CN114878568A - Metallographic phase display method of AlNd alloy - Google Patents
Metallographic phase display method of AlNd alloy Download PDFInfo
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Abstract
The invention relates to a metallographic display method of AlNd alloy, belonging to the technical field of metallographic detection and analysis. The method comprises the following steps: forming a first polishing surface; mechanically polishing the first polishing surface by using a polishing agent to form a second polishing surface; placing the stainless steel as a cathode and the second polished surface as an anode in a fluoboric acid aqueous solution for anode coating to form a display surface; wherein the fluoroboric acid aqueous solution consists of 5.5g of boric acid, 15ml of 49% hydrofluoric acid and 480ml of pure water. The anode coating process is carried out in a fluoboric acid aqueous solution, a layer of anisotropic oxide film is coated on the surface of the AlNd alloy, the oxide film has thickness difference, and crystal grains in different phases of the oxide film have obvious chromatic aberration under polarized light illumination, so that a clear AlNd metallographic structure can be obtained.
Description
Technical Field
The invention relates to a metallographic display method of AlNd alloy, belonging to the technical field of metallographic detection and analysis.
Background
The AlNd alloy is applied to the liquid crystal display screen, and the film of the AlNd alloy as a TFT electrode conducting layer has good resistivity and etching performance and higher substrate combination rate. However, specific textures and high purity and density are required for the target to perform its function. At present, the EBSD analysis can obtain AlNd texture information and metallographic structure information, but the obtaining of an AlNd metallographic specimen without strain and a fuzzy layer is a difficult point.
At present, two preparation methods for preparing the metallographic phase of aluminum and aluminum alloy are generally adopted, firstly, a method of mechanical polishing and chemical corrosion is adopted, but a strain layer and a paste layer are easy to appear in the preparation process of the method, and particularly, the chemical corrosion of a sample is difficult to perform because Nd is one of the most active rare earth elements and has high activity. And secondly, by adopting a method of electropolishing and anodic coating, although the prepared sample can eliminate a strain layer and a fuzzy layer, the preparation method is complicated, the electrolyte is generally high-risk liquid such as phosphoric acid, perchloric acid and the like, the risk of ignition and even explosion is easily caused by temperature change in the electrolytic process, and the electrolyte is difficult to recover.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a metallographic display method of AlNd alloy, which can obtain a clear AlNd metallographic structure.
In order to achieve the purpose, the invention adopts the technical scheme that: the metallographic display method of the AlNd alloy comprises the following steps:
(1) polishing: sequentially polishing the surface of the AlNd alloy by using 600-mesh, 1200-mesh and 2500-mesh water-based sand paper to form a first polishing surface;
(2) polishing: mechanically polishing the first polishing surface by using a polishing agent to form a second polishing surface;
(3) anode film coating: placing the stainless steel as a cathode and the second polished surface as an anode in a fluoboric acid aqueous solution for anode coating to form a display surface; wherein the fluoroboric acid aqueous solution consists of 5.5g of boric acid, 15ml of 49% hydrofluoric acid and 480ml of pure water;
(4) and (3) metallographic observation: the display surface was observed using a metallographic microscope.
According to the technical scheme, after grinding, the formed first polishing surface is mechanically polished, then the second polishing surface obtained by mechanical polishing is subjected to anode film coating, and the anode film coating process is carried out in a fluoboric acid aqueous solution. The anodic coating is a process of forming various different films on the surface of a sample under a certain electrical system through an electrolyte solution, and is different from chemical corrosion, wherein the electrochemical reaction can be generated when the anodic coating is etched by a chemical reagent due to different physicochemical properties and different free energies of crystal grains in metal and alloy among the crystal grains, intra-crystal and grain boundaries and among phases, and the interface or phase corrosion is finally caused. The scratches on the first polishing surface can be effectively removed by adopting mechanical polishing, so that the smooth brightness of the formed second polishing surface is improved. The improvement of the smoothness of the second polishing surface is beneficial to the corrosion of the fluoroboric acid aqueous solution to the crystal boundary position in the second polishing surface, and the result of metallographic phase display is improved. The fluoboric acid aqueous solution can not be influenced by temperature to generate danger in the electrolytic process, and meanwhile, a film with thickness difference is formed on the surface of the AlNd alloy in the fluoboric acid aqueous solution, so that obvious color difference is achieved, and the metallographic display result is favorably improved.
Alternatively, the AlNd alloy sample obtained by cutting out a portion from the AlNd alloy material by means of, for example, a hand saw, a sawing machine, or a cutting machine may be processed on the AlNd alloy before grinding. The size of the AlNd alloy sample is suitable for the subsequent process. In the process of obtaining the AlNd alloy sample, attention is paid to the temperature condition of the AlNd alloy sample, and the AlNd alloy sample is cooled by water in the process of obtaining the AlNd alloy sample if necessary, so that the metallographic structure of the AlNd alloy sample is prevented from being changed due to the overhigh temperature.
In the polishing stage, the coarse grinding abrasive paper is selected and ground by using No. 600 water-based abrasive paper, the selection mesh is too small, the abrasion of the test sample is large, the surface of the test sample is too rough, and the strain layer is too large. The selected sand paper has an excessively large mesh, and the grinding efficiency of the sample is reduced. The 2500# water-based abrasive paper is selected for polishing the fine grinding abrasive paper, and the abrasive paper with the mesh number has a good grinding effect on the AlNd alloy and ensures a low roughness value of the surface of the sample.
Optionally, in the step (3), the parameters of the anodic coating are: the anode coating voltage is 8-12V, the anode coating current is 0.9-1.2A, and the anode coating time is 2-5 min.
In the anode film coating process, a stable oxide film is difficult to form on the second polished surface due to the excessively low voltage or current and the excessively short film coating time; and the second polished surface has obvious electrolysis phenomenon due to the overhigh current voltage, so that the state of the second polished surface is fuzzy.
Optionally, in the step (2), the step of mechanically polishing is: and mechanically polishing the first polishing surface by using wool fabric polishing cloth and matching with a diamond polishing agent.
The first polished surface has scratches and therefore needs to be mechanically polished to obtain a smooth and flat second polished surface. The wool fabric polishing cloth has a good polishing effect on soft materials, the diamond polishing agent can reduce scratches of the first polishing surface, and the polishing cloth and the polishing agent are matched for use, so that the smoothness and the flatness of the second polishing surface can be further improved.
Optionally, in the step (2), the rotation speed of the mechanical polishing is 250-350r/min, and the polishing time of each surface is 1-8 min.
In the mechanical polishing process, the polishing effect is poor and the surface smoothness is poor due to too short polishing time; the polishing time of the process results in smearing of the second polished surface.
Optionally, the diamond polishing agent has a particle size of 2.5 μm.
Optionally, in the step (1), the grinding rotation speed is 400r/min, and the grinding time of each surface is 1-3 min.
The AlNd alloy surface has a natural oxidation layer, and the presence of the natural oxidation layer hinders the display of grain boundaries. And the polishing is used for removing the natural oxide layer on the surface of the AlNd alloy to expose the surface of the AlNd alloy and form a first polishing surface. In addition, the polishing can also be used for improving the flatness of the surface of the AlNd alloy so as to form a flat and bright first polished surface.
If the polishing time is too short, the natural oxide layer on the surface of the surface to be displayed cannot be completely removed, so that the subsequent display of the grain boundary is hindered; if the polishing time is too long, it causes a problem of material waste and increased process difficulty.
Optionally, the water-based sandpaper is made of silicon carbide.
Optionally, one or more cleaning treatments are performed between any two steps of grinding, mechanical polishing, anodizing, and metallographic observation.
The cleaning process may remove residues generated during the process. Specifically, the cleaning treatment includes: the cleaning treatment is performed by means of a cleaning treatment agent rinse. Wherein the cleaning treatment agent comprises water and absolute ethyl alcohol.
In the invention, after polishing and before mechanical polishing, the first polished surface is subjected to first cleaning treatment by using water, so that abrasive dust generated in the polishing process is cleared, and the abrasive dust is prevented from entering the next process. After the first cleaning treatment, drying treatment is performed by cold air blow-drying.
After the mechanical polishing, before the anodic coating, the metallographic display method further includes: and sequentially carrying out second cleaning treatment on the obtained second polishing surface by adopting pure water and absolute ethyl alcohol, so as to remove the polishing agent remained on the surface of the second polishing surface and prevent the polishing agent from polluting subsequent processes. And after the second cleaning treatment, drying treatment is carried out by cold air blow drying.
After the anode is coated with the film, the obtained display surface is sequentially subjected to third cleaning treatment by sequentially adopting pure water and absolute ethyl alcohol, and after the third cleaning treatment, drying treatment is carried out by drying through cold air blowing.
Compared with the prior art, the invention has the beneficial effects that: according to the technical scheme, after grinding, the formed first polishing surface is mechanically polished, then the second polishing surface obtained through mechanical polishing is subjected to anodic coating, the anodic coating process is carried out in a fluoboric acid aqueous solution, a layer of anisotropic oxide film is coated on the surface of the AlNd alloy, the oxide film has thickness difference, and crystal grains of different phases of the oxide film have obvious chromatic aberration under polarized illumination, so that a clear AlNd metallographic structure can be obtained. The scratches on the first polishing surface can be effectively removed by adopting mechanical polishing, so that the smooth brightness of the formed second polishing surface is improved. The improvement of the smoothness of the second polishing surface is beneficial to the corrosion of the fluoroboric acid aqueous solution to the crystal boundary position in the second polishing surface, and the result of metallographic phase display is improved. The fluoboric acid aqueous solution can not be influenced by temperature to generate danger in the electrolytic process, and meanwhile, a film with thickness difference is formed on the surface of the AlNd alloy in the fluoboric acid aqueous solution, so that obvious color difference is achieved, and the metallographic display result is favorably improved.
Drawings
FIG. 1 is a view showing a metallographic structure of an AlNd alloy in example 1;
FIG. 2 is a view showing a metallographic structure of an AlNd alloy in example 2;
FIG. 3 is a view showing a metallographic structure of an AlNd alloy in comparative example 1;
FIG. 4 is a representation of a second polished surface of the AlNd alloy of comparative example 2;
FIG. 5 is a representation of a second polished surface of the AlNd alloy of comparative example 3;
FIG. 6 is a graph showing the AlNd alloy of comparative example 4 after vibratory finishing;
fig. 7 is a view showing a metallographic structure of an AlNd alloy in comparative example 4.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the following detailed description and accompanying drawings.
In the following examples and comparative examples, the water-based sandpaper is made of silicon carbide.
Example 1
In the present example, the content of Nd in the AlNd alloy was 5%, and the content of Al was 95%.
The embodiment relates to a metallographic display method of an AlNd alloy, which comprises the following steps:
(1) sampling: cutting the AlNd alloy into AlNd alloy samples of 15x15x15mm by using a water cutting machine, wherein the surfaces of the AlNd alloy samples are required to be flat;
(2) polishing: sequentially polishing the surface of the AlNd alloy by using 600-mesh, 1200-mesh and 2500-mesh water-based sand paper until the surface of the AlNd alloy sample is flat and the scratch directions are consistent, so as to form a first polishing surface; wherein the grinding rotating speed is 400r/min, the grinding time is 2min each time, after grinding, the first grinding surface is washed by tap water, and then the first grinding surface is dried by a blower with cold air;
(3) polishing: mechanically polishing the first polishing surface by using wool fabric polishing cloth and matching with a diamond polishing agent with 2.5 mu m abrasive particles to form a second polishing surface; wherein the rotation speed of mechanical polishing is 300r/min, and the time of mechanical polishing is 4 min; after the mechanical polishing is finished, washing the second polishing surface by using pure water and absolute ethyl alcohol in sequence, and then drying by using a blower with cold air;
(4) anode film coating: and (3) placing the stainless steel as a cathode and the second polished surface as an anode in a fluoboric acid aqueous solution for anode film coating, wherein the parameters of the anode film coating are as follows: the anode film coating voltage is 10V, the anode film coating current is 1A, and the anode film coating time is 4min to form a display surface; wherein the fluoroboric acid aqueous solution consists of 5.5g of boric acid, 15ml of 49% hydrofluoric acid and 480ml of pure water; after the anode film covering is finished, washing the display surface by using pure water and absolute ethyl alcohol in sequence, and then drying by using a blower with cold air;
(5) and (3) metallographic observation: and observing the display surface by using a metallographic microscope, shooting a picture of the display surface, marking crystal grains, and counting the sizes of the crystal grains.
The metallographic structure of the AlNd alloy of this example is shown in fig. 1, and it can be seen that the grain boundaries of the metallographic structure of the AlNd alloy are clear, and the grain size is about 100 μm.
Example 2
In the AlNd alloy of the present example, the content of Nd was 3% and the content of Al was 97%.
The embodiment relates to a metallographic display method of an AlNd alloy, which comprises the following steps:
(1) sampling: cutting the AlNd alloy into AlNd alloy samples of 15x15x15mm by using a water cutting machine, wherein the surfaces of the AlNd alloy samples are required to be flat;
(2) polishing: sequentially polishing the surface of the AlNd alloy by using 600-mesh, 1200-mesh and 2500-mesh water-based sand paper until the surface of the AlNd alloy sample is flat and the scratch directions are consistent, so as to form a first polishing surface; wherein the grinding rotating speed is 400r/min, the grinding time is 3min each time, after grinding is finished, the first grinding surface is washed by tap water, and then the first grinding surface is dried by a blower with cold air;
(3) polishing: mechanically polishing the first polishing surface by using wool fabric polishing cloth and matching with a diamond polishing agent with 2.5 mu m abrasive particles to form a second polishing surface; wherein the rotation speed of mechanical polishing is 250r/min, and the time of mechanical polishing is 5 min; after the mechanical polishing is finished, washing the second polishing surface by using pure water and absolute ethyl alcohol in sequence, and then drying by using a blower with cold air;
(4) anode film coating: and (3) placing the stainless steel as a cathode and the second polished surface as an anode in a fluoboric acid aqueous solution for anode film coating, wherein the parameters of the anode film coating are as follows: the anode film coating voltage is 8V, the anode film coating current is 1.2A, and the anode film coating time is 5min to form a display surface; wherein the fluoroboric acid aqueous solution consists of 5.5g of boric acid, 15ml of 49% hydrofluoric acid and 480ml of pure water; after the anode film covering is finished, washing the display surface by using pure water and absolute ethyl alcohol in sequence, and then drying by using a blower with cold air;
(5) and (3) metallographic observation: and observing the display surface by using a metallographic microscope, shooting a picture of the display surface, marking the crystal grains, and counting the sizes of the crystal grains.
The metallographic structure diagram of the AlNd alloy in the example is shown in fig. 2, and it can be seen that the grain boundary of the metallographic structure of the AlNd alloy is clear, the grains are uniform, and the size of the grains is about 100 μm; and the grain boundary of the AlNd alloy with lower Nd content is finer.
Example 3
In the present example, the content of Nd in the AlNd alloy was 5%, and the content of Al was 95%.
The embodiment relates to a metallographic display method of an AlNd alloy, which comprises the following steps:
(1) sampling: cutting the AlNd alloy into AlNd alloy samples of 15x15x15mm by using a water cutting machine, wherein the surfaces of the AlNd alloy samples are required to be flat;
(2) polishing: sequentially polishing the surface of the AlNd alloy by using 600-mesh, 1200-mesh and 2500-mesh water-based sand paper until the surface of the AlNd alloy sample is flat and the scratch directions are consistent, so as to form a first polishing surface; wherein the grinding rotating speed is 400r/min, the grinding time is 1min each time, after grinding is finished, the first grinding surface is washed by tap water, and then the first grinding surface is dried by a blower with cold air;
(3) polishing: mechanically polishing the first polishing surface by using wool fabric polishing cloth and matching with a diamond polishing agent with 2.5 mu m abrasive particles to form a second polishing surface; wherein the rotation speed of mechanical polishing is 350r/min, and the time of mechanical polishing is 3 min; after the mechanical polishing is finished, washing the second polishing surface by using pure water and absolute ethyl alcohol in sequence, and then drying by using a blower with cold air;
(4) anode film coating: and (3) placing the stainless steel as a cathode and the second polished surface as an anode in a fluoboric acid aqueous solution for anode film coating, wherein the parameters of the anode film coating are as follows: the anode film coating voltage is 12V, the anode film coating current is 0.9A, and the anode film coating time is 2min, so that a display surface is formed; wherein the fluoroboric acid aqueous solution consists of 5.5g of boric acid, 15ml of 49% hydrofluoric acid and 480ml of pure water; after the anode film covering is finished, washing the display surface by using pure water and absolute ethyl alcohol in sequence, and then drying by using a blower with cold air;
(5) and (3) metallographic observation: and observing the display surface by using a metallographic microscope, shooting a picture of the display surface, marking crystal grains, and counting the sizes of the crystal grains.
The metallographic structure of the AlNd alloy of this example shows that the grain boundaries of the metallographic structure of the AlNd alloy are clear, and the grain size is about 100 μm.
Comparative example 1
In the comparative example, the content of Nd in the AlNd alloy was 5%, and the content of Al was 95%.
The comparative example relates to a metallographic display method of an AlNd alloy, which comprises the following steps:
(1) sampling: cutting the AlNd alloy into AlNd alloy samples of 15x15x15mm by using a water cutting machine, wherein the surfaces of the AlNd alloy samples are required to be flat;
(2) polishing: sequentially polishing the surface of the AlNd alloy by using 600-mesh, 1200-mesh and 2500-mesh water-based sand paper until the surface of the AlNd alloy sample is flat and the scratch directions are consistent, so as to form a first polishing surface; wherein the grinding rotating speed is 400r/min, the grinding time is 2min each time, after grinding, the first grinding surface is washed by tap water, and then the first grinding surface is dried by a blower with cold air;
(3) polishing: mechanically polishing the first polishing surface by using wool fabric polishing cloth and matching with a diamond polishing agent with 2.5 mu m abrasive particles to form a second polishing surface; wherein the rotation speed of mechanical polishing is 300r/min, and the time of mechanical polishing is 4 min; after the mechanical polishing is finished, washing the second polishing surface by using pure water and absolute ethyl alcohol in sequence, and then drying by using a blower with cold air;
(4) chemical corrosion: placing the AlNd alloy sample after mechanical polishing in a Kaile reagent, and corroding the second polished surface for 5min to form a display surface; after the chemical corrosion is finished, washing the display surface by using pure water and absolute ethyl alcohol in sequence, and then drying by using a blower with cold air;
(5) and (3) metallographic observation: and observing the display surface by using a metallographic microscope, shooting a picture of the display surface, marking crystal grains, and counting the sizes of the crystal grains.
As shown in fig. 3, the metallographic structure of the AlNd alloy of this example showed that grain boundaries of the metallographic structure of the AlNd alloy were blurred, and it was difficult to mark the grain size.
Comparative example 2
As a comparative example of the metallographic display method of an AlNd alloy according to the present invention, the only difference between this comparative example and example 1 was that in the step (3), the mechanical polishing time was 1 min.
The second polished surface is observed by using a metallographic microscope, and the result is shown in fig. 4, and it can be seen from fig. 4 that the second polished surface has poor smoothness, which indicates that the polishing effect is poor due to too short polishing time, and is not favorable for the subsequent process.
Comparative example 3
As a comparative example of the metallographic display method of an AlNd alloy according to the present invention, the only difference between this comparative example and example 1 was that in the step (3), the mechanical polishing time was 8 min.
The second polished surface is observed by using a metallographic microscope, and the result is shown in fig. 5, and it can be seen from fig. 5 that the second polished surface has a tailing phenomenon due to an excessively long polishing time, which is not favorable for the subsequent process.
Comparative example 4
In the present example, the content of Nd in the AlNd alloy was 5%, and the content of Al was 95%.
This comparative example shows the crystalline phase of AlNd alloy using the method of example 1 in the CN201410223760 patent.
In the step of vibration polishing, the vibration polishing process is complex, consumes long time and needs 3 hours; the surface view of the AlNd alloy after vibration polishing is shown in fig. 6, and it can be seen from fig. 6 that the vibration polishing step in CN201410223760 patent has poor AlNd polishing effect.
As shown in fig. 7, the crystal phase surface of the AlNd alloy after the anodic coating was observed to be blurred in the grain boundaries of the AlNd alloy metallographic structure and to make it difficult to mark the grain size in fig. 7.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. A metallographic display method of AlNd alloy is characterized by comprising the following steps:
(1) polishing: sequentially polishing the surface of the AlNd alloy by using 600-mesh, 1200-mesh and 2500-mesh water-based sand paper to form a first polishing surface;
(2) polishing: mechanically polishing the first polishing surface by using a polishing agent to form a second polishing surface;
(3) anode film coating: placing the stainless steel as a cathode and the second polished surface as an anode in a fluoboric acid aqueous solution for anode coating to form a display surface; wherein the fluoroboric acid aqueous solution consists of 5.5g of boric acid, 15ml of 49% hydrofluoric acid and 480ml of pure water;
(4) and (3) metallographic observation: the display surface was observed using a metallographic microscope.
2. The method for metallographic representation of AlNd alloy according to claim 1, wherein in said step (3), the parameters of the anodic coating are: the anode coating voltage is 8-12V, the anode coating current is 0.9-1.2A, and the anode coating time is 2-5 min.
3. The method for metallographic representation of AlNd alloy according to claim 1, wherein said step (2), the step of mechanical polishing, is: and mechanically polishing the first polishing surface by using wool fabric polishing cloth and matching with a diamond polishing agent.
4. The method for metallographic representation of an AlNd alloy according to claim 3, wherein in said step (2), the rotation speed of the mechanical polishing is 250-.
5. A metallographic display method according to claim 3, wherein said diamond polishing agent has a particle size of 2.5 μm.
6. The method for metallographic representation of AlNd alloy according to claim 1, wherein in step (1), the rotational speed of polishing is 400r/min and the polishing time per surface is 1 to 3 min.
7. The method for displaying the metallographic phase of an AlNd alloy according to claim 1, wherein the water-based sand paper is made of silicon carbide.
8. A metallographic display method according to claim 1, wherein said cleaning is carried out one or more times between any two of the steps of grinding, mechanical polishing, anodizing and metallographic observation.
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