CN112485084A - Method for displaying high-purity aluminum-gold phase - Google Patents

Method for displaying high-purity aluminum-gold phase Download PDF

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CN112485084A
CN112485084A CN202011317843.6A CN202011317843A CN112485084A CN 112485084 A CN112485084 A CN 112485084A CN 202011317843 A CN202011317843 A CN 202011317843A CN 112485084 A CN112485084 A CN 112485084A
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grinding
sample
water
acid
hydrochloric acid
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岳晓聪
余飞
黄宇彬
童培云
朱刘
吴彩红
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Vital Thin Film Materials Guangdong Co Ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00—Etching metallic material by chemical means
    • C23F1/10—Etching compositions
    • C23F1/14—Aqueous compositions
    • C23F1/16—Acidic compositions
    • C23F1/20—Acidic compositions for etching aluminium or alloys thereof
    • 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
    • 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
    • G01N1/34—Purifying; Cleaning
    • 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 provides a method for displaying high-purity aluminum metallography, belonging to the field of high-purity metallography. The invention takes the absolute ethyl alcohol as the cooling liquid during fine grinding, compared with water, the absolute ethyl alcohol has poor oxidation performance and good heat absorption performance, and can avoid the influence on the observation of the metallographic phase caused by the passivation of high-purity aluminum in the fine grinding process; meanwhile, the invention only needs simple processes of flattening, grinding, chemical corrosion and the like, is simple and convenient, has low requirement on equipment and saves more time.

Description

Method for displaying high-purity aluminum-gold phase
Technical Field
The invention belongs to the field of high-purity metallographic phase, and particularly relates to a method for displaying a high-purity aluminum-gold phase.
Background
The properties of the metal material such as strength, hardness, ductility and the like are closely related to the internal structure of the metal material, and the observation of the metallographic phase is the most direct and effective method for researching and analyzing the internal structure of the metal material. The high-purity aluminum has the excellent performances of small density, high heat conductivity, electric conductivity, high light reflectivity, strong atmospheric corrosion resistance, good processing and forming performance, no low-temperature brittleness, increased strength and plasticity along with the reduction of temperature and the like, and is widely applied to the fields of electronic industry and aerospace. At present, the method for preparing a metallographic specimen of high-purity aluminum comprises the following steps: sand paper grinding, flannelette mechanical polishing/electrolytic polishing, chemical corrosion/electrolytic etching, and then observing the metallographic structure of the sample by using a metallographic microscope. However, pure aluminum is soft in texture, silicon carbide in sand paper is easily embedded in the grinding process, and the silicon carbide is easily passivated in the fine grinding process, so that the requirements on the rotating speed, the force and the cooling liquid during grinding are high, and the surface is difficult to grind into a mirror surface.
CN106596214A proposes to combine grinding, mechanical polishing, electrolytic polishing and chemical etching to prepare high purity aluminum gold phase samples; CN106987893A proposes to use electrolytic corrosion to prepare high purity aluminum gold phase samples. The methods not only have higher requirements on equipment and are not simple and convenient enough to operate, but also can not avoid the problems in the grinding process and have longer treatment time.
Therefore, it is necessary to optimize the preparation method of the high-purity aluminum gold phase sample, avoid embedding silicon carbide in sand paper into high-purity aluminum, prevent the surface of the high-purity aluminum from being passivated in the fine grinding process, reduce the requirements on equipment, and shorten the treatment time by adopting simpler and more convenient operation.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the method for displaying the high-purity aluminum-gold phase, which can prevent the surface of high-purity aluminum from being passivated in the fine grinding process, is simpler and more convenient to operate and has lower requirements on equipment.
In order to achieve the above object, the present invention provides a method for displaying a high purity aluminum gold phase, comprising the following preparation steps:
(1) sampling, namely flattening the surface of the sample;
(2) sequentially grinding by using water-based sand paper with gradually smaller granularity;
(3) performing fine grinding by using water-based abrasive paper with a particle size smaller than that in the step (2), wherein the fine grinding takes absolute ethyl alcohol as cooling liquid;
(4) polishing the surface of the sample after fine grinding;
(5) and chemically corroding the surface of the polished sample, cleaning with a cleaning agent, and drying.
The passivation is caused by the action of metal and oxidizing substances, so that a very thin, compact and well-covered passivation film which is firmly adsorbed on the metal surface is generated on the metal surface. In the fine grinding process, the high-purity aluminum is easily passivated, so that a passivation layer exists on the surface to influence the observation of the metallographic phase. The method takes the absolute ethyl alcohol as the cooling liquid in the fine grinding process, and because the oxidation performance of the absolute ethyl alcohol is not as good as that of water and the heat absorption performance of the absolute ethyl alcohol is better than that of water, the oxidation speed of the high-purity aluminum can be reduced in the fine grinding process, and the surface passivation of the high-purity aluminum in the fine grinding process is greatly avoided.
The grinding in the step (2) can select absolute ethyl alcohol, water or a mixture of the absolute ethyl alcohol and the water as a cooling liquid. Considering that the passivation problem of the refining process is the main factor affecting the metallographic observation and considering the cost, it is preferable that water be used as the cooling liquid in the step (2).
Preferably, in the step (2), the rotation speed of each grinding is 350-; in the step (3), the rotation speed of fine grinding is 300-500 r/min. When the grinding in the step (2) and the step (3) is performed at the above-mentioned specific rotation speed, the silicon carbide in the aqueous sandpaper can be prevented from being embedded into the high-purity aluminum during the grinding.
Further preferably, in the step (3), the rotation speed of the fine grinding is 350 r/min.
Preferably, when the grinding is performed in the step (2) and the step (3), the directions of two adjacent grinding on the same surface are vertical; each grinding is carried out until the surface of the sample is flat, and the trace of the last turning or grinding cannot be seen. The direction of two adjacent grinding on the same surface is vertical, so that the next grinding can grind off grinding marks generated by the previous grinding.
Preferably, in the step (3), the surface of the sample after the fine grinding is flat, no scratch is visible to naked eyes, and a mirror surface appears.
Preferably, in the step (2), the used water-based sand paper is 1000#, 1500#, 2000#, 3000# water-based sand paper in sequence; in the step (3), the used water-based sand paper is 5000 #. When the grinding time of each surface of the 1000# water-based sand paper is 4-6 min, the grinding time of each surface of the 1500# water-based sand paper is 4-6 min, the grinding time of each surface of the 2000# water-based sand paper is 1-3 min, and the grinding time of each surface of the 3000# water-based sand paper is 5-7 min, the marks of the previous turning or grinding can be ground, and the marks can not be seen by naked eyes. When the grinding time of each surface of the No. 5000 water-based sand paper is 4-8 min, the surface of the sample can be smooth, no visible scratches exist, and a mirror surface appears. By adopting the specific process, the grinding time is greatly shortened.
Preferably, in the step (2), the grinding time of each surface of the 1000# water-based sand paper is 4-6 min, the grinding time of each surface of the 1500# water-based sand paper is 4-6 min, the grinding time of each surface of the 2000# water-based sand paper is 1-3 min, and the grinding time of each surface of the 3000# water-based sand paper is 5-7 min; in the step (3), the grinding time of each surface is 4-8 min.
Preferably, the etchant used for the chemical etching is a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, wherein the volume ratio of hydrofluoric acid to nitric acid to hydrochloric acid is hydrofluoric acid: nitric acid: hydrochloric acid is 1: 4-6: 9-10, the mass concentration of HF in hydrofluoric acid is 40-49%, and HNO in nitric acid3The mass concentration of (A) is 60-68%, and the mass concentration of HCl in hydrochloric acid is 60-68%.
Preferably, the etchant used for the chemical etching is a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, wherein the volume ratio of hydrofluoric acid to nitric acid to hydrochloric acid is hydrofluoric acid: nitric acid: the mass concentration of HF in hydrofluoric acid, HNO3 in nitric acid and HCl in hydrochloric acid were 1:5:10, 49%, 68% and 68%, respectively.
The corrosion resistance of high purity aluminum makes it difficult for typical corrosive agents to obtain the desired metallurgical phase. The mixture of the hydrofluoric acid, the nitric acid and the hydrochloric acid can well display the metallographic phase.
Preferably, the etchant is dropped to the surface of the sample while the chemical etching is performed. When the chemical etching is performed, the sample can be soaked in the etchant, or the etchant can be dripped on the surface of the sample. However, the sample is corroded, so that the corrosion degree is not easy to control and excessive corrosion is easy to cause. It is preferable to drop the etchant onto the surface of the sample, which makes it easier to control the degree of etching.
Preferably, the corrosive is dripped on the surface of the sample for 10-20 s and then is cleaned by a cleaning agent. And dropwise adding the corrosive to the surface of a sample, and waiting for the surface reaction for 10-20 s, so that the metallographic phase can be well displayed.
Preferably, in the step (4), the particle size of the polishing agent is not more than 1 μm, the polishing rotation speed is 300-500 r/min, and the polishing time is 3-5 min.
Preferably, the sample after the flattening treatment has a flat surface, a metallic luster and a surface roughness of less than 0.4 μm.
The cleaning agent in the step (5) can be selected from absolute ethyl alcohol, water or a mixture thereof.
The drying treatment in the step (5) can be selected from drying, blow-drying and the like.
Compared with the prior art, the invention has the beneficial effects that: the invention uses the absolute ethyl alcohol to replace water as the cooling liquid for fine grinding, compared with water, the absolute ethyl alcohol has poor oxidation performance and good heat absorption performance, and can avoid the influence of passivation on the metallographic observation in the fine grinding process of high-purity aluminum; meanwhile, the invention only needs simple processes of flattening, grinding, chemical corrosion and the like, is simple and convenient, has low requirement on equipment and has lower cost.
Drawings
FIG. 1 is a photograph of a metallographic phase of high purity aluminum obtained in example 1;
FIG. 2 is a photograph of a metallographic phase of high purity aluminum obtained in example 2.
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
This example provides one example of a method of displaying a high purity aluminum metallographic phase. The method for displaying the high-purity aluminum metallographic phase comprises the following steps:
(1) sampling and vehicle surface
Sampling by using a linear cutting device, flattening the surface of a sample to be observed by using a lathe, wherein the surface has metallic luster and surface roughness less than 0.4 mu m;
(2) coarse grinding
Slightly placing 1000# water-based sand paper on the surface of the sample which is turned, grinding until the surface of the sample is flat and no trace of the previous turning is seen, wherein the grinding speed is 400r/min, the grinding time of each surface is 5min, and the cooling liquid is water;
grinding by 1500# water-based sand paper along the direction vertical to the grinding mark generated by the previous grinding until the surface of the sample is flat and no grinding mark of the previous grinding can be seen, wherein the grinding speed is 400r/min, the grinding time of each surface is 5min, and the cooling liquid is water;
then grinding the sample by using 2000# water-based sand paper along a direction vertical to a grinding mark generated by the previous grinding until the surface of the sample is flat and no mark of the previous grinding is seen, wherein the grinding speed is 400r/min, the grinding time of each surface is 2min, and the cooling liquid is water;
then, grinding by using 3000# water-based sand paper along a direction vertical to a grinding mark generated by the previous grinding until the surface of the sample is flat and no mark of the previous grinding is seen, wherein the grinding speed is 400r/min, the grinding time of each surface is 6min, and the cooling liquid is water;
(3) finish grinding
Grinding with No. 5000 water-based abrasive paper in a direction perpendicular to grinding marks generated by the last grinding until the surface of the sample is flat, no visible scratches exist, and a mirror surface appears, wherein the grinding speed is 300r/min, the grinding time of each surface is 8min, and the cooling liquid is absolute ethyl alcohol;
(4) polishing of
Polishing with a polishing agent with a particle size of not more than 1 μm for 3min at a polishing speed of 500 r/min;
(5) etching of
Absorbing the corrosive (the corrosive is a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, wherein the volume ratio of the hydrofluoric acid to the nitric acid to the hydrochloric acid is 5:25:50, the mass concentration of HF in the hydrofluoric acid is 49%, and HNO in the nitric acid is absorbed by a test tube3The mass concentration of (2) is 68%, the mass concentration of HCl in hydrochloric acid is 68%), two drops (about 1-2 mL) are dropped on the polished surface for corrosion, after the surface reaction is carried out for 20s, the surface is cleaned by absolute ethyl alcohol, and then the surface is wiped dry.
The sample obtained by the method of the embodiment is observed, and the specific treatment is as follows: the computer is opened, the metallographic microscope is opened again, a clean sample is placed on a microscope objective table, a microscope objective lens is converted into a low-power lens (5X), a coarse focusing screw is adjusted to display an object image, a fine focusing screw is adjusted to be clear to the object image, the image is shot and stored by utilizing test software, the objective lens is converted into the high-power lens, the coarse focusing screw and the fine focusing screw are sequentially adjusted to be clear to the object image, whether the image is to be shot and stored is selected according to actual needs (if a small structural unit is found, the image is shot and stored), and the size of a crystal grain is marked on the image.
Example 2
This example provides one example of a method of displaying a high purity aluminum metallographic phase. The method for displaying the high-purity aluminum metallographic phase comprises the following steps:
(1) sampling and vehicle surface
Sampling by using a linear cutting device, flattening the surface of a sample to be observed by using a lathe, wherein the surface has metallic luster and surface roughness less than 0.4 mu m;
(2) coarse grinding
Slightly placing 1000# water-based abrasive paper on the surface of the sample after the sample is turned for grinding until the surface of the sample is flat and no trace of the previous turning is seen, wherein the grinding speed is 350r/min, the grinding time of each surface is 6min, and the cooling liquid is water;
grinding by 1500# water-based sand paper along the direction vertical to the grinding mark generated by the previous grinding until the surface of the sample is flat and no grinding mark of the previous grinding can be seen, wherein the grinding speed is 350r/min, the grinding time of each surface is 6min, and the cooling liquid is water;
then grinding the sample by using 2000# water-based abrasive paper along a direction vertical to a grinding mark generated by the previous grinding until the surface of the sample is flat and no mark of the previous grinding is seen, wherein the grinding speed is 350r/min, the grinding time of each surface is 3min, and the cooling liquid is water;
then, grinding by using 3000# water-based sand paper along a direction vertical to a grinding mark generated by the previous grinding until the surface of the sample is flat and no mark of the previous grinding is seen, wherein the grinding speed is 350r/min, the grinding time of each surface is 7min, and the cooling liquid is water;
(3) finish grinding
Grinding with No. 5000 water-based sand paper in a direction perpendicular to the grinding marks generated by the last grinding until the surface of the sample is flat, no visible scratches exist, and a mirror surface appears, wherein the grinding speed is 400r/min, the grinding time of each surface is 6min, and the cooling liquid is absolute ethyl alcohol;
(4) polishing of
Polishing with a polishing agent with a particle size of not more than 1 μm for 4min at a polishing speed of 400 r/min;
(5) etching of
Absorbing the corrosive (the corrosive is a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, wherein the volume ratio of the hydrofluoric acid to the nitric acid to the hydrochloric acid is 5:25:50, the mass concentration of HF in the hydrofluoric acid is 49%, and HNO in the nitric acid is absorbed by a test tube3The mass concentration of (2) is 68%, the mass concentration of HCl in hydrochloric acid is 68%), two drops (about 1-2 mL) are dropped on the polished surface for corrosion, after the surface reaction is carried out for 15s, the surface is cleaned by absolute ethyl alcohol, and then the surface is wiped dry.
The sample obtained by the method of the embodiment is observed, and the specific treatment is as follows: the computer is opened, the metallographic microscope is opened again, a clean sample is placed on a microscope objective table, a microscope objective lens is converted into a low-power lens (5X), a coarse focusing screw is adjusted to display an object image, a fine focusing screw is adjusted to be clear to the object image, the image is shot and stored by utilizing test software, the objective lens is converted into the high-power lens, the coarse focusing screw and the fine focusing screw are sequentially adjusted to be clear to the object image, whether the image is to be shot and stored is selected according to actual needs (if a small structural unit is found, the image is shot and stored), and the size of a crystal grain is marked on the image.
Example 3
This example provides one example of a method of displaying a high purity aluminum metallographic phase. The method for displaying the high-purity aluminum metallographic phase comprises the following steps:
(1) sampling and vehicle surface
Sampling by using a linear cutting device, flattening the surface of a sample to be observed by using a lathe, wherein the surface has metallic luster and surface roughness less than 0.4 mu m;
(2) coarse grinding
Slightly placing 1000# water-based sand paper on the surface of the sample which is turned, grinding until the surface of the sample is flat and no trace of the previous turning is seen, wherein the grinding speed is 450r/min, the grinding time of each surface is 4min, and the cooling liquid is water;
grinding by 1500# water-based sand paper along the direction vertical to the grinding mark generated by the previous grinding until the surface of the sample is flat and no grinding mark of the previous grinding can be seen, wherein the grinding speed is 450r/min, the grinding time of each surface is 4min, and the cooling liquid is water;
then grinding the sample by using 2000# water-based abrasive paper along a direction vertical to a grinding mark generated by the previous grinding until the surface of the sample is flat and no mark of the previous grinding is seen, wherein the grinding speed is 450r/min, the grinding time of each surface is 1min, and the cooling liquid is water;
then, grinding by using 3000# water-based sand paper along a direction vertical to a grinding mark generated by the previous grinding until the surface of the sample is flat and no mark of the previous grinding is seen, wherein the grinding speed is 450r/min, the grinding time of each surface is 5min, and the cooling liquid is water;
(3) finish grinding
Grinding with No. 5000 water-based abrasive paper in a direction perpendicular to grinding marks generated by the last grinding until the surface of the sample is flat, no visible scratches exist, and a mirror surface appears, wherein the grinding speed is 500r/min, the grinding time of each surface is 4min, and the cooling liquid is absolute ethyl alcohol;
(4) polishing of
Polishing with a polishing agent with the particle size not greater than 1 μm for 5min at a polishing speed of 300 r/min;
(5) etching of
Absorbing the corrosive (the corrosive is a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, wherein the volume ratio of the hydrofluoric acid to the nitric acid to the hydrochloric acid is 5:25:50, the mass concentration of HF in the hydrofluoric acid is 49%, and HNO in the nitric acid is absorbed by a test tube3The mass concentration of (2) is 68%, the mass concentration of HCl in hydrochloric acid is 68%), two drops (about 1-2 mL) are dropped on the polished surface for corrosion, after the surface reaction lasts for 10s, the surface is cleaned by absolute ethyl alcohol, and then the surface is wiped dry.
The sample obtained by the method of the embodiment is observed, and the specific treatment is as follows: the computer is opened, the metallographic microscope is opened again, a clean sample is placed on a microscope objective table, a microscope objective lens is converted into a low-power lens (5X), a coarse focusing screw is adjusted to display an object image, a fine focusing screw is adjusted to be clear to the object image, the image is shot and stored by utilizing test software, the objective lens is converted into the high-power lens, the coarse focusing screw and the fine focusing screw are sequentially adjusted to be clear to the object image, whether the image is to be shot and stored is selected according to actual needs (if a small structural unit is found, the image is shot and stored), and the size of a crystal grain is marked on the image.
Compared with the methods provided by CN106596214A and CN106987893A, the method 1-3 of the embodiment avoids the influence on the observation of the metallographic phase caused by passivation of high-purity aluminum in the fine grinding process, and simultaneously does not need electrolytic polishing and electrolytic corrosion, so that the method is simpler and more convenient, saves time and has low requirements on equipment.
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.

Claims (10)

1. A method of displaying a high purity aluminum gold phase, comprising the steps of:
(1) sampling, namely flattening the surface of the sample;
(2) sequentially grinding by using water-based sand paper with gradually smaller granularity;
(3) performing fine grinding by using water-based abrasive paper with a particle size smaller than that in the step (2), wherein the fine grinding takes absolute ethyl alcohol as cooling liquid;
(4) polishing the surface of the sample after fine grinding;
(5) and chemically corroding the surface of the polished sample, cleaning with a cleaning agent, and drying.
2. The method as claimed in claim 1, wherein in the step (2), the rotation speed of each grinding is 350-450 r/min; in the step (3), the rotation speed of fine grinding is 300-500 r/min.
3. The method according to claim 1, wherein when the grinding is performed in the step (2) and the step (3), the direction of the two adjacent grinding on the same surface is vertical; each grinding is carried out until the surface of the sample is flat, and the trace of the last turning or grinding cannot be seen.
4. The method of claim 1, wherein in step (3), the sample after the refining is smooth and has no visible scratches and a mirror surface.
5. The method according to claim 1, wherein in the step (2), the aqueous sandpaper used is 1000#, 1500#, 2000#, 3000# aqueous sandpaper; in the step (3), the used water-based sand paper is 5000# water-based sand paper.
6. The method according to claim 5, wherein in the step (2), the grinding time of each surface of the 1000# water-based sandpaper is 4-6 min, the grinding time of each surface of the 1500# water-based sandpaper is 4-6 min, the grinding time of each surface of the 2000# water-based sandpaper is 1-3 min, and the grinding time of each surface of the 3000# water-based sandpaper is 5-7 min; in the step (3), the grinding time of each surface is 4-8 min.
7. The method of claim 1, wherein the chemical etching uses an etchant which is a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, wherein the volume ratio of hydrofluoric acid to nitric acid to hydrochloric acid is hydrofluoric acid: nitric acid: hydrochloric acid is 1: 4-6: 9-10, the mass concentration of HF in hydrofluoric acid is 40-49%, and HNO in nitric acid3The mass concentration of (A) is 60-68%, and the mass concentration of HCl in hydrochloric acid is 60-68%.
8. The method of claim 7, wherein the chemical etching uses an etchant which is a mixture of hydrofluoric acid, nitric acid and hydrochloric acid, wherein the volume ratio of hydrofluoric acid to nitric acid to hydrochloric acid is hydrofluoric acid: nitric acid: hydrochloric acid is 1:5:10, the mass concentration of HF in hydrofluoric acid is 49%, and HNO in nitric acid3The mass concentration of (3) is 68%, and the mass concentration of HCl in hydrochloric acid is 68%.
9. The method as claimed in claim 1, wherein the chemical etching is performed by dropping an etchant onto the surface of the sample for 10-20 seconds and then cleaning the sample with a cleaning agent.
10. The method according to claim 1, wherein the sample after the flattening treatment has a flat surface with metallic luster and a surface roughness of < 0.4 μm; in the step (4), the granularity of the polishing agent is not more than 1 micron, the polishing rotating speed is 300-500 r/min, and the polishing time is 3-5 min.
CN202011317843.6A 2020-11-20 2020-11-20 Method for displaying high-purity aluminum-gold phase Pending CN112485084A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103837382A (en) * 2013-12-24 2014-06-04 利达光电股份有限公司 Preparation method for high pure aluminium metallographic sample
CN104422611A (en) * 2013-09-02 2015-03-18 宁波江丰电子材料股份有限公司 Metallurgical corrosive and metallurgical structure display method
CN106596214A (en) * 2016-10-25 2017-04-26 常州苏晶电子材料有限公司 Efficient preparation method of high purity aluminum gold-phase sample
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