CN108760785B - Method for observing barium titanate ultrafine powder by scanning electron microscope - Google Patents
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Abstract
The invention relates to a method for observing barium titanate ultrafine powder by a scanning electron microscope, which is characterized by comprising the following steps: 1) placing the barium titanate ultrafine powder in a dispersing agent, and performing ultrasonic oscillation to prepare a barium titanate ultrafine powder turbid liquid; 2) transferring the turbid liquid of the barium titanate superfine powder on a carrier sheet; 3) vacuum drying the carrier sheet; 4) placing the dried carrier sheet on a sample press to prepare a sample to be detected; 5) adhering a sample to be detected on a metal sample table by using a conductive adhesive, and spraying a layer of conductive coating in an ion sputtering spraying vacuum instrument; 6) controlling the scanning vacuum shooting condition of the electron microscope; 7) and after the testing distance is adjusted, selecting the area at will. The invention has the beneficial effects that: 1. the problems of uneven dispersion and overlapping agglomeration of the powder are effectively avoided; 2. the sample preparation method is simple, good in repeatability and high in utilization rate; 3. the picture is clear and the appearance is regular when the film is shot under the condition of low voltage, thereby facilitating the statistical analysis of the particle size distribution state; 4. the accuracy and the repeatability of the detection of the ultrafine powder particles are improved.
Description
Technical Field
The invention belongs to the technical field of instrument analysis, relates to a Scanning Electron Microscope (SEM) analysis technology, and particularly relates to a method for observing barium titanate ultrafine powder by using a scanning electron microscope.
Background
Currently, in the observation of barium titanate ultrafine powder by a Scanning Electron Microscope (SEM), there are two main methods for preparing samples: drying and sample preparation after wet dispersion and dry sample preparation. The drying after the wet dispersion is to disperse the barium titanate ultrafine powder into solution, place the solution on a sample table to be tested, dry the solution at the temperature of more than 80 ℃, and perform Scanning Electron Microscope (SEM) observation and analysis after drying; the dry sample preparation is to directly spread barium titanate powder on the double-sided adhesive or the conductive adhesive, blow off the powder which is not adhered on the surface of the conductive adhesive or the double-sided adhesive through an ear washing ball, and perform Scanning Electron Microscope (SEM) observation and analysis after gold spraying or carbon spraying.
The barium titanate ultrafine powder is easy to agglomerate due to large specific surface free energy and specific surface area, so that the problems that the barium titanate ultrafine powder is unclear in picture and difficult to observe the full appearance of particles when observed through a scanning electron microscope due to nonuniform dispersion and mutual superposition of the barium titanate ultrafine powder in a certain degree in the prior art no matter a drying sample or a dry sample is prepared after wet dispersion.
Disclosure of Invention
The invention aims to solve the problem of blurred pictures caused by agglomeration of barium titanate ultrafine powder in the observation of the barium titanate ultrafine powder by using a scanning electron microscope, and provides a method for observing the barium titanate ultrafine powder by using the scanning electron microscope.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for observing barium titanate ultrafine powder by a scanning electron microscope is characterized by comprising the following steps:
1) mixing barium titanate superfine powder (particle diameter D)50Less than or equal to 500 nm) is placed in a dispersant which is not mutually soluble, the mass ratio of the dispersant to the barium titanate superfine powder is controlled to be 600:1-1000:1, ultrasonic oscillation is carried out for 10-30min, and the ultrasonic frequency is 40-80HZ, so as to prepare a barium titanate superfine powder turbid solution (the concentration is between 10 and 30 percent);
2) using a capillary or a trace extractor (gun) to extract (0.1-2 ml) the turbid liquid of the barium titanate ultrafine powder prepared in the step 1) and placing the turbid liquid on a carrier sheet (glass, tin foil paper, conductive adhesive, copper mesh or silicon wafer);
3) vacuum drying the carrier sheet with the turbid solution of barium titanate superfine powder in a vacuum drying oven at 80-110 deg.c and 0.2-0.8MPa for 30 min;
4) placing the carrier sheet obtained after drying in the step 3) on a sample press to obtain a sample to be tested, and controlling the pressure to be 0.01-3.0Mpa and the time to be 5-30 s;
5) putting the sample to be tested prepared in the step 4) on a metal sample table by using a conductive adhesive (conductive double-sided adhesive), then putting the sample in an ion sputtering spraying vacuum instrument for spraying a layer of conductive coating (gold and carbon) with the thickness of 10nm, and controlling the vacuum condition of the spraying of the ion sputtering spraying vacuum instrument to be 5 multiplied by 10-2-6×10-2Pa, current 5-10 mA;
6) controlling the scanning vacuum shooting conditions of the electron microscope: vacuum degree greater than 10-5MPa, low voltage is 2KV-5 KV;
7) after the testing distance is adjusted, a powder electron microscope image with good pixels and excellent appearance effect can be shot by randomly selecting the area.
Further, the dispersant in the step 1) is one or two mixed solvents of absolute ethyl alcohol, acetone and sodium hexametaphosphate.
The invention has the beneficial effects that: 1. the problems of uneven dispersion and overlapping agglomeration of the powder are effectively avoided; 2. the sample preparation method is simple, good in repeatability and high in utilization rate; 3. the picture is clear and the appearance is regular when the film is shot under the condition of low voltage, thereby facilitating the statistical analysis of the particle size distribution state; 4. the accuracy and the repeatability of the detection of the ultrafine powder particles are improved.
Drawings
FIG. 1 is a scanning electron microscope image of a powder sample of example 1 at a magnification of 6 ten thousand times;
FIG. 2 is an X-ray diffraction pattern (20 ℃ to 90 ℃) of the crystal structure of the powder in example 1;
FIG. 3 is a scanning electron microscope image of the powder sample of example 1 at a magnification of 12 ten thousand times;
FIG. 4 is a scanning electron microscope image of the powder sample of example 2 at a magnification of 6 ten thousand times;
FIG. 5 is a scanning electron microscope image of the powder sample of example 3 at a magnification of 6 ten thousand times;
FIG. 6 is an X-ray diffraction pattern (20 ℃ to 90 ℃) of the powder crystals of example 3.
Detailed Description
A sample preparation and observation method for observing barium titanate ultrafine powder by a scanning electron microscope comprises the following specific implementation steps:
example 1
1) 0.1 g of (cubic phase nanoscale) barium titanate ultrafine powder with the particle size of 80-120 nm prepared by a hydrothermal method is placed in a beaker, 60 ml of absolute ethyl alcohol solution is added, and the mixture is shaken up after being subjected to ultrasonic oscillation for 15min at 60HZ in an ultrasonic oscillator to prepare a barium titanate ultrafine powder turbid liquid;
2) sucking out 1ml of barium titanate ultrafine powder turbid liquid by using a clean suction pipe, and uniformly coating the barium titanate ultrafine powder turbid liquid on the conductive adhesive;
3) placing the conductive adhesive stained with the barium titanate ultrafine powder turbid liquid in a vacuum drier, and drying for 30min at 95 ℃ under the vacuum degree of 0.5 MPa;
4) placing the conductive adhesive dried in the step 3) in the center of a sample carrier of a sample pressing machine, and setting the pressure maintaining time to be 10s and the pressure to be 1.0 MPa;
5) blowing off floating particles on the edge of the sample of the pressed sample prepared in the step 4), placing the sample in an ion sputtering vacuum instrument, and performing vacuum treatment under the conditions of current 10mA and vacuum degree of 5 multiplied by 0-5Taking out after Pa metal spraying for 1min, then placing on a sample table in a vacuum chamber of an electron microscope, and vacuumizing to 5 multiplied by 10- 5Under the excitation of 5KV current, observing at any position, and observing that the nano-grade barium titanate ceramic powder particles are uniformly dispersed, the size and the shape are clear, and the particle diameter D of the particles50≦100nm。
Example 2
1) 0.15 g of (tetragonal phase nanoscale) barium titanate ultrafine powder with the particle size of 300-500 nm prepared by a hydrothermal method is placed in a test tube, 0.02 g of sodium hexametaphosphate and 80 ml of absolute ethyl alcohol are added, and the barium titanate ultrafine powder is shaken up after being ultrasonically oscillated for 20min at 50HZ in an ultrasonic oscillator to prepare barium titanate ultrafine powder turbid liquid;
2) sucking out 1ml of barium titanate superfine powder turbid liquid by a clean suction pipe and uniformly coating the barium titanate superfine powder turbid liquid on a silicon wafer;
3) placing the silicon chip stained with the barium titanate ultrafine powder turbid liquid in a vacuum drier, and drying for 30min at 100 ℃ under the vacuum degree of 0.5 MPa;
4) placing the silicon chip dried in the step 3) in the center of a sample carrier of a sample pressing machine, and setting the pressure maintaining time to be 5s and the pressure to be 0.5 MPa;
5) blowing off floating particles on the edge of the pressed sample prepared in the step 4), adhering the pressed sample on a sample measuring table, placing the sample on an ion sputtering vacuum instrument, and carrying out ion sputtering under the conditions of current 10mA and vacuum degree of 5 multiplied by 0-5Taking out after Pa carbon spraying for 1min, then placing on a sample table in a vacuum chamber of an electron microscope, and vacuumizing to 5 × 10-5Under the excitation of 3KV current, observing at any position, and observing that the nano-scale tetragonal phase barium titanate ceramic powder particles are uniformly dispersed, the size and the shape are clear, and the particle diameter D is50≦100nm。
Example 3
1) 0.2g of (tetragonal phase submicron grade) barium titanate ultrafine powder with the particle size of 400-500 mu m, which is obtained after the cubic phase barium titanate powder prepared by a hydrothermal method is calcined, is placed in a beaker, 0.02 g of sodium hexametaphosphate and 100 ml of acetone solution are added, and the mixture is shaken up after being ultrasonically oscillated for 30min at 70HZ in an ultrasonic oscillator to prepare barium titanate ultrafine powder turbid liquid;
2) sucking out 2ml of barium titanate superfine powder turbid liquid by a clean suction pipe and uniformly coating the barium titanate superfine powder turbid liquid on a silicon wafer;
3) placing the silicon chip stained with the barium titanate ultrafine powder turbid liquid in a vacuum drier, and drying for 30min at 100 ℃ under the vacuum degree of 0.5 MPa;
4) placing the silicon chip dried in the step 3) in the center of a sample carrier of a sample pressing machine, and setting the pressure maintaining time to be 5s and the pressure to be 1.0 MPa;
5) blowing off floating particles on the edge of the pressed sample prepared in the step 4), adhering the pressed sample on a sample measuring table, placing the sample on an ion sputtering vacuum instrument, and carrying out ion sputtering under the conditions of current 10mA and vacuum degree of 5 multiplied by 0-5Taking out after Pa carbon spraying for 1min, then placing on a sample table in a vacuum chamber of an electron microscope, and vacuumizing to 5 × 10-5Under the excitation of 5KV current, observing at any position under MPa, and observing that the submicron-grade tetragonal-phase barium titanate ceramic powder particles are uniformly dispersed, the size and the shape are clear, and the particle diameter D is50≦500nm。
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (4)
1. A method for observing barium titanate ultrafine powder by a scanning electron microscope is characterized by comprising the following steps:
1) placing barium titanate ultrafine powder into an immiscible dispersant, controlling the mass ratio of the dispersant to the barium titanate ultrafine powder to be 600:1-1000:1, carrying out ultrasonic oscillation for 10-30min, and carrying out ultrasonic frequency to be 40-80HZ, thus obtaining a barium titanate ultrafine powder turbid solution;
2) transferring the barium titanate ultrafine powder turbid liquid prepared in the step 1) on a carrier sheet by using a capillary or a micro transfer device;
3) vacuum drying the carrier sheet with the turbid solution of barium titanate superfine powder in a vacuum drying oven at 80-110 deg.c and 0.2-0.8MPa for 30 min;
4) placing the carrier sheet obtained after drying in the step 3) on a sample press to obtain a sample to be tested, and controlling the pressure to be 0.01-3.0Mpa and the time to be 5-30 s;
5) adhering the sample to be tested prepared in the step 4) on a metal sample table by using a conductive adhesive, then spraying a layer of conductive coating in an ion sputtering spraying vacuum instrument, and controlling the vacuum condition of spraying of the ion sputtering spraying vacuum instrument to be 5 multiplied by 10-2-6×10-2Pa, current 5-10 mA;
6) controlling the scanning vacuum shooting conditions of the electron microscope: vacuum degree greater than 10-5MPa, low voltage is 2KV-5 KV;
7) after the testing distance is adjusted, the area is selected randomly, and then a powder electron microscope picture can be shot.
2. The method of claim 1, wherein the step of observing the ultra-fine barium titanate powder by using a scanning electron microscope comprises the following steps: the dispersing agent in the step 1) is one or two mixed solvents of absolute ethyl alcohol, acetone and sodium hexametaphosphate.
3. The method of claim 1, wherein the step of observing the ultra-fine barium titanate powder by using a scanning electron microscope comprises the following steps: in the step 2), the carrier sheet is any one of glass, tin foil paper, conductive adhesive, copper mesh or silicon chip.
4. The method of claim 1, wherein the step of observing the ultra-fine barium titanate powder by using a scanning electron microscope comprises the following steps: the conductive plating layer in the step 5) is gold or carbon.
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| CN109444195A (en) * | 2018-12-27 | 2019-03-08 | 中建材蚌埠玻璃工业设计研究院有限公司 | A kind of preparation method of the scanning electron microscope sample of nanoscale barium titanate powder |
| CN109916942B (en) * | 2019-04-18 | 2021-09-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Electron microscopy characterization method of collecting agent |
| CN110186945B (en) * | 2019-05-21 | 2022-03-04 | 东莞东阳光科研发有限公司 | Three-dimensional shape detection method of electrode foil for electrolytic capacitor |
| CN110987549A (en) * | 2019-10-23 | 2020-04-10 | 包头钢铁（集团）有限责任公司 | Sample preparation method for detecting particle size of blast furnace slag particles |
| CN112229864A (en) * | 2020-10-20 | 2021-01-15 | 蚌埠中光电科技有限公司 | Method for analyzing components of foreign matters mixed in spacer paper |
| CN113063717A (en) * | 2021-03-17 | 2021-07-02 | 包头钢铁（集团）有限责任公司 | Method for guiding ore blending by measuring shape of iron ore particles |
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Address after: 233000 28 yuan yuan Road, Huaihe Industrial Park, Huaishang District, Bengbu, Anhui Patentee after: Anhui Kaisheng Applied Materials Co.,Ltd. Patentee after: Bengbu Glass Industry Design and Research Institute Co., Ltd Address before: 233000 28 yuan yuan Road, Huaihe Industrial Park, Huaishang District, Bengbu, Anhui Patentee before: ANHUI ZHONGCHUANG ELECTRONIC INFORMATION MATERIAL Co.,Ltd. Patentee before: Bengbu Glass Industry Design and Research Institute Co., Ltd |
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