Method for measuring wall thickness of hollow glass bead

Abstract

The invention discloses a method for measuring the wall thickness of a hollow glass bead, and relates to the technical field of glass wall thickness measurement, and the method comprises the following steps: putting a sample table into an FIB-SEM; when the vacuum degree is smaller than 5 * 10 <-3 > Pa, the electron beam is turned on, and a target sample is found; rotating the sample table T = 5 degrees, observing whether the target sample is in the view center under the electron beam, and if not, adjusting the Z axis to the center; repeatedly rotating T = 20 degrees and T = 52 degrees to ensure that the target sample is always in the center of the visual field; opening the ion beam to ensure that the target sample is in the view center under the view of the electron beam and the ion beam; t refers to Tilt and is an axis of a sample table of the FIB-SEM; cCSpattern is adopted to cut a selected area of the sample, X is 8 microns, Y is 2 microns, and Z is 2 microns; and rotating T = 0 degree, observing the sample under the electron beam, and measuring the wall thickness. According to the method for measuring the wall thickness of the hollow glass bead, the wall thickness of the hollow glass bead can be rapidly measured, and the accuracy rate is high.

Description

Technical Field

[0001] The present invention relates to a method for measuring the wall thickness of hollow glass microspheres, and particularly to the technical field of glass wall thickness measurement. Background Art

[0002] Hollow glass microspheres are a new type of inorganic non-metallic spherical powder material, which are composed of spherical thin-walled (0.5 - 2.0 μm) glass particles with diameters of 10 - 200 μm and above. Wall thickness is an important physical parameter of hollow glass microspheres, which has a great influence on their strength and density. Generally speaking, the methods for measuring wall thickness include: optical interference method, microscopic observation method, and estimation method. The optical interference method is complex to operate and has low accuracy. The microscopic observation method simply uses SEM to find damaged spheres for detection under the electron beam, requiring the cross-section to be perpendicular to the axis of the microscope, so the efficiency is low and the error is large. The estimation method mainly obtains the wall thickness of hollow glass microspheres through mathematical calculations, which is cumbersome and can only estimate its wall thickness. Therefore, it is necessary to conduct relevant research, develop new measurement methods, and improve the detection efficiency and accuracy. Summary of the Invention

[0003] The purpose of the present invention is to provide a method for measuring the wall thickness of hollow glass microspheres. This method realizes the rapid and accurate measurement of the wall thickness of hollow glass microspheres by precisely cutting the hollow glass microspheres using FIB-SEM and optimizing the experimental parameters.

[0004] To achieve the above purpose, the present invention is realized through the following technical solutions:

[0005] A method for measuring the wall thickness of hollow glass microspheres includes the following steps:

[0006] Place the sample stage into the FIB-SEM;

[0007] Wait until the vacuum degree is reached, turn on the electron beam, and find the target sample;

[0008] Rotate the sample stage to ensure that the target sample is at the center of the field of view under both the electron beam and the ion beam fields of view;

[0009] Use CCSPattern to cut the selected area of the sample;

[0010] Rotate the sample stage, observe the sample under the electron beam, and measure the wall thickness.

[0011] The further technology of the present invention:

[0012] Preferably, before placing the sample stage into the FIB-SEM, paste the conductive adhesive on the scanning electron microscope sample stage, take an appropriate amount of hollow glass microsphere sample with a small spoon and gently sprinkle it on the conductive adhesive, and then gold-plate it.

[0013] Preferably, the gold-plating duration is 60S.

[0014] Preferably, the required vacuum degree is < 5*10-3 Pa.

[0015] Preferably, rotate the sample stage and observe whether the target sample is at the center of the field of view under the electron beam. If it is not at the center, adjust the Z-axis to the center; repeat the sample stage to ensure that the target sample is always at the center of the field of view.

[0016] The beneficial effects of the present invention are as follows:

[0017] The method of the present invention for measuring the wall thickness of hollow glass microspheres can achieve rapid determination of the wall thickness of hollow glass microspheres with high accuracy, and at the same time, the required microspheres can be directionally selected according to actual requirements. This method is simple to operate and is beneficial to guiding industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic flow diagram of the present invention.

[0019] Figure 2 It is a diagram of finding the target sample by turning on the electron beam.

[0020] Figure 3 It is a diagram of observing the target sample at the center of the field of view under the electron beam.

[0021] Figure 4 It is a diagram of observing the target sample at the center of the field of view under the ion beam.

[0022] Figure 5 It is to cut the selected area of the sample with CCSPattern Figure 1 .

[0023] Figure 6 It is to cut the selected area of the sample with CCSPattern Figure 2 .

[0024] Figure 7 It is a diagram of observing the sample to measure the wall thickness under the electron beam. DETAILED DESCRIPTION OF THE INVENTION

[0025] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0026] As Figure 1 shown, the present invention provides a method for measuring the wall thickness of hollow glass microspheres, including the following steps:

[0027] Step S1: Paste the conductive adhesive on the scanning electron microscope sample stage;

[0028] Step S2: Use a small spoon to take an appropriate amount of hollow glass microsphere sample and gently sprinkle it on the conductive adhesive and then gold-plate it. Gold-plating is to increase conductivity, and the gold-plating time is 60S;

[0029] Step S3: Place the sample stage into the FIB-SEM;

[0030] Step S4: Wait until the vacuum degree < 5 * 10-3 Pa, such as Figure 2 , turn on the electron beam and find the target sample;

[0031] Step S5: Rotate the sample stage T = 5°, and observe whether the target sample is at the center of the field of view under the electron beam. If it is not at the center, adjust the Z-axis to the center; repeat the rotation T = 20°, T = 52°, such as Figure 3 , ensure that the target sample is always at the center of the field of view; at the same time, turn on the ion beam to ensure that the target sample is at the center of the field of view under both the electron beam and the ion beam, such as Figure 4 ;

[0032] It should be noted that T refers to Tilt, which is an axis of the sample stage of the FIB-SEM.

[0033] Step S6: Such as Figures 5-6 , use CCSPattern to cut the selected area of the sample, X = 8μm, Y = 2μm, Z = 2μm;

[0034] Step S7: Such as Figure 7 , rotate T = 0°, observe the sample under the electron beam and measure the wall thickness.

[0035] The above is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution and inventive concept of the present invention, makes equivalent substitutions or changes, and all should be covered within the protection scope of the present invention.

Claims

1. A method for measuring the wall thickness of hollow glass microspheres, characterized in that: The steps include: Place the sample stage into the FIB-SEM; When the vacuum degree is reached, turn on the electron beam and find the target sample; Rotate the sample stage to ensure that the target sample is in the center of the electron beam and ion beam fields of view; CCSPattern was used to cut the selected area of ​​the sample; Rotate the sample stage to observe the sample under the electron beam and measure the wall thickness.

2. A method for measuring the wall thickness of hollow glass microspheres according to claim 1, characterized in that: Before placing the sample stage into FIB-SEM, stick the conductive glue on the SEM sample stage, take an appropriate amount of hollow glass microbead sample with a small spoon, sprinkle it gently on the conductive glue and plate it with gold.

3. A method for measuring the wall thickness of hollow glass microspheres according to claim 1, characterized in that: The gold plating time is 60S.

4. A method for measuring the wall thickness of hollow glass microspheres according to claim 1, characterized in that: The vacuum degree requirement is <5*10-3Pa.

5. A method for measuring the wall thickness of hollow glass microspheres according to claim 1, characterized in that: Rotate the sample stage and observe whether the target sample is in the center of the field of view under the electron beam. If not, adjust the Z axis to the center; repeat the sample stage to ensure that the target sample is always in the center of the field of view.

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