CN114459854B - Sample preparation method for analyzing silicon steel precipitate - Google Patents
Sample preparation method for analyzing silicon steel precipitate Download PDFInfo
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- CN114459854B CN114459854B CN202210087470.0A CN202210087470A CN114459854B CN 114459854 B CN114459854 B CN 114459854B CN 202210087470 A CN202210087470 A CN 202210087470A CN 114459854 B CN114459854 B CN 114459854B
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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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- Sampling And Sample Adjustment (AREA)
Abstract
The application discloses a sample preparation method for analyzing silicon steel precipitate, which adopts a replica method to erode away a matrix to expose the precipitate, utilizes carbon spraying to form a thin carbon film, adsorbs the precipitate out, and carries out transmission electron microscope observation on the carbon film to solve the problem of sample oxidation.
Description
Technical Field
The application relates to a sample preparation method for analyzing silicon steel precipitate.
Background
Factors influencing the magnetic properties of the silicon steel include components, textures and precipitates, the size of the precipitates influencing the magnetic properties of the silicon steel is 10-300 nm, and the sample preparation steps for detecting the precipitates are more and more difficult, so that the link is very critical and important.
Currently, application number 201810472828.5 discloses a process for controlling precipitation of inclusions in silicon steel for motors. The key points are to introduce a permanent magnetic material and a processing technology thereof, which illustrate the influence of the precipitate on the magnetic performance, but the sample preparation process of the precipitate analysis is not illustrated. The method is suitable for sample preparation methods for analyzing the precipitates of the oriented silicon steel and the non-oriented silicon steel, details the sample preparation process and the attention problem, and has important significance for deeply analyzing the types, the sizes, the distribution and the morphology of the precipitates.
Application number 2011811300377.3 discloses an analysis method for inhibitors in oriented silicon steel, which adopts nonaqueous-based solution electrolytic corrosion sample preparation and details the process of analyzing the precipitate. The application elaborates the sample preparation process for analyzing the silicon steel precipitate, basically establishes the inherent sample preparation method and flow, and enables the sample preparation of the precipitate analysis to be convenient and quick.
The existing sample preparation method is to prepare a film sample by electrolysis double spraying, and for silicon steel, as silicon steel is easy to oxidize, after the film sample is prepared by double spraying, a layer of oxidized rust layer is formed on the surface of the sample, so that the analysis of the precipitate of a transmission electron microscope is seriously affected.
Disclosure of Invention
The application aims to provide a sample preparation method for analyzing silicon steel precipitate, which adopts a replica method to erode away a matrix to expose the precipitate, utilizes carbon spraying to form a thin carbon film, adsorbs the precipitate out, and carries out transmission electron microscope observation on the carbon film to solve the problem of sample oxidation.
In order to solve the technical problems, the application adopts the following technical scheme:
the application relates to a sample preparation method for analyzing silicon steel precipitates, which comprises the following steps:
(1) Sampling
Shearing a sample with a thickness of 15mm in the rolling direction and 10mm in the transverse direction on a hot rolled, normalized and decarburized annealed plate;
(2) Polishing
Coarse grinding is carried out on No. 50 coarse sand paper, and then fine grinding is carried out on No. 280 fine sand paper and No. 400 fine sand paper;
(3) Physical polishing
Polishing on a metallographic polishing machine;
(4) Electrolyte attack
The electrolyte is a mixed solution of 44.5% methanol, 5% acetylacetone and 5g tetramethyl ammonium chloride, the sample is an anode, the stainless steel plate is a cathode, the constant voltage is 12V, and the current changes according to the size of the sample; erosion is to etch away the iron matrix, exposing the precipitates;
(5) Carbon film
Fixing the sample on a sample table by using 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 2.4X103 Pa; the carbon spraying uses a high-purity carbon rod, the carbon rods at two sides are electrified and contacted, the current is controlled to be about 30A, the carbon rod is heated and volatilized, a thin carbon film is formed on the surface of a sample, and the carbon film can adsorb exposed precipitates; after the carbon spraying is finished, the vacuum degree is restored to the atmospheric pressure, and the sample is taken out;
(6) Carbon removal film
The carbon removal 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, firstly, the carbon film is divided into small squares by tweezers, so that the film is removed conveniently; sucking the carbon film out of the solution by a suction pipe after stripping, and cleaning; the cleaning solution is a diluted perchloric acid alcohol solution, pure alcohol and an alcohol aqueous solution with the volume fraction of 2/3 in sequence;
(7) Carbon film for fishing
After the carbon film is cleaned, taking out the carbon film by using a 300-400 mesh nickel screen with the diameter of 3mm, adsorbing the carbon film on the nickel screen, and airing the nickel screen on dry filter paper; and finally, the nickel screen and the carbon film are put into a transmission electron microscope sample box for storage, so that the subsequent analysis of the precipitate by the transmission electron microscope is facilitated.
Compared with the prior art, the application has the beneficial technical effects that:
the application adopts a carbon copy method to prepare a silicon steel precipitate analysis sample, and solves the problem that an oxidized rust layer is easy to form on the sample surface by the existing electrolytic double-spray method.
Drawings
The application is further described with reference to the following description of the drawings.
FIG. 1 is a carbon film taken out of a nickel screen;
Detailed Description
The present application 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 (rolling direction) and 10mm (transverse direction) was cut on the hot rolled, normalized and decarburized annealed sheet.
(2) Polishing
Coarse sandpaper No. 50 is coarsely ground, and fine sandpaper No. 280 and No. 400 is finely ground.
(3) Physical polishing
Polishing on a metallographic polishing machine.
(4) Electrolyte attack
The electrolyte was a mixed solution of 44.5% methanol, 5% acetylacetone and 5g tetramethylammonium chloride, the sample was an anode, the stainless steel plate was a cathode, the constant voltage was 12V, and the current was varied according to the sample size. Erosion is to etch away the iron matrix, exposing the precipitates.
(5) Carbon film
The sample was fixed on a sample stage with a double-sided tape, and carbon spraying was performed with a multifunctional sample surface treatment machine (carbon spraying instrument). The carbon spraying pretreatment machine is vacuumized, and carbon spraying is carried out when the vacuum degree reaches about 2.4X103 Pa. The carbon spraying uses high-purity carbon rods, the carbon rods at two sides are electrified and contacted, the current is controlled to be about 30A, the carbon rods are heated and volatilized, a thin carbon film is formed on the surface of a sample, and the carbon film can adsorb exposed precipitates. After the end of the carbon spraying, the vacuum was restored to atmospheric pressure, and the sample was taken out.
(6) Carbon removal film
The carbon removal 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 changes 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 film is removed conveniently. After the stripping, the carbon film was sucked out of the solution with a suction tube and washed. The cleaning solution is diluted perchloric acid alcohol solution, pure alcohol and 2/3 volume fraction alcohol water solution in sequence. On one hand, the electrolytic solution on the surface of the carbon film is cleaned, and on the other hand, the carbon film is slowly diffused and is not cracked.
(7) Carbon film for fishing
And after the carbon film is cleaned, taking out the carbon film by using a 300-400 mesh nickel screen with the diameter of 3mm, adsorbing the carbon film on the nickel screen, and putting the nickel screen on dry and clean filter paper for airing. And finally, the nickel screen and the carbon film are put into a transmission electron microscope sample box for storage, so that the subsequent analysis of the precipitate by the transmission electron microscope is facilitated.
Silicon steel precipitates are difficult to analyze, and the morphology, size, type and distribution of the precipitates need to be observed on a transmission electron microscope. The sample preparation process is also relatively difficult, and the current common sample preparation method for analyzing the steel precipitate is to prepare a film sample by electrolysis double spraying, so that the prepared sample is extremely easy to oxidize due to the specificity of silicon steel components, and the subsequent analysis of the precipitate is seriously influenced. The embodiment of the application adopts a replica method, the matrix is eroded to expose the precipitate, a thin carbon film is formed by carbon spraying, the precipitate is adsorbed out, and the carbon film is observed by a transmission electron microscope, so that the problem of sample oxidation is solved.
The above embodiments are only illustrative of the preferred embodiments of the present application and are not intended to limit the scope of the present application, and various modifications and improvements made by those skilled in the art to the technical solutions of the present application should fall within the protection scope defined by the claims of the present application without departing from the design spirit of the present application.
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 a thickness of 15mm in the rolling direction and 10mm in the transverse direction on a hot rolled, normalized and decarburized annealed plate;
(2) Polishing
Coarse grinding is carried out on No. 50 coarse sand paper, and then fine grinding is carried out on No. 280 fine sand paper and No. 400 fine sand paper;
(3) Physical polishing
Polishing on a metallographic polishing machine;
(4) Electrolyte attack
The electrolyte is a mixed solution of 44.5% methanol, 5% acetylacetone and 5g tetramethyl ammonium chloride, the sample is an anode, the stainless steel plate is a cathode, the constant voltage is 12V, and the current changes according to the size of the sample; erosion is to etch away the iron matrix, exposing the precipitates;
(5) Carbon film
Fixing the sample on a sample table by using 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 2.4X103 Pa; the carbon spraying uses a high-purity carbon rod, the carbon rods at two sides are electrified and contacted, the current is controlled to be about 30A, the carbon rod is heated and volatilized, a thin carbon film is formed on the surface of a sample, and the carbon film can adsorb exposed precipitates; after the carbon spraying is finished, the vacuum degree is restored to the atmospheric pressure, and the sample is taken out;
(6) Carbon removal film
The carbon removal 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, firstly, the carbon film is divided into small squares by tweezers, so that the film is removed conveniently; sucking the carbon film out of the solution by a suction pipe after stripping, and cleaning; the cleaning solution is a diluted perchloric acid alcohol solution, pure alcohol and an alcohol aqueous solution with the volume fraction of 2/3 in sequence;
(7) Carbon film for fishing
After the carbon film is cleaned, taking out the carbon film by using a 300-400 mesh nickel screen with the diameter of 3mm, adsorbing the carbon film on the nickel screen, and airing the nickel screen on dry filter paper; and finally, the nickel screen and the carbon film are put into a transmission electron microscope sample box for storage, so that the subsequent analysis of the precipitate by the transmission electron microscope is facilitated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 CN114459854A (en) | 2022-05-10 |
| CN114459854B true 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 |
|---|
| 硅钢中析出物的尺寸分布以及体积分数的测定;马红旭, 李友国;材料科学与工程(第03期);全文 * |
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