CN101105463B - TEM sample least effective thickness detection method - Google Patents
TEM sample least effective thickness detection method Download PDFInfo
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- CN101105463B CN101105463B CN2006100287863A CN200610028786A CN101105463B CN 101105463 B CN101105463 B CN 101105463B CN 2006100287863 A CN2006100287863 A CN 2006100287863A CN 200610028786 A CN200610028786 A CN 200610028786A CN 101105463 B CN101105463 B CN 101105463B
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Abstract
The invention relates to an examination method for the examining the smallest effective thickness of transmission electron microscope sample. The laminated shape sample is etched and wedge-shaped substrate is obtained, the transmission electron microscope image of the wedge-shaped substrate is obtained, and the boundary line position of the crystalling phase and amorphous phase is determined. The wedge-shaped substrate is etched and wedge-shaped sample is obtained, and the thickness of the wedge-shaped sample at the position corresponding to the boundary line position is determined as the smallest effective thickness.
Description
Technical field
The present invention relates to semiconductor manufactured materials analysis technical field, particularly the detection method of the minimum net thickness of TEM sample.
Background technology
Along with device feature size reduces, utilization has high-resolution instrument to be observed and analyzes defective and specific microsize, and then optimization technology becomes more and more important.
Transmission electron microscope (transmission electron microscope, TEM) as the important tool of electron micrology, usually in order to the micromechanism of research material, comprise crystal morphology, pore size, heterogeneous structure and lattice imperfection etc., point resolution can reach 0.1nm.Its principle of work is: scattering, absorption, interference and diffraction take place when high-power electron beam penetrates sample, make to form contrast at imaging plane, demonstrate image.
(Focused Ion Beam FIB) has and similar structure of TEM and function focused ion beam.But different with TEM, FIB utilizes high energy ion beam scanning samples surface, by detect the secondary electron that is inspired from sample, forms contrast at imaging plane, demonstrates image.
Now, the main purposes of FIB is to utilize the sputtering phenomenon of its generation, by the energy that increases ion beam the atomic quantity of sputter is increased, to reach the purpose of material being carried out etching processing.Use FIB and can accurately process interesting areas, and can shorten the Production Time of sample significantly, and be not prone to etch rate difference in the specimen material, the manufactured samples material is even.Current, the associated methods that adopts FIB processing and tem observation usually promptly before using the tem analysis material microstructure, adopts FIB technology to carry out the preparation of sample as the microscopic fields structure analysis method.Because the penetration power of electron beam is lower, the density of sample, thickness etc. all can have influence on last image quality.When too high the or thickness of the density of sample is excessive, detect the image that all can't obtain to reflect the specimen material micromechanism by TEM.So sample is necessary for ultra-thin section.
Fig. 1 is a sample structure synoptic diagram in the prior art, as shown in Figure 1, via FIB technology obtain substrate 110 and on sheet sample 100; Described substrate 110 has strip groove, forms the sidewall 111 and the diapire 112 of substrate through strip groove thus; Sheet sample is positioned on the substrate, and the relative side of this sheet sample two and the bottom surface that connects two sides link to each other with diapire 112 with the sidewall 111 of substrate respectively.The thickness 101 of sheet sample is 50～200nm, and the height 102 of sheet sample and width 103 require to determine according to actual detected.
But prepare in the sample process in application FIB technology, when high energy ion beam bombards specimen material with the formation sample, can cause damage to sample surfaces, thereby influence the quality of sample, and then finally have influence on precision of analysis.
Fig. 2 is the cross-sectional view of sample in the prior art, as shown in Figure 2, sample has three-decker, wherein, two is outer for causing sample surfaces to damage formed amorphous layer 130 owing to bombarded by high energy ion beam in the FIB sample making course, and the middle layer is intac crystal layer 120.Fig. 3 is a specimen material micromechanism TEM testing result synoptic diagram, detects the sample structure image obtain as shown in Figure 3 by TEM.According to the contrast principle of TEM light field imaging as can be known, when using tem analysis and having the sample of this three-decker, it has been generally acknowledged that, when having only gross thickness when two amorphous layers, can obtain image 121 orderly, that can reflect the specimen material crystalline phase less than crystal layer thickness; Otherwise what see can only be image 131 unordered, counter sample material amorphous phase.
In the actual production, analyze quality, can reduce sample thickness as far as possible for promoting.But the thickness of the amorphous layer that causes the sample surfaces damage when using existing FIB technology attenuate sample and form is metastable, even sample is thin excessively, the gross thickness that very easily causes two amorphous layers is greater than crystal layer thickness, at this moment, to can not get reflecting the image of specimen material crystal structure, lose the meaning of tem analysis then.Thus, how to form under the certain thickness amorphous layer condition, determining that the thickness of sample that can observe reflection specimen material crystal structure image becomes tem analysis slip-stick artist problem demanding prompt solution.
Application number provides a kind of sample and preparation method thereof in the Chinese patent application of " 200311012961.1 ", use the damage that FIB technology causes sample surfaces but utilize this sample to observe, and can't determine the influence degree of this damage to tem analysis, be that adopting said method can't be judged under the certain thickness amorphous layer condition of formation, how many times thickness of sample is at least, and just can observe the TEM image of reflection specimen material crystal structure.Thus, be badly in need of the detection method of the minimum net thickness of a kind of sample, utilize the method can determine to have the minimum net thickness of the sample of certain thickness amorphous layer, this thickness can guarantee can observe by this sample the TEM image of reflection specimen material crystal structure.
Summary of the invention
The invention provides the detection method of the minimum net thickness of a kind of TEM sample, in order to the minimum net thickness of the sample of determining to have the certain thickness amorphous layer; The invention provides a kind of TEM sample, utilize this sample to carry out tem analysis, can observe the TEM image of reflection specimen material crystalline phase, noncrystalline structure, can assist the minimum net thickness of the sample of determining to have the certain thickness amorphous layer; The invention provides a kind of TEM sample preparation methods, utilize the method to assist to determine the minimum net thickness of sample, and make sample in order to the minimum net thickness of assistant analysis sample with certain thickness amorphous layer.
The detection method of the minimum net thickness of a kind of sample for use in transmitted electron microscope provided by the invention comprises:
The etching sheet sample obtains the wedge shape matrix;
Obtain the images of transmissive electron microscope of wedge shape matrix, and definite crystalline phase, amorphous phase image boundary line position;
Etching wedge shape matrix obtains the wedge shape sample;
The wedge shape thickness of sample of corresponding boundary line position is defined as the minimum net thickness of sample.
Described wedge shape matrix forms after via the focused-ion-beam lithography sheet sample; Described wedge shape matrix is a tri-prismoid; Described wedge shape matrix links to each other with the substrate diapire by a bottom surface; Described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by the side bottom surface; Described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by the side base; Described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by side bottom surface and side base; Described wedge shape matrix thickness is equal to or less than the thickness of sheet sample; Described wedge shape matrix width is equal to or less than the width of sheet sample; Described wedge shape matrix height is equal to or less than the height of sheet sample; Described wedge shape matrix is carried out before the TEM (transmission electron microscope) analysis, in advance etching reference marker on described wedge shape matrix; Described reference marker runs through described wedge shape matrix along described wedge shape matrix thickness direction; The height of described reference marker is less than or equal to the height of described wedge shape matrix; Described reference marker has a tag plane at least, and described tag plane is parallel to wedge shape matrix side bottom surface; Corresponding wedge shape matrix images of transmissive electron microscope crystalline phase boundary line, described wedge shape matrix side bottom surface; Corresponding wedge shape matrix images of transmissive electron microscope amorphous phase boundary line, wedge shape matrix side base; The images of transmissive electron microscope of the wedge shape matrix at corresponding reference marker tag plane place is a mark line; Described mark line is parallel to wedge shape matrix images of transmissive electron microscope crystalline phase boundary line or amorphous phase boundary line; The particular location of crystalline phase, amorphous phase image boundary line is determined by the distance between described boundary line and mark line in the described wedge shape matrix images of transmissive electron microscope; The particular location of crystalline phase, amorphous phase image boundary line is determined by the distance between described boundary line and amorphous phase boundary line in the described wedge shape matrix images of transmissive electron microscope; Before making the wedge shape sample, cover a protective seam at the wedge shape matrix surface; Described step at TEM wedge shape matrix surface protective mulch comprises:
Choose smooth, a smooth finished surface, on described finished surface, drip protective agent;
Described wedge shape matrix is placed described protective agent;
Solidify described protective agent, form protective seam at described wedge shape matrix surface;
The wedge shape matrix of etching protective mulch, the wedge shape sample of acquisition desired thickness.
Described protective agent material is a kind of or its combination in the materials such as various epoxy resin, synthetic resin; Described wedge shape matrix reference marker place is full of protective agent; Described wedge shape sample forms after via focused-ion-beam lithography wedge shape matrix; The particular location of crystalline phase, amorphous phase image boundary line is determined by the distance between described boundary line and mark line in the described wedge shape sample images of transmissive electron microscope; The particular location of crystalline phase, amorphous phase image boundary line is determined by the distance between described boundary line and amorphous phase boundary line in the described wedge shape sample images of transmissive electron microscope.
A kind of sample for use in transmitted electron microscope method for making provided by the invention comprises:
The etching sheet sample obtains the wedge shape matrix;
Etching wedge shape matrix obtains the wedge shape sample;
Described wedge shape matrix forms after via focused particle beam etching sheet sample; Described wedge shape matrix is a tri-prismoid; Described wedge shape matrix links to each other with the substrate diapire by a bottom surface; Described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by the side bottom surface; Described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by the side base; Described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by side bottom surface and side base; Described wedge shape matrix thickness is equal to or less than the thickness of sheet sample; Described wedge shape matrix width is equal to or less than the width of sheet sample; Described wedge shape matrix height is equal to or less than the height of sheet sample; Described wedge shape matrix is carried out before the TEM (transmission electron microscope) analysis, in advance etching reference marker on described wedge shape matrix; Described reference marker runs through described wedge shape matrix along described wedge shape matrix thickness direction; The height of described reference marker is less than or equal to the height of described wedge shape matrix; Described reference marker has a tag plane at least, and described tag plane is parallel to wedge shape matrix side bottom surface; Described wedge shape sample obtains by high energy ion beam etching wedge shape matrix.
Before making the wedge shape sample, cover a protective seam at the wedge shape matrix surface; Described step at wedge shape matrix surface protective mulch comprises:
Choose smooth, a smooth finished surface, on described finished surface, drip protective agent;
Described wedge shape matrix is placed described protective agent;
Solidify described protective agent, form protective seam at described wedge shape matrix surface;
Etching wedge shape matrix, the wedge shape sample of acquisition desired thickness.
Described protective agent material is a kind of or its combination in the materials such as various epoxy resin, synthetic resin; Corresponding wedge shape matrix reference marker place is full of protective agent in the described wedge shape sample; Described wedge shape sample forms after via focused-ion-beam lithography wedge shape matrix.
A kind of sample for use in transmitted electron microscope provided by the invention, described wedge shape sample is a tri-prismoid; Protected dose of encirclement of described wedge shape sample both side surface; Corresponding wedge shape matrix reference marker place is full of protective agent in the described wedge shape sample.
Compared with prior art, the present invention has the following advantages:
1. in the preparation process of wedge shape sample provided by the invention, can obtain to reflect simultaneously the TEM image of wedge shape specimen material crystalline phase, noncrystalline structure, the TEM image of using this TEM image and the final wedge shape sample that forms can determine to have the minimum net thickness of the sample of certain thickness amorphous layer, sample with this thickness is carried out tem analysis, can observe the image of reflection specimen material crystal structure;
2. by in the preparation process of TEM wedge shape matrix provided by the invention, making reference marker, can obtain the minimum net thickness size of accurate sample;
3. pass through in the preparation process of TEM wedge shape sample provided by the invention at wedge shape matrix surface protective mulch; can protect the amorphous layer consistency of thickness of the amorphous layer thickness of the wedge shape sample that makes with the wedge shape matrix; simultaneously; by in TEM wedge shape matrix reference marker, being full of protective layer material; can obtain to have the TEM wedge shape sample of reference marker, the two has all advantageously guaranteed precision of analysis.
Description of drawings
Fig. 1 is a sample structure synoptic diagram in the prior art;
Fig. 2 is the cross-sectional view of sample in the prior art;
Fig. 3 is a specimen material micromechanism TEM testing result synoptic diagram;
Fig. 4 detects synoptic diagram for the wedge shape matrix TEM of the explanation embodiment of the invention one;
Fig. 5 is the wedge shape matrix TEM testing result synoptic diagram of the explanation embodiment of the invention one;
Fig. 6 is the making schematic flow sheet of the wedge shape sample of the explanation embodiment of the invention one;
Fig. 7 is the wedge shape sample TEM testing result synoptic diagram of the explanation embodiment of the invention one;
Fig. 8 detects synoptic diagram for the wedge shape matrix TEM of the explanation embodiment of the invention two;
Fig. 9 is the wedge shape sample TEM testing result synoptic diagram of the explanation embodiment of the invention two.
Wherein:
100: sheet sample; 110: substrate;
101: sheet sample thickness; 102: the sheet sample height;
103: the sheet sample width; 111: the substrate sidewall;
112: the substrate diapire; 120: the specimen material crystal layer;
121: specimen material crystalline phase TEM image; 130: the specimen material amorphous layer;
131: specimen material amorphous phase TEM image; 200: the wedge shape matrix;
210: wedge shape matrix crystal layer; 211: wedge shape matrix crystalline phase TEM image;
212: wedge shape sample crystalline phase TEM image; 220: wedge shape matrix amorphous layer;
221: wedge shape matrix amorphous phase TEM image; 222: wedge shape sample amorphous phase TEM image;
230: reference marker; 231: reference marker TEM image;
240: index face; 241: mark line;
250: wedge shape matrix drift angle; 260: the wedge shape matrix thickness;
270: the wedge shape matrix height; 280: the wedge shape matrix width;
301: the crystalline phase boundary line; 302: crystalline phase, amorphous phase TEM image boundary line;
303: the amorphous phase boundary line; 400: finished surface;
500: protective agent; 510: protective seam.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, the specific embodiment of the present invention is described in detail below in conjunction with accompanying drawing.
The main process of the detection method of the minimum net thickness of TEM sample provided by the invention is: at first, based on sheet sample, utilize FIB technology to obtain the wedge shape matrix; Then, described wedge shape matrix is carried out tem analysis, obtain to reflect simultaneously the TEM image of specimen material crystalline phase, noncrystalline structure, and the particular location of definite crystalline phase, amorphous phase image boundary; Subsequently, obtain the wedge shape sample; At last, described wedge shape sample is carried out tem analysis, the sheet sample thickness of corresponding crystalline phase, amorphous phase image boundary particular location is defined as the minimum net thickness of sample.
As the first embodiment of the present invention, the concrete steps of the detection method of the minimum net thickness of described sample are:
At first, utilize FIB technology, the etching sheet sample obtains the wedge shape matrix.
Fig. 4 detects synoptic diagram for the wedge shape matrix TEM of the explanation embodiment of the invention one, and as shown in Figure 4, described wedge shape matrix 200 forms behind negative Z direction etching sheet sample via FIB; Described wedge shape matrix is a tri-prismoid; Described tri-prismoid is the bottom surface with the triangular surface, and promptly described tri-prismoid xsect is a triangle; Described triangular cross section has a base and dual-side, and described triangular cross section can link to each other with substrate sidewall 111 by the base; The common side bottom surface of forming described wedge shape matrix, the base of triangular cross section; The end points of the triangular cross section of described base correspondence is the summit; The common side base of forming described wedge shape matrix, the summit of triangular cross section; Two side surfaces of described wedge shape matrix link to each other via the side base; The interior angle of corresponding vertex is the drift angle 250 of described wedge shape matrix in the described triangular cross section; The drift angle 250 of described wedge shape matrix is determined according to sheet sample specification, technological parameter etc.; Described wedge shape matrix thickness 260 is less gradually to the side base from the side bottom surface; Described wedge shape matrix height 270 is equal to or less than the height of sheet sample; Described wedge shape matrix width 280 is equal to or less than the width of sheet sample; The thickness 260 of described wedge shape matrix is equal to or less than the thickness of sheet sample; Described wedge shape matrix 200 is positioned on the substrate 110, and this wedge shape matrix links to each other with substrate diapire 112 by a bottom surface, and simultaneously, its side bottom surface and side base can link to each other with substrate sidewall 111 respectively or link to each other with substrate sidewall 111 jointly; Again or, this wedge shape matrix only links to each other with substrate diapire 112 by a bottom surface.As the embodiment of the inventive method, select drift angle to be 15 °, to link to each other with substrate by a bottom surface, the wedge shape matrix that its side bottom surface links to each other with substrate sidewall 111 is the concrete implementation step of example explanation this method.
Really; the special selection that the concrete connected mode of described wedge shape matrix of selecting for use and substrate is made for ease of the explanation specific embodiment of the invention; should be as qualification to the inventive method embodiment; the arbitrarily rational change that those skilled in the art make this does not influence the enforcement of the inventive method, and should be included in protection scope of the present invention.
As shown in Figure 4, two side surfaces of described wedge shape matrix have amorphous structure, and described amorphous structure is to produce when using FIB processes wedge shape matrix.
Then, described wedge shape matrix is carried out tem analysis, obtain to reflect simultaneously the TEM image of specimen material crystalline phase, noncrystalline structure, and the particular location of definite crystalline phase, noncrystalline structure boundary.
Before described wedge shape matrix is carried out tem analysis,, need on described wedge shape matrix, to make in advance reference marker 230 for obtaining the particular location of crystalline phase, amorphous phase image boundary accurately.The making of described reference marker makes via the ion etching step; Described reference marker runs through described wedge shape matrix along described wedge shape matrix thickness direction; Described reference marker has a tag plane 240 at least, and described tag plane is parallel to the side bottom surface of wedge shape matrix; The particular location of described reference marker is determined according to the concrete thickness of existing technological parameter and wedge shape matrix diverse location; The particular location of described reference marker should guarantee that follow-up wedge shape matrix TEM testing result presents crystalline phase in reference marker TEM image peripheral region; The height of described reference marker is less than or equal to the height of described wedge shape matrix.
As the embodiment of the inventive method, selecting described reference marker is that rectangle and height are the concrete implementation step of example explanation this method less than the wedge shape matrix of described wedge shape matrix height at wedge shape matrix side surface place xsect.At this moment, the side of selecting to be parallel to wedge shape matrix side bottom surface and the described reference marker nearer apart from the side base is a tag plane.
Really; described wedge shape matrix is made the special selection that this reference marker is made for ease of the explanation specific embodiment of the invention; should be as qualification to the inventive method embodiment; the arbitrarily rational change that those skilled in the art make this does not influence the enforcement of the inventive method, and should be included in protection scope of the present invention.
When the described wedge shape matrix that has reference marker was carried out tem analysis, described TEM electron beam was along the normal direction incident of any side surface of wedge shape matrix.
As the embodiment of the inventive method, be the concrete implementation step of the described wedge shape matrix side surface of Y-axis negative sense as plane of incidence explanation this method of TEM electron beam with the normal direction.
Really; the special selection that described TEM electron beam incident face is made for ease of the explanation specific embodiment of the invention; should be as qualification to the inventive method embodiment; the arbitrarily rational change that those skilled in the art make this does not influence the enforcement of the inventive method, and should be included in protection scope of the present invention.
Fig. 5 is the wedge shape matrix TEM testing result synoptic diagram of the explanation embodiment of the invention one, as shown in Figure 5, the described wedge shape matrix that has reference marker carried out tem analysis after, reflected the wedge shape matrix TEM image of specimen material crystalline phase, noncrystalline structure simultaneously; There is tangible boundary line 302 between the image-region of reflection specimen material crystalline phase, noncrystalline structure in the described wedge shape matrix TEM image; Corresponding wedge shape matrix TEM image crystalline phase boundary line, wedge shape matrix side bottom surface 301; Corresponding wedge shape matrix TEM image amorphous phase boundary line, wedge shape matrix side base 303; The TEM image of the wedge shape matrix at corresponding reference marker place is a white space 231; The TEM image of the wedge shape matrix at the tag plane place of corresponding described reference marker is a mark line 241, and described mark line is parallel to wedge shape matrix images of transmissive electron microscope crystalline phase boundary line or amorphous phase boundary line; Measure and write down the distance L 1 between described boundary line and mark line, promptly determined the particular location of crystalline phase, amorphous phase image boundary.
Subsequently, etching wedge shape matrix obtains the wedge shape sample.
Utilize high energy ion beam etching wedge shape matrix, to make the wedge shape sample; Described wedge shape thickness of sample comprises any thickness value of tem analysis requirement.
Fig. 6 is the making schematic flow sheet of the wedge shape sample of the explanation embodiment of the invention one; as shown in Figure 6; before making the wedge shape sample, the amorphous layer thickness of established wedge shape sample side surface is not impacted for guaranteeing described high energy ion beam, need to cover a protective seam at the wedge shape matrix surface.
Described concrete steps at TEM wedge shape matrix surface protective mulch are:
Step 61: choose smooth, a smooth finished surface 400, on described finished surface, drip protective agent 500.
Step 62: described wedge shape matrix 200 is placed described protective agent, make the wedge shape matrix surface cover a protective agent layer, and wedge shape matrix reference marker inside is full of described protective agent.
For making things convenient for subsequent technique to carry out; usually be axle with described wedge shape matrix with its side surface and substrate diapire connecting line; flip an angle,, and then make described wedge shape matrix 200 place described protective agent so that described wedge shape matrix 200 is statically placed in described finished surface 400.In the specific embodiment of the present invention, be axle with it with its side surface and substrate diapire connecting line, overturn 90 °, be about to described wedge shape matrix 200 and place described protective agent the wedge shape matrix.Described flip angle is determined according to substrate shape.Fig. 6 is with after 90 ° of the wedge shape matrix upsets, the synoptic diagram that obtains along wedge shape body upper surface normal direction.
Step 63: solidify described protective agent, form protective seam at described wedge shape matrix surface.
Described protective agent material is a kind of or its combination in the materials such as various epoxy resin, synthetic resin; The selection of described solidification temperature and set time is determined according to the protective agent material character.
Step 64: in wedge shape matrix reference marker altitude range, etching wedge shape matrix makes the wedge shape sample of desired thickness.
The xsect of described wedge shape sample is a triangle; Described etching technics adopts FIB to carry out; Protected dose of encirclement of described wedge shape sample dual-side; Corresponding wedge shape matrix reference marker place is a discontinuity area in the described wedge shape sample, is full of protective agent in the described discontinuity area.Obviously, described wedge shape sample is the part of wedge shape matrix, and real wedge shape matrix for highly reducing is so be applicable to described wedge shape sample to the description of wedge shape basal body structure.
At last, described wedge shape sample is carried out tem analysis, the wedge shape thickness of sample of corresponding crystalline phase, noncrystalline structure boundary particular location is defined as the minimum net thickness of wedge shape sample.
Fig. 7 is the wedge shape sample TEM testing result synoptic diagram of the explanation embodiment of the invention one, and as shown in Figure 7, described wedge shape sample dual-side protected seam 510 surrounds; Corresponding wedge shape matrix reference marker place is a discontinuity area in the described wedge shape sample, is full of protective agent in the described discontinuity area; Can clear differentiation specimen material crystal phase structure 212 in the described wedge shape sample TEM image, noncrystalline structure 222 images, but can not obtain specimen material crystalline phase, amorphous phase image; Corresponding wedge shape sample TEM image crystalline phase boundary line, wedge shape sample side bottom surface 301; Corresponding wedge shape sample TEM image amorphous phase boundary line, wedge shape sample side base 303; The TEM image of the wedge shape sample at corresponding reference marker place is a white space 231; The TEM image of the wedge shape sample at the tag plane place of corresponding described reference marker is a mark line 241, and described mark line is parallel to wedge shape sample images of transmissive electron microscope crystalline phase boundary line;
With described mark line is benchmark, between described mark line and described amorphous phase frontier point, measuring distance L1, be to be the L1 place with the mark line distance in described mark line and the described amorphous phase frontier point interval region, present the particular location of crystalline phase, noncrystalline structure boundary in the corresponding wedge shape sample TEM image.
Measure the wedge shape thickness of sample L of corresponding crystalline phase, noncrystalline structure boundary, this one-tenth-value thickness 1/10 is the minimum net thickness of the sample with certain thickness amorphous layer, promptly, all can guarantee to observe the TEM image of reflection specimen material crystal structure by this sample when thickness of sample during greater than this minimum net thickness L.
As second embodiment of the inventive method, the concrete steps of the detection method of the minimum net thickness of described sample are:
At first, utilize FIB technology, the etching sheet sample obtains the wedge shape matrix.
Then, described wedge shape matrix is carried out tem analysis, obtain to reflect simultaneously the TEM image of wedge shape specimen material crystalline phase, noncrystalline structure, and the particular location of definite crystalline phase, noncrystalline structure boundary.
Fig. 8 detects synoptic diagram for the wedge shape matrix TEM of the explanation embodiment of the invention two, as shown in Figure 8, described wedge shape matrix carried out tem analysis after, reflected the wedge shape matrix TEM image of specimen material crystalline phase, noncrystalline structure simultaneously; There is tangible boundary line 302 between the image-region of reflection specimen material crystalline phase 211, amorphous phase 221 structures in the described wedge shape matrix TEM image; Corresponding wedge shape matrix TEM image crystalline phase boundary line, described wedge shape matrix side bottom surface 301; Corresponding wedge shape matrix TEM image amorphous phase boundary line, described wedge shape matrix side base 303.Measure and write down the distance L 2 between described boundary line and amorphous phase boundary line, promptly in described crystalline phase boundary line and amorphous phase boundary line spacing distance apart from L2 place, amorphous phase boundary line, present the particular location of crystalline phase, noncrystalline structure boundary in the corresponding wedge shape sample TEM image.
Subsequently, utilize FIB technology, etching wedge shape matrix obtains the wedge shape sample.
Described wedge shape thickness of sample comprises any thickness value of tem analysis requirement.Before making the wedge shape sample, the thickness of established wedge shape sample side surface amorphous layer is not impacted for guaranteeing described high energy ion beam, need to cover a protective seam at the wedge shape matrix surface.
Described concrete steps at TEM wedge shape matrix surface protective mulch are:
Step 81: choose smooth, a smooth finished surface, on described finished surface, drip protective agent.
Step 82: described wedge shape matrix is placed described protective agent, make the wedge shape matrix surface cover a protective agent layer.
Step 83: solidify described protective agent, form protective seam at described wedge shape matrix surface.
Described protective agent material is a kind of or its combination in the materials such as various epoxy resin, synthetic resin; The selection of described solidification temperature and set time is determined according to the protective agent material character.
Step 84: etching wedge shape matrix makes the wedge shape sample of desired thickness.
The xsect of described wedge shape sample is a triangle; Described wedge shape sample dual-side protected seam surrounds.
At last, described wedge shape sample is carried out tem analysis, the wedge shape thickness of sample of corresponding crystalline phase, noncrystalline structure boundary particular location is defined as the minimum net thickness of sample.
Fig. 9 is the wedge shape sample TEM testing result synoptic diagram of the explanation embodiment of the invention two, as shown in Figure 9, can clear differentiation specimen material crystal phase structure 212 in the described wedge shape sample TEM image, noncrystalline structure 222 images, but can not obtain specimen material crystalline phase, amorphous phase image; Described wedge shape sample both side surface protected seam 510 surrounds; Corresponding wedge shape sample TEM image crystalline phase boundary line, wedge shape sample side bottom surface 301; Corresponding wedge shape sample TEM image amorphous phase boundary line, wedge shape sample side base 303; With described amorphous phase boundary line is benchmark, between amorphous phase boundary line and crystalline phase boundary line, measuring distance L2, promptly in described crystalline phase boundary line and amorphous phase boundary line spacing distance, be the L2 place, present the particular location of crystalline phase, noncrystalline structure boundary in the corresponding wedge shape sample TEM image with described amorphous phase boundary line distance.
Measure the wedge shape sample thickness L of corresponding crystalline phase, noncrystalline structure boundary, this one-tenth-value thickness 1/10 is the minimum net thickness of the sample with certain thickness amorphous layer, promptly, all can guarantee to observe the TEM image of reflection wedge shape specimen material crystal structure by this sample when thickness of sample during greater than this minimum net thickness L.
Adopt the inventive method, in the preparation process of wedge shape matrix, can obtain to reflect simultaneously the TEM image of specimen material crystalline phase, noncrystalline structure, the TEM image of using this TEM image and the final wedge shape sample that forms can determine to have the minimum net thickness of the sample of certain thickness amorphous layer; By in the preparation process of wedge shape matrix provided by the invention, making reference marker, can obtain the minimum net thickness size of accurate sample; By in the preparation process of wedge shape sample provided by the invention at wedge shape matrix surface protective mulch; can protect the amorphous layer consistency of thickness of the amorphous layer thickness of the wedge shape sample that makes with the wedge shape matrix; simultaneously; by in wedge shape matrix mark, being full of protective layer material; can obtain to have the wedge shape sample of reference marker, the two has all advantageously guaranteed precision of analysis.
Though the present invention with preferred embodiment openly as above; but it is not to be used for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; can make possible change and modification, so protection scope of the present invention should be as the criterion with the scope that claim of the present invention was defined.
Claims (44)
1. the detection method of the minimum net thickness of sample for use in transmitted electron microscope is characterized in that, comprising:
The etching sheet sample obtains the wedge shape matrix;
Obtain the images of transmissive electron microscope of wedge shape matrix, and definite crystalline phase, amorphous phase image boundary line position;
Etching wedge shape matrix obtains the wedge shape sample;
Obtain the images of transmissive electron microscope of wedge shape sample, according to described wedge shape matrix images of transmissive electron microscope definite crystalline phase, amorphous phase image boundary line position, in described wedge shape sample images of transmissive electron microscope, the wedge shape thickness of sample of corresponding boundary line position is defined as the minimum net thickness of sample.
2. method according to claim 1 is characterized in that: described wedge shape matrix forms after via the focused-ion-beam lithography sheet sample.
3. method according to claim 2 is characterized in that: described wedge shape matrix is a tri-prismoid.
4. method according to claim 3 is characterized in that: described wedge shape matrix links to each other with the substrate diapire by a bottom surface.
5. method according to claim 3 is characterized in that: described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by the side bottom surface.
6. method according to claim 3 is characterized in that: described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by the side base.
7. method according to claim 3 is characterized in that: described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by side bottom surface and side base.
8. method according to claim 3 is characterized in that: described wedge shape matrix thickness is equal to or less than the thickness of sheet sample.
9. method according to claim 3 is characterized in that: described wedge shape matrix width is equal to or less than the width of sheet sample.
10. method according to claim 3 is characterized in that: described wedge shape matrix height is equal to or less than the height of sheet sample.
11. method according to claim 1 is characterized in that: described wedge shape matrix is carried out before the TEM (transmission electron microscope) analysis, in advance etching reference marker on described wedge shape matrix.
12. method according to claim 11 is characterized in that: described reference marker runs through described wedge shape matrix along described wedge shape matrix thickness direction.
13. method according to claim 12 is characterized in that: the height of described reference marker is less than or equal to the height of described wedge shape matrix.
14. method according to claim 13 is characterized in that: described reference marker has a tag plane at least, and described tag plane is parallel to wedge shape matrix side bottom surface.
15. method according to claim 1 is characterized in that: corresponding wedge shape matrix images of transmissive electron microscope crystalline phase boundary line, described wedge shape matrix side bottom surface; Corresponding wedge shape matrix images of transmissive electron microscope amorphous phase boundary line, wedge shape matrix side base.
16. method according to claim 15 is characterized in that: the images of transmissive electron microscope of the wedge shape matrix at corresponding reference marker tag plane place is a mark line; Described mark line is parallel to wedge shape matrix images of transmissive electron microscope crystalline phase boundary line or amorphous phase boundary line.
17. method according to claim 1 is characterized in that: the particular location of crystalline phase, amorphous phase image boundary line is determined by the distance between described boundary line and mark line in the described wedge shape matrix images of transmissive electron microscope.
18. method according to claim 1 is characterized in that: the particular location of crystalline phase, amorphous phase image boundary line is determined by the distance between described boundary line and amorphous phase boundary line in the described wedge shape matrix images of transmissive electron microscope.
19. method according to claim 1 is characterized in that: before making the wedge shape sample, cover a protective seam at the wedge shape matrix surface.
20. method according to claim 19 is characterized in that: described step at TEM wedge shape matrix surface protective mulch comprises:
Choose smooth, a smooth finished surface, on described finished surface, drip protective agent;
Described wedge shape matrix is placed described protective agent;
Solidify described protective agent, form protective seam at described wedge shape matrix surface;
The wedge shape matrix of etching protective mulch, the wedge shape sample of acquisition desired thickness.
21. method according to claim 20 is characterized in that: described protective agent material is a kind of or its combination in various epoxy resin, the synthetic resin material.
22. method according to claim 21 is characterized in that: described wedge shape matrix reference marker place is full of protective agent.
23. method according to claim 1 is characterized in that: described wedge shape sample forms after via focused-ion-beam lithography wedge shape matrix.
24. according to claim 1 or 17 described methods, it is characterized in that: the particular location of crystalline phase, amorphous phase image boundary line is determined by the distance between described boundary line and mark line in the described wedge shape sample images of transmissive electron microscope.
25. according to claim 1 or 18 described methods, it is characterized in that: the particular location of crystalline phase, amorphous phase image boundary line is determined by the distance between described boundary line and amorphous phase boundary line in the described wedge shape sample images of transmissive electron microscope.
26. a sample for use in transmitted electron microscope method for making is characterized in that, comprising:
The etching sheet sample obtains the wedge shape matrix, and described wedge shape matrix forms after via the focused-ion-beam lithography sheet sample;
Etching wedge shape matrix obtains the wedge shape sample.
27. method according to claim 26 is characterized in that: described wedge shape matrix is a tri-prismoid.
28. method according to claim 27 is characterized in that: described wedge shape matrix links to each other with the substrate diapire by a bottom surface.
29. method according to claim 27 is characterized in that: described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by the side bottom surface.
30. method according to claim 27 is characterized in that: described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by the side base.
31. method according to claim 27 is characterized in that: described wedge shape matrix links to each other with the substrate diapire by a bottom surface, links to each other with the substrate sidewall by side bottom surface and side base.
32. method according to claim 27 is characterized in that: described wedge shape matrix thickness is equal to or less than the thickness of sheet sample.
33. method according to claim 27 is characterized in that: described wedge shape matrix width is equal to or less than the width of sheet sample.
34. method according to claim 27 is characterized in that: described wedge shape matrix height is equal to or less than the height of sheet sample.
35. method according to claim 26 is characterized in that: described wedge shape matrix is carried out before the TEM (transmission electron microscope) analysis, in advance etching reference marker on described wedge shape matrix.
36. method according to claim 35 is characterized in that: described reference marker runs through described wedge shape matrix along described wedge shape matrix thickness direction.
37. method according to claim 36 is characterized in that: the height of described reference marker is less than or equal to the height of described wedge shape matrix.
38. according to the described method of claim 37, it is characterized in that: described reference marker has a tag plane at least, described tag plane is parallel to wedge shape matrix side bottom surface.
39. method according to claim 26 is characterized in that: described wedge shape sample obtains by focused-ion-beam lithography wedge shape matrix.
40. method according to claim 26 is characterized in that: before making the wedge shape sample, cover a protective seam at the wedge shape matrix surface.
41. according to the described method of claim 40, it is characterized in that: described step at wedge shape matrix surface protective mulch comprises:
Choose smooth, a smooth finished surface, on described finished surface, drip protective agent;
Described wedge shape matrix is placed described protective agent;
Solidify described protective agent, form protective seam at described wedge shape matrix surface;
Etching wedge shape matrix, the wedge shape sample of acquisition desired thickness.
42. according to the described method of claim 41, it is characterized in that: described protective agent material is a kind of or its combination in various epoxy resin, the synthetic resin material.
43. according to the described method of claim 42, it is characterized in that: corresponding wedge shape matrix reference marker place is full of protective seam in the described wedge shape sample.
44. method according to claim 26 is characterized in that: described wedge shape sample forms after via focused-ion-beam lithography wedge shape matrix.
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| JP5649583B2 (en) | 2008-10-31 | 2015-01-07 | エフ イー アイ カンパニＦｅｉ Ｃｏｍｐａｎｙ | Processing end point detection method and apparatus |
| CN104677709A (en) * | 2015-02-12 | 2015-06-03 | 江苏省沙钢钢铁研究院有限公司 | Method for making interface high resolution transmission electron microscopy (HRTEM) sample with special crystalline orientation relation |
| CN110174424A (en) * | 2019-04-25 | 2019-08-27 | 南方科技大学 | Transmitted electron microscope sample preparation method |
| CN112881439A (en) * | 2021-03-09 | 2021-06-01 | 洪启集成电路(珠海)有限公司 | OLED TEM sample preparation method and OLED TEM sample |
| CN113189370A (en) * | 2021-05-28 | 2021-07-30 | 上海华力微电子有限公司 | Preparation method of TEM sample |
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