CN105928767A - Preparation method of nickel steel-containing sample for EBSD analysis - Google Patents
Preparation method of nickel steel-containing sample for EBSD analysis Download PDFInfo
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- CN105928767A CN105928767A CN201610239377.1A CN201610239377A CN105928767A CN 105928767 A CN105928767 A CN 105928767A CN 201610239377 A CN201610239377 A CN 201610239377A CN 105928767 A CN105928767 A CN 105928767A
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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
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Abstract
The invention discloses a preparation method of a nickel steel-containing sample for an EBSD analysis. The method comprises the following steps: rough machining of the nickel steel-containing sample, fine polishing after polishing and erosion, surface cleaning after fine polishing of the sample, and the sample for the EBSD analysis is obtained; the fine polishing process comprises the following steps: diamond suspension liquid is used for polishing the sample after polishing and erosion, and aluminum oxide suspension liquid is used for polishing the sample. Special sample preparation links are reduced for facilitating implementation; the fine polishing process can relieve stress; compared with the conventional polishing method, the method has the advantages of simplicity, saved time, reduced sample preparation cost, and improved sample preparation efficiency, and the sample has a high desorption rate which can meet the requirements of EBSD analysis. The method has high operability, so that sample preparation is simple and timesaving, and preparation efficiency of the sample is improved. The sample for the EBSD analysis has a high desorption rate and good stability, the calibrate rate of the sample reaches 90% or above, general demands are satisfied, and the effects are good.
Description
Technical field
The present invention relates to the preparation method of a kind of electron microscopic sample, a kind of preparation method containing nickel steel EBSD sample for analysis.
Background technology
EBSD (EBSD) technology is to tilt, based on electron beam in scanning electron microscope, the analysis of diffraction Kikuchi band that sample surfaces excites and formed, the data collected can draw orientation mapping figure OIM, pole figure and inverse pole figure, also can calculate orientation (poor) distribution function.EBSD technology just can obtain the substantial amounts of crystallography information about sample, such as: texture and misorientation analysis in a short period of time；Crystallite dimension and distribution of shapes analysis；Crystal boundary, subgrain and twin boundary property analysis；Strain and the analysis of recrystallization；The identification of phases and compare calculating etc., EBSD all originates from these information that EBSD is comprised to the research of a lot of materials.
By EBSD technology, sample is carried out observation analysis, it is necessary first to preparation meet EBSD analyze require sample, sample surfaces need smooth, cleaning, without residual stress；Due to the inclination of sample stage, need to reach applicable size and dimension；And electron microscopic observation to be met to also need to sample electric conductivity good, the bad sample of electric conductivity can affect EBSD to be observed.The preparation method of EBSD sample has Mechanical Method, chemical method, electrolysis, ion bombardment etc., although method is numerous, but owing to there is component of organization difference between every kind of material, the preparation effect of sample is also not quite similar.For ferrous materials, generally selecting mechanical polishing method or electrolysis, traditional mechanical polishing method generally requires the longest sample preparation time, and electrolysis because of in electrolyte choose and the electrolysis process of complexity causes the EBSD sample of preparation undesirable.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of quick, measured preparation method containing nickel steel EBSD sample for analysis of matter.
For solving above-mentioned technical problem, the technical solution used in the present invention is: the described sample containing nickel steel carries out essence throwing after roughing, polish attack, and essence throws the cleaned surface of sample, i.e. available described EBSD sample for analysis；Described essence throwing process is: first uses diamond suspension to be polished the sample after polish attack, then is polished sample with aluminum oxide suspension.
During essence of the present invention is thrown, in diamond suspension, the granularity of diamond is 1～2.5 micron.Polishing disk rotating speed when using diamond suspension polishing is 100r/min and following.
During essence of the present invention is thrown, in aluminum oxide suspension, the granularity of aluminium oxide is 0.05 micron and less.Polishing disk rotating speed when using aluminum oxide suspension polishing is 50～80r/min, and polishing time is not less than 15 minutes.
Polish attack process of the present invention: rough machined study first polishes through diamond suspension, then immerse erosion in etchant.
During polish attack of the present invention, in diamond suspension, the granularity of diamond is 2.5～5 microns.During described polish attack, polishing disk rotating speed is 200～600r/min, and polishing time is 3～5min.
During polish attack of the present invention, aggressive agent is 4% nital.Described erosion time is no less than 30 seconds.
Use and have the beneficial effects that produced by technique scheme: the preparation process of sample of the present invention reduces special sample preparation link, it is simple to implement；Throwing process in essence and eliminate stress, more conventional polishing processes more simply saves time, and sample preparation cost reduces, and sample preparation efficiency improves, and sample has high resolution factor, can meet EBSD and analyze requirement.
The present invention has the highest operability, prepares that sample is simple, saves time, is greatly improved the preparation efficiency of sample.The EBSD sample for analysis using the present invention to prepare has higher resolution factor, and stability is high, and sample demarcation rate reaches more than 90%, meets primary demand, respond well.
Accompanying drawing explanation
The present invention is further detailed explanation with detailed description of the invention below in conjunction with the accompanying drawings.
Fig. 1 is the band contrast figure of the EBSD sample for analysis prepared by embodiment 1；
Fig. 2 is the distribution of orientations figure of the EBSD sample for analysis prepared by embodiment 1；
Fig. 3 is the band contrast figure of the EBSD sample for analysis prepared by embodiment 2；
Fig. 4 is the distribution of orientations figure of the EBSD sample for analysis prepared by embodiment 2；
Fig. 5 is the band contrast figure of the EBSD sample for analysis prepared by embodiment 3；
Fig. 6 is the distribution of orientations figure of the EBSD sample for analysis prepared by embodiment 3.
Detailed description of the invention
This preparation method containing nickel steel EBSD sample for analysis uses following method step to be prepared from:
(1) roughing process: described containing Ni content in nickel steel at 8.5wt%～9.5wt%, it is a kind of low-carbon (LC) quenched and tempered steel, it is organized as martensite and adds bainite, there is good toughness and intensity at low temperatures, be the main material for manufacturing LNG tank and ships that transport.
Preparing sample with metallographic sample preparation requirement, sample is processed into suitable size, sequentially pass through 240#, 400#, 800# and polish with 1000# waterproof abrasive paper, during corase grind, sample is next sand paper replaceable after one sand paper mark is completely covered；After changing sand paper, sample needs 90-degree rotation direction；Finally obtain study.This process does not introduce new sample preparation requirement, and main purpose is in order to sample preparation can be simply effective, sample final test will be made to be affected because special sample preparation requires unmet.
(2) polish attack process: be polished study on buffing machine, polishing disk rotating speed is 200～600r/min, and polishing uses the diamond suspension of the granularity of 2.5～5 microns, and polishing time is 3～5min；Specimen surface light after polishing is seamless, rinses with clear water afterwards, then rinses surface with anhydrous alcohol, dries up with hair-dryer.
Being immersed in aggressive agent by the most polished sample, aggressive agent uses the alcoholic solution of 4% nitric acid, and after corroding 10～20 seconds, polished surface gradually tarnishes, and in order to ensure the demarcation rate of EBSD, erosion time is no less than 30 seconds；Finally obtain erosion sample.Increasing erosion time, Main Function is the erosion in order to deepen sample surfaces, fully gets rid of Surface stress layer, and observing sample under metallographic was erosion state.
(3) essence throwing process: uses the diamond suspension of 1～2.5 micron to be polished corroding sample, skims the surface erosion vestige of erosion sample, makes sample again present light, and polishing disk rotating speed is 100r/min and following；During polishing, flicking sample, make surface not produce bigger residual stress.
Then use 0.05 micron and following aluminum oxide suspension carry out essence throwing again to sample, and main purpose is to remove residual stress, and polishing rotating speed is 50～80r/min, and polishing time was not less than 15 minutes；I.e. available essence throws sample.
Essence throwing process is for removing the sample surfaces residual stress layer stage, sample re-polishing will be corroded, grinding and polishing in step (1) and step (2) can be produced stressor layers to eliminate, use 0.05 micron and the throwing of following aluminum oxide suspension essence, sample is thrown without the essence of residual stress in available surface.
(4) cleaning surface process: essence is thrown sample and dries, use alcohol washes surface, and dry up with hair-dryer, i.e. available described EBSD sample for analysis.The purpose of this process is cleaning sample surfaces, it is ensured that sample is not affected by surface blot when EBSD observes.
Using tempering state containing nickel steel in following embodiment, nickel content is at 8wt%；Scanning electron microscope uses the ULTRA55 field emission scanning electron microscope that Zeiss manufactures；Electron accelerating voltage is 20kV, and sample stage tilts 70 °, and electronic beam current aperture is 60 μm, and pole shoe to sample surfaces distance is 20mm.
Embodiment 1: the concrete technology of this preparation method containing nickel steel EBSD sample for analysis is as described below.
(1) roughing: prepare sample with metallographic sample preparation requirement, sequentially passes through the polishing of 240#, 400#, 800# and 1000# waterproof abrasive paper.
(2) polish attack: using the diamond suspension of 2.5 micron granularities, polishing disk rotating speed is 400r/min, and polishing time is 5min；Aggressive agent uses the alcoholic solution of 4% nitric acid, and erosion time is 40 seconds.
(3) essence is thrown: using the diamond suspension of 1 micron to be polished, polishing disk rotating speed is 100r/min.The aluminum oxide suspension using 0.05 micron polishes again, and polishing rotating speed is 70r/min, polishing time 20 minutes.
(4) cleaning surface: the sample handled well is dried, uses alcohol washes surface, and dry up with hair-dryer, obtain described EBSD sample for analysis.
The analytic band contrast figure of the present embodiment gained EBSD sample for analysis as it is shown in figure 1, EBSD distribution of orientations as shown in Figure 2；The resolution factor of the present embodiment gained EBSD sample for analysis is 93.51%, and in Fig. 2, grain contours is clear, and crystal boundary is obvious, can meet orientation calculation requirement, respond well.
Embodiment 2: the concrete technology of this preparation method containing nickel steel EBSD sample for analysis is as described below.
(1) roughing: prepare sample with metallographic sample preparation requirement, sequentially passes through the polishing of 240#, 400#, 800# and 1000# waterproof abrasive paper.
(2) polish attack: using the diamond suspension of 5 micron granularities, polishing disk rotating speed is 600r/min, and polishing time is 3min；Aggressive agent uses the alcoholic solution of 4% nitric acid, and erosion time is 30 seconds.
(3) essence is thrown: using the diamond suspension of 1.5 microns to be polished, polishing disk rotating speed is 80r/min.The aluminum oxide suspension using 0.05 micron polishes again, and polishing rotating speed is 80r/min, polishing time 15 minutes.
(4) cleaning surface: the sample handled well is dried, uses alcohol washes surface, and dry up with hair-dryer, obtain described EBSD sample for analysis.
The analytic band contrast figure of the present embodiment gained EBSD sample for analysis as it is shown on figure 3, EBSD distribution of orientations as shown in Figure 4；The resolution factor of the present embodiment gained EBSD sample for analysis is 92.24%, and in Fig. 4, grain contours is clear, and crystal boundary is obvious, can meet orientation calculation requirement, respond well.
Embodiment 3: the concrete technology of this preparation method containing nickel steel EBSD sample for analysis is as described below.
(1) roughing: prepare sample with metallographic sample preparation requirement, sequentially passes through the polishing of 240#, 400#, 800# and 1000# waterproof abrasive paper.
(2) polish attack: using the diamond suspension of 4 micron granularities, polishing disk rotating speed is 200r/min, and polishing time is 4min；Aggressive agent uses the alcoholic solution of 4% nitric acid, and erosion time is 50 seconds.
(3) essence is thrown: using the diamond suspension of 2.5 microns to be polished, polishing disk rotating speed is 90r/min.The aluminum oxide suspension using 0.05 micron polishes again, and polishing rotating speed is 50r/min, polishing time 17 minutes.
(4) cleaning surface: the sample handled well is dried, uses alcohol washes surface, and dry up with hair-dryer, obtain described EBSD sample for analysis.
The band contrast figure of the present embodiment gained EBSD sample for analysis as it is shown in figure 5, EBSD distribution of orientations as shown in Figure 6；The resolution factor of the present embodiment gained EBSD sample for analysis is 86.23%, example three is shown as the EBSD analysis at around defect, owing to fault location is that null solution analyses point, total resolution factor is caused slightly to decline, but Fig. 6 shows that grain contours is the most obvious, the sample effect that the method is prepared by defect is the least, and sample preparation effect is good.
Claims (10)
1. the preparation method containing nickel steel EBSD sample for analysis, it is characterised in that: the described sample containing nickel steel carries out essence throwing after roughing, polish attack, and essence throws the cleaned surface of sample, i.e. available described EBSD sample for analysis；Described essence throwing process is: first uses diamond suspension to be polished the sample after polish attack, then is polished sample with aluminum oxide suspension.
Preparation method containing nickel steel EBSD sample for analysis the most according to claim 1, it is characterised in that: during described essence is thrown, in diamond suspension, the granularity of diamond is 1～2.5 micron.
Preparation method containing nickel steel EBSD sample for analysis the most according to claim 2, it is characterised in that: polishing disk rotating speed when using diamond suspension polishing is 100r/min and following.
Preparation method containing nickel steel EBSD sample for analysis the most according to claim 1, it is characterised in that: during described essence is thrown, in aluminum oxide suspension, the granularity of aluminium oxide is 0.05 micron and less.
Preparation method containing nickel steel EBSD sample for analysis the most according to claim 4, it is characterised in that: polishing disk rotating speed when using aluminum oxide suspension polishing is 50～80r/min, and polishing time is not less than 15 minutes.
6. according to the preparation method containing nickel steel EBSD sample for analysis described in claim 1-5 any one, it is characterised in that described polish attack process: rough machined study first polishes through diamond suspension, then immerse erosion in etchant.
Preparation method containing nickel steel EBSD sample for analysis the most according to claim 6, it is characterised in that: during described polish attack, in diamond suspension, the granularity of diamond is 2.5～5 microns.
Preparation method containing nickel steel EBSD sample for analysis the most according to claim 7, it is characterised in that: during described polish attack, polishing disk rotating speed is 200～600r/min, and polishing time is 3～5min.
Preparation method containing nickel steel EBSD sample for analysis the most according to claim 6, it is characterised in that: during described polish attack, aggressive agent is 4% nital.
Preparation method containing nickel steel EBSD sample for analysis the most according to claim 9, it is characterised in that: described erosion time is no less than 30 seconds.
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Cited By (6)
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| CN106840744A (en) * | 2017-03-02 | 2017-06-13 | 河钢股份有限公司 | A kind of preparation method of mild steel EBSD sample for analysis |
| CN107063786A (en) * | 2016-12-06 | 2017-08-18 | 重庆大学 | A kind of preparation method of nanometer gradient structural material top layer EBSD samples |
| CN107543819A (en) * | 2017-08-29 | 2018-01-05 | 中核四0四有限公司 | MOX pellet metallographic detection methods |
| CN109030134A (en) * | 2018-06-15 | 2018-12-18 | 燕山大学 | The preparation method of high nitrogen and nickel-less austenitic stainless steel EBSD sample |
| CN109839393A (en) * | 2019-03-22 | 2019-06-04 | 南京理工大学 | Slicker solder and its composite material or its alloy electron backscatter diffraction sample preparation technique |
| CN113532978A (en) * | 2021-06-07 | 2021-10-22 | 广西柳钢华创科技研发有限公司 | EBSD sample preparation method for iron and steel material scale |
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| CN109839393A (en) * | 2019-03-22 | 2019-06-04 | 南京理工大学 | Slicker solder and its composite material or its alloy electron backscatter diffraction sample preparation technique |
| CN113532978A (en) * | 2021-06-07 | 2021-10-22 | 广西柳钢华创科技研发有限公司 | EBSD sample preparation method for iron and steel material scale |
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