CN103808540A - Transmission electron microscope sample preparation method - Google Patents
Transmission electron microscope sample preparation method Download PDFInfo
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- CN103808540A CN103808540A CN201210444665.2A CN201210444665A CN103808540A CN 103808540 A CN103808540 A CN 103808540A CN 201210444665 A CN201210444665 A CN 201210444665A CN 103808540 A CN103808540 A CN 103808540A
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Abstract
The present invention discloses a transmission electron microscope sample preparation method, which comprises cutting a wafer to provide an initial transmission electron microscope (TEM )sample, depositing protection layers in regions according to different material contrasts TEM sample observation regions, wherein the concrete depositing method comprises that a carbon or silicon oxide protection layer is deposited on the surface of a sample material with the deep contrast, and a platinum or tungsten protection layer is deposited on the surface of a sample material with the light contrast. According to the present invention, the morphology of different structures in the same TEM sample can be clearly observed.
Description
Technical field
The present invention relates to Analysis of Semiconductor Materials technology, particularly a kind of method for making of example of transmission electron microscope.
Background technology
Transmission electron microscope (transmission electron microscope, TEM) be the IC industry observation very important instrument of micromechanism and means, it is using high-power electron beam as light source, make lens with electromagnetic field, to project on very thin sample through the electron beam accelerating and assemble, because the penetration power of electron beam is very weak, therefore must make the ultra-thin section of the about 100nm of thickness left and right for the sample of Electronic Speculum.
When prior art is prepared sample thin slice; generally first by wafer cutting being provided to an initial TEM sample; then adopt the method for focused ion beam (FIB) to cut attenuate to initial TEM sample; but generally at initial TEM sample surfaces deposition layer protective layer, made sample distortion for preventing the high energy ion beam of FIB from acting on sample surfaces or damaged before adopting FIB method.Protective seam can be for having metal platinum (Pt) or the tungsten (W) of dark contrast, can be also carbon (C) layer or the silicon oxide layer with shallow contrast.
Along with the exploitation of semicon industry advanced process, the critical size of device is more and more less, below processing procedure is 45 nanometers time, the live width of sample figure may be much smaller than the thickness of transmission electron microscopy observation sample, so may comprise multi-layer material and structure within the scope of the TEM thickness of sample of preparing.While using the cross section of transmission electron microscopy observation sample; different materials has different depth contrasts; and it is general only at the unified protective seam of sample surfaces deposition in prior art; if the contrast of this protective seam is similar with the material contrast of the structure that need to observe; just there will be ghost image phenomenon, affect the judgement of this structure and morphology and the measurement of size.
Summary of the invention
In view of this, the invention provides a kind of method for making of example of transmission electron microscope, can in same TEM sample, clearly observe the pattern of different structure.
Technical scheme of the present invention is achieved in that
A method for making for example of transmission electron microscope, the method comprises:
By wafer cutting being provided to an initial transmission electron microscope TEM sample;
At described initial TEM sample surfaces; according to the difference of the material contrast of TEM sample observation area; subregion deposition protective seam; concrete grammar is: have specimen material surface deposition carbon or the monox protective seam of dark contrast, having specimen material surface deposition platinum or the tungsten protective seam of shallow contrast.
The specimen material with dark contrast is germanium-silicon layer; The specimen material with shallow contrast is silicon oxide layer.
Described initial TEM sample at least comprises the active area germanium-silicon layer higher than wafer substrate surface, has polysilicon gate, take this orientation as directions X in the relative both sides of germanium-silicon layer; Another relative both sides have the shallow channel isolation area lower than wafer substrate surface, take this orientation as Y-direction;
The carbon protective layer that forms patterning at described initial TEM sample surfaces, the carbon protective layer of described patterning is cover part germanium-silicon layer in the Y direction, and covers respectively the shallow channel isolation area of the relative both sides of germanium-silicon layer;
At described initial TEM sample surfaces deposition platinum protective seam, described platinum protective seam covers the edge of germanium-silicon layer and carbon protective layer in the Y direction, covers the polysilicon gate of the relative both sides of germanium-silicon layer on directions X.
Described initial TEM sample is multiple repeat patterns of arranging in turn, and each pattern at least comprises the active area germanium-silicon layer higher than wafer substrate surface, has polysilicon gate, take this orientation as directions X in the relative both sides of germanium-silicon layer; Another relative both sides have the shallow channel isolation area lower than wafer substrate surface, take this orientation as Y-direction;
At described initial TEM sample surfaces deposit carbon protective seam, described carbon protective layer covers a predetermined number pattern;
At described initial TEM sample surfaces deposition platinum protective seam, described platinum protective seam covers residue pattern.
Also coated carbon protective seam of described platinum protective seam.
Described initial TEM sample is multiple repeat patterns of arranging in turn, and each pattern at least comprises the active area germanium-silicon layer higher than wafer substrate surface, has polysilicon gate, take this orientation as directions X in the relative both sides of germanium-silicon layer; Another relative both sides have the shallow channel isolation area lower than wafer substrate surface, take this orientation as Y-direction;
At described initial TEM sample surfaces deposition platinum protective seam, described platinum protective seam covers a predetermined number pattern;
At described initial TEM sample surfaces deposit carbon protective seam, described carbon protective layer covers residue pattern.
It is residual that described polysilicon gate both sides have monox.
Described wafer is cut to the focused ion beam method of adopting.
Can find out from such scheme; the method of the present invention per sample contrast of zones of different material is chosen flexibly protective seam and is covered; unlike prior art; same sample is chosen unified protective seam; can, in the time adopting TEM observation, in same TEM sample, obtain abundant sample message like this.
Accompanying drawing explanation
Fig. 1 a is embodiment mono-by the schematic top plan view of the initial TEM sample that wafer cutting is obtained.
Fig. 1 b is the Y-direction sectional view corresponding with Fig. 1 a.
Fig. 1 c is the directions X sectional view corresponding with Fig. 1 a.
Fig. 2 a is the schematic top plan view of the embodiment of the present invention one at TEM sample surfaces deposition protective seam.
Fig. 2 b is the Y-direction sectional view corresponding with Fig. 2 a.
Fig. 2 c is the directions X sectional view corresponding with Fig. 2 a.
Fig. 3 a is embodiment bis-by the schematic top plan view of the initial TEM sample that wafer cutting is obtained.
Fig. 3 b is the schematic top plan view of the embodiment of the present invention two at TEM sample surfaces deposition protective seam.
Fig. 3 c be corresponding with Fig. 3 b to pattern (2) at Y-direction sectional view.
Fig. 3 d be corresponding with Fig. 3 b to pattern (1) or (3) at Y-direction sectional view.
Embodiment
For making object of the present invention, technical scheme and advantage clearer, referring to the accompanying drawing embodiment that develops simultaneously, the present invention is described in further detail.
Core concept of the present invention is: by wafer cutting being provided to an initial TEM sample; Then at described initial TEM sample surfaces; according to the difference of the material contrast of TEM sample observation area; subregion deposition protective seam; concrete grammar is: have specimen material surface deposition carbon or the monox protective seam of dark contrast, having specimen material surface deposition platinum or the tungsten protective seam of shallow contrast.Here, those skilled in the art can know, the difference of dark contrast and shallow contrast, and general platinum, tungsten, germanium-silicon layer etc. are dark contrast material, carbon-coating, silicon oxide layer etc. is shallow contrast material.
Embodiment mono-:
Fig. 1 a is embodiment mono-by the schematic top plan view of the initial TEM sample that wafer cutting is obtained.After FIB cutting attenuate, reservation be the pattern of Fig. 1 a core, because the critical size of device is less, so after FIB method, TEM sample remains with active area and shallow channel isolation area.TEM sample at least comprises the active area germanium-silicon layer 101 higher than wafer substrate 100 surfaces, has polysilicon gate 102 in the relative both sides of germanium-silicon layer 101, is defined as directions X with this orientation; Another relative both sides have the shallow channel isolation area 103 lower than wafer substrate 100 surfaces, are defined as Y-direction with this orientation.
Fig. 1 b is the Y-direction sectional view corresponding with Fig. 1 a.Fig. 1 c is the directions X sectional view corresponding with Fig. 1 a.Can find out from Fig. 1 b and Fig. 1 c, shallow channel isolation area 103 is lower than wafer substrate 100 surfaces, and germanium-silicon layer 101 epitaxial growths form, so can be higher than wafer substrate 100 surfaces.
By the analysis to this TEM sample in cross section, need to obtain two kinds of information: the one, whether observation has monox 104 residual in polysilicon gate 102 both sides; The 2nd, the pattern of observation germanium-silicon layer 101.If as prior art, deposit unified protective seam at TEM sample surfaces, for example deposit the platinum protective seam of dark contrast, while analyzing so TEM sample, because outstanding germanium-silicon layer 101 is also dark contrast material, so what see is the ghost image of germanium-silicon layer 101 and platinum protective seam, is difficult to judge the accurate pattern of germanium-silicon layer 101; If but because polysilicon gate both sides have monox residual, monox is shallow contrast material, so the contrast of platinum protective seam and monox is very large, can judges and whether have monox residual.Again for example, deposit the carbon protective layer of shallow contrast, while analyzing so TEM sample, because outstanding germanium-silicon layer 101 is dark contrast materials, so both contrasts are very large, can judge the accurate pattern of germanium-silicon layer 101; If but because polysilicon gate both sides have monox residual, whether monox is also shallow contrast material, just cannot judge and have monox residual.To sum up, can only obtain one of them information according to the protective seam of prior art deposition.
Fig. 2 a is the schematic top plan view of the embodiment of the present invention one at TEM sample surfaces deposition protective seam.Concrete grammar is first deposit carbon protective seam 201, then deposits platinum protective seam 202.Wherein, the carbon protective layer 201 of patterning cover part germanium-silicon layer 101 in the Y direction, and cover respectively the shallow channel isolation area 103 of germanium-silicon layer 101 relative both sides.Platinum protective seam 202 covers the edge of germanium-silicon layer 101 and carbon protective layer 201 in the Y direction, covers the polysilicon gate of the relative both sides of germanium-silicon layer on directions X.In fact, more convenient for implementing in the time of deposition protective seam, be to be all generally to cover sample surfaces, as shown in Figure 2 a blockly.
Fig. 2 b is the Y-direction sectional view corresponding with Fig. 2 a.Fig. 2 c is the directions X sectional view corresponding with Fig. 2 a.By the analysis to this TEM sample in cross section, because the carbon protective layer lining of shallow contrast is after the outstanding germanium-silicon layer 101 of dark contrast material, both contrasts are very large, therefore can judge the accurate pattern of germanium-silicon layer 101; The platinum protective seam of dark contrast material covers the residual silicon oxide surface of shallow contrast, and both contrasts are also very large, therefore also can accurately judge whether monox has residual.
Embodiment bis-
Fig. 3 a is embodiment bis-by the schematic top plan view of the initial TEM sample that wafer cutting is obtained.After FIB cutting attenuate, reservation be the pattern of Fig. 3 a core.Can find out from Fig. 3 a, this embodiment is the amplification of embodiment mono-, that is to say that TEM sample is multiple repeat patterns of arranging in turn, each pattern at least comprises the active area germanium-silicon layer higher than wafer substrate surface, relative both sides at germanium-silicon layer have polysilicon gate, take this orientation as directions X; Another relative both sides have the shallow channel isolation area lower than wafer substrate surface, take this orientation as Y-direction.This embodiment illustrates three repeat patterns.
Fig. 3 b is the schematic top plan view of the embodiment of the present invention two at TEM sample surfaces deposition protective seam.Concrete grammar is: at described initial TEM sample surfaces deposit carbon protective seam, described carbon protective layer covers a predetermined number pattern; At described initial TEM sample surfaces deposition platinum protective seam, described platinum protective seam covers residue pattern.Specific implementation is got up, due to carbon protective layer and platinum protective seam independence separately, so the sedimentary sequence of carbon protective layer and platinum protective seam can be adjusted, can be also: at described initial TEM sample surfaces deposition platinum protective seam, described platinum protective seam covers a predetermined number pattern; At described initial TEM sample surfaces deposit carbon protective seam, described carbon protective layer covers residue pattern.In this embodiment, adopt carbon protective layer 301 to cover (1) and (3) individual pattern, adopt platinum protective seam 302 to cover (2) individual pattern.
Fig. 3 c be corresponding with Fig. 3 b to pattern (2) at Y-direction sectional view.Fig. 3 d be corresponding with Fig. 3 b to pattern (1) or (3) at Y-direction sectional view.By the analysis to this TEM sample in cross section, for pattern (1) or (3) of surface deposition carbon protective layer, because the carbon protective layer 301 of shallow contrast serves as a contrast after the outstanding germanium-silicon layer 101 of dark contrast material, both contrasts are very large, therefore can judge the accurate pattern of germanium-silicon layer 101; For the pattern (2) of surface deposition platinum protective seam, the platinum protective seam 302 of dark contrast material covers the residual silicon oxide surface of shallow contrast, and both contrasts are also very large, therefore also can accurately judge whether monox has residual.
Be simple and easy to realize for making to deposit protective seam, also can be at initial TEM sample surfaces deposit carbon protective seam, described carbon protective layer covers a predetermined number pattern; And then deposition platinum protective seam, the platinum protective seam depositing covers above-mentioned all body structure surfaces.According to the protective seam of this method deposition, analyze respectively by the cross section to different pattern, equally also can reach object of the present invention.
In addition, it should be noted that, the present invention preferably adopts metal platinum for the protective seam of dark contrast, also can adopt tungsten; Protective seam for shallow contrast preferably adopts carbon, also can adopt monox, and because carbon has good electric conductivity, the electric charging effect that the TEM sample of making produces is smaller, can accurately obtain TEM information.
To sum up; the present invention per sample contrast of zones of different material chooses flexibly protective seam and covers; for TEM sample; at least comprise the active area germanium-silicon layer higher than wafer substrate surface; relative both sides at germanium-silicon layer have polysilicon gate; another relative both sides have the shallow channel isolation area lower than wafer substrate surface; by subregion protective mulch; in the time of observation TEM sample; not only can obtain grid both sides and whether have the residual information of monox; and can obtain active area germanium-silicon layer pattern accurately, greatly enrich TEM sample message.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of making, be equal to replacement, improvement etc., within all should being included in the scope of protection of the invention.
Claims (8)
1. a method for making for example of transmission electron microscope, the method comprises:
By wafer cutting being provided to an initial transmission electron microscope TEM sample;
At described initial TEM sample surfaces; according to the difference of the material contrast of TEM sample observation area; subregion deposition protective seam; concrete grammar is: have specimen material surface deposition carbon or the monox protective seam of dark contrast, having specimen material surface deposition platinum or the tungsten protective seam of shallow contrast.
2. the method for claim 1, is characterized in that, the specimen material with dark contrast is germanium-silicon layer; The specimen material with shallow contrast is silicon oxide layer.
3. method as claimed in claim 2, is characterized in that,
Described initial TEM sample at least comprises the active area germanium-silicon layer higher than wafer substrate surface, has polysilicon gate, take this orientation as directions X in the relative both sides of germanium-silicon layer; Another relative both sides have the shallow channel isolation area lower than wafer substrate surface, take this orientation as Y-direction;
The carbon protective layer that forms patterning at described initial TEM sample surfaces, the carbon protective layer of described patterning is cover part germanium-silicon layer in the Y direction, and covers respectively the shallow channel isolation area of the relative both sides of germanium-silicon layer;
At described initial TEM sample surfaces deposition platinum protective seam, described platinum protective seam covers the edge of germanium-silicon layer and carbon protective layer in the Y direction, covers the polysilicon gate of the relative both sides of germanium-silicon layer on directions X.
4. method as claimed in claim 2, is characterized in that,
Described initial TEM sample is multiple repeat patterns of arranging in turn, and each pattern at least comprises the active area germanium-silicon layer higher than wafer substrate surface, has polysilicon gate, take this orientation as directions X in the relative both sides of germanium-silicon layer; Another relative both sides have the shallow channel isolation area lower than wafer substrate surface, take this orientation as Y-direction;
At described initial TEM sample surfaces deposit carbon protective seam, described carbon protective layer covers a predetermined number pattern;
At described initial TEM sample surfaces deposition platinum protective seam, described platinum protective seam covers residue pattern.
5. method as claimed in claim 4, is characterized in that, also coated carbon protective seam of described platinum protective seam.
6. method as claimed in claim 2, is characterized in that,
Described initial TEM sample is multiple repeat patterns of arranging in turn, and each pattern at least comprises the active area germanium-silicon layer higher than wafer substrate surface, has polysilicon gate, take this orientation as directions X in the relative both sides of germanium-silicon layer; Another relative both sides have the shallow channel isolation area lower than wafer substrate surface, take this orientation as Y-direction;
At described initial TEM sample surfaces deposition platinum protective seam, described platinum protective seam covers a predetermined number pattern;
At described initial TEM sample surfaces deposit carbon protective seam, described carbon protective layer covers residue pattern.
7. the method as described in claim 3,4,5 or 6, is characterized in that, it is residual that described polysilicon gate both sides have monox.
8. the method for claim 1, is characterized in that, described wafer is cut to the focused ion beam method of adopting.
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| CN105334086A (en) * | 2014-08-13 | 2016-02-17 | 中芯国际集成电路制造(上海)有限公司 | Preparation method of TEM sample and TEM sample |
| CN105510092A (en) * | 2014-09-22 | 2016-04-20 | 中芯国际集成电路制造(上海)有限公司 | TEM sample preparation method |
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| CN106323713A (en) * | 2016-08-22 | 2017-01-11 | 上海华力微电子有限公司 | Preparation method of germanium-silicon TEM sample |
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| CN105334086A (en) * | 2014-08-13 | 2016-02-17 | 中芯国际集成电路制造(上海)有限公司 | Preparation method of TEM sample and TEM sample |
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| CN105990172A (en) * | 2015-01-30 | 2016-10-05 | 上海华力微电子有限公司 | Design of embedded Si-Ge epitaxial test block |
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| CN106645243A (en) * | 2016-12-23 | 2017-05-10 | 北京有色金属研究总院 | Preparation method of large-particle powder transmission electron microscope sample |
| CN111051845A (en) * | 2017-12-07 | 2020-04-21 | 株式会社Lg化学 | Sample for analyzing shape of antistatic antifouling layer and preparation method thereof |
| CN108398302A (en) * | 2018-02-09 | 2018-08-14 | 上海华虹宏力半导体制造有限公司 | Micro-structure method for making sample |
| CN109374663A (en) * | 2018-12-29 | 2019-02-22 | 中国工程物理研究院材料研究所 | A kind of preparation method of flexibility high atomic number material transmission electron microscope sample |
| CN109374663B (en) * | 2018-12-29 | 2021-05-04 | 中国工程物理研究院材料研究所 | Preparation method of transmission electron microscope sample made of flexible high-atomic number material |
| CN110133020A (en) * | 2019-04-25 | 2019-08-16 | 中国科学院上海微系统与信息技术研究所 | A kind of in-situ preparation method of ultra-thin TEM sample and thus obtained ultra-thin TEM film |
| CN111397989A (en) * | 2020-05-08 | 2020-07-10 | 上海华力集成电路制造有限公司 | Preparation method of inspection sample of semiconductor device |
| CN114441561A (en) * | 2020-10-20 | 2022-05-06 | 陈健群 | Test sample for electron microscope and method for producing the same |
| CN114441561B (en) * | 2020-10-20 | 2023-12-01 | 陈健群 | Test sample for electron microscope and manufacturing method thereof |
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