CN115406918A - Martensite high-strength steel EBSD sample preparation method - Google Patents

Martensite high-strength steel EBSD sample preparation method Download PDF

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CN115406918A
CN115406918A CN202210843763.7A CN202210843763A CN115406918A CN 115406918 A CN115406918 A CN 115406918A CN 202210843763 A CN202210843763 A CN 202210843763A CN 115406918 A CN115406918 A CN 115406918A
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ebsd
sample
detected
polishing
strength steel
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武雪婷
尹仕伟
吴志伟
张军
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Chengdu Advanced Metal Materials Industry Technology Research Institute Co Ltd
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Chengdu Advanced Metal Materials Industry Technology Research Institute Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/203—Measuring back scattering

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Abstract

The invention provides a martensite high-strength steel EBSD sample preparation method which comprises the steps of cutting an EBSD sample to be detected on martensite high-strength steel by using linear cutting, then carrying out mechanical polishing treatment on the EBSD sample to be detected, then carrying out chemical corrosion on the EBSD sample to be detected after the mechanical polishing, then carrying out vibration polishing treatment on the EBSD sample to be detected after the chemical corrosion, and finally washing and cleaning the surface of the EBSD sample to be detected after the vibration polishing is finished until no polishing liquid residue exists on the surface. The invention provides a method for processing martensite high-strength steel with a multi-scale structure by adopting a linear cutting-mechanical polishing-chemical corrosion-vibration polishing process, so as to obtain a martensite high-strength steel sample suitable for EBSD detection, wherein the sample simultaneously meets the requirements of high surface flatness, low stress value and original surface stress distribution rule of the sample to be detected, the EBSD calibration rate can be stably kept above 85%, the sample preparation cost is reduced, and the safety of sample preparation operation is improved.

Description

Martensite high-strength steel EBSD sample preparation method
Technical Field
The invention belongs to the technical field of detection sample preparation, and particularly relates to an martensite high-strength steel EBSD sample preparation method.
Background
The secondary hardening type ultrahigh-strength martensitic steel has high strength, high toughness and excellent corrosion resistance, and is widely applied to the field of aerospace. Different from single-phase materials, the self organization structure of the martensite steel matrix has the characteristics of multi-level, multi-phase and the like, and the research on the comprehensive control mechanism of the multi-level organization structure of the martensite has important significance in improving the comprehensive performance index of the material and playing the application potential of the material. And the multi-scale structure research mainly relates to martensite lath blocks, martensite lath bundles, martensite laths and the like, wherein the research on the martensite blocks is mainly realized by an Electron Back Scattered Diffraction (EBSD) technology.
The back scattering electron diffraction is a material characterization technology combining the microscopic structure of the material with the crystallography characteristic analysis, and the method adopts a crystal orientation analysis method of the back scattering electron diffraction chrysanthemic ray in a scanning electron microscope, and can comprehensively reflect the information of each phase proportion, grain size and shape, interface, crystallography orientation and the like in the material. Since EBSD analysis is performed with the vicinity of the sample surface as a detection target, it occurs only at a depth of about 10 to 30nm in the surface layer of the sample, and the state of the sample surface has a great influence on the experimental results. The samples used for EBSD analysis require a smooth surface, no oxide film and no continuous etch pits present, and no residual process strain layer, and therefore sample preparation is a prerequisite and key to EBSD analysis techniques.
The conventional EBSD sample preparation method comprises mechanical sample preparation, electrolytic polishing, ion thinning and the like. The sample preparation time of electrolytic polishing is short, but the parameters of electrolyte, electrolytic voltage, time and the like adopted by different materials are different, the process adjustment range is wide, and the selection of the electrolyte is complicated. For ultra-high strength martensitic stainless steel, the prior literature adopts more EBSD sample preparation methods as electrolytic polishing sample preparation, the selected electrolytic polishing solution is generally perchloric acid alcohol solution, and perchloric acid has strong corrosivity and is exploded by combustionDanger exists, and great potential safety hazard exists. During mechanical polishing, a sample is prepared by polishing ground samples respectively by using polishing agents with different particle sizes, the sample preparation time is long, the sample preparation modes of materials with different hardness are different, and the polishing solution adopted in the mechanical polishing process is generally Al 2 O 3 The safety of the suspension is greatly improved by chloric acid solution, but the mechanical polishing adopts different processes for different materials, so that the sample preparation success rate is difficult, and the current mechanical polishing sample preparation method is mostly used for single-phase materials. The ion thinning sample preparation effect is good, but the sample preparation needs to be made into a 60-100 mu m thin slice, the sample preparation time consumption is long, the cost is high, and the ion polishing is generally carried out under the condition that the electrolytic polishing and the mechanical polishing can not be met, so that the existing high-strength martensite steel ion thinning sample preparation cost is high, the safety of an electrolytic polishing perchloric acid solution is low, the process is complicated, and the success rate of mechanical polishing sample preparation is difficult to ensure.
Disclosure of Invention
Aiming at the problems, the invention provides a martensite high-strength steel EBSD sample preparation method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a martensite high-strength steel EBSD sample preparation method comprises the following steps:
cutting an EBSD sample to be detected on the martensite high-strength steel by using linear cutting;
performing mechanical polishing treatment on the EBSD sample to be detected;
carrying out chemical corrosion on the mechanically polished EBSD sample to be detected;
carrying out vibration polishing treatment on the EBSD sample to be detected after chemical corrosion;
and after the vibration polishing is finished, washing and cleaning the surface of the sample to be detected of the EBSD until no polishing solution is left on the surface.
Preferably, the mechanical polishing treatment is performed on the sample to be tested for EBSD, and includes the following steps:
grinding the EBSD sample to be detected obtained by linear cutting on silicon oxide abrasive paper, wherein the abrasive paper grinding is sequentially from 200 meshes, 400 meshes, 600 meshes, 800 meshes, 1000 meshes to 1500 meshes, and the polishing agent is a diamond polishing agent with the particle size of 2.5 mu m until the surface of the sample is flat and has no scratch.
Preferably, the chemical etching is performed on the mechanically polished sample to be tested for EBSD, and includes the following steps:
preparing a chemical corrosive agent;
and (3) carrying out titration corrosion on the EBSD sample to be detected by using a chemical corrosive, wherein the corrosion time is 10-30 s.
Preferably, the proportion of the chemical corrosive agent is 3.5g FeCl 3 、1gCuCl 2 50mL of anhydrous ethanol, 50mL of distilled water and 2.5mL of anhydrous ethanol 3 。
Preferably, the chemical etchant is prepared, comprising the steps of:
distilled water was placed in a beaker, and 99% absolute ethanol for analysis, 99% concentrated HCl for analysis, and 99% concentrated HNO for analysis were added to distilled water in this order 3 、FeCl 3 And CuCl 2 Fully stirring, uniformly mixing and cooling for later use.
Preferably, the vibration polishing treatment is performed on the chemically corroded EBSD sample to be detected, and the vibration polishing treatment method comprises the following steps:
and (5) using a vibration polishing machine to perform vibration polishing on the EBSD sample to be detected.
Preferably, the vibration polishing process parameters of the vibration polishing machine are as follows:
the vibration frequency is 1000-10000 Hz;
the applied load is 400-500 g, and the polishing time is 4-5 h;
the polishing solution used by the vibration polishing machine is sol-gel alumina polishing suspension with the granularity of 0.04-0.05 mu m.
Preferably, the method further comprises the following steps:
and (3) washing and cleaning the surface of the EBSD sample to be detected until no polishing solution remains on the surface, and analyzing the EBSD sample to be detected through EBSD to obtain the EBSD calibration rate.
Preferably, the wire-cut cutting wire is a molybdenum wire.
Preferably, the martensitic high-strength steel comprises low-carbon high-alloy secondary hardening type ultrahigh-strength martensitic steel, and the alloy elements of the low-carbon high-alloy secondary hardening type ultrahigh-strength martensitic steel comprise Cr, co and Mo.
The invention has the beneficial effects that:
the invention provides a method for processing martensite high-strength steel with a multi-scale structure by adopting a linear cutting-mechanical polishing-chemical corrosion-vibration polishing process to obtain a martensite high-strength steel sample suitable for EBSD detection, wherein the sample simultaneously meets the requirements of high surface flatness, low stress value and original surface stress distribution rule of the sample to be detected, the EBSD calibration rate can be stably kept above 85%, the sample preparation cost is reduced, and the safety of sample preparation operation is improved.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 shows an EBSD analysis chart of example 1 of the sample preparation method for martensite high-strength steel EBSD of the invention;
FIG. 2 shows an EBSD analysis chart of example 2 of the sample preparation method for martensite high-strength steel EBSD of the invention;
FIG. 3 shows an EBSD analysis chart of comparative example 1 of the EBSD sample preparation method for martensite high-strength steel of the invention;
fig. 4 shows an EBSD analysis chart of comparative example 2 of the EBSD sample preparation method for martensitic high-strength steel according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A martensite high-strength steel EBSD sample preparation method comprises the following steps:
firstly, cutting an EBSD sample to be detected on martensite high-strength steel by using wire cutting, wherein the size of the sample is less than or equal to 15 multiplied by 3mm, and a wire rod subjected to wire cutting is a molybdenum wire;
then mechanically polishing the EBSD sample to be detected;
the main purpose of the step is to perform mechanical grinding and polishing to obtain a surface to be detected with a flat surface. The specific operation steps are as follows: grinding a sample obtained by linear cutting on silicon oxide abrasive paper, wherein the abrasive paper is sequentially ground from 200 meshes, 400 meshes, 600 meshes, 800 meshes and 1000 meshes to 1500 meshes, and the polishing agent is a diamond polishing agent with the particle size of 2.5 mu m, so that the mechanical polishing time is not too long until the surface of the sample is flat and has no scratches.
Carrying out chemical corrosion on the mechanically polished EBSD sample to be detected;
the main purpose of the step is to remove residual stress brought by a mechanical polishing process by a chemical corrosion method. The chemical corrosive agent used in the step comprises the following components in percentage by weight: 3.5g FeCl 3 、1gCuCl 2 50mL of anhydrous ethanol, 50mL of distilled water and 2.5mL of anhydrous ethanol 3 The preparation process comprises the following steps: distilled water was placed in a beaker, and 99% absolute ethanol for analysis, 99% concentrated HCl for analysis, and 99% concentrated HNO for analysis were added to distilled water in this order 3 、FeCl 3 And CuCl 2 Fully stirring, uniformly mixing and cooling for later use. The corrosion time is different according to different heat treatment states of the samples, and titration is adoptedThe method carries out chemical corrosion, the corrosion time is controlled to be 10-30 s, if the corrosion time is too short, residual stress brought by mechanical polishing cannot be eliminated, and if the corrosion time is too long, corrosion pits can be formed on the surface of the sample, so that subsequent EBSD analysis is influenced.
Carrying out vibration polishing treatment on the EBSD to-be-detected sample which is chemically corroded;
it should be noted that the surface topography of the sample after chemical etching completely presents a martensite lath structure, the microscopic fluctuation is obvious, and the sample cannot be directly used for EBSD analysis, and further vibration treatment is required to keep the surface of the sample in a flat state. The parameters of the vibration polishing process are as follows: vibration frequency: 1000-10000 Hz, the applied load is 400-500 g, the polishing time is 4-5 h, and the used polishing solution is sol-gel alumina polishing suspension with the granularity of 0.04-0.05 mu m.
And after the vibration polishing is finished, washing and cleaning the surface of the EBSD sample to be detected until no polishing solution remains on the surface, and finally analyzing the EBSD sample to be detected through EBSD to obtain the EBSD calibration rate.
The martensitic high-strength steel comprises low-carbon high-alloy secondary hardening type ultrahigh-strength martensitic steel, wherein alloy elements of the low-carbon high-alloy secondary hardening type ultrahigh-strength martensitic steel comprise Cr, co and Mo.
The following examples and comparative examples were obtained by taking a low-carbon high-alloy secondary-hardening type ultrahigh-strength martensitic steel as an example:
example 1
Cutting an EBSD sample to be detected on the martensite high-strength steel by using a linear cutting process;
and grinding the sample obtained by linear cutting on silicon oxide abrasive paper, wherein the abrasive paper grinding is sequentially 200, 400, 600, 800, 1000 to 1500, and the polishing agent is 2.5 mu m diamond polishing agent until the surface of the sample is flat and has no scratch.
And chemically corroding the mechanically polished sample, wherein the chemical corrosive is prepared from the following components in percentage by weight: 3.5g FeCl 3 、1gCuCl 2 50mL of anhydrous ethanol, 50mL of distilled water and 2.5mL of anhydrous ethanol 3 . Chemical corrosion is carried out by adopting a titration mode, and the corrosion time is controlledAt 10s.
Carrying out vibration polishing treatment on the sample subjected to chemical corrosion, wherein the vibration polishing process parameters are as follows: vibration frequency: 1000-10000 Hz, 460g of applied load and 4h of polishing time, and the used polishing solution is sol-gel alumina polishing suspension with the granularity of 0.05 μm.
And after the vibration polishing is finished, washing the surface of the sample to be clean until no polishing solution is left on the surface.
As shown in fig. 1, the white non-texture area is an EBSD unmarked area, and the final EBSD mark rate is 87%.
Example 2
Cutting an EBSD sample to be detected on the martensite high-strength steel by using a linear cutting process;
and grinding the sample obtained by linear cutting on silicon oxide abrasive paper, wherein the abrasive paper grinding is sequentially 200, 400, 600, 800, 1000 to 1500, and the polishing agent is 2.5 mu m diamond polishing agent until the surface of the sample is flat and has no scratch.
Carrying out chemical corrosion on the mechanically polished sample, wherein the chemical corrosion agent comprises the following components in percentage by weight: 3.5g FeCl 3 、1gCuCl 2 50mL of anhydrous ethanol, 50mL of distilled water and 2.5mL of anhydrous ethanol 3 . Chemical corrosion is carried out by adopting a titration mode, and the corrosion time is controlled to be 30s.
Carrying out vibration polishing treatment on the sample subjected to chemical corrosion, wherein the vibration polishing process parameters are as follows: vibration frequency: 1000-10000 Hz, the applied load is 460g, the polishing time is 5h, and the used polishing solution is sol-gel alumina polishing suspension with the granularity of 0.05 mu m.
And after the vibration polishing is finished, washing the surface of the sample to be clean until no polishing solution is left on the surface.
As shown in fig. 2, the white non-textured area is an EBSD unmarked area, and the final EBSD mark rate is 93%.
Comparative example 1
Cutting an EBSD sample to be detected on the martensite high-strength steel by using a linear cutting process;
and grinding the sample obtained by linear cutting on silicon oxide abrasive paper, wherein the abrasive paper grinding is sequentially 200, 400, 600, 800, 1000 to 1500, and the polishing agent is 2.5 mu m diamond polishing agent until the surface of the sample is flat and has no scratch.
And (3) carrying out vibration polishing treatment on the mechanically polished sample, wherein the vibration polishing process parameters are as follows: vibration frequency: 1000-10000 Hz, 460g of applied load and 5h of polishing time, and the used polishing solution is sol-gel alumina polishing suspension with the granularity of 0.05 μm.
And after the vibration polishing is finished, washing the surface of the sample to be clean until no polishing solution is left on the surface.
As shown in fig. 3, the white non-structured area is an EBSD unmarked area, and the final EBSD mark rate is 40%.
Comparative example 2
Cutting an EBSD sample to be detected on the martensite high-strength steel by using a linear cutting process;
and grinding the sample obtained by linear cutting on silicon oxide abrasive paper, wherein the abrasive paper grinding is sequentially 200, 400, 600, 800, 1000 to 1500, and the polishing agent is 2.5 mu m diamond polishing agent until the surface of the sample is flat and has no scratch.
And (3) carrying out vibration polishing treatment on the mechanically polished sample, wherein the vibration polishing process parameters are as follows: vibration frequency: 1000-10000 Hz, 460g of applied load and 7h of polishing time, and the used polishing solution is sol-gel alumina polishing suspension with the granularity of 0.05 μm.
And after the vibration polishing is finished, washing the surface of the sample to be clean until no polishing solution is left on the surface.
As shown in fig. 4, the white non-structured area is an EBSD unmarked area, and the final EBSD mark rate is 60%.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. The method for preparing the martensite high-strength steel EBSD sample is characterized by comprising the following steps of:
cutting an EBSD sample to be detected on the martensite high-strength steel by using linear cutting;
performing mechanical polishing treatment on the EBSD sample to be detected;
carrying out chemical corrosion on the mechanically polished EBSD sample to be detected;
carrying out vibration polishing treatment on the EBSD to-be-detected sample which is chemically corroded;
and after the vibration polishing is finished, washing and cleaning the surface of the sample to be detected for EBSD until no polishing solution is left on the surface.
2. The method for preparing the martensitic high-strength steel EBSD sample according to claim 1, wherein the mechanical polishing treatment is carried out on the sample to be detected for EBSD, and the method comprises the following steps:
grinding the EBSD sample to be detected obtained by linear cutting on silicon oxide abrasive paper, wherein the abrasive paper grinding is sequentially from 200 meshes, 400 meshes, 600 meshes, 800 meshes, 1000 meshes to 1500 meshes, and the polishing agent is a diamond polishing agent with the particle size of 2.5 mu m until the surface of the sample is flat and has no scratch.
3. The method for preparing the martensitic high-strength steel EBSD sample according to claim 2, wherein the chemical corrosion is carried out on the sample to be detected of the EBSD which is mechanically polished, and the method comprises the following steps:
preparing a chemical corrosive agent;
and (3) carrying out titration corrosion on the EBSD sample to be detected by using a chemical corrosive, wherein the corrosion time is 10-30 s.
4. The method for preparing the martensitic high-strength steel EBSD sample according to claim 3, wherein the chemical etchant is prepared according to the proportion of 3.5g FeCl 3 、1gCuCl 2 50mL of anhydrous ethanol, 50mL of distilled water and 2.5mL of anhydrous ethanol 3 。
5. The method for preparing the martensitic high-strength steel EBSD sample according to claim 4, wherein the step of preparing the chemical corrosive comprises the following steps:
distilled water was placed in a beaker, and 99% absolute ethanol for analysis, 99% concentrated HCl for analysis, and 99% concentrated HNO for analysis were added to distilled water in this order 3 、FeCl 3 And CuCl 2 Fully stirring, uniformly mixing and cooling for later use.
6. The martensite high-strength steel EBSD sample preparation method according to claim 1, wherein the vibration polishing treatment is carried out on the sample to be detected of EBSD which is subjected to chemical corrosion, and the method comprises the following steps:
and (5) using a vibration polishing machine to perform vibration polishing on the EBSD sample to be detected.
7. The method for preparing the martensitic high-strength steel EBSD sample according to claim 6, wherein the vibration polishing process parameters of the vibration polishing machine are as follows:
the vibration frequency is 1000-10000 Hz;
the applied load is 400-500 g, and the polishing time is 4-5 h;
the polishing solution used by the vibration polishing machine is sol-gel alumina polishing suspension with the granularity of 0.04-0.05 mu m.
8. The method for preparing the martensitic high-strength steel EBSD sample according to claim 1, further comprising the following steps:
and washing and cleaning the surface of the EBSD sample to be detected until no polishing solution is left on the surface, and analyzing the EBSD sample to be detected through EBSD to obtain the EBSD calibration rate.
9. The martensitic high-strength steel EBSD sample preparation method as claimed in any one of claims 1 to 8, wherein the cutting wire for wire cutting is a molybdenum wire.
10. The method for preparing the martensitic high-strength steel EBSD sample according to any one of claims 1 to 8, wherein the martensitic high-strength steel comprises low-carbon high-alloy secondary hardening type ultrahigh-strength martensitic steel, and the alloying elements of the low-carbon high-alloy secondary hardening type ultrahigh-strength martensitic steel comprise Cr, co and Mo.
CN202210843763.7A 2022-07-18 2022-07-18 Martensite high-strength steel EBSD sample preparation method Pending CN115406918A (en)

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