CN112858362B - Preparation method of micron-sized spherical particle section for electron microscope observation - Google Patents
Preparation method of micron-sized spherical particle section for electron microscope observation Download PDFInfo
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- CN112858362B CN112858362B CN202110023510.0A CN202110023510A CN112858362B CN 112858362 B CN112858362 B CN 112858362B CN 202110023510 A CN202110023510 A CN 202110023510A CN 112858362 B CN112858362 B CN 112858362B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The invention discloses a preparation method of a micron-sized spherical particle section for electron microscope observation, which comprises the following steps: (1) adhering the conductive adhesive tape to the conductive metal substrate; (2) taking micron-sized spherical particle powder, flatly paving and adhering the micron-sized spherical particle powder on a conductive adhesive tape, and blowing away redundant powder; (3) and (3) placing the conductive metal matrix adhered with the powder in an ion beam polishing machine for polishing, wherein a plane polishing mode is adopted, the polishing angle is 0-2 degrees, the polishing voltage and time are 5-8 kV 5-40 min + 3-5 kV 5-20 min + 0.5-2 kV 5-20 min, and the particle section meeting the observation of a scanning electron microscope can be obtained. The invention does not need embedding treatment and consumes no extra sample preparation consumables; the time is short, the cost is low, and the operability is strong; the time consumption is only one tenth of that of a cross section polishing mode, and the polishing efficiency is high; the obtained sample has large effective area and more selectable regions for observation of a scanning electron microscope.
Description
Technical Field
The invention belongs to the technical field of sample preparation of scanning electron microscopes, and particularly relates to a preparation method of a micron-sized spherical particle section for electron microscope observation.
Background
Cross-sectional samples of micron-sized spherical particles have been lacking in high quality means of preparation. Conventional methods include embedded damascene polishing, which is a complicated and time-consuming process, and the polishing solution may contaminate, corrode, or damage the surface of the sample. The improved means include focused ion beam cutting, ultra-thin slicing, and ion beam polishing, wherein the focused ion beam cutting has precise positioning, high cutting efficiency for single particles, and good observation surface, but the high-energy ion cutting inevitably introduces ion implantation pollution. In addition, the focused ion beam cutting equipment has high cost, which causes difficulty in popularization of the method. The ultrathin section method can obtain a smooth spherical particle section, and is suitable for high-quality scanning electron microscope observation, however, before the spherical particle is cut, resin embedding and curing pretreatment needs to be adopted, the time consumption is long, the efficiency is low, and only a plurality of particle sections can be obtained in each sample preparation. Neibo Ying et al adopt an ion beam polishing technology to prepare a particle section sample, the section obtained by the method has good flatness and a large area, and can meet the observation requirement of a scanning electron microscope (Neibo Ying et al, preparation of NCM particle section sample [ J ], an analytical instrument, 2019, 3: 90-93); the method comprises the steps of mixing spherical particles with carbon conductive glue solution, embedding the mixture with aluminum foil, tabletting, cutting to form a section polishing sample, and then transferring the section polishing sample to an ion polishing machine for section polishing, wherein the polishing voltage is 6.5kV, and the time is 6 h.
The existing ion beam polishing technology for preparing a cross-section sample has the following defects that firstly, the sample pretreatment step is complicated, and the carbon conductive glue solution is used as a dispersing agent, a fixing agent and a filling agent, so that the raw material consumption is large and the cost is high; and secondly, the ion polishing adopts a cross section polishing mode, so that the polishing time is long and the efficiency is low.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a micron-sized spherical particle section for electron microscope observation.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a micron-sized spherical particle section for electron microscope observation is characterized by comprising the following steps:
(1) adhering the conductive adhesive tape to the conductive metal substrate;
(2) spreading micron-sized spherical particle powder on a conductive adhesive tape, and blowing away redundant powder;
(3) and (3) placing the conductive metal matrix adhered with the powder in an ion beam polishing machine for polishing, wherein a plane polishing mode is adopted, the polishing angle is 0-2 degrees, the polishing voltage and time are 5-8 kV 5-40 min + 3-5 kV 5-20 min + 0.5-2 kV 5-20 min, and the particle section meeting the observation of a scanning electron microscope can be obtained.
Preferably, the conductive tape is a double-sided conductive carbon tape or a copper tape.
Preferably, the conductive metal matrix is copper or aluminum.
Preferably, the polishing voltage and time are 5-8 kV for 5-15 min + 3-5 kV for 5-20 min + 0.5-2 kV for 5-20 min.
Further preferably, the polishing voltage and time are 7kV 5min +4kV 10min +1kV 10 min.
Preferably, the conductive metal matrix is 8mm x 8mm in size.
Preferably, the micron-sized spherical particle powder has a diameter of 5 to 20 μm.
Preferably, the micron-sized spherical particles are metallic, inorganic non-metallic or ceramic spherical particles.
Further preferably, the micron-sized spherical particles are LiNiCoMnO2A battery anode material or a pure titanium microsphere material.
Preferably, the ion beam polisher is an argon ion polisher.
The invention has the beneficial effects that: the spherical particle powder is directly paved on the metal matrix for polishing pretreatment, embedding treatment is not needed, and extra sample preparation consumables are not consumed. The pretreatment steps are few, the time is short, the cost is low, and the operability is strong; secondly, the ion polishing adopts a plane polishing mode, the polishing time is short, the time consumption is only one tenth of that of a cross section polishing mode, and the polishing efficiency is high; and thirdly, the effective area of the sample obtained in the plane polishing mode is large, and the selectable area for observing by the scanning electron microscope is large.
Drawings
FIG. 1 is a LiNiCoMnO2Scanning electron microscope images of the surfaces of the spherical particles before ion polishing of the battery anode material powder.
FIG. 2 is a scanning electron micrograph of a cross section of a spherical particle after ion polishing in example 1.
FIG. 3 is a scanning electron micrograph of a cross section of a spherical particle after ion polishing in example 2.
FIG. 4 is a scanning electron micrograph of a cross section of a spherical particle after ion polishing in example 3.
FIG. 5 is a scanning electron microscope image of the surface of the spherical particles before ion polishing of the industrial pure titanium microsphere powder.
FIG. 6 is a scanning electron micrograph of a cross section of a spherical particle after ion polishing in example 4.
FIG. 7 is a scanning electron micrograph of a cross section of a spherical particle after ion polishing in example 5.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
The experimental procedures in the following examples are conventional unless otherwise specified.
The embodiment of the invention uses main reagents and devices:
LiNiCoMnO2battery positive electrode material: the diameter of the powder of a certain lithium ion battery anode material manufacturer in China is 5-20 mu m, and the scanning electron microscope image of the surface of spherical particles before ion polishing is shown in figure 1.
Industrial pure titanium microsphere material: the diameter of the powder of a certain domestic metal powder manufacturer is 2-15 μm, and the scanning electron microscope image of the surface of the spherical particles before ion polishing is shown in FIG. 5.
Argon ion polishing machine: brand name: gatan, type: ilions 697.
Example 1
Preparing a micron-sized spherical particle section for observation of a scanning electron microscope, and operating according to the following steps:
(1) adhering a double-sided conductive carbon adhesive tape to an aluminum metal substrate with the size of 8mm multiplied by 8 mm;
(2) using toothpick to pick up small quantity of LiNiCoMnO2The powder of the battery anode material is flatly paved and adhered on the conductive adhesive tape, and the excessive powder is blown away by a blower, and only the powder adhered on the conductive adhesive tape is remained;
(3) and (3) polishing the aluminum metal matrix with the powder in an argon ion polishing machine in a plane polishing mode, wherein the angle of an ion gun is 2 degrees, and the polishing voltage and time are 7kV 5min +4kV 10min +1kV 10min, so that a section meeting the observation requirement of a scanning electron microscope can be obtained, and the scanning electron microscope image of the section of the spherical particles after ion polishing is shown in figure 2.
Example 2
Preparing a micron-sized spherical particle section for observation by a scanning electron microscope, and operating according to the following steps:
(1) adhering the double-sided conductive copper adhesive tape to a copper metal substrate with the size of 8mm multiplied by 8 mm;
(2) using toothpick to pick up small quantity of LiNiCoMnO2The powder of the battery anode material is flatly paved and adhered on the conductive adhesive tape, and the excessive powder is blown away by a blower;
(3) the copper metal matrix with the powder is placed in an argon ion polishing machine for polishing, a plane polishing mode is adopted, the angle of an ion gun is 0.5 degrees, the polishing voltage and time are 7kV 5min +4kV 10min +1kV 10min, the section meeting the observation requirement of a scanning electron microscope can be obtained, and the scanning electron microscope image of the section of the spherical particles after ion polishing is shown in figure 3.
Example 3
Preparing a micron-sized spherical particle section for observation by a scanning electron microscope, and operating according to the following steps:
(1) adhering the double-sided conductive copper adhesive tape on an aluminum metal substrate with the size of 8mm multiplied by 8 mm;
(2) using toothpick to pick up small quantity of LiNiCoMnO2The battery anode material powder is flatly paved and adhered on the conductive adhesive tape, and the excessive powder is blown away by a blower;
(3) the copper metal matrix with the powder is placed in an argon ion polishing machine for polishing, a plane polishing mode is adopted, the angle of an ion gun is 0 degree, the polishing voltage and time are 7kV 5min +4kV 10min +1kV 10min, and then the section which meets the observation requirement of a scanning electron microscope can be obtained, and the scanning electron microscope image of the section of the spherical particles after ion polishing is shown in figure 4.
Example 4
Preparing an industrial pure titanium micron-sized spherical particle section for scanning electron microscope observation, and operating according to the following steps:
(1) the double-sided conductive carbon adhesive tape is stuck on an aluminum metal substrate with the size of 8mm multiplied by 8 mm;
(2) a small amount of industrial pure titanium microsphere material powder is stuck by a toothpick, laid flat and stuck on the conductive adhesive tape, and the excess powder is blown away by a blower, so that only the powder stuck on the conductive adhesive tape is remained;
(3) the aluminum metal matrix with the powder is placed in an argon ion polishing machine for polishing, a plane polishing mode is adopted, the angle of an ion gun is 0 degree, the polishing voltage and time are 8kV 15min +4kV 10min +1kV 10min, the cross section meeting the observation requirement of a scanning electron microscope can be obtained, and the scanning electron microscope image of the cross section of the spherical particles after ion polishing is shown in figure 6.
Example 5
Preparing an industrial pure titanium micron-sized spherical particle section for scanning electron microscope observation, and operating according to the following steps:
(1) adhering the double-sided conductive copper adhesive tape to a copper metal substrate with the size of 8mm multiplied by 8 mm;
(2) a small amount of industrial pure titanium microsphere material powder is stuck by a toothpick, laid flat and stuck on a conductive adhesive tape, and excess powder is blown away by a blower, so that only the powder stuck on the conductive adhesive tape is remained;
(3) the copper metal matrix with the powder is placed in an argon ion polishing machine for polishing, a plane polishing mode is adopted, the angle of an ion gun is 0 degree, the polishing voltage and time are 8kV 40min +4kV 20min +1kV 20min, and then the section which meets the observation requirement of a scanning electron microscope can be obtained, and the scanning electron microscope image of the section of the spherical particles after ion polishing is shown in figure 7.
As can be seen from the scanning electron micrographs of FIGS. 1-7, the spherical particles of examples 1-5, prepared by the process of the present invention, had intact particles, no fragmentation or contamination, clear spherical edges, and intact internal structures. The effective area of the obtained cross section sample is large, a cross section with the area of tens of square centimeters can be obtained after ion beam polishing in theory, and the number of selectable regions for scanning electron microscope observation is large. After ion beam polishing by the method, the section of the spherical particle can be shown under low observation times. And polishing parameters are optimized, and an observation section with good flatness can be obtained. Under high observation times, the size and distribution information of the internal pores of the spherical particles can be obtained.
Claims (5)
1. A preparation method of a micron-sized spherical particle section for electron microscope observation is characterized by comprising the following steps:
(1) adhering the conductive adhesive tape to the conductive metal substrate;
(2) taking micron-sized spherical particle powder, flatly paving and adhering the micron-sized spherical particle powder on a conductive adhesive tape, and blowing away redundant powder; the micron-sized spherical particles are LiNiCoMnO2The diameter of the micron-sized spherical particle powder is 5-20 mu m;
(3) and (3) placing the conductive metal matrix adhered with the powder in an argon ion beam polishing machine for polishing, wherein a plane polishing mode is adopted, the polishing angle is 0-2 degrees, the polishing voltage and time are 7-8 kV 5-15 min +4kV 10min +1kV 10min, and the particle section meeting the observation of a scanning electron microscope can be obtained.
2. The method of claim 1, wherein: the conductive adhesive tape is a double-sided conductive carbon adhesive tape or a copper adhesive tape.
3. The method of claim 1, wherein: the conductive metal matrix is copper or aluminum.
4. The method of claim 1, wherein: the polishing voltage and time are 7kV 5min +4kV 10min +1kV 10 min.
5. The method of claim 1, wherein: the size of the conductive metal matrix is 8mm multiplied by 8 mm.
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| CN114062076A (en) * | 2021-11-04 | 2022-02-18 | 九江德福科技股份有限公司 | Sample preparation method for copper foil crystal analysis |
| CN115684229A (en) * | 2022-09-21 | 2023-02-03 | 哈尔滨工业大学 | Preparation method of micron-sized particle section capable of being repeatedly used for electron microscope observation |
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