CN113984813A - High-throughput thin film crystal structure characterization device and method - Google Patents
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Abstract
The invention provides a high-flux thin film crystal structure characterization device and a method, comprising an electron gun emission mechanism, a surface detector, a low-temperature control system, a sample table control device, a sample table and a vacuum system; the electron beam which is easy to focus is used as a detection source, and the diameter of the beam spot of the electron beam can be reduced to micrometer magnitude by the convergence action of the focusing element, so that the spatial resolution of the surface of the sample is improved; the incident angle of the electron beam can be changed through the deflection effect on the electron beam, so that the spatial resolution of the surface of the sample can be changed according to the actual experiment requirement; the sample stage moving mechanism can realize high-precision controllable movement of the sample stage along the plane, and the crystal structure characterization of all samples in the high-flux film is completed by scanning each sample one by one, so that the sample stage moving mechanism can be used for the crystal structure characterization of the high-flux film.
Description
Technical Field
The invention relates to the technical field of high-throughput characterization, in particular to a high-throughput thin film crystal structure characterization device and method.
Background
The genetic engineering of materials has been proved to greatly accelerate the development process of new materials through the organic fusion of high-throughput calculation, high-throughput experiments and large data of the materials. The united states promoted the "material genome project" to the national strategy in 2014, after which similar projects were launched successively in the european union, japan and india. The research of Chinese material genetic engineering has made an important progress since the initiation of 'material genetic engineering key special item' by the national department of science and technology in 2015, and especially in the aspect of high-throughput film preparation technology, a batch of key technologies and equipment for obtaining high-throughput films with components distributed in a continuous gradient manner and in a discrete manner are developed. The development of high-throughput thin film fabrication techniques has placed a demand on higher spatial resolution for high-throughput characterization techniques. However, due to the limitations of the light source intensity and the spot size in common laboratories, the high-throughput characterization of materials in terms of crystal structure still depends greatly on the synchrotron radiation light source large scientific device with the advantages of high intensity, high spatial resolution, and the like. However, synchrotron radiation light sources belong to national large scientific equipment and cannot be conveniently used anytime and anywhere as common laboratory equipment. Therefore, there is a need to develop a high-throughput thin film crystal structure characterization technique that can be popularized and popularized.
The existing high-throughput crystal structure characterization technology suitable for common laboratories is a micro-area X-ray diffraction technology. In the micro-area X-ray diffraction technology, the diameter of a focused X-ray spot is within 100 mu m, and compared with the common X-ray diffraction technology, the micro-area X-ray diffraction technology has higher light source intensity and spatial resolution, and can meet the characterization requirement of a high-flux crystal structure to a certain extent. However, even if the spot diameter of the X-ray in the micro-area X-ray diffraction technique is still over 50 μm, the requirements of high-throughput thin films with higher sample unit density and smaller sample size on the light source intensity and spatial resolution cannot be met; and different crystal face families generate diffraction in different directions, and a detector needs to be rotated to collect comprehensive crystal structure information, so that the measurement efficiency is low. In addition, the existing micro-area X-ray diffraction technology only provides a crystal structure testing function at room temperature and does not have a temperature-variable testing condition.
Besides X-rays, electron beams can also be used for crystal structure characterization, and electron beams have the advantages of high intensity and easy focusing compared with X-rays. In addition, because the wavelength of the electron beam is shorter than that of the X-ray, the Herval reflecting sphere has large radius and can collect two-dimensional diffraction spots in a narrower angle range, so that rich crystal structure information can be obtained through a fixed surface detector, the angle scanning of X-ray diffraction is avoided, the measurement efficiency is improved, and the method is suitable for rapid micro-area structure characterization of a high-flux film sample. Therefore, it is of great significance to develop a high-throughput thin film crystal structure characterization technique which utilizes electron beams as a detection source, is suitable for use in common laboratories and can realize large-range temperature-changing tests.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a high-throughput thin film crystal structure characterization device and a method, and the technical scheme of the invention is implemented as follows:
a high-flux thin film crystal structure characterization device comprises an electron gun emission mechanism, a surface detector, a low-temperature control system, a sample table control device, a sample table and a vacuum system; wherein the content of the first and second substances,
the electron gun emission mechanism comprises an electron gun, a focusing element and an electron beam deflection device;
the low-temperature control system comprises a closed-cycle refrigerator and a heat exchange mechanism;
the sample table control device comprises a sample table moving mechanism, a sample table rotating mechanism and a hollow Z-axis driver;
the vacuum system comprises a vacuum pump, a vacuum gauge, a vacuum cavity and a vacuum interface;
the closed-cycle refrigerator is connected with the heat exchange mechanism and is positioned above the sample table; the vacuum interface is positioned above the hollow Z-axis driver and closes the vacuum cavity, the sample stage moving mechanism and the sample stage rotating mechanism are arranged on the vacuum interface and connected with the hollow Z-axis driver, and the electron gun and the surface detector are respectively positioned at two sides of the vacuum cavity; the electron beam deflection device is positioned in the vacuum chamber, and the focusing element is arranged between the electron gun and the electron beam deflection device; the vacuum pump is arranged on the side wall of the vacuum cavity, and the vacuum gauge is arranged on the side wall of the vacuum cavity;
the sample stage moving mechanism controls the sample stage to move along the directions of an x axis, a y axis and a z axis; the sample table rotating mechanism controls the rotation of the sample table along the z axis; the hollow Z-axis driver is used for controlling the whole movement of the low-temperature control system and the sample table along the Z-axis;
and a temperature feedback control system is integrated on the sample table.
Preferably, the focusing element is an electromagnetic lens.
Preferably, the electron beam deflection device is an electric field deflection device or a magnetic field deflection device.
Preferably, the closed cycle refrigerator comprises a refrigeration head, a compressor and a gas delivery conduit. The refrigerating head extends into the heat exchange mechanism, and the compressor is connected with the refrigerating head through a gas transmission pipeline.
Preferably, the heat exchange mechanism comprises a thermal radiation shield; the thermal radiation shield is located in the vacuum chamber and isolates the vacuum chamber from the cryogenic control system.
Preferably, the closed cycle refrigerator is a pulse tube refrigerator or a gifford-mcmahon refrigerator.
A high-throughput thin film crystal structure characterization method uses a high-throughput thin film crystal structure characterization device.
The method comprises the following steps:
s1, adhering the high-flux film to the center of the surface of the sample stage through an adhesive;
s2, providing a temperature environment required by the test through a low-temperature control system and a temperature feedback control system;
s3, emitting electron beams by the electron gun;
s4, focusing the electron beam by the focusing element;
s5, setting the deflection angle of the electron beam according to the requirement of the practical experiment on the spatial resolution, and deflecting the focused electron beam by using an electron beam deflection device;
s6, adjusting the sample stage to a proper position through the sample stage control device, so that the incident electron beam is aligned with the selected sample position of the high-flux film;
s7, the surface detector is used for receiving the diffracted electron beams diffracted by the high-flux film, and the surface detector can collect and obtain all crystal structure information of the sample through the rotation of the sample stage;
s8, scanning all samples in the high-throughput film by sequentially moving selected sample positions.
The invention uses electron beam instead of X-ray as the detecting light source of high flux film crystal structure, because the electron beam has the characters of high intensity, easy focusing, short wave length, etc. compared with X-ray, compared with the existing micro-area X-ray diffraction system, the invention has the advantages of higher light source intensity, higher space resolution and high testing efficiency.
The invention can reduce the diameter of the beam spot of the electron beam to micron order by the convergence of the focusing element on the electron beam, thereby improving the spatial resolution of the surface of the sample; meanwhile, the incident angle of the electron beam can be increased through the electron beam deflection device, so that the spatial resolution of the electron beam on the surface of the sample is further improved. For example, when the diameter of the beam spot of the electron beam is 5 μm and the incident angle is 20 degrees, the spatial resolution reaches 14.6 μm, which is far smaller than the unit sample size of the current high-flux film, and the crystal structure characterization requirement of the high-flux film is met.
The low-temperature control system and the temperature feedback control system in the sample stage provide a large-range temperature changing condition for the high-flux thin film crystal structure test.
The invention is suitable for common laboratories and has the advantages of popularization and promotion compared with large scientific devices such as synchrotron radiation light sources and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only one embodiment of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
In which like parts are designated by like reference numerals. It should be noted that the terms "front," "back," "left," "right," "upper" and "lower" used in the following description refer to directions in the drawings, and the terms "bottom" and "top," "inner" and "outer" refer to directions toward and away from, respectively, the geometric center of a particular component.
FIG. 1 is a view showing the structure of the apparatus of the present invention.
In the above drawings, the reference numerals denote:
1-sample stage moving mechanism, 2-sample stage rotating mechanism, 3-sample stage, 4-high-flux film, 5-electron gun, 6-focusing element, 7-electron beam deflection device, 8-plane detector, 9-vacuum pump, 10-vacuum gauge, 11-vacuum chamber, 12-incident electron beam, 13-diffraction electron beam, 14-vacuum interface, 15-hollow Z-axis driver, 16-closed-cycle refrigerator and 17-heat exchange mechanism
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
In a specific embodiment, as shown in fig. 1, the high-throughput thin film crystal structure characterization device provided by the present invention includes an electron gun emission mechanism, a surface detector 8, a low temperature control system, a sample stage control device, a sample stage 3, and a vacuum system; wherein, the electron gun emission mechanism comprises an electron gun 5, a focusing element 6 and an electron beam deflection device 7; the low-temperature control system comprises a closed-cycle refrigerator 16 and a heat exchange mechanism 17; the sample table control device comprises a sample table moving mechanism 1, a sample table rotating mechanism 2 and a hollow Z-axis driver; the vacuum system comprises a vacuum pump 9, a vacuum gauge 10, a vacuum cavity 11 and a vacuum interface 14. The electron gun emission mechanism and the surface detector 8 are respectively positioned at two sides of the vacuum cavity 11, the electron gun emission mechanism is used for emitting an electron beam 12 to the surface of the high-flux film 4, and the surface detector 8 is used for receiving a diffracted electron beam 13 diffracted by the high-flux film 4. The sample stage 3 is arranged below the heat exchange mechanism 17 of the cryogenic control system, this whole being movable by a hollow Z-axis drive 15, so that the incident electron beam 12 deflected by the electron beam deflection device 7 can reach the surface of the high-flux film 4. The vacuum pump 9 is disposed on a sidewall of the vacuum chamber 11, and is configured to evacuate the vacuum chamber 11 to provide a vacuum environment for normal operation of the electron beam, and the vacuum gauge 10 is configured to monitor a vacuum degree of the vacuum chamber 11.
In the electron gun emitting mechanism, an electron gun 5, a focusing element 6, and an electron beam deflection device 7 are connected in order. The electron gun 5 is used to emit an electron beam having a specific energy. The focusing element 6 is an electromagnetic lens for focusing the electron beam emitted from the electron gun 5 to the micrometer scale. The electron beam deflection device 7 may be one of an electric field deflection device or a magnetic field deflection device, and it can change and control the deflection direction of the electron beam, and change the incident angle of the electron beam.
In the cryogenic control system, the closed-cycle refrigerator 16 includes a refrigeration head, a compressor, and a gas delivery conduit. The refrigeration head stretches into heat exchange mechanism 17, and heat exchange mechanism 17 stretches into vacuum chamber 11 through vacuum interface 14 inside and refrigerates the sample, provides low temperature environment for the crystal structure test. The heat exchange mechanism 17 can be filled with a refrigerant gas as a cooling medium, and can be further cooled by arranging a throttle valve, a liquid helium tank and the like in the heat exchange mechanism. The low temperature control is not the main creation point of the invention, and can be used for reference to various prior arts in the refrigeration field to achieve low temperature control, and is not developed here.
In the sample stage control apparatus, the sample stage moving mechanism 1 can provide controllable movement of the sample stage 3 in the x-axis and y-axis directions such that the incident electron beam 12 is aligned with a selected sample location in the plane of the high-throughput film 4 and all samples in the high-throughput film 4 are scanned by sequentially moving the selected sample location. The sample stage moving mechanism 1 can control the movement of the sample stage 3 along the z-axis direction at the same time, so that the relative distance between the sample stage 3 and the heat exchange mechanism 17 is changed. The sample stage rotating mechanism 2 is used for controlling the rotation of the sample stage 3 along the z-axis. When the sample table 3 is at a certain angle, the surface detector 8 can receive a plurality of diffracted electron beams 13 with partial crystal structure information, the rotation of the sample table 3 is controlled through the sample table rotating mechanism 2, and all crystal structure information of the sample can be collected and obtained.
The sample stage 3 is integrated with a temperature feedback control system (the technology is a common technology in the field, and therefore, the development is not performed, and a specific structure is not shown in the drawing), and the high-flux film 4 is adhered to the surface center position of the sample stage 3 through an adhesive which has good heat conduction and high and low temperature resistance. When the sample table moving mechanism 1 raises the sample table 3, the sample table 3 is completely contacted with the bottom end of the heat exchange mechanism 17 of the low-temperature control system, and the temperature control below the room temperature can be realized by combining the low-temperature control system and the temperature feedback control system in the sample table 3; when the sample table 3 is lowered through the sample table moving mechanism 1, the sample table 3 is far away from the heat exchange mechanism 17, and the temperature control higher than the room temperature can be realized through the temperature feedback control system in the sample table 3.
In the above scheme, the incident angle of the incident electron beam 12 on the surface of the high-flux film 4 can be changed by the deflection action of the electron beam deflection device 7 on the electron beam, and the spatial resolution of the electron beam on the surface of the sample can be changed because the spatial resolution of the surface of the sample is proportional to the inverse of the sine of the incident angle. Under the condition that the diameter of an electron beam spot is 5 mu m, when the incident angle of the electron beam is 3 degrees, the calculated spatial resolution of the surface of the sample is 96 mu m; and under the condition that the diameter of the beam spot of the electron beam is also 5 mu m, the incident angle of the electron beam deflected by the electron beam deflection device 7 to the surface of the high-flux film 4 is increased, so that the spatial resolution of the surface of the sample is greatly improved. For example, with an incident angle of 20 °, the spatial resolution can reach 14.6 μm.
In the above scheme, the moving precision of the sample stage moving mechanism 1 should be as high as possible. In fact, the precision of the existing high-precision stepping motor can reach 1 μm, and the requirement of high-flux thin film crystal structure representation on the moving precision of the sample stage is completely met. In the actual test process, the scanning step length is set as the interval between the adjacent samples in the high-flux film 4, and the scanning ranges of the x axis and the y axis are set as the sizes of the high-flux film 4 along the x axis and the y axis respectively, so that all samples in the high-flux film 4 can be scanned.
In the above scheme, the heat exchange mechanism 17 isolates the low-temperature environment inside the heat exchange mechanism from the vacuum environment through the heat radiation shielding cover. The thermal radiation shield may be made of a material generally suitable for vacuum sealing, such as, but not limited to, austenitic stainless steel. The thermal radiation shield is generally in the form of a long tubular structure which facilitates cooling of the sample through the vacuum chamber 11.
In the above-described arrangements, the types of closed cycle refrigerators 16 include, but are not limited to, pulse tube refrigerators, gifford-mcmahon refrigerators, and modified refrigerators based on these principles. The selection of the model of the refrigerator depends on the specific refrigeration requirement.
In the above solution, the control of the diameter of the beam spot of the electron beam by the focusing element 6, the setting of the deflection angle of the electron beam by the electron beam deflection device 7, and the setting of the displacement value of the sample stage 3 along the z-axis direction depend on the sample size and the spatial resolution requirement in the high-throughput thin film 4 to be measured.
High throughput thin film crystal structure characterization was performed using the apparatus of this example.
The method comprises the following steps:
s1, adhering the high-flux film 4 to the center of the surface of the sample table 3 through an adhesive;
s2, providing a temperature environment required by the test through a low-temperature control system and a temperature feedback control system;
s3, the electron gun 5 emits electron beams;
s4, the focusing element 6 focuses the electron beam;
s5, setting the deflection angle of the electron beam according to the requirement of the practical experiment on the spatial resolution, and deflecting the focused electron beam by using the electron beam deflection device 7;
s6, adjusting the sample stage 3 to a suitable position by the sample stage control device, so that the incident electron beam 12 is aligned with the selected sample position of the high flux film 4;
s7, the surface detector 8 is used for receiving the diffracted electron beam 13 diffracted by the high-flux film 4, and the surface detector 8 can collect and obtain all crystal structure information of the sample through the rotation of the sample stage 3;
s8, scanning all samples in the high-throughput film 4 by sequentially moving the selected sample position.
According to the invention, an electron beam which is easy to focus is used as a detection source for high-flux thin film crystal structure representation, and the diameter of a beam spot of the electron beam can be reduced to a micrometer magnitude by the convergence effect of a focusing element 6 on the electron beam, so that the spatial resolution of the surface of a sample is improved;
the invention can change the incident angle of the electron beam through the deflection action of the electron beam deflection device 7 on the electron beam, thereby changing the spatial resolution of the surface of the sample according to the actual experiment requirement;
the low-temperature control system and the temperature feedback control system in the sample table 3 provide a large-range temperature changing condition for the high-flux thin film crystal structure test;
the invention can realize the high-precision controllable movement of the sample stage 3 along the plane through the sample stage moving mechanism 1, and can finish the crystal structure characterization of all samples in the high-flux film by scanning each sample one by one, and can be used for the crystal structure characterization of the high-flux film.
The invention can be integrated in a high-flux thin film preparation system, simultaneously realizes the high-flux preparation of the thin film and the in-situ characterization of the high-flux crystal structure, and greatly improves the experimental efficiency.
It should be understood that the above-described embodiments are merely exemplary of the present invention, and are not intended to limit the present invention, and that any modification, equivalent replacement, or improvement made without departing from the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (8)
1. A high throughput thin film crystal structure characterization device, characterized by: comprises an electron gun emission mechanism, a surface detector, a low-temperature control system, a sample stage control device, a sample stage and a vacuum system; wherein the content of the first and second substances,
the electron gun emission mechanism comprises an electron gun, a focusing element and an electron beam deflection device;
the low-temperature control system comprises a closed-cycle refrigerator and a heat exchange mechanism;
the sample table control device comprises a sample table moving mechanism, a sample table rotating mechanism and a hollow Z-axis driver;
the vacuum system comprises a vacuum pump, a vacuum gauge, a vacuum cavity and a vacuum interface;
the closed-cycle refrigerator is connected with the heat exchange mechanism and is positioned above the sample table; the vacuum interface is positioned above the hollow Z-axis driver and closes the vacuum cavity, the sample stage moving mechanism and the sample stage rotating mechanism are arranged on the vacuum interface and connected with the hollow Z-axis driver, and the electron gun and the surface detector are respectively positioned at two sides of the vacuum cavity; the electron beam deflection device is positioned in the vacuum chamber, and the focusing element is arranged between the electron gun and the electron beam deflection device; the vacuum pump is arranged on the side wall of the vacuum cavity, and the vacuum gauge is arranged on the side wall of the vacuum cavity;
the sample stage moving mechanism controls the sample stage to move along the directions of an x axis, a y axis and a z axis; the sample table rotating mechanism controls the rotation of the sample table along the z axis; the hollow Z-axis driver is used for controlling the whole movement of the low-temperature control system and the sample table along the Z-axis;
and a temperature feedback control system is integrated on the sample table.
2. The high throughput thin film crystalline structure characterization device of claim 1, wherein: the focusing element is an electromagnetic lens.
3. The high throughput thin film crystal structure characterization device of claim 2, wherein: the electron beam deflection device is an electric field deflection device or a magnetic field deflection device.
4. A high throughput thin film crystalline structure characterization device according to claim 3, wherein: the closed-cycle refrigerator comprises a refrigerating head, a compressor and a gas conveying pipeline. The refrigerating head extends into the heat exchange mechanism, and the compressor is connected with the refrigerating head through a gas transmission pipeline.
5. The high throughput thin film crystal structure characterization device of claim 4, wherein: the heat exchange mechanism comprises a heat radiation shielding cover; the thermal radiation shield is located in the vacuum chamber and isolates the vacuum chamber from the cryogenic control system.
6. The high throughput thin film crystal structure characterization device of claim 5, wherein: the closed-cycle refrigerator is a pulse tube refrigerator or a Gilford-Mecanes refrigerator.
7. A method for characterizing the crystal structure of a high-throughput thin film, comprising: use of a high throughput thin film crystalline structure characterization device according to any one of claims 1-6.
8. The method of claim 7, wherein the method comprises the steps of: the method comprises the following steps:
s1, adhering the high-flux film to the center of the surface of the sample stage through an adhesive;
s2, providing a temperature environment required by the test through a low-temperature control system and a temperature feedback control system;
s3, emitting electron beams by the electron gun;
s4, focusing the electron beam by the focusing element;
s5, setting the deflection angle of the electron beam according to the requirement of the practical experiment on the spatial resolution, and deflecting the focused electron beam by using an electron beam deflection device;
s6, adjusting the sample stage to a proper position through the sample stage control device, so that the incident electron beam is aligned with the selected sample position of the high-flux film;
s7, the surface detector is used for receiving the diffracted electron beams diffracted by the high-flux film, and the surface detector can collect and obtain all crystal structure information of the sample through the rotation of the sample stage;
s8, scanning all samples in the high-throughput film by sequentially moving selected sample positions.
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Citations (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09167588A (en) * | 1995-12-14 | 1997-06-24 | Hitachi Ltd | Scanning type electron microscope |
| US20020036264A1 (en) * | 2000-07-27 | 2002-03-28 | Mamoru Nakasuji | Sheet beam-type inspection apparatus |
| US20030089852A1 (en) * | 2001-11-13 | 2003-05-15 | Isao Ochiai | Apparatus and method for observing sample using electron beam |
| CN101334345A (en) * | 2007-06-29 | 2008-12-31 | Fei公司 | Method for attaching a sample to a manipulator |
| CN102156304A (en) * | 2010-12-30 | 2011-08-17 | 中国航天科技集团公司第五研究院第五一○研究所 | Small-sized comprehensive simulation system of lunar environment |
| JP2011165669A (en) * | 2011-03-25 | 2011-08-25 | Hitachi High-Technologies Corp | Mirror electron type sample inspection device |
| US20120217391A1 (en) * | 2009-11-06 | 2012-08-30 | Hiroyasu Shichi | Charged particle microscope |
| CN103123329A (en) * | 2012-12-31 | 2013-05-29 | 上海大学 | Rapid detection method and rapid detection device of non-metallic inclusions in metal |
| CN103134825A (en) * | 2013-02-05 | 2013-06-05 | 山东大学 | A multi-purpose synchrotron radiation coherent X-ray diffraction microscopic imaging device and application |
| CN103257064A (en) * | 2012-02-17 | 2013-08-21 | 卡尔蔡司显微镜有限责任公司 | Method and devices for preparing microscopic samples with the aid of pulsed light |
| CN103776858A (en) * | 2014-01-17 | 2014-05-07 | 西安交通大学 | Panel type collection device and method for measuring secondary electron emission coefficient |
| US20140270071A1 (en) * | 2013-03-15 | 2014-09-18 | MARS TOHKEN X-RAY INSPECTION Co., LTD. | X-ray tube comprising field emission type electron gun and x-ray inspection apparatus using the same |
| CN104617482A (en) * | 2015-02-10 | 2015-05-13 | 中国工程物理研究院激光聚变研究中心 | Laser micro-focus plasma K alpha radiation source |
| CN105891171A (en) * | 2016-03-01 | 2016-08-24 | 中国科学院重庆绿色智能技术研究院 | Efficient high-precision low-temperature laser scanning double-focus microscope system |
| CN106024563A (en) * | 2015-03-31 | 2016-10-12 | Fei 公司 | Charged particle beam processing using process gas and cooled surface |
| KR20170010229A (en) * | 2015-07-17 | 2017-01-26 | 한국표준과학연구원 | Scanning electron microscopy and method for observing a sample using thereof |
| CN106409635A (en) * | 2016-10-19 | 2017-02-15 | 中国科学院西安光学精密机械研究所 | Short magnetic focusing device and method for transversal compression of ultrafast electronic pulses |
| CN106770405A (en) * | 2016-12-09 | 2017-05-31 | 清华大学 | Ultraphotic diffraction imaging device under a kind of complete atmospheric pressure |
| JP2017123320A (en) * | 2016-01-08 | 2017-07-13 | エフ イー アイ カンパニＦｅｉ Ｃｏｍｐａｎｙ | Charged particle microscope with atmospheric pressure correction |
| CN107123584A (en) * | 2016-02-24 | 2017-09-01 | Fei 公司 | The research trends sample behavior in charged particle microscope |
| CN107479330A (en) * | 2016-06-08 | 2017-12-15 | 清华大学 | A kind of photolithography method using electron beam |
| CN107966464A (en) * | 2016-10-20 | 2018-04-27 | Fei 公司 | Low-temperature sample processing in charged particle microscope |
| CN110133462A (en) * | 2019-05-20 | 2019-08-16 | 国网陕西省电力公司 | Composite insulator ageing properties pilot system and method based on space charge effect |
| CN110849926A (en) * | 2018-08-20 | 2020-02-28 | Fei 公司 | Method for examining a sample using a charged particle microscope |
-
2021
- 2021-09-27 CN CN202111134382.3A patent/CN113984813A/en active Pending
Patent Citations (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09167588A (en) * | 1995-12-14 | 1997-06-24 | Hitachi Ltd | Scanning type electron microscope |
| US20020036264A1 (en) * | 2000-07-27 | 2002-03-28 | Mamoru Nakasuji | Sheet beam-type inspection apparatus |
| US20030089852A1 (en) * | 2001-11-13 | 2003-05-15 | Isao Ochiai | Apparatus and method for observing sample using electron beam |
| CN101334345A (en) * | 2007-06-29 | 2008-12-31 | Fei公司 | Method for attaching a sample to a manipulator |
| US20120217391A1 (en) * | 2009-11-06 | 2012-08-30 | Hiroyasu Shichi | Charged particle microscope |
| CN102156304A (en) * | 2010-12-30 | 2011-08-17 | 中国航天科技集团公司第五研究院第五一○研究所 | Small-sized comprehensive simulation system of lunar environment |
| JP2011165669A (en) * | 2011-03-25 | 2011-08-25 | Hitachi High-Technologies Corp | Mirror electron type sample inspection device |
| CN103257064A (en) * | 2012-02-17 | 2013-08-21 | 卡尔蔡司显微镜有限责任公司 | Method and devices for preparing microscopic samples with the aid of pulsed light |
| CN103123329A (en) * | 2012-12-31 | 2013-05-29 | 上海大学 | Rapid detection method and rapid detection device of non-metallic inclusions in metal |
| CN103134825A (en) * | 2013-02-05 | 2013-06-05 | 山东大学 | A multi-purpose synchrotron radiation coherent X-ray diffraction microscopic imaging device and application |
| US20140270071A1 (en) * | 2013-03-15 | 2014-09-18 | MARS TOHKEN X-RAY INSPECTION Co., LTD. | X-ray tube comprising field emission type electron gun and x-ray inspection apparatus using the same |
| CN103776858A (en) * | 2014-01-17 | 2014-05-07 | 西安交通大学 | Panel type collection device and method for measuring secondary electron emission coefficient |
| CN104617482A (en) * | 2015-02-10 | 2015-05-13 | 中国工程物理研究院激光聚变研究中心 | Laser micro-focus plasma K alpha radiation source |
| CN106024563A (en) * | 2015-03-31 | 2016-10-12 | Fei 公司 | Charged particle beam processing using process gas and cooled surface |
| KR20170010229A (en) * | 2015-07-17 | 2017-01-26 | 한국표준과학연구원 | Scanning electron microscopy and method for observing a sample using thereof |
| JP2017123320A (en) * | 2016-01-08 | 2017-07-13 | エフ イー アイ カンパニＦｅｉ Ｃｏｍｐａｎｙ | Charged particle microscope with atmospheric pressure correction |
| CN107123584A (en) * | 2016-02-24 | 2017-09-01 | Fei 公司 | The research trends sample behavior in charged particle microscope |
| CN105891171A (en) * | 2016-03-01 | 2016-08-24 | 中国科学院重庆绿色智能技术研究院 | Efficient high-precision low-temperature laser scanning double-focus microscope system |
| CN107479330A (en) * | 2016-06-08 | 2017-12-15 | 清华大学 | A kind of photolithography method using electron beam |
| CN106409635A (en) * | 2016-10-19 | 2017-02-15 | 中国科学院西安光学精密机械研究所 | Short magnetic focusing device and method for transversal compression of ultrafast electronic pulses |
| CN107966464A (en) * | 2016-10-20 | 2018-04-27 | Fei 公司 | Low-temperature sample processing in charged particle microscope |
| CN106770405A (en) * | 2016-12-09 | 2017-05-31 | 清华大学 | Ultraphotic diffraction imaging device under a kind of complete atmospheric pressure |
| CN110849926A (en) * | 2018-08-20 | 2020-02-28 | Fei 公司 | Method for examining a sample using a charged particle microscope |
| CN110133462A (en) * | 2019-05-20 | 2019-08-16 | 国网陕西省电力公司 | Composite insulator ageing properties pilot system and method based on space charge effect |
Non-Patent Citations (4)
| Title |
|---|
| 游燕;臧侃;郭方准;: "国产高能量电子枪的研发", 物理, no. 11 * |
| 章效锋;: "可输入气体及加热样品的高分辨原位电子显微镜及其应用(英文)", 电子显微学报, no. 05, 15 October 2007 (2007-10-15) * |
| 董关平: "仿生银网络结构柔性透明导电电极制备及其性能研究", 中国博士学位论文全文数据库 工程科技Ⅰ辑, no. 02, 15 February 2021 (2021-02-15) * |
| 陈飞;周洪庆;朱海奎;韦鹏飞;陈栋;刘敏: "(Zr, Sn)TiO4薄膜的制备及电性能研究进展", 硅酸盐通报, vol. 28, no. 05, 15 October 2009 (2009-10-15) * |
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