CN109884097B - Tilting transmission mode electron back scattering diffraction experimental device - Google Patents
Tilting transmission mode electron back scattering diffraction experimental device Download PDFInfo
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- CN109884097B CN109884097B CN201910143821.3A CN201910143821A CN109884097B CN 109884097 B CN109884097 B CN 109884097B CN 201910143821 A CN201910143821 A CN 201910143821A CN 109884097 B CN109884097 B CN 109884097B
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- 230000005540 biological transmission Effects 0.000 title claims abstract description 13
- 239000000523 sample Substances 0.000 claims abstract description 93
- 230000001360 synchronised effect Effects 0.000 claims abstract description 23
- 238000002474 experimental method Methods 0.000 claims abstract description 12
- 238000001514 detection method Methods 0.000 claims abstract description 6
- 238000010894 electron beam technology Methods 0.000 claims description 7
- 210000001503 joint Anatomy 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001887 electron backscatter diffraction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000001133 acceleration Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000007516 Chrysanthemum Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000003032 molecular docking Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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Abstract
The invention discloses a tilting transmission mode electronic back scattering diffraction experimental device, which comprises a machine base fixed on an observation table surface of a scanning electron microscope, wherein a slot is formed in the machine base, a fixed plate is arranged on the machine base at the rear side of the slot, a servo motor is fixed on the fixed plate, and a driving synchronous pulley is fixed on a rotor of the servo motor; the two sides of the slot are provided with supporting arms; the bracket arm is provided with a shaft hole, and the bracket arm is provided with a movable arm through a rotating shaft; the movable arm is provided with a U-shaped groove, and a driven synchronous belt pulley is fixed in the U-shaped groove of the movable arm on the rotating shaft; one side of the rotating shaft is connected with a rotation angle detection sensor through a coupler; the front end face of the movable arm is fixedly provided with a wedge-shaped probe, the upper surface of the probe is fixedly provided with a sample table, and the two sides of the sample table are fixedly provided with structures such as sample clamps; the device reduces the collision accident rate of the probe and the sample table, saves the experiment time cost, and enables the scanning electron microscope equipment to be more easily upgraded to the technical level of the transmission electron microscope.
Description
Technical Field
The invention relates to the field of scanning electron microscope observation experimental devices, in particular to a novel Scanning Electron Microscope (SEM) experimental device, and specifically relates to a tilting transmission mode electron back scattering diffraction experimental device.
Background
The t-EBSD analysis technology in the scanning electron microscope is mainly applied to researches such as crystal structure orientation analysis in large-deformation metal, two-dimensional crystal structure analysis of oxide films and metal oxide layers, intermetallic superfine grain texture analysis, nano-particle crystal structure, nano-phase growth mechanism in a matrix and the like.
In the experiment, the included angle between the sample and the probe needs to be adjusted in real time according to different sample thicknesses, different required acceleration voltages and different target area atomic masses. There are two main types of existing regulation, but there are limitations in experimental operation. In the first mode, the scanning electron microscope sample table can tilt towards the direction of the probe, and adjustment can be achieved through tilting the sample table. The angle of the device can be adjusted at will, which is convenient, but the distance between the sample and the detector is adjusted at any time, because the distance between the sample and the probe extending into the scanning electron microscope is about 10mm, and the sample of the transmission electron microscope is thin and small, the collision accident between the probe and the sample table is easy to occur in the experimental process, and huge loss is caused.
In another mode, if the tilting direction of the sample stage of the scanning electron microscope cannot change the included angle between the probe and the sample, a series of sample stages with certain included angles prepared in advance can be additionally arranged, and then the sample stages with different included angles are tried to be changed according to different samples. However, a large number of attempts are required to prepare the laboratory bench in advance, the experimental amount is large, the time cost is high, and the implementation is difficult. Even if a sample of one material is observed, the thickness of the transmission electron microscope sample prepared each time is necessarily different and the phase difference is possibly larger, and in actual experiments, multiple samples of multiple materials are often required to be observed, and a sample table with a fixed angle is used, so that the test result and the effect are necessarily influenced. Therefore, a new device is urgently needed to solve the above-mentioned problems.
Disclosure of Invention
The invention aims to provide a method for developing a novel t-EBSD technology, which reduces the collision accident rate of a probe and a sample table, saves the experiment time cost, enables the t-EBSD technology to be commercialized as soon as possible, enables scanning electron microscope equipment to be more easily upgraded to the technical level of a transmission electron microscope, and releases the experiment pressure of the transmission electron microscope, so that the problems of sub-nanometer and picometer-level science are better and more focused.
The tilting transmission mode electron back scattering diffraction experimental device is characterized by comprising a base fixed on an observation table surface of a scanning electron microscope, wherein a slot is formed in the base, a fixed plate is arranged on a back side base of the slot, a servo motor is fixed on the fixed plate, and a driving synchronous pulley is fixed on a rotor of the servo motor; the two sides of the slot are provided with supporting arms; the bracket arm is provided with a shaft hole, and the bracket arm is provided with a movable arm through a rotating shaft; the movable arm is provided with a U-shaped groove, and a driven synchronous belt pulley is fixed in the U-shaped groove of the movable arm on the rotating shaft; one side of the rotating shaft is connected with a rotation angle detection sensor through a coupler; the front end face of the movable arm is fixedly provided with a wedge-shaped probe, the upper surface of the probe is fixedly provided with a sample table, and sample clamps are fixedly arranged on two sides of the sample table; the driving synchronous pulley is connected with the driven synchronous pulley through a synchronous belt.
Preferably, the rotating shaft is a stepped rotating shaft.
Preferably, the probe is detachably and fixedly connected with the movable arm through a pin shaft, the butt joint surface of the probe and the movable arm is a convex surface, a pin hole is formed in the convex surface, the movable arm and the probe are connected in a butt joint mode to be a concave surface, the probe is provided with the pin hole, the positions of the pin holes of the movable arm and the probe are consistent, and the probe is inserted into the concave surface of the movable arm and is fixed through the pin shaft.
Preferably, the electron beam of any SEM is at an angle of-30 DEG to 150 DEG or-15 DEG to 165 DEG or-5 DEG to 175 DEG or 0 DEG to 180 DEG with respect to the probe plane by taking the vertical plane of the electron beam of the SEM as a 0 DEG plane.
Preferably, the rotating shaft is fixed with the trailing arm through a bearing, and the bearing is a ball bearing.
Preferably, the movable arm is mounted with the rotating shaft in a key slot fit.
Preferably, the driving synchronous pulley is mounted in a key slot matched mode with the servo motor.
Preferably, a rubber pad is arranged between the servo motor and the fixed plate.
The invention has the beneficial effects that the problem that the collision accident between the current scanning electron microscope sample table and the probe is easy to occur to the EBSD probe and the sample table can be completely avoided, and the test result and effect can be influenced in another mode; meanwhile, the method is applicable to any SEM, so that the TEM sample can obtain the morphology image and the chrysanthemum pool line information under the transmission electron beam.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a schematic diagram of an explosive structure according to the present invention.
FIG. 3 is a schematic view of the docking of a probe with a moveable arm according to the present invention.
Fig. 4 is a schematic view of the structure of the movable arm according to the present invention.
In the figure, a machine base 1, a slot 1-1, a fixed plate 2, a servo motor 3, a driving synchronous pulley 4, a bracket arm 5, a shaft hole 5-1, a movable arm 6, a U-shaped slot 6-1, a driven synchronous pulley 7, a rotation angle detection sensor 8, a probe 9, a sample stage 10, a sample clamp 11, a synchronous belt 12 and a rotating shaft 13.
Detailed Description
As shown in the figure, the invention designs a tilting transmission mode electron back scattering diffraction experimental device, which mainly comprises a base 1 fixed on an observation table of a scanning electron microscope, wherein a slot 1-1 is formed in the base 1, a fixed plate 2 is welded on the base 1 at the rear side of the slot 1-1, a servo motor 3 is fixed on the fixed plate 2 through four bolts, the servo motor 3 can be ensured to be stably fixed on the base 1 by the four bolts, and the bolts are gradually loosened in consideration of the possible vibration of the servo motor 3 during working, so that a layer of rubber gasket is arranged between the servo motor 3 and the fixed plate 2, the bolts are not easy to loosen during working, damage to experimental equipment is caused, and a synchronous belt 12 is fixed on a rotor of the servo motor 3; the two sides of the slotting 1-1 are provided with the bracket arms 5; the bracket arm 5 is provided with a shaft hole 5-1, and a ball bearing with the inner diameter of 4mm is arranged in the shaft hole 5-1 in an interference fit manner; the movable arm 6 is fixedly arranged in the shaft hole 5-1 (in the bearing hole) on the bracket arm 5 through the stepped rotating shaft 13, grooves are respectively formed in the rotating shaft 13 and the mounting surface of the movable arm 6 for realizing synchronous rotation of the rotating shaft 13 and the movable arm 6, keys are arranged in the grooves, and the grooves and the movable arm are matched through key grooves, so that parts are convenient to replace, only parts need to be replaced after damage or precision is reduced, the cost of a laboratory is reduced, and the angle of the movable arm 6 can be conveniently calibrated, thereby providing convenience for maintenance and maintenance of the device; according to the invention, a U-shaped groove 6-1 structure is processed on a movable arm 6, a driven synchronous pulley 7 is fixed on a rotating shaft 13 and positioned in the U-shaped groove 6-1 of the movable arm 6 in an interference fit manner, one side of the rotating shaft 13 is connected with a rotation angle detection sensor 8 through a coupler, and the rotation angle detection sensor 8 can accurately detect the rotation angle of the movable arm 6; the front end face of the movable arm 6 is detachably and fixedly connected with the movable arm 6 through a pin shaft, the butt joint face of the probe 9 and the movable arm 6 is a convex face, pin holes are formed in the convex face, the butt joint face of the movable arm 6 and the probe 9 is a concave face, pin holes are formed in the probe 9, the positions of the pin holes of the two pin holes are consistent, the probe 9 is inserted into the concave face of the movable arm 6 and is fixed with the pin shaft, thus the probe 9 and the movable arm 6 form a whole, the rotating angle of the movable arm 6 is the rotating angle of the probe 9, the included angle between the sample and the probe 9 is adjusted in real time according to different sample thicknesses, different required acceleration voltages and different target area atomic masses of experimental requirements, the probe 9 and the sample table 10 can be adjusted quickly and accurately, collision between the probe 9 and the sample table 10 can be avoided, the equipment can be damaged due to collision between the probe 9 and the sample table 10, and huge loss can be avoided; a sample table 10 is arranged on the upper side surface of the probe 9, and a sample clamp 11 is fixed on the probes 9 on two sides of the sample table 10; the driving synchronous pulley 4 is connected with the driven synchronous pulley 7 through a synchronous belt 12, and the accurate rotation amount of the servo motor 3 is added, so that the rotation angle precision of the probe 9 is very high.
The angle adjustment range of the probe 9 is wide, the vertical plane of the electron beam of the SEM is taken as the 0 DEG plane, the included angle between the electron beam of any SEM and the plane of the probe 9 can be in any included angle range from-30 DEG to 150 DEG or-15 DEG to 165 DEG or-5 DEG to 175 DEG or 0 DEG to 180 DEG, and the maximum guarantee is provided for the test result and effect of the experiment.
When the invention is used, the angle of the sample stage 10 needs to be adjusted in the experimental process, the rotation quantity of the servo motor 3 can be accurately adjusted only by controlling, and the sample stage 10 is directly arranged on the probe 9, so that the collision accident between the sample stage 10 and the probe 9 can not happen at all when the angle of the sample is adjusted, the efficiency is extremely high, and meanwhile, the test result and effect can not be influenced because the angle can be changed.
Claims (7)
1. The tilting transmission mode electron back scattering diffraction experimental device is characterized by comprising a base fixed on an observation table surface of a scanning electron microscope, wherein a slot is formed in the base, a fixed plate is arranged on a back side base of the slot, a servo motor is fixed on the fixed plate, and a driving synchronous pulley is fixed on a rotor of the servo motor; the two sides of the slot are provided with supporting arms; the bracket arm is provided with a shaft hole, and the bracket arm is provided with a movable arm through a rotating shaft; the movable arm is provided with a U-shaped groove, and a driven synchronous belt pulley is fixed in the U-shaped groove of the movable arm on the rotating shaft; one side of the rotating shaft is connected with a rotation angle detection sensor through a coupler; the front end face of the movable arm is fixedly provided with a wedge-shaped probe, the upper surface of the probe is fixedly provided with a sample table, and sample clamps are fixedly arranged on two sides of the sample table; the driving synchronous pulley is connected with the driven synchronous pulley through a synchronous belt; the butt joint surface of the probe and the movable arm is a convex surface, the bulge is provided with a pin hole, the butt joint of the movable arm and the probe is a concave surface, the probe is provided with a pin hole, the positions of the pin holes of the probe and the probe are consistent, and the probe is inserted into the concave surface of the movable arm and is fixed by a pin shaft; the probe and the movable arm form a whole, and the rotating angle of the movable arm is the rotating angle of the probe.
2. The tilting transmissive mode electron back scattering diffraction experiment device according to claim 1, wherein: the rotating shaft is a stepped rotating shaft.
3. The tilting transmissive mode electron back scattering diffraction experiment device according to claim 1, wherein: the vertical plane of the electron beam of the SEM is 0 DEG, so that the included angle between the electron beam of any SEM and the plane of the probe is in any included angle range from-30 DEG to 150 DEG or-15 DEG to 165 DEG or-5 DEG to 175 DEG or 0 DEG to 180 deg.
4. The tilting transmissive mode electron back scattering diffraction experiment device according to claim 1, wherein: the rotating shaft is fixed with the trailing arm through a bearing, and the bearing is a ball bearing.
5. The tilting transmissive mode electron back scattering diffraction experiment device according to claim 1, wherein: the movable arm and the rotating shaft are mounted in a key slot matched mode.
6. The tilting transmissive mode electron back scattering diffraction experiment device according to claim 1, wherein: the driving synchronous pulley and the servo motor are mounted in a key slot matched mode.
7. The tilting transmissive mode electron back scattering diffraction experiment device according to claim 1, wherein: a rubber pad is arranged between the servo motor and the fixed plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910143821.3A CN109884097B (en) | 2019-02-27 | 2019-02-27 | Tilting transmission mode electron back scattering diffraction experimental device |
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| CN201910143821.3A CN109884097B (en) | 2019-02-27 | 2019-02-27 | Tilting transmission mode electron back scattering diffraction experimental device |
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| CN109884097A CN109884097A (en) | 2019-06-14 |
| CN109884097B true CN109884097B (en) | 2024-10-01 |
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| CN106165055A (en) * | 2014-02-11 | 2016-11-23 | 牛津仪器纳米技术工具有限公司 | The method that sample is carried out electron diffraction pattern analysis |
| CN207281180U (en) * | 2017-09-15 | 2018-04-27 | 成都睿腾万通科技有限公司 | Scanning support elevation mount based on Antenna testing system |
| CN209673682U (en) * | 2019-02-27 | 2019-11-22 | 内蒙古科技大学 | One kind can vert transmission mode electron backscatter diffraction experimental provision |
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| US7491934B2 (en) * | 2006-01-13 | 2009-02-17 | Ut-Battelle, Llc | SEM technique for imaging and measuring electronic transport in nanocomposites based on electric field induced contrast |
| JP5476087B2 (en) * | 2008-12-03 | 2014-04-23 | 日本電子株式会社 | Charged particle beam object positioning device |
| WO2011145292A1 (en) * | 2010-05-20 | 2011-11-24 | 株式会社 日立ハイテクノロジーズ | Scanning electron microscope |
| CN203345245U (en) * | 2013-06-20 | 2013-12-18 | 四川长虹电器股份有限公司 | Rotating positioning mechanism |
| EP2824448B1 (en) * | 2013-07-08 | 2016-12-14 | Bruker Nano GmbH | Sample holder for transmission Kikuchi diffraction in SEM |
| CN106935464B (en) * | 2017-02-17 | 2019-05-03 | 西北工业大学 | Tools and Diffraction Image Imaging Methods for Transmission-Electron Backscatter Diffraction |
| CN107053248A (en) * | 2017-04-27 | 2017-08-18 | 浙江长兴平适尔机器人科技有限公司 | Double bracket six-joint robots |
| CN206892007U (en) * | 2017-05-11 | 2018-01-16 | 广东省肇庆市质量计量监督检测所 | A kind of scanning electron microscope electron back scattering diffraction test sample platform |
| CN207705979U (en) * | 2017-10-16 | 2018-08-07 | 抚顺市盛业石化煅造厂 | A kind of transmission device of multi-direction adjustment gear angle |
| CN208262148U (en) * | 2018-05-22 | 2018-12-21 | 天津嘉胤机械科技有限公司 | A kind of novel pipe fitting welding manipulator with auto-steering function |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106165055A (en) * | 2014-02-11 | 2016-11-23 | 牛津仪器纳米技术工具有限公司 | The method that sample is carried out electron diffraction pattern analysis |
| CN207281180U (en) * | 2017-09-15 | 2018-04-27 | 成都睿腾万通科技有限公司 | Scanning support elevation mount based on Antenna testing system |
| CN209673682U (en) * | 2019-02-27 | 2019-11-22 | 内蒙古科技大学 | One kind can vert transmission mode electron backscatter diffraction experimental provision |
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