Low-temperature cleaning device

By using a low-temperature cleaning device of a single-stage refrigeration system in the vacuum chamber of the analytical instrument, condensing and/or adsorbing gas molecules, the problem of vacuum chamber pollution is solved, efficient and regular cleaning is achieved, and experimental throughput is improved and costs are reduced.

CN119746455APending Publication Date: 2025-04-04FEI CO
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Patent Information

Application Number
CN202411390502.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Priority Date
2023-10-03
Filing Date
2024-10-08
Publication Date
2025-04-04

AI Technical Summary

Technical Problem

The prior art is difficult to effectively remove vacuum chamber contaminants in analytical instruments, especially under low vacuum conditions, and the size and vibration problems of the cryopump limit their application.

Method used

A low temperature cleaning device is provided, which adopts a single-stage refrigeration system to reduce contamination in the vacuum chamber by condensing and/or adsorbing gas molecules on the cooling surface. The device includes a valve to close the fluid path, maintain vacuum conditions, and remove accumulated gas molecules by a baking cleaning device.

Benefits of technology

The vacuum chamber of the analytical instrument is achieved without destroying the vacuum conditions, which improves the throughput of experiments and imaging, reduces equipment costs and complexity, and allows the use of a cryogenic cleaning device without the need for additional vibration isolation equipment.

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Abstract

The present disclosure relates to a cryogenic cleaning device comprising a body and an attachment element for attaching the body to a vacuum chamber of an analytical instrument to provide a fluid path between the body and the vacuum chamber. The surface is configured to accumulate gas molecules received into the body via the fluid path by condensing and / or adsorbing the gas molecules on the surface when cooled by the single stage refrigeration system. The pump is configured to pump accumulated gas molecules during baking of the cryogenic cleaning device. A valve of the cryogenic cleaning device is movable between a first position, in which the fluid path is open to allow the gas molecules to exit from the vacuum chamber into the body, and a second position, in which the fluid path is closed to prevent the gas molecules from being received into the body.
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Description

Technical Field

[0001] The present disclosure generally relates to systems and methods for cleaning analytical instruments, particularly analytical instruments including vacuum chambers, and more particularly to a cryogenic cleaning apparatus. Background Art

[0002] Clean vacuum chambers are useful for analytical instrumentation so that the desired pressure can be quickly reached when the chamber is evacuated. Clean vacuum chambers are also required to provide high-quality measurements (including images) when operating analytical instrumentation. For example, a clean SEM vacuum chamber can improve the resolution and accuracy of images generated by the SEM system. In addition, a clean SEM vacuum chamber can reduce the amount of system maintenance required.

[0003] Water (including water vapor and ice) is a common contaminant in vacuum chambers. This is especially true in high vacuum chambers and low vacuum chambers, where vacuum requirements may not be as stringent as in chambers configured to provide ultra-high vacuum (UHV) or extreme high vacuum (XHV) conditions. Therefore, in high vacuum chambers and low vacuum chambers, ambient air (including water vapor) may leak into the vacuum chamber, for example, via a weak seal in the vacuum chamber.

[0004] When water or ice is present on the sample surface during observation, this may affect the results obtained by the analytical instrument. For example, the signal of the emitted electrons may be affected by the water layer on the sample surface. In addition, samples that are sensitive to oxidation (for example, battery samples or (metal) samples heated on a heating table in a vacuum chamber) may be oxidized by residual water. In addition, any water or ice in or on the sample may change the structure of the sample. Due to any one or more of these reasons, accurate data may not be easily obtained. Therefore, it is desirable to remove water and other contaminants from the vacuum chamber so that useful results can be obtained.

[0005] Certain parts of the analytical instrument and / or vacuum system often prevent direct baking of the vacuum chamber or analytical instrument to remove contaminants. For example, a chromatography column may include electronics that prevent the analytical instrument from being heated above 80°C. Therefore, a cleaning device may be used to purge the vacuum chamber.

[0006] A cryopump (also referred to herein as a cryopump) is a device that can be used to remove contaminants from a vacuum chamber. A cryopump is a vacuum pump that captures gases and vapors received into the cryopump by condensing the gases or vapors on a cold surface. When the amount of condensed gas on the surface approaches saturation, the ability of the surface to collect gas molecules decreases. Therefore, the cryopump is regenerated by heating the cryopump, allowing the trapped gas to be released through a pressure relief valve.

[0007] However, cryopumps are large and expensive, in part due to the need for a two-stage refrigeration system to cool the surface to very low temperatures (20K or less). The size of a cryopump may mean that it cannot be easily used with certain analytical equipment because there is not enough space to attach the cryopump to the analytical instrument. In addition, saturation of the surface occurs very quickly under low vacuum conditions. For these reasons, cryopumps are usually used only for ultra-high vacuum conditions, especially because other instruments (which may be smaller in size) can provide high vacuum conditions at a lower cost.

[0008] Cryopump operation may also result in large vibrations, making it unsuitable for many applications without additional equipment. For example, a cryopump cannot usually be used with a standard SEM system without additional equipment to isolate the vibrations (because the vibrations will degrade the performance and resolution of the SEM system). These additional equipment can be very expensive, and there may not be any straightforward way to connect the additional equipment to a standard analytical instrument that does not typically use a cryopump.

[0009] There is a need to overcome the above problems. Summary of the invention

[0010] Against this background, a cryogenic cleaning device, system and method for removing or reducing contaminants in analytical instruments are provided as described in the independent claims. Additional aspects emerge from the description and claims.

[0011] The methods described herein may be implemented by a controller configured to operate a system including a cryogenic cleaning device and an analytical instrument, the analytical instrument including a vacuum chamber. Similarly, the methods described herein may be implemented in a system including a cryogenic cleaning device, an analytical instrument, and a controller configured to operate the cryogenic cleaning device and / or the analytical instrument.

[0012] The above method can be implemented as a computer program, which includes instructions for operating a computer or computer system (or other hardware and / or software configured to implement the method). The computer program can be stored on a computer readable medium (e.g., a non-transitory computer readable medium).

[0013] For example, a computer system may include a processor, such as a central processing unit (CPU). The processor may execute logic in the form of a software program. The computer system may include a memory, which includes volatile and / or non-volatile storage media. Different parts of the system may be connected using a network (e.g., a wireless network and a wired network). The computer system may include one or more interfaces. For example, a computer system may contain a suitable operating system, such as UNIX (including Linux), or Windows (RTM).

[0014] It should be noted that any feature described herein may be used with any specific aspect or embodiment of the invention. In addition, any combination of specific device, structural or method features is also provided, even if the combination is not explicitly described.

[0015] The invention will now be described with reference to the accompanying drawings which depict various embodiments of the invention, provided purely by way of example and not limitation. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] The invention may be implemented in many ways and a preferred embodiment will now be described by way of example only and with reference to the accompanying drawings, in which:

[0017] Figure 1 Schematically illustrates an exemplary system including a cryogenic cleaning device and an analytical instrument including a vacuum chamber and connected to the cryogenic cleaning device via a fluid path including a valve;

[0018] Figure 2 Another exemplary system is schematically illustrated including a cryogenic cleaning apparatus and an analytical instrument including a vacuum chamber;

[0019] Figure 3 A flow chart showing a method for reducing contamination in a vacuum chamber of an analytical instrument;

[0020] Figure 4 A schematic diagram of an exemplary system comprising a cryogenic cleaning apparatus and an analytical instrument connected via a fluid path including a gate valve is shown;

[0021] Figure 5A illustrates a schematic diagram of an exemplary system including a detachable connector connected to an analytical instrument;

[0022] Figure 5B illustrates a schematic diagram of an exemplary system including a removable connector in a retracted position; and

[0023] Figure 5C A schematic diagram of an exemplary system including a removable connector in another retracted position is shown.

[0024] It should be noted that the figures are shown for simplicity and are not necessarily drawn to scale. Similar features are provided using the same (or similar) reference numerals. DETAILED DESCRIPTION

[0025] The present disclosure provides a cryogenic device for reducing contamination in a vacuum chamber of an analytical instrument, which may also be referred to herein as a (cryogenic) purification device or a (cryogenic) cleaning device. Cryogenic technology refers to the production and behavior of materials at very low temperatures, and is considered to be related to refrigeration below about 120K (-153°C) to distinguish cryogenic technology from conventional refrigeration. Therefore, a cryogenic device can be considered to be a device configured to operate at low temperatures (below 120K).

[0026] Since the apparatus described herein is primarily concerned with reducing water (or water vapor) contamination, the apparatus may also be referred to as a dehydrator or water purification apparatus. However, even when a single-stage refrigeration system is employed, other contaminants, such as hydrocarbons, may be removed from the vacuum chamber by using cryogenic apparatus.

[0027] The device comprises a main body and an attachment element, and the attachment element is used to attach or install the main body to the vacuum chamber of the analytical instrument to provide a fluid path between the main body and the vacuum chamber. The fluid may include a liquid, a gas or any other material that can flow. Therefore, the fluid path may also be referred to as a gas path in this article. The main body may be a bakeable volume of the device. The attachment element may include a flange for installing the main body to the vacuum chamber, but it should be understood that other attachment or installation methods may be used.

[0028] The device also includes a surface configured to accumulate gas molecules (or gas particles) received into the body via a fluid path. The surface is configured to collect gas molecules by condensing and / or adsorbing the gas molecules on the surface when the surface is cooled. Therefore, the device also includes a single-stage (low-temperature) refrigeration system configured to cool the surface. As used herein, the term single-stage refrigeration system does not include second-stage refrigeration. Therefore, the device can cool the surface to a temperature in the range of 60K to 120K, and can therefore operate within a certain temperature range to remove water and hydrocarbon contaminants from the vacuum chamber. The device can be configured to operate at a specific temperature according to the contaminants to be removed. For example, the device can be controlled to operate at, for example, 80K or 100K to remove water vapor from the vacuum chamber of the analytical instrument.

[0029] As gas molecules accumulate on a cooled surface, the ability of the surface to collect more gas molecules decreases. In the case of condensation, as the thickness of the layer of condensed gas molecules increases, the surface temperature of the condensed layer increases, thereby reducing the rate of condensation of the gas molecules. In the case of adsorption (i.e., the attachment of molecules to a surface), the rate of adsorption of gas molecules decreases significantly as the amount of adsorbed gas molecules approaches saturation (which may depend on the temperature and pressure of the adsorbed gas molecules).

[0030] Due to adsorbed and / or condensed molecules, the ability of a low temperature cleaning device to remove contaminants from the vacuum chamber of an analytical instrument decreases as the amount of condensed and / or adsorbed molecules on the cooling surface increases. Therefore, the collected gas molecules must be removed to restore the original operating capacity of the cleaning device. This is achieved by baking the device (applying high temperature and sometimes vacuum to the device). As a result, the accumulated gas molecules vaporize or evaporate, causing the gas molecules to be discharged from the cleaning device (e.g., by using a pump during baking).

[0031] In conventional cleaning devices with only a single-stage refrigeration system, baking out and evacuating the cleaning device requires disconnecting the cleaning device from the vacuum chamber. Since conventional cleaning devices are (directly) connected to the vacuum chamber, disconnecting the cleaning device results in an interruption of the vacuum system. As a result, the vacuum conditions of the vacuum chamber cannot be adequately maintained. Therefore, cleaning of the device is usually performed only after the cleaning device is completely filled with contaminants (e.g., filled with ice due to the removal of water vapor from the vacuum chamber).

[0032] However, as mentioned above, the cleaning ability of the cleaning device decreases as the contaminants in the cleaning device increase. Therefore, in the later stages of an experiment (or series of experiments), the cleaning ability of the device decreases, which means that it may be more difficult (or even impossible) to maintain the vacuum conditions necessary for the experiment or data collection. The lower vacuum may result in the analytical instrument producing poor data and / or poor image quality, and in the worst case, no (useful) data may be obtained at all.

[0033] In addition, cleaning the device may require time and manpower, which significantly reduces the throughput of experiments and / or imaging due to, for example, the need to remove the device (or a portion thereof) for baking. When removing contaminants from the cleaning device, the analytical instrument cannot be used, at least because the lack of the cleaning device will mean poor results due to the accumulation of contaminants. In other words, when the device (or a portion thereof) is removed for baking, the experiment or measurement needs to be stopped.

[0034] In contrast, the currently disclosed cleaning device includes a valve that can be moved between a first position, in which the fluid path is open to allow gas molecules to be discharged from the vacuum chamber into the body, and a second position, in which the fluid path is closed or blocked to prevent gas molecules from being received into the body. Thus, when the cleaning device is baked and evacuated, the valve can be closed to close the fluid path. This can allow the vacuum conditions of the connected vacuum chamber to be maintained, which in turn can lead to less contamination in the vacuum chamber, because, for example, when the cleaning device is removed for cleaning, ambient air cannot enter the vacuum chamber. The valve can also allow cleaning to be performed more regularly, because the cleaning device does not have to be removed for cleaning, and the risk of breaking the vacuum can therefore be reduced.

[0035] Thus, the time required to clean the device can be reduced because the cleaning device is not only cleaned when completely full. In addition, the vacuum chamber may be able to be cleaned more efficiently because the effectiveness of the cleaning device can be maintained by regularly evacuating condensed and / or adsorbed gas molecules. This can allow vacuum chambers with weaker seals (e.g., in vacuum chambers where UHV is not required), such as O-rings, to be used in a wider range of applications because contaminants (e.g., water vapor) in such vacuum chambers can be removed more efficiently. Similarly, the valve can allow a vacuum chamber with one or more openable holes that can be opened fairly regularly (e.g., one or more doors to allow a user to insert a sample when setting up an experiment), or allow a vacuum chamber that otherwise cannot provide sufficient vacuum conditions using conventional cleaners to be used. This can also increase the life of vacuum chambers used in analytical instruments because degradation of the vacuum chamber can be overcome by more effective cleaning of the cleaning device.

[0036] Furthermore, since the closed gas path allows the vacuum in the vacuum chamber to be maintained, the analytical instrument can continue to operate while the fluid path is closed. Thus, the throughput of experiments or imaging can be increased.

[0037] Furthermore, the use of an effective cryogenic cleaning device can be achieved without the need for additional equipment (eg, for eliminating vibrations to allow a cryogenic pump to be connected to the SEM vacuum chamber).Thus, the cost and complexity of the analytical instrumentation setup can be reduced.

[0038] refer to Figure 1 , shows an example system 100 including a cryogenic cleaning device 104 and an analytical instrument 120, the analytical instrument including a vacuum chamber 102 connected to the cryogenic cleaning device 104. The cryogenic cleaning device 104 is attached to the analytical instrument via an attachment element 122. Figure 1 Only one low temperature cleaning device 104 is shown in the figure, but the system 100 may also include one or more additional low temperature cleaning devices 104, such as the reference Figure 2 The system may also include a controller (not shown) configured to operate the cleaning device 104 and / or the analytical instrument 120 according to the methods disclosed herein.

[0039] The cryo cleaner 104 may include a device or component, such as a heating element, for baking the cleaning device 104. In other words, the cryo cleaner 104 may be bakeable and may include a device configured to bake the cryo cleaner 104. For example, the cryo cleaner may include a resistive heating element 116, such as Figure 1It should be understood that another component may be used to bake the cleaning device in addition to or in place of the resistive heating element 116. For example, the device may include a radiant heating element and / or a conductive heating element.

[0040] In other examples, the system 100 may include a baking device other than the low temperature cleaner 104. For example, the baking device may include an infrared lamp to bake the low temperature cleaning device 104. In another example, the baking device may include an oven. In another example, the baking device may include a flexible heating material (e.g., a cloth heating jacket). The flexible heating material may include a resistive wire sewn into a liner to provide heat. The flexible heating material may be designed and manufactured to a specific size and configuration based on the size of the low temperature cleaning device 104 to allow surface contact to generate consistent heat throughout the area. In yet another example, the baking device may include a heating cable or a heating belt.

[0041] The cryogenic cleaner 104 includes a valve 101, which may preferably be a gate valve (also known as a sluice valve) or may be another type of valve, including a ball valve, a butterfly valve, or a plug valve. Other types of valves are also possible. The valve 101 allows a fluid path 105 between the cryogenic cleaner 104 and the vacuum chamber 102 (which may be provided by a channel or conduit in the attachment element 122, such as Figure 1 , or provided by the attachment element 122 itself) to prevent gas molecules from being received into the body 103 of the cryo-cleaner.

[0042] The cryocleaner 104 also includes a single-stage refrigeration system. Figure 1 In the illustrated example, the single-stage refrigeration system includes a cryogen storage component 107 disposed outside the body 103 of the cryogenic cleaning device 104 and one or more refrigerant pipes 106 disposed at least partially within the body 103 and connected to the cryogen storage component 107. The cryogen storage component 107 may also be referred to herein as a cryogenic storage container 107.

[0043] Cryogenic storage component 107 can be or include cryogenic storage dewar flask (or dewar flask container), cryogenic storage cylinder or cryogenic storage tank. Cryogenic storage dewar flask is a vacuum bottle configured to store cryogen, and can be smaller than cryogenic storage cylinder or storage tank, but similar in other aspects. Cryogenic agent usually has a boiling point lower than 120K, although carbon dioxide and nitrous oxide have a boiling point higher than 120K, but are usually included in this type of cryogenic agent. The cryogenic agent that can be stored in storage component 107 can include any one of the following items: nitrogen, hydrogen, helium, argon, oxygen, liquefied natural gas (LNG), nitrous oxide and carbon dioxide. Although cryogenic agent can usually be a liquefied gas (which can also be referred to as a cryogenic liquid) lower than 120K, cryogenic agent can alternatively be a cryogenic gas that keeps lower than 120K but higher than the boiling point of cryogenic agent. Therefore, cryogenic agent can be referred to as a cryogenic substance (particularly relative to cryogenic liquid or cryogenic gas) in this article.

[0044] exist Figure 1 In the example shown, the cryogen storage part 107 includes a heating element 113. In other examples, the cryogen storage part 107 may be connected to a heating element alternatively. The heating element 113 may be configured to heat the cryogen storage part 107 to the boiling point of the cryogen stored in the cryogen storage part 107. For example, when the cryogen is nitrogen, the cryogen storage part 107 may be heated to the boiling point of nitrogen (about 78K or -196°C at atmospheric pressure), and the nitrogen is maintained at a cooling temperature. For example, the nitrogen may be kept "cooled" at a temperature in the range of -160°C to -60°C. For example, the nitrogen may be cooled to -120°C. The temperature may be selected based on the type of hardware used in the system.

[0045] Cold nitrogen gas may flow through one or more refrigerant conduits 106 to cool surfaces in the cryogenic cleaning device 104, which is configured to accumulate gas molecules received into the body 103 via the fluid path 105 by condensing and / or adsorbing the gas molecules on the surfaces when cooled. In other words, the gas molecules are deposited on the cooled surfaces. Since the gas molecules may condense on the surfaces (i.e., may form droplets), the deposited gas molecules may be referred to as liquid molecules or simply "molecules".

[0046] The cryogenic cleaner 104 also includes a pump configured to pump out the accumulated gas molecules during bakeout of the cryogenic cleaner. Figure 1In the illustrated example, the pump includes a vacuum pump 108 (or a series of vacuum pumps) configured to create a vacuum in the vacuum chamber 102 of the analytical instrument 120. The vacuum pump 108 may be connected to the main body 103 via a valve 110. The vacuum pump 108 may include a vacuum pump with a gas delivery function (e.g., a turbomolecular pump, a vortex pump, an oil diffusion pump, etc.) or a vacuum pump with a gas entrapment function (e.g., an ion getter pump, a cryogenic pump, etc.), or other vacuum pumps configured to create a vacuum. It should be understood that in other examples, the pump of the cryogenic cleaner 104 may be a non-vacuum pump and / or may be a different pump from the pump configured to create a vacuum in the vacuum chamber 102 (although the pump may still be a pump of the analytical instrument 120).

[0047] The cryogenic cleaning device 104 may be or include any device capable of capturing water discharged from the vacuum chamber. For example, the cryogenic cleaning device 104 may include a cryogenic stage (or cold stage) configured to capture water. In some analytical instrument applications (e.g., cryogenic SEM applications), a cold stage may be used to cool a portion of the analytical instrument (e.g., a vacuum chamber). This may cause water to be trapped in the analytical instrument because the water is frozen by the low temperature of the cryogenic stage (cryo-stage) and therefore cannot be discharged. This may cause ice to form inside or on the surface of the sample, which is not ideal. However, by using a cold stage as a cryogenic cleaning device (outside the vacuum chamber of the analytical instrument), this water capture capability can be utilized to clean the vacuum chamber. That is, even in applications that do not utilize low temperatures, a cold stage may also be present in the system.

[0048] In some examples, the cold stage can be removably connected to the analytical instrument 120 or the cryogenic cleaning device 104. The cold stage can include one or more conduits or channels to allow cryogenic substances to flow within the cold stage to achieve cryogenic cooling. The cold stage can include a cold finger (a piece of equipment configured to create a local cold surface and a type of cold trap) and a sample holder.

[0049] Cold stages can be used for cryo-SEM applications (also known as cryogenic scanning electron microscopy). Cryogenic SEM (cryo-SEM) can allow analysis of materials that are not normally possible using conventional SEM methods (e.g., due to conventional preparation techniques such as critical point drying). For example, liquids, biological materials, and "wet" foods can be analyzed using cryo-SEM. In addition, cryo-SEM allows cold fracture of samples to reveal internal microstructures that may not be visible using conventional SEM methods.

[0050] Additionally or alternatively, the cryogenic cleaning device 104 may include a cold trap. A cold trap or a cryogenic stage may be sufficiently effective to clean the vacuum chamber alone, but a combination of the two may achieve more effective cleaning. For example, if the vacuum chamber is already filled with contaminants such as water, providing both a cold trap and a cryogenic stage may be useful.

[0051] In some examples, a cold trap can be removably connected to the cryogenic cleaning device 104. A cold trap is a device configured to condense vapor into a liquid or solid, and is typically used to prevent vapors exhausted from an experiment from entering a vacuum pump, where they might otherwise condense and contaminate the vacuum pump. Similar to a cold stage, a cold trap can be used in a cryogenic SEM. However, a cold trap can be present in a system even when a cryogenic SEM is not in use. For example, placing a cold trap near a cryogenic cleaner can enhance the cleaning capabilities of the cryogenic cleaner. Thus, a system device that connects a cold trap to a cryogenic cleaner can increase the speed and efficiency of the cryogenic cleaner.

[0052] Additionally or alternatively, the purification device 104 may include a cryogenic transfer system for transferring samples or specimens between sample preparation stations at low temperatures. When transferred to the vacuum chamber of the analytical instrument, the cryogenic transfer system can prevent or reduce chemical or morphological changes or destruction of samples (e.g., samples sensitive to the environment or heat) by utilizing temperature control and / or operating at low temperatures. The cryogenic transfer system includes components that allow the transfer system to operate at low temperatures, which can also be used for low-temperature cleaning vacuum chambers and can be conveniently used as a cryogenic purification device. For example, one or more refrigerant pipelines that provide low temperatures for sample transfer can also be used for surfaces in a cryogenic cooling system. In other words, the purification device 104 can be a cryogenic transfer system.

[0053] Figure 1 The illustrated analytical instrument 120 includes a particle beam source 114 directed to a sample 112 in a vacuum chamber 102. The vacuum chamber can be configured to operate under low vacuum (also referred to as rough vacuum), medium vacuum (also referred to as fine vacuum), high vacuum or UHV conditions. Operating the chamber 102 under high vacuum conditions may mean that molecules may not have a high probability of colliding with other molecules, and thus a (substantially) directed molecular beam may be formed. This may be useful for particle beam applications. However, lower vacuum conditions (e.g., medium and low vacuum conditions) may be useful in SEM devices, for example, because lower vacuum operation may reduce many sample preparations required for high vacuum operation.

[0054] The cryogenic cleaning device 104 may be configured to reduce contamination in the vacuum chamber so that the vacuum chamber is configured to operate under a specific vacuum state. For example, the cryogenic cleaning device 104 may be configured to reduce contamination in the vacuum chamber so that the vacuum chamber may operate under a high vacuum or higher vacuum. High vacuum may be comparable to 1×10 -6 Pa to 0.1Pa (1×10 -8 mbar to 1×10 -3 mbar), and ultra-high vacuum can correspond to 1×10 -9 Pa to 1×10 -6 Pa(1×10 -11 mbar to 1×10- 8 mbar) range, as defined in ISO 3529-1:2019. Rough vacuum can correspond to 0.1 Pa to 100 Pa (1×10 -3 mbar to 1 mbar), while a fine vacuum may correspond to a pressure in the range of 100 Pa (1 mbar) to the prevailing atmospheric pressure (approximately 31 KPa to 110 KPa, or 310 mbar to 1100 mbar), as also defined in ISO 3529-1:2019. However, it should be understood that other pressure ranges may be used, as the pressure range corresponding to a particular vacuum condition may depend on various factors, such as the size of the vacuum chamber 102, the temperature within the vacuum chamber 102, and the molecular species within the vacuum chamber 102. For molecules with a larger collision cross section, the pressure in the vacuum chamber 102 may need to be lower than 10 -3 mbar to avoid or substantially reduce collisions. Larger volumes of vacuum chamber 102 may also require less than 10 -3 mbar to substantially reduce collisions. Preferably, the pressure range corresponds to operating the vacuum chamber under high vacuum or ultra-high vacuum.

[0055] The presence of molecular flow (and therefore high or ultra-high vacuum conditions) can be determined in a direct and empirically verifiable manner by the Knudsen number. The Knudsen number is a dimensionless number defined as Where λ is the mean free path, and L corresponds to a physical length, which may be the length of the vacuum chamber in one dimension. When the Knudsen number is greater than 0.5, the probability of molecular collision may be low or substantially zero, such that the molecular flow may correspond to high vacuum conditions. In some examples, the Knudsen number may be greater than or equal to 1. In other examples, the Knudsen number may be greater than or equal to ten to further reduce the likelihood of molecular collisions. Thus, the molecules may be in a free molecular flow.

[0056] The particle beam source 114 may include an electron source, an ion source, an X-ray source or other sources. Therefore, the analytical instrument 120 may be or include a particle beam device. For example, the analytical instrument 120 may be or include a scanning electron microscope (SEM) device, a focused ion beam (FIB) device, an X-ray photoelectron spectroscopy (XPS) device, a transmission electron microscope (TEM) device or other particle beam device devices. In the SEM device, a focused electron beam can be used to image the sample 112 in the vacuum chamber 102 by detecting the reflected or backscattered electrons. Therefore, the SEM system can provide information about the surface and composition of the sample 112. The FIB device is a similar scientific instrument setting, but a focused ion beam is used instead of an electron. In the XPS device, an X-ray beam is used to irradiate the sample 112 in the vacuum chamber to obtain an electron population spectrum. The vacuum chamber in the XPS device may preferably be operated under UHV. In the TEM device, a focused electron beam can be used to image the sample 112 in the vacuum chamber 102 by detecting the electrons transmitted through the sample 112. Thus, the TEM system can provide information about the internal structure of the sample 112, such as crystal structure, morphology, and stress state information.

[0057] In some examples, analytical instrument 120 may include more than one particle beam device arrangement, such as in a focused ion beam scanning electron microscope (FIB-SEM). A FIB-SEM arrangement may allow sample 112 to be studied using one or both of the particle beams.

[0058] Each component can be controlled by a controller (not shown). The controller may include a computer that acts as a data processor for receiving data from a detector (e.g., an X-ray detector, a secondary electron detector, a secondary ion detector, etc.). The data may represent the distribution and abundance of elements in the sample and / or the chemical state of the elements. The computer may also be used as a data processor for processing data to provide an image of the sample. The controller may also include a display and a user input device so that the user can view and enter or select information. The user input device may include a keyboard and / or a mouse.

[0059] refer to Figure 2 , another example system 200 is shown including a cryogenic cleaning device 204 and an analytical instrument 220, the analytical instrument including a vacuum chamber 202 connected to the cryogenic cleaning device 204. An optional additional cryogenic cleaning device 204a is illustrated, as will be discussed in further detail below, and it should be understood that other cryogenic cleaning devices may also be included in the system 200. Thus, the system 200 may include one or more cleaning devices 104, 204. The system 200 may also include a controller (not shown) configured to operate the cleaning device 204 and / or the analytical instrument 220 according to the methods disclosed herein.

[0060] System 200 is similar in many respects to the above referenced Figure 1 The system 100 described is similar. For example, the cryo-cleaner 204 includes a valve 201, which may preferably be a gate valve, to allow a fluid path 205 (e.g., which may be provided by a channel or pipe) between the cryo-cleaner 204 and the vacuum chamber 202 to be closed to prevent gas molecules from being received into the cryo-cleaner body 203. A gate valve is a valve that is opened by lifting or moving a barrier out of the fluid path.

[0061] Low temperature cleaner 204 also includes a single stage refrigeration system. Figure 2 In the illustrated example, the single-stage refrigeration system includes a cryogen storage component 207 disposed within the body 203 of the cryogenic cleaning device 204. Figure 1 As discussed, the cryogenic storage component 207 may be a cryogenic storage dewar (or dewar container), a cryogenic storage cylinder, or a cryogenic storage tank. The cryogenic substances that may be stored in the storage component 207 may include any of the following: nitrogen, hydrogen, helium, argon, oxygen, LNG, nitrous oxide, and carbon dioxide.

[0062] In the cryogenic cleaning device 204, the cryogenic storage component 207 is a container surrounded by the main body 203 of the cryogenic cleaning device 204. The space between the cryogenic storage component 207 and the main body 203 is evacuated, which can be achieved by the pump 208 of the analytical instrument 220. The cryogenic storage component 207 is then filled with a cryogenic substance (e.g., liquid nitrogen) and sealed. In this example, the cryogenic substance does not flow in the main body 203, but is stationary.

[0063] The cryogenic storage component 207 may include a closable hole for refilling the cryogenic storage component 207 with a cryogenic substance. The cryogenic storage component 207 may be removed from the cryogenic cleaning device 204, for example, to allow the removal of condensed contaminants. In a typical cryogenic cleaning device, removing the cryogenic storage component may require opening the vacuum chamber to ambient air and then placing a cover on the body to seal the vacuum chamber. This may introduce contaminants into the vacuum chamber and increase the pressure in the vacuum chamber (reduce the vacuum level) before the vacuum chamber is sealed again. In contrast, since the cryogenic cleaning device 204 disclosed in the present invention includes a valve 201 that can be used to close the fluid path 205 between the cryogenic cleaning device 204 and the analytical instrument 220, removing the cryogenic storage component may not result in a loss (or reduction) of vacuum or the introduction of contaminants into the vacuum. In some examples, the cryogenic cleaning device 104, 204 may be removable (rather than the specific cryogenic storage component 207).

[0064] Since the cryogenic storage components in this example are disposed within the body of the cryogenic cleaning device 204, the size of the cryogenic cleaning device 204 can be reduced compared to other cryogenic cleaning devices (because, for example, the cryogenic cleaning device 204 does not need to include one or more refrigerant pipes). Therefore, a smaller volume cryogenic cleaning device can be used with the analytical instrument while still substantially reducing contamination in the vacuum chamber of the analytical instrument 220. Therefore, the gas path 205 can be shorter than in other embodiments to reduce the overall system size.

[0065] exist Figure 2 In the illustrated example, the low temperature cleaning device 204 does not include a baking device or component. Instead, the system 200 may also include a baking device for use with the low temperature cleaning device 204. Figure 1 As described, the equipment for baking cleaning device 204 may include a heating element. For example, the baking equipment may include an infrared lamp, an oven, a flexible heating material, or a heating cable. In other examples, the low temperature cleaning device 204 may include an integrated baking component, such as an integrated heating element.

[0066] The system 200 also includes a pump configured to pump out the accumulated gas molecules during baking of the low temperature cleaning device. Figure 2 In the illustrated example, the pump includes a vacuum pump 208 configured to create a vacuum in a vacuum chamber 202 of an analytical instrument 220. Optionally, the vacuum pump 208 can be connected to the cryogenic cleaning device 204 via a fluid path 218. Thus, the vacuum pump 208 can be configured to evacuate the volume of the cryogenic cleaning device 204 (e.g., during a bakeout). As described herein, during such a bakeout, the fluid path 205 can be closed using a valve 201 (which can be, for example, a gate valve). It should be understood that in other examples, the pump can be a non-vacuum pump and / or can be a different pump than the pump 208 of the analytical instrument 220, which is configured to create a vacuum in the vacuum chamber 202.

[0067] Figure 2 The illustrated analytical instrument 220 includes a particle beam source 214 directed toward a sample 212 in a vacuum chamber 202. The particle beam source 214 may be as described with reference to Figure 1 As described. For example, particle beam source 214 can be an electron, ion or X-ray source, and analysis instrument 220 can be or include a scanning electron microscope (SEM) device, a focused ion beam (FIB) device or an X-ray photoelectron spectroscopy (XPS) device accordingly. In some examples, particle beam source 214 can include more than one source, such as in a focused ion beam scanning electron microscope (FIB-SEM) device.

[0068] As described above, the system may include additional devices 204a for reducing contamination. Figure 2The additional device 204a is illustrated as being of the same device type as the low temperature cleaning device 204. Thus, the additional device 204a may have the same components or similar types of components as the low temperature cleaning device 204 and may be attached to the analytical instrument 220 in the same or similar manner. In other examples, the additional device 204a may be a different type of cleaning device. For example, the reference Figure 1 In another example, a cryopump may be attached to the analytical instrument 220. In other words, where the system includes more than one purification device 204, each purification device 204 may be of the same type, or some or all purification devices 204 may be of different types.

[0069] Including two or more purge units in the system can further increase the throughput of the experiment or reduce contamination in the vacuum chamber. For example, while a single purge unit allows for more regular cleaning of the vacuum chamber without loss of vacuum conditions (e.g., Figure 3 Further discussed), but it may still take some time to clean the purge. By using two or more purges, at least one of which includes a valve, one purge can remain operational and connected to the vacuum chamber to reduce contamination in the chamber while the other purge is baked out and evacuated.

[0070] refer to Figure 3 , a flow chart showing a method for reducing contamination in a vacuum chamber of an analytical instrument. The method can be implemented in any system or device discussed herein.

[0071] In step 301, a surface in a body of a cryogenic cleaning device is cooled using a single-stage refrigeration system. The cooling of the surface causes gas molecules received into the body via a closable gas path to accumulate on the cooled surface via condensation and / or adsorption. In conventional cryogenic cleaning devices, it may take more than five hours (typically about ten hours) for enough molecules to accumulate on the surface to sufficiently reduce contamination in a vacuum chamber. However, according to the devices and systems described herein, the duration of step 301 may be less than ten hours or less than five hours to sufficiently reduce contamination in a vacuum chamber.

[0072] After a large number of gas molecules have accumulated on the cooling surface, the fluid path is closed in step 302 to prevent more gas molecules from being received into the body. The fluid path can be closed by using a valve configured to block the fluid path. The valve can be a gate valve, a ball valve, a butterfly valve, a plug valve, or other type of valve. In some examples, the valve can include a series of valves, and one or more of the series of valves can be closed. In the case where the valve includes a series of valves, some or all of the series of valves can be different types of valves.

[0073] At step 303, after closing the fluid path, the low temperature cleaning device is baked. Baking the device may include heating the device to a temperature of 80°C or higher. For example, the device (or a portion of the device, such as a low temperature storage component) may be heated to a temperature in the range of 90°C to 120°C. The device may be baked for at least several minutes (e.g., at least two minutes, at least five minutes, at least ten minutes, at least twenty minutes, or longer). The device may typically be baked for about two hours.

[0074] At step 304, the low temperature cleaning device is evacuated to remove gas molecules from the low temperature cleaning device that have accumulated on the cooling surface. Evacuating the cleaning device may occur during the bakeout or may occur after the bakeout.

[0075] After the low temperature cleaning device is evacuated, the fluid path can be opened to allow more gas molecules to accumulate in the low temperature cleaning device. For example, when the low temperature cleaning device is newly cleaned (deposited contaminants have been removed) and has been cooled down to low temperature again, the fluid path can be opened. The fluid path can be opened by opening or moving a valve.

[0076] Therefore, after step 304, the method can return to step 301 to repeat steps 301-304. According to the device and system described herein, the cleaning cycle (steps 301-304) can be performed more regularly than using a conventional cleaning device, and this can be performed without destroying the vacuum conditions in the vacuum chamber. For example, the cleaning cycle can be performed less than once every fifteen hours. More specifically, the cleaning cycle can be performed once every hour, every five hours, or every ten hours, for example. In other examples, the cleaning cycle can be performed more regularly. In short, the device and system described herein can allow continuous, pseudo-continuous or nearly continuous cleaning of the vacuum chamber because the fluid path can be closed at any time without destroying the vacuum of the vacuum chamber. Since the closed gas path allows the vacuum in the vacuum chamber to be maintained, the analytical instrument can continue to operate when the fluid path is closed. Therefore, the throughput of experiments or imaging can be improved.

[0077] Figure 4 A schematic diagram of a system 400 including a cryogenic cleaning device 404 and an analytical instrument 420 having a vacuum chamber 402 is illustrated. Figure 4 The system 400 illustrated in FIG. 1 is similar in many respects to Figure 1 and Figure 2 Even without reference to Figure 4 Clear description of Figure 1 and Figure 2 Any of the components and / or configurations discussed may exist in Figure 4In the illustrated embodiment, for example, the analytical instrument 420 includes a particle beam source 414, which may include any one or more of the particle beam sources discussed herein or other particle beam sources.

[0078] exist Figure 4 In the illustrated system 400, the low temperature cleaning device 404 includes a heating element 416 for baking the low temperature cleaning device. The heating element 416 can be arranged in the bakeable volume of the low temperature cleaning device 404, such as Figure 4 As shown, or may be connected to the body 403 of the low temperature cleaning device 404 but external thereto. It should be understood that in other examples, the heating element 416 may not be present in or connected to the low temperature cleaning device 404, and a separate baking device may be used to bake the cleaning device 404.

[0079] The cryogenic cleaning device 404 further comprises a cold stage 419 connected to a cryogenic storage component (not shown) arranged outside the body 403 of the cryogenic cleaning device 404 via two refrigerant pipes 406. In other examples, a different number of refrigerant pipes may be provided.

[0080] exist Figure 4 , the low temperature cleaning device 404 is connected to a vacuum pump 408, which is configured to generate a vacuum in the chamber 402 via a fluid channel 418. Figure 2 As discussed, vacuum pump 408 can be configured to evacuate the volume of cryogenic cleaning device 404, for example, during bakeout. Fluid passage 418 can be closed via valve 410. In other examples, another pump of the analytical instrument or a separate pump can be configured to evacuate the volume of cryogenic cleaning device 404 during bakeout.

[0081] The system 400 includes an accessory 422 that provides a fluid path 405 between the cryogenic cleaning device and the analytical instrument 420 via a conduit or channel, and the fluid path 405 can be closed via a gate valve 401. The accessory 422 can also allow a cryogenic stage (or cold stage) and / or a cold trap to be connected to or inserted into the analytical instrument 420. In some examples, the cold trap and / or cold stage can be retractably attached to the analytical instrument 420, as shown in FIG. FIG. 5A to FIG. 5C discussed.

[0082] The use of a cold trap in combination with a cryogenic cleaning device can improve the ability of the cryogenic cleaner to discharge water vapor or other contaminants from the vacuum chamber. However, the cold trap may not always be in use (e.g., when the cryogenic SEM is not in use). When not in use, the cold trap may take up space that can be used for other equipment. In addition, the cold trap may not be bakeable, which may prevent the cryogenic cleaner from being baked, or at least make baking the cryogenic cleaner more difficult, time-consuming and / or expensive. For example, additional equipment may be required, the cryogenic cleaner may need to be redesigned, or only certain types of cryogenic cleaners may be able to be baked. Therefore, it is useful to be able to detachably connect the cold trap to the cryogenic cleaning device.

[0083] Figure 5A , Figure 5B and Figure 5C A schematic diagram of a system 500 including a cryogenic cleaning device 504 and an analytical instrument 520 having a vacuum chamber 502 is shown, illustrating a removable connector 524 for removably connecting a cold stage and / or cold trap to the vacuum chamber 502. The cold stage and / or cold trap may be connected to the vacuum chamber 502 in one of a variety of ways.

[0084] Figure 5A A cryogenic cleaning device 504 is illustrated that includes a cold trap 526. The cold trap 526 in this example is disposed within the body 503 of the cryogenic cleaning device 504, but in other examples the cold trap 526 may be connected to the cryogenic cleaning device 504 but located outside the body 503. The cold trap 526 includes a detachable connector 524.

[0085] Figure 5A The cold trap 526 is illustrated when the removable connector 524 has been inserted into the analytical instrument 520. Inserting the removable connector 524 into the analytical instrument 520 may include attaching the removable connector 524 to the analytical instrument 520 or a component of the analytical instrument (e.g., the vacuum chamber 502). The removable connector 524 may be inserted into the analytical instrument 520 during cleaning (i.e., when a cryo cleaner is operating to remove or reduce contamination in the vacuum chamber of the analytical instrument 520).

[0086] Figure 5B The detachable connector 524 is shown when separated or disconnected from the analytical instrument 520. The detachable connector 524 can be separated from the vacuum chamber during baking and / or evacuation of the low-temperature cleaning device 504. In the case where the cold stage remains arranged in the low-temperature cleaning device 504 when separated from the vacuum chamber, the cold stage can therefore be baked and / or evacuated when the low-temperature cleaning device is baked and / or evacuated after closing the gate valve 501. Therefore, contamination in the cold stage (or cold trap) can be removed in a direct manner.

[0087] exist Figure 5BIn the exemplary system shown, the removable connector 524 is retracted to separate the removable connector 524 from the analytical instrument 520 (and thus may also be referred to as a retractable connector 524). In other examples, the cold stage (or cold trap) may be movable to separate the cold stage from the vacuum chamber of the analytical instrument (although the cryogenic cleaning device may remain attached to the analytical instrument). Figure 5C One such exemplary embodiment is shown. In either of these cases, the cold stage can remain disposed within the cryogenic cleaning apparatus 504 when separated from the vacuum chamber. In another example, the cold stage (or cold trap) can be movable to separate the cold stage from the cryogenic cleaning apparatus. In these examples, the removable connector 524 may still be present, but it may not be retractable.

[0088] like Figure 5B As shown, the retractable connector 524 can be at least partially accommodated in the attachment part 522 when retracted, which provides a fluid path 505 between the low-temperature cleaning device and the analytical instrument 520. A valve 501 for closing the fluid path 505 can be provided in the attachment 522, so that when the retractable connector 524 is retracted and at least partially accommodated in the attachment 522, the valve 501 is closable.

[0089] When the retractable connector 524 is partially contained within the attachment member 522, the retractable connector 524 can also be at least partially contained within the body 503 of the cleaning device 504. In some examples, the size of the attachment member 522 can be designed so that the retractable connector 524 can be completely contained within the attachment member 522 when not in use. In other examples, the retractable connector can be completely contained within the body 503.

[0090] As reference Figure 2 and Figure 4 As discussed, the cryogenic cleaning device 504 is connected to a vacuum pump 508, which is configured to create a vacuum in the chamber 502 via a fluid channel or path 518. The fluid path 518 can be closed via a valve 510. In some examples, the cryogenic cleaning device 504 can be connected to the vacuum pump 508 via an attachment member 522, which can include one or more holes for connecting to a (vacuum) pump. In some examples, the fluid path 518 may not be present, and a separate (vacuum) pump may be connected to the cryogenic cleaning device 504, for example, via one or more holes of the attachment member 522.

[0091] Figure 5C An exemplary embodiment is illustrated in which the cold stage 526 is movable to separate the removable connector 524 from the vacuum chamber 502. Figure 5C , the cold stage 526 is in the retracted position (where Figure 5AExample attachment locations are illustrated).

[0092] Standard cryopumps cannot be connected to cold traps, and this is particularly true for removable cold traps. To enable a cryopump to be connected to a cold trap would require extensive and expensive hardware redesign. Since many analytical instrumentation applications do not require the extremely low temperatures provided by cryopumps, and cryopumps may be disadvantageous to use for the reasons discussed herein (e.g., their large size, their operation causing vibrations, etc.), it may be advantageous to provide a single-stage refrigeration cryogenic cleaning device that can be attached to a cold trap.

[0093] although FIG. 5A to FIG. 5C 526 is described with reference to a cold stage 526 including a retractable connector 524, wherein the cold stage 526 is optionally removable, but it should be understood that, in addition or alternatively, the cold trap 519 may include a removable and / or retractable connector and may optionally be removable. In these examples, the cold stage 526 may not be present (e.g., as Figure 4 as exemplified in ).

[0094] FIG. 5A to FIG. 5C The system illustrated in FIG. 1 can be compared in many respects to the system illustrated in FIG. Figure 1 , Figure 2 and Figure 4 Even if not explicitly described, Figure 1 , Figure 2 and Figure 4 Any of the components and / or configurations discussed may exist in FIG. 5A to FIG. 5C In the illustrated embodiment.

[0095] The methods described herein may be implemented using computer system configurations including handheld devices, microprocessor systems, microprocessor-based or programmable consumer electronics, minicomputers, mainframe computers, etc. The embodiments may also be practiced in distributed computing environments where tasks are performed by remote processing devices linked through a network.

[0096] The computer system may include a processor, such as a central processing unit (CPU). The processor may execute logic in the form of a software program. The computer system may include a memory including volatile and non-volatile storage media. Different parts of the system may be connected using a network (e.g., a wireless network and a wired network). The computer system may include one or more interfaces. For example, the computer may contain a suitable operating system, such as, for example, UNIX (including Linux) or Windows (RTM).

[0097] Certain embodiments may also be implemented as computer-readable code on a non-transitory computer-readable medium. A computer-readable medium may be any data storage device that can store data that can be read thereafter by a computer system. Examples of computer-readable media include hard drives, network attached storage (NAS), read-only memory, random access memory, CD-ROM, CD-R, CD-RW, magnetic tape, and other optical and non-optical data storage devices. Computer-readable media may also be distributed on a network-coupled computer system so that the computer-readable code is stored and executed in a distributed manner. Although embodiments according to the present disclosure have been described with reference to specific types of devices and applications (specifically mass spectrometers) and the embodiments have specific advantages in this case, as discussed herein, methods according to the present disclosure may be applied to other types of devices and / or applications. The specific calibration details of a cryogenic cleaning device and / or system are not only potentially advantageous (particularly in view of known calibration constraints and capabilities), but may also be significantly varied to obtain a device with similar or identical operation. Unless otherwise stated, each feature disclosed in this specification may be replaced with an alternative feature for the same, equivalent, or similar purpose. Therefore, unless otherwise stated, each feature disclosed is only an example of a series of equivalent or similar attribute features.

[0098] All aspects and / or features disclosed in this specification may be combined in any combination, except for combinations in which at least some of such features and / or steps are mutually exclusive. Specifically, the preferred features of the present disclosure are applicable to all aspects and embodiments of the present disclosure and may be used in any combination. For example, a system including a cryocleaner and an analytical instrument with a vacuum chamber may include any one or more cryocleaners and / or analytical instruments described herein. Similarly, the features described in the non-essential combination may be used alone (rather than in combination). It should be understood that there is an implicit "about" before the temperature, concentration, time, pressure, flow rate, cross-sectional area, voltage, current, etc. discussed in the present teaching content, so that there is a slight and non-substantial deviation within the scope of the present teaching content. In addition, the value referred to as "equal" may actually differ by less than a threshold amount. For example, the threshold amount may be 5%. Depending on the context, the threshold may also be greater than 5% (e.g., 10%, 20% or 50%) or less than 5% (e.g., 2% or 1%).

[0099] As used herein, including in the claims, unless the context indicates otherwise, the singular forms of the terms herein should be interpreted as including the plural forms, and vice versa. For example, unless the context indicates otherwise, singular references such as "a", "an" (such as, a purification device) herein (including in the claims) mean "one or more" (e.g., one or more purification devices).

[0100] In the specification and claims of the present disclosure, the words "comprise", "include", "have" and "contain" and variations of these words, for example, "include" and "includes" or similar words mean "including but not limited to", and are not intended to (and do not) exclude other components. In addition, the use of "or" is inclusive, such that the phrase "A or B" is true when "A" is true, "B" is true, or both "A" and "B" are true. In addition, the use of terms in brackets (terms in brackets) can be inclusive, such as the phrase "(C)D" is true when "D" is true, or both "C" and "D" are true. For example, the term "(vacuum) pump" can mean "vacuum pump" or "pump". In other cases, the use of a term in brackets can indicate optional language in the term, such that the phrase "(C)D" can mean that a certain element can be referred to as "D" or "(C)D". For example, the term "(low temperature) cleaning device" can mean that the component can be referred to as "low temperature cleaning device" or "cleaning device" in this article.

[0101] The use of any and all examples or exemplary language ("for example," "such as," and similar language) provided herein is intended to better illustrate the present disclosure only and does not indicate a limitation on the scope of the present disclosure unless otherwise required. No language in this specification should be construed as indicating any non-claimed element necessary to practice the present disclosure.

[0102] The terms "first" and "second" may be reversed without changing the scope of the invention. That is, an element referred to as a "first" element (e.g., a first position) may alternatively be referred to as a "second" element (e.g., a second position), and an element referred to as a "second" element (e.g., a second position) may alternatively be considered a "first" element (e.g., a first position).

[0103] Unless otherwise specified or the context requires otherwise, any steps described in this specification may be performed in any order or simultaneously. In addition, where a step is described as being performed after a step, this does not exclude intermediate steps being performed.

[0104] It should also be understood that, unless otherwise implicitly or explicitly understood or stated, for any given component or embodiment described herein, any possible candidate or alternative listed for that component may generally be used alone or in combination with each other. It should be understood that any list of such candidates or alternatives is merely illustrative and not restrictive, unless otherwise implicitly or explicitly understood or stated.

[0105] In the detailed description of various embodiments, for the purpose of explanation, many specific details are set forth to provide a thorough understanding of the disclosed embodiments. However, those skilled in the art will appreciate that these various embodiments may be practiced with or without these specific details. Furthermore, those skilled in the art can readily appreciate that the specific order in which the methods are presented and executed is illustrative, and it is contemplated that the order may be changed and still remain within the scope of the various embodiments disclosed herein.

[0106] All literature and similar materials cited in this application, including but not limited to patents, patent applications, papers, books, monographs and internet web pages, are expressly incorporated in their entirety by reference for any purpose. Unless otherwise defined, all technical and scientific terms used herein have the meaning commonly understood by one of ordinary skill in the art to which the various embodiments described herein belong.

Claims

1. A low temperature cleaning device, comprising: a body and an attachment element for attaching the body to a vacuum chamber of an analytical instrument to provide a fluid path between the body and the vacuum chamber; a surface configured to accumulate gas molecules received into the body via the fluid path by condensing and / or adsorbing the gas molecules on the surface when cooled; a single-stage refrigeration system configured to cool the surface; a pump configured to pump out accumulated gas molecules during bakeout of the cryogenic cleaning device; and A valve is movable between a first position in which the fluid path is open to allow the gas molecules to be exhausted from the vacuum chamber into the body and a second position in which the fluid path is closed to prevent the gas molecules from being received into the body. 2 . The low-temperature cleaning device according to claim 1 , wherein the valve comprises one or more of the following: a gate valve, a ball valve, a butterfly valve and a plug valve.

3. The low-temperature cleaning device according to claim 1, wherein the single-stage refrigeration system includes a refrigerant storage component arranged in the main body, or the single-stage refrigeration system includes a refrigerant storage component arranged outside the main body and one or more refrigerant pipes at least partially arranged in the main body and connected to the refrigerant storage component.

4. The low temperature cleaning apparatus according to claim 3, wherein the cryogen storage component comprises a cryogen selected from the group consisting of nitrogen, hydrogen, helium, argon, oxygen, liquefied natural gas (LNG), nitrous oxide, and carbon dioxide. 5 . The low-temperature cleaning device according to claim 1 , wherein the low-temperature cleaning device comprises a cold stage, a cold trap, a low-temperature storage device and / or a low-temperature transfer system. The low temperature cleaning device of claim 1 , wherein the gas molecules include water molecules.

7. The cryogenic cleaning apparatus of claim 1, wherein the analytical instrument comprises a particle beam device.

8. The cryogenic cleaning apparatus of claim 1, wherein the particle beam device comprises one or more of: a scanning electron microscope (SEM) apparatus, a focused ion beam (FIB) apparatus, an X-ray photoelectron spectroscopy (XPS) apparatus, and a transmission electron microscope (TEM) apparatus.

9. The cryogenic cleaning apparatus of claim 1, wherein the cryogenic cleaning apparatus is configured to reduce contamination in the vacuum chamber such that the vacuum chamber is configured to operate at a high vacuum or higher.

10. A system comprising one or more cryogenic cleaning devices according to claim 1 and an analytical instrument having a vacuum chamber connected to the one or more cryogenic cleaning devices.

11. The system of claim 10, wherein the analytical instrument comprises a particle beam device, the particle beam device comprising one or more of the following: a scanning electron microscope (SEM) device, a focused ion beam (FIB) device, an X-ray photoelectron spectroscopy (XPS) device, and a transmission electron microscope (TEM) device.

12. The system of claim 10, further comprising an apparatus configured to bake out the one or more low temperature cleaning devices.

13. The system of claim 12, wherein the device comprises one or more of: a resistive heating element, a radiant heating element, and a conductive heating element.

14. The system of claim 10, wherein the pump comprises a pump of the analytical instrument configured to create a vacuum in the vacuum chamber of the analytical instrument.

15. The system of claim 10, wherein the vacuum chamber is configured to operate at a high vacuum or higher.

16. The system of claim 10, further comprising a cold trap configured to be retractably attached to the vacuum chamber.

17. A method comprising the steps of: In a system including an analytical instrument and a cryogenic cleaning apparatus connected to a vacuum chamber of the analytical instrument via a closable fluid path, cooling a surface in a body of the cryogenic cleaning apparatus using a single-stage refrigeration system to accumulate gas molecules received into the body via the fluid path on the cooled surface via condensation and / or adsorption; After accumulating the gas molecules, closing the fluid path to prevent more gas molecules from being received into the body; as well as After closing the fluid path, the cryogenic cleaning device is baked out and evacuated to remove the gas molecules accumulated on the cooled surfaces from the cryogenic cleaning device.

18. The method according to claim 17, further comprising the steps of: A cold trap is removably connected to the vacuum chamber during cooling of the surface.

19. The method according to claim 17, further comprising the steps of: The cold trap is separated from the vacuum chamber during bakeout and evacuation of the low temperature cleaning device.

20. The method of claim 17, wherein the system further comprises at least one additional low temperature cleaning device connected to the vacuum chamber via an additional closable fluid path, wherein during baking out and pumping down the low temperature cleaning device, the method further comprises the steps of: An additional single-stage refrigeration component is used to cool surfaces in the body of the additional cryogenic cleaning device to accumulate gas molecules received into the body of the additional cryogenic cleaning device via the additional fluid path on the cooled surfaces via condensation and / or adsorption.