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A preparation method and measurement method of a pearlescent pigment cross-section sample for scanning electron microscope determination

An electron microscope and pearlescent pigment technology, which is applied in the field of pearlescent pigment materials, can solve the problems of affecting measurement, affecting authenticity, and difficulty in film thickness measurement, achieving the effect of improving reliability and simple and convenient operation

Active Publication Date: 2021-08-06
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the microscopic analysis of pearlescent pigments is in the grinding and grading of mica, the size and distribution of mica flakes are roughly analyzed, and the surface morphology, cracks, pores and other defects of the pigment are observed with the help of a scanning electron microscope. For the observation of film thickness, its natural cross-section is usually selected, but because the "core" layer of pearlescent pigments is a large-diameter-thick-ratio, flake-shaped material, this results in most of the samples lying flat, and only the coating can be roughly observed. The number of layers cannot accurately measure the film thickness. Even if the film thickness data is obtained, there will be a large deviation due to the influence of the inclination angle; it is even more difficult to measure the film thickness at the nanometer level, so the cross-sectional sample preparation technology of pearlescent pigments is very important. important
At present, the commonly used cross-section sample preparation method is mainly the mechanical polishing method. The mechanical polishing method is used for pearlescent pigments. First, the powder material needs to be fixed with resin, and the powder particles are dispersed in the non-conductive resin. When observing with a microscope, image drift and even charging phenomenon will also occur. On the one hand, it will affect the measurement of the nanoscale microstructure inside the powder, and on the other hand, it will also make the analysis of nanoscale components more difficult.
Secondly, since pearlescent pigments belong to the compound of metal and inorganic, dense and loose structure, due to the differences in rigidity and brittleness of each component unit, mechanical polishing will lead to the destruction of the complex structure, which is likely to cause gaps between the film layers, affecting The authenticity of scanning electron microscope observation; and mechanical polishing will produce a lot of scratches, resulting in far insufficient accuracy for nanoscale film thickness measurement

Method used

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  • A preparation method and measurement method of a pearlescent pigment cross-section sample for scanning electron microscope determination
  • A preparation method and measurement method of a pearlescent pigment cross-section sample for scanning electron microscope determination
  • A preparation method and measurement method of a pearlescent pigment cross-section sample for scanning electron microscope determination

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Experimental program
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Effect test

Embodiment 1

[0064] Prepare the mica powder into a 10% suspended aqueous solution, adjust the pH to 2.0 with concentrated hydrochloric acid, heat and stir at 80°C, add 2mol / LTiCl4 aqueous solution to the suspension dropwise, and add NaOH solution dropwise at the same time to stabilize the pH value at 2, after 15 minutes Stop adding the TiCl4 aqueous solution, and the pH value of the reaction system rises to 8.5; slowly add a certain amount of tetraethyl orthosilicate solution to the reaction system dropwise, and keep the pH of the reaction solution stable at 8.5±0.2. The pH of the solution was adjusted to 2.0, and TiCl was added dropwise to the reaction system again 4 Aqueous solution, stop adding after 10 minutes, settle, filter with suction, wash with water, and dry to obtain mica titanium pearlescent pigment.

Embodiment 2

[0066] First, the pearlescent pigment is fixed on the surface of a silicon wafer (0.2mm) by the above method, and the initial sample with the pearlescent pigment coating layer fixed is obtained after drying. The mass ratio of the water-based liquid carbon conductive adhesive to the pearlescent pigment is 1:5 , the thickness of the fixed pearlescent pigment is 1mm. First load the sample stage with the initial sample into the argon ion beam polisher, and make the side of the silicon wafer not coated with pearlescent pigments close to the baffle, so that the ion beam first breaks down the silicon wafer, and then It is polished with pearlescent pigments. Among them, the parameters of ion beam section polishing include: acceleration voltage: 5kV, current: 2mA, polishing time: 4h. Secondly, use a scanning electron microscope to observe the pearlescent pigment section sample after ion beam section polishing, select a magnification of 40,000 times, voltage: 5kV, current: 25pA, to obt...

Embodiment 3

[0068] First, the pearlescent pigment is fixed on the surface of a silicon wafer (0.2mm) by the above method, and the initial sample with the pearlescent pigment coating layer fixed is obtained after drying. The mass ratio of the water-based liquid carbon conductive adhesive to the pearlescent pigment is 1:5 , the thickness of the fixed pearlescent pigment is 1mm. First load the sample stage with the initial sample into the argon ion beam polisher, and make the side of the silicon wafer not coated with pearlescent pigments close to the baffle, so that the ion beam first breaks down the silicon wafer, and then It is polished with pearlescent pigments. Among them, the parameters of ion beam section polishing include: acceleration voltage: 5kV, current: 2mA, polishing time: 4h. Secondly, select one of the pearlescent pigment cross-sections and select a magnification of 50,000 times, voltage: 5kV, current: 25pA, to obtain a clear secondary electron image, see the attached figur...

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Abstract

The invention provides a method for preparing and measuring a pearlescent pigment section sample for scanning electron microscope measurement. The preparation method includes: mixing liquid carbon conductive adhesive and pearlescent pigment and coating it on one side of a silicon chip, drying Obtain an initial sample fixed with a pearlescent pigment coating layer, the pearlescent pigment is coated with at least one continuous film layer and the thickness of the film layer is more than 2 nm; the obtained initial sample is subjected to ion beam cross-sectional polishing to obtain a cross-sectional sample of the pearlescent pigment , The parameters of the ion beam section polishing include: the ion beam accelerating voltage is 3-7 kV; the sample polishing time can be 120-480 minutes; the current is 1.5-3mA.

Description

technical field [0001] The invention relates to a method for preparing the section of a pearlescent pigment observed by a scanning electron microscope using an ion beam section polishing technology, and a method for analyzing and measuring the interface bonding, defects, number of layers, and thickness of a pearlescent pigment film layer using a scanning electron microscope, belonging to The field of pearlescent pigment materials. Background technique [0002] Pearlescent pigment is an inorganic functional material with excellent performance. It has a unique luster similar to pearls, which can endow objects with pearly luster and present a profound three-dimensional texture. The microstructure of pearlescent pigments is a flaky multi-layer core-shell structure, and its coloring principle comes from the synergistic effect of the high-reflection "core" layer material and the high-refraction "shell" layer on the reflection, refraction and interference of incident light. Common...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/2251G01N23/2202
CPCG01N23/2202G01N23/2251
Inventor 刘紫微王焱张积梅林初城华佳捷王墉哲姜彩芬曾毅
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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