CN114459854A - Sample preparation method for analyzing silicon steel precipitate - Google Patents
Sample preparation method for analyzing silicon steel precipitate Download PDFInfo
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- CN114459854A CN114459854A CN202210087470.0A CN202210087470A CN114459854A CN 114459854 A CN114459854 A CN 114459854A CN 202210087470 A CN202210087470 A CN 202210087470A CN 114459854 A CN114459854 A CN 114459854A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
- G01N1/06—Devices for withdrawing samples in the solid state, e.g. by cutting providing a thin slice, e.g. microtome
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a sample preparation method for analyzing silicon steel precipitates, which is characterized in that a replica method is adopted to erode away a matrix to expose the precipitates, a thin carbon film is formed by carbon spraying, the precipitates are adsorbed out, and the carbon film is observed by a transmission electron microscope, so that the problem of sample oxidation is solved.
Description
Technical Field
The invention relates to a sample preparation method for analyzing silicon steel precipitates.
Background
Factors influencing the magnetic performance of the silicon steel include components, textures and precipitates, the size of the precipitates influencing the magnetic performance of the silicon steel is 10-300 nm, and the sample preparation steps for detecting the precipitates are multiple and difficult, so that the process is critical and important.
At present, application No. 201810472828.5 discloses an inclusion precipitation control process for silicon steel for a motor. The permanent magnetic material and the processing technology thereof are mainly introduced, the influence of the precipitate on the magnetic property is explained, but the sample preparation process of precipitate analysis is not explained. The sample preparation method is suitable for analyzing precipitates of oriented silicon steel and non-oriented silicon steel, elaborates the problems of sample preparation process and attention in detail, and has important significance for deeply analyzing the types, sizes, distribution and appearances of the precipitates.
Application No. 2011811300377.3 discloses a method for analyzing inhibitors in grain-oriented silicon steel, which uses a non-aqueous solution to prepare a sample by electrolytic etching, and describes the process of analyzing precipitates in detail. The invention elaborates the sample preparation process for analyzing the silicon steel precipitate in detail, and basically sets up the inherent sample preparation method and flow, so that the sample preparation for precipitate analysis is legal, convenient and quick.
The existing sample preparation method is to prepare a film sample by electrolytic double spraying, and for silicon steel, because the silicon steel is easy to oxidize, after the film sample is prepared by double spraying, an oxidized rust layer can be quickly formed on the surface of the sample, and the analysis of precipitates of a transmission electron microscope is seriously influenced.
Disclosure of Invention
The invention aims to provide a sample preparation method for analyzing silicon steel precipitates, which adopts a replica method to erode away a matrix to expose the precipitates, forms a thin carbon film by carbon spraying, adsorbs the precipitates, and performs transmission electron microscope observation on the carbon film to solve the problem of sample oxidation.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention relates to a sample preparation method for analyzing silicon steel precipitates, which comprises the following steps:
(1) sampling
Shearing a sample with the thickness multiplied by the rolling direction multiplied by 15mm multiplied by the transverse direction multiplied by 10mm on a hot-rolled, normalized and decarburized annealed plate;
(2) polishing
Coarse grinding with coarse 50 grit paper, then fine grinding with fine 280 and 400 grit paper;
(3) physical polishing
Polishing on a metallographic polishing machine;
(4) electrolyte corrosion
The electrolyte is a mixed solution of 44.5 percent methanol, 5 percent acetylacetone and 5g tetramethylammonium chloride, a sample is taken as an anode, a stainless steel plate is taken as a cathode, the constant voltage is 12V, and the current is changed according to the size of the sample; the corrosion is to corrode the iron matrix to expose precipitates;
(5) carbon-sprayed film
Fixing a sample on a sample table by using a double-sided adhesive tape, and spraying carbon by using a multifunctional sample surface treatment machine; vacuumizing the carbon spraying pretreatment machine, and spraying carbon when the vacuum degree reaches 2.4 multiplied by 103 Pa; carbon spraying uses a high-purity carbon rod, the carbon rods on two sides are electrified and contacted, the current is controlled to be about 30A, the current is kept for 1-2 s, the carbon rod is heated and volatilized, a thin carbon film is formed on the surface of the sample, and the carbon film can adsorb the exposed precipitate; recovering the vacuum degree to atmospheric pressure after the carbon spraying is finished, and taking out the sample;
(6) decarbonizing membrane
The decarbonization film adopts 7% perchloric acid alcohol electrolytic solution, the sample is an anode, the stainless steel plate is a cathode, the constant voltage is 18V, and the current is changed according to the size of the sample; before the carbon film is removed, the carbon film is divided into small squares by tweezers, so that the carbon film is convenient to remove; after the membrane is removed, sucking the carbon membrane out of the solution by using a suction pipe, and cleaning; the cleaning solution is sequentially diluted perchloric acid alcohol solution, pure alcohol and 2/3 volume fraction alcohol water solution;
(7) carbon fishing film
After the carbon film is cleaned, taking out the carbon film by using a 300-400 mesh nickel net with the diameter of phi 3mm, adsorbing the carbon film on the nickel net, and putting the nickel net on dry filter paper for drying; and finally, putting the nickel net and the carbon film into a transmission electron microscope sample box for storage, so that the precipitate can be conveniently analyzed by a subsequent transmission electron microscope.
Compared with the prior art, the invention has the beneficial technical effects that:
the invention adopts a carbon-restoration method to prepare the silicon steel precipitate analysis sample, and solves the problem that the surface of the sample is easy to form an oxidation rust layer by the existing electrolysis double-spraying method.
Drawings
The invention is further illustrated in the following description with reference to the drawings.
FIG. 1 is a carbon film taken out of a nickel mesh;
Detailed Description
The present invention will be described in further detail with reference to specific examples.
A sample preparation method for analyzing silicon steel precipitates comprises the following steps:
(1) sampling
A specimen having a thickness of 15mm (roll direction) 10mm (transverse direction) was cut out from a hot-rolled, normalized and decarburized annealed sheet.
(2) Polishing
Coarse sandpaper 50, then fine sandpaper 280 and 400.
(3) Physical polishing
And (5) polishing on a metallographic polishing machine.
(4) Electrolyte corrosion
The electrolyte was a mixed solution of 44.5% methanol, 5% acetylacetone and 5g tetramethylammonium chloride, the sample was an anode, a stainless steel plate was a cathode, a constant voltage was 12V, and the current was varied depending on the size of the sample. The corrosion is to etch away the iron matrix and expose precipitates.
(5) Carbon-sprayed film
The sample was fixed on the sample table with a double-sided tape, and carbon spraying was performed with a multifunctional sample surface treatment machine (carbon spraying instrument). And (4) vacuumizing the carbon spraying pretreatment machine, and spraying carbon when the vacuum degree reaches about 2.4X 103 Pa. And (3) carbon spraying uses a high-purity carbon rod, the carbon rods on two sides are electrified and contacted, the current is controlled to be about 30A and kept for 1-2 s, the carbon rod is heated and volatilized, a thin carbon film is formed on the surface of the sample, and the carbon film can adsorb the exposed precipitate. And after the carbon spraying is finished, restoring the vacuum degree to the atmospheric pressure, and taking out the sample.
(6) Decarbonizing membrane
The decarbonization membrane was prepared by using a 7% perchloric acid alcohol electrolytic solution, the sample was an anode, a stainless steel plate was a cathode, a constant voltage was 18V, and the current was varied depending on the size of the sample. Before the carbon film is removed, the carbon film is divided into small squares by tweezers, so that the carbon film is convenient to remove. After the membrane was removed, the carbon membrane was removed from the solution with a pipette and washed. The cleaning solution is sequentially diluted perchloric acid alcohol solution, pure alcohol and 2/3 volume fraction alcohol water solution. On one hand, the method is used for cleaning the electrolytic solution on the surface of the carbon film, and on the other hand, the carbon film is slowly diffused and is not cracked.
(7) Carbon fishing film
And after the carbon film is cleaned, taking out the carbon film by using a 300-400 mesh nickel net with the diameter of phi 3mm, adsorbing the carbon film on the nickel net, and putting the nickel net on dry and clean filter paper for drying. And finally, putting the nickel net and the carbon film into a transmission electron microscope sample box for storage, so that the precipitate can be conveniently analyzed by a subsequent transmission electron microscope.
The analysis of silicon steel precipitates is very difficult and requires the observation of the morphology, size, type and distribution of the precipitates on a transmission electron microscope. The sample preparation process is relatively difficult, the conventional method for analyzing and preparing the precipitates of the steel is to prepare a film sample by electrolytic double spraying, and the sample prepared by the method is very easy to oxidize due to the particularity of silicon steel components, so that the subsequent precipitate analysis is seriously influenced. In the embodiments of the present application, a replica method is adopted to erode away the matrix, so that the precipitates are exposed, a thin carbon film is formed by carbon spraying, the precipitates are adsorbed, and the carbon film is observed by a transmission electron microscope, so that the problem of sample oxidation is solved.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (1)
1. A sample preparation method for analyzing silicon steel precipitates is characterized by comprising the following steps:
(1) sampling
Shearing a sample with the thickness multiplied by the rolling direction multiplied by 15mm multiplied by the transverse direction multiplied by 10mm on a hot-rolled, normalized and decarburized annealed plate;
(2) polishing
Coarse grinding with coarse 50 grit paper, then fine grinding with fine 280 and 400 grit paper;
(3) physical polishing
Polishing on a metallographic polishing machine;
(4) electrolyte corrosion
The electrolyte is a mixed solution of 44.5 percent methanol, 5 percent acetylacetone and 5g tetramethylammonium chloride, a sample is taken as an anode, a stainless steel plate is taken as a cathode, the constant voltage is 12V, and the current is changed according to the size of the sample; the corrosion is to corrode the iron matrix to expose precipitates;
(5) carbon-sprayed film
Fixing a sample on a sample table by using a double-sided adhesive tape, and spraying carbon by using a multifunctional sample surface treatment machine; vacuumizing the carbon spraying pretreatment machine, and spraying carbon when the vacuum degree reaches 2.4 multiplied by 103 Pa; carbon spraying uses a high-purity carbon rod, the carbon rods on two sides are electrified and contacted, the current is controlled to be about 30A, the current is kept for 1-2 s, the carbon rod is heated and volatilized, a thin carbon film is formed on the surface of the sample, and the carbon film can adsorb the exposed precipitate; recovering the vacuum degree to atmospheric pressure after the carbon spraying is finished, and taking out the sample;
(6) decarbonization film
The decarbonization film adopts 7% perchloric acid alcohol electrolytic solution, the sample is an anode, the stainless steel plate is a cathode, the constant voltage is 18V, and the current is changed according to the size of the sample; before the carbon film is removed, the carbon film is divided into small squares by tweezers, so that the carbon film is convenient to remove; after the membrane is removed, sucking the carbon membrane out of the solution by using a suction pipe, and cleaning; the cleaning solution is sequentially diluted perchloric acid alcohol solution, pure alcohol and 2/3 volume fraction alcohol water solution;
(7) carbon fishing film
After the carbon film is cleaned, taking out the carbon film by using a 300-400 mesh nickel net with the diameter of phi 3mm, adsorbing the carbon film on the nickel net, and putting the nickel net on dry filter paper for drying; and finally, putting the nickel net and the carbon film into a transmission electron microscope sample box for storage, so that the precipitate can be conveniently analyzed by a subsequent transmission electron microscope.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210087470.0A CN114459854B (en) | 2022-01-25 | 2022-01-25 | Sample preparation method for analyzing silicon steel precipitate |
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| CN202210087470.0A CN114459854B (en) | 2022-01-25 | 2022-01-25 | Sample preparation method for analyzing silicon steel precipitate |
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| CN114459854A true CN114459854A (en) | 2022-05-10 |
| CN114459854B CN114459854B (en) | 2023-09-26 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005181082A (en) * | 2003-12-18 | 2005-07-07 | Nippon Steel Corp | Preparing method of sample for strain part observation inside of steel product |
| CN102620971A (en) * | 2012-03-20 | 2012-08-01 | 上海大学 | Sample preparation method for researching Cu precipitated phase in steel by means of extraction replica |
| CN109142415A (en) * | 2018-11-02 | 2019-01-04 | 首钢智新迁安电磁材料有限公司 | The analysis method of inhibitor in a kind of orientation silicon steel |
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- 2022-01-25 CN CN202210087470.0A patent/CN114459854B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005181082A (en) * | 2003-12-18 | 2005-07-07 | Nippon Steel Corp | Preparing method of sample for strain part observation inside of steel product |
| CN102620971A (en) * | 2012-03-20 | 2012-08-01 | 上海大学 | Sample preparation method for researching Cu precipitated phase in steel by means of extraction replica |
| CN109142415A (en) * | 2018-11-02 | 2019-01-04 | 首钢智新迁安电磁材料有限公司 | The analysis method of inhibitor in a kind of orientation silicon steel |
Non-Patent Citations (1)
| Title |
|---|
| 马红旭, 李友国: "硅钢中析出物的尺寸分布以及体积分数的测定", 材料科学与工程, no. 03 * |
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