CN109855931A - A kind of preparation method of austenitic alloy EBSD sample - Google Patents
A kind of preparation method of austenitic alloy EBSD sample Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of austenitic alloy EBSD sample, the preparation method includes the sample preparation of austenitic alloy sample, polishing, polishing, essence is thrown, two steps are ultrasonically treated and drying process；The essence throws process, and smart throwing process uses the silica suspension of 20-50nm granularity, metallographical polishing machine revolving speed≤100 rev/min, and essence throws time >=10min；Two step is ultrasonically treated process, and sample is placed in 10-45 DEG C of 10%NaOH aqueous solution by the ultrasonic treatment first step to be cleaned by ultrasonic, scavenging period >=3min.The present invention does not need electrobrightening process compared with national standard GBT19501, is not required to purchase special equipment, reduces preparation link, simple and convenient, reduces costs；It effectively overcomes existing electrolytic polishing method and needs the problems such as professional equipment, sample preparation are at high cost, polishing process gropes long time and electrolyte contamination environment.
Description
Technical field
The invention belongs to the preparation fields of electron microscopic sample, and in particular to a kind of preparation side of austenitic alloy EBSD sample
Method.
Background technique
Austenitic alloy, including stainless steel and nickel-base alloy etc. are widely used in petroleum as key structure material, change
The industrial departments such as work, nuclear power.The sensibility for damaging material environment with complex stress coupling by corrosion in Service Environment
It greatly increases, and crystal boundary is the weak link of material, it is prone to fail.
Electron backscatter diffraction (EBSD) technology is based on electronic action in scanning electron microscope in inclined specimen surface institute shape
At Kikuchi style determine crystal structure, orientation and the method for other information, can be used for studying the crystalline substance of austenitic alloy
Boundary's feature and structure and the overstrain of grain boundaries etc..
The Kikuchi style that EBSD experiment obtains requires smooth specimen surface, cleaning, without strained layer, and common mechanical is thrown
The specimen surface of light is not able to satisfy experiment needs.National standard GBT19501 is recommended to use electrolytic polishing method system for metal material
Sample, this method sample preparation complex process need special equipment, need early period grope electrolyte ratio and electric current electricity plenty of time
Pressure, and cryogenic polishing energy consumption is high, electrolyte contamination environment.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation methods of austenitic alloy EBSD sample.
In order to solve the above technical problems, the technical solution used in the present invention is: a kind of austenitic alloy EBSD sample
Preparation method, the preparation method includes the sample preparation of austenitic alloy sample, polishing, polishing, essence is thrown, two steps are ultrasonically treated and drying
Process；The essence throws process, and smart throwing process uses the silica suspension of 20-50nm granularity, metallographical polishing machine revolving speed≤100
Rev/min, essence throws time >=10min；Two step is ultrasonically treated process, is ultrasonically treated the first step for sample and is placed in 10-45 DEG C
10%NaOH aqueous solution in be cleaned by ultrasonic, scavenging period >=3min.
Polishing operation of the present invention, bruting process successively use 80-150 mesh, 400-600 mesh, 800-1000 mesh and
2000-3000 mesh silicon carbide silicon carbide paper, metallographical polishing machine revolving speed≤400 rev/min, grinding effect are ground with removing preceding a time
Trace is good.
Polishing process of the present invention, polishing process successively use the Buddha's warrior attendant of 2.5-3.5 μm, 1-1.5 μm and 0.5 μm granularity
The polishing of stone antiscuffing paste, metallographical polishing machine revolving speed≤400 rev/min, effect is good to remove preceding a time sleek mark per pass
It is good, smooth, bright and clean surface can be obtained.
Two step of the present invention is ultrasonically treated process, and ultrasonic treatment second step places a sample into 10-55 DEG C of dehydrated alcohol
In be cleaned by ultrasonic, scavenging period >=5min.
NaOH of the present invention, dehydrated alcohol reagent be analyze it is pure.
Of the present invention with water is deionized water, and resistivity reaches 18.25M Ω/cm.
The applicable alloy microscopic structure of preparation method of the present invention is austenite equiax crystal, and crystal structure is vertical for the center of area
Square structure.
The EBSD sample of austenitic alloy of the present invention is clear through EBSD analysis picture quality, and different type crystal boundary is distinguished bright
It is aobvious.
The sample of the preparation method preparation of austenitic alloy EBSD sample of the present invention, the reference of EBSD Standard of analytical methods
GB/T 19501-2013。
The beneficial effects of adopting the technical scheme are that the smart throwing process of the 1, present invention is suspended using silica
Liquid carries out the mechanical-chemical polishing of final step, significantly shortens the sample preparation time.2, the present invention ultrasonic treatment first step is adopted
Nano particles of silicon dioxide of the smart throwing stage reunion on sample surfaces can be thoroughly cleaned with 10%NaOH aqueous solution, is cleaned
Surface.3, the present invention compared with national standard GBT19501, do not need electrobrightening process, that is, be not necessarily to electrolyte, clean and environmental protection, simultaneously
It is not required to purchase special equipment, reduces preparation link, it is simple and convenient, it reduces costs.4, the present invention effectively overcomes existing
Electrolytic polishing method needs the problems such as professional equipment, sample preparation are at high cost, polishing process gropes long time and electrolyte contamination environment.
Detailed description of the invention
Fig. 1 is that sample EBSD prepared by embodiment 1 analyzes Grain Boundary Character distribution map；
Fig. 2 is that sample EBSD prepared by embodiment 2 analyzes Grain Boundary Character distribution map；
Fig. 3 is that sample EBSD prepared by embodiment 3 analyzes Grain Boundary Character distribution map.
Specific embodiment
Present invention will be explained in further detail in the following with reference to the drawings and specific embodiments.
Embodiment 1
The preparation method of the present embodiment austenitic alloy EBSD sample includes the sample preparation of austenitic alloy sample, polishing, polishing, essence
It throws, two steps are ultrasonically treated and drying process, specific process step are as described below:
(1) sample preparation process: 316L austenite stainless steel curved beam is through Wire EDM sample preparation；
(2) polishing operation: bruting process successively uses 150 mesh, 400 mesh, 1000 mesh and 2000 mesh silicon carbide silicon carbide papers to examination
Sample progress four-pass polishing, 300 revs/min of metallographical polishing machine revolving speed；
(3) polishing process: polishing process successively use the diamond polishing cream of 2.5 μm, 1.5 μm and 0.5 μm granularities to sample into
The polishing of three passage of row, metallographical polishing machine revolving speed are 400 revs/min；
(4) essence throws process: washing with water surface after grinding and polishing, then carries out smart throwing process, essence throws the silica for using 40nm granularity
Suspension, metallographical polishing machine revolving speed are 60 revs/min, time 10min；
(5) two steps are ultrasonically treated process: essence carries out ultrasonication after throwing, and sample is placed in 15 DEG C of 10%NaOH water first
Ultrasonic cleaning 3min is carried out in solution, then sample is placed in 20 DEG C of dehydrated alcohol and is carried out ultrasonic cleaning 10min；
(6) dry up process: sample dries up the ethyl alcohol of specimen surface with hair dryer after ultrasonic treatment, carries out EBSD experiment.
It is FEI-XL30 type that EBSD, which tests scanning electron microscope used, and EBSD analysis system is TSL-OIM software, and acceleration voltage is
15KV.Fig. 1 is the Grain Boundary Character distribution map of the present embodiment 316L austenitic stainless steel EBSD, and as seen from Figure 1, picture quality is clear
Clear, different type crystal boundary is distinguished obviously, and calibration rate is more than 90%.
Embodiment 2
The preparation method of the present embodiment austenitic alloy EBSD sample includes the sample preparation of austenitic alloy sample, polishing, polishing, essence
It throws, two steps are ultrasonically treated and drying process, specific process step are as described below:
(1) sample preparation process: 600 austenite stainless steel curved beam of Inconel is through Wire EDM sample preparation；
(2) polishing operation: bruting process successively uses 80 mesh, 600 mesh, 800 mesh and 3000 mesh silicon carbide silicon carbide papers to sample
Progress four-pass polishing, 400 revs/min of metallographical polishing machine revolving speed；
(3) polishing process: polishing process successively use the diamond polishing cream of 3.5 μm, 1.0 μm and 0.5 μm granularities to sample into
The polishing of three passage of row, metallographical polishing machine revolving speed are 400 revs/min；
(4) essence throws process: washing with water surface after grinding and polishing, then carries out smart throwing process, essence throws the silica for using 30nm granularity
Suspension, metallographical polishing machine revolving speed are 50 revs/min, time 15min；
(5) two steps are ultrasonically treated process: essence carries out ultrasonication after throwing, and sample is placed in 20 DEG C of 10%NaOH water first
Ultrasonic cleaning 5min is carried out in solution, then sample is placed in 30 DEG C of dehydrated alcohol and is carried out ultrasonic cleaning 5min；
(6) dry up process: sample dries up the ethyl alcohol of specimen surface with hair dryer after ultrasonic treatment, carries out EBSD experiment.
It is LEO-1450 type that EBSD, which tests scanning electron microscope used, and EBSD analysis system is 5 type of HKL Channel, accelerates electricity
Pressure is 20KV.Fig. 2 is the Grain Boundary Character distribution map of 600 austenitic alloy welding heat affected zone EBSD of the present embodiment Inconel,
From Figure 2 it can be seen that picture quality is clear, different type crystal boundary is distinguished obviously, and calibration rate is more than 90%.
Embodiment 3
The preparation method of the present embodiment austenitic alloy EBSD sample includes the sample preparation of austenitic alloy sample, polishing, polishing, essence
It throws, two steps are ultrasonically treated and drying process, specific process step are as described below:
(1) sample preparation process: 304 austenite stainless steel curved beams are through Wire EDM sample preparation；
(2) polishing operation: bruting process successively uses 80 mesh, 400 mesh, 800 mesh and 2000 mesh silicon carbide silicon carbide papers to sample
Progress four-pass polishing, 375 revs/min of metallographical polishing machine revolving speed；
(3) polishing process: polishing process successively use the diamond polishing cream of 3.5 μm, 1.5 μm and 0.5 μm granularities to sample into
The polishing of three passage of row, metallographical polishing machine revolving speed are 300 revs/min；
(4) essence throws process: washing with water surface after grinding and polishing, then carries out smart throwing process, essence throws the silica for using 50nm granularity
Suspension, metallographical polishing machine revolving speed are 100 revs/min, time 12min；
(5) two steps are ultrasonically treated process: essence carries out ultrasonication after throwing, and sample is placed in 25 DEG C of 10%NaOH water first
Ultrasonic cleaning 4min is carried out in solution, then sample is placed in 40 DEG C of dehydrated alcohol and is carried out ultrasonic cleaning 6min；
(6) dry up process: sample dries up the ethyl alcohol of specimen surface with hair dryer after ultrasonic treatment, carries out EBSD experiment.
It is FEI-XL30 type that EBSD, which tests scanning electron microscope used, and EBSD analysis system is TSL-OIM type, and acceleration voltage is
20KV.Fig. 3 is the Grain Boundary Character distribution map of 304 austenitic stainless steel EBSD of the present embodiment, and as seen from Figure 3, picture quality is clear,
Different type crystal boundary is distinguished obviously, and calibration rate is more than 95%.
Embodiment 4
The preparation method of the present embodiment austenitic alloy EBSD sample includes the sample preparation of austenitic alloy sample, polishing, polishing, essence
It throws, two steps are ultrasonically treated and drying process, specific process step are as described below:
(1) sample preparation process: 304 austenite stainless steel curved beams are through Wire EDM sample preparation；
(2) polishing operation: bruting process successively uses 100 mesh, 500 mesh, 1000 mesh and 2000 mesh silicon carbide silicon carbide papers to examination
Sample progress four-pass polishing, 330 revs/min of metallographical polishing machine revolving speed；
(3) polishing process: polishing process successively use the diamond polishing cream of 3.0 μm, 1.0 μm and 0.5 μm granularities to sample into
The polishing of three passage of row, metallographical polishing machine revolving speed are 350 revs/min；
(4) essence throws process: washing with water surface after grinding and polishing, then carries out smart throwing process, essence throws the silica for using 25nm granularity
Suspension, metallographical polishing machine revolving speed are 80 revs/min, time 12min；
(5) two steps are ultrasonically treated process: essence carries out ultrasonication after throwing, and sample is placed in 35 DEG C of 10%NaOH water first
Ultrasonic cleaning 6min is carried out in solution, then sample is placed in 50 DEG C of dehydrated alcohol and is carried out ultrasonic cleaning 8min；
(6) dry up process: sample dries up the ethyl alcohol of specimen surface with hair dryer after ultrasonic treatment, carries out EBSD experiment.
It is LEO-1450 type that EBSD, which tests scanning electron microscope used, and EBSD analysis system is 4 type of HKL-Channel, accelerates electricity
Pressure is 20KV.The Grain Boundary Character distribution map of 304 austenitic stainless steel EBSD of the present embodiment is similar with Fig. 3, therefore omits, picture quality
Clearly, different type crystal boundary is distinguished obvious, and calibration rate is more than 93%.
Embodiment 5
The preparation method of the present embodiment austenitic alloy EBSD sample includes the sample preparation of austenitic alloy sample, polishing, polishing, essence
It throws, two steps are ultrasonically treated and drying process, specific process step are as described below:
(1) sample preparation process: 316 austenite stainless steel curved beams are through Wire EDM sample preparation；
(2) polishing operation: bruting process successively uses 120 mesh, 400 mesh, 800 mesh and 2000 mesh silicon carbide silicon carbide papers to sample
Progress four-pass polishing, 200 revs/min of metallographical polishing machine revolving speed；
(3) polishing process: polishing process successively use the diamond polishing cream of 2.5 μm, 1.0 μm and 0.5 μm granularities to sample into
The polishing of three passage of row, metallographical polishing machine revolving speed are 240 revs/min；
(4) essence throws process: washing with water surface after grinding and polishing, then carries out smart throwing process, essence throws the silica for using 20nm granularity
Suspension, metallographical polishing machine revolving speed are 65 revs/min, time 13min；
(5) two steps are ultrasonically treated process: essence carries out ultrasonication after throwing, and sample is placed in 10 DEG C of 10%NaOH water first
Ultrasonic cleaning 9min is carried out in solution, then sample is placed in 10 DEG C of dehydrated alcohol and is carried out ultrasonic cleaning 12min；
(6) dry up process: sample dries up the ethyl alcohol of specimen surface with hair dryer after ultrasonic treatment, carries out EBSD experiment.
It is LEO-1450 type that EBSD, which tests scanning electron microscope used, and EBSD analysis system is 5 type of HKL Channel, accelerates electricity
Pressure is 20KV.The Grain Boundary Character distribution map of the present embodiment 316L austenitic stainless steel EBSD is similar with Fig. 1, therefore omits, image matter
Amount is clear, and different type crystal boundary is distinguished obviously, and calibration rate is more than 92%.
Embodiment 6
The preparation method of the present embodiment austenitic alloy EBSD sample includes the sample preparation of austenitic alloy sample, polishing, polishing, essence
It throws, two steps are ultrasonically treated and drying process, specific process step are as described below:
(1) sample preparation process: 308 austenite stainless steel curved beams are through Wire EDM sample preparation；
(2) polishing operation: bruting process successively uses 100 mesh, 500 mesh, 1000 mesh and 3000 mesh silicon carbide silicon carbide papers to examination
Sample progress four-pass polishing, 225 revs/min of metallographical polishing machine revolving speed；
(3) polishing process: polishing process successively use the diamond polishing cream of 2.5 μm, 1.5 μm and 0.5 μm granularities to sample into
The polishing of three passage of row, metallographical polishing machine revolving speed are 210 revs/min；
(4) essence throws process: washing with water surface after grinding and polishing, then carries out smart throwing process, essence throws the silica for using 35nm granularity
Suspension, metallographical polishing machine revolving speed are 45 revs/min, time 18min；
(5) two steps are ultrasonically treated process: essence carries out ultrasonication after throwing, and sample is placed in 45 DEG C of 10%NaOH water first
Ultrasonic cleaning 8min is carried out in solution, then sample is placed in 55 DEG C of dehydrated alcohol and is carried out ultrasonic cleaning 15min；
(6) dry up process: sample dries up the ethyl alcohol of specimen surface with hair dryer after ultrasonic treatment, carries out EBSD experiment.
It is LEO-1450 type that EBSD, which tests scanning electron microscope used, and EBSD analysis system is HKL-Tango type, and acceleration voltage is
20KV.The Grain Boundary Character distribution map of 308 austenitic stainless steel EBSD of the present embodiment is similar with Fig. 2, therefore omits, and picture quality is clear
Clear, different type crystal boundary is distinguished obviously, and calibration rate is more than 94%.
The above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although referring to above-described embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that: still the present invention can be modified or be waited
With replacement, without departing from the spirit or scope of the invention, or any substitutions, should all cover in power of the invention
In sharp claimed range.
Claims (7)
1. a kind of preparation method of austenitic alloy EBSD sample, which is characterized in that the preparation method includes austenitic alloy
Sample sample preparation, polishing, polishing, essence is thrown, two steps are ultrasonically treated and drying process；The essence throws process, and smart throwing process uses 20-
The silica suspension of 50nm granularity, metallographical polishing machine revolving speed≤100 rev/min, essence throw time >=10min；Two step
It is ultrasonically treated process, sample is placed in 10-45 DEG C of 10%NaOH aqueous solution by the ultrasonic treatment first step to be cleaned by ultrasonic, clearly
Wash the time >=3min.
2. a kind of preparation method of austenitic alloy EBSD sample according to claim 1, which is characterized in that the polishing
Process, bruting process successively use 80-150 mesh, 400-600 mesh, 800-1000 mesh and 2000-3000 mesh silicon carbide water milling
Paper, metallographical polishing machine revolving speed≤400 rev/min.
3. a kind of preparation method of austenitic alloy EBSD sample according to claim 1, which is characterized in that the polishing
Process, polishing process successively use the diamond polishing cream of 2.5-3.5 μm, 1-1.5 μm and 0.5 μm granularity to polish, metallic phase polishing
Machine revolving speed≤400 rev/min.
4. a kind of preparation method of austenitic alloy EBSD sample according to claim 1 to 3, feature exist
Process is ultrasonically treated in, two step, and ultrasonic treatment second step places a sample into 10-55 DEG C of dehydrated alcohol that carry out ultrasound clear
It washes, scavenging period >=5min.
5. a kind of preparation method of austenitic alloy EBSD sample according to claim 1 to 3, feature exist
In the NaOH, dehydrated alcohol reagent are that analysis is pure.
6. a kind of preparation method of austenitic alloy EBSD sample according to claim 1 to 3, feature exist
In described with water is deionized water, and resistivity reaches 18.25M Ω/cm.
7. a kind of preparation method of austenitic alloy EBSD sample according to claim 1 to 3, feature exist
In the applicable alloy microscopic structure of the preparation method is austenite equiax crystal, and crystal structure is face-centred cubic structure.
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| CN110618149A (en) * | 2019-10-17 | 2019-12-27 | 江苏理工学院 | Preparation method of magnesium alloy EBSD sample |
| CN112229860A (en) * | 2020-08-26 | 2021-01-15 | 东莞材料基因高等理工研究院 | Austenitic stainless steel electrolytic polishing method for EBSD test |
| CN113466272A (en) * | 2021-06-23 | 2021-10-01 | 太原理工大学 | Sample preparation method of ultrathin niobium strip EBSD sample |
| CN114235864A (en) * | 2021-11-11 | 2022-03-25 | 泛锐云智科技(郑州)有限公司 | Preparation method of bismuth alloy sample for EBSD test |
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| CN114235864A (en) * | 2021-11-11 | 2022-03-25 | 泛锐云智科技(郑州)有限公司 | Preparation method of bismuth alloy sample for EBSD test |
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