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Preparation method of PVC paste resin scanning electron microscope sample

A scanning electron microscope and sample preparation technology, which is used in measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to obtain images of micro-nano particles with high dispersion of PVC paste resin, and achieve the effect of simple operation.

Pending Publication Date: 2022-01-18
SHANGHAI CHLOR ALKALI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In a word, it is impossible to obtain the image of highly dispersed micro-nano particles of PVC paste resin by conventional scanning electron microscope sample preparation method.

Method used

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  • Preparation method of PVC paste resin scanning electron microscope sample
  • Preparation method of PVC paste resin scanning electron microscope sample
  • Preparation method of PVC paste resin scanning electron microscope sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) In an ultrasonic bath, the dispersant is dissolved in deionized water to form a dispersant aqueous solution, and then the detected PVC paste resin powder is mixed with the dispersant aqueous solution to obtain an ultrasonic microsuspension, and then the suspension is Drop it on the carbon conductive tape on the sample stage of the scanning electron microscope, shake the sample stage gently, so that the liquid forms a thin liquid layer on the carbon conductive adhesive layer, and dry it at a temperature of 95 ° C for 30 minutes to obtain the sample precursor;

[0028] Described dispersant is polyethylene glycol, and the weight concentration of dispersant is 0.1%;

[0029] The mass ratio of the PVC paste resin powder to the dispersant aqueous solution is 1:500;

[0030] Ultrasonic dispersion for 5 minutes, the temperature rise does not exceed 35°C, and the suspension is allowed to stand for 5 minutes, and the upper and middle layers of the suspension are used;

[003...

Embodiment 2

[0035] (1) In an ultrasonic bath, the dispersant is dissolved in deionized water to form a dispersant aqueous solution, and then the detected PVC paste resin powder is mixed with the dispersant aqueous solution to obtain an ultrasonic microsuspension, and then the suspension is Drop it on the carbon conductive tape on the sample stage of the scanning electron microscope, shake the sample stage gently, so that the liquid forms a thin liquid layer on the carbon conductive adhesive layer, and dry it at a temperature of 120°C for 20 minutes to obtain the sample precursor;

[0036] Described dispersant is polyethylene glycol, and the weight concentration of dispersant is 0.3%;

[0037] The mass ratio of the PVC paste resin powder to the dispersant aqueous solution is 1:5000;

[0038] Ultrasonic disperse for 20 minutes, raise the temperature to 30°C, let the suspension stand for 30 minutes, and take the middle and upper layer suspension;

[0039] (2) The sample precursor was treate...

Embodiment 3

[0043] (1) In an ultrasonic bath, the dispersant is dissolved in deionized water to form a dispersant aqueous solution, and then the detected PVC paste resin powder is mixed with the dispersant aqueous solution to obtain an ultrasonic microsuspension, and then the suspension is Drop it on the carbon conductive tape on the sample stage of the scanning electron microscope, shake the sample stage gently, so that the liquid forms a thin liquid layer on the carbon conductive adhesive layer, and dry it at a temperature of 100 ° C for 25 minutes to obtain the sample precursor;

[0044] Described dispersant is polyethylene glycol and methoxypolyethylene glycol, and the weight concentration of dispersant is respectively 0.2% and 0.1%;

[0045] The mass ratio of the PVC paste resin powder to the dispersant aqueous solution is 1:1000;

[0046]Ultrasonic disperse for 10 minutes, raise the temperature to 30°C, let the suspension stand for 20 minutes, and take the middle and upper layer sus...

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Abstract

The invention discloses a preparation method of a PVC paste resin scanning electron microscope sample, which comprises the following steps of (1) dissolving a dispersing agent in deionized water to form a dispersing agent aqueous solution, mixing detected PVC paste resin powder with the dispersing agent aqueous solution to obtain a micro-suspension, dripping the micro-suspension on a carbon conductive adhesive tape of a scanning electron microscope sample table, shaking the sample table to enable the suspension liquid to form a thin liquid layer on the carbon conductive adhesive layer, and drying to obtain a sample precursor, (2) treating the sample precursor by adopting a magnetron sputtering gold plating method to obtain a PVC paste resin scanning electron microscope sample, and (3) preparing the sample obtained in the step (2). The method has the advantages that (1) the non-toxic and non-volatile dispersing agent is used as the dispersing agent of the PVC paste resin powder sample; and (2) the operation is simple, and a clear and high-quality PVC paste resin high-dispersity micro-nano particle image can be obtained on the basis of not changing the morphology of the original PVC paste resin powder particles.

Description

technical field [0001] The invention relates to a detection method for the performance of PVC paste resin. Background technique [0002] PVC paste resin refers to a PVC resin that can form a stable suspension (PVC plastic paste) after being mixed with a plasticizer. PVC paste resin has low strength and a texture similar to talcum powder. PVC paste resin has good foaming and high-speed scraping properties, and can be mixed with high content of fillers. It is suitable for the foam layer of elastic floor, foam artificial leather and wallpaper. PVC paste resin is also widely used in industries such as gloves and automobile interior decoration. [0003] PVC paste resin is usually produced by seed emulsion method and micro-suspension method, and PVC paste resin products containing nearly 100 um secondary particles can be formed by spray drying. The PVC paste resin produced by the seed emulsion method, because the seeds (0.1-1um) are not completely coagulated, the primary partic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/2202G01N23/2251
CPCG01N23/2202G01N23/2251
Inventor 浦旭鑫
Owner SHANGHAI CHLOR ALKALI CHEM