CN113533405B - Method for observing Al5FeSi phase in aluminum-silicon coating original plate alloy layer - Google Patents
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- CN113533405B CN113533405B CN202110851433.8A CN202110851433A CN113533405B CN 113533405 B CN113533405 B CN 113533405B CN 202110851433 A CN202110851433 A CN 202110851433A CN 113533405 B CN113533405 B CN 113533405B
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Abstract
The invention provides Al in an Al-Si coating original plate alloy layer 5 The observation method of the FeSi phase specifically comprises the following steps: (1) preparing a sample; (2) chemical corrosion: putting the sample prepared in the step (1) into a corrosive liquid for chemical corrosion, wherein the corrosive liquid is prepared from a stannous chloride aqueous solution, a hydrochloric acid aqueous solution and a sodium chloride aqueous solution; (3) cleaning; (4) scanning electron microscope observation and thermoelectric spectrometer determination: observation of Al by scanning Electron microscope 5 The morphology, size and distribution of FeSi phase, and Al is measured by a thermal spectrometer 5 Atomic ratio of each element of the FeSi phase. The method provided by the invention can obtain complete and clear Al 5 The three-dimensional structure of FeSi phase can fully display Al in the Al-Si coating original plate alloy layer 5 The morphology, size distribution and growth condition of the FeSi phase can accurately determine the Al 5 The atomic ratio of each element in the FeSi phase has the characteristics of low detection cost, rapidness, simplicity and accuracy.
Description
Technical Field
The invention belongs to the technical field of metal coating detection, and particularly relates to Al in an Al-Si coating original plate alloy layer 5 Method for observing FeSi phase.
Background
Because the aluminum silicon coated steel plate has good oxidation resistance and corrosion resistance, the research and development and the application of the product are increasingly wide, and the requirements on the physical properties of the product are also increasingly improved.
At present, the research aiming at the phase structure of the aluminum-plated silicon coating mainly stays on the phase structure of the aluminum-silicon layer, and the research on the phase structure, the appearance and the proportion of each phase in the alloy layer is less.
Investigating the phase structure of alloy layers, including Al 5 The three-dimensional morphology of the FeSi phase and the components of the phase have important significance for guiding the process improvement and improving the product quality. When the steel plate is put into a pot, the alloy layer is firstly generated on the surface of the steel plate, and the condition of each phase in the alloy layer can directly reflect the production process. The composition of the phases is generally determined by XRD, which is expensive, and therefore a simple and practical method for displaying and observing the phases in the Al-Si coating alloy layer is urgently needed.
The method provided by the invention creates Al in the Al-Si coating alloy layer 5 The three-dimensional morphology analysis of the FeSi phase structure changes the tradition that the research on the coating structure is mainly focused on the aluminum silicon layer, and leads the research on the coating phase structure to enter a deeper stage.
Disclosure of Invention
The invention aims to solve the technical problem of providing Al in an Al-Si coating original plate alloy layer 5 The observation method of FeSi phase can obtain complete and clear Al 5 A FeSi phase three-dimensional structure, and can fully display Al 5 The growth condition of the FeSi phase, and has the characteristics of low detection cost, rapidness, simplicity and accuracy.
In order to solve the technical problems, the invention adopts the technical scheme that:
an observation method of an Al5FeSi phase in an Al-Si coating original plate alloy layer comprises sample preparation, chemical corrosion, cleaning, scanning electron microscope observation and energy spectrometer determination, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coated steel plate, cutting a part of the aluminum-silicon coated steel plate to be used as a sample, and sequentially carrying out inlaying and polishing treatment on the sample;
(2) chemical corrosion: putting the sample prepared in the step (1) into an etching solution for chemical etching, wherein the etching solution is prepared from a stannous chloride aqueous solution, a hydrochloric acid aqueous solution and a sodium chloride aqueous solution;
(3) cleaning: washing the corroded sample with clear water, then putting the sample into an ultrasonic cleaner for cleaning, then washing the sample with alcohol, and then blowing the sample to dry;
(4) scanning electron microscope observation and thermoelectric spectrometer determination: observing Al by scanning electron microscope 5 The morphology, size and distribution of FeSi phase, and Al is measured by a thermal spectrometer 5 Atomic ratio of each element of the FeSi phase.
Preferably, the sample of step (1) of the present invention has a size of (15. + -.5) mm X (15. + -.5) mm.
Preferably, the specific operations of the inlaying in step (1) of the present invention are: and horizontally placing the surface of the sample coating into an inlaying machine for inlaying, wherein the inlaid sample is ensured to be completely exposed on the surface of the coating.
Preferably, the polishing process in step (1) of the present invention is specifically performed by: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent on the polishing cloth, and then performing polishing treatment at the rotating speed of the polishing machine of 600-900 revolutions per minute for less than or equal to 20 s.
Preferably, the polishing cloth in step (1) of the invention is a 200mm and 250mm pressure-sensitive adhesive wool polishing cloth.
Preferably, the particle size of the high-efficiency metallographic polishing agent in the step (1) of the invention is 0.5-2.5 μm.
Preferably, the concentration of the stannous chloride aqueous solution in the step (2) of the invention is 0.02-0.05 g/ml.
Preferably, the mass concentration of sodium chloride in the sodium chloride aqueous solution in the step (2) of the invention is 4-5%.
Preferably, the concentration of the hydrochloric acid aqueous solution in the step (2) of the present invention is 0.01% to 0.5%. .
Preferably, the corrosive liquid in the step (2) of the invention is prepared by stannous chloride aqueous solution, hydrochloric acid aqueous solution and sodium chloride aqueous solution according to the volume ratio of 0.5-2: 0.5-1.5: 1-3.
Preferably, the etching time of the chemical etching in step (2) of the present invention is 3 to 8 minutes.
Preferably, the time for rinsing with clear water in the step (3) of the present invention is 1-4 minutes, and the time for ultrasonic cleaning is 2-5 minutes.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
1. the invention provides a method for displaying and observing Al in an Al-Si coating original plate alloy layer 5 The method for the three-dimensional morphology of the FeSi phase can clearly and completely display and observe Al 5 The structure, morphology, proportion, size and distribution of the FeSi phase provide a basis for process improvement and quality improvement.
2. The method provided by the invention adopts stannous chloride aqueous solution, hydrochloric acid aqueous solution and NaCl aqueous solution as aggressive agents, and can clearly and completely display Al in the Al-Si coating alloy layer 5 A FeSi phase.
3. The method provided by the invention has the characteristics of low detection cost, rapidness, simplicity and accuracy.
Drawings
FIG. 1 is the observation result of the scanning electron microscope of example 1;
FIG. 2 shows the results of the measurement by the thermal spectrometer of example 1;
FIG. 3 shows the observation results of the scanning electron microscope of example 2;
FIG. 4 is the results of the thermal spectrometer measurements of example 2;
FIG. 5 shows the observation results of the scanning electron microscope of example 3;
FIG. 6 shows the results of the measurement of the thermoelectric spectrometer of example 3.
Detailed Description
The technical solutions of the present invention will be described in detail and fully with reference to the accompanying drawings and examples, and it should be understood that the described examples are only a part of the examples, but not all of the examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for observing an Al5FeSi phase in an Al-Si coating original plate alloy layer, which comprises the steps of sample preparation, chemical corrosion, cleaning, scanning electron microscope observation and energy spectrometer determination, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coated steel plate, cutting a part of the aluminum-silicon coated steel plate to be used as a sample, and sequentially carrying out inlaying and polishing treatment on the sample;
(2) chemical corrosion: putting the sample prepared in the step (1) into a corrosive liquid for chemical corrosion, wherein the corrosive liquid is prepared from a stannous chloride aqueous solution, a hydrochloric acid aqueous solution and a sodium chloride aqueous solution;
(3) cleaning: washing the corroded sample with clear water, then putting the sample into an ultrasonic cleaner for cleaning, then washing the sample with alcohol, and then blowing the sample to dry;
(4) scanning electron microscope observation and thermoelectric spectrometer determination: observing Al by scanning electron microscope 5 The morphology, size and distribution of FeSi phase, and Al is measured by a thermal spectrometer 5 Atomic ratio of each element of the FeSi phase.
In some embodiments of the invention, the sample in step (1) has a size of (15 ± 5) mm × (15 ± 5) mm (e.g. may be 10mm × 10mm, 12mm × 13mm, 15mm × 15mm, 18mm × 15mm, 20mm × 20 mm).
In some embodiments of the present invention, the specific operations of inlaying in the step (1) are: and horizontally placing the surface of the sample coating into an inlaying machine for inlaying, wherein the inlaid sample is ensured to be completely exposed on the surface of the coating.
In some embodiments of the present invention, the specific operation of the polishing treatment in step (1) is: water and a high-efficiency metallographic polishing agent are uniformly sprayed on the polishing cloth in sequence, and then polishing treatment is carried out at the rotation speed of 600-900 rpm (for example, 600 rpm, 700 rpm, 800 rpm and 00 rpm) of a polishing machine, wherein the polishing time is less than or equal to 20s (for example, 20s, 19s, 18s, 17s, 16s and 15 s).
In some embodiments of the invention, the polishing cloth in step (1) is a 200mm, 250mm pressure sensitive latex cloth.
In some embodiments of the invention, the particle size of the high efficiency metallurgical polishing agent in step (1) is 0.5-2.5 μm (e.g., may be 0.5 μm, 1 μm, 1.5 μm, 2 μm, 2.5 μm).
In some embodiments of the invention, the concentration of the stannous chloride aqueous solution in step (2) is 0.02-0.05g/ml (e.g., may be 0.02g/ml, 0.03g/ml, 0.04g/ml, 0.05 g/ml).
In some embodiments of the present invention, the mass concentration of sodium chloride in the sodium chloride aqueous solution in the step (2) is 4% to 5%.
In some embodiments of the present invention, the concentration of the hydrochloric acid in the aqueous solution in the step (2) is 0.01% to 0.5% (e.g., may be 0.01%, 0.05%, 0.1%, 0.2%, 0.3%, 0.4%, 0.5%).
In some embodiments of the present invention, the corrosion solution in step (2) is prepared from stannous chloride aqueous solution, hydrochloric acid aqueous solution and sodium chloride aqueous solution in a volume ratio of 0.5-2: 0.5-1.5: 1-3 (for example, 0.5: 1, 1:1, 1.5: 1: 1.5, 2: 1.5: 2, 2: 1.5: 3).
In some embodiments of the present invention, the etching time of the chemical etching in the step (2) is 3 to 8 minutes (e.g., 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes). The etching time is related to the concentration of the etching solution, and the larger the concentration of the etching solution is, the shorter the etching time is, and correspondingly, the smaller the concentration of the etching solution is, the longer the etching time is.
In some embodiments of the present invention, the rinsing time in step (3) is 1-4 minutes, and the ultrasonic cleaning time is 2-5 minutes.
Some embodiments of the present invention will be described in detail below with reference to specific examples. The embodiments described below and the features of the embodiments can be combined with each other without conflict.
Example 1
Al in aluminum-silicon coating original plate alloy layer 5 The observation method of FeSi phase includes sample preparation and chemical reactionCorrosion, cleaning, scanning electron microscope observation and energy spectrometer determination, specifically:
(1) preparing a sample: taking an aluminum-silicon coating steel plate (1500 + AS mark), cutting a sample with the thickness of 15mm multiplied by 15mm, horizontally placing the surface of the sample coating into an inlaying machine for inlaying, completely exposing the surface of the inlaid sample coating, and then performing polishing treatment, specifically: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent with the particle size of 2.5 microns on a pressure-sensitive adhesive wool fabric polishing cloth with the particle size of 200mm, and then performing polishing treatment for 15s at the rotating speed of a polishing machine of 600 revolutions per minute.
(2) Chemical corrosion: putting the sample prepared in the step (1) into an etching solution for chemical etching, wherein the etching solution is prepared from a stannous chloride aqueous solution with the concentration of 0.03g/ml, a sodium chloride aqueous solution with the mass concentration of 4% and a hydrochloric acid aqueous solution with the volume ratio of 0.1% according to the volume ratio of 1.5: 1, and the etching time is 5 minutes;
(3) cleaning: and (3) washing the corroded sample for 1 minute by using clean water, then putting the sample into an ultrasonic cleaner for cleaning for 2 minutes, washing the sample by using alcohol, and then blowing the sample to dry.
(4) Scanning electron microscope observation and thermoelectric spectrometer determination: KYKY-EM3200 scanning electron microscope for observing Al 5 The morphology, size and distribution of the FeSi phase are shown in fig. 1. As can be seen from FIG. 1, the method provided by the invention can obtain the Al in the complete Al-Si coating original plate alloy layer 5 The three-dimensional structure of FeSi phase can fully display Al in the Al-Si coating original plate alloy layer 5 Morphology and growth of FeSi phase.
Qualitative determination of Al by thermal spectrometer 5 The atomic ratio of the elements of the FeSi phase, as shown in FIG. 2, can be determined that the structure after etching is Al 5 A FeSi phase having an atomic ratio of 5.1:1: 1.
Example 2
Al in aluminum-silicon coating original plate alloy layer 5 The observation method of the FeSi phase comprises sample preparation, chemical corrosion, cleaning, scanning electron microscope observation and energy spectrometer determination, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coating steel plate (DC 52D + AS mark), cutting a sample with the size of 20mm multiplied by 20mm, horizontally placing the surface of a sample coating into an inlaying machine for inlaying, completely exposing the surface of the inlaid sample coating, and then performing polishing treatment, wherein the method specifically comprises the following steps: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent with the particle size of 0.5 mu m on pressure-sensitive adhesive wool fabric polishing cloth with the particle size of 250mm, and then performing polishing treatment for 20s at the rotating speed of a polishing machine of 600 revolutions per minute.
(2) Chemical corrosion: putting the sample prepared in the step (1) into an etching solution for chemical etching, wherein the etching solution is prepared from a stannous chloride aqueous solution with the concentration of 0.02g/ml, a sodium chloride aqueous solution with the mass concentration of 5% and a hydrochloric acid aqueous solution with the volume ratio of 0.05% according to the volume ratio of 2: 1.5: 3, and the etching time is 3 minutes;
(3) cleaning: and (3) washing the corroded sample with clear water for 2 minutes, then putting the sample into an ultrasonic cleaner for cleaning for 3 minutes, washing the sample with alcohol, and then drying the sample by blowing.
(4) Scanning electron microscope observation and thermoelectric spectrometer determination: KYKY-EM3200 scanning electron microscope for observing Al 5 The morphology, size and distribution of the FeSi phase are shown in fig. 3. As can be seen from FIG. 3, the method provided by the present invention can obtain complete Al 5 A FeSi phase three-dimensional structure, and can fully display Al 5 Morphology and growth of FeSi phase.
Qualitative determination of Al by thermal spectrometer 5 The atomic ratio of the elements of the FeSi phase, as shown in FIG. 4, can be determined that the structure after etching is Al 5 A FeSi phase in an atomic ratio of 5.1:1.1: 1.1.
Example 3
Al in aluminum-silicon coating original plate alloy layer 5 The observation method of the FeSi phase comprises sample preparation, chemical corrosion, cleaning, scanning electron microscope observation and energy spectrometer determination, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coated steel plate (DC 51D + AS mark), cutting a sample with the thickness of 10mm multiplied by 10mm, horizontally placing the surface of a sample coating into an inlaying machine for inlaying, completely exposing the surface of the inlaid sample coating, and then performing polishing treatment, wherein the method specifically comprises the following steps: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent with the particle size of 1.5 mu m on pressure-sensitive adhesive wool fabric polishing cloth with the particle size of 200mmmm, and then performing polishing treatment for 15s at the rotating speed of a polishing machine of 900 revolutions per minute.
(2) Chemical corrosion: putting the sample prepared in the step (1) into an etching solution for chemical etching, wherein the etching solution is prepared from a stannous chloride aqueous solution with the concentration of 0.05g/ml, a sodium chloride aqueous solution with the mass concentration of 4% and a hydrochloric acid aqueous solution with the volume ratio of 0.2% according to the volume ratio of 0.5: 1, and the etching time is 8 minutes;
(3) cleaning: and (3) washing the corroded sample with clear water for 2 minutes, then putting the sample into an ultrasonic cleaner for cleaning for 3 minutes, washing the sample with alcohol, and then drying the sample by blowing.
(4) Scanning electron microscope observation and thermoelectric spectrometer determination: KYKY-EM3200 scanning electron microscope for observing Al 5 The morphology, size and distribution of the FeSi phase are shown in fig. 5. From FIG. 5, it can be seen that the method provided by the present invention can obtain complete Al 5 A FeSi phase three-dimensional structure, and can fully display Al 5 Morphology and growth of FeSi phase.
Qualitative determination of Al by thermal spectrometer 5 The atomic ratio of the elements of the FeSi phase, as shown in FIG. 6, can be determined that the structure after etching is Al 5 A FeSi phase with an atomic ratio of 5:1: 1.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. Al in aluminum-silicon coating original plate alloy layer 5 The observation method of the FeSi phase is characterized in that: the method comprises the steps of sample preparation, chemical corrosion, cleaning, scanning electron microscope observation and thermoelectric spectrometer determination, and specifically comprises the following steps:
(1) preparing a sample: taking an aluminum-silicon coated steel plate, cutting a part of the aluminum-silicon coated steel plate to be used as a sample, and then sequentially carrying out inlaying and polishing treatment on the sample;
(2) chemical corrosion: putting the sample prepared in the step (1) into a corrosive liquid for chemical corrosion, wherein the corrosive liquid is prepared from a stannous chloride aqueous solution, a hydrochloric acid aqueous solution and a sodium chloride aqueous solution;
(3) cleaning: washing the corroded sample with clear water, then putting the sample into an ultrasonic cleaner for cleaning, then washing the sample with alcohol, and then drying the sample by blowing;
(4) scanning electron microscope observation and thermoelectric spectrometer determination: observing Al by scanning electron microscope 5 The morphology, size and distribution of FeSi phase, and Al is measured by a thermal spectrometer 5 Atomic ratio of each element of the FeSi phase;
the concentration of the stannous chloride aqueous solution in the step (2) is 0.02-0.05 g/ml;
the mass concentration of sodium chloride in the sodium chloride aqueous solution in the step (2) is 4-5%;
the volume concentration of the hydrochloric acid aqueous solution in the step (2) is 0.01-0.5%;
the corrosive liquid in the step (2) is prepared by stannous chloride solution, hydrochloric acid aqueous solution and sodium chloride aqueous solution according to the volume ratio of 0.5-2: 0.5-1.5: 1-3;
the corrosion time of the chemical corrosion in the step (2) is 3-8 minutes.
2. The Al-Si coated raw plate alloy layer according to claim 1 5 The observation method of the FeSi phase is characterized in that: the concrete operations of the inlaying in the step (1) are as follows: and horizontally placing the surface of the sample coating into an inlaying machine for inlaying, wherein the inlaid sample is ensured to be completely exposed on the surface of the coating.
3. The Al alloy layer of claim 1 5 The observation method of the FeSi phase is characterized in that: the polishing treatment in the step (1) comprises the following specific operations: and (3) sequentially and uniformly spraying water and a high-efficiency metallographic polishing agent on the polishing cloth, and then performing polishing treatment at the rotating speed of the polishing machine of 600-900 revolutions per minute for less than or equal to 20 s.
4. Al in Al-Si coated raw sheet alloy layer according to claim 3 5 The observation method of the FeSi phase is characterized in that: the polishing cloth in the step (1) is pressure-sensitive adhesive wool fabric polishing cloth with the thickness of 200mm and 250 mm.
5. Al in Al-Si coated raw sheet alloy layer according to claim 3 5 The observation method of the FeSi phase is characterized in that: the particle size of the high-efficiency metallographic polishing agent in the step (1) is 0.5-2.5 mu m.
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