CN109030134A - The preparation method of high nitrogen and nickel-less austenitic stainless steel EBSD sample - Google Patents
The preparation method of high nitrogen and nickel-less austenitic stainless steel EBSD sample Download PDFInfo
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- CN109030134A CN109030134A CN201810617275.8A CN201810617275A CN109030134A CN 109030134 A CN109030134 A CN 109030134A CN 201810617275 A CN201810617275 A CN 201810617275A CN 109030134 A CN109030134 A CN 109030134A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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Abstract
A kind of preparation method of high nitrogen and nickel-less austenitic stainless steel EBSD sample mainly processes the sample to grinding and polishing with NC wirecut EDM machine and inlays sample with epoxy resin；First polished 3~5 minutes with 4000# sand paper；It uses the diamond paste of W0.1 as polishing agent again, just throws 1 minute；Using the colloidal silicon dioxide that the widely applied partial size in silicon wafer polishing field is 20nm as polishing fluid, finishing polish is carried out to the sample just thrown；900~1400 revs/min of polishing machine revolving speed, sample is located at away from polishing 20~50mm of disk center, and polishing drop speed is 5~10 ml/mins, total polishing time 5~10 minutes；EBSD sample distilled water flushing is clean, drying.The present invention is at low cost, high-efficient, is easy to grasp, suitable for deformation states, annealed state high nitrogen and nickel-less austenitic stainless steel inside, the observation of mantle micro structure, the sample there are crackle is also suitable.
Description
Technical field
The present invention relates to metal physical and chemical inspection methods, the especially preparation method of stainless steel EBSD sample.
Background technique
High nitrogen and nickel-less austenitic stainless steel is that nickel expensive in tradition AISI300 series austenitic stainless steel is replaced with nitrogen
Element.The solution strengthening effect of nitrogen is very strong, improves the work hardening rate of steel, can get very high good tough combination.Nitrogen is to expand
The element of big austenitic area, high nitrogen and nickel-less austenitic stainless steel even large deformation at quite low temperatures are also less prone to and answer
Become induced martensite, what can be kept is nonmagnetic.Moreover, nitrogen can improve resistance to spot corrosion and the slit and corrosion resistant energy of material
Power.High nitrogen and nickel-less austenitic stainless steel is applied more and more widely in the energy, is changed because of its excellent performance and cheap price
Work, machinery and health field.
In the casting of high nitrogen and nickel-less austenitic stainless steel, powder metallurgy, forging, rolling, punching press, heat treatment and crystal boundary work
During journey processing, it is often necessary to carry out institutional framework inspection to workpiece or part, EBSD (backscattered electron diffraction) is very
A kind of strong detection means.Analyzed by EBSD, can obtain crystallite dimension and orientation, texture, crystal boundary type, Taylor because
The results such as son distribution.However, high nitrogen and nickel-less austenitic stainless steel is softer, and when preparing EBSD sample, conventional grinding and polishing
Program, it is difficult to obtain smooth, bright and clean, without residual stress sample surfaces.EBSD sample surfaces quality is bad, can be to high-nitrogen nickel-free
Austenitic stainless steel EBSD analysis brings very big adverse effect.
Summary of the invention
It not only can get smooth, bright and clean, without residual stress sample surfaces, Er Qiezhi the object of the present invention is to provide a kind of
The preparation method of amount stability high nitrogen and nickel-less austenitic stainless steel EBSD sample that is high, at low cost, being easy to grasp.
Technical solution of the present invention is specific as follows:
Step 1, the sample to grinding and polishing is processed with NC wirecut EDM machine, 2~3mm of thickness of sample, sample is long
5~10mm, length 2mm long compared with width are spent, it is optimal having a size of 6mm × 4mm × 2mm.
Step 2, sample step 1 processed is inlayed with epoxy resin, 15~30mm of diameter of inlaying samples, with a thickness of straight
The 1/2~2/3 of diameter, it is optimal having a size of 20 × 10mm of Φ.
Step 3, with 4000# sand paper polish 3~5 minutes, until sample surfaces wire cutting oxidation decoloration, be covered with mill
Trace；Bruting process takes common tap water and washes away abrasive dust on sand paper.
Step 4, attached flannelette is added on rotary polisher polishing disk, uses the diamond paste of W0.1 as polishing agent, just
It throws 1 minute.
Step 5, attached flannelette is added on rotary polisher polishing disk, is 20nm by the widely applied partial size in silicon wafer polishing field
Colloidal silicon dioxide as polishing fluid, the sample that step 4 was just thrown carries out finishing polish；900~1400 turns of polishing machine revolving speed/
Minute, sample is located at away from polishing 20~50mm of disk center, and polishing drop speed is 5~10 ml/mins, polishing fluid dripping position
It is polishing sample close to polishing disk center of circle side, every 1 minute with 100ml distilled water flushing polishing disk, total polishing time 5~10
Minute.
Step 6, the inlay of sample is crushed after being thrown step 5 essence with mechanical force, and EBSD sample distilled water flushing is clean,
Drying.
The invention has the following advantages over the prior art:
(1) CNC WEDM processing to grinding and polishing sample, size meets the testing requirements of EBSD equipment, and just
In judging sample position and direction from sample topography；
(2) the sample size after inlaying is easily guaranteed that buffed surface is smooth convenient for hand-held polishing, is easy to grasp.
(3) high nitrogen and nickel-less austenitic stainless steel quality is softer, directly with 4000# sand paper polish, can in 3~5 minutes incite somebody to action
The oxide layer of wire cutting section is cut, and efficiency is good many by number mode of polishing compared with by low sand paper to height sand paper, and does not deposit
In the polishing of low sand paper, strained layer is difficult to the problem of being removed with height sand paper deeply very much.
(4) polishing fluid uses the widely applied partial size of silicon wafer manufacture field for the colloidal silicon dioxide of 20nm, cheap.
(5) angular speed, linear velocity, polishing fluid rate of addition this three it is reasonably combined, be able to achieve optimal essence and throw effect,
It was dumped every 1 minute with 10ml distilled water flushing, can avoid polishing fluid crystallization, lesioned sample surface.
(6) rotary machine polishing machine is used, it is much lower compared with using vibratory finishing machine cost.
(7) fracture edges and fractured edge can be kept bright and sharp.
(8) technology be suitable for inside the high nitrogen and nickel-less austenitic stainless steel of deformation states, annealed state, mantle micro structure
Observation, is also suitable the sample there are crackle.
Detailed description of the invention
Fig. 1 is high nitrogen and nickel-less austenitic stainless steel 18Mn18Cr0.5N steel, microscopic structure after annealing 1 hour at 1200 DEG C
EBSD mass contrast figure (Image quality figure), also known as Kikuchi lines contrast figure (Band contrast image).
Fig. 2 is high nitrogen and nickel-less austenitic stainless steel 18Mn18Cr0.5N steel, at 1000 DEG C with 0.01s-1After compression 30%
The EBSD mass contrast figure of microscopic structure.
Fig. 3 is high nitrogen and nickel-less austenitic stainless steel 18Mn18Cr0.6N steel, at 1100 DEG C with 0.001s-1After stretching 30%
The EBSD mass contrast figure of microscopic structure and crackle.
Fig. 4 is high nitrogen and nickel-less austenitic stainless steel 18Mn18Cr0.6N steel, at 1100 DEG C with 0.001s-1After breaking, fracture
The EBSD mass contrast figure of neighbouring microscopic structure.
Specific embodiment
Below by way of specific embodiment, the present invention will be described in detail.
Embodiment 1
By typical high nitrogen and nickel-less austenitic stainless steel 18Mn18Cr0.5N, anneal 1 hour at 1200 DEG C.
Step 1, the sample to grinding and polishing, thickness of sample 3mm, sample length are processed with NC wirecut EDM machine
10mm, width 8mm.
Step 2, sample step 1 processed is inlayed with epoxy resin, the diameter 30mm of inlaying samples, with a thickness of 15mm.
Step 3, with 4000# sand paper polish 5 minutes, until sample surfaces wire cutting oxidation decoloration, be covered with polishing scratch；It beats
Honed journey takes common tap water and washes away abrasive dust on sand paper.
Step 4, attached flannelette is added on rotary polisher polishing disk, uses the diamond paste of W0.1 as polishing agent, just
It throws 1 minute.
Step 5, attached flannelette is added on rotary polisher polishing disk, is 20nm by the widely applied partial size in silicon wafer polishing field
Colloidal silicon dioxide as polishing fluid, the sample that step 4 was just thrown carries out finishing polish；1400 revs/min of polishing machine revolving speed,
Sample is located at away from polishing disk center 50mm, and polishing drop speed is 10 ml/mins, and polishing fluid dripping position is that polishing sample leans on
Nearly polishing disk center of circle side, every 1 minute with 100ml distilled water flushing polishing disk, total polishing time 10 minutes.
Step 6, the inlay of sample is crushed after being thrown step 5 essence with mechanical force, and EBSD sample distilled water flushing is clean,
Drying.
The EBSD mass contrast figure of sample microscopic structure is polished as shown in Figure 1, being clear that crystal boundary and twin boundary.At
Image quality amount is very high, no marking, the residual stress without sample preparation introducing, smooth no relief.
Embodiment 2
By typical high nitrogen and nickel-less austenitic stainless steel 18Mn18Cr0.5N, at 1000 DEG C with 0.01s-1Compression 30%.
Step 1, the sample to grinding and polishing, thickness of sample 2mm, sample length are processed with NC wirecut EDM machine
5mm, the long 3mm of width.
Step 2, sample step 1 processed is inlayed with epoxy resin, the diameter 15mm of inlaying samples, with a thickness of diameter
10mm。
Step 3, with 4000# sand paper polish 3 minutes, until sample surfaces wire cutting oxidation decoloration, be covered with polishing scratch；It beats
Honed journey takes common tap water and washes away abrasive dust on sand paper.
Step 4, attached flannelette is added on rotary polisher polishing disk, uses the diamond paste of W0.1 as polishing agent, just
It throws 1 minute.
Step 5, attached flannelette is added on rotary polisher polishing disk, is 20nm by the widely applied partial size in silicon wafer polishing field
Colloidal silicon dioxide as polishing fluid, the sample that step 4 was just thrown carries out finishing polish；900 revs/min of polishing machine revolving speed,
Sample is located at away from polishing disk center 20, and polishing drop speed is 5 ml/mins, and polishing fluid dripping position is that polishing sample is close
Polishing disk center of circle side, every 1 minute with 100ml distilled water flushing polishing disk, total polishing time 5 minutes.
Step 6, the inlay of sample is crushed after being thrown step 5 essence with mechanical force, and EBSD sample distilled water flushing is clean,
Drying.
The EBSD mass contrast figure of sample microscopic structure is polished as shown in Fig. 2, being clear that sub boundary and crystal boundary.At
Image quality amount is very high, no marking, the residual stress without sample preparation introducing, smooth no relief.
Embodiment 3
By typical high nitrogen and nickel-less austenitic stainless steel 18Mn18Cr0.6N, at 1100 DEG C with 0.001s-1Stretch 30%.
Step 1, the sample to grinding and polishing is processed in necking down position with NC wirecut EDM machine, thickness of sample 2mm,
Sample is having a size of 6mm × 4mm × 2mm.
Step 2, sample step 1 processed is inlayed with epoxy resin, and the size of inlaying samples is 20 × 10mm of Φ.
Step 3, with 4000# sand paper polish 4 minutes, until sample surfaces wire cutting oxidation decoloration, be covered with polishing scratch；It beats
Honed journey takes common tap water and washes away abrasive dust on sand paper.
Step 4, attached flannelette is added on rotary polisher polishing disk, uses the diamond paste of W0.1 as polishing agent, just
It throws 1 minute.
Step 5, attached flannelette is added on rotary polisher polishing disk, is 20nm by the widely applied partial size in silicon wafer polishing field
Colloidal silicon dioxide as polishing fluid, the sample that step 4 was just thrown carries out finishing polish；1400 revs/min of polishing machine revolving speed,
Sample is located at away from polishing disk center 40mm, and polishing drop speed is 6 ml/mins, and polishing fluid dripping position is that polishing sample leans on
Nearly polishing disk center of circle side, every 1 minute with 100ml distilled water flushing polishing disk, total polishing time 8 minutes.
Step 6, the inlay of sample is crushed after being thrown step 5 essence with mechanical force, and EBSD sample distilled water flushing is clean,
Drying.
The EBSD mass contrast figure of sample microscopic structure is polished as shown in figure 3, being clear that the crackle of black, crackle
Extensions path includes along brilliant and transcrystalline.The sharpness of border of crackle, the crystal boundary and twin boundary in other regions are clearly demarcated, and image quality is very
Height, no marking, the residual stress without sample preparation introducing, smooth no relief.
Embodiment 4
By typical high nitrogen and nickel-less austenitic stainless steel 18Mn18Cr0.6N, at 1100 DEG C with 0.001s-1It stretches disconnected.
Step 1, the sample to grinding and polishing, sample are processed along sample axis in incision position with NC wirecut EDM machine
Thickness 2mm, sample length 6mm, width 4mm.
Step 2, sample step 1 processed is inlayed with epoxy resin, and the size of inlaying samples is 20 × 10mm of Φ.
Step 3, with 4000# sand paper polish 3 minutes, until sample surfaces wire cutting oxidation decoloration, be covered with polishing scratch；It beats
Honed journey takes common tap water and washes away abrasive dust on sand paper.
Step 4, attached flannelette is added on rotary polisher polishing disk, uses the diamond paste of W0.1 as polishing agent, just
It throws 1 minute.
Step 5, attached flannelette is added on rotary polisher polishing disk, is 20nm by the widely applied partial size in silicon wafer polishing field
Colloidal silicon dioxide as polishing fluid, the sample that step 4 was just thrown carries out finishing polish；900 revs/min of polishing machine revolving speed,
Sample is located at away from polishing disk center 40mm, and polishing drop speed is 8 ml/mins, and polishing fluid dripping position is that polishing sample leans on
Nearly polishing disk center of circle side, every 1 minute with 100ml distilled water flushing polishing disk, total polishing time 10 minutes.
Step 6, the inlay of sample is crushed after being thrown step 5 essence with mechanical force, and EBSD sample distilled water flushing is clean,
Drying.
The EBSD mass contrast figure of sample microscopic structure is polished as shown in figure 4, the black region in figure left side is except fracture.
It is clear that the small grains of fracture surface layer and the coarse grain far from fracture.Crystal boundary and twin boundary are clearly demarcated, at image quality
Measure very high, no marking, the residual stress without sample preparation introducing, smooth no relief.
Claims (3)
1. a kind of preparation method of high nitrogen and nickel-less austenitic stainless steel EBSD sample, it is characterised in that: the method includes following
Step:
Step 1, the sample to grinding and polishing is processed with NC wirecut EDM machine, 2~3mm of thickness of sample, sample length 5~
10mm, length 2mm long compared with width,
Step 2, sample step 1 processed is inlayed with epoxy resin, 15~30mm of diameter of inlaying samples, with a thickness of diameter
1/2~2/3,
Step 3, with 4000# sand paper polish 3~5 minutes, until sample surfaces wire cutting oxidation decoloration, be covered with polishing scratch；It beats
Honed journey takes common tap water and washes away abrasive dust on sand paper,
Step 4, attached flannelette is added on rotary polisher polishing disk, uses the diamond paste of W0.1 as polishing agent, just throws 1 point
Clock,
Step 5, attached flannelette is added on rotary polisher polishing disk, the glue for being 20nm by the widely applied partial size in silicon wafer polishing field
For state silica as polishing fluid, the sample that step 4 was just thrown carries out finishing polish；900~1400 revs/min of polishing machine revolving speed
Clock, sample are located at away from polishing 20~50mm of disk center, and polishing drop speed is 5~10 ml/mins, and polishing fluid dripping position is
Sample is polished close to polishing disk center of circle side, every 1 minute with 100ml distilled water flushing polishing disk, 5~10 points of total polishing time
Clock,
Step 6, the inlay of sample is crushed after being thrown step 5 essence with mechanical force, and EBSD sample distilled water flushing is clean, blows
It is dry.
2. the preparation method of high nitrogen and nickel-less austenitic stainless steel EBSD sample according to claim 1, it is characterised in that: sample
Product are optimal having a size of 6mm × 4mm × 2mm.
3. the preparation method of high nitrogen and nickel-less austenitic stainless steel EBSD sample according to claim 1, it is characterised in that: edge
Embedding sample is optimal having a size of 20 × 10mm of Φ.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109855931A (en) * | 2018-12-20 | 2019-06-07 | 河钢股份有限公司 | A kind of preparation method of austenitic alloy EBSD sample |
| CN111855337A (en) * | 2019-04-26 | 2020-10-30 | 国标（北京）检验认证有限公司 | Method for preparing high-purity ruthenium target EBSD sample |
| CN113046534A (en) * | 2021-03-15 | 2021-06-29 | 长春工业大学 | Preparation method of high-nitrogen nickel-free austenitic stainless steel with high twin crystal density |
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Application publication date: 20181218 |