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Preparation method of cubic boron nitride micro-powder scanning electron microscopy sample

A technology of boron nitride micropowder and scanning electron microscopy, which is applied in the preparation of test samples, etc., can solve the problems of not being able to see the specific shape of a single particle, not being able to clearly locate the particle size, and not being able to determine the existence of impurities, etc., to achieve a simple dispersant Easy to obtain, easy to observe and locate, and the effect of clear single particle shape

Inactive Publication Date: 2015-07-15
FUNIK ULTRAHARD MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] When studying cubic boron nitride, it is necessary to use scanning electron microscopy to observe and detect the morphology and size of cubic boron nitride ultrafine powder. However, the traditional cubic boron nitride ultrafine powder scanning electron microscope sample preparation method (dry sample preparation ) shortcomings are gradually exposed during the sample preparation process of ultrafine powders with a size not greater than 300nm
Ultrafine powder has small particle size, large specific surface area and high surface energy, and the lack of adjacent coordination atoms on the surface results in a large number of unsaturated bonds on the surface of the particle, which has high surface activity and is at the thermodynamic extreme. In an unstable state, it is easy to spontaneously agglomerate with each other, and even form secondary particles. The ultrafine powder is easy to absorb moisture in the air. The appearance of the ultrafine powder obtained by dry sample preparation is all agglomerated under the scanning electron microscope. , resulting in the inability to clearly locate the size of the particles, the existence of impurities, and the specific shape of individual particles.
In addition, the untreated ultrafine powder can easily pollute the electron microscope sample chamber of the scanning electron microscope, which brings great trouble to the actual production and detection

Method used

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Embodiment 1

[0025] The preparation method of the cubic boron nitride micropowder SEM sample of the present embodiment comprises the following steps:

[0026] 1) Crush the agglomerated ultrafine powder with a hard object to obtain cubic boron nitride powder, with a single particle size ≤ 300nm;

[0027] 2) Place the cubic boron nitride micropowder obtained in step 1) in a test tube, and add absolute ethanol at the same time, the mass ratio of the cubic boron nitride micropowder and absolute ethanol is 1:10000; the test tube is placed in an ultrasonic device, and at F =Under the condition of 100KHz, ultrasonically oscillate for 5 minutes, shake the test tube constantly to shake the sample evenly, to obtain a suspension; the pH of the obtained suspension is 9.

[0028] 3) Take the suspension obtained in step 2) with a rubber dropper, drop 1 drop on the conductive adhesive, and after it is completely dried naturally, the scanning electron microscope sample of the cubic boron nitride micropowd...

Embodiment 2

[0031] The preparation method of the cubic boron nitride micropowder SEM sample of the present embodiment comprises the following steps:

[0032] 1) Crush the agglomerated ultrafine powder with a hard object to obtain cubic boron nitride powder, with a single particle size ≤ 300nm;

[0033] 2) Take the cubic boron nitride micropowder obtained in step 1) and place it in a test tube, add sodium hexametaphosphate (LPL) and absolute ethanol at the same time, the volume ratio of sodium hexametaphosphate and absolute alcohol is 1:1000, cubic nitriding The mass ratio of boron micropowder to absolute ethanol is 3:10000; the test tube is placed in an ultrasonic device, and under the condition of F=60KHz, ultrasonic vibration is performed for 20 minutes, and the test tube is constantly shaken to shake the sample to obtain a suspension; the pH of the obtained suspension is 10.

[0034] 3) Take the suspension obtained in step 2) with a rubber dropper, drop 2 drops on the silicon wafer ad...

Embodiment 3

[0037] The preparation method of the cubic boron nitride micropowder SEM sample of the present embodiment comprises the following steps:

[0038] 1) Crush the agglomerated ultrafine powder with a hard object to obtain cubic boron nitride powder, with a single particle size ≤ 300nm;

[0039] 2) Take the cubic boron nitride micropowder obtained in step 1) and place it in a test tube, add polyacrylic acid (PAA) and dehydrated alcohol simultaneously, the volume ratio of polyacrylic acid and dehydrated alcohol is 3:1000, cubic boron nitride micropowder and dehydrated alcohol The mass ratio of water to ethanol is 8:10000; the test tube is placed in an ultrasonic device, under the condition of F=20KHz, ultrasonically oscillates for 30 minutes, and the test tube is shaken continuously to shake the sample to obtain a suspension; the pH of the obtained suspension is 11.

[0040] 3) Take the suspension obtained in step 2) with a rubber dropper, drop 3 drops on the silicon wafer adhered t...

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Abstract

The invention discloses a preparation method of a cubic boron nitride micro-powder scanning electron microscopy sample. The method comprises the following steps: 1, taking cubic boron nitride micro-powder, adding the micro-powder into a dispersant, and carrying out ultrasonic dispersion to obtain a suspension; and 2, adding the suspension obtained in step 1 to conducting resin in a dropwise manner or adhering the suspension to the silicon chip of the conducting resin, and drying to obtain the sample. The cubic boron nitride micro-powder in the sample prepared through the preparation method of the cubic boron nitride micro-powder scanning electron microscopy sample has less agglomeration and is uniformly dispersed, and the microscopic morphology of the micro-powder can be easily observed; the process is simple and fast when the sample is used in scanning electron microscopy detection, and a high-amplification clear electron microscope photograph is obtained, so the dimension of the cubic boron nitride micro-powder is convenient to observe and position, and the sample is suitable for sample production detection of ultrafine micro-powder with the particle size of 300nm or less; in the preparation process, the sample is difficult to pollute, and damages of the micro-powder to an electron microscope sample chamber are reduced; and the preparation method has the advantages of simple process, convenient operation, simple and easily available dispersant, and suitableness for popularization and application.

Description

technical field [0001] The invention belongs to the technical field of scanning electron microscope sample preparation, in particular to a method for preparing cubic boron nitride micropowder scanning electron microscope samples. Background technique [0002] The hardness of cubic boron nitride is second only to diamond, but its thermal stability and chemical inertness are far superior to diamond. Therefore, in recent years, with the continuous development of science and technology, the application of cubic boron nitride ultrafine powder in aerospace, automobile manufacturing and other high-tech industries has more and more broad prospects. [0003] When studying cubic boron nitride, it is necessary to use scanning electron microscopy to observe and detect the morphology and size of cubic boron nitride ultrafine powder. However, the traditional cubic boron nitride ultrafine powder scanning electron microscope sample preparation method (dry sample preparation ) shortcomings ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
Inventor 王丽
Owner FUNIK ULTRAHARD MATERIAL
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