient of the composite material is predicted by the variation law of the thermal expansion coefficient of the composite material with the number of thermal cycles and the change rule of the free radical content with the thermal cycle number to predict the thermal expansion coefficient of the polymer matrix composite material.
采用本发明的方法来预测热循环后聚合物基复合材料的热膨胀系数，可以节约80％的热膨胀系数的测量时间，而且本发明根据自由基含量来预测热膨胀系数，即不必将复杂结构的聚合物基复合材料制成标准件，就能实现对热膨胀系数测量，大大简化了测量的过程，降低了测量的难度。Using the method of the present invention to predict the thermal expansion coefficient of the polymer matrix composite material after thermal cycling can save 80% of the measurement time of the thermal expansion coefficient, and the present invention predicts the thermal expansion coefficient according to the content of free radicals, that is, it is not necessary to use the polymer with complex structure to predict the thermal expansion coefficient. The matrix composite material is made into a standard part, and the thermal expansion coefficient can be measured, which greatly simplifies the measurement process and reduces the difficulty of measurement.
实施例2Example 2
本发明的一种基于自由基含量预估热循环对聚合物基复合材料热膨胀系数影响的方法，按以下步骤进行：A method of the present invention based on the content of free radicals to estimate the influence of thermal cycle on the thermal expansion coefficient of polymer-based composite materials, is carried out according to the following steps:
步骤一、选用碳纤维环氧树脂复合材料作为实验样品，实验样品的尺寸为：长度25mm，宽度5mm，厚度2mm；在真空度小于1Pa的条件下，对选用的实验样品进行热循环实验，根据航天器在轨的任务期限要求和在轨的工作时间，设定热循环实验的温度范围为-150℃～150℃，升温速率和降温速率均为1.5℃/min；Step 1. Select carbon fiber epoxy resin composite material as the experimental sample. The size of the experimental sample is: length 25mm, width 5mm, thickness 2mm; under the condition that the vacuum degree is less than 1Pa, the thermal cycle experiment is carried out on the selected experimental sample. According to aerospace According to the mission period requirements and on-orbit working time of the orbiter, the temperature range of the thermal cycle experiment is set to be -150°C to 150°C, and the heating rate and cooling rate are both 1.5°C/min;
步骤二、根据实验要求，每次热循环后均取出实验样品，并对取出的实验样品进行热膨胀系数测试，分别计算各组热循环试验的相同热循环次数对应的热膨胀系数的平均值。为了保证测试过程中温度均匀以及防止氧化，测试时采用氩气保护，流量为50ml/min，根据0次、50次、100次和200次热循环对应的热膨胀系数的平均值，绘制出热循环试验的热膨胀系数随着热循环次数的变化规律，如图7所示。Step 2: According to the experimental requirements, the experimental samples are taken out after each thermal cycle, and the thermal expansion coefficient test is carried out on the taken out experimental samples, and the average value of the thermal expansion coefficient corresponding to the same thermal cycle times of each group of thermal cycle tests is calculated respectively. In order to ensure uniform temperature and prevent oxidation during the test, argon protection was used during the test, and the flow rate was 50ml/min. The thermal cycle was drawn according to the average value of the thermal expansion coefficient corresponding to 0, 50, 100 and 200 thermal cycles. The variation law of the thermal expansion coefficient of the test with the number of thermal cycles is shown in Figure 7.
步骤三、对步骤二中每次取出的实验样品进行自由基含量测试，测试时需要调整设备的频率，磁场和增益，如图5所示，为不同热循环次数条件下自由基特征峰的变化曲线图。Step 3: Test the free radical content of the experimental sample taken out in step 2. During the test, the frequency, magnetic field and gain of the equipment need to be adjusted. As shown in Figure 5, it is the change of the characteristic peak of free radicals under different thermal cycle times Graph.
根据0次、50次、100次和200次热循环对应的自由基含量的平均值，绘制出热循环试验的自由基含量随着热循环次数的变化规律，如图6所示。According to the average value of the free radical content corresponding to 0, 50, 100 and 200 thermal cycles, the variation law of the free radical content in the thermal cycle test with the number of thermal cycles was drawn, as shown in Figure 6.
步骤四、利用步骤二和步骤三得出的热循环试验的自由基含量随热循环次数变化的曲线和热膨胀系数随热循环次数变化的曲线；得出自由基含量随着热循环次数的变化规律与热膨胀系数随着热循环次数的变化规律一致。Step 4: Use the curve of the free radical content of the thermal cycle test obtained in Steps 2 and 3 with the number of thermal cycles and the curve of the thermal expansion coefficient with the number of thermal cycles; obtain the change rule of the free radical content with the number of thermal cycles It is consistent with the variation law of thermal expansion coefficient with the number of thermal cycles.
实施例3Example 3
本发明的一种基于自由基含量预估热循环对聚合物基复合材料热膨胀系数影响的方法，按以下步骤进行：A method of the present invention based on the content of free radicals to estimate the influence of thermal cycle on the thermal expansion coefficient of polymer-based composite materials, is carried out according to the following steps:
步骤一、选用碳纤维氰酸酯树脂复合材料作为实验样品，实验样品的尺寸为：长度25mm，宽度5mm，厚度2mm；在真空度小于1Pa的条件下，对选用的实验样品进行热循环实验，根据航天器在轨的任务期限要求和在轨的工作时间，设定热循环实验的温度范围为-150℃～150℃，升温速率和降温速率均为2.5℃/min；Step 1. Select the carbon fiber cyanate ester resin composite material as the experimental sample. The size of the experimental sample is: length 25mm, width 5mm, thickness 2mm; under the condition that the vacuum degree is less than 1Pa, the selected experimental sample is subjected to a thermal cycle test, according to For the spacecraft's on-orbit mission period and on-orbit working time, the temperature range of the thermal cycle experiment is set to be -150°C to 150°C, and the heating rate and cooling rate are both 2.5°C/min;
步骤二、根据实验要求，每次热循环后均取出实验样品，并对取出的实验样品进行热膨胀系数测试，分别计算各组热循环试验的相同热循环次数对应的热膨胀系数的平均值。为了保证测试过程中温度均匀以及防止氧化，测试时采用氩气保护，流量为50ml/min，根据0次、50次、100次、200次和2000次热循环对应的热膨胀系数的平均值，绘制出热循环试验的热膨胀系数随着热循环次数的变化规律，如图10所示。Step 2: According to the experimental requirements, the experimental samples are taken out after each thermal cycle, and the thermal expansion coefficient test is carried out on the taken out experimental samples, and the average value of the thermal expansion coefficient corresponding to the same thermal cycle times of each group of thermal cycle tests is calculated respectively. In order to ensure uniform temperature and prevent oxidation during the test, argon protection was used during the test, and the flow rate was 50ml/min. According to the average value of the thermal expansion coefficient corresponding to 0, 50, 100, 200 and 2000 thermal cycles, draw The variation law of the thermal expansion coefficient of the heat cycle test with the number of thermal cycles is shown in Figure 10.
步骤三、对步骤二中每次取出的实验样品进行自由基含量测试，测试时需要调整设备的频率，磁场和增益，如图8所示，为不同热循环次数条件下自由基特征峰的变化曲线图。Step 3: Test the free radical content of the experimental sample taken out in step 2. During the test, the frequency, magnetic field and gain of the equipment need to be adjusted. As shown in Figure 8, it is the change of the free radical characteristic peak under different thermal cycle times Graph.
根据0次、50次、100次、200次和2000次热循环对应的自由基含量的平均值，绘制出热循环试验的自由基含量随着热循环次数的变化规律，如图9所示。According to the average value of the free radical content corresponding to 0, 50, 100, 200 and 2000 thermal cycles, the variation law of the free radical content in the thermal cycling test with the number of thermal cycles was drawn, as shown in Figure 9.
步骤四、利用步骤二和步骤三得出的热循环试验的自由基含量随热循环次数变化的曲线和热膨胀系数随热循环次数变化的曲线；得出自由基含量随着热循环次数的变化规律与热膨胀系数随着热循环次数的变化规律一致。Step 4: Use the curve of the free radical content of the thermal cycle test obtained in Steps 2 and 3 with the number of thermal cycles and the curve of the thermal expansion coefficient with the number of thermal cycles; obtain the change rule of the free radical content with the number of thermal cycles It is consistent with the variation law of thermal expansion coefficient with the number of thermal cycles.
实施例4Example 4
本发明的一种基于自由基含量预估热循环对聚合物基复合材料热膨胀系数影响的方法，按以下步骤进行：A method of the present invention based on the content of free radicals to estimate the influence of thermal cycle on the thermal expansion coefficient of polymer-based composite materials, is carried out according to the following steps:
步骤一、选用碳纤维环氧树脂复合材料作为实验样品，实验样品的尺寸为：长度25mm，宽度5mm，厚度2mm；在真空度小于1Pa的条件下，对选用的实验样品进行热循环实验，根据航天器在轨的任务期限要求和在轨的工作时间，设定热循环实验的温度范围为-150℃～150℃，升温速率和降温速率均为2.5℃/min；Step 1. Select carbon fiber epoxy resin composite material as the experimental sample. The size of the experimental sample is: length 25mm, width 5mm, thickness 2mm; under the condition that the vacuum degree is less than 1Pa, the thermal cycle experiment is carried out on the selected experimental sample. According to aerospace According to the mission period requirements and on-orbit working time of the orbiter, the temperature range of the thermal cycle experiment is set to -150℃～150℃, and the heating rate and cooling rate are both 2.5℃/min;
步骤二、根据实验要求，每次热循环后均取出实验样品，并对取出的实验样品进行热膨胀系数测试，分别计算各组热循环试验的相同热循环次数对应的热膨胀系数的平均值。为了保证测试过程中温度均匀以及防止氧化，测试时采用氩气保护，流量为50ml/min，根据0次、50次、100次、200次和2000次热循环对应的热膨胀系数的平均值，绘制出热循环试验的热膨胀系数随着热循环次数的变化规律，如图13所示。Step 2: According to the experimental requirements, the experimental samples are taken out after each thermal cycle, and the thermal expansion coefficient test is carried out on the taken out experimental samples, and the average value of the thermal expansion coefficient corresponding to the same thermal cycle times of each group of thermal cycle tests is calculated respectively. In order to ensure uniform temperature and prevent oxidation during the test, argon protection was used during the test, and the flow rate was 50ml/min. According to the average value of the thermal expansion coefficient corresponding to 0, 50, 100, 200 and 2000 thermal cycles, draw The variation law of the thermal expansion coefficient of the heat cycle test with the number of thermal cycles is shown in Figure 13.
步骤三、对步骤二中每次取出的实验样品进行自由基含量测试，测试时需要调整设备的频率，磁场和增益，如图11所示，为不同热循环次数条件下自由基特征峰的变化曲线图。Step 3: Test the free radical content of the experimental sample taken out in step 2. During the test, the frequency, magnetic field and gain of the equipment need to be adjusted. As shown in Figure 11, it is the change of the free radical characteristic peak under different thermal cycle times Graph.
根据0次、50次、100次、200次和2000次热循环对应的自由基含量的平均值，绘制出热循环试验的自由基含量随着热循环次数的变化规律，如图12所示。According to the average value of the free radical content corresponding to 0, 50, 100, 200 and 2000 thermal cycles, the variation law of the free radical content in the thermal cycling test with the number of thermal cycles was drawn, as shown in Figure 12.
步骤四、利用步骤二和步骤三得出的热循环试验的自由基含量随热循环次数变化的曲线和热膨胀系数随热循环次数变化的曲线；得出自由基含量随着热循环次数的变化规律与热膨胀系数随着热循环次数的变化规律一致。Step 4: Use the curve of the free radical content of the thermal cycle test obtained in Steps 2 and 3 with the number of thermal cycles and the curve of the thermal expansion coefficient with the number of thermal cycles; obtain the change rule of the free radical content with the number of thermal cycles It is consistent with the variation law of thermal expansion coefficient with the number of thermal cycles.
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