CN103926263B - A kind of accurate EBSD technical research alloy base band recrystallization and the method for cubic texture formation mechenism in situ - Google Patents
A kind of accurate EBSD technical research alloy base band recrystallization and the method for cubic texture formation mechenism in situ Download PDFInfo
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Abstract
A kind of accurate EBSD technical research alloy base band recrystallization and the method for cubic texture formation mechenism in situ, belong to conductor of high-temperature superconductor coat textured alloy base band research field.Owing to existing EBSD equipment can not carry out high-temperature heating, thus limit and use the mechanism that under original position EBSD technical research high temperature, alloy base band recrystallization and cubic texture are formed.The present invention proposes a kind of quasi-original position EBSD technical research alloy base band recrystallization and method of cubic texture formation mechenism of using, and the difference (plane or cross section) for institute's study sample devises the sample stage for standard EBSD test in situ.The proposition of accurate EBSD technology in situ provides a kind of new method for the mechanism that research alloy base band recrystallization and cubic texture are formed.
Description
Technical field
The present invention relates to a kind of accurate EBSD technical research alloy base band recrystallization and the method for cubic texture formation mechenism in situ, belong to
In conductor of high-temperature superconductor coat textured alloy base band research field.
Technical background
Since last century the nineties, the technology of application EBSD (EBSD) technical Analysis crystal microcell orientation takes
Obtained bigger development, and be widely used in the microstructure of material and the sign of texture.At present, leading for coating
In the body research by textured alloy base band, the means generally used are by different under EBSD characterized by techniques different heat treatment technique
The content of texture studies the formation of its texture.But, at present frequently with research means can not well be used for alloy base band again
Crystallization and the research of cubic texture formation mechenism.In the research to its recrystallization and cubic texture formation mechenism, it would be desirable to pass through
Follow the tracks of the differentiation with heat treatment time of each crystal grain, the growing mechanism of analyze and research its recrystal grain and cubic grain, clearly
Its recrystallization and cubic texture formation mechenism.So, the in-situ test under high temperature is research alloy base band recrystallization and cubic texture
The effective means of formation mechenism.But, existing EBSD technology is owing to being limited by equipment itself, it is impossible to carries out high temperature and adds
Heat, so the formation mechenism of recrystallization and cubic texture is by test equipment under the technique study alloy base band high temperature that employing is in situ
Limit.Therefore, the present invention proposes a kind of accurate EBSD technical research alloy base band recrystallization in situ and cubic texture formation mechenism
Method.
Accurate EBSD technical research alloy base band recrystallization and the method for cubic texture formation mechenism in situ that the present invention proposes, i.e. first
The method first passing through dozen hardness carries out labelling at the sample surfaces studied；The sample heat treatment at a certain temperature of labelling will be carried out
After certain time, it is carried out EBSD test；Then sample is taken out, again carry out the heat treatment of certain time, then to same
One position carries out EBSD test；Carry out repeatedly heat treatment as required, and repeatedly carry out EBSD test at same position.By
In testing at EBSD, sample is fixed on sample stage by conventional carbon paste band, but is difficult to intact the taking off of sample and carries out many
Secondary retest.Therefore, the difference (plane or cross section) for institute's study sample devises and is specifically designed to accurate EBSD survey in situ
The sample stage of examination, as depicted in figs. 1 and 2.
Summary of the invention
It is an object of the invention to provide a kind of accurate EBSD technical research alloy base band recrystallization in situ and cubic texture formation mechenism
Method.Owing to existing EBSD equipment can not carry out high-temperature heating, thus limit employing EBSD technical research high temperature in situ
The mechanism that lower alloy base band recrystallization and cubic texture are formed.The present invention proposes the accurate EBSD technical research alloy in situ of a kind of employing
Base band recrystallization and the method for cubic texture formation mechenism, and the difference (plane or cross section) for institute's study sample devises use
Sample stage in standard EBSD test in situ.The proposition of accurate EBSD technology in situ is research alloy base band recrystallization and cubic texture
The mechanism formed provides a kind of new method.
In the method for accurate EBSD technical research alloy base band recrystallization and cubic texture formation mechenism in situ, for institute's study sample
Difference (plane or cross section) devise the sample stage for standard in situ EBSD test, it is characterised in that plane sample used
The accurate EBSD test specimens sample platform in situ of product is mainly by the flat bottom of surface band grid scale with for fixing the sheet metal group of sample
Become, sheet metal lays respectively at two offsides of grid scale on flat bottom, planar sample by grid scale both sides with screw
Sheet metal be fixed on have grid scale flat bottom central authorities；Cross-sectional sample with accurate EBSD test specimens sample platform in situ mainly by
The vertical fixation clamp flat board composition that base is relative with the left and right sides, base is provided with the guide groove vertical with vertical fixation clamp flat board, its
In a vertical fixation clamp flat board be fixed on base, the bottom of another vertical fixation clamp flat board is provided with the guide wheel mated with guide groove or convex
Rise so that this vertical fixation clamp flat board can be along the parallel slip of guide groove, and two vertical fixation clamp flat boards can carry out consolidating by screw
Fixed, the end face of two vertical fixation clamp flat boards is plane, and plane is provided with scale.
Accurate EBSD technical research alloy base band recrystallization and the method for cubic texture formation mechenism in situ, comprise the following steps:
(1) firstly, for planar sample, labelling is carried out by the method beating hardness on the planar sample surface studied；For cross section
Sample, owing to cannot beat hardness labelling on the surface to be measured of cross-sectional sample, so come preliminary mainly by the scale on cross-sectional sample platform
The position of localizing sample；
(2) by the planar sample studied or cross-sectional sample, it is being connected with Ar/H2Protective atmosphere in, according to research need at a constant temperature
The degree lower heat treatment regular hour；
(3) planar sample is placed on the flat bottom with grid scale of the accurate EBSD test specimens sample platform in situ of planar sample,
Dual-side is placed in below sheet metal and is screwed；Cross-sectional sample is placed on the accurate EBSD test specimens sample platform in situ of cross-sectional sample
Two are vertically relatively fixed presss from both sides in the middle of flat board, and fixation clamp flat board is screwed, and the cross section of cross-sectional sample is put down with two vertical fixation clamps
Surveyed planar sample or cross-sectional sample in the same direction, are then put in Electronic Speculum by the end face of plate, carry out EBSD test at selection area；
(4) surveyed planar sample or the cross-sectional sample of step (3) are taken out, continue to extend heat treatment time at desired temperatures, so
Rear repetition step (3), carries out EBSD test at selection area again；
(5) according to experimental analysis need same plane sample or cross-sectional sample are repeated several times heat treatment and step (3) with
One region carries out repeatedly EBSD test；
(6) evolution mechanism extended with heat treatment time by each microstructure and texture in analysis and research same sample the same area, is used
In the study mechanism that alloy base band recrystallization and cubic texture are formed.
Fig. 1 is the accurate EBSD test specimens sample platform schematic diagram in situ of planar sample, show respectively bowing of this sample stage in schematic diagram
View, front view and upward view.Sample stage shown in Fig. 1 mainly is used for fixing sample by the bottom surface of band grid scale and surface
Sheet metal composition.Planar sample is fixed on the sample stage central authorities with grid chart by both sides with the sheet metal of screw, and leads to
Cross mesh coordinate Primary Location sample position.Fig. 2 is cross-sectional sample accurate EBSD test specimens sample platform schematic diagram, schematic diagram in situ
In show respectively the top view of this cross-sectional sample platform, front view and left view.Sample stage shown in Fig. 2 is mainly by two, left and right
Being grouped into, right side is fixed together with base, then can be slided by bottom guide groove in left side.Cross-sectional sample passes through specimen holder both sides spiral shell
Silk is fixing, and can be slided by guide groove in specimen holder side, specimen holder left and right sides end face has scale equally, for Primary Location sample
Grade is put.
Accompanying drawing explanation
Fig. 1 planar sample standard EBSD test specimens sample platform schematic diagram in situ；
Fig. 2 cross-sectional sample standard EBSD test specimens sample platform schematic diagram in situ；
Fig. 3 planar sample standard EBSD Testing Technology Study Cu-Ni alloy base band cubic texture formation mechenism EBSD in situ schemes, i.e.
2 minutes (a), 10 minutes (b), 30 minutes (c) and 60 minutes (d) it is incubated respectively at 1000 DEG C；
Fig. 4 cross-sectional sample standard EBSD testing research NiW alloy base band recrystal grain growing mechanism EBSD in situ schemes, and i.e. exists
700 DEG C are incubated 10 minutes (a) and 15 minutes (b) respectively.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, but the present invention is not limited to following example.
Embodiment 1
U-Ni alloy base band is used the formation mechenism of strong cubic texture under accurate EBSD technical research high temperature in situ.First, logical
The method crossing dozen hardness carries out labelling at the sample surfaces studied；Secondly, the sample that will be studied, at 1000 DEG C of heat treatments 2
After min, being fixed on the sample stage shown in Fig. 1, selection area carries out EBSD test；Then, test sample is taken out,
Continue to extend heat treatment time at 1000 DEG C, again carry out EBSD test at selection area；Need to divide according to experimental analysis
Other same sample is repeated several times heat treatment and the same area carry out repeatedly EBSD test.Choose accurate EBSD in situ to survey
Four width figures in test result figure, as it is shown on figure 3, the method for the explanation present invention can analyze cubic texture formation mechenism.
Embodiment 2
Ni5W alloy base band is used accurate EBSD technical research recrystal grain growing mechanism in situ.Owing to sample in cross section only has
80 μm, the method not fitting through dozen hardness makes marks at the sample surfaces studied, mainly by the scale on sample stage
It is positioned；First, the sample that will be studied, after 700 DEG C of heat treatment 5min, it is fixed on the sample shown in Fig. 2
On platform, selection area carries out EBSD test；Then, test sample is taken out, continues to extend heat treatment time at 700 DEG C,
Again carry out EBSD test at selection area.Choose two width in accurate EBSD test result figure in situ, as shown in Figure 4, say
The method of the bright present invention can analyze recrystallization mechanism.
Claims (1)
1. utilize the accurate EBSD test specimens sample platform in situ of planar sample or the accurate EBSD test specimens sample platform research in situ of cross-sectional sample
Alloy base band recrystallization and the method for cubic texture formation mechenism, it is characterised in that comprise the following steps:
(1) firstly, for planar sample, labelling is carried out by the method beating hardness on the planar sample surface studied；For cross section
Sample, owing to cannot beat hardness labelling on the surface to be measured of cross-sectional sample, so come preliminary mainly by the scale on cross-sectional sample platform
The position of localizing sample；
(2) by the planar sample studied or cross-sectional sample, it is being connected with Ar/H2Protective atmosphere in, according to research need at a constant temperature
The degree lower heat treatment regular hour；
(3) planar sample is placed on the flat bottom with grid scale of the accurate EBSD test specimens sample platform in situ of planar sample,
Dual-side is placed in below sheet metal and is screwed；Cross-sectional sample is placed on the accurate EBSD test specimens sample platform in situ of cross-sectional sample
Two are vertically relatively fixed presss from both sides in the middle of flat board, and fixation clamp flat board is screwed, and the cross section of cross-sectional sample is put down with two vertical fixation clamps
Surveyed planar sample or cross-sectional sample in the same direction, are then put in Electronic Speculum by the end face of plate, carry out EBSD test at selection area；
(4) surveyed planar sample or the cross-sectional sample of step (3) are taken out, continue to extend heat treatment time at desired temperatures, so
Rear repetition step (3), carries out EBSD test at selection area again；
(5) according to experimental analysis need same plane sample or cross-sectional sample are repeated several times heat treatment and step (3) with
One region carries out repeatedly EBSD test；
(6) evolution mechanism extended with heat treatment time by each microstructure and texture in analysis and research same sample the same area, is used
In the study mechanism that alloy base band recrystallization and cubic texture are formed；
The accurate EBSD test specimens sample platform in situ of above-mentioned planar sample, mainly by the flat bottom of surface band grid scale be used for fixing
The sheet metal composition of sample, sheet metal lays respectively at the both sides of grid scale on flat bottom, and planar sample passes through grid scale two
The sheet metal with screw of side is fixed on the flat bottom central authorities with grid scale；
The accurate EBSD test specimens sample platform in situ of above-mentioned cross-sectional sample, it is characterised in that the most relative with the left and right sides by base
Vertically fixation clamp flat board composition, base is provided with the guide groove vertical with vertical fixation clamp flat board, and wherein a vertical fixation clamp flat board is solid
Being scheduled on base, the bottom of another vertical fixation clamp flat board is provided with the guide wheel or projection mated with guide groove so that this vertical fixation clamp
Flat board can be along the parallel slip of guide groove, and two vertical fixation clamp flat boards can be fixed by screw, two vertical fixation clamp flat boards
End face be plane, plane is provided with scale.
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| CN201410140650.6A CN103926263B (en) | 2014-04-09 | 2014-04-09 | A kind of accurate EBSD technical research alloy base band recrystallization and the method for cubic texture formation mechenism in situ |
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| CN201141821Y (en) * | 2007-11-16 | 2008-10-29 | 山东理工大学 | Special sample seat for electron back scattering diffraction |
| CN201122146Y (en) * | 2007-11-16 | 2008-09-24 | 山东理工大学 | Scanning electron microscope example bench |
| CN201145662Y (en) * | 2007-11-16 | 2008-11-05 | 山东理工大学 | Scanning electron microscope sample platform |
| CN201556600U (en) * | 2009-09-17 | 2010-08-18 | 宝山钢铁股份有限公司 | Scanning electronic microscope electronic backscatter diffraction test sample stand |
| CN201698989U (en) * | 2010-06-10 | 2011-01-05 | 常州天合光能有限公司 | Cross section observation platform of scanning electron microscope |
| CN201697885U (en) * | 2010-06-13 | 2011-01-05 | 武汉钢铁(集团)公司 | Multifunctional sample stage for measuring electron back scattered diffraction (EBSD) |
| CN202351191U (en) * | 2011-11-22 | 2012-07-25 | 南京钢铁股份有限公司 | Sample holder used for EBSD (electron back-scatter diffraction) of scanning electron microscope |
| CN103128657A (en) * | 2011-11-24 | 2013-06-05 | 宝山钢铁股份有限公司 | Clamp used for electron back scattering diffraction sample vibration polishing and use method thereof |
| CN203216878U (en) * | 2013-04-14 | 2013-09-25 | 首钢总公司 | Sample holder device applied to EBSD (electron back-scattered diffraction) placement sample |
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Effective date of registration: 20170717 Address after: Support 530000 Nanning Road, the Guangxi Zhuang Autonomous Region No. 32 South Lake Garden 4-2004 Patentee after: Guo Fuliang Address before: 100124 Chaoyang District, Beijing Ping Park, No. 100 Patentee before: Beijing University of Technology |
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Effective date of registration: 20221017 Address after: A1501, Innovation Plaza, No. 2007, Pingshan Avenue, Liulian Community, Pingshan Street, Pingshan District, Shenzhen, Guangdong 518118 Patentee after: Shenchuang Superconductor (Shenzhen) Technology Co.,Ltd. Address before: 4-2004, Nanhu Scenic Garden, No. 32, Shuangyong Road, Nanning City, 530000 Guangxi Zhuang Autonomous Region Patentee before: Guo Fuliang |
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