An in-situ transmission electron microscope optical sample holder

Abstract

The embodiment of the present invention discloses an in-situ transmission electron microscope optical sample holder, comprising a sample holder shaft and a sample holder head which are coaxially arranged and connected to each other, a three-dimensional adjustable sample stage for carrying a sample is installed inside the sample holder head, a rear end of the sample holder shaft is connected to a parallel light beam generator through an optical interface, a vacuum channel for the parallel light beam to pass through is provided inside the sample holder shaft, and a condenser lens for receiving a light beam and focusing the light beam and projecting it onto the three-dimensional adjustable sample stage is provided inside the sample holder head directly opposite to the end of the vacuum channel; the parallel light beam in the embodiment of the present invention passes through the optical interface and the vacuum channel inside the sample holder shaft to irradiate the condenser lens, the condenser lens focuses the light and irradiates it near the three-dimensional adjustable sample stage, and by adjusting the position of the three-dimensional adjustable sample stage, the light source can be focused on a specified micro-area of ​​the sample, so as to facilitate in-situ observation.

Description

Technical Field

[0001] The embodiment of the present invention relates to the technical field of transmission electron microscopy, and in particular to an in-situ transmission electron microscopy optical sample holder. Background Art

[0002] The transmission electron microscope is an electron microscope with high resolution and high magnification. With the advancement of science and technology, the most advanced transmission electron microscopes can already achieve image observation at the picometer level and capture clear atomic images. People are gradually no longer satisfied with just taking transmission electron microscope pictures, but have begun to study how to capture this dynamic process in situ while applying other excitations to the sample in the transmission electron microscope. As a result, a series of in-situ transmission electron microscope sample rods were born to achieve this function. In-situ optical research has always been an important research direction in in-situ transmission electron microscopy technology. This scheme introduces a light source to the transmission electron microscope sample, and in-situ photographs the structural changes of the sample caused by changes in laser wavelength or power, or in-situ collects spectral signals reflected or scattered by the sample.

[0003] In the past, there were two types of in-situ transmission electron microscope optical sample rods. One type is an in-situ optical rod that uses an LED lamp as the light source. The LED lamp is integrated into the end of the sample rod and irradiates the sample after it is lit. The disadvantage of this solution is that the wavelength and power of the light source cannot be changed. In addition, the light is not focused and the signal cannot be collected. The other is a fiber-optic in-situ optical sample rod, which uses an optical fiber to introduce light and irradiate it on the sample. Although this solution can change the wavelength and power of the light, the optical fiber cannot focus the light. Therefore, many studies that require high-power irradiation cannot be carried out, such as the study of in-situ melting samples or in-situ studies that require high-power irradiation to produce structural changes. Summary of the invention

[0004] To this end, an embodiment of the present invention provides an in-situ transmission electron microscope optical sample holder to solve the problem that the in-situ optical rod using LED lamp as the light source in the prior art cannot change the wavelength of light and the fiber-optic in-situ optical sample holder power cannot achieve fiber focusing.

[0005] In order to achieve the above purpose, the embodiment of the present invention provides the following technical solutions:

[0006] An in-situ transmission electron microscope optical sample holder comprises a sample holder shaft and a sample holder head which are coaxially arranged and connected to each other, a three-dimensionally adjustable sample stage for carrying samples is installed inside the sample holder head, a parallel light beam generator is connected to the tail of the sample holder shaft via an optical interface, a vacuum channel for the parallel light beam to pass through is provided inside the sample holder shaft, and a focusing lens for receiving a light beam and focusing the light beam and projecting it onto the three-dimensionally adjustable sample stage is provided inside the sample holder head directly facing the end of the vacuum channel.

[0007] The embodiment of the present invention is also characterized in that the three-dimensional adjustable sample stage includes a fixing frame, a universal adjustment ball and a sample loading platform, the front of the sample loading platform is provided with a sample fixing groove, the universal adjustment ball is connected to the bottom surface of the sample loading platform through a connecting column, the fixing frame is vertically installed on the head of the sample rod, and the fixing frame is provided with an X-axis adjustment mechanism for driving the universal adjustment ball to rotate horizontally and a Y-axis adjustment mechanism for driving the universal adjustment ball to rotate vertically.

[0008] The embodiment of the present invention is also characterized in that the X-axis adjustment mechanism includes a first L-connecting plate, a horizontal bracket is arranged in the middle of the fixed frame, one end of the first L-connecting plate is connected to a first rotating shaft, the first rotating shaft longitudinally passes through the horizontal bracket and is connected to a first power end for driving the first rotating shaft to rotate, the other end of the first L-connecting plate is rotatably connected to a transmission rod, and the transmission rod is fixedly connected to the universal adjustment ball.

[0009] The embodiment of the present invention is also characterized in that the Y-axis adjustment mechanism includes a second L-connecting plate, one end of the second L-connecting plate is rotatably mounted on the connecting column, the other end of the second L-connecting plate is connected to a second rotating shaft, the second rotating shaft transversely passes through the top of the fixed frame and is connected to a second power end for driving the second rotating shaft.

[0010] The embodiment of the present invention is also characterized in that both the first power end and the second power end are rotating motors.

[0011] The embodiment of the present invention is also characterized in that the first power end and the second power end are both rotation stop handles arranged outside the sample rod head, and the first rotation axis and the second rotation axis respectively penetrate the side and bottom of the sample rod head and are connected to the external rotation stop handle.

[0012] The embodiment of the present invention is also characterized in that the rotation stop handle includes a stop angle disk fixedly connected to the rod head of the sample rod and a positioning handle arranged at the center of the stop angle disk, the positioning handle includes a fixed section with one end fixedly connected to the first rotating shaft and the second rotating shaft and a telescopic section vertically connected to the other end of the fixed section, the end of the telescopic section is connected to a press-pop-up section, the stop angle disk is provided with a plurality of ring grooves from the outside to the inside, and a plurality of positioning holes matching the pop-up end of the press-pop-up section are equidistantly opened in each ring groove.

[0013] The embodiment of the present invention is also characterized in that the parallel light beam generator is a fiber laser, and a collimating lens is installed at the output end of the fiber laser.

[0014] The embodiment of the present invention is also characterized in that the sample rod shaft and the sample rod head are connected by bolts, screws, locking screws or micro sealing flanges.

[0015] The embodiment of the present invention is also characterized in that the maximum cross-sectional diameter of the focusing lens is larger than the diameter of the vacuum channel.

[0016] The embodiments of the present invention have the following advantages:

[0017] In the embodiment of the present invention, a parallel light beam generator is used as a light source. The parallel light beam passes through an optical interface and a vacuum channel inside the sample holder to illuminate the focusing lens. The focusing lens focuses the light and irradiates it near the three-dimensional adjustable sample stage. By adjusting the position of the three-dimensional adjustable sample stage, the light source can be focused on a specified micro-area of ​​the sample, which is convenient for in-situ observation. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the implementation methods of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for the implementation methods or the description of the prior art. Obviously, the drawings in the following description are only exemplary, and for ordinary technicians in this field, other implementation drawings can be derived from the provided drawings without creative work.

[0019] The structures, proportions, sizes, etc. illustrated in this specification are only used to match the contents disclosed in the specification so as to facilitate understanding and reading by persons familiar with the technology. They are not used to limit the conditions under which the present invention can be implemented, and therefore have no substantial technical significance. Any structural modification, change in proportion or adjustment of size shall still fall within the scope of the technical contents disclosed in the present invention without affecting the effects and purposes that can be achieved by the present invention.

[0020] Figure 1 A schematic diagram of the overall structure of an optical sample holder provided by an embodiment of the present invention;

[0021] Figure 2 A schematic structural diagram of a three-dimensional adjustable sample stage in an optical sample holder provided by an embodiment of the present invention;

[0022] Figure 3 A schematic diagram of the structure of a rotation stop handle in an optical sample holder provided by an embodiment of the present invention;

[0023] Figure 4 A schematic structural diagram of a positioning handle in an optical sample holder provided by an embodiment of the present invention.

[0024] In the figure:

[0025] 1- sample rod body; 2- sample rod head; 3- three-dimensional adjustable sample stage; 4- optical interface; 5- parallel beam generator; 6- vacuum channel; 7- focusing lens;

[0026] 31-fixed frame; 32-universal adjustment ball; 33-sample loading platform; 34-X-axis adjustment mechanism; 35-Y-axis adjustment mechanism; 36-connecting column;

[0027] 331-sample fixing groove;

[0028] 341 - first L-type connecting plate; 342 - horizontal bracket; 343 - first rotating shaft; 344 - transmission rod; 345 - first power end;

[0029] 351 - second L-connecting plate; 352 - second rotating shaft; 353 - second power end;

[0030] 81 - stop angle plate; 82 - fixed section; 83 - telescopic section; 84 - push-to-pop-out section; 85 - annular groove; 86 - positioning hole. DETAILED DESCRIPTION

[0031] The following is a description of the implementation of the present invention by specific embodiments. People familiar with the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0032] like Figure 1 As shown, the present invention provides an in-situ transmission electron microscope optical sample holder, comprising a sample holder shaft 1 and a sample holder head 2 which are coaxially arranged and connected to each other, a three-dimensional adjustable sample stage 3 for carrying samples is installed inside the sample holder head 2, a parallel light beam generator 5 is connected to the tail of the sample holder shaft 1 through an optical interface 4, a vacuum channel 6 for parallel light beams to pass through is provided inside the sample holder shaft 1, and a focusing lens 7 for receiving a light beam and focusing the light beam and projecting it onto the three-dimensional adjustable sample stage 3 is provided inside the sample holder head 2 directly facing the end of the vacuum channel 6.

[0033] The working process of the embodiment of the present invention for in-situ observation of samples is as follows:

[0034] First, the sample is placed on the three-dimensional adjustable sample stage 3, and the parallel beam generator 5 is turned on. The parallel beam emitted by the generator passes through the optical interface 4 and the vacuum channel 6 inside the sample rod 1 to irradiate the focusing lens 7. The focusing lens 7 focuses the light and irradiates it near the sample. By adjusting the position of the three-dimensional adjustable sample stage 3, the light source can be focused on the specified micro-area of ​​the sample, which is convenient for in-situ observation.

[0035] In the above process, the parallel beam generator 5 refers to a light source that can emit a parallel beam, and its specific structure can be free space parallel light, such as sunlight, or a fiber laser, and a collimating lens is installed at the output end of the fiber laser.

[0036] Optical interface 4 is compatible with mainstream interfaces in the market, such as SMA, FC, etc.

[0037] The three-dimensional adjustable sample stage 3 refers to a sample stage that can be tilted in the X-axis and Y-axis directions. In the embodiment of the present invention, Figure 2 As shown, the specific structure of the three-dimensional adjustable sample stage 3 is as follows: the three-dimensional adjustable sample stage 3 includes a fixing frame 31, a universal adjustment ball 32 and a sample loading platform 33, the front of the sample loading platform 33 is provided with a sample fixing groove 331, the universal adjustment ball 32 is connected to the bottom surface of the sample loading platform 33 through a connecting column 36, the fixing frame 31 is vertically installed on the sample rod head 2, and the fixing frame 31 is provided with an X-axis adjustment mechanism 34 for driving the universal adjustment ball 32 to rotate horizontally and a Y-axis adjustment mechanism 35 for driving the universal adjustment ball 32 to rotate vertically.

[0038] The X-axis adjustment mechanism 34 drives the universal adjustment ball 32 to rotate horizontally, so that the X-axis tilting (i.e. Figure 2 The sample loading platform shown in the figure can be flipped left and right), and the Y-axis adjustment mechanism 35 can drive the universal adjustment ball 32 to rotate vertically to achieve the Y-axis tilting of the sample fixing groove 331 on the sample loading platform 33 (i.e. Figure 2 The sample loading station is flipped forward and backward as shown).

[0039] Furthermore, the X-axis adjustment mechanism 34 includes a first L-connecting plate 341, a horizontal bracket 342 is arranged in the middle of the fixed frame 31, one end of the first L-connecting plate 341 is connected to a first rotating shaft 343, the first rotating shaft 343 longitudinally passes through the horizontal bracket 342 and is connected to a first power end 345 for driving the first rotating shaft 343 to rotate, the other end of the first L-connecting plate 341 is rotatably connected to a transmission rod 344, and the transmission rod 344 is fixedly connected to the universal adjustment ball 32.

[0040] The Y-axis adjustment mechanism 35 includes a second L-connecting plate 351, one end of which is rotatably mounted on the connecting column 36, and the other end of the second L-connecting plate 351 is connected to a second rotating shaft 352, which transversely passes through the top of the fixing frame 31 and is connected to a second power end 353 for driving the second rotating shaft 352 to rotate.

[0041] The first power end 345 and the second power end 353 here can be an electrically controlled rotating device or a manually driven rotating device. When the first power end 345 and the second power end 353 are rotating motors, the first power end 345 and the second power end 353 can be connected to an external PLC system. The first rotating shaft 343 is driven to rotate by controlling the rotation of the first power end 345, so that the first L-connecting plate 341 connected to the first rotating shaft 343 drives the transmission rod 344 to achieve horizontal rotation. Since the transmission rod 344 is fixedly connected to the universal adjustment ball 32, the universal adjustment ball 32 drives the sample fixing groove 331 of the sample loading platform 33 to achieve X-axis tilting. Similarly, the second rotating shaft 352 is driven to rotate by controlling the rotation of the second power end 353, so that the second L-connecting plate 351 connected to the second rotating shaft 352 is rotated, and further drives the sample fixing groove 331 of the sample loading platform 33 to achieve Y-axis tilting.

[0042] In the embodiment of the present invention, when the first power end 345 and the second power end 353 are manually controlled, such as Figure 3 and Figure 4 As shown, the first power end 345 and the second power end 353 are preferably rotation stop handles arranged outside the sample rod head 2, and the first rotating shaft 343 and the second rotating shaft 352 respectively penetrate the side and bottom of the sample rod head 2 and are connected to the external rotation stop handle.

[0043] The rotation stop handle here drives the rotating shaft to rotate by manual rotation and can lock its own position when it rotates to a certain position without rotating.

[0044] The specific structure is as follows: the rotation stop handle includes a stop angle disk 81 fixedly connected to the sample rod head 2 and a positioning handle arranged at the center of the stop angle disk 81, the positioning handle includes a fixed section 82 fixedly connected to the first rotating shaft 343 and the second rotating shaft 352 at one end and a telescopic section 83 vertically connected to the other end of the fixed section 82, the end of the telescopic section 83 is connected to a press-pop-up section 84, the stop angle disk 81 is provided with a plurality of annular grooves 85 from the outside to the inside, and a plurality of positioning holes 86 matching the pop-up end of the press-pop-up section 84 are equidistantly opened in each of the annular grooves 85.

[0045] Since the positioning handle is directly connected to the first rotating shaft 343 and the second rotating shaft 352, the rotation angle of the positioning handle itself is equal to the rotation angle of the first rotating shaft 343 and the second rotating shaft 352. An ordinary cylindrical single handle has a small cross-section and the control of small angles remains unchanged. Therefore, the embodiment of the present invention designs the positioning handle into an L-shaped structure to increase its rotation area.

[0046] The design of the telescopic section 83 can be a simple telescopic sleeve structure, and the length adjustment of the positioning handle can change its rotation area, and the specific structure of the press-to-pop-out section 84 is the structure of an automatic ballpoint pen commonly used in the prior art. Pressing once causes the internal refill to pop out, and pressing again causes the refill to retract. The pop-up end of the press-to-pop-out section 84 here is a cylindrical shape that matches the positioning hole 86. When the pop-up end extends into one of the positioning holes 86, the position locking of the positioning handle is achieved.

[0047] The multi-circle design of the stop angle disk 81 makes the outer circle have a large number of positioning holes 86, and the angle between two adjacent positioning holes 86 is a fixed value and the angle is small, while the inner circle has a relatively small number of positioning holes 86, and the angle between two adjacent positioning holes 86 is also a fixed value and the angle is large, which can be suitable for adjustment and locking of different rotation angles.

[0048] For example, the number of positioning holes 86 of the outer ring is designed to be 72, and the angle between each adjacent two positioning holes 86 is 5 degrees. The number of positioning holes 86 of the inner ring is designed to be 18, and the angle between each adjacent two positioning holes 86 is 20 degrees. When the positioning handle needs to be rotated to a larger angle, such as 60 degrees, the end of the push-to-pop-out section 84 can be directly popped out and inserted through three positioning holes corresponding to the inner ring positioning hole 86. When the positioning handle needs to be adjusted to a smaller angle, such as 10 degrees, the telescopic section 83 can be stretched and rotated to the corresponding outer ring positioning hole 86 through two positioning holes 86 to insert the end of the push-to-pop-out section 84.

[0049] In summary, the tilting angle of the sample fixing slot 331 in the X-axis or Y-axis direction can be controlled by controlling the rotation angle of the first power end 345 and the second power end 353. When the X-axis adjustment mechanism or the Y-axis adjustment mechanism operates independently, due to the rotational connection between the second L-connecting plate 351 and the connecting column 36 and the rotational connection between the transmission rod 344 and the first L-connecting plate 341, the X-axis adjustment mechanism 34 and the Y-axis adjustment mechanism 35 operate independently without interfering with each other.

[0050] The three-dimensional angle of the sample stage 3 is adjusted three-dimensionally by a controller until the sample fixing groove 331 is located at the focus of the condenser lens 7 , so that the light source is focused on the sample to be observed.

[0051] At the same time, the maximum cross-sectional diameter of the condenser lens 7 is larger than the diameter of the vacuum channel 6 , so that all parallel light beams passing through the vacuum channel 6 can be received and focused by the condenser lens 7 .

[0052] The connection between the sample rod shaft 1 and the sample rod head 2 must ensure sealing to prevent light leakage, so the sample rod shaft 1 and the sample rod head 2 can be connected by bolts, screws, locking screws or micro sealing flanges.

[0053] In addition, in addition to the above high-power irradiation function, the sample holder of the embodiment of the present invention can also realize spectroscopy (CL) research such as cathode luminescence spectroscopy. In CL spectroscopy research, the sample is fixed on the three-dimensional adjustable sample stage 3, and the electron beam light source of the transmission electron microscope is used as an excitation source. After irradiating the sample, the sample emits light, and the light source irradiates the focusing lens 7. The light signal passes through the vacuum channel 6 in the sample holder shaft 1 and then passes through the optical interface 4. It is received by an external spectrometer and other equipment to analyze the spectrum.

[0054] Although the present invention has been described in detail above by general description and specific embodiments, it is obvious to those skilled in the art that some modifications or improvements can be made to the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention all belong to the scope of protection claimed by the present invention.

Claims

1. An in-situ transmission electron microscope optical sample holder, comprising a sample holder shaft (1) and a sample holder head (2) coaxially arranged and connected to each other, characterized in that: A three-dimensionally adjustable sample stage (3) for carrying samples is installed inside the sample rod head (2); the tail of the sample rod body (1) is connected to a parallel light beam generator (5) via an optical interface (4); a vacuum channel (6) for the parallel light beam to pass through is provided inside the sample rod body (1); a focusing lens (7) for receiving the light beam and focusing the light beam and projecting it onto the three-dimensionally adjustable sample stage (3) is provided on the upper end of the sample rod head (2) directly facing the end of the vacuum channel (6); the three-dimensionally adjustable sample stage (3) comprises a fixing frame (31) , a universal adjustment ball (32) and a sample loading platform (33), wherein a sample fixing groove (331) is arranged on the front of the sample loading platform (33), the universal adjustment ball (32) is connected to the bottom surface of the sample loading platform (33) via a connecting column (36), the fixing frame (31) is vertically mounted on the sample rod head (2), and the fixing frame (31) is provided with an X-axis adjustment mechanism (34) for driving the universal adjustment ball (32) to rotate horizontally, and a Y-axis adjustment mechanism (35) for driving the universal adjustment ball (32) to rotate vertically.

2. The in-situ transmission electron microscope optical sample holder according to claim 1, characterized in that: The X-axis adjustment mechanism (34) comprises a first L-type connecting plate (341), a horizontal bracket (342) is arranged in the middle of the fixed frame (31), one end of the first L-type connecting plate (341) is connected to a first rotating shaft (343), the first rotating shaft (343) longitudinally passes through the horizontal bracket (342) and is connected to a first power end (345) for driving the first rotating shaft (343) to rotate, and the other end of the first L-type connecting plate (341) is rotatably connected to a transmission rod (344), and the transmission rod (344) is fixedly connected to the universal adjustment ball (32).

3. The in-situ transmission electron microscope optical sample holder according to claim 2, characterized in that: The Y-axis adjustment mechanism (35) comprises a second L-type connecting plate (351), one end of which is rotatably sleeved on the connecting column (36), and the other end of which is connected to a second rotating shaft (352). The second rotating shaft (352) transversely passes through the top of the fixing frame (31) and is connected to a second power end (353) for driving the second rotating shaft (352).

4. The in-situ transmission electron microscope optical sample holder according to claim 3, characterized in that: The first power end (345) and the second power end (353) are both rotating motors.

5. The in-situ transmission electron microscope optical sample holder according to claim 3, characterized in that: The first power end (345) and the second power end (353) are both rotation stop handles arranged outside the sample rod head (2); the first rotation axis (343) and the second rotation axis (352) respectively penetrate the side and bottom of the sample rod head (2) and are connected to the external rotation stop handles.

6. The in-situ transmission electron microscope optical sample holder according to claim 5, characterized in that: The rotation stop handle comprises a stop angle disc (81) fixedly connected to the sample rod head (2) and a positioning handle arranged at the center of the stop angle disc (81); the positioning handle comprises a fixed section (82) fixedly connected to the first rotating shaft (343) and the second rotating shaft (352) at one end and a telescopic section (83) vertically connected to the other end of the fixed section (82); the end of the telescopic section (83) is connected to a press-pop-out section (84); the stop angle disc (81) is provided with a plurality of annular grooves (85) from the outside to the inside, and a plurality of positioning holes (86) matching the pop-out end of the press-pop-out section (84) are equidistantly provided in each annular groove (85).

7. The in-situ transmission electron microscope optical sample holder according to claim 1, characterized in that: The parallel light beam generator (5) is a fiber laser, and a collimating lens is installed at the output end of the fiber laser.

8. The in-situ transmission electron microscope optical sample holder according to claim 1, characterized in that: The sample rod shaft (1) and the sample rod head (2) are connected via bolts, screws, locking screws or micro-sealing flanges.

9. The in-situ transmission electron microscope optical sample holder according to claim 1, characterized in that: The maximum cross-sectional diameter of the condenser lens (7) is greater than the diameter of the vacuum channel (6).

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