石英纤维/聚酰亚胺复合材料的制备与性能

肖沅谕; 高龙飞; 陈博; 李松

doi:10.13801/j.cnki.fhclxb.20200215.001

石英纤维/聚酰亚胺复合材料的制备与性能

doi: 10.13801/j.cnki.fhclxb.20200215.001

北京玻钢院复合材料有限公司，北京 102101

详细信息

通讯作者:
李松，博士，教授级高工，研究方向为耐高温树脂基及陶瓷基透波复合材料　E-mail：lisong1996@126.com

中图分类号: TB332
计量
- 文章访问数: 1351
- HTML全文浏览量: 647
- PDF下载量: 115
- 被引次数: 0
出版历程
- 收稿日期: 2019-11-27
- 录用日期: 2020-01-02
- 网络出版日期: 2020-02-17
- 刊出日期: 2020-10-15

Preparation and performance of quartz fiber/polyimide composites

Beijing Composite Materials Co. Ltd., Beijing 102101, China

摘要

摘要: 采用DSC、TG、FTIR和流变仪对KH-370聚酰亚胺树脂的化学反应特性和流变性能进行了表征。以QWB200石英纤维为增强体，采用热压成型工艺制备了QWB200/KH-370复合材料。研究了加压温度、压力大小、固化温度等不同工艺参数对QWB200/KH-370复合材料力学性能的影响，在此基础上确定了复合材料的成型工艺制度。考察了QWB200/KH-370复合材料400℃高温下的力学强度及宽频范围内的介电性能。结果表明，制备QWB200/KH-370复合材料的最佳工艺参数为：加压温度290~310℃，压力范围3.0~4.0 MPa，固化温度380℃。所得QWB200/KH-370复合材料具有良好的力学性能，400℃下力学强度保持率高于58%，表现出良好的耐热性能；而且在1~18 GHz的宽频范围内具有稳定的介电常数和介电损耗。
- 聚酰亚胺 /
- 热压成型 /
- 介电性能 /
- 力学性能 /
- 耐热性能
Abstract: The chemical reaction characterization and rheological property of KH-370 polyimide resin were characterized by DSC, TG, FTIR and rheometer. The QWB200/KH-370 composite was prepared by hot pressing technology with QWB200 quartz fiber as reinforcement.The effects of different process parameters (pressing temperature, pressure, curing temperature) on the mechanical properties of QWB200/KH-370 composites were studied. On this basis, the molding process system of the composites was determined.The mechanical strength of the composite at 400℃ and the dielectric properties at broad frequency were also investigated. According to the results, the best process parameters for the preparation of QWB200/KH-370 composites are: pressing temperature of 290-310℃, pressure range of 3.0-4.0 MPa, curing temperature of 380℃. The prepared QWB200/KH-370 composites exhibit excellent mechanical properties at room temperature, and the retention rates of mechanical strength at 400℃ is above 58%, showing good heat resistance. The QWB200/KH-370 composites show stable dielectric constant and dielectric loss at broad frequency from 1 GHz to 18 GHz.
- polyimide resin /
- hot pressing process /
- dielectric properties /
- mechanical properties /
- heat-resistance properties

HTML全文

图 1 真空脱除溶剂后KH-370聚酰亚胺树脂粉末的DSC曲线(a)、TG及DTG曲线(b)

Figure 1. DSC(a), TG and DTG curves(b) of KH-370 polyimide resin powder after vacuum removal of solvent

下载: 全尺寸图片幻灯片

图 2 不同温度处理KH-370树脂的FTIR图谱

Figure 2. FTIR spectra of KH-370 resin treated at different temperatures

下载: 全尺寸图片幻灯片

图 3 KH-370树脂B阶段的黏温曲线

Figure 3. Viscosity temperature curve of KH-370 resin at stage B

下载: 全尺寸图片幻灯片

图 4 加压温度对QWB200石英纤维/KH-370复合材料力学性能的影响

Figure 4. Effect of pressing temperatures on mechanical properties of QWB200 quartz fiber/KH-370 composite

下载: 全尺寸图片幻灯片

图 5 加压大小对QWB200/KH-370复合材料力学性能的影响

Figure 5. Effect of pressure on mechanical properties of QWB/200/KH-370 composite

下载: 全尺寸图片幻灯片

图 6 固化温度对QWB200/KH-370复合材料力学性能的影响

Figure 6. Effect of curing temperatures on mechanical properties of QWB200/KH-370 composite

下载: 全尺寸图片幻灯片

图 7 QWB200/KH-370复合材料在不同频率的介电性能

Figure 7. Dielectric properties of QWB200/KH-370 composites at different frequencies

下载: 全尺寸图片幻灯片

表 1 QWB200/KH-370复合材料的高温力学性能

Table 1. High temperature mechanical properties of QWB200/KH-370 composite

Parameter	Tensile strength/MPa	Flexural strength/MPa	Interlaminate shear strength/MPa
Room temperature	650	634	51
400℃	442	371	31.1
High temperature retention/%	68.0	58.5	61.0

下载: 导出CSV

参考文献(28)

[1]	张朋, 杜家楠. RTM成型聚酰亚胺复合材料的热氧老化特性[J]. 宇航材料工艺, 2018(4):51-55. doi: 10.12044/j.issn.1007-2330.2018.04.009 ZHANG Peng, DU Jia'nan. Thermo-oxidative ageing properties of polyimide composites fabricated by RTM[J]. Aerospace Materials & Technology,2018(4):51-55(in Chinese). doi: 10.12044/j.issn.1007-2330.2018.04.009
[2]	杨家义, 杨博峰. 热固性聚酰亚胺树脂成型工艺研究进展[J]. 功能材料, 2018, 49(2):2054-2059. YANG Jiayi, YANG Bofeng. Reserch progress of moulding press for thermosetting polyimideresins[J]. Journal of Functional Materials,2018,49(2):2054-2059(in Chinese).
[3]	赵一兰, 胡程耀, 魏春, 等. 聚酰亚胺表面处理玻璃纤维/环氧树脂复合材料力学性能[J]. 复合材料学报, 2018, 35(7):1850-1856. ZHAO Yilan, HU Chengyao, WEI Chun, et al. Mechanical properties of polyimides of polyimide surface treated glass fiber/epoxy resin composites[J]. Acta Materiae Compo-sitae Sinica,2018,35(7):1850-1856(in Chinese).
[4]	李敏, 张佐光, 仲伟虹, 等. 聚酰亚胺树脂研究与应用进展[J]. 复合材料学报, 2000, 17(4):48-53. doi: 10.3321/j.issn:1000-3851.2000.04.010 LI Min, ZHANG Zuoguang, ZHONG Weihong, et al. Study and application development of polyimides[J]. Acta Materiae Compositae Sinica,2000,17(4):48-53(in Chinese). doi: 10.3321/j.issn:1000-3851.2000.04.010
[5]	HERGENROTHER P M. The use, design, synthesis, and properties of high performance/high temperature polymers: An overview[J]. High Performance Polymers,2003,15(1):3-45. doi: 10.1177/095400830301500101
[6]	MITTAL K L. Polyimides and other high temperature polymers[M]. The Netherlands: VSP/Brill, 2009: 19-31.
[7]	MEADOR M A. Recent advances in the development of processable high temperature polymers[J]. Annual Review of Materials Science,1998,28:599-630. doi: 10.1146/annurev.matsci.28.1.599
[8]	包建文, 陈祥宝. 发动机用耐高温聚酰亚胺树脂基复合材料的研究进展[J]. 航空材料学报, 2012, 32(6):1-12. doi: 10.3969/j.issn.1005-5053.2012.6.001 BAO Jiaowen, CHEN Xiangbao. Advance in high temperature polyimide resin matrix composites for aeroengine[J]. Journal of Aeronautical Materials,2012,32(6):1-12(in Chinese). doi: 10.3969/j.issn.1005-5053.2012.6.001
[9]	杨涛, 张朋, 董波涛. 热固性聚酰亚胺树脂基复合材料的增韧改性研究进展[J]. 航空制造技术, 2019, 62(10):66-72. YANG Tao, ZHANG Peng, DONG Botao. Advance in toughening methods of thermosetting polyimide resin matrix composites[J]. Aeronautical Manufacturing Technology,2019,62(10):66-72(in Chinese).
[10]	高艺航, 石玉红, 王鲲鹏, 等. 聚酰亚胺树脂基MT300/KH420复合材料高温力学性能(II)—弯曲性能[J]. 复合材料学报, 2016, 33(12):2699-2705. GAO Y H, SHI Y H, WANG K P, et al. High-temperature mechanical properties of polyimide resin matrix MT300/KH420 composites(II)—Flexural properties[J]. Acta Materiae Compositae Sinica,2016,33(12):2699-2705(in Chinese).
[11]	郝继璨, 鲁云华, 肖国勇, 等. 原位氨基化氧化石墨烯/聚酰亚胺复合材料的制备及性能[J]. 复合材料学报, 2018, 35(6):1377-1385. HAO J C, LU Y H, XIAO G Y, et al. Preparation and properties of in-situ aminated graphene oxide/polyimide composites[J]. Acta Materiae Compositae Sinica,2018,35(6):1377-1385(in Chinese).
[12]	王晓龙, 王李波, 宋艺赫, 等. Ti₃C₂T_x/聚酰亚胺复合材料的制备及性能[J]. 复合材料学报, 2019, 36(7):1575-1582. WANG Xiaolong, WANG Libo, SONG Yihe, et al. Preparation and performances of Ti₃C₂T_x/polyimide composites[J]. Acta Materiae Compositae Sinica,2019,36(7):1575-1582(in Chinese).
[13]	陈东, 居建国, 郝旭峰. 石英纤维/KH308复合材料的介电性能[J]. 复合材料学报, 2014, 31(3):563-568. CHEN Dong, JU Jianguo, HAO Xufeng. Dielectric properties of quartz fiber reinforced KH308 composites[J]. Acta Materiae Compositae Sinica,2014,31(3):563-568(in Chinese).
[14]	张雄, 王义, 程海峰. 石英纤维透波复合材料的研究进展[J]. 材料导报, 2012, 26(19):96-100. ZHANG Xiong, WANG Yi, CHENG Haifeng. Researchand and development of wave-transparent composites reinforced by silica fibers[J]. Materials Review,2012,26(19):96-100(in Chinese).
[15]	陈建升, 范琳. 短切石英纤维/聚酰亚胺复合材料的制备与性能[J]. 复合材料学报, 2006, 23(5):79-83. doi: 10.3321/j.issn:1000-3851.2006.05.015 CHEN Jiansheng, FAN Lin. Preparation and properties of chopped quartz fiber/PMR polyimide composites[J]. Acta Materiae Compositae Sinica,2006,23(5):79-83(in Chinese). doi: 10.3321/j.issn:1000-3851.2006.05.015
[16]	GAO S Q, WANG X C, HU A J, et al. Preparation and properties of PMR-II polyimide/chopped quartz fibre compo-sites[J]. High Performance Polymers,2000,12(3):405-417. doi: 10.1088/0954-0083/12/3/304
[17]	杨士勇, 范琳, 冀棉, 等. 耐高温聚酰亚胺材料研究进展[J]. 高分子通报, 2011(10):70-78. YANG Shiyong, FAN Lin, JI Mian, et al. Advances in high temperature polyimide materials[J]. Polymer Bulletin,2011(10):70-78(in Chinese).
[18]	张朋, 周立正, 包建文. 耐350℃RTM聚酰亚胺树脂及其复合材料性能[J]. 复合材料学报, 2014, 31(2):345-352. ZHANG Peng, ZHOU Lizheng, BAO Jianwen. Properties of 350℃ temperature-resistant RTM polyimide matrix resin and its composites[J]. Acta Materiae Compositae Sinica,2014,31(2):345-352(in Chinese).
[19]	王震, 益小苏, 丁孟贤. 含联苯结构的聚酰亚胺复合材料[J]. 复合材料学报, 2003, 20(3):27-30. doi: 10.3321/j.issn:1000-3851.2003.03.006 WANG Zhen, YI Xiaosu, DING Mengxian. Polyimide composite containing biphenyl structure[J]. Acta Materiae Compositae Sinica,2003,20(3):27-30(in Chinese). doi: 10.3321/j.issn:1000-3851.2003.03.006
[20]	全国纤维增强塑料标准化技术委员会. 纤维增强塑料拉伸性能试验方法: GB/T1447—2005[S]. 北京: 中国标准出版社, 2005. National Technical Committee on Fiber Reinforced Plastic of Standardization Administration of China. Fiber-reinforced plastics composites—Determination of tensile properties: GB/T1447—2005[S]. Beijing: Standards Press of China, 2005(in Chinese).
[21]	全国纤维增强塑料标准化技术委员会. 纤维增强塑料弯曲性能试验方法: GB/T1449—2005[S]. 北京: 中国标准出版社, 2005. National Technical Committee on Fiber Reinforced Plastic of Standardization Administration of China. Fiber-reinforced plastics composites—Determination of flexural properties: GB/T1449—2005[S]. Beijing: Standards Press of China, 2005(in Chinese).
[22]	全国纤维增强塑料标准化技术委员会. 纤维增强塑料层间剪切性能试验方法: GB/T1450.1—2005[S]. 北京: 中国标准出版社, 2005. National Technical Committee on Fiber Reinforced Plastic of Standardization Administration of China. Fiber-reinforced plastics composites—Determination of interlaminar shear strength properties: GB/T1450.1—2005[S]. Beijing: Standards Press of China, 2005(in Chinese).
[23]	全国纤维增强塑料标准化技术委员会. 纤维增强塑料层间剪切性能试验方法: GB/T9979—2005[S]. 北京: 中国标准出版社, 2005. National Technical Committee on Fiber Reinforced Plastic of Standardization Administration of China. Guide rule of test for mechanical properties of fiber-reinforced plastics at elevated and reduced temperatures: GB/T9979—2005[S]. Beijing: Standards Press of China, 2005(in Chinese).
[24]	丁孟贤. 聚酰亚胺-化学、结构与性能的关系及材料[M]. 北京: 科学出版社, 2006: 1-7. DING Mengxian. Polyimides: Chemistry, relationship between structure and properties and materials[M]. Beijing: Science Press, 2006: 1-7(in Chinese).
[25]	SMITH J J, CONNELL J W, HERGENROYHER P M, et al. High temperature transfer molding resins[C]//45th International SAMPE Symposium and Exhibition, 2000: 1584-1597.
[26]	DING M X. Isomeric polyimides[J]. Progress in Polymer Science,2007,32(6):623-668. doi: 10.1016/j.progpolymsci.2007.01.007
[27]	陈建升, 左红军, 范琳, 等. 耐高温聚酰亚胺材料研究进展[J]. 宇航材料工艺, 2006(2):7-12. doi: 10.3969/j.issn.1007-2330.2006.z1.002 CHEN Jiansheng, ZUO Hongjun, FAN Lin, et al. Development of high temperature polyimide[J]. Aerospace Materials & Technology,2006(2):7-12(in Chinese). doi: 10.3969/j.issn.1007-2330.2006.z1.002
[28]	姚逸伦, 张朋, 包建文, 等. 耐高温高韧性聚酰亚胺树脂分子量与性能关系[J]. 复合材料学报, 2016, 33(9):1973-1980. YAO Y L, ZHANG P, BAO J W, et al. Relation between mo molecular weight and properties of high temperature and high toughness polyimide resin[J]. Acta Materiae Compo-sitae Sinica,2016,33(9):1973-1980(in Chinese).