本文關(guān)鍵詞： Ag粒子 聚酰亞胺 復(fù)合泡沫 電磁屏蔽 熱穩(wěn)定性　出處：《哈爾濱理工大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：聚酰亞胺(PI)材料是一種具有優(yōu)異性能的聚合物材料,該種材料由于具有優(yōu)異的物理機(jī)械性能、化學(xué)性能以及耐高低溫性能,被廣泛應(yīng)用于航空航天領(lǐng)域、微電子領(lǐng)域和通訊等高技術(shù)領(lǐng)域。近年來,越來越多的研究者對(duì)PI材料進(jìn)行研究,對(duì)其研究方向正朝著高性能化、多功能化和低成本化發(fā)展。PI的耐高低溫性能和優(yōu)異的物理機(jī)械性能,為通過納米改性該P(yáng)I材料提供了重要的性能保證,也因此獲得了眾多研究者對(duì)該領(lǐng)域研究的青睞。本文以PI泡沫材料為基體,選擇三種不同特性的粒子(金屬Ag納米粒子、Fe_3O_4磁性粒子及羥基化石墨微片)為摻雜填料,獲得了 一系列摻雜填料含量不同的PI基復(fù)合泡沫。對(duì)這三種PI基復(fù)合泡沫材料進(jìn)行了結(jié)構(gòu)表征,分析不同摻雜填料及其摻雜含量對(duì)PI基復(fù)合泡沫的結(jié)構(gòu)及其性能的影響。測(cè)試實(shí)驗(yàn)結(jié)果表明:本實(shí)驗(yàn)采用直接離子交換自金屬化法所制備獲得的Ag納米是納米級(jí)的。Ag納米粒子在PI復(fù)合泡沫中存在輕微的團(tuán)聚現(xiàn)象。XRD分析表明,PI/Ag 泡沫的 XRD 曲線在 2θ 為 38.45°、44.1°、64.55°、77.6°處出現(xiàn)了特征衍射峰,分別對(duì)應(yīng)于銀粒子的(111)、(200)、(220)、(311)晶面,證實(shí)本實(shí)驗(yàn)中所制備的單質(zhì)Ag是面心立方晶系的,且曲線的衍射峰峰形尖銳,均無雜峰,說明單質(zhì)Ag的結(jié)晶性能良好。熱性能分析表明,Ag納米粒子的引入對(duì)PI基復(fù)合泡沫的初始熱分解溫度幾乎沒有影響。紅外測(cè)試結(jié)果表明Ag納米粒子的引入并沒有破壞PI基泡沫材料的化學(xué)結(jié)構(gòu)。SEM測(cè)試結(jié)果表明隨著前體溶液中初始含Ag量w(Ag)逐漸增加,PI/Ag復(fù)合泡沫中Ag納米粒子的空間分布密度明顯增大,Ag納米粒子的尺寸不斷減小。通過紫外測(cè)試可以知道隨著Ag納米粒子含量的增加,PI/Ag復(fù)合泡沫的反射率逐漸增加。并且反射率與Ag納米粒子含量之間有良好的線性關(guān)系,但Ag納米粒子含量增加到一定量后反射率與Ag納米粒子含量之間不再呈線性關(guān)系,PI/Ag復(fù)合泡沫的反射率隨Ag納米粒子含量的增加變化越來越小。當(dāng)以羥基化石墨微片為填料時(shí),掃描電鏡表明所制備的石墨微片直徑為微米級(jí)且能較好的分散在PI泡沫基體中。將石墨微片摻雜到PI泡沫基體中對(duì)石墨微片的結(jié)晶幾乎沒有影響。通過FT-IR分析測(cè)試可知,在PI/石墨微片復(fù)合泡沫中引入的石墨微片對(duì)PI泡沫化學(xué)結(jié)構(gòu)基本沒有影響。DSC測(cè)試結(jié)果顯示出PI/石墨微片復(fù)合泡沫具有比較高的玻璃化轉(zhuǎn)變溫度,能夠保證在較高溫度環(huán)境下材料的正常使用。從TGA分析測(cè)試可知,PI/石墨微片復(fù)合泡沫熱穩(wěn)定性與純PI泡沫相比有所提高,說明石墨微片在一定程度上能夠提高聚合物材料的熱穩(wěn)定性。通過SEM對(duì)PI/石墨微片復(fù)合泡沫材料的微觀泡孔結(jié)構(gòu)及其粒子分散狀態(tài)進(jìn)行分析,結(jié)果表明石墨微片與PI泡沫基體緊密結(jié)合且在PI泡沫中均勻分散。通過力學(xué)性能測(cè)試可以看出,在PI/石墨微片復(fù)合泡沫中引入石墨微片使得泡沫基體輕度變硬,同時(shí)柔韌性有所降低。當(dāng)選擇Fe_3O_4磁性粒子為填料時(shí),通過紅外光譜分析,純PI泡沫與不同F(xiàn)e_3O_4含量的PI/Fe_3O_4復(fù)合泡沫材料的化學(xué)結(jié)構(gòu)基本相同,Fe_3O_4的加入對(duì)PI泡沫基體的結(jié)構(gòu)并沒有明顯的影響。通過SEM測(cè)試得出,隨著Fe_3O_4磁性納米粒子含量的逐漸增加,Fe_3O_4磁性納米粒子粒徑逐漸減小,但當(dāng)Fe_3O_4納米粒子在PI基復(fù)合泡沫中達(dá)到10 wt%時(shí)會(huì)發(fā)生輕微的團(tuán)聚現(xiàn)象。通過XRD測(cè)試可知,不同F(xiàn)e_3O_4納米粒子摻雜量的PI/Fe_3O_4復(fù)合泡沫的結(jié)晶性能良好,而且均沒有雜峰。通過TG測(cè)試得出,不同F(xiàn)e_3O_4納米粒子摻雜量的PI/Fe_3O_4復(fù)合泡沫的分解溫度與PI泡沫材料的分解溫度相差較小,說明Fe_3O_4納米粒子對(duì)PI泡沫基體的熱穩(wěn)定性影響比較小。對(duì)PI/Fe_3O_4復(fù)合泡沫材料的力學(xué)性能測(cè)試,得出隨著Fe_3O_4磁性粒子含量的增加,壓縮強(qiáng)度逐漸增強(qiáng),泡沫材料抵抗變形的能力增大。綜上所述,當(dāng)Fe_3O_4磁性粒子的添加量達(dá)到13 wt%時(shí),能夠使PI/Fe_3O_4復(fù)合泡沫各性能指標(biāo)達(dá)到最優(yōu),最終制得兼具熱穩(wěn)定性,物理機(jī)械性及電磁屏蔽性的PI/Fe_3O_4復(fù)合泡沫材料。
[Abstract]:Polyimide (PI) material is a polymer material with excellent properties. The material has excellent physical and mechanical properties, chemical properties and high temperature properties, is widely used in the field of aerospace, microelectronics and communications and other high-tech fields. In recent years, more and more researchers to study PI materials. The research direction is towards high performance, multifunction and low cost development of.PI high temperature performance and excellent physical properties, provides important guarantee for the performance of the modified nano PI material, also won many researchers in this research field. This paper takes PI foam favored the matrix materials to choose three different characteristics of the particle (Ag nanoparticles, Fe_3O_4 magnetic particles and hydroxyl graphite microchip) as doping filler, obtained a series of PI doped with different filler content complex Synthetic foam. Of the three kinds of PI composite foams were characterized. The influence analysis of structures with different doping filler and the doping content of PI based composite foam and its performance. The experimental results show that this experiment adopts direct ion-exchange self metallization method for Ag nano preparation is the aggregation of.XRD minor the analysis indicated the presence of nano.Ag nanoparticles in the PI composite foam, PI/Ag foam XRD curve at 2 theta 38.45 degrees, 44.1 degrees, 64.55 degrees, 77.6 degrees at the characteristic diffraction peaks, corresponding to the silver particles (111), (200), (220), (311) crystal in this experiment, confirmed that the prepared Elemental Ag is face centered cubic structure, and the diffraction peaks of the curve are sharp, no miscellaneous peak, indicating the crystallization properties of elemental Ag. Analysis shows that the thermal properties of Ag nanoparticles on the introduction of the initial thermal decomposition temperature of PI composite foam hardly Influence. Infrared test results show that the introduction of nano Ag and.SEM chemical structure damage PI based foam material test results show that with the initial Ag content of W precursor solution (Ag) increased gradually, PI/Ag composite foams of Ag nanoparticles in the spatial distribution of the density increase obviously, Ag particle size decreases. By UV the test can know that with the increase of Ag nanoparticles content, the reflectivity of PI/Ag composite foams increased gradually. And there is a good linear relationship between the reflectance and the content of Ag nanoparticles, but Ag nanoparticles content is not a linear relationship between the amount of reflectivity and reflectivity of Ag nanoparticles content of PI/Ag composite foams with Ag nanoparticles with the increase of the content of change more and smaller. When the hydroxylated graphite sheet as filler, scanning electron microscopy indicated that the prepared graphite sheet and micron diameter Can be better dispersed in the PI matrix. The foam graphite Microflake doped into crystalline PI foam matrix of graphite micro sheet has little effect. Through the FT-IR analysis results, introduced in PI/ graphite MICROFLAKY foam in graphite sheet of PI foam chemical structure does not affect the basic results of.DSC test showed that PI/ graphite micro composite foam having a glass transition temperature is relatively high, can guarantee the normal use of materials in high temperature environment. The analysis test shows from TGA, PI/ graphite MICROFLAKY foam thermal stability was improved compared with that of pure PI foam, graphite sheet to a certain extent, can improve the thermal stability of polymer materials. Through the analysis of the micro pore structure of SEM PI/ graphite Microflake composites and the particle dispersion state, results show that the graphite sheet and PI foam matrix combination and in PI foam Dispersed. Through the test of mechanical property can be seen in the introduction of PI/ graphite graphite MICROFLAKY foam microchip makes the foam matrix mild harden, while the flexibility decreased. When choosing Fe_3O_4 magnetic particles as filler, through infrared spectrum analysis, the chemical structure of PI/Fe_3O_4 composite foam pure PI foam with different content of Fe_3O_4 basic the same, the addition of Fe_3O_4 on the structure of PI foam matrix has no obvious influence. With the SEM test, with the increasing content of Fe_3O_4 nanoparticles, Fe_3O_4 nanoparticles particle size gradually decreases, but when the Fe_3O_4 reached 10 wt% nanoparticles in PI based composite foam happens weak aggregation. By XRD test the crystallization properties of PI/Fe_3O_4 composite foams with different Fe_3O_4 nanoparticles doping amount is good, and no impurity peaks. With the TG test, not PI/Fe_3O_4 composite foam with Fe_3O_4 nanoparticles doped with PI decomposition temperature of the foam decomposition temperature difference is small, it shows that the thermal stability effect of Fe_3O_4 nanoparticles on PI foam matrix is relatively small. Test the mechanical properties of PI/Fe_3O_4 composite foam material, with the increase of Fe_3O_4 magnetic particle content, the compressive strength gradually increased, the foam resistance the ability of deformation increases. To sum up, when the adding amount of Fe_3O_4 magnetic particles reached 13 wt%, can make PI/Fe_3O_4 composite foam the performance index of optimal, finally prepared with thermal stability, PI/Fe_3O_4 composite foam material physical mechanical and electromagnetic shielding.

【學(xué)位授予單位】：哈爾濱理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TQ328;TB33

【參考文獻(xiàn)】

相關(guān)期刊論文 前7條

1 康思琦;尹庚明;余愛民;;銅系水性丙烯酸電磁屏蔽涂料的制備[J];五邑大學(xué)學(xué)報(bào)(自然科學(xué)版);2010年04期

2 馮猛;曾敏;張敬霖;張羊換;王新林;;炭黑填充丁苯/天然橡膠的電磁屏蔽性能[J];安全與電磁兼容;2010年03期

3 張洪艷;王海泉;;電場(chǎng)制備不飽和樹脂/石墨微片復(fù)合材料的研究[J];赤峰學(xué)院學(xué)報(bào)(自然科學(xué)版);2009年09期

4 王闖;李克智;李賀軍;郭領(lǐng)軍;;碳纖維增強(qiáng)水泥基復(fù)合材料的電磁屏蔽性能[J];精細(xì)化工;2008年06期

5 李正莉;王煊軍;劉祥萱;張有智;;高導(dǎo)電性銅基復(fù)合導(dǎo)電涂料的研制[J];材料保護(hù);2005年12期

6 周文君,駱超群;鍍銀銅粉導(dǎo)電涂料的研究[J];杭州師范學(xué)院學(xué)報(bào)(自然科學(xué)版);2005年04期

7 毛倩瑾,于彩霞,周美玲;Cu/Ag復(fù)合電磁屏蔽涂料的研究[J];涂料工業(yè);2004年04期

，

本文編號(hào)：1493597