Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for displaying a pure tin metallographic phase.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for displaying a pure tin metallographic phase comprises the following steps:
providing a pure tin sample to be detected;
sequentially polishing the surface of the pure tin sample to be detected by adopting first water-based abrasive paper, second water-based abrasive paper and third water-based abrasive paper to form a first polished surface, wherein the grain sizes of the first water-based abrasive paper, the second water-based abrasive paper and the third water-based abrasive paper are sequentially increased;
carrying out first electrolytic polishing on the first polished surface by using first electrolytic polishing liquid to form a second polished surface, wherein the first electrolytic polishing liquid is HClO4And ethanol, wherein the direct current electrolytic voltage of the first electrolytic polishing is 25-30V, and the time of the first electrolytic polishing is 50-70 s;
carrying out second electrolytic polishing on the second polished surface by using second electrolytic polishing liquid to form a display surface of a pure tin metallographic phase, wherein the second electrolytic polishing liquid is HClO4And ethanol, wherein the direct current electrolytic voltage of the second electrolytic polishing is 6-10V, and the time of the second electrolytic polishing is 15-25 s.
At present, a metallographic sample of tin is obtained mainly by mechanical grinding and mechanical polishing, and a deformation layer is easily formed due to low hardness and recrystallization temperature of pure tin, so that the tin and the tin alloy are easy to cause a deformation layer, a pseudo structure, a twin crystal and the like which interfere with metallographic judgment in the sample preparation process. In metallographic phase preparation, silicon carbide in sandpaper is easily embedded during grinding and a polishing agent is easily embedded during polishing, resulting in difficulty in polishing the sample into a mirror image and a considerable time consumption in the polishing stage. The method can obtain the non-deformation tin-gold phase sample in a short time by adopting electrolytic polishing, thereby greatly improving the metallographic preparation efficiency.
Chemical corrosion is generally adopted in the current tin metallographic corrosion stage, the obtained metallographic structure is not clear enough, the corrosion process is difficult to control, and the experimental reproducibility is low. The mechanical polishing most commonly adopted in the pure tin polishing stage is optimized into first electrolytic polishing; the chemical corrosion adopted by the pure tin metallographic appearance mode is optimized to be the second electrolytic polishing. The method for displaying the pure tin metallographic phase disclosed by the invention combines the first electrolytic polishing and the second electrolytic polishing, can realize the polishing of a display surface and the display of the metallographic phase under the electrolysis condition, is simple to operate, consumes short time, can simply and efficiently corrode a tin crystal boundary, and has a clear and attractive metallographic structure.
In a preferred embodiment of the method for displaying a pure tin phase according to the present invention, the first, second, and third aqueous sandpaper are: 600# water sand paper, 1200# water sand paper and 2500# water sand paper.
As a preferred embodiment of the method for displaying the pure tin metallographic phase, the rotating speed of the first water-based sand paper grinding, the rotating speed of the second water-based sand paper grinding and the rotating speed of the third water-based sand paper grinding are all 350-450 r/min, and the grinding time is 1-3 min.
As a preferred embodiment of the method for displaying the pure tin metallographic phase, the method further comprises the step of cleaning the surface of the target to be detected after the first water-based sand paper is used for polishing, the second water-based sand paper is used for polishing and the third water-based sand paper is used for polishing.
As a preferable embodiment of the method for displaying a pure tin phase of the present invention, the first electrolytic polishing liquid and the second electrolytic polishing liquid are 70 wt.% of HClO4Mixed with absolute ethanol, 70 wt.% of HClO4The volume ratio of the alcohol to absolute ethyl alcohol is as follows: 70 wt.% HClO4The ratio of absolute ethyl alcohol is 1: 9. The inventors found that under the electrolysis of the first electrolytic polishing solution and the second electrolytic polishing solution, the polishing and display of the metallographic phase can be better realized by controlling the electrolysis conditions.
As a preferable embodiment of the method for displaying a pure tin metal phase of the present invention, the anodes of the first electrolytic polishing and the second electrolytic polishing are pure tin samples, and the cathodes are stainless steel.
As a preferable embodiment of the method for displaying a pure tin phase according to the present invention, the method further includes, after the first electrolytic polishing is completed: and washing the second polished surface for more than 15 seconds by adopting pure water, washing by using absolute ethyl alcohol, and finally drying.
As a preferable embodiment of the method for displaying a pure tin phase according to the present invention, the method further includes, after the second electrolytic polishing is completed: and washing the display surface of the pure tin metallographic phase for more than 15 seconds by adopting pure water, washing by using absolute ethyl alcohol, and finally drying.
As a preferred embodiment of the method for displaying the pure tin metallographic phase, the method further comprises the steps of marking the pure tin sample to be detected before the surface of the pure tin sample to be detected is polished by sequentially using the first water-based sand paper, the second water-based sand paper and the third water-based sand paper, and then performing water cutting.
The invention has the beneficial effects that: the invention provides a method for displaying a pure tin metallographic phase. The method for displaying the pure tin metallographic phase combines the first electrolytic polishing and the second electrolytic polishing, is simple to operate, consumes short time, can simply and efficiently corrode a tin crystal boundary, and has a clear and attractive metallographic structure.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
The method for displaying the pure tin phase comprises the following steps:
providing a pure tin sample to be tested: sampling by adopting water cutting equipment, and scribing a sample before sampling to ensure that the surface of the water cutting sample is smooth, and the cross section of the sample is 15 x 15 mm;
it is right the surface of the pure tin sample that awaits measuring adopts first water-based abrasive paper, second water-based abrasive paper and third water-based abrasive paper to polish in proper order, forms first polished surface, first water-based abrasive paper, second water-based abrasive paper and third water-based abrasive paper are respectively: 600# water-based sandpaper, 1200# water-based sandpaper and 2500# water-based sandpaper; the grinding speed of the first water-based abrasive paper is 400r/min, the grinding time is 2min, and after grinding is finished, the grinding scraps are washed clean by tap water to prevent the first water-based abrasive paper from being brought into the next grinding process; the grinding speed of the second water-based abrasive paper is 400r/min, the second water-based abrasive paper is ground until the surface is smooth and no previous scratch exists, the new scratch is shallow and the orientation is consistent, the grinding time is 2min, and after the grinding is finished, the abrasive dust is washed clean by tap water to prevent the abrasive dust from being brought into the next grinding process; the polishing rotation speed of the third water-based abrasive paper is 400r/min, the third water-based abrasive paper is polished until the surface is smooth and no previous scratch exists, the new scratch is shallow and the orientation is consistent, the polishing time is 2min, after polishing is finished, the third water-based abrasive paper is washed by tap water, washed by absolute ethyl alcohol and dried by cold air;
carrying out first electrolytic polishing on the first polished surface by using first electrolytic polishing liquid to form a second polished surface: a pure tin sample is taken as an anode, and a stainless steel plate is taken as a cathode; the first electrolytic polishing solution is 70 wt.% HClO4The volume ratio of the alcohol to absolute ethyl alcohol is as follows: 70 wt.% HClO4Absolute ethyl alcohol is 1:9, the direct current electrolytic voltage of the first electrolytic polishing is 25V, and the time of the first electrolytic polishing is 70 s; the electrolysis temperature is lower than 40 ℃, the sample to be electrolyzed is shaken during the electrolysis, after the first electrolytic polishing is finished, the sample is washed by pure water for more than 15s, then washed by absolute ethyl alcohol, and dried by a blower;
carrying out second electrolytic polishing on the second polished surface by using second electrolytic polishing liquid to form a pure tin metallographic phase display surface; the second electrolytic polishing solution is 70 wt.% of HClO4The volume ratio of the alcohol to absolute ethyl alcohol is as follows: 70 wt.% HClO4Absolute ethyl alcohol is 1:9, the direct current electrolytic voltage of the second electrolytic polishing is 6V, and the time of the second electrolytic polishing is 25 s; and (3) the electrolysis temperature is lower than 40 ℃, the sample to be electrolyzed is shaken during the electrolysis, and after the first electrolytic polishing is finished, the sample is washed by pure water for more than 15s, then washed by absolute ethyl alcohol and dried by a blower with cold air.
Example 2
The method for displaying the pure tin phase comprises the following steps:
providing a pure tin sample to be tested: sampling by adopting water cutting equipment, and scribing a sample before sampling to ensure that the surface of the water cutting sample is smooth, and the cross section of the sample is 15 x 15 mm;
it is right the surface of the pure tin sample that awaits measuring adopts first water-based abrasive paper, second water-based abrasive paper and third water-based abrasive paper to polish in proper order, forms first polished surface, first water-based abrasive paper, second water-based abrasive paper and third water-based abrasive paper are respectively: 600# water-based sandpaper, 1200# water-based sandpaper and 2500# water-based sandpaper; the polishing rotation speed of the first water-based abrasive paper is 450r/min, the polishing time is 2min, and after polishing is finished, the first water-based abrasive paper is washed clean by tap water to prevent the first water-based abrasive paper from being brought into the next polishing process; the polishing speed of the second water-based abrasive paper is 450r/min, the second water-based abrasive paper is polished until the surface is smooth and no previous scratch exists, the new scratch is shallow and the orientation is consistent, the polishing time is 2min, and after polishing is finished, the abrasive dust is washed clean by tap water to prevent the second water-based abrasive paper from being brought into the next polishing process; the polishing speed of the third water-based abrasive paper is 450r/min, the third water-based abrasive paper is polished until the surface is flat and no previous scratch exists, the new scratch is shallow and the orientation is consistent, the polishing time is 2min, after polishing is finished, the third water-based abrasive paper is washed clean by tap water, washed by absolute ethyl alcohol and dried by cold air;
carrying out first electrolytic polishing on the first polished surface by using first electrolytic polishing liquid to form a second polished surface: a pure tin sample is taken as an anode, and a stainless steel plate is taken as a cathode; the first electrolytic polishing solutionIs 70 wt.% HClO4The volume ratio of the alcohol to absolute ethyl alcohol is as follows: 70 wt.% HClO4Absolute ethyl alcohol is 1:9, the direct current electrolytic voltage of the first electrolytic polishing is 30V, and the time of the first electrolytic polishing is 50 s; the electrolysis temperature is lower than 40 ℃, the sample to be electrolyzed is shaken during the electrolysis, after the first electrolytic polishing is finished, the sample is washed by pure water for more than 15s, then washed by absolute ethyl alcohol, and dried by a blower;
carrying out second electrolytic polishing on the second polished surface by using second electrolytic polishing liquid to form a pure tin metallographic phase display surface; the second electrolytic polishing solution is 70 wt.% of HClO4The volume ratio of the alcohol to absolute ethyl alcohol is as follows: 70 wt.% HClO4Absolute ethyl alcohol is 1:9, the direct current electrolytic voltage of the second electrolytic polishing is 10V, and the time of the second electrolytic polishing is 15 s; and (3) the electrolysis temperature is lower than 40 ℃, the sample to be electrolyzed is shaken during the electrolysis, and after the first electrolytic polishing is finished, the sample is washed by pure water for more than 15s, then washed by absolute ethyl alcohol and dried by a blower with cold air.
Comparative example
The method for displaying the pure tin metallographic phase comprises the following steps:
providing a pure tin sample to be tested: sampling by adopting water cutting equipment, and scribing a sample before sampling to ensure that the surface of the water cutting sample is smooth, and the cross section of the sample is 15 x 15 mm;
it is right the surface of the pure tin sample that awaits measuring adopts first waterborne abrasive paper, second waterborne abrasive paper, third waterborne abrasive paper to polish and fourth waterborne abrasive paper to polish in proper order and forms first polished surface, first waterborne abrasive paper, second waterborne abrasive paper, third waterborne and fourth waterborne abrasive paper are respectively: 600# water-based sandpaper, 1200# water-based sandpaper, 2500# water-based sandpaper and 4000# water-based sandpaper; the grinding speed of the first water-based abrasive paper is 400r/min, the grinding time is 2min, and after grinding is finished, the grinding scraps are washed clean by tap water to prevent the first water-based abrasive paper from being brought into the next grinding process; the grinding speed of the second water-based abrasive paper is 400r/min, the second water-based abrasive paper is ground until the surface is smooth and no previous scratch exists, the new scratch is shallow and the orientation is consistent, the grinding time is 2min, and after the grinding is finished, the abrasive dust is washed clean by tap water to prevent the abrasive dust from being brought into the next grinding process; the grinding speed of the third water-based abrasive paper is 400r/min, the third water-based abrasive paper is ground until the surface is smooth and no previous scratch exists, the new scratch is shallow and the orientation is consistent, the grinding time is 2min, and after the grinding is finished, the abrasive dust is washed clean by tap water to prevent the abrasive dust from being brought into the next grinding process; the fourth aqueous abrasive paper is polished at the rotating speed of 400r/min until the surface is flat and no previous scratch exists, the new scratch is shallow and consistent in orientation, the polishing time is 2min, after polishing is finished, the fourth aqueous abrasive paper is washed clean by tap water, washed by absolute ethyl alcohol and dried by cold air;
and mechanically polishing the first polishing surface to obtain a second polishing surface: using wool fabric polishing cloth, spraying diamond spraying polishing agent with the granularity of 1um on 1/3-1/2 area of the polishing cloth, improving the fine polishing effect, polishing the polishing surface into a mirror surface at the polishing speed of 350r/min for 5min, washing the polished surface with tap water, washing the polished surface with absolute ethyl alcohol, and drying the polished surface with cold air;
and chemically corroding the second polished surface to obtain a metallographic display surface: the chemical corrosive liquid is: 5ml (36% by volume) HCl +95ml pure water +2 drops of H2O2And immersing the tin sample with the second polished surface in a chemical corrosive liquid for 60s, washing the tin sample with pure water for more than 15s after the immersion is finished, washing the tin sample with absolute ethyl alcohol, and drying the tin sample with cold air of a blower.
The display surfaces of the pure tin metallography described in the test examples 1 and 2 and the comparative example were photographed with a metallographic microscope, and the grain sizes were marked on the pictures, and the results are shown in fig. 1 to 3. FIG. 1 is a photomicrograph of the display surface of a pure tin phase as described in example 1, and FIG. 2 is a photomicrograph of the display surface of a pure tin phase as described in example 2; fig. 3 is a photomicrograph of the display surface of a pure tin phase described in the comparative example. As can be seen from the graphs 1-3, the pure tin phase shown in the graphs 1 and 2 is successfully displayed, the grain boundary is clear and attractive, the grain size can be easily counted, and the grain boundary shown in the graph 3 is fuzzy and is difficult to count the grain size.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.