A Scanning Electron Microscope Observation Method for Barium Titanate Ultrafine Powder

An electron microscope and barium titanate technology, which is applied in the field of instrument analysis, can solve the problems of blurred pictures, uneven dispersion, and difficulty in observing the whole picture of particles, so as to achieve a simple sample preparation method, good repeatability, and avoid powder dispersion. uneven effect

Active Publication Date: 2021-04-09
安徽凯盛应用材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Barium titanate ultrafine powder is prone to agglomeration due to its large specific surface free energy and specific surface area. To a certain extent, due to the uneven dispersion and superposition of barium titanate ultrafine powder, when the barium titanate ultrafine powder is observed by scanning electron microscope, the picture is blurred and it is difficult to observe the whole picture of the particles.

Method used

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  • A Scanning Electron Microscope Observation Method for Barium Titanate Ultrafine Powder
  • A Scanning Electron Microscope Observation Method for Barium Titanate Ultrafine Powder
  • A Scanning Electron Microscope Observation Method for Barium Titanate Ultrafine Powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Put 0.1 g of barium titanate ultrafine powder with a particle size of 80-120 nm (cubic phase nanoscale) prepared by the hydrothermal method in a beaker, add 60 ml of absolute ethanol solution, and place in an ultrasonic oscillator After oscillating ultrasonically at 60HZ for 15 minutes, shake well to obtain a turbid liquid of barium titanate ultrafine powder;

[0025] 2) Use a clean straw to suck out 1ml of barium titanate ultrafine powder turbid liquid and spread it evenly on the conductive adhesive;

[0026] 3) Put the conductive adhesive stained with the turbid liquid of barium titanate ultrafine powder in a vacuum dryer, and dry at 95°C for 30min at a vacuum of 0.5MPa;

[0027] 4) Place the dried conductive adhesive in step 3) in the center of the sample loading platform of the sample press, set the holding time for 10s, and the pressure is 1.0MPa;

[0028] 5) Blow off the floating particles on the edge of the pressed sample prepared in step 4), and place it in ...

Embodiment 2

[0030] 1) Put 0.15 g of barium titanate ultrafine powder with a particle size of 300-500 nm (tetragonal phase nanoscale) prepared by the hydrothermal method into a test tube, add 0.02 g of sodium hexametaphosphate and 80 ml of absolute ethanol , in an ultrasonic oscillator at 50HZ ultrasonic oscillation for 20min and then shake well to obtain barium titanate ultrafine powder turbid liquid;

[0031] 2) Suck out 1ml barium titanate ultrafine powder turbid liquid with a clean straw and spread it evenly on the silicon wafer;

[0032] 3) Place the silicon wafer with the turbid solution of barium titanate ultrafine powder in a vacuum dryer, and dry at 100°C for 30 minutes at a vacuum of 0.5 MPa;

[0033] 4) Place the dried silicon wafer in step 3) in the center of the sample loading platform of the sample press, set the holding time for 5s, and the pressure is 0.5MPa;

[0034] 5) Blow off the floating particles on the edge of the pressed sample prepared in step 4), and stick it on ...

Embodiment 3

[0036] 1) Put 0.2 g of ultrafine barium titanate powder with a particle size of 400-500 μm (tetragonal phase submicron order) obtained by calcining the cubic phase barium titanate powder prepared by the hydrothermal method into a beaker, and add 0.02 g Sodium hexametaphosphate and 100 ml of acetone solution were shaken in an ultrasonic oscillator at 70HZ for 30 minutes to obtain a barium titanate ultrafine powder turbid solution;

[0037] 2) Suck out 2 ml barium titanate ultrafine powder turbid liquid with a clean straw and spread it evenly on the silicon wafer;

[0038] 3) Place the silicon wafer with the turbid solution of barium titanate ultrafine powder in a vacuum dryer, and dry at 100°C for 30 minutes at a vacuum of 0.5 MPa;

[0039] 4) Place the dried silicon wafer in step 3) in the center of the sample loading platform of the sample press, set the holding time for 5s, and the pressure is 1.0MPa;

[0040] 5) Blow off the floating particles on the edge of the pressed sa...

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Abstract

The invention relates to a scanning electron microscope observation method for barium titanate superfine powder, which is characterized in that it comprises the following steps: 1) the barium titanate superfine powder is placed in a dispersant, and ultrasonically oscillated to prepare barium titanate superfine powder Powder turbid solution; 2) Pipette the barium titanate ultrafine powder turbid solution and place it on the carrier sheet; 3) Vacuum dry the carrier sheet; 4) Put the dried carrier sheet on a press to prepare the sample to be tested; 5) Stick the sample to be tested on the metal sample stage with a conductive adhesive, and place it in an ion sputtering vacuum apparatus to spray a layer of conductive coating; 6) Control the scanning vacuum shooting conditions of the electron microscope; 7) After adjusting the test distance, select any area arbitrarily. Beneficial effects of the present invention: 1. Effectively avoid the problems of uneven powder dispersion and superimposed agglomeration; 2. The sample preparation method is simple, repeatable, and high utilization; 3. Shooting under low voltage conditions, the picture is clear and the appearance is regular , to facilitate the statistical analysis of particle size distribution; 4. Improve the accuracy and repeatability of ultrafine powder particle detection.

Description

technical field [0001] The invention belongs to the technical field of instrument analysis, and relates to a scanning electron microscope (SEM) analysis technology, in particular to a scanning electron microscope observation method for barium titanate superfine powder. Background technique [0002] At present, in the observation of barium titanate ultrafine powder with a scanning electron microscope (SEM), there are two main sample preparation methods commonly used: dry sample preparation after wet dispersion and dry sample preparation. Drying after wet dispersion is to disperse ultra-fine barium titanate powder into a solution, place it on the sample platform to be tested and dry it at a temperature greater than 80°C, and then conduct scanning electron microscope (SEM) observation and analysis after drying; dry method The sample is to sprinkle the barium titanate powder directly on the double-sided adhesive or conductive adhesive, blow off the powder that is not stuck on th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/2202G01N23/2251
CPCG01N23/22G01N23/2202
Inventor 严回倪晶晶张望毛素韩晖王友乐王永和
Owner 安徽凯盛应用材料有限公司
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