CN114964986A - Metallographic preparation method of CoFeB alloy - Google Patents

Metallographic preparation method of CoFeB alloy Download PDF

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Publication number
CN114964986A
CN114964986A CN202210568847.4A CN202210568847A CN114964986A CN 114964986 A CN114964986 A CN 114964986A CN 202210568847 A CN202210568847 A CN 202210568847A CN 114964986 A CN114964986 A CN 114964986A
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sample
metallographic
cofeb alloy
polishing
preparing
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肖惠云
蔡新志
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Vital Thin Film Materials Guangdong Co Ltd
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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
    • G01N1/32—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
    • G01N1/286—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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention belongs to the field of metallographic phase display, and discloses a method for preparing a metallographic phase of a CoFeB alloy, which comprises the following steps: (1) providing a CoFeB alloy metallographic sample, cutting the CoFeB alloy metallographic sample according to a gold phase sample preparation standard to obtain a sample, and then carrying out sample embedding treatment; (2) carrying out rough polishing and fine polishing on the sample inlaid in the step (1) in sequence; (3) preparing corrosive liquid to carry out metallographic chemical corrosion treatment on the sample subjected to fine polishing in the step (2) to form a metallographic display surface; wherein, in the step (3), the corrosive liquid is prepared from concentrated hydrochloric acid: concentrated nitric acid: water in a volume ratio of 2: 1: 1, wherein the mass percent concentration of the concentrated nitric acid is 60-70%, and the mass percent concentration of the concentrated hydrochloric acid is 28-35%. The method has the advantages of simple operation steps, low cost and short time consumption, and the CoFeB alloy sample treated by the method has clear metallographic structure when observed under a metallographic microscope, so that an excellent metallographic observation result is obtained.

Description

Metallographic preparation method of CoFeB alloy
Technical Field
The invention belongs to the field of metallographic phase display, and particularly relates to a metallographic phase preparation method of a CoFeB alloy.
Background
The CoFeB alloy has high hardness, is an important spin electron material and is mainly applied to the preparation of high-performance magnetic tunnel junctions. The internal structure of the metal material is directly and closely related to the material properties such as hardness, strength, ductility and the like, and metallographic observation is the most direct and effective method for researching the internal structure of the metal material. The metallographic phase refers to chemical components of metal or alloy and physical states and chemical states of various components in the metal or alloy, and the metallographic phase display is a common technology for observing the internal structure of the metal and the alloy thereof.
The correct metallographic preparation method is a precondition for obtaining a high-definition high-quality material microstructure, and the conventional metallographic preparation method cannot be well applied to the CoFeB alloy at present and cannot obtain an excellent metallographic result, so that the metallographic preparation method suitable for the CoFeB alloy needs to be developed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for preparing a CoFeB alloy metallographic phase, which has the advantages of simple operation steps, low cost and short time consumption, and the CoFeB alloy sample treated by the method has a clear metallographic structure and obtains an excellent metallographic observation result when observed under a metallographic microscope.
In order to realize the purpose of the invention, the specific technical scheme is as follows:
a method for preparing a CoFeB alloy metallographic phase comprises the following steps:
(1) providing a CoFeB alloy metallographic sample, cutting the CoFeB alloy metallographic sample according to a gold phase sample preparation standard to obtain a sample, and then carrying out sample inlaying treatment;
(2) carrying out rough polishing and fine polishing on the sample inlaid in the step (1) in sequence;
(3) preparing corrosive liquid to carry out metallographic chemical corrosion treatment on the sample subjected to fine polishing in the step (2) to form a metallographic display surface;
wherein, in the step (3), the corrosive liquid is prepared from concentrated hydrochloric acid: concentrated nitric acid: water in a volume ratio of 2: 1: 1, wherein the mass percent concentration of the concentrated nitric acid is 60-70%, and the mass percent concentration of the concentrated hydrochloric acid is 28-35%.
Preferably, the process of the sample mounting treatment in the step (1) is as follows: placing the sample in a mold, and mixing the epoxy resin and the curing agent according to the mass ratio of the epoxy resin: curing agent = 4: 1 mixing materials, pouring into a mould, and taking out after curing.
Preferably, in step (2), rough polishing is performed by using P180, P320, P500 and P1200 sandpaper in sequence.
Preferably, the rough polishing step is:
grinding for 30-60 min by using P180 sand paper, setting the rotating speed to be 200-300 r/min, and grinding until no obvious cutting mark exists on the surface;
and (3) sequentially replacing the P320 sand paper, the P500 sand paper and the P1200 sand paper for grinding, wherein the grinding time is 1-2 min each time, and the rotating speed is set to be 200-300 r/min.
Preferably, in the step (2), fine polishing is performed by using P2500 sandpaper and 0.25 μm polishing cloth in sequence.
Preferably, the fine polishing step is:
grinding for 2-4 min by using P2500 abrasive paper, setting the rotating speed to be 200-300 r/min, and removing traces generated by rough polishing;
and replacing the polishing cloth with the thickness of 0.25 mu m, and polishing for 2-4 min by matching with the polishing solution with the thickness of 0.25 mu m until the surface is bright, and the surface presents an obvious mirror surface and has no scratches.
Preferably, in the step (3), the etching time is 1-2 min.
Preferably, the mass percentage concentration of the concentrated nitric acid is 68%, and the mass percentage concentration of the concentrated hydrochloric acid is 32%.
Preferably, after the fine polishing in the step (2) and the corrosion in the step (3) are finished, pure water and absolute ethyl alcohol are sequentially used for cleaning.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the CoFeB alloy metallographic phase fills up the gap of the CoFeB alloy metallographic phase display technology at present, can effectively enable the metallographic structure of the CoFeB alloy to be clearly observed, and can clearly mark the grain size;
(2) by the metallographic preparation method, the obvious defects of the CoFeB alloy can be determined under a metallographic microscope, and whether the alloy meets the product requirements or not can be conveniently judged, so that the preparation process and related parameters of the alloy can be timely adjusted, the failure rate of the product is reduced, and the economic benefit of the product is improved;
(3) the method has the advantages of simple operation steps, low cost and short time consumption, and the CoFeB alloy sample treated by the method has clear metallographic structure when observed under a metallographic microscope.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a gold phase diagram (5 times) of a CoFeB alloy in example 1;
FIG. 2 is a diagram (50 times) of the gold phase of the CoFeB alloy in example 1;
FIG. 3 is a gold phase diagram (100 times) of a CoFeB alloy in example 1;
FIG. 4 is a gold phase diagram (5 times) of a CoFeB alloy in comparative example 1;
FIG. 5 is a gold phase diagram (5 times) of a CoFeB alloy in example 2;
FIG. 6 is a gold phase diagram (50X) of a CoFeB alloy in example 2;
FIG. 7 is a gold phase diagram (100 times) of a CoFeB alloy in example 2;
FIG. 8 is a gold phase diagram (5 times) of the CoFeB alloy in comparative example 2.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
The embodiment discloses a method for preparing a CoFeB alloy metallographic phase, which specifically comprises the following steps:
(1) sampling the CoFeB target by using water cutting equipment to obtain a sample with the size of 15 multiplied by 2 mm;
(2) placing the sample in a mould, and mixing the following components in percentage by mass: curing agent = 4: 1 preparing materials, pouring the materials into a mold, and taking out a sample from the mold after curing;
(3) roughly polishing the sample on a metallographic automatic polishing machine, grinding for 30min by using new P180 sand paper at a rotating speed of 250 r/min, and removing obvious cutting marks on the surface; then sequentially replacing the P320, P500 and P1200 sandpaper for rough polishing, and grinding for 1.5min each time at the rotating speed of 250 r/min;
(4) finely polishing the roughly polished sample on an automatic metallographic polishing machine, polishing the sample for 2min by using P2500 abrasive paper, rotating at a speed of 250 r/min, removing traces generated by rough polishing, replacing 0.25 mu m polishing cloth, and finally polishing the sample by matching with 0.25 mu m polishing solution, wherein after 2min, the surface of the sample is bright, and the sample presents an obvious mirror surface without scratches, can be washed by clear water and then scrubbed by alcohol;
(5) as hydrochloric acid (32%): nitric acid (68%): water = 2: 1: 1, preparing a corrosive liquid, and specifically operating as follows: firstly, measuring 10ml of pure water by using a measuring cup, pouring the pure water into a beaker with the capacity of 50ml, then respectively measuring 20ml of hydrochloric acid (the concentration is 32%) and 10ml of nitric acid (the concentration is 68%), slowly pouring the pure water into the beaker, and stirring the pure water and the nitric acid by using a glass rod to uniformly mix the pure water and the nitric acid;
(6) pouring prepared corrosive liquid into a small beaker with the capacity of 50ml, putting a polished sample into the corrosive liquid to ensure that the sample is immersed in the corrosive liquid, so that the surface of the sample to be corroded is fully contacted with the corrosive liquid, corroding for 1.5min, taking out the sample after the corrosion is finished, washing the sample with a large amount of pure water, and scrubbing the surface of the sample by using dust-free paper and alcohol to ensure that no corrosive liquid residue exists on the surface of the sample;
(7) and after the corrosion is finished, the surface of the sample is placed under a microscope for observation.
Referring to the attached drawings 1-3, the metallographic pictures of the CoFeB alloy in this example are shown in different multiples. After the CoFeB alloy is treated by the method of the embodiment 1, the CoFeB alloy has clear and obvious metallographic structure, clear grain boundary and fine grains.
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that the etching solution used in step (5) was different from that used in the conventional etching solution prepared from glacial acetic acid (75 ml) and hydrogen peroxide (30%, 25 ml).
A metallographic sample obtained in the comparative example 1 is placed in a metallographic microscope to be observed, the attached drawing 4 is a metallographic picture of the CoFeB alloy in the comparative example 1, and the comparison with the drawings 1-3 in the example 1 shows that the corrosive liquid used in the comparative example 1 has no corrosive effect on the CoFeB alloy.
Example 2
The embodiment discloses a method for preparing a CoFeB alloy metallographic phase, which specifically comprises the following steps:
(1) sampling the CoFeB target by using water cutting equipment to obtain a sample of 15 x 2 mm;
(2) the sample was placed in a mold, with the epoxy resin: curing agent = 4: 1, pouring the prepared sample into a mold, and taking out the sample from the mold after the sample is solidified;
(3) roughly polishing the sample on a metallographic automatic polishing machine, grinding the sample for 5min by using new P180 abrasive paper at the rotating speed of 350r/min, and removing obvious cutting marks on the surface; then sequentially replacing the P320, P500 and P1200 sandpaper for rough polishing, and grinding for 1min each time at the rotating speed of 350 r/min;
(4) finely polishing the roughly polished test sample on an automatic metallographic polishing machine, polishing the sample for 1min by using P2500 abrasive paper, rotating at a speed of 350r/min, removing traces generated by rough polishing, replacing polishing cloth with the thickness of 0.25 mu m, and finally polishing the sample by matching with polishing solution with the thickness of 0.25 mu m, wherein after 1min, the surface of the sample is bright, and the sample presents an obvious mirror surface without scratches, can be washed by clear water and then scrubbed by alcohol;
(5) as hydrochloric acid (32%): nitric acid (68%): water = 2: 1: 1, preparing a corrosive liquid, and specifically operating as follows: firstly, measuring 10ml of pure water by using a measuring cup, pouring the pure water into a beaker with the capacity of 50ml, then respectively measuring 20ml of hydrochloric acid (the concentration is 32%) and 10ml of nitric acid (the concentration is 68%), slowly pouring the pure water into the beaker, and stirring the pure water and the nitric acid by using a glass rod to uniformly mix the pure water and the nitric acid;
(6) pouring prepared corrosive liquid into a small beaker with the capacity of 50ml, putting a polished sample into the corrosive liquid to ensure that the sample is immersed in the corrosive liquid, so that the surface of the sample to be corroded is fully contacted with the corrosive liquid, corroding for 1.5min, taking out the sample after the corrosion is finished, washing the sample with a large amount of pure water, and scrubbing the surface of the sample by using dust-free paper and alcohol to ensure that no corrosive liquid residue exists on the surface of the sample;
(7) and after the corrosion is finished, the surface of the sample is placed under a microscope for observation.
Referring to fig. 5-7, the metallographic images of the CoFeB alloy in this example are shown in different multiples. It can be obviously seen that the metallographic structure of the alloy is clear and obvious, the grain boundary is clear, and the grains are fine.
Comparative example 2
Comparative example 2 is substantially the same as example 2 except that the etching solution used in step (5) was different from that used in the conventional etching solution prepared from glacial acetic acid (75 ml) and hydrogen peroxide (30%, 25 ml).
And (3) observing the metallographic sample obtained in the comparative example 2 in a metallographic microscope, wherein the attached figure 8 is a metallographic picture of the CoFeB alloy in the comparative example 2, and comparing the metallographic picture with the figures 5-7 in the example 2 shows that the corrosive liquid used in the comparative example 2 has no corrosive effect on the CoFeB alloy.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (9)

1. A method for preparing a CoFeB alloy metallographic phase is characterized by comprising the following steps:
(1) providing a CoFeB alloy metallographic sample, cutting the CoFeB alloy metallographic sample according to a gold phase sample preparation standard to obtain a sample, and then carrying out sample embedding treatment;
(2) carrying out rough polishing and fine polishing on the sample inlaid in the step (1) in sequence;
(3) preparing corrosive liquid to carry out metallographic chemical corrosion treatment on the sample subjected to fine polishing in the step (2) to form a metallographic display surface;
wherein, in the step (3), the corrosive liquid is prepared from concentrated hydrochloric acid: concentrated nitric acid: water according to a volume ratio of 2: 1: 1, wherein the mass percent concentration of the concentrated nitric acid is 60-70%, and the mass percent concentration of the concentrated hydrochloric acid is 28-35%.
2. The method for preparing the CoFeB alloy metallography according to claim 1, wherein the process of the sample inlaying treatment in the step (1) is as follows: placing the sample in a mold, and mixing the epoxy resin and the curing agent according to the mass ratio of the epoxy resin: curing agent = 4: 1 mixing materials, pouring into a mould, and taking out after curing.
3. The metallographic preparation method of a CoFeB alloy according to claim 1, wherein in step (2), the rough polishing is performed by using P180, P320, P500 and P1200 sandpaper in sequence.
4. The method for preparing the CoFeB alloy metallographic phase according to claim 3, wherein the rough polishing step comprises:
grinding the mixture for 30-60 min by using P180 sand paper, wherein the rotating speed is set to be 200-300 r/min;
and (3) sequentially replacing the P320 sand paper, the P500 sand paper and the P1200 sand paper for grinding, wherein the grinding time is 1-2 min each time, and the rotating speed is set to be 200-300 r/min.
5. The method for preparing the CoFeB alloy metallographic phase according to claim 1, wherein in the step (2), fine polishing is performed by using P2500 sandpaper and 0.25 μm polishing cloth in this order.
6. The method for preparing the CoFeB alloy metallographic phase according to claim 5, wherein the fine polishing step comprises:
grinding for 2-4 min by using P2500 sand paper, wherein the rotating speed is set to be 200-300 r/min;
and replacing the polishing cloth with the thickness of 0.25 mu m, and polishing for 2-4 min by matching with the polishing solution with the thickness of 0.25 mu m.
7. The method for preparing the CoFeB alloy metallography according to claim 1, wherein in the step (3), the corrosion time is 1-2 min.
8. The method for preparing the CoFeB alloy metallographic phase according to claim 1, wherein the concentration of the concentrated nitric acid is 68% by mass and the concentration of the concentrated hydrochloric acid is 32% by mass.
9. The method for preparing the CoFeB alloy metallographic phase according to claim 1, wherein after the finish polishing in step (2) and the etching in step (3) are completed, the alloy is washed with pure water and absolute ethanol.
CN202210568847.4A 2022-05-24 2022-05-24 Metallographic preparation method of CoFeB alloy Pending CN114964986A (en)

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