CN103325649B - Dress coupling fiber transmission electron microscope digital imaging method of a kind of end and device thereof - Google Patents
Dress coupling fiber transmission electron microscope digital imaging method of a kind of end and device thereof Download PDFInfo
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- CN103325649B CN103325649B CN201310234702.1A CN201310234702A CN103325649B CN 103325649 B CN103325649 B CN 103325649B CN 201310234702 A CN201310234702 A CN 201310234702A CN 103325649 B CN103325649 B CN 103325649B
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Abstract
The present invention relates to dress coupling fiber transmission electron microscope digital imaging method of a kind of end and device thereof, the method comprises the following steps: (1) makes A optical fiber electric optical converter and B optical fiber electric optical converter; (2) A optical fiber electric optical converter and A digital image-forming device are linked into an integrated entity, B optical fiber electric optical converter and B digital image-forming device are linked into an integrated entity; (3) the optical fiber electric optical converter linked into an integrated entity and digital image-forming device are arranged in vacuum envelope; (4) vacuum envelope is connected with the flange-interface bottom the projection chamber of transmission electron microscope.The present invention can carry out high-resolution, the shooting of wide dynamic range static state by the imageing sensor of two independent imagings to transmitted electron image or diffraction pattern, high-resolution, the video recording of high frame per second can be carried out again, solve existing transmission electron microscope digital imaging apparatus can not meet original position electron micrology research needs problem because dynamic imaging frame per second is low.
Description
Technical field
The present invention relates to transmission electron microscope and formation method and device thereof, particularly relate to a kind of by the flange-interface installation bottom transmission electron microscope projection chamber, comprise two unjacketed optical fiber coupled mode imaging devices, both can to the transmitted electron image of sample or diffraction pattern carry out high-resolution, wide dynamic range static state shooting, can carry out again high-resolution, high frame per second video recording transmission electron microscope digital imaging method and device.
Background technology
Transmission electron microscope is that to carry out microexamination to the material world the most effectively, be also most important scientific instrument, and people amplify sample with transmission electron microscope, observes, analyzes and record sample message with image mode.As shown in Figure 1, the transmitted electron image of sample or diffraction pattern 11 are incident upon through projection lens 12 and main phosphor screen 15 is transformed into optical imagery observes for people, also can install the shooting of side-plug-in film camera at 35mm camera interface 13 place or with digital camera imaging; Also the available end, inserts film 16 or installs end dress digital camera imaging by the flange-interface 18 of bottom.Obviously, transmitted electron image or diffraction pattern 11 to insert at side illustration image-position sensor 14, main phosphor screen 15, the end on film 16, end dress imageing sensor 19 become the characteristic of image different because transmitted electron image or diffraction pattern 11 different with electron density in the multiplication factor of above-mentioned diverse location.For Philips EM208S transmission electron microscope, the end insert film 16, main phosphor screen 15, side illustration image-position sensor 14, end dress imageing sensor 19 the ratio of image magnification be that 1:0.888:0.313:1.2 ~ 2.0(depends on end dress digital camera and installation site), the ratio of the image electronic density of their correspondences is about 1:1.27:10.2:0.7
~0.25, namely the multiplication factor of electronic image that receives of side illustration image-position sensor 14 is minimum, and the electron density of image is maximum, and the multiplication factor of the electronic image that end dress imageing sensor 19 receives is maximum, and the electron density of image is minimum.
Resolution (multiplication factor) is the most important index of reflection transmission electron microscope performance, the linear resolution of EM208S transmission electron microscope is 0.34nm, refer to and insert film 16 when multiplication factor is 200,000 times the end of with, the sample image of shooting can differentiate the grid of spacing 0.34nm, if and now taken by side-plug-in camera with same film, multiplication factor only has 20 × 0.313=6.26 ten thousand times, does not obviously reach the linear resolution of 0.34nm.Therefore, in order to the problem that the multiplication factor making full use of transmission electron microscope is low with the electron density making up high-amplification-factor hypograph, what current high-end transmission electron microscope digital imaging apparatus adopted is all end dress optical-fiber-coupling type structure.
The dynamic imaging of fast development to micro/nano-scale in the field such as new material, microelectronics proposes more and more higher requirement, in the original position electron micrology researchs such as nanowire growth, original position stretching experiment, original position e-beam induced deposition, even record the needs of sample transient changing under the transmission electron microscope digital imaging apparatus of most significant end can not meet high-resolution at present.Such as current Tvips company most significant end TemCam-F816 transmission electron microscope digital imaging apparatus, although its spatial resolution up to 8192 × 8192, dynamic range is up to 10000:1, perfection is can be rated as in static state shooting, but the most rapid rate of its dynamic imaging only has 6.7fps, corresponding resolution is also only 1024 × 1024, also far apart from the high-resolution and high frame per second needs meeting the research of original position electron micrology.Sensitivity and dynamic range are the most important indexs of static shooting, and in order to reach high-performance, require that the photon of imageing sensor (electronics) is long for integration time, the signal reading speed of electronic circuit is slow; And high frame per second dynamic imaging will be realized, imageing sensor integration time must be reduced as far as possible, improve signal reading speed as early as possible; For same picture transducer, the demand is obviously contradiction.
Summary of the invention
In order to overcome, high-end transmission electron microscope digital imaging apparatus dynamic imaging frame per second based on prior art is low, resolution is not high, can not meet the needs requiring to record at high resolutions sample transient changing in the research of original position electron micrology, the technical problem to be solved in the present invention is to provide a kind of structure uniqueness, is easy to the end dress coupling fiber transmission electron microscope digital imaging method of realization and device thereof.
In order to solve the problems of the technologies described above, technical scheme one of the present invention is: dress coupling fiber transmission electron microscope digital imaging apparatus of a kind of end, comprise transmission electron microscope, bottom the projection chamber of described transmission electron microscope, there is flange-interface, described flange-interface is connected with vacuum envelope, A optical fiber electric optical converter and B optical fiber electric optical converter is provided with in described vacuum envelope, described A optical fiber electric optical converter is connected with A digital image-forming device, and described B optical fiber electric optical converter is connected with B digital image-forming device; Described A digital image-forming device comprises full frame type ccd image sensor, and described B digital image-forming device comprises sCMOS imageing sensor.
Further, described A optical fiber electric optical converter comprises the A light cone be drawn into by optical fibre rod, described B optical fiber electric optical converter comprises the B light cone be drawn into by optical fibre rod, the optical input side of described A light cone and B light cone is respectively equipped with electronic fluorescent bisque, and described electronic fluorescent bisque surface is respectively equipped with the aluminium conductive film layer with the locular wall conducting that projects.
Further, the optical input port of described A light cone is circular large end, and the optics output of described A light cone is the rectangle small end adapted with the imageing sensor photosurface of A digital image-forming device; The optical input port of described B light cone is circular large end, and the optics output of described B light cone is the rectangle small end adapted with the imageing sensor photosurface of B digital image-forming device.
Further, the outside of described A light cone and B light cone be respectively equipped be convenient to its install the conformal support of aluminium matter, described A light cone with the electronic fluorescent bisque of B light cone is separately installed with the aluminum annular-shaped frame be fixedly connected with the conformal support of aluminium matter.
Further, described A digital image-forming device and B digital image-forming device are arranged on a sliding support in vacuum envelope.
Further, described A digital image-forming device is connected with ambient controller by a socket with B digital image-forming device, and described socket is mounted in the vacuum seal socket on vacuum envelope.
In order to solve the problems of the technologies described above, technical scheme two of the present invention is: dress coupling fiber transmission electron microscope digital imaging method of a kind of end, comprises the following steps: (1) makes A optical fiber electric optical converter and B optical fiber electric optical converter; (2) A optical fiber electric optical converter and A digital image-forming device are linked into an integrated entity, B optical fiber electric optical converter and B digital image-forming device are linked into an integrated entity, described A digital image-forming device comprises full frame type ccd image sensor, and described B digital image-forming device comprises sCMOS imageing sensor; (3) the optical fiber electric optical converter linked into an integrated entity and digital image-forming device are arranged in vacuum envelope; (4) vacuum envelope is connected with the flange-interface bottom the projection chamber of transmission electron microscope.
Further, the manufacture method of the A optical fiber electric optical converter in step (1) and B optical fiber electric optical converter is carried out according to the following steps: two optical fibre rods are drawn into light cone by different cones ratio by (1.1), and small end face is cut into rectangle, A light cone and B light cone; (1.2) on the large end face of A light cone and B light cone, one deck electronic fluorescent bisque is made respectively; (1.3) respectively process the conformal support of an aluminium matter to facilitate the installation of A light cone and B light cone according to the profile of A light cone and B light cone, on A light cone with the electronic fluorescent bisque of B light cone, respectively lay an aluminum annular-shaped frame and be fixedly connected with the conformal support of aluminium matter; (1.4) one deck aluminium conductive film layer is respectively plated with direct current evaporation coating method on the electronic fluorescent bisque surface of A light cone and B light cone.
Further, the optical fiber electric optical converter in step (2) and the method for attachment of digital image-forming device are carried out according to the following steps: (2.1) select digital camera, mechanically throw off the cover glass on digital camera image sensors surface; (2.2) imageing sensor is put into the culture dish filling deionized water, with ultrasonic cleaning machine cleaning twice; (2.3) with optical cement, the optical output side of optical fiber electric optical converter and imageing sensor photosurface are bondd.
Further, step (3) the digital image-forming device linked into an integrated entity and optical fiber electric optical converter is arranged on a sliding support in vacuum envelope.
Further, the digital image-forming device in step (4) is connected with ambient controller by socket, and described socket is mounted in the vacuum seal socket on vacuum envelope.
Compared with prior art, the present invention has following beneficial effect: the end of the present invention dress optical-fiber-coupling type transmission electron microscope digital imaging apparatus comprises the imageing sensor of two independent imagings, can solve prior art and can not meet the high-resolution of original position electron micrology research requirement, the problem of high frame per second dynamic imaging needs.Large format, full frame CCD imageing sensor that the present invention adopts are particularly suitable for high sensitivity, the shooting of high dynamic range static state, the Scientific Grade CMOS(sCMOS of employing) imageing sensor is particularly suitable for high-resolution, high frame per second dynamic imaging; All adopt optical fiber (cone) coupling technique with very high coupling efficiency between imageing sensor of the present invention and electronic screen, be particularly conducive to the imaging of low electron density image.Therefore, the present invention is applicable to the transmission electron microscope imaging comprising all spectras such as material, microelectronics, life science and medical science.
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Accompanying drawing explanation
Fig. 1 is existing transmission electron microscope structure and imaging schematic diagram.
Fig. 2 is the end of the present invention dress coupling fiber transmission electron microscope digital imaging apparatus schematic diagram.
Fig. 3 is the structural representation of optical fiber electric optical converter of the present invention.
In figure: 11-transmitted electron image or diffraction pattern, 12-projection lens, 13-35mm camera interface, 14-side illustration image-position sensor, the main phosphor screen of 15-, inserts film at the bottom of 16-, and 17-projects locular wall, 18-flange-interface, fills imageing sensor at the bottom of 19-, 21-vacuum envelope, 22-A digital image-forming device, 23-B digital image-forming device, 24-A optical fiber electric optical converter, 25-B optical fiber electric optical converter, 26-socket, 31-A light cone, 32-B light cone, 35-electronic fluorescent bisque, 36-aluminium conductive film layer.
Embodiment
As shown in Fig. 2 ~ 3, dress coupling fiber transmission electron microscope digital imaging apparatus of a kind of end, comprise transmission electron microscope, there is bottom the projection chamber of described transmission electron microscope flange-interface 18, described flange-interface 18 is connected with vacuum envelope 21, A optical fiber electric optical converter 24 and B optical fiber electric optical converter 25 is provided with in described vacuum envelope 21, described A optical fiber electric optical converter 24 is connected with A digital image-forming device 22, described B optical fiber electric optical converter 25 is connected with B digital image-forming device 23, namely described A digital image-forming device 22 and B digital image-forming device 23 are coupled with A optical fiber electric optical converter 24 and B optical fiber electric optical converter 25 respectively, described A digital image-forming device 22 comprises full frame type ccd image sensor, and described B digital image-forming device 23 comprises sCMOS imageing sensor.
In the present embodiment, described A optical fiber electric optical converter 24 comprises the A light cone 31 be drawn into by optical fibre rod, described B optical fiber electric optical converter 25 comprises the B light cone 32 be drawn into by optical fibre rod, the outside of described A light cone 31 and B light cone 32 is respectively equipped with the conformal support of aluminium matter (not shown in FIG.) be convenient to it and installed, the optical input side of described A light cone 31 and B light cone 32 is respectively equipped with electronic fluorescent bisque 35, described electronic fluorescent bisque 35 is provided with the aluminum annular-shaped frame (not shown in FIG.) be fixedly connected with the conformal support of aluminium matter, described electronic fluorescent bisque 35 surface is respectively equipped with the aluminium conductive film layer 36 with locular wall 17 conducting that projects.The optical input port of described A light cone 31 is circular large end, and the optics output of described A light cone 31 is the rectangle small end adapted with the imageing sensor photosurface of A digital image-forming device 22; The optical input port of described B light cone 32 is circular large end, and the optics output of described B light cone 32 is the rectangle small end adapted with the imageing sensor photosurface of B digital image-forming device 23.
In the present embodiment, on the sliding support that described A digital image-forming device 22 and B digital image-forming device 23 are arranged on a metal in vacuum envelope 21 (not shown in FIG.), this sliding support is formed by magnetism-free stainless steel materials processing, is realized the switching of this device static state shooting and dynamic recording function by sliding support and drive motors thereof; A digital image-forming device 22 is connected with ambient controller (not shown in FIG.) by a socket 26 with B digital image-forming device 23, realize the feed of two digital image devices etc. and control and other function, this socket 26 is vacuum seal socket MX15-8 preferably, and it is installed on vacuum envelope 21.
As shown in Fig. 2 ~ 3, dress coupling fiber transmission electron microscope digital imaging method of a kind of end, comprises the following steps: (1) makes A optical fiber electric optical converter 24 and B optical fiber electric optical converter 25; (2) A optical fiber electric optical converter 24 and A digital image-forming device 22 are linked into an integrated entity, B optical fiber electric optical converter 25 and B digital image-forming device 23 are linked into an integrated entity, described A digital image-forming device 22 comprises full frame type ccd image sensor, and described B digital image-forming device 23 comprises sCMOS imageing sensor; (3) the optical fiber electric optical converter linked into an integrated entity and digital image-forming device are arranged in vacuum envelope 21; (4) vacuum envelope 21 is connected with the flange-interface 18 bottom the projection chamber of transmission electron microscope.
In the present embodiment, the manufacture method of the optical fiber electric optical converter in step (1) is carried out according to the following steps: an end face of the optical fibre rod of the long 50mm of diameter 70mm that is made up of the image transmission optical fibre of core diameter 6 μm by (1.1) is drawn into diameter 54mm, cut into the square of 36.8 mm × 36.8 mm and by end face polishing, this i.e. A light cone 31; An end face of the optical fibre rod of the long 35mm of diameter 70mm be made up of the image transmission optical fibre of core diameter 6 μm is drawn into diameter 22mm, cuts into the rectangle of 16.4 mm × 14.0 mm and by end face polishing, this i.e. B light cone 32; (1.2) the thick electronic fluorescent bisque 35 of one deck 15 μm is made at the large end face of A light cone 31 and B light cone 32 respectively with settling methods; (1.3) respectively process the conformal support of an aluminium matter to facilitate the installation of A light cone 31 and B light cone 32 according to the profile of A light cone 31 and B light cone 32, on A light cone 31 with the electronic fluorescent bisque 35 of B light cone 32, lay an aluminum annular-shaped frame and be fixedly connected with (not shown in FIG.) with the conformal support of aluminium matter; (1.4) one deck aluminium is respectively plated to form aluminium conductive film layer 36 with direct current evaporation coating method on electronic fluorescent bisque 35 surface of A light cone 31 and B light cone 32.
In the present embodiment, optical fiber electric optical converter in step (2) and the method for attachment of digital image-forming device are carried out according to the following steps: (2.1) preferably the highly sensitive camera STX-16803 of U.S. SBIG large format, as A digital image-forming device 22, mechanically throw off the cover glass on camera CCD surface; (2.2) preferably Britain ANDOR company Zyla sCMOS high speed high-sensitivity camera, as B digital image-forming device 23, mechanically throws off the cover glass of camera sCMOS chip surface; (2.2) CCD and sCMOS chip is put into the culture dish filling deionized water, with ultrasonic cleaning machine cleaning twice, each 15 minutes; (2.3) with optical cement, the square end faces of A light cone 31 and CCD are bondd on superclean bench, the rectangle end face of B light cone 32 and sCMOS are bondd, and during bonding, CCD and sCMOS lays respectively at the top of A light cone 31 and B light cone 32, horizontal positioned.
In the present embodiment, in step (3) be the digital image-forming device linked into an integrated entity and optical fiber electric optical converter are arranged on a metal in vacuum envelope 21 sliding support on (not shown in FIG.), this sliding support is formed by magnetism-free stainless steel materials processing, is realized the switching of this device static state shooting and dynamic recording function by sliding support and drive motors thereof; A digital image-forming device 22 is connected with ambient controller (not shown in FIG.) by a socket 26 with B digital image-forming device 23, realize the feed of two digital image devices etc. and control and other function, this socket 26 is vacuum seal socket MX15-8 preferably, and it is installed on vacuum envelope 21.
The foregoing is only preferred embodiment of the present invention, the contents such as the title of equipment cited by the present invention or device or model are to more specifically, intuitively, clearly the present invention and advantage thereof are described, instead of the restriction to the claims in the present invention scope, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (9)
1. fill coupling fiber transmission electron microscope digital imaging apparatus at the bottom of one kind, comprise transmission electron microscope, bottom the projection chamber of described transmission electron microscope, there is flange-interface, it is characterized in that: described flange-interface is connected with vacuum envelope, A optical fiber electric optical converter and B optical fiber electric optical converter is provided with in described vacuum envelope, described A optical fiber electric optical converter is connected with A digital image-forming device, and described B optical fiber electric optical converter is connected with B digital image-forming device; Described A digital image-forming device comprises full frame type ccd image sensor, and described B digital image-forming device comprises sCMOS imageing sensor; Described A digital image-forming device and B digital image-forming device are arranged on a sliding support in vacuum envelope, are realized the switching of this imaging device static state shooting and dynamic recording function by sliding support and drive motors thereof.
2. the end according to claim 1 dress coupling fiber transmission electron microscope digital imaging apparatus, it is characterized in that: described A optical fiber electric optical converter comprises the A light cone be drawn into by optical fibre rod, described B optical fiber electric optical converter comprises the B light cone be drawn into by optical fibre rod, the optical input side of described A light cone and B light cone is respectively equipped with electronic fluorescent bisque, and described electronic fluorescent bisque surface is respectively equipped with the aluminium conductive film layer with the locular wall conducting that projects.
3. the end according to claim 2 dress coupling fiber transmission electron microscope digital imaging apparatus, it is characterized in that: the optical input port of described A light cone is circular large end, and the optics output of described A light cone is the rectangle small end adapted with the imageing sensor photosurface of A digital image-forming device; The optical input port of described B light cone is circular large end, and the optics output of described B light cone is the rectangle small end adapted with the imageing sensor photosurface of B digital image-forming device.
4. the end dress coupling fiber transmission electron microscope digital imaging apparatus according to Claims 2 or 3, it is characterized in that: the outside of described A light cone and B light cone be respectively equipped be convenient to its install the conformal support of aluminium matter, described A light cone with the electronic fluorescent bisque of B light cone is separately installed with the aluminum annular-shaped frame be fixedly connected with the conformal support of aluminium matter.
5. the end according to claim 1 dress coupling fiber transmission electron microscope digital imaging apparatus, it is characterized in that: described A digital image-forming device is connected with ambient controller by a socket with B digital image-forming device, and described socket is mounted in the vacuum seal socket on vacuum envelope.
6. fill a coupling fiber transmission electron microscope digital imaging method at the bottom of, it is characterized in that, comprise the following steps: (1) makes A optical fiber electric optical converter and B optical fiber electric optical converter; (2) A optical fiber electric optical converter and A digital image-forming device are linked into an integrated entity, B optical fiber electric optical converter and B digital image-forming device are linked into an integrated entity, described A digital image-forming device comprises full frame type ccd image sensor, and described B digital image-forming device comprises sCMOS imageing sensor; (3) the A optical fiber electric optical converter linked into an integrated entity and A digital image-forming device, the B optical fiber electric optical converter linked into an integrated entity and B digital image-forming device are arranged on a sliding support in vacuum envelope, are realized the switching of the shooting of transmission electron microscope static state and dynamic recording function by sliding support and drive motors thereof; (4) vacuum envelope is connected with the flange-interface bottom the projection chamber of transmission electron microscope.
7. the end according to claim 6 dress coupling fiber transmission electron microscope digital imaging method, it is characterized in that: the manufacture method of the A optical fiber electric optical converter in step (1) and B optical fiber electric optical converter is carried out according to the following steps: two optical fibre rods are drawn into light cone by different cones ratio by (1.1), and small end face is cut into rectangle, A light cone and B light cone; (1.2) on the large end face of A light cone and B light cone, one deck electronic fluorescent bisque is made respectively; (1.3) respectively process the conformal support of an aluminium matter to facilitate the installation of A light cone and B light cone according to the profile of A light cone and B light cone, on A light cone with the electronic fluorescent bisque of B light cone, respectively lay an aluminum annular-shaped frame and be fixedly connected with the conformal support of aluminium matter; (1.4) one deck aluminium conductive film layer is respectively plated with direct current evaporation coating method on the electronic fluorescent bisque surface of A light cone and B light cone.
8. the end according to claim 6 dress coupling fiber transmission electron microscope digital imaging method, it is characterized in that: the method for attachment of the method for attachment of the A optical fiber electric optical converter in step (2) and A digital image-forming device, B optical fiber electric optical converter and B digital image-forming device is carried out all according to the following steps: (2.1) select digital camera, mechanically throw off the cover glass on digital camera image sensors surface; (2.2) imageing sensor is put into the culture dish filling deionized water, with ultrasonic cleaning machine cleaning twice; (2.3) with optical cement, the optical output side of optical fiber electric optical converter and imageing sensor photosurface are bondd.
9. the end according to claim 6 dress coupling fiber transmission electron microscope digital imaging method, it is characterized in that: step (4) is also comprised digital image-forming device and is connected with ambient controller by socket, described socket is mounted in the vacuum seal socket on vacuum envelope.
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| CN201310234702.1A CN103325649B (en) | 2013-06-14 | 2013-06-14 | Dress coupling fiber transmission electron microscope digital imaging method of a kind of end and device thereof |
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|---|---|---|---|---|
| EP2383769A1 (en) * | 2010-04-28 | 2011-11-02 | Fei Company | Method of using a direct electron detector for a TEM |
| CN102315067A (en) * | 2010-07-02 | 2012-01-11 | 株式会社其恩斯 | Magnifying Observation Apparatus |
| CN102446683A (en) * | 2011-09-22 | 2012-05-09 | 中国人民解放军南京军区福州总医院 | Bottom-mounted lens coupled transmission electron microscope digital imaging device |
| CN203339106U (en) * | 2013-06-14 | 2013-12-11 | 中国人民解放军南京军区福州总医院 | A bottom-mounted optical fiber coupling transmission electron microscope digital imaging device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7745786B2 (en) * | 2008-03-19 | 2010-06-29 | Fama Leo A | Method and apparatus allowing simultaneous direct observation and electronic capture of scintillation images in an electron microscope |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2383769A1 (en) * | 2010-04-28 | 2011-11-02 | Fei Company | Method of using a direct electron detector for a TEM |
| CN102315067A (en) * | 2010-07-02 | 2012-01-11 | 株式会社其恩斯 | Magnifying Observation Apparatus |
| CN102446683A (en) * | 2011-09-22 | 2012-05-09 | 中国人民解放军南京军区福州总医院 | Bottom-mounted lens coupled transmission electron microscope digital imaging device |
| CN203339106U (en) * | 2013-06-14 | 2013-12-11 | 中国人民解放军南京军区福州总医院 | A bottom-mounted optical fiber coupling transmission electron microscope digital imaging device |
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