CN105403440B - A kind of preparation method of metal sheet and thin slice cross section transmission electron microscope sample - Google Patents
A kind of preparation method of metal sheet and thin slice cross section transmission electron microscope sample Download PDFInfo
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Abstract
A kind of preparation method of metal sheet and thin slice cross section transmission electron microscope sample, it is mainly characterized by：Mechanical reduction to 30 50 microns of thick cross-sectional samples is placed in the pit on the conducting strip of the bottom plate of general electrolysis double-spraying device fixture, non-conductive thin slice is placed on the outside of sample again, 2 2.5 millimeters on bottom plate of circular hole is sheltered from completely, and non-conductive thin slice mid-diameter is less than the micropore of cross-sectional sample width in electrolysis pair spray regions of the cross-sectional sample surface formation diameter equal to micro-pore diameter.As long as occurring hole in micro-porous area, photosensitive control unit will be caused to act immediately, and be electrolysed double spray process and be automatically stopped, so as to obtain the thin area that the maximum electronic energy of area penetrates.The present invention easily can prepare metal sheet and the transmission electron microscope sample of thin slice cross section on general electrolysis double-spraying device；The area in the permeable thin area of electronics can not only be significantly increased, and the reliability for obtaining the permeable thin area of electronics of large area greatly improves.
Description
Technical field
The present invention relates to a kind of transmission electron microscope sample preparation method, is particularly thinned with the double sprays of electrolysis and prepares transmission electron microscope sample
The method of product.
Background technology
Prediction based on Hall-Petch Formula, nanocrystalline/super fine crystal material has high intensity, thus causes generation
The extensive concern of various countries of boundary material science worker.In the research process of nanocrystalline/ultrafine grain metal material, it will usually run into
Thickness only has the thin plate and lamellar material of 0.2-2 millimeters, in order to inquire into the Microstructure evolution of Ultra-fine Grained/nanocrystalline, plasticity
The problem in science such as deformation mechanism, Strengthening and Toughening theory, it is sometimes desirable to hom ology these Ultra-fine Graineds/nanocrystalline material thin plate
With the microstructure in thin slice cross section.In addition, a kind of new manufacturing technology-micro manufacturing obtains flourishing hair in the late two decades
Exhibition, this technology are widely used for manufacture with the miniature parts in various micro-systems, miniature thin plate therein, thin sheet of metal
Part occupies critical role in various miniature parts, has a wide range of applications, and is also required to sometimes with hom ology system
Make the microstructure in miniature thin plate, the metal sheet of sheet parts and thin slice cross section.Metal sheet and thin slice
Prepared by the transmission electron microscope sample of cross section turn into the premise for carrying out above-mentioned transmission electron microscope Analysis on Microstructure.Below will be first to system
Standby metal sheet and thin slice cross section transmission electron microscope sample are analyzed.Metal sheet and thin slice cross-sectional sample are
Along the sample for being generally shaped like cuboid that is cut out perpendicular to its surface, in order to for the sake of hereafter sake of clarity, to metal material
Relation of the involved position between is specified below (as shown in Figure 1) in thin plate and thin slice and its cross-sectional sample：Cross section
The width of sample is the thickness direction of former thin plate and thin slice, width is contained in cross-sectional sample and perpendicular to former thin plate
With sheet surface, have greater depth plane be cross-sectional sample surface, without width and parallel to former thin plate and
The plane of sheet surface is the side of cross-sectional sample, in cross-sectional sample perpendicular to cross-sectional sample surface direction yardstick
For the thickness of cross-sectional sample.Based on defined above, the metal sheet of thickness 0.2-2 millimeters and the cross-sectional sample of thin slice
Narrower in width (the thickness 0.2-2 millimeters for being equal to metal sheet and thin slice), on the thickness direction of this cross-sectional sample
It is an extremely challenging job to obtain the permeable thin area of electronics, due to ion milling method, ultrathin sectioning, focused ion
Beam patterning method can introduce extra crystal defect in the material or cause material damage, can so being only electrolysed double spray methods
Take, but when being finally thinned using the double spirt rows of electrolysis, it is difficult to ensure that the acquisition in the permeable thin area of larger electronics, to say
This bright problem, first the double spray process of the electrolysis to the conventional sample of 3 millimeters of diameter make a brief introduction.Mechanical reduction is to thickness 30-50
When micron, 3 millimeters of diameter conventional sample is fixed by the fixture of electrolysis double-spraying device, sample is placed on one in bottom plate
In the circular pit of individual 3 millimeters of diameter, pit is located on the conducting strip in bottom plate (in order to form electricity in the double spray process of electrolysis
Loop), there is the circular hole of an a diameter of 2-2.5 millimeter in pit center, also have on matched auxiliary splint one it is same therewith
The equal diameter circular hole of the heart so that in the electrolyte sprayed by two surfaces of the center section of fixed sample exposed to nozzle, such as
Shown in Fig. 2.Because 3 millimeters of sample of diameter can cover the circular hole on fixture (including bottom plate and auxiliary splint), double sprays are electrolysed
Photosensitive control unit on device can be enabled, and when on sample without hole, light path is blocked, and the pump of power is provided for jet electrolytic liquid
Power supply circuit conducting, double spray process carry out；Once it is double be sprayed onto hole and occurring on sample surfaces when, light path turns on immediately, production
The power supply circuit of raw corresponding signal cut pump, stop double spray process, the permeable thin area's area of electronics now obtained is most
Greatly.For the cross-sectional sample of width 0.2-2 millimeters, because its width is less than on general electrolysis double-spraying device circle in sample clamp
The diameter 2-2.5 millimeters in hole so that cause to be electrolysed double-spraying device with the presence of gap between circular hole wall in cross-sectional sample and fixture
On photosensitive control unit can not enable, it is difficult at the time of determining that sample surfaces have just been ejected hole, so as to it is difficult to ensure that larger
The acquisition in the permeable thin area of electronics of area.For the transmission with the double sprays of electrolysis for metal sheet and thin slice cross section
Electron microscopic sample, existing a few thing are improved the double spray methods of traditional electrolysis, its purpose be try to increase it is transversal
The width of face sample, the cross-sectional sample that the circular hole in fixture is broadened is set to be completely covered, such as with plating [Journal of
Microscopy 252 (2013) 251-257] or be stitched together [Chinese invention patent with several narrow cross-sectional samples
201310218516.9th, rare metal 1 (1984) 69-72] cross-sectional sample widened, when mechanical reduction is to being electrolysed needed for double sprays
During the 30-50 microns wanted, scattered sometimes between electrodeposited coating and cross-sectional sample, between the cross-sectional sample that is stitched together；
For the cross-sectional sample widened of being stitched together with several narrow cross-sectional samples, although electrolysis double-spraying device can be completely covered
Circular hole in upper fixture, but the dissolving for being electrolysed sample in double spray process still preferentially occurs in sample and sample or sample with gluing
Knot agent (such as：The copper electroplated in rare metal 1 (1984) 69-72 work) interface on so that sample surfaces are also without being thinned
When going out hole, because preferential lysigenous gap causes photosensitive control single between sample and sample or sample and binding agent
Metaaction, the power supply that electrolyte injection provides the pump of power is cut to, stops the double spray process of electrolysis.
The content of the invention
It is an object of the invention to provide a kind of reliable and easy-to-use with the double sprays of electrolysis for 0.2-2 millimeters thicks gold
Belong to sheet of material and the method for thin slice cross section transmission electron microscope sample.
It is (major and minor that the present invention is more than fixture mainly on the fixture of existing general electrolysis double-spraying device using a piece of external diameter
Clamping plate) in Circularhole diameter (2-2.5 millimeters), center be less than the non-conductive thin slice of micropore of cross-sectional sample width with diameter and cover
Cover before cross-sectional sample, shelter from the circular hole on fixture (major and minor clamping plate) completely, while in the surface shape of cross-sectional sample
It is equal to the double spray regions of electrolysis of non-conductive thin slice center micro-pore diameter into diameter.
The preparation method of the present invention, is comprised the following steps that：
(1) cutting of cross-sectional sample：Along perpendicular to the metal sheet of thickness 0.2-2 millimeters and the side of sheet surface
To the cross-sectional sample that is about 3 millimeters is cut out, (cross-sectional sample width is the thickness 0.2-2 millis of metal sheet and thin slice
Rice).The metal material includes simple metal, alloy, metal-base composites and intermetallic compound.It is described thin from metal material
When plate and thin slice cutting cross-sectional sample, best method used is Wire EDM (wire electrical
discharge machining)。
(2) mechanical reduction of cross-sectional sample：The cross-sectional sample of width 0.2-2 millimeters is subtracted along its thickness direction machinery
It is as thin as 30-50 microns.Polished preferably with sand paper and sample is thinned.
(3) making of non-conductive thin slice：A piece of 3 millimeters of diameter, thickness 0.2-0.4 millimeters are cut out from electrically non-conductive material
Thin slice, and micropore of the diameter less than cross-sectional sample width in steps 1 and 2 is pierced out with syringe needle at its central.It is described not lead
The material of electric thin slice is with the relatively low high-molecular compound of certain plasticity and hardness, includes but is not limited to meet these
Part various general-purpose plastics (such as：Vinyon, igelite, polypropylene plastics, polystyrene plastics, propylene
Nitrile-butadiene-styrene plastics etc.) and engineering plastics (such as：Maranyl, polycarbonate plastic, polyurethane plastics,
Polytetrafluoroethylplastic plastic, polyethylene terephthalate plastics etc.).
(4) clamping of pre- thinned cross-sectional sample：
The cross-sectional sample of mechanical reduction to 30-50 microns is placed on the bottom plate of general electrolysis double-spraying device fixture by a
Conducting strip on the circular pit for 3 millimeters of diameter for fixing sample in (circular hole on bottom plate is located in pit
Centre), both sides for being about 3 millimeters parallel to cross-sectional sample and between this both sides with the equidistant straight line quilt in both sides
It is placed on above-mentioned circular pit diametrically.
The non-conductive thin slice that b makes step 3 is placed on side i.e. adjacent with auxiliary splint on the outside of sample, shelters from master completely
The circular hole of 2-2.5 millimeters on clamping plate, and the micropore on non-conductive thin slice forms diameter on cross-sectional sample surface and is equal to micropore
The double spray regions of the electrolysis of diameter.The major and minor clamping plate of the fixture is assembled together, completes the clamping of cross-sectional sample.
(5) the double sprays of electrolysis：The fixture that step 4 is made is put into the electrolytic cell of electrolysis double-spraying device, starts photosensitive control
Unit, according to cross-sectional sample material type (i.e. the material type of sheet metal and thin slice), from different electrolytic solutions,
The double spray parameters (voltage, temperature, electrolyte injection rate etc.) of electrolysis carry out being electrolysed double sprays, until cross-sectional sample surface is perforated,
Photosensitive control unit acts immediately, stops the double sprays of electrolysis.
The operation principle of the present invention：When mechanical reduction to 30-50 microns thick metal sheet and thin slice cross section sample
Product (cross-sectional sample width is the thickness 0.2-2 millimeters of metal sheet and thin slice) are by the folder on general electrolysis double-spraying device
While tool is fixed, the thin slice that Circularhole diameter (2-2.5 millimeters) in fixture (major and minor clamping plate) is more than with a piece of external diameter is covered in horizontal stroke
Before cross-sectional sample, so as to shelter from the circular hole on fixture completely；It is wide to be less than cross-sectional sample with diameter on the thin slice simultaneously
The micropore of degree, so that in the region that the micropore that double spray regions are limited on thin slice is determined；In order to thoroughly avoid thin slice from participating in
The double spray process of electrolysis, so as to cause to be electrolysed the interference of double spray process to cross-sectional sample, cause cross-sectional sample electrolysis double sometimes
The failure of spray process, thin slice is made using non electrically conductive material.Using the above method, when the double sprays of electrolysis start due to more than
The presence of the non-conductive thin slice of Circularhole diameter in fixture (major and minor clamping plate), the general photosensitive control unit being electrolysed on double-spraying device
Light path separated, photosensitive control unit is come into operation；It is less than the micropore of cross-sectional sample width on non-conductive thin slice
So that being thinned for cross-sectional sample surface caused by the double sprays of electrolysis is carried out in the region that thin slice micropore is determined；As long as in micropore
Occur hole in region, photosensitive control unit will be caused to act immediately, be electrolysed double spray process and be automatically stopped, at this moment can obtain area
The thin area that maximum electronic energy penetrates.
The present invention has the following advantages that compared with prior art：The present invention in sample after solid mechanical is thinned by not leading
The use of electric thin slice, easily it can prepare the saturating of metal sheet and thin slice cross section on general electrolysis double-spraying device
Penetrate electron microscopic sample；Compared with the method with the double sprays of electrolysis for metal sheet and the transmission electron microscope sample of thin slice cross section
Compare, the area in the permeable thin area of electronics can not only be significantly increased, and obtain the permeable thin area of electronics of large area
Reliability greatly improve.
Brief description of the drawings
Fig. 1 is the three-dimensional signal of relation of the position involved in metal sheet and thin slice and its cross-sectional sample between
Sketch.
Fig. 2 is the fixture section signal of the conventional sample of 3 millimeters of fixed diameter in the general electrolysis double-spraying device of prior art
Sketch.
Fig. 3 is that the 30-50 microns thick cross-sectional sample of the invention that is thinned to is placed on the conducting strip in bottom plate admittedly
Determine the main view schematic diagram that pit and non-conductive thin slice are placed on sample.
Fig. 4 is to be thinned to the thick cross-sectional sample of 30-50 microns in the present invention to be fixed on folder together with non-conductive thin slice
Section simplified schematic diagram in tool.
The cross-sectional sample of the pure Zr thin plates of 2 millimeters thicks is by the double hole edges sprayed of electrolysis in Fig. 5 embodiment of the present invention 1
Neighbouring transmission electron microscope bright field image figure.
Fig. 6 is the SEAD figure of Fig. 5 transmission electron microscope bright field image upper left quarter.
Fig. 7 be the ply rolling of 0.5 millimeters thick in the embodiment of the present invention 2 and anneal 5083Al thin plates cross-sectional sample be electrolysed
The hole figure of double ejections.
Fig. 8 is by transmission electron microscope light field figure (the transmission electricity near the double hole edges sprayed of electrolysis in the embodiment of the present invention 2
4.5 microns of mirror bright field image centre-to-centre spacing hole edge).
Fig. 9 is the high-resolution in double regions of the hole edge sprayed less than 5 microns of distance electrolysis in the embodiment of the present invention 2
Transmission electron microscope picture.
Figure 10 is by the transmission electron microscope light field figure (transmission near the double hole edges sprayed of electrolysis in the embodiment of the present invention 2
10.5 microns of Electronic Speculum bright field image centre-to-centre spacing hole edge).
Figure 11 is the SEAD figure of Figure 10 transmission electron microscope light field figure corresponding region.
Figure 12 is that the cross-sectional sample of the Mg-1.5at.%Zn thin plates of 0.5 millimeters thick in the embodiment of the present invention 3 is double by electrolysis
The hole figure of ejection.
Figure 13 is by the transmission electron microscope light field figure (transmission near the double hole edges sprayed of electrolysis in the embodiment of the present invention 3
8.5 microns of Electronic Speculum bright field image centre-to-centre spacing hole edge).
Figure 14 is that the 5083Al thin slices of 0.2 millimeters thick that aximal deformation value rolling obtains in the embodiment of the present invention 4 are double by electrolysis
Transmission electron microscope light field figure (3.5 microns of transmission electron microscope bright field image centre-to-centre spacing hole edge) near the hole edge of ejection.
Figure 15 is the high score in double regions of the hole edge sprayed less than 2 microns of distance electrolysis in the embodiment of the present invention 4
Distinguish transmission electron microscope picture.
Figure 16 is by the transmission electron microscope light field figure (transmission near the double hole edges sprayed of electrolysis in the embodiment of the present invention 4
12 microns of Electronic Speculum bright field image centre-to-centre spacing hole edge).
Figure 17 is the SEAD figure of Figure 16 transmission electron microscope light field figure corresponding region.
Figure 18 is the Al/Al of 1 millimeters thick in the embodiment of the present invention 52O3Nano composite material thin slice cross-sectional sample is electrolysed
The hole figure of double ejections.
Figure 19 is by the transmission electron microscope light field figure near the double hole edges sprayed of electrolysis in the embodiment of the present invention 5.
Figure 20 is the SEAD figure in the region of lower left corner mark 1 in Figure 19.
Figure 21 is the as cast condition Ni of 1.5 millimeters thicks in the embodiment of the present invention 63Al intermetallic compound thin slice cross-sectional sample quilts
The double hole figures sprayed of electrolysis.
Figure 22 is by the transmission electron microscope light field figure (transmission near the double hole edges sprayed of electrolysis in the embodiment of the present invention 6
8 microns of Electronic Speculum bright field image centre-to-centre spacing hole edge).
Figure 23 is the SEAD figure in the region of Figure 22 transmission electron microscope light field figure upper right corner mark 1.
In figure：1st, thin plate or sheeting, 2, thin plate or sheeting thickness are cross-sectional sample width, 3, cross section sample
Product length, 4, cross-sectional sample thickness, 5, cross-sectional sample side, 6, bottom plate, 7, auxiliary splint, 8, conducting strip, 9, conventional sample
Product, 10, non-conductive thin slice, 11, cross-sectional sample.
Embodiment
Following examples give the detailed embodiment and specific operation process of technical solution of the present invention, but the present invention
Protection domain is not limited to following embodiment.
Fig. 3 and Fig. 4 is that the present invention is used for the fixture simplified schematic diagram with sample on general electrolysis double-spraying device, fixture master
To include bottom plate 6, auxiliary splint 7, conducting strip 8 and non-conductive thin slice 10.Corresponding lead is provided with the groove of bottom plate
Electric piece, the cross-sectional sample 11 for being thinned to 30-50 microns is placed in the pit of the conducting strip, non-conductive thin slice is placed on transversal
It is side adjacent with auxiliary splint on the outside of the sample of face, and it is corresponding with cross-sectional sample and straight with one on the non-conductive thin slice
Footpath is less than the micropore of cross-sectional sample width.
Embodiment 1
The pure Zr thin plates for obtaining 2 millimeters thicks are rolled under liquid nitrogen temperature through aximal deformation value, with Wire EDM along vertical
About 0.3 millimeters thick, 3.2 millimeters of long cross-sectional samples (width is 2 millimeters) are cut out in the direction of Zr plate surfaces, are used successively
400#, 600#, 800#, 1000#, 1500#, 2000# sand paper are micro- to 30-50 by cross-sectional sample through-thickness mechanical reduction
Rice.A piece of 3 millimeters of diameter is gone out from the vinyon piece of 0.2 millimeter of a thickness with 3 millimeters of punching instrument of punch diameter
Non-conductive thin slice, go out the hole of about 1 millimeter of diameter in the central spine of thin slice with stainless steel syringe needle.By the cross section after mechanical reduction
Sample is placed in the pit of 3 millimeters of diameter on the bottom plate of general electrolysis double-spraying device, parallel to about 3 millimeters long (machinery
Cross-sectional sample length is kept to about 3 millimeters in thinning process) both sides and be placed on the straight of pit with the equidistant straight line in this both sides
(see Fig. 3) on footpath；Above-mentioned non-conductive thin slice is placed on the outside of cross-sectional sample again, shelters from 2-2.5 millimeters in bottom plate
Major-minor clamping plate, is then assembled together (see Fig. 4) by circular hole (see Fig. 3).To be assembled together with cross-sectional sample and not
The fixture of conductive foil is put into the electrolytic cell of electrolysis double-spraying device, starts photosensitive control unit, with 90vol.% perchloric acid and
The electrolyte of 10vol.% acetic acid composition carries out double sprays at room temperature, until hole is on cross-sectional sample, 1 on plastic tab
The region that millimeter micropore is limited occurs, and photosensitive control unit acts immediately causes the pump for providing power for jet electrolytic liquid to stop
Work, it is electrolysed double spray process and terminates.
Observed with the adjacent edges of hole of the type transmission electron microscopes of JEOL JEM 2010 to being sprayed in cross-sectional sample,
Fig. 5 gives the transmission electron microscope bright field image of 7 microns × 7 microns of a size, and the contrast of microstructure is obvious on image, can be clear
Dislocation cell structure caused by observation plastic deformation, or even can be clearly observed light and dark caused by intracellular stress field of a dislocation
Striated Microstructure characteristics.Diffraction spot from the upper left region farthest from hole is also clear, bright as shown in Figure 6
Bright.Above-mentioned Microstructure characteristics point out that 7 microns × 7 um regions are thin to the thickness for carrying out transmission electron microscope analysis in Fig. 5, thin
Area's size is at least 7 microns × 7 microns.
Embodiment 2
The 5083Al lattens for being 0.5 millimeter to the thickness for accumulating ply rolling are annealed 2 hours at 225 DEG C, use electric spark
Wire cutting cuts out about 0.2 millimeters thick, 3.4 millimeters of long cross-sectional samples along perpendicular to the direction of 5083Al thin sheet surfaces
(width be 0.5 millimeter), successively with 400#, 600#, 800#, 1000#, 1500#, 2000# sand paper by cross-sectional sample along thickness
Direction machinery is thinned to 30-50 microns.Polyvinyl chloride plastic with the punching instrument of 3 millimeters of punch diameter from 0.3 millimeter of a thickness
The non-conductive thin slice of a piece of 3 millimeters of diameter is gone out on tablet, goes out about 0.4 millimeter of diameter in the central spine of thin slice with stainless steel syringe needle
Hole.Cross-sectional sample after mechanical reduction is placed on the recessed of general 3 millimeters of diameter being electrolysed on the bottom plate of double-spraying device
In hole, both sides parallel to about 3 millimeters long (cross-sectional sample length is kept to about 3 millimeters during mechanical reduction) and with this both sides
Equidistant straight line be placed on pit diametrically (see Fig. 3)；Above-mentioned non-conductive thin slice is placed on the outside of cross-sectional sample again, blocked
Major-minor clamping plate, is then assembled together (see Fig. 4) by the firmly circular hole (see Fig. 3) of the 2-2.5 millimeters in bottom plate.It will assemble one
The rise, fixture with cross-sectional sample and non-conductive thin slice is put into the electrolytic cell of electrolysis double-spraying device, starts photosensitive control
Unit, the electrolyte formed with 25vol.% nitric acid and 75vol.% methanol carries out double sprays at -30 DEG C, until hole is transversal
Above the sample of face, 0.4 millimeter of micropore is limited on thin slice region occurs as shown in fig. 7, photosensitive control unit acts draw immediately
Rise and the pump of power is provided for jet electrolytic liquid be stopped, electrolysis pair spray process termination.
Observed with the adjacent edges of hole of the type transmission electron microscopes of JEOL JEM 2010 to being sprayed in cross-sectional sample,
Fig. 8 gives about 3.5 microns × 3.5 microns of size, a transmission electron microscope bright field image for 4.5 microns of centre-to-centre spacing hole edge, figure
As upper microstructure contrast is obvious, ultra-fine equiax crystal and lamellar structure can be clearly observed, it is bright inside lamellar structure
Striped and network-like tissue signature between dark phase is also fully aware of.It can be taken clearly from region of the hole edge less than 5 microns
Clear high-resolution-ration transmission electric-lens image (Fig. 9).Even in the transmission electron microscope light field figure at about 10.5 microns from hole edge of center
(Figure 10), also high-visible similar to the Microstructure characteristics in Fig. 8, the electron diffraction diagram for coming from this region is also clear that
As shown in figure 11.The above results show that hole, which is nearby more than 12 microns of wide regions, can carry out transmission electron microanalysis.
Embodiment 3
For the Mg-1.5at.%Zn thin plates of 0.5 millimeters thick of casting, with Wire EDM along perpendicular to sheet
The direction in face cuts out about 0.2 millimeters thick, 3.3 millimeters of long cross-sectional samples (width is 0.5 millimeter), successively with 400#,
600#, 800#, 1000#, 1500#, 2000# sand paper are by cross-sectional sample through-thickness mechanical reduction to 30-50 microns.With punching
The punching instrument of 3 millimeters of diameter of head goes out the non-conductive of a piece of 3 millimeters of diameter from the polypropylene plastics tablet of 0.3 millimeter of a thickness
Thin slice, go out the hole of about 0.35 millimeter of diameter in the central spine of thin slice with stainless steel syringe needle.By the cross-sectional sample after mechanical reduction
In the pit for 3 millimeters of diameter being placed on the bottom plate of general electrolysis double-spraying device, parallel to about 3 millimeters of long (mechanical reductions
During cross-sectional sample length be kept to about 3 millimeters) both sides and be placed on pit diametrically with the equidistant straight line in this both sides
(see Fig. 3)；Above-mentioned non-conductive thin slice is placed on the outside of cross-sectional sample again, shelters from the circular hole of the 2-2.5 millimeters in bottom plate
(see Fig. 3), then major-minor clamping plate is assembled together (see Fig. 4).By it is being assembled together, with cross-sectional sample and non-conductive
The fixture of thin slice is put into the electrolytic cell of electrolysis double-spraying device, starts photosensitive control unit, with 6vol.% perchloric acid and
The electrolyte of 94vol.% ethanol composition carries out double sprays at -30 DEG C, until hole is on cross-sectional sample, 0.35 on thin slice
The region that millimeter micropore is limited occurs as shown in figure 12, and photosensitive control unit is acted to cause to provide for jet electrolytic liquid immediately and moved
The pump of power is stopped, and is electrolysed double spray process and terminates.
Observed with the adjacent edges of hole of the type transmission electron microscopes of JEOL JEM 2010 to being sprayed in cross-sectional sample,
Figure 13 gives about 7 microns × 7 microns of size, a transmission electron microscope bright field image for 8.5 microns of centre-to-centre spacing hole edge, on image
Microstructure contrast is obvious, can be clearly observed the Second Phase Particle being distributed on matrix.The above results show, near hole
The region wide more than 12 microns can carry out transmission electron microanalysis.
Embodiment 4
The thin slice that aximal deformation value rolling obtains 0.2 millimeters thick is carried out to 5083Al alloys at room temperature, uses Wire EDM
Along cut out about 0.1 millimeters thick perpendicular to the direction of 5083Al sheet surfaces, (width is for 3.2 millimeters of long cross-sectional samples
0.2 millimeter), it is with 400#, 600#, 800#, 1000#, 1500#, 2000# sand paper that cross-sectional sample through-thickness is mechanical successively
It is thinned to 30-50 microns.Rushed with 3 millimeters of punching instrument of punch diameter from the polystyrene plastics piece of 0.4 millimeter of a thickness
Go out the non-conductive thin slice of a piece of 3 millimeters of diameter, go out the hole of about 0.15 millimeter of diameter in the central spine of thin slice with stainless steel syringe needle.Will
Cross-sectional sample after mechanical reduction is placed in the pit of 3 millimeters of diameter on the bottom plate of general electrolysis double-spraying device, is put down
It is capable in the both sides of about 3 millimeters long (cross-sectional sample length is kept to about 3 millimeters during mechanical reduction) and equidistant with this both sides
Straight line be placed on pit diametrically (see Fig. 3)；Above-mentioned non-conductive thin slice is placed on the outside of cross-sectional sample again, shelters from main folder
Major-minor clamping plate, is then assembled together (see Fig. 4) by the circular hole (see Fig. 3) of the 2-2.5 millimeters in plate.By it is being assembled together,
Fixture with cross-sectional sample and non-conductive thin slice is put into the electrolytic cell of electrolysis double-spraying device, starts photosensitive control unit,
The electrolyte formed with 25vol.% nitric acid and 75vol.% methanol carries out double sprays at -30 DEG C, until hole is in cross section sample
Above product, 0.15 millimeter of micropore is limited on thin slice region occur, photosensitive control unit acts immediately to be caused for jet electrolytic
The pump that liquid provides power is stopped, and is electrolysed double spray process and terminates.
Observed with the adjacent edges of hole of the type transmission electron microscopes of JEOL JEM 2010 to being sprayed in cross-sectional sample,
Figure 14 gives 4.2 microns × 4.2 microns of a size, the transmission electron microscope light field figure of 3.5 microns of centre-to-centre spacing hole edge, image
Upper microstructure contrast is obvious, can be clearly observed caused by the rolling of aximal deformation value from nanometer to the lamellar of ultra-fine size
Light and dark striated Microstructure characteristics in tissue and some synusia.Can in the region for being less than 2 microns from hole edge
Clearly high-resolution-ration transmission electric-lens figure is taken, as shown in figure 15.Even in the transmission electron microscope at about 12 microns from hole edge of center
In light field figure (Figure 16), lamellar structure feature is also clearer, and it is also clearer to come from the electron diffraction diagram in this region, such as schemes
Shown in 17.The above results show that hole, which is nearby more than 14 microns of wide regions, can carry out transmission electron microanalysis.
Embodiment 5
To the Al/Al of about 1 millimeters thick obtained by powder consolidation approach2O3Nano composite material thin slice, uses wire electric discharge
Cutting cuts out about 0.2 millimeters thick, 3.3 millimeters long of cross section sample along perpendicular to the direction of aluminum matrix composite sheet surface
Product (width is about 1 millimeter) are thick by cross-sectional sample edge with 400#, 600#, 800#, 1000#, 1500#, 2000# sand paper successively
Degree direction machinery is thinned to 30-50 microns.Moulded with 3 millimeters of punching instrument of punch diameter from the polyamide of 0.3 millimeter of a thickness
The non-conductive thin slice of a piece of 3 millimeters of diameter is gone out on tablet, goes out about 0.6 millimeter of diameter in the central spine of thin slice with stainless steel syringe needle
Hole.Cross-sectional sample after mechanical reduction is placed on the recessed of general 3 millimeters of diameter being electrolysed on the bottom plate of double-spraying device
In hole, both sides parallel to about 3 millimeters long (cross-sectional sample length is kept to about 3 millimeters during mechanical reduction) and with this both sides
Equidistant straight line be placed on pit diametrically (see Fig. 3)；Above-mentioned non-conductive thin slice is placed on the outside of cross-sectional sample again, blocked
Major-minor clamping plate, is then assembled together (see Fig. 4) by the firmly circular hole (see Fig. 3) of the 2-2.5 millimeters in bottom plate.It will assemble one
The rise, fixture with cross-sectional sample and non-conductive thin slice is put into the electrolytic cell of electrolysis double-spraying device, starts photosensitive control
Unit, the electrolyte formed with 25vol.% nitric acid and 75vol.% methanol carries out double sprays at -30 DEG C, until hole is transversal
Occur as shown in figure 18 above the sample of face, around the region that 0.6 millimeter of micropore is limited on thin slice, photosensitive control unit is moved immediately
Work causes the pump for providing power for jet electrolytic liquid to be stopped, and is electrolysed double spray process and terminates.
The region near the hole that is sprayed in cross-sectional sample is observed with the type transmission electron microscopes of JEOL JEM 2010,
Figure 19 is that a size is 5.5 microns × 5.5 microns of transmission electron microscope light field figure, and the contrast of microstructure is obvious on image, energy
Clear view is to nano-sized grains/oxide particle.Even (1 position is marked in Figure 19 in the region for leaving about 5 microns of hole
Put), diffraction spot/ring is also clearer, as shown in figure 20.Above-mentioned Microstructure characteristics point out that hole edge nearby at least has 5.5
Micron × 5.5 microns of thin areas, can be to Al/Al2O3Nano composite material carries out transmission electron microscope analysis.
Embodiment 6
The Ni of 1.5 millimeters thicks is obtained by casting3Al intermetallic compound sheetings, with Wire EDM along hang down
Directly in Ni3The direction of Al sheet surfaces cuts out about 0.4 millimeters thick, (width is 1.5 millis to 3.2 millimeters of long cross-sectional samples
Rice), successively with 400#, 600#, 800#, 1000#, 1500#, 2000# sand paper by cross-sectional sample through-thickness mechanical reduction
To 30-50 microns.Gone out with 3 millimeters of punching instrument of punch diameter from the plasticized polyurethane tablet of 0.2 millimeter of a thickness a piece of
The non-conductive thin slice of 3 millimeters of diameter, go out the hole of about 0.8 millimeter of diameter in the central spine of thin slice with stainless steel syringe needle.Machinery is subtracted
Cross-sectional sample after thin is placed in the pit of 3 millimeters of diameter on the bottom plate of general electrolysis double-spraying device, parallel to about 3
Millimeter long (cross-sectional sample length is kept to about 3 millimeters during mechanical reduction) both sides and put with the equidistant straight line in this both sides
In pit diametrically (see Fig. 3)；Above-mentioned non-conductive thin slice is placed on the outside of cross-sectional sample again, shelters from the 2- in bottom plate
Major-minor clamping plate, is then assembled together (see Fig. 4) by 2.5 millimeters of circular hole (see Fig. 3).By it is being assembled together, with transversal
The fixture of face sample and non-conductive thin slice is put into the electrolytic cell of electrolysis double-spraying device, starts photosensitive control unit, is used
The electrolyte of 15vol.% sulfuric acid and 85vol.% methanol composition carries out double sprays at -25 DEG C, until hole is in cross-sectional sample
Above, the region that 0.8 millimeter of micropore is limited on thin slice occurs as shown in figure 21, and photosensitive control unit acts immediately to be caused for spray
The pump for penetrating electrolyte offer power is stopped, and is electrolysed double spray process and terminates.
The hole edge sprayed in cross-sectional sample is nearby observed with the type transmission electron microscopes of JEOL JEM 2010, schemed
22 give 7 microns × 7 microns of transmission electron microscope light field figure of about 8 microns of a centre-to-centre spacing hole edge, microcosmic group on image
The contrast knitted is obvious, the dislocation in energy clear view to coarse-grain, and the crystal boundary between two coarse-grains is also clear；It is farthest away from hole edge
The upper right corner SEAD figure on diffraction spot it is also extremely clear, as shown in figure 23.The above results show that hole is attached
Transmission electron microanalysis can be carried out by being closely more than 11 microns of wide regions.
Claims (5)
1. the preparation method of a kind of metal sheet and thin slice cross section transmission electron microscope sample, prepares metal material in this way
Material thin plate and thin slice cross section transmission electron microscope sample comprise the following steps that：
(1) cutting of cross-sectional sample：Cut perpendicular to the metal sheet of thickness 0.2-2 millimeters and the direction of sheet surface on edge
Cut out and be about 3 millimeters of cross-sectional sample, cross-sectional sample width is the thickness 0.2-2 millimeters of metal sheet and thin slice；
(2) mechanical reduction of cross-sectional sample：By the cross-sectional sample of width 0.2-2 millimeters along its thickness direction mechanical reduction extremely
30-50 microns；It is characterized in that：
(3) making of non-conductive thin slice：Cut out from electrically non-conductive material a piece of 3 millimeters of diameter, thickness 0.2-0.4 millimeters it is thin
Piece, and micropore of the diameter less than cross-sectional sample width in steps 1 and 2 is pierced out with syringe needle at its central；
(4) clamping of the cross-sectional sample of mechanical reduction：
The cross-sectional sample of mechanical reduction to 30-50 microns is placed on leading for the bottom plate of general electrolysis double-spraying device fixture by a
It is used to fix in the circular pit of 3 millimeters of diameter of sample on electric piece, the circular hole on bottom plate is located at the center of pit, parallel
It is placed in the both sides for being about 3 millimeters of cross-sectional sample and between this both sides with the equidistant straight line in both sides
State circular pit diametrically；
The non-conductive thin slice that b makes step 3 is placed on side i.e. adjacent with auxiliary splint on the outside of sample, shelters from bottom plate completely
The circular hole of upper 2-2.5 millimeters, and the micropore on non-conductive thin slice forms diameter on cross-sectional sample surface and is equal to micro-pore diameter
The double spray regions of electrolysis, the major and minor clamping plate of the fixture is assembled together, completes the clamping of cross-sectional sample；
(5) the double sprays of electrolysis：The fixture that step 4 is made is put into the electrolytic cell of electrolysis double-spraying device, starts photosensitive control unit,
According to the material type of cross-sectional sample, carry out being electrolysed double sprays from different electrolytic solutions, the double spray parameters of electrolysis, until transversal
Face sample surfaces perforation, photosensitive control unit act immediately, stop the double sprays of electrolysis.
2. the preparation method of metal sheet according to claim 1 and thin slice cross section transmission electron microscope sample, it is special
Sign is：The metal material includes simple metal, alloy, metal-base composites or intermetallic compound.
3. the preparation method of metal sheet according to claim 1 and thin slice cross section transmission electron microscope sample, it is special
Sign is：When cutting cross-sectional sample from metal sheet and thin slice, using Wire EDM.
4. the preparation method of metal sheet according to claim 1 and thin slice cross section transmission electron microscope sample, it is special
Sign is：Polished using sand paper by cross-sectional sample mechanical reduction.
5. the preparation method of metal sheet according to claim 1 and thin slice cross section transmission electron microscope sample, it is special
Sign is：The material of the non-conductive thin slice is with the relatively low high-molecular compound of certain plasticity and hardness.
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| CN103033403A (en) * | 2011-09-29 | 2013-04-10 | 鞍钢股份有限公司 | Preparation method of thin-sheet metal film test sample |
| CN103335872A (en) * | 2013-06-04 | 2013-10-02 | 首钢总公司 | Method for preparing transmission electron microscope thin film sample of longitudinal section of filament by electrolysis double-spray method |
| CN103592171A (en) * | 2013-11-27 | 2014-02-19 | 内蒙古包钢钢联股份有限公司 | Method for preparing transmission electron microscope sample |
| US9016325B2 (en) * | 2013-06-11 | 2015-04-28 | Dale R. Cowie | Salt guard |
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| CN103033403A (en) * | 2011-09-29 | 2013-04-10 | 鞍钢股份有限公司 | Preparation method of thin-sheet metal film test sample |
| CN103335872A (en) * | 2013-06-04 | 2013-10-02 | 首钢总公司 | Method for preparing transmission electron microscope thin film sample of longitudinal section of filament by electrolysis double-spray method |
| US9016325B2 (en) * | 2013-06-11 | 2015-04-28 | Dale R. Cowie | Salt guard |
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