CN-116773508-B - Method for measuring microscopic information of polymer-based nano noble metal composite material interface

CN116773508BCN 116773508 BCN116773508 BCN 116773508BCN-116773508-B

Abstract

The invention belongs to the technical field of nanocomposite interface performance measurement, and provides a method for measuring microscopic information of a polymer-based nano noble metal composite interface. The method comprises the following steps of S1, collecting an interface Raman signal generated by plasmon resonance of a polymer-based nano noble metal composite material by a double-beam Raman system, S2, collecting an intrinsic Raman signal of a polymer matrix by the double-beam Raman system, S3, collecting a pure polymer Raman signal of the same polymer material which does not contain nano noble metal by the double-beam Raman system, and S4, carrying out contrast analysis on the interface Raman signal, the intrinsic Raman signal and the pure polymer Raman signal to obtain interface microscopic information. By the method provided by the invention, the obtained interface Raman signal and the intrinsic Raman signal are combined accurately, and the interface information of the polymer/nano noble metal composite material is obtained in a lossless manner.

Inventors

ZHOU BINBIN
LIU YUAN
ZENG XIAOLIANG
LI ZHE
YU ZHENWEI
LIU XIAOWEI
HAN MENG
SUN RONG

Assignees

深圳先进电子材料国际创新研究院
中国科学院深圳先进技术研究院

Dates

Publication Date: 20260505
Application Date: 20230620

Claims (8)

1. A method of measuring interfacial microscopic information of a polymer-based nano-noble metal composite, the polymer-based nano-noble metal composite comprising a polymer substrate and a nano-noble metal filler, comprising the steps of: S1, a double-beam Raman system excites plasmon resonance of the polymer-based nano noble metal composite material by utilizing laser with a first wavelength to obtain Raman signals of an interface and a polymer body; s2, the dual-beam Raman system collects intrinsic Raman signals of the polymer matrix by using second-wavelength laser; S3, the dual-beam Raman system collects pure polymer Raman signals of the same polymer material which does not contain nano noble metals by utilizing the first wavelength laser and the second wavelength laser; and S4, carrying out comparative analysis on the interface Raman signal acquired in the step S1, the intrinsic Raman signal acquired in the step S2 and the pure polymer Raman signal acquired in the step S3 to obtain interface microscopic information.
2. The method of measuring interfacial microscopic information of a polymer-based nano-noble metal composite material according to claim 1, wherein the interfacial microscopic information includes vibration information of molecular groups, microcell stress information, conformation information of molecules, and molecular aggregation state information.
3. The method for measuring interfacial microscopic information of polymer-based nano-noble metal composite material according to claim 1, wherein, The interface Raman signal in the S1 comprises first Raman characteristic peak information and first fluorescence background information, wherein the first Raman characteristic peak information comprises the number, the position, the width, the intensity, the area and the relative intensity of the first Raman characteristic peaks; s2, the intrinsic Raman signal comprises second Raman characteristic peak information and second fluorescence background information, wherein the second Raman characteristic peak information comprises the number, the position, the width, the intensity, the area and the relative intensity of second Raman characteristic peaks; the comparative analysis in S4 includes comparative analysis of the first raman feature peak information, the second raman feature peak information, the first fluorescent background information, and the second fluorescent background information.
4. The method of measuring microscopic information of a polymer-based nano-noble metal composite interface of claim 1, wherein the power of the first wavelength laser and the second wavelength laser is between 1 mW and 100 mW.
5. The method of measuring interfacial microscopic information of a polymer-based nano-noble metal composite material according to claim 1, wherein the integration time of the dual beam raman system is between 1s and 1000 s.
6. The method of measuring microscopic information of a polymer-based nano-noble metal composite interface of claim 1, wherein the first wavelength laser and the second wavelength laser have wavelengths selected from any two of 266nm, 325nm, 514nm, 532nm, 633nm, 785nm, 830nm, and 1064 nm.
7. The method of measuring interfacial microscopic information of a polymer-based nano-noble metal composite material according to claim 1, wherein the polymer substrate is selected from one or more of epoxy, polyimide, and silicone.
8. The method of measuring interfacial microscopic information of a polymer-based nano-noble metal composite material according to claim 1, wherein the nano-noble metal filler is selected from one or more of gold, silver, and copper.

Description

Method for measuring microscopic information of polymer-based nano noble metal composite material interface Technical Field The invention belongs to the technical field of nanocomposite interface performance measurement, and particularly relates to a method for measuring microscopic information of a polymer-based nano noble metal composite interface. Background The polymer/nano noble metal composite material composed of the polymer matrix and the nano filler is an advanced packaging material playing a key role in the integrated circuit industry, and can be used as wafer-level epoxy plastic packaging material, chip-level substrate filling glue, thermal interface material and the like [1] required by electronic packaging. However, the high temperature environment created when the electronic device is in operation tends to accelerate the aging of the polymer/nano noble metal composite, resulting in reduced performance and reduced lifetime [2] of the electronic device. The method has important significance for researching the aging mechanism of the polymer/nano noble metal composite material, can timely replace the material with the performance no longer reaching the standard by monitoring the aging process and the residual service life of the polymer/nano noble metal composite material in real time, ensures the high-efficiency and safe operation of electronic devices, and can provide theoretical guidance for researching and developing the polymer/nano noble metal composite material with more excellent performance. At present, the research on the aging mechanism of the polymer/nano noble metal composite material is usually a characterization method of directly moving the polymer, and the key role of the interface between the nano filler and the polymer in the composite material is often ignored. The microscopic nature of the interface is affected not only by the chemical modification of the nanofiller surface, but also by the polymer type and microphase morphology [3,4], which can result in a molecular chain at the interface that has a microscopic nature that is very different [5,6] from the polymer matrix. More critical is that the microscopic state of the molecules at the interface greatly affects the properties [7] of the polymer/nano-noble metal composite through the large specific surface area and high surface activity of the nanofiller. Therefore, researching the aging mechanism of the interface in the polymer/nano noble metal composite material has a key effect on understanding the polymer/nano noble metal composite material and regulating the performance of the polymer/nano noble metal composite material. However, the results of studying the interfacial microscopic information acquisition of the polymer nanocomposite using conventional characterization means such as Scanning Electron Microscopy (SEM), transmission Electron Microscopy (TEM), X-ray photoelectron spectroscopy (XPS) or X-ray diffraction (XRD) are not accurate. These methods all require the destruction of the polymer nanocomposite exposing the interface, which can destroy the original structure and loss of information. The biggest defect in the prior art is that accurate microscopic information of a polymer/nano noble metal composite interface cannot be obtained. Reference is made to: [1] liu Peidong, hu Xiaodan, song Shihui, et al, research progress on polymer-based electronic packaging materials [ J ]. Engineering plastics applications, 2022,50 (07): 160-167. [2]Low,Z.X.,Budd P.M.,Mckeown N.B.,et al.Gas permeation properties,physical aging,and its mitigation in high free volume glassy polymers[J].Chem.Rev.,2018,118(12):5871-5911. [3]Gao,K.,Wan H.X.,Tsen E.J.L.,et al.Unveiling the mechanism of the location of the grafted nanoparticles in a lamellar-forming block copolymer[J].Langmuir,2020,36(1):194-203. [4]Gao,K.,Zhao H.H.,Wang Y.C.,et al.Heterogeneous dynamics of polymer melts exerted by chain loops anchored on the substrate:Insights from molecular dynamics simulation[J].Langmuir,2021,37(42):12290-12303. [5]Zhao,H.H.,Wei X.F.,Fang Y.,et al.Molecular dynamics simulation of the structural,mechanical,and reprocessing properties of vitrimers based on a dynamic covalent polymer network[J].Macromolecules,2022,55(4):1091-1103. [6]Chang,Z.C.,Wang Y.F.,Zhang Z.Y.,et al.Creep behavior of polymer nanocomposites:Insights from molecular dynamics simulation[J].Polymer,2021,228. [7]Idumah,C.I.,Obele C.M.Understanding interfacial influence on properties of polymer nanocomposites[J].Surf.Interfaces,2021,22. Disclosure of Invention In order to solve the problem that accurate microscopic information of a polymer/nano noble metal composite material interface cannot be obtained, the invention provides a method for measuring microscopic information of a polymer-based nano noble metal composite material interface, wherein the polymer-based nano noble metal composite material comprises a polymer substrate and nano noble metal filler. The method for measuring micr