CN107063797A - A kind of EBSD preparation method of sample of alloy thin band thickness x cross sectional - Google Patents
A kind of EBSD preparation method of sample of alloy thin band thickness x cross sectional Download PDFInfo
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- CN107063797A CN107063797A CN201710251085.4A CN201710251085A CN107063797A CN 107063797 A CN107063797 A CN 107063797A CN 201710251085 A CN201710251085 A CN 201710251085A CN 107063797 A CN107063797 A CN 107063797A
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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
- G01N1/32—Polishing; Etching
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention discloses a kind of EBSD preparation method of sample of alloy thin band thickness x cross sectional.The preparation method utilizes the two block length cube conducting metal blocks close with band alloy rigidity, and chilling is got rid of into the very thin sheet metal strip that band obtains is clamped in two pieces of conducting metal blocks, two block length cube conducting metal blocks and strip is fixed together.The thickness x cross sectional level for making alloy thin band parallel with conducting metal block downwards, is placed in hot edge machine vertically.Then it is embedded in using hot edge method in conductive mosaic powder, and after being roughly ground on abrasive paper for metallograph, recycle hot edge method that its entirety is set into the cylinder with certain diameter and height, then Mechanical polishing light and vibropolish are carried out and removes Surface stress layer, prepare excellent surface quality, thickness only have tens microns strip thickness x cross sectional EBSD sample.Prepare good, the characteristics of demarcation rate of EBSD is high of the conductive energy of sample.
Description
Technical field
The present invention relates to micro-analysis characterization technique field, specifically, it is related to a kind of electricity of alloy thin band thickness x cross sectional
Sub- back scattering diffraction preparation method of sample.
Background technology
In recent years, electron backscattered style (Electron Back-scattering Patterns, abbreviation EBSP) crystal
Microcell is orientated and the analytical technology of crystal structure achieves larger development, and in microstructure and micro- texture table
Levy middle extensive use, the technology be also referred to as EBSD (Electron Backscattered Diffraction,
Abbreviation EBSD).EBSD is characterized in carry out space while the conventional feature of SEM is retained
Resolution ratio is the data for providing crystallography for the diffraction of submicron order, it has also become a kind of effective analysis means in investigation of materials.
But backscattered electron only occurs in the depth bounds of tens nanometers in sample top layer, so overstrain layer, the oxygen of specimen surface
Change the generation that the defect such as film and etch pit can all influence or even completely inhibit diffraction Kikuchi lines, therefore the preparation matter of specimen surface
Amount is largely fixed the quality of EBSD.Compared with general metallographic specimen, a qualified electronics back of the body
Scattering and diffracting sample, it is desirable to specimen surface is unstressed layer, non-oxidation layer, can not excessive, table without continuous etch pit, surface undulation
Clean without dirt in face.EBSD sample preparation is the particularly significant and work that acquires a certain degree of difficulty of tool.At present, electronics is prepared
The main method of back scattering diffraction sample has:Mechanical polishing, electrobrightening and ion etching.
The distribution of orientations of the crystal grain of material can directly affect the various performances of material, such as polycrystalline alloy with texture,
On different crystallographic directions, the performance of its each side can show significant difference, and this phenomenon is referred to as anisotropy, utilize
This anisotropic characteristic, the application of the expansible various materials of raising and performance.Patent of invention
CN201410157327.X discloses the sample preparation methods that a kind of Thin Specs ferrous materials carry out EBSD analysis,
This method takes the fritter plate face of Thin Specs ferrous materials as sample, is first fixed on sample on one cylinder with paraffin, then
The sample for being fixed on cylinder is ground, polished；Again by corrosion 3-15 seconds in nitric acid alcohol of the sample after polishing, finally
Sample can carry out observation analysis in EBSD equipment.This method is highly suitable for thickness and is no more than 0.5mm's
The EBSD of Thin Specs ferrous materials analyzes the preparation of sample.But this method is only applicable to prepare Thin Specs sample
Plate face and may not apply to thickness x cross sectional, the thickness x cross sectional of general sample includes whole orientation informations of sample, and the preparation
Method cannot be used for the sample that thickness is only tens microns, hardly result in the EBSD examination with excellent surface quality
Sample.
The content of the invention
In order to avoid the deficiency that prior art is present, the present invention proposes a kind of the electron backscattered of alloy thin band thickness x cross sectional
Diffraction preparation method of sample.The preparation method utilizes the two piece conducting metal blocks close with band alloy rigidity, by very thin gold
Belong to band clamping therebetween, recycle hot edge method that its entirety is set into the cylinder with certain diameter and height, then carry out
Mechanical polishing light and vibropolish remove Surface stress layer, prepare excellent surface quality, thickness there was only tens microns thin
The EBSD sample of the thickness x cross sectional of band；Sample is conductive can be good, and the demarcation rate of EBSD is high
The characteristics of.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of EBSD preparation method of sample of alloy thin band thickness x cross sectional, it is characterised in that including following step
Suddenly:
Step 1. chooses the straight unnotched alloy thin band of thickness x cross sectional；
Step 2. chooses two pieces of identical cuboid conducting metal blocks, and metal derby is consistent with selected alloy thin band length,
Hardness is close, makes the thickness face level of the alloy thin band of needs analysis downward and consistent with the plane of two pieces of conducting metal blocks, will
Alloy thin band is clamped between two pieces of conducting metal blocks；
Step 3. clamps two pieces of conducting metal blocks with tweezers, conducting metal block is tightly clamped alloy thin band, and in its back of the body
Glue is instilled between the gap of face, Quick-air-drying makes two pieces of conducting metal blocks be fixed together with alloy thin band；
The thickness x cross sectional level of the alloy thin band parallel with conducting metal block downwards, is placed on hot edge machine by step 4. vertically
In, pour into conductive mosaic powder and hide sample, cover pressure head, be heated up to 140 DEG C and apply pressure until definite value, 10 points of heat-insulation pressure keeping
Clock, turns off heater switch, waits and is cooled to room temperature, sheds pressure, takes out the sample inlayed, obtains cylindric sample；
Step 5. roughly grinds the cylinder sample inlayed on 600,1000,1200,1500,2000 mesh sand paper successively,
Demander is to consistent when being polished on one of sand paper, whne cut on sample in one direction when change sand paper, rotated when changing sand paper
90 degree；Mechanically polished again after corase grind, until cut is all removed；Then counterweight is added, is added in vibratory finishing machine
Silica gel solution, selection 30Hz vibration frequencies polish four hours, and taking-up is rinsed well with clear water, obtains the electricity in strip thickness section
Sub- back scattering diffraction sample.
Beneficial effect
The EBSD preparation method of sample of a kind of alloy thin band thickness x cross sectional proposed by the present invention, first by chilling
Get rid of the strip that band obtains to be clamped in two pieces of rectangular blocks of conducting metal consistent with its hardness, be then embedded in using hot edge method
In conductive mosaic powder, after being roughly ground on abrasive paper for metallograph, then polish through machinery and vibrations, obtain high electron backscattered of demarcation rate and spread out
Penetrate sample.
Its effect compared with prior art:(1) present invention only has the thickness x cross sectional of tens microns of strip suitable for thickness
EBSD sample preparation；(2) strip is clamped in the middle of cuboid metal derby, in heat edge, electricity need to be ensured
The section of the strip of sub- back scattering diffraction analysis is horizontal plane, is not toppled over, it is ensured that the analysis of later stage EBSD takes
To accuracy；(3) using hardness it is close cuboid metal derby clamping, make grind away process strip it is not chipping and polishing
Face is level；In later stage polishing process, it is ensured that the whole uniform unstressed layer of strip mirror polish；(4) using the clamping of conducting metal block,
And conductive powder of inlaying is inlayed, it is ensured that the electric conductivity of sample is good, when EBSD is gathered, will not occur charged
Effect, effectively improves demarcation rate.The EBSD sample of the thickness x cross sectional for the strip that the present invention is prepared has good
Good surface quality, unstressed layer, the good conductivity of sample, the demarcation rate of EBSD is up to more than 90%.
Brief description of the drawings
A kind of EBSD of alloy thin band thickness x cross sectional of the invention is tried with embodiment below in conjunction with the accompanying drawings
Sample preparation method is described in further detail.
Fig. 1 prepares the EBSD sample schematic diagram of alloy thin band thickness x cross sectional for the present invention, and a, b is respectively length
Cube metal derby clamps strip trailing flank and schematic bottom view, and c is to inlay the schematic bottom view that powder inlays rear sample with conductive.
Fig. 2 is the EBSD sample testing result for preparing NiMnIn alloy thin bands.
Fig. 3 is flow chart of the invention.
In figure
1. the conducting metal block 3. of alloy thin band 2. inlays powder
Embodiment
The present embodiment is a kind of EBSD preparation method of sample of alloy thin band thickness x cross sectional.
Refering to Fig. 1~Fig. 3, the strip that thickness only has tens microns is first clamped in two consistent with its hardness by the present embodiment
In the rectangular block of block conducting metal, protection sample will not be damaged in grinding and polishing process, be then embedded in conduction using hot edge method
Inlay be easy in powder the later stage Mechanical polishing and vibrations polish, on abrasive paper for metallograph roughly grind after, then through machinery and vibrations polishing go
Except Surface stress layer, the high EBSD sample of demarcation rate is obtained, recycles hot edge method that its entirety is set into one
Cylinder with definite value diameter and height, then carries out Mechanical polishing light and vibropolish removes Surface stress layer, prepares table
The thickness of face good quality only has the EBSD sample in tens microns of strip thickness section.
The specific method for preparing the EBSD sample of alloy thin band thickness x cross sectional is as follows:
First, the straight unnotched strip of complete, thickness x cross sectional is selected.
Secondly, make the thickness face level of the alloy thin band of needs analysis downward, it is flat with two block length cube conducting metal blocks
Face is consistent, and strip is clamped between two block length cube conducting metal blocks.
Then, two block length cube conducting metal blocks are clamped with tweezers, metal derby is tightly clamped alloy thin band, and at it
502 glue are instilled between the gap of the back side, quick drying makes two block length cube conducting metal blocks and strip be fixed together.
Then, the thickness x cross sectional level for the alloy thin band analyzed the need for will be parallel with conducting metal block downwards, is put vertically
In hot edge machine, pour into conductive mosaic powder and hide sample, cover pressure head, be heated up to 140 DEG C and apply pressure until maximum, insulation
Pressurize 10 minutes, turns off heater switch, waits and be cooled to room temperature, sheds pressure, takes out the sample inlayed, obtains cylindric examination
Sample.
Finally, by the cylinder sample inlayed, roughly ground successively on 600,1000,1200,1500,2000 mesh sand paper,
Mechanically polished again after corase grind, then plus counterweight, silica gel solution is added in vibratory finishing machine, 30Hz vibration frequencies are selected
Polishing four hours, taking-up is rinsed well with clear water, so as to obtain the EBSD sample in strip thickness section.
Embodiment
The present embodiment is used for EBSD of the thickness for the thickness x cross sectional of 40 microns of NiMnInCo alloy thin bands
Prepared by sample, specific implementation step is as follows:
1st, the straight unnotched strip of complete, section port is selected.
2nd, two pieces of, hardness and strip identical cuboid conducting metal blocks consistent with selected strip length are chosen, make needs
The thickness face level of the alloy thin band of analysis downwards, is consistent with the plane of two pieces of conducting metal blocks, strip is clamped in into two
Between block conducting metal block.
3rd, two pieces of conducting metal blocks are clamped with tweezers, conducting metal block is clamped alloy thin band, then in its back side gap
Between instill 1 ﹣ 2 and drip 502 glue, quick drying makes two pieces of conducting metal blocks and alloy thin band be fixed together.
4th, make parallel with conducting metal block, it is necessary to which the thickness x cross sectional level of the alloy thin band of analysis is downward, vertically
Put and stand in hot edge machine, pour into conductive mosaic powder and hide sample, cover pressure head, be heated up to 140 DEG C of application pressure, heat-insulation pressure keeping
10 minutes, turn off heater switch, wait and be cooled to room temperature, shed pressure, take out the sample inlayed, obtain cylindric sample.
5th, by the cylinder sample inlayed, roughly ground successively on 600,1000,1200,1500,2000 mesh sand paper, one
On road sand paper polish when keep same direction, whne cut on sample in one direction when change sand paper, rotate 90 when changing sand paper
Degree；Mechanically polished again after corase grind, until cut is all removed；Then counterweight is added, silicon is added in vibratory finishing machine
Sol solution, selection 30Hz vibration frequencies are polished four hours, and taking-up is rinsed well with clear water, so as to obtain alloy thin band thickness x cross sectional
EBSD sample.The thickness of preparation dissipates for the electronics back of the body of the thickness x cross sectional of 40 microns of NiMnInCo alloy thin bands
Diffraction experiment result such as Fig. 2 is penetrated, its surface demarcation rate is up to 90%.
Claims (1)
1. a kind of EBSD preparation method of sample of alloy thin band thickness x cross sectional, it is characterised in that including following step
Suddenly:
Step 1. chooses the straight unnotched alloy thin band of thickness x cross sectional；
Step 2. chooses two pieces of identical cuboid conducting metal blocks, and metal derby is consistent with selected alloy thin band length, hardness
It is close, make the thickness face level of the alloy thin band of needs analysis downward and consistent with the plane of two pieces of conducting metal blocks, by alloy
Strip is clamped between two pieces of conducting metal blocks；
Step 3. clamps two pieces of conducting metal blocks with tweezers, conducting metal block is tightly clamped alloy thin band, and in its back side seam
Glue is instilled between gap, Quick-air-drying makes two pieces of conducting metal blocks be fixed together with alloy thin band；
The thickness x cross sectional level of the alloy thin band parallel with conducting metal block downwards, is placed in hot edge machine by step 4. vertically,
Pour into conductive mosaic powder and hide sample, cover pressure head, be heated up to 140 DEG C and apply pressure until definite value, heat-insulation pressure keeping 10 minutes,
Turn off heater switch, wait and be cooled to room temperature, shed pressure, take out the sample inlayed, obtain cylindric sample；
Step 5. roughly grinds the cylinder sample inlayed, one on 600,1000,1200,1500,2000 mesh sand paper successively
Demander is to consistent when being polished on road sand paper, whne cut on sample in one direction when change sand paper, be rotated by 90 ° when changing sand paper；
Mechanically polished again after corase grind, until cut is all removed；Then counterweight is added, silica gel is added in vibratory finishing machine molten
Liquid, selection 30Hz vibration frequencies polish four hours, and taking-up is rinsed well with clear water, and the electronics back of the body for obtaining strip thickness section dissipates
Penetrate diffraction sample.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760782A (en) * | 2018-06-06 | 2018-11-06 | 广东省新材料研究所 | A kind of electron backscatter diffraction sample of column crystal zirconia coating and preparation method thereof |
| CN109283204A (en) * | 2018-09-10 | 2019-01-29 | 西北工业大学 | A method of preparing near atomic ratio Co-Ni-Al magnetic control shape memory alloy electron backscatter diffraction sample |
| CN110455840A (en) * | 2019-07-23 | 2019-11-15 | 乳源瑶族自治县东阳光化成箔有限公司 | A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD |
| CN110596163A (en) * | 2019-09-27 | 2019-12-20 | 西北有色金属研究院 | Preparation method of EBSD sample of titanium alloy fracture section |
| CN111220637A (en) * | 2020-01-16 | 2020-06-02 | 北京科技大学 | Nano precipitate image acquisition method based on scanning electron microscope backscattering mode |
| CN111595876A (en) * | 2020-06-02 | 2020-08-28 | 全球能源互联网研究院有限公司 | Electrolytic clamp and method for preparing EBSD sample of metal sheet |
| CN111879593A (en) * | 2020-07-02 | 2020-11-03 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Embedded metallographic sample suitable for electropolishing instrument and preparation method thereof |
| CN113092200A (en) * | 2021-03-15 | 2021-07-09 | 中国航天标准化研究所 | Method for rapidly obtaining grain size of nickel electrode ceramic capacitor |
| CN113295724A (en) * | 2021-05-19 | 2021-08-24 | 上海大学 | Sample for analysis and characterization of electron back scattering diffraction after alloy corrosion and preparation method thereof |
| CN113466272A (en) * | 2021-06-23 | 2021-10-01 | 太原理工大学 | Sample preparation method of ultrathin niobium strip EBSD sample |
| CN113960082A (en) * | 2021-11-08 | 2022-01-21 | 东北大学 | Sample preparation method for hot-rolled strip steel iron scale EBSD analysis |
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| CN108760782A (en) * | 2018-06-06 | 2018-11-06 | 广东省新材料研究所 | A kind of electron backscatter diffraction sample of column crystal zirconia coating and preparation method thereof |
| CN109283204A (en) * | 2018-09-10 | 2019-01-29 | 西北工业大学 | A method of preparing near atomic ratio Co-Ni-Al magnetic control shape memory alloy electron backscatter diffraction sample |
| CN110455840A (en) * | 2019-07-23 | 2019-11-15 | 乳源瑶族自治县东阳光化成箔有限公司 | A kind of sample preparation methods that electrolytic capacitor is analyzed with electronics aluminum foil method to EBSD |
| CN110596163A (en) * | 2019-09-27 | 2019-12-20 | 西北有色金属研究院 | Preparation method of EBSD sample of titanium alloy fracture section |
| CN111220637A (en) * | 2020-01-16 | 2020-06-02 | 北京科技大学 | Nano precipitate image acquisition method based on scanning electron microscope backscattering mode |
| CN111220637B (en) * | 2020-01-16 | 2021-05-04 | 北京科技大学 | Nano precipitate image acquisition method based on scanning electron microscope backscattering mode |
| CN111595876A (en) * | 2020-06-02 | 2020-08-28 | 全球能源互联网研究院有限公司 | Electrolytic clamp and method for preparing EBSD sample of metal sheet |
| CN111879593A (en) * | 2020-07-02 | 2020-11-03 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Embedded metallographic sample suitable for electropolishing instrument and preparation method thereof |
| CN113092200A (en) * | 2021-03-15 | 2021-07-09 | 中国航天标准化研究所 | Method for rapidly obtaining grain size of nickel electrode ceramic capacitor |
| CN113295724A (en) * | 2021-05-19 | 2021-08-24 | 上海大学 | Sample for analysis and characterization of electron back scattering diffraction after alloy corrosion and preparation method thereof |
| CN113466272A (en) * | 2021-06-23 | 2021-10-01 | 太原理工大学 | Sample preparation method of ultrathin niobium strip EBSD sample |
| CN113960082A (en) * | 2021-11-08 | 2022-01-21 | 东北大学 | Sample preparation method for hot-rolled strip steel iron scale EBSD analysis |
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Application publication date: 20170818 |