Patent Publication Number: US-2022216031-A1

Title: Sample protection device for scanning electron microscopy

Description:
CROSS REFERENCE TO RELATED APPLICATIONS 
     This application claims priority to Chinese Patent Applications No. 201921890783.X, filed on Nov. 5, 2019, entitled “sample transferring box for scanning electron microscope”, and No. 201921763316.0, filed on Oct. 21, 2019, entitled “solid-state battery in-situ observing compartment for scanning electron microscope”, the contents of which are incorporated herein in entirety by reference. 
     TECHNICAL FIELD 
     The present disclosure relates to a field of sample protection technology, and in particular, to a sample protection device for a scanning electron microscope. 
     BACKGROUND 
     Scanning electron microscopes are instruments used to observe surface morphologies of objects or materials. When using the scanning electron microscope to observe samples, the requirements for samples are higher. The surface morphology of the observed material exhibits a microstructure. Since some samples are exposed to air, they are easily contaminated by the air when they are transferred to the chamber of the scanning electron microscope, which leads to changes in the micro-morphology of the surface of the material, thereby affecting results of the observation. 
     SUMMARY 
     An object of the present application provides a sample protection device for a scanning electron microscope, to address problems mentioned in the background. 
     According to a first aspect of the present application, a sample protection device for a scanning electron microscope is provided. The sample protection device includes: a shell; an accommodating part including an accommodating space for accommodating a sample, and the accommodating part being disposed in the shell in such a way that the accommodating part and the shell are movable relative to each other, so that the accommodating part is at least partially moved into the shell, or is moved out of the shell; a sealing part connected to the accommodating part, and when the accommodating part is at least partially received in the shell, a seal between the accommodating part and the shell is achieved; and a driving member configured to drive a relative movement of the shell and the accommodating part. 
     The shell is used to at least partially receive the accommodating part accommodating the sample, and the sealing part is used to achieve the seal between the accommodating part and the shell, thereby preventing the influence of the air on the observation results of the sample, which is beneficial to improve the accuracy of observation. 
     In one embodiment, the sealing part is a gastight rubber ring. 
     In one embodiment, the accommodating part is in communication with an internal space of the shell. The accommodating part is disposed with a one-way gas valve. The one-way gas valve is configured to evacuate gas in the shell during the accommodating part entering the shell. 
     In one embodiment, the driving member is a non-magnetic elastic member. The driving member is configured to be in a deformed state due to compression of the accommodating part, after the accommodating part enters the shell; is configured to restore its deformation when gas pressure outside the shell is less than gas pressure inside the shell; and pushes the accommodating part out of the shell during restoring its deformation. 
     In one embodiment, the sample protection device further includes a sliding rail. The shell is slidably connected to the sliding rail. The driving member is a motor. The motor drives the shell to slide along the sliding rail. 
     In one embodiment, the sample protection device further includes a clamping and fixing component configured to fix the sample to the accommodating part. 
     In one embodiment, the clamping and fixing component includes a moving end position and a fixed end position that are coaxially arranged. The sample is accommodated in an area between the fixed end position and the moving end position. 
     According to a second aspect of the present application, a sample transferring box for a scanning electron microscope is provided, which includes a housing with a cavity and an observing compartment slidably disposed in the housing. The housing is disposed with a gap configured to observe objects in the observing compartment. A cavity in the observing compartment is in communication with the cavity in the housing. The observing compartment is disposed with a one-way gas valve. The observing compartment is disposed with a gastight rubber ring configured to seal the housing and the observing compartment. A non-magnetic elastic member is disposed between the observing compartment and the housing. The non-magnetic elastic member is configured to push the observing compartment out of the housing without the observing compartment being separated from the housing. 
     In one embodiment, the housing includes a main housing and a main housing rear cover. The main housing rear cover is connected to the main housing by a bolt. One end of the non-magnetic elastic member is detachably connected to the main housing rear cover, and the other end of the non-magnetic elastic member is engaged in a groove of the observing compartment. 
     In one embodiment, the non-magnetic elastic member is a non-magnetic spring. 
     In one embodiment, the non-magnetic spring is a SUS304L spring, a SUS304H spring or a SUS316L spring. 
     In one embodiment, the gastight rubber ring is connected to the observing compartment in such a way that the gastight rubber ring is engaged in an engaging groove of the observing compartment. 
     In one embodiment, the housing is made of one or more selected from copper, stainless steel, aluminum alloy, resin, or high polymer material. 
     In one embodiment, the observing compartment is made of one or more selected from copper, stainless steel, aluminum alloy, resin, or high polymer material. 
     In one embodiment, the gastight rubber ring is made of one or more selected from silica gel, reinforced polypropylene, and polytetrafluoroethylene. 
     In one embodiment, two non-magnetic elastic members are provided. The non-magnetic elastic members are symmetrically disposed on an inner wall of the observing compartment. 
     According to a third aspect of the present application, a solid-state battery in-situ observing compartment for a scanning electron microscope is provided. The solid-state battery in-situ observing compartment includes a housing disposed with a gastight compartment, a gastight compartment driving motor configured to drive the gastight compartment to be displaced, a clamping and fixing component, a driving member configured to drive the clamping and fixing component to operate, and a test solid-state battery. The clamping and fixing component is configured to clamp and fix the test solid-state battery. A gastight rubber ring is sleeved on an outer surface of the clamping and fixing component. The housing is further disposed with a gastight compartment sliding rail. The gastight compartment is slidable along the gastight compartment sliding rail. The gastight compartment is provided opposite to the clamping and fixing component, and is configured to enclose the test solid-state battery. 
     In one embodiment, the clamping and fixing component includes a fixed end position and a moving end position. The fixed end position and the moving end position are coaxially provided. The test solid-state battery is placed in an area between the fixed end position and the moving end position. 
     In one embodiment, the driving member include a moving end position driving motor. 
     In one embodiment, the moving end position driving motor is a stator coil motor. 
     In one embodiment, the gastight compartment driving motor is a stator coil motor. 
     In one embodiment, the housing and the gastight compartment are made of non-magnetic conductive materials. 
     In one embodiment, the housing and the gastight compartment are made of copper. 
     According to a fourth aspect of the present application, a method of using a sample transferring box for a scanning electron microscope is provided. The sample transferring box for the scanning electron microscope includes a housing with a cavity and an observing compartment slidably disposed in the housing. The housing is disposed with a gap configured to observe objects in the observing compartment. The housing and the observing compartment are a non-magnetic housing and a non-magnetic observing compartment, respectively. A cavity in the observing compartment is in communication with the cavity in the housing. The observing compartment is disposed with a one-way gas valve. The observing compartment is disposed with a gastight rubber ring configured to seal the housing and the observing compartment. A non-magnetic elastic member is disposed between the observing compartment and the housing. The non-magnetic elastic member is configured to push the observing compartment out of the housing without the observing compartment being separated from the housing. 
     The method of using the sample transferring box for the scanning electron microscope includes: 
     putting a sample in the observing compartment in a glove box protected by inert gas, and pushing the observing compartment to a bottom of the housing; 
     placing the sample transferring box for the scanning electron microscope in a chamber of the scanning electron microscope, evacuating gas in the chamber, so that the observing compartment is pushed out of the housing through the non-magnetic elastic member; observing the sample in the observing compartment through the gap; 
     injecting gas into the chamber of the scanning electron microscope to increase gas pressure around the sample protection device, so as to press the observing compartment back into the housing due to increased external gas pressure. 
     According to a fifth aspect of the present application, a method of using a solid-state battery in-situ observing compartment for a scanning electron microscope is provided. The solid-state battery in-situ observing compartment for the scanning electron microscope includes a housing disposed with a gastight compartment, a gastight compartment driving motor configured to drive the gastight compartment to be displaced, a clamping and fixing component, a driving member configured to drive the clamping and fixing component to operate, and a test solid-state battery. The clamping and fixing component is configured to clamp and fix the test solid-state battery. A gastight rubber ring is sleeved on an outer surface of the clamping and fixing component. The housing is further disposed with a gastight compartment sliding rail. The gastight compartment is slidable along the gastight compartment sliding rail. The gastight compartment is provided opposite to the clamping and fixing component, and is configured to enclose the test solid-state battery. 
     The method of using the solid-state battery in-situ observing compartment for the scanning electron microscope includes: 
     assembling the observing compartment and the test solid-state battery in a glove box protected by argon gas, and clamping and fixing the test solid-state battery by the moving end position driven by the moving end position driving motor; 
     the gastight compartment moving along the gastight compartment sliding rail toward the gastight rubber ring to enclose the test solid-state battery driven by the gastight compartment driving motor; 
     placing the solid-state battery in-situ observing compartment in a chamber of the scanning electron microscope; evacuating gas in the chamber; opening the gastight compartment driven again by the gastight compartment driving motor; completing a transfer of the test solid-state battery from the glove box into the chamber of the scanning electron microscope. 
     Details of one or more embodiments of the present application are set forth in the following drawings and description. Other features and advantages of the present application will become apparent from the description, drawings, and claims. 
    
    
     
       BRIEF DESCRIPTION OF THE DRAWINGS 
       To illustrate the technical solutions according to the embodiments of the present application more clearly, the accompanying drawings for describing the embodiments are introduced briefly in the following. Apparently, the accompanying drawings in the following description are only some embodiments of the present application, and persons of ordinary skill in the art can derive other drawings from the accompanying drawings without creative efforts. 
         FIG. 1  is a structural schematic view of a sample protection device according to the present application. 
         FIG. 2  is a structural schematic view of a sample protection device according to one embodiment of the present application. 
         FIG. 3  is a structural schematic view of an observing compartment when enclosed in a housing according to one embodiment of the present application. 
         FIG. 4  is a structural schematic view of an observing compartment when moved out of a housing according to one embodiment of the present application. 
         FIG. 5  is an overall structural schematic view of a sample protection device according to another embodiment of the present application. 
     
    
    
     REFERENCE NUMERALS 
       10 —shell,  20 —accommodating part,  30 —sealing part,  40 —driving member,  1 —observing compartment,  2 —engaging groove,  3 ,  202 —gastight rubber ring,  4 —one-way gas valve,  5 —gap,  6 —housing,  7 —non-magnetic elastic member,  8 —main housing rear cover,  100 —housing,  201 —gastight compartment,  300 —fixed end position,  400 —moving end position,  501 —gastight compartment driving motor,  502 —moving end position driving motor,  600 —gastight compartment sliding rail,  700 —test solid-state battery. 
     DETAILED DESCRIPTION OF THE EMBODIMENTS 
     Technical solutions in embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Apparently, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the protection scope of the present application. 
     Referring to  FIG. 1 , according to one embodiment of the present application, a sample protection device for a scanning electron microscope is provided, which includes a shell  10  and an accommodating part  20 . The accommodating part  20  has an accommodating space. During using the scanning electron microscope, a sample to be observed can be put into the accommodating space. The shell  10  can be moved relative to the accommodating part  20 , so that the accommodating part  20  is disposed in the shell  10  in a movable manner with respect to the shell  10 . In this way, the accommodating part  20  is at least partially received in the shell  10 , or is moved out of the shell  10 . The accommodating part  20  is connected to a sealing part  30 . The sealing part  30  can achieve a seal between the accommodating part  20  and the shell  10  when the accommodating part  20  is at least partially received in an observing compartment, so as to ensure the sample in the accommodating part  20  is not in contact with external air. The sample protection device further includes a driving member  40  configured to drive a relative movement of the shell  10  and the accommodating part  20 . It should be understood that although the driving member  40  is shown as being connected to the accommodating part  20  in  FIG. 1 , it is only an embodiment. In other embodiments, the driving member  40  may also be connected to the shell  10 , as long as the driving member  40  can realize the relative movement of the shell  10  and the accommodating part  20 . 
     Further, the sealing part  30  may be a gastight rubber ring, which is detachably disposed on the accommodating part  20 . As those skilled in the art can understand, the sealing part  30  can be other components according to actual needs, such as components made of polytetrafluoroethylene, soft bakelites, graphite rings, etc., as long as the sealing part  30  can realize the seal between the accommodating part  20  and the shell  10 . Preferably, the sealing part  30  is made of an elastic material and has abrasion resistance. The accommodating part  20  may be disposed with a one-way gas valve. The accommodating part  20  is in communication with an internal space of the shell  10 . The driving member  40  may be a non-magnetic elastic member, such as a spring, etc. 
     During the accommodating part  20  entering the shell  10 , since the accommodating part  20  is in communication with the shell  10 , the gas in the shell  10  is compressed, and is discharged outside of the shell  10  via the one-way gas valve disposed on the accommodating part  20 . In this case, the spring is compressed by the accommodating part  20  and then deformed. When the gas in the shell  10  is emptied, the shell  10  is in a high vacuum state. In this case, the outside gas pressure is higher than the gas pressure in the shell  10 , and the spring remains in a deformed state due to the existence of the gas pressure difference. When the gas pressure outside the shell  10  is less than the gas pressure inside the shell  10 , the spring restores its deformation and pushes the accommodating part  20  out of the shell  10  during the process of restoring its deformation. 
     Specifically, referring to  FIGS. 2-4 , in one embodiment, the above-mentioned sample protection device for the scanning electron microscope may be a sample transferring box of the scanning electron microscope. The shell  10  can be a housing  6  with a cavity. The accommodating part  20  can be an observing compartment  1 . The sealing part  30  can be a gastight rubber ring  3 . The driving member  40  can be a non-magnetic elastic member  7 . Specifically, the observing compartment  1  is slidably disposed in the housing  6 . The housing  6  is disposed with a gap  5 , which facilitates the observation of objects in the observing compartment  1 . A cavity in the observing compartment  1  is in communication with the cavity in the housing  6 . The observing compartment  1  is disposed with a one-way gas valve  4 . The observing compartment  1  is disposed with the gastight rubber ring  3  for sealing the housing  6  and the observing compartment  1 . The non-magnetic elastic member  7  is disposed between the observing compartment  1  and the housing  6 . The non-magnetic elastic member  7  is used to push the observing compartment out of the housing  6  and keep the observing compartment  1  from being separated from the housing  6 . It should be understood that  FIG. 2  is an exploded view of this embodiment, which is only intended to show the independent form of each component, and does not mean that the positional relationship and connection relationship between these components are necessarily to be provided as shown. In other words, the positional relationship and connection relationship between components should be understood in conjunction with other drawings. 
     Preferably, the housing  6  includes a main housing and a main housing rear cover  8 . The main housing rear cover  8  and the main housing are connected by connecting bolts. One end of the non-magnetic elastic member  7  is detachably connected to the main housing rear cover  8 , and the other end of the non-magnetic elastic member  7  is engaged in a groove on the observing compartment  1 , which is convenient for disassembly and replacement of the non-magnetic elastic member  7 . 
     Preferably, the non-magnetic elastic member  7  is a non-magnetic spring, which has a long service life. 
     Preferably, the non-magnetic spring is a SUS316L spring, which has good resistance to intergranular corrosion. 
     In other embodiments, the non-magnetic spring  7  is a SUS304H spring or a SUS304L spring. 
     Preferably, the gastight rubber ring  3  is connected to the observing compartment  1  in such a way that the gastight rubber ring  3  is engaged in an engaging groove  2  on the observing compartment  1  to facilitate the disassembly and replacement of the gastight rubber ring  3 . 
     Preferably, the housing  6  is made of copper, which has good wear resistance. 
     In other embodiments, the housing  6  is made of one or more selected from stainless steel, aluminum alloy, resin, or high polymer material. 
     Preferably, the observing compartment  1  is made of copper, which has good wear resistance. 
     In other embodiments, the observing compartment  1  is made of one or more selected from stainless steel, aluminum alloy, resin, or high polymer material. 
     Preferably, the gastight rubber ring  3  is made of polytetrafluoroethylene and has a low friction coefficient. 
     In other embodiments, the gastight rubber ring  3  is made of silica gel or reinforced polypropylene. 
     Preferably, two non-magnetic elastic members  7  are provided. The non-magnetic elastic members  7  are symmetrically disposed on an inner wall of the observing compartment  1 , which has a good push-out effect on the observing compartment  1 . 
     The method of using the sample protection device according to this embodiment is as follows. 
     Firstly, the sample is put in the observing compartment  1  in a glove box protected by inert gas. Then, the observing compartment  1  is pushed to the bottom of the main housing. The gas in the main housing is discharged to the outside of the main housing through the one-way gas valve  4 . The observing compartment  1  is fixed to the bottom of the main housing (as shown in  FIG. 3 ) under the external atmospheric pressure. The gastight rubber ring  3  prevents external gas from penetrating into the main housing, ensuring the gastight effect. 
     Then, the assembled and enclosed sample device is placed in a chamber of the scanning electron microscope, and the air in the chamber is evacuated, so that the observing compartment  1  is pushed out of the main housing through the non-magnetic elastic member  7  (as shown in  FIG. 4 ). In this case, the sample in the observing compartment  1  can be observed. 
     After the observation is completed, if it is necessary for the observing compartment  1  to return to the main housing, gas can be injected into the chamber of the scanning electron microscope to increase the gas pressure around the sample protection device. In this case, the observing compartment  1  will be pressed back into the main housing due to the increased external gas pressure. 
     According to the above embodiment, the sample device and the elastic member made of non-magnetic materials can be used to prevent the influence of the magnetic material on the imaging of the observation results of the sample, which is beneficial to improve the accuracy of the observation. In addition, when the observing compartment is enclosed, the gas in the main housing is discharged through the one-way gas valve. In addition, the one-way gas valve can prevent the entering of the external gas, so that the observing compartment is not opened under the external gas pressure. When the sample device enters the chamber of the scanning electron microscope, the gas pressure decreases, and thus the non-magnetic elastic member pushes the observing compartment out of the main housing. In this case, the sample can be observed, and the use of motors or electromagnets can be avoided. In addition, no external controlling cables are required. 
     According to another embodiment of the present application, the sample protection device includes a sliding rail. The shell  10  is slidably connected to the sliding rail. The driving member  40  is a motor. The shell  10  can slide along the sliding rail driven by the motor. The sample protection device further includes a clamping and fixing component for fixing the sample to the accommodating part  20 . As an example, the clamping and fixing component may include a moving end position and a fixed end position that are coaxially arranged. The sample is accommodated in an area between the fixed end position and the moving end position. 
     Specifically, referring to  FIG. 5 , in one embodiment, the sample protection device for the scanning electron microscope may be a solid-state battery in-situ observing compartment for a scanning electron microscope. The shell  10  can be a gastight compartment  201 . The sealing part  30  can be a gastight rubber ring  202 . The driving member  40  can be a gastight compartment driving motor  501  for driving the gastight compartment  201  to be displaced. The gastight compartment  201  and the accommodating part  20  are both disposed in a housing  100 . The solid-state battery in-situ observing compartment further includes a clamping and fixing component. The sample is a solid-state battery  700 . The clamping and fixing component is used to clamp and fix the test solid-state battery  700 . The gastight rubber ring  202  is disposed on an outer surface of the clamping and fixing component. A gastight compartment sliding rail  600  is further disposed in the housing  100 . The gastight compartment  201  can slide on the gastight compartment sliding rail  600 . The gastight compartment  201  is provided opposite to the clamping and fixing component, and is used to enclose the test solid-state battery  700 . 
     Preferably, the clamping and fixing component includes a fixed end position  300  and a moving end position  400 . The fixed end position  300  and the moving end position  400  are coaxially provided. The test solid-state battery  700  is placed in an area between the fixed end position  300  and the moving end position  400 . 
     Preferably, the driving member includes a moving end position driving motor  502 . More specifically, the moving end position driving motor  502  and the gastight compartment driving motor  501  are both stator coil motors. 
     Preferably, both the housing  100  and the gastight compartment  201  are made of non-magnetic conductive materials. Preferably, the housing  100  and the gastight compartment  201  are made of copper. 
     A method of using the sample protection device according to this embodiment is as follows. 
     Firstly, the observing compartment and the test solid-state battery  700  are assembled in a glove box protected by argon gas. The test solid-state battery  700  is clamped and fixed by the moving end position  400  driven by the moving end position driving motor  502 . Then, the gastight compartment  201  is driven by the gastight compartment driving motor  501  to move along the gastight compartment sliding rail  600  toward the gastight rubber ring  202  to enclose the test solid-state battery  700 . 
     The assembled and enclosed observing compartment is placed in the chamber of the scanning electron microscope. The gas in the chamber is evacuated. The gastight compartment  201  is opened driven again by the gastight compartment driving motor  501 . Thus, a transfer of the test solid-state battery  700  from the glove box into the chamber of the scanning electron microscope is completed. 
     According to the above embodiment, the test solid-state battery is mounted between the fixed end position of the solid-state battery and the moving end position of the solid-state battery, through the gastight compartment in the glove box filled with argon. After the gastight compartment is closed, the observing compartment is moved to the chamber of the scanning electron microscope, it is ensured that the test solid-state battery is not polluted by the air before the observation. In addition, the stator coil motor can be used to prevent the magnetism of a permanent magnet motor from affecting the imaging of the scanning electron microscope, thereby facilitating the accuracy of observation. Furthermore, through the control of the stator coil motor, it is convenient to open a cover of the observing compartment in the chamber of the scanning electron microscope. In addition, the use of non-magnetic conductive materials prevents the magnetism of the permanent magnet motor from affecting the imaging of the scanning electron microscope, thereby facilitating the accuracy of observation. 
     While the embodiments of the present application have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, replacements, and variations can be made to these embodiments without departing from the principle and spirit of the present application., the scope of the present application shall be subject to the appended claims and their equivalents.