CN219416920U - Ion thinning device applied to transmission sample preparation - Google Patents

Abstract

The utility model provides an ion thinning device applied to transmission sample preparation, which at least comprises a vacuum pump assembly, a main body, a sample table assembly and a perforation detection assembly, wherein the sample table assembly and the perforation detection assembly are positioned in the main body; the utility model adopts the symmetrical configuration of the three ion guns, and has higher ion thinning efficiency; the ion gun does not tilt, and the included angle between the sample and the ion beam is controlled by the sample table assembly, so that a larger tilting angle can be allowed; providing a visual window, and visually observing the ion beam state and the ion thinning state; the sample changing chamber capable of being separated in vacuum is configured, the sample changing chamber is small, the vacuumizing time is short, the thinned sample is transferred to the sample changing chamber for sampling and sample changing, the efficiency is faster, the main body can always keep a high vacuum state, the air inlet pollution is avoided, the ion beam is stable, and the ion gun can keep longer service life.

Description

Ion thinning device applied to transmission sample preparation

Technical Field

The utility model belongs to the technical field of sample preparation and electron microscope detection, and particularly relates to an ion thinning device applied to transmission sample preparation.

Background

Ion thinning technology is the main stream of the current transmission electron microscope sample preparation technology, an ion gun is utilized to provide high-energy inert gas ion flow in a high vacuum environment, two sides of a continuously rotating thin sheet sample are bombarded at a certain angle, surface layer atoms of a material are sputtered under the continuous action of bombardment energy which is larger than the atom combination energy of the material, two sides of the sample are continuously thinned, the center part of the final sample is perforated, and an electron beam transparent observation thin area with the thickness of less than 100nm and even up to 10nm is obtained at the edge of the perforation.

The ion thinning equipment has low requirements on sample materials, is not influenced by material conductivity, can also cope with the use of a low-energy ion gun function on energy-sensitive materials, adopts inert gas type ions as an ion source, can not influence the tissue structure of the sample due to ion infiltration, and is suitable for the preparation of transmission electron microscope samples of various materials such as ceramics, metals, semiconductors and the like. In addition, the ion thinning equipment has the advantages of low cost, simple and convenient operation, high quality of prepared samples and the like, and is widely applied to the fields of chemistry, biology and material science at present.

At present, commercial ion thinning equipment generally takes a long time, a sample is prepared for a few hours or even days, analysis and test progress is seriously delayed, and the ion thinning equipment with high thinning efficiency needs to be developed.

Disclosure of Invention

The utility model provides an ion thinning device for preparing a transmission sample, which adopts three ion guns with different angles to improve the thinning efficiency, is provided with a vacuum sample changing assembly, can ensure that a main body keeps a high vacuum environment for a long time, reduces external pollution, ensures that ion beams are more stable, can observe the sample state of a thinning chamber through a visible window when in thinning, and can make operations of adjusting the angle of the sample, testing the vacuum degree and the like according to the sample state in real time.

In order to solve the problems, the utility model adopts the following technical scheme:

an ion thinning device applied to transmission sample preparation at least comprises a vacuum pump assembly, a main body, a sample stage assembly and a perforation detection assembly, wherein the sample stage assembly and the perforation detection assembly are positioned in the main body; the perforation detection assembly is used for detecting a sample thinning state and comprises an opposite-emission laser sensor transmitting end and an opposite-emission laser sensor receiving end; the main body is also connected with an ion gun assembly in a sealing way, the ion gun assembly is used for providing an ion beam and comprises at least one ion gun, and the focus of the ion gun is positioned on the sample stage assembly.

Preferably, the sample holder is an elongated sheet and is mounted above the sample stage in a suspended manner.

Preferably, the ion thinning apparatus further comprises a visual window assembly sealingly mounted to the top of the main body, the visual window assembly comprising a visual window and a window flange.

Preferably, the ion thinning device further comprises a laser baffle mechanism arranged on the side face of the main body, wherein the laser baffle mechanism comprises a baffle sealing cover, an electric push rod and a U-shaped baffle, the electric push rod is positioned in the baffle sealing cover, and the electric push rod is fixedly connected with the U-shaped baffle.

Preferably, the U-shaped baffle opening is towards the sample stage, and when the perforation detection assembly detects a sample, the U-shaped baffle is positioned in the baffle sealing cover, and when the perforation detection assembly does not detect the sample, the U-shaped baffle is positioned in the main body, and the upper baffle and the lower baffle can respectively cover the emitting end of the laser sensor and the receiving end of the opposite laser sensor.

Preferably, the ion thinning device further comprises a vacuum sample changing assembly arranged on the side face of the main body, the vacuum sample changing assembly comprises a sample changing cavity, a sample changing cavity sealing cover plate, a sample table moving mechanism and a manual inserting plate, a sample changing chamber is arranged in the sample changing cavity, the sample changing cavity sealing cover plate is located above the sample changing chamber and can seal the sample changing chamber, and the manual inserting plate is located at the joint of the vacuum sample changing assembly and the main body and used for controlling the communication between the sample changing chamber and the thinning chamber. Further, the sample stage movement mechanism is connected to the side edge of the sample exchange cavity and comprises a translation mechanism, a rotation mechanism and a tilting mechanism. Further, the sample stage is connected with a sample stage movement mechanism.

Preferably, the ion thinning device further comprises a vacuum measuring assembly arranged on the side face of the main body, wherein the vacuum measuring assembly comprises a vacuum gauge and a vacuum gauge joint, and the vacuum gauge is communicated with the main body through the vacuum gauge joint.

Preferably, the vacuum pump assembly is sealingly connected to the main body and comprises a mechanical pump and a molecular pump, the air inlet of which is connected to the bottom of the main body.

The utility model has the following beneficial effects:

1. the utility model adopts three ion guns with different angles, and has high thinning efficiency;

2. the sample stage of the utility model can adjust the angle, and allows a larger relative inclination angle of the ion beam and the sample surface;

3. the utility model is provided with the vacuum sample changing group price, so that the main body can keep a high vacuum environment for a long time, the external pollution is reduced, and the ion beam is more stable;

4. the sample changing chamber is smaller than the main body, the time required for vacuumizing is less, and the sample changing is efficient;

5. the utility model is provided with the visual window assembly, the perforation detection assembly, the laser baffle mechanism and the vacuum measurement assembly, the visual window assembly can observe the sample state of the thinning chamber through the visual window during thinning, can make operations such as adjusting the angle of the sample, testing the vacuum degree and the like according to the sample state in real time, is convenient for grasping the sample thinning condition in real time, does not need to damage the vacuum degree in the main body, and improves the thinning efficiency; the perforation detection assembly can detect sample thinning state, and the laser baffle mechanism can protect the perforation detection assembly when the perforation detection assembly does not detect, shelter from ion thinning sputtering material, avoid the opposite irradiation laser sensor transmitting end and the opposite irradiation laser sensor receiving end to produce deposition pollution, and vacuum measurement assembly can measure the vacuum in the main part, and the staff of being convenient for knows vacuum in the main part.

Drawings

FIG. 1 is a schematic structural view of an ion thinning apparatus;

FIG. 2 is an exploded schematic view of an ion thinning apparatus;

FIG. 3 is a top view of an ion thinning apparatus;

FIG. 4 is a cross-sectional view of FIG. 3;

FIG. 5 is a schematic view of the internal structure of the main body;

fig. 6 is a schematic structural view of the sample vacuum changing assembly.

In the figure: 1. a main body; 2. a window flange; 3. a visual window; 4. a seal ring; 5. a first ion gun; 6. a tilting shaft; 7. a second ion gun; 8. a thinning chamber; 9. a third ion gun; 10. a first motor; 11. a vacuum gauge; 12. a vacuum gauge joint; 13. a second motor; 14. a sample changing cavity; 15. a sample exchange cavity sealing cover plate; 16. a screw motor; 17. a manual plugboard; 18. a rotation shaft; 19. a gear; 20. a sample holder; 21. a sample stage; 22. a sample stage movement mechanism; 23. an emission end of the correlation laser sensor; 24. the transmitting end is fixed with a bracket; 25. a receiving end of the correlation laser sensor; 26. the receiving end is fixedly provided with a bracket; 27. an electric push rod; 28. a U-shaped baffle; 29. a baffle seal cover; 30. a molecular pump; 31. mechanical pump, 32 vacuum system.

Detailed Description

In order to more particularly describe the present utility model, the following detailed description of the technical scheme of the present utility model is provided with reference to the accompanying drawings and the specific embodiments. These descriptions are merely illustrative of how the present utility model may be implemented and are not intended to limit the specific scope of the utility model. The scope of the utility model is defined in the claims.

As shown in fig. 1 to 3, the present embodiment provides an ion thinning apparatus for transmission sample preparation, the ion thinning apparatus including:

the main body 1 is a hollow regular eight-prism and is vertically arranged, a cavity in the middle of the main body is a thinning chamber 8, an ion gun assembly is connected to the outside of the main body, namely three ion guns with identical structures are connected to three of the eight side faces in a sealing way, the ion guns are respectively a first ion gun 5, a second ion gun 7 and a third ion gun 9, the included angles of the axes of the first ion gun and the second ion gun are 135 degrees, the included angles of the axes of the second ion gun and the third ion gun are 135 degrees, the axes of the first ion gun, the second ion gun and the third ion gun are all perpendicular to the central axis of the main body, and the angular bisectors of the included angles of the axes of the first ion gun, the second ion gun and the third ion gun are collinear; the first ion gun, the second ion gun and the third ion gun all adopt argon ion sources, and the ion beam focuses of the first ion gun, the second ion gun and the third ion gun are overlapped and positioned on the central shaft of the main body, so that the ion beam can be projected onto a sample; in the embodiment, three ion guns positioned at different angles are adopted for ion thinning, so that the thinning efficiency can be improved, and the thinning time is greatly shortened;

the vacuum sample exchange assembly is fixed on the side between the first ion gun and the second ion gun on the main body and comprises a sample exchange cavity 14, a sample exchange cavity sealing cover plate 15, a sample platform moving mechanism and a manual insertion plate 17, a sealed sample exchange chamber is arranged in the sample exchange cavity, the sample exchange cavity sealing cover plate is positioned above the sample exchange chamber and can seal the sample exchange chamber, the manual insertion plate is positioned at the joint of the vacuum sample exchange assembly and the main body and is used for controlling the communication between the sample exchange chamber and the thinning chamber, and the manual insertion plate can move up and down in the sample exchange cavity. The sample platform movement mechanism comprises a translation mechanism, a rotation mechanism and a tilting mechanism, and can control the sample platform to perform horizontal movement and rotation movement. The sample exchange cavity is provided with a vacuum system 32, so that the vacuum state of the sample exchange chamber can be freely controlled. When the sample changing chamber is in a vacuum state, the manual inserting plate moves upwards, a gas path channel between the sample changing chamber and the thinning chamber is smooth, samples can be transferred from the thinning chamber to the sample changing chamber, and the samples can be translated and rotated through the sample table moving mechanism in the process; when the manual plugboard moves downwards, the sample changing chamber and the thinning chamber are closed, the operation of taking out the sample from the thinning chamber is completed, the inner spaces of the sample changing chamber and the thinning chamber are mutually independent, and the vacuum state of the thinning chamber is not influenced by the air inlet sampling of the sample changing chamber; meanwhile, the sample exchange chamber of the embodiment has small cavity, fast vacuumizing time, and the thin processed sample is transferred to the sample exchange chamber for sampling and sample exchange, so that the efficiency is faster, the main body can always keep a high vacuum state, the air inlet pollution is avoided, the ion beam stability is facilitated, and the ion gun can keep longer service life.

As shown in fig. 6, the sample stage moving mechanism 22 includes a translation mechanism, a rotation mechanism and a tilting mechanism rotation mechanism, the rotation mechanism includes a first motor 10 and a rotation shaft 18 connected to an output port of the first motor, the sample stage is fixed at an end of the rotation shaft and is driven by a gear 19 to realize rotation, the tilting mechanism includes a second motor 13 and a tilting shaft 6, the tilting shaft is sleeved outside the rotation shaft, and the tilting shaft is driven by a gear to realize tilting; the translation mechanism comprises a main support plate and a screw motor 16 positioned on the main support plate, and the whole sample platform movement mechanism horizontally moves through screw transmission so as to control the horizontal movement of the sample;

as shown in fig. 5, the sample stage assembly is located on the central axis of the main body, and further, the first ion gun, the second ion gun and the third ion gun are at the focal points; the sample platform assembly is used for loading samples and comprises a sample clamp 20 and a sample platform 21, the front end of the sample platform is oblong and connected with a sample motion mechanism, the sample clamp is fixed above the sample platform through bolts, and the sample clamp is suspended above the sample platform and is used for clamping sheet samples with phi 3 mm. The sample clamp body is a pair of upper and lower long thin plates with the thickness of 0.1mm, and a through hole with the thickness of 2.5mm is arranged in the center of each long thin plate, so that the ion beam can bombard the sample conveniently; the sample is suspended and fixed above the sample table through the sample clamp, so that the sample clamp is ensured not to block the ion beam from entering the center of the sample; meanwhile, the oblong shape of the front end of the sample clamp can avoid interference with the ion gun when the sample tilts;

the vacuum measurement assembly comprises a vacuum gauge 11 (penning vacuum gauge is selected in the embodiment) and a vacuum gauge connector 12 (KF 25 vacuum gauge connector is selected in the embodiment), wherein the vacuum gauge is connected to the side surface of the main body between the second ion gun and the third ion gun through the vacuum gauge connector, and the vacuum gauge is directly connected with the inner space of the main body to measure the vacuum degree of the main body.

As shown in fig. 4, the perforation detection assembly is used for detecting a sample thinning state and comprises an opposite-shooting laser sensor transmitting end 23 and an opposite-shooting laser sensor receiving end 25, wherein the opposite-shooting laser sensor transmitting end is fixed above a main body through a transmitting end fixing bracket 24, the opposite-shooting laser sensor receiving end is fixed below the main body through a receiving end fixing bracket 26, the opposite-shooting laser sensor receiving end and the receiving end fixing bracket are both positioned in the vertical direction of the sample, the transmitting end fixing bracket and the receiving end fixing bracket are both in cylindrical structures, and the central axes of the transmitting end fixing bracket and the receiving end fixing bracket coincide with the central axis of the main body; the detection mechanism is that before the sample is not perforated, laser emitted by the emitting end of the opposite-emission laser sensor is shielded by the sample, and a receiving end of the opposite-emission laser sensor cannot receive signals and does not output signals; when the sample is thinned to be perforated by the ion beam, laser emitted by the emitting end of the opposite laser sensor passes through the sample perforation and enters the receiving end of the opposite laser sensor, and the opposite laser sensor outputs signals to detect that the sample is perforated;

the laser baffle mechanism is hermetically arranged on the side surface of the main body between the first ion gun and the third ion gun, and comprises a baffle sealing cover 29, an electric push rod 27 and a U-shaped baffle 28, wherein the electric push rod is positioned in the baffle sealing cover and is fixedly connected with the U-shaped baffle; the U-shaped baffle is a copper baffle, an opening of the U-shaped baffle faces the sample table, when the electric push rod is started to enable the U-shaped baffle to move into the thinning chamber, upper and lower baffle blades of the U-shaped baffle are respectively positioned on the upper side and the lower side of the sample table, at the moment, the upper and lower baffle blades respectively completely shield an emission end of the opposite-emission laser sensor and a receiving end of the opposite-emission laser sensor, the perforation detection assembly does not detect, and meanwhile ions are shielded to thin sputtering substances, so that deposition pollution is avoided to the emission end of the opposite-emission laser sensor and the receiving end of the opposite-emission laser sensor; when the electric push rod drives the U-shaped baffle to shrink into the baffle sealing cover, the emission end of the opposite-emission laser sensor and the receiving end of the opposite-emission laser sensor are exposed, so that the state of a sample can be detected;

the visual window assembly is hermetically arranged at the top of the main body and comprises a visual window 3 (quartz glass wafer is selected in the embodiment) and a visual window flange 2, wherein the visual window flange is a circular flange provided with a groove matched with the visual window in appearance, and the visual window is clamped in the groove of the visual window flange; during thinning, the sample state of the thinning chamber can be observed through the visual window, and operations such as sample angle adjustment, vacuum degree test and the like can be performed in real time according to the sample state, so that the sample thinning condition can be mastered in real time without damaging the vacuum degree in the main body, and the thinning efficiency is improved;

the vacuum pump assembly provides vacuum environment and sealing connection and main part bottom for the main part, and it includes mechanical pump 30 and molecular pump 31, and diaphragm mechanical pump and turbomolecular pump are selected for use to this embodiment, and diaphragm mechanical pump is as the preceding stage pump of turbomolecular pump, and turbomolecular pump air inlet is connected with the main part bottom, guarantees that the gas circuit is unobstructed in the main part. Because the ion gun adopts an argon ion source, the vacuum environment of the main body is favorable for the ion gun to generate stable and continuous ion beams, and the stability of the thinning environment is ensured;

in the embodiment, a main body is taken as a center, and a visual window assembly, an ion gun, a vacuum measuring assembly, a vacuum sample changing assembly, a sample table assembly, a perforation detecting assembly, a laser baffle mechanism and a vacuum pump assembly are all connected with the main body in a sealing way, and a sealing ring 4 is selected for sealing in the embodiment; specifically, the visual window assembly forms a seal with the top of the main body by arranging a sealing ring in the visual window flange, and a visual window flange gland clamped with the visual window; a sealing ring is sleeved at the joint of the ion gun and the side surface of the main body for sealing; a sealing ring is sleeved at the joint of the vacuum gauge joint and the side surface of the main body for sealing; the vacuum sample changing assembly is sealed by arranging sealing rings on two sides of the manual insertion plate; the laser baffle mechanism enables the baffle sealing cover to tightly press the sealing ring and be fixed on the main body by arranging the sealing ring encircling the electric push rod in the annular groove on the side surface of the main body. The sealing connection mode ensures the vacuum environment of the main body, avoids air inlet pollution, is beneficial to the stability of the ion beam, and can keep longer service life of the ion gun.

Although the present utility model is disclosed above, the present utility model is not limited thereto. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the utility model, and the scope of the utility model should be assessed accordingly to that of the appended claims.

Claims (10)

1. An ion thinning device applied to transmission sample preparation at least comprises a vacuum pump assembly, and is characterized by further comprising a main body, a sample stage assembly and a perforation detection assembly, wherein the sample stage assembly and the perforation detection assembly are positioned in the main body, the main body is used for providing a thinning operation cavity and is connected with the vacuum pump assembly, and the sample stage assembly is used for loading a sample and is positioned in the middle of the perforation detection assembly and comprises a sample clamp and a sample stage; the perforation detection assembly is used for detecting a sample thinning state and comprises an opposite-emission laser sensor transmitting end and an opposite-emission laser sensor receiving end; the main body is also connected with an ion gun assembly in a sealing way, the ion gun assembly is used for providing an ion beam and comprises at least one ion gun, and the focus of the ion gun is positioned on the sample stage assembly.

2. The ion milling apparatus of claim 1 wherein the sample holder is an elongated sheet and is suspended above the sample stage.

3. The ion beam thinning apparatus of claim 1, further comprising a visual window assembly sealingly mounted to the top of the body, the visual window assembly comprising a visual window and a window flange.

4. The ion thinning apparatus of claim 1, further comprising a laser baffle mechanism mounted to the side of the main body, the laser baffle mechanism comprising a baffle seal housing, an electric push rod, and a U-shaped baffle, wherein the electric push rod is located in the baffle seal housing, and the electric push rod is fixedly connected to the U-shaped baffle.

5. The ion thinning apparatus according to claim 4, wherein the U-shaped baffle is opened toward the sample stage, the U-shaped baffle is positioned in the baffle sealing cover when the perforation detecting assembly detects the sample, and the U-shaped baffle is positioned in the main body and upper and lower baffle blades thereof can respectively shield the emitting end and the receiving end of the laser sensor when the perforation detecting assembly does not detect the sample.

6. The ion thinning device according to claim 1, further comprising a vacuum sample exchange assembly mounted on the side of the main body, wherein the vacuum sample exchange assembly comprises a sample exchange cavity, a sample exchange cavity sealing cover plate, a sample stage moving mechanism and a manual plug board, a sample exchange chamber is arranged in the sample exchange cavity, the sample exchange cavity sealing cover plate is located above the sample exchange chamber and can seal the sample exchange chamber, and the manual plug board is located at the joint of the vacuum sample exchange assembly and the main body and used for controlling the communication between the sample exchange chamber and the thinning chamber.

7. The ion thinning apparatus of claim 6, wherein the sample stage movement mechanism is coupled to a side of the sample exchange chamber and comprises a translation mechanism, a rotation mechanism, and a tilting mechanism.

8. The ion thinning apparatus of claim 7, wherein the sample stage is coupled to a sample stage motion mechanism.

9. The ion thinning apparatus of claim 1, further comprising a vacuum measurement assembly mounted to a side of the main body, the vacuum measurement assembly comprising a vacuum gauge and a vacuum gauge fitting, the vacuum gauge in communication with the main body through the vacuum gauge fitting.

10. The ion thinning apparatus of claim 1, wherein the vacuum pump assembly is sealingly coupled to the main body and comprises a mechanical pump and a molecular pump, and wherein an air inlet of the molecular pump is coupled to a bottom of the main body.