發(fā)布時(shí)間：2018-01-24 08:43

  本文關(guān)鍵詞： 聚合物基復(fù)合材料 納米壓痕技術(shù) 微結(jié)構(gòu) 粘彈性 力學(xué)性能　出處：《揚(yáng)州大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：聚合物基復(fù)合材料由于具有比強(qiáng)度高、比模量大、耐疲勞、耐腐蝕等優(yōu)良的物理化學(xué)特性以及多功能性、結(jié)構(gòu)易設(shè)計(jì)、易加工等優(yōu)點(diǎn),被廣泛應(yīng)用于各個(gè)領(lǐng)域。為了滿足各個(gè)領(lǐng)域?qū)Σ牧显絹碓礁叩男阅芎徒Y(jié)構(gòu)的要求,從微觀上設(shè)計(jì)、表征材料的結(jié)構(gòu)和性能顯得尤為重要。納米壓痕技術(shù)是一種測試材料微尺度力學(xué)性能的實(shí)驗(yàn)方法,該方法通過記錄壓痕過程中的載荷和深度的變化關(guān)系獲得材料局部力學(xué)性能,可以實(shí)現(xiàn)對復(fù)合材料微結(jié)構(gòu)的表征。近年來雖然納米壓入技術(shù)在實(shí)驗(yàn)方法,實(shí)驗(yàn)原理及儀器分辨率等方面有了明顯的提高,但是對于高分子聚合物材料,尤其是粘彈性材料的微區(qū)力學(xué)性能的測試與應(yīng)用仍然存在很多問題。本文圍繞納米壓痕技術(shù)在橡塑材料中的應(yīng)用進(jìn)行了相關(guān)研究。復(fù)合材料的整體力學(xué)性能與組成相及界面的力學(xué)性能密切相關(guān),本文利用納米壓痕技術(shù)對納米顆粒增強(qiáng)的塑料、顆粒增強(qiáng)橡膠復(fù)合材料和并用膠各組成相及其界面進(jìn)行細(xì)觀力學(xué)性能表征,通過繪制同力學(xué)性能相對應(yīng)的三維形貌圖來建立復(fù)合材料微結(jié)構(gòu)同宏觀性能之間的關(guān)系。另外粘彈性會影響納米壓痕力學(xué)性能的測試結(jié)果,本文通過改變壓痕實(shí)驗(yàn)中的測試條件,從微尺度研究了材料的粘彈性。具體的研究工作如下:(1)采用準(zhǔn)靜態(tài)和動(dòng)態(tài)壓痕技術(shù)研究了羥基磷灰石/聚乳酸(HA/PLA)復(fù)合材料在微尺度的表面力學(xué)性能。通過改變保載時(shí)間、卸載時(shí)間討論了粘彈性對樣品準(zhǔn)靜態(tài)力學(xué)性能的影響;在動(dòng)態(tài)模式下探究了材料的動(dòng)態(tài)力學(xué)性能;通過蠕變行為和劃痕測試研究了復(fù)合材料的尺寸穩(wěn)定性。結(jié)果表明準(zhǔn)靜態(tài)模式下只有當(dāng)蠕變不充分時(shí),加載條件會影響模量和硬度的測試結(jié)果;動(dòng)態(tài)模式下存儲模量和硬度隨著壓入深度的增加而減小。HA/PLA復(fù)合物的微區(qū)硬度曲線顯示在相同載荷下,局部壓痕塑性變形較小,表明HA提高了 PLA的力學(xué)性能。(2)利用納米壓痕技術(shù)表征鈦酸銅鈣/硅橡膠(CCTO/PDMS)復(fù)合材料的微結(jié)構(gòu)信息,主要工作集中在利用超低載荷的壓痕條件繪制同力學(xué)性能相對應(yīng)的三維相貌圖,從而反映微結(jié)構(gòu)同宏觀性能之間的關(guān)系,并分析不同粒徑的CCTO對基體增強(qiáng)效果產(chǎn)生差異的原因。通過比較不同載荷繪制得到的模量圖,得出5μN(yùn)為最佳載荷。通過比較不同顆粒周圍微區(qū)的模量變化曲線發(fā)現(xiàn)CCTO粒徑小于1μm時(shí),隨著粒徑的減小,基體微區(qū)模量增大,界面過渡區(qū)范圍擴(kuò)大,表現(xiàn)出模量均化現(xiàn)象,但粒徑降低為300nm時(shí),微區(qū)模量不再增加,表明顆粒增強(qiáng)效果與顆粒粒徑有關(guān)。(3)利用納米壓痕技術(shù)對膠粉并用膠進(jìn)行準(zhǔn)靜態(tài)和動(dòng)態(tài)納米壓痕實(shí)驗(yàn),通過改變準(zhǔn)靜態(tài)實(shí)驗(yàn)中的加載、保載、卸載時(shí)間,研究了時(shí)間速率對準(zhǔn)靜態(tài)力學(xué)性能的影響;在動(dòng)態(tài)模式下探究了測試頻率,動(dòng)態(tài)載荷對動(dòng)態(tài)力學(xué)性能的影響。綜合考慮實(shí)驗(yàn)結(jié)果采用加載和卸載時(shí)間5s,保載20s作為準(zhǔn)靜態(tài)模式下的理想測試條件。動(dòng)態(tài)壓痕實(shí)驗(yàn)結(jié)果表明存儲模量依賴于載荷的頻率,膠粉含量越多,對測試頻率的依賴性越明顯;損耗因子隨著頻率的增加先增大后減小;相同頻率下動(dòng)態(tài)力越大,損耗角越大。通過測試不同膠粉含量的并用膠的微區(qū)力學(xué)性能發(fā)現(xiàn)隨著膠粉含量的增加,微區(qū)內(nèi)部膠粉分布密集,由于硫化不均形成的具有交聯(lián)梯度的界面越多,材料在宏觀力學(xué)性能上表現(xiàn)為拉伸強(qiáng)度隨著膠粉含量的增多單調(diào)遞減。
[Abstract]:Polymer composites due to their high specific strength, high specific modulus, fatigue resistance, corrosion resistance and other excellent physical and chemical properties and functional structure, easy to design, easy processing and other advantages, is widely used in various fields. In order to meet the performance and structure of the various fields of higher material and design requirements, from the micro structure, and material characterization is particularly important. The nano indentation technique is an experimental method to test the mechanical properties of micro scale materials, the method of obtaining local mechanical properties of materials through the relationship between the changes of load and indentation depth recording process, can realize the characterization of microstructure of composite materials. In recent years, although the nanoindentation the technology in the aspects of experimental methods, experimental principle and instrument resolution has been significantly improved, but for polymer materials, especially the micro mechanics of viscoelastic materials The test and application can still exist many problems. This paper focuses on the application of nano indentation technology in rubber materials in composite materials was studied. The mechanical properties and phase composition and is closely related to the mechanical properties of the interface, the enhancement of the nano particle by using the nano indentation technique of plastic particle reinforced rubber composites and blends each constituent phase and interface micromechanical characterization, to establish the relationship between micro structure and macro properties of composite materials by 3D drawing with the mechanical properties of the corresponding test results. Also will affect the viscoelastic properties of nano indentation, by changing the test conditions in indentation test, from the micro scale study the viscoelastic material. The specific studies are as follows: (1) the study of hydroxyapatite / poly lactic acid dynamic and quasi-static indentation technique (HA/PLA) composite The surface mechanical properties of materials in micro scale. By changing the holding time, the unloading time discusses the influence of viscoelastic quasi static mechanical properties of the samples; in the dynamic mode of dynamic mechanical properties of materials; the creep behavior and scratch test on the dimensional stability of the composites. The results show that the quasi static mode only when creep is not sufficient, the loading conditions will affect the test results of modulus and hardness; micro hardness curve of storage modulus and hardness under dynamic mode with increasing indentation depth and the decrease of the.HA/PLA complexes show under the same load, the local indentation plastic deformation is small, show that the HA can improve the mechanical properties of PLA (2). Using nanoindentation characterization of calcium copper titanate / silicone rubber (CCTO/PDMS) microstructure information of composite materials, mainly concentrated in the work of drawing Tongli indentation conditions by using ultra low load performance The corresponding three-dimensional appearance map, which reflects the relationship between micro structure and macro property, and analysis of different size CCTO the reasons for the differences of the matrix enhancement effect. By comparing the different load modulus by drawing, the 5 N is the best load. By comparing the different modulus curves of particles around the micro area CCTO found that the diameter of less than 1 m, with the decrease of particle size, matrix micro area modulus increase, transition zone of interface expansion, showing modulus phenomenon, but the particle size is reduced to 300nm, micro area modulus is not increased, indicating that the particles and enhancement effect of particle size of powder (3). And with a rubber quasi-static and dynamic nanoindentation experiments using nanoindentation technique, by changing the quasi-static experiments of loading, loading, unloading time, effect of time rate on static mechanical properties; in the dynamic mode of measurement Test frequency, dynamic load influence on dynamic mechanical properties. Considering the experimental results by loading and unloading time 5S, holding 20s as an ideal test conditions in quasi-static mode. Dynamic indentation experimental results show that the storage modulus depends on the load frequency, powder content more, the test frequency dependence is more obvious; loss factor with the increase of frequency increases first and then decreases; the same frequency under the dynamic force the greater the loss angle is greater. By testing different rubber content and mechanical properties of micro zones with glue with increasing rubber content, the micro area of powder distribution intensive, due to uneven sulfide formation interface more with cross-linked gradient. The material in the mechanical properties as tensile strength with the rubber content increased monotonically decreasing.

【學(xué)位授予單位】：揚(yáng)州大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TB324

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