Ultrahigh vacuum rapid sampling device and method

Abstract

The invention discloses an ultrahigh vacuum rapid sample injection device and method, and belongs to the field of vacuum sample parking, the ultrahigh vacuum rapid sample injection device comprises a rapid sample injection chamber, and a first 100CF flange port, a second 100CF flange port, a third 100CF flange port, a first 63CF flange port, a first 35CF flange port, a second 35CF flange port and a second 63CF flange port which are arranged on the rapid sample injection chamber. According to the invention, the volume of the cavity is reduced; the operation is simple and convenient, the use experience of a user is good, automatic sample transfer can be upgraded, and butt joint of a glove transfer cavity / an ultrahigh vacuum transfer cavity can be compatible.

Description

Technical Field

[0001] The present invention relates to a sample injection device and method, and in particular to an ultra-high vacuum rapid sample injection device and method. Background Art

[0002] At present, the sample parking devices in the ultra-high vacuum field are relatively simple. Generally, they can only park 1 to 2 sample holders. They have a single function, are inconvenient to transfer samples, and the injection and sampling operations are relatively cumbersome, which greatly affects the efficiency of researchers in the ultra-high vacuum field to do experiments. The support structure of the parking platform is not reliable, and the parking platform material has serious outgassing, which affects the vacuum degree of the vacuum device. Summary of the Invention

[0003] In order to solve the above technical problems, the present invention provides an ultra-high vacuum rapid sampling device on the one hand, including a rapid sampling chamber, and a first 100CF flange port, a second 100CF flange port, a third 100CF flange port, a first 63CF flange port, a first 35CF flange port, a second 35CF flange port and a second 63CF flange port arranged on the rapid sampling chamber.

[0004] Furthermore, the rapid injection chamber is made of 304 stainless steel, and the cavity size is 108 mm in diameter and 225 mm in height.

[0005] Furthermore, the rapid injection chamber is a cylindrical cavity.

[0006] Furthermore, the internal volume of the rapid injection chamber is less than or equal to 1.2L, and a molecular pump with a pumping speed of 300L / s and a dry pump with a pumping speed of 15L are used to evacuate the rapid injection chamber to achieve a vacuum of 10 within 30 minutes. -6 The purpose of mbar.

[0007] Furthermore, a sample holder is provided on the second 100CF flange port, and the sample holder is connected to the magnetic coupling rotator.

[0008] Furthermore, in the cavity of the rapid sampling chamber, the sample holder adopts two silicon nitride bearings as rotation and axial support, and the ends of the sample holder are placed facing each other.

[0009] Furthermore, the sample holder storage rack is made of three stacked pieces of stainless steel.

[0010] Furthermore, a shutter with a glass observation window is provided on the first 63CF flange port; and observation windows are provided on the first 35CF flange port and the second 63CF flange port.

[0011] Another aspect of the present invention provides a method for using an ultra-high vacuum rapid sample introduction device, comprising the steps of:

[0012] S1: Preparation work before chamber degassing: confirm that the plug valve connecting the rapid injection chamber and the first 100CF flange port is closed; close the vacuum gauge connected to the second 35CF flange port; release the shutter buckle; turn off the pump group connected to the third 100CF flange port (3) until the molecular pump speed drops to 0rpm;

[0013] S2: Deflate the rapid injection chamber through the air inlet of the molecular pump until the shutter can be opened;

[0014] S3: Open the shutter, place the sample holder containing the sample on the sample holder, and close the shutter;

[0015] S4: Turn on the pump group to evacuate the fast injection chamber, and then turn on the vacuum gauge to check the vacuum degree;

[0016] S5: Wait until the vacuum degree is greater than 10 -8 mbar, open the valve between the fast sampling chamber and the UFO to transfer the sample into the UFO cavity.

[0017] In summary, the present invention has the following beneficial effects compared to the prior art:

[0018] The present invention reduces the volume of the cavity; is simple and convenient to operate, provides a good user experience, can be upgraded to automated sample transfer, and is compatible with glove transfer chamber / ultra-high vacuum transfer chamber docking. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] The drawings described herein are used to provide a further understanding of the present invention and constitute a part of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:

[0020] Figure 1 A schematic diagram of the overall structure of an ultra-high vacuum rapid sampling device provided by the present invention;

[0021] Figure 2 This is a top view of the ultra-high vacuum rapid sampling device;

[0022] Figure 3 It is a cross-sectional view of section AA;

[0023] Figure 4 This is a bottom view of the ultra-high vacuum rapid sampling device;

[0024] Figure 5 This is a side view of the ultra-high vacuum rapid sampling device;

[0025] Figure 6 This is a front view of the ultra-high vacuum rapid sampling device;

[0026] Figure 7Schematic diagram of the overall structure of the sample holder.

[0027] The above drawings include the following reference numerals:

[0028] 1. First 100CF flange port; 2. Second 100CF flange port; 3. Third 100CF flange port; 4. First 63CF flange port; 5. First 35CF flange port; 6. Second 35CF flange port; 7. Second 63CF flange port; 8. Molecular pump; 9. Sample holder; 10. Shutter; 11. First observation window; 12. Second observation window; 13. Third observation window. DETAILED DESCRIPTION

[0029] It should be noted that, in the absence of conflict, the embodiments and features of the embodiments of the present invention can be combined with each other. The present invention will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0030] It should be noted that the terms used herein are only for describing specific embodiments and are not intended to limit the exemplary embodiments according to the present invention. As used herein, unless the context clearly indicates otherwise, the singular form can also include the plural form. In addition, it should be understood that when the terms "comprise" and / or "include" are used in this specification, they indicate the presence of features, steps, operations, devices, components and / or combinations thereof.

[0031] Unless otherwise specifically stated, the relative arrangement of the parts and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention. At the same time, it should be understood that, for ease of description, the sizes of the various parts shown in the drawings are not drawn according to actual proportional relationships. The techniques, methods and equipment known to those of ordinary skill in the relevant art may not be discussed in detail, but where appropriate, the techniques, methods and equipment should be considered as part of the authorized specification. In all examples shown and discussed herein, any specific values should be interpreted as being merely exemplary and not as limitations. Therefore, other examples of the exemplary embodiments may have different values. It should be noted that similar numbers and letters represent similar items in the following figures, and therefore, once an item is defined in one figure, it does not need to be further discussed in subsequent figures.

[0032] See also Figures 1 to 7 As shown, the present invention provides an ultra-high vacuum rapid sampling device, comprising:

[0033] The sampling device body has a cavity inside, which is referred to as a rapid sampling chamber in the present invention;

[0034] The rapid injection chamber is constructed of 304 stainless steel and is a cylindrical chamber with a diameter of 108mm and a height of 225mm. The entire rapid injection chamber has an internal volume of less than 1.2L. It is evacuated using a 300L / s molecular pump 8 combined with a 15L dry pump, achieving a vacuum of 10-6 mbar within 30 minutes.

[0035] The main surface of the sampling device is provided with 7 CF flange ports connected to the rapid sampling chamber, namely: the first 100CF flange port 1, the second 100CF flange port 2, the third 100CF flange port 3, the first 63CF flange port 4, the first 35CF flange port 5, the second 35CF flange port 6 and the second 63CF flange port 7.

[0036] The function of the first 100CF flange port 1 is to connect the sample transfer chamber (UFO chamber) to realize the transfer of the sample holder between the two chambers;

[0037] The second 100CF flange port 2 provides support and placement for the sample holder 9 in the rapid sampling chamber;

[0038] The third 100CF flange port 3 is connected to the molecular pump 8 and combined with the front-stage dry pump to vacuum the interior of the fast injection chamber;

[0039] The first 63CF flange port 4 is connected to a "shutter 10" with a glass first observation window 11, which can realize sample loading after the cavity is deflated, and can also be connected to the sample transfer cavity to realize the transfer of samples without exposure to air;

[0040] The first 35CF flange port 5 is used to install the second observation window 12, which reserves another angle for observing the sample holder in the rapid injection chamber;

[0041] The second 35CF flange port 6 is used to connect a 35CF full-scale vacuum gauge.

[0042] The second 63CF flange opening 7 is used to accommodate a 63CF third observation window 13, which facilitates observation of the sample grabbing and transferring process.

[0043] like Figure 2As shown, by using a magnetic coupling rotator to connect the sample holder 9 structure in the rapid sampling chamber, the rotation of the sample holder in the rapid sampling chamber is realized, which meets the position adjustment requirements of the sample transfer structure in the UFO cavity for sample grabbing and transfer. In addition, by adding an external motor to control the rotation of the magnetic coupling rotator, the demand for automated sample transfer can be met. The sample holder 9 in the rapid sampling chamber adopts two silicon nitride bearings as rotation and axial support, and the end structure of the sample holder storage rack adopts a face-to-face placement design, which can meet the requirements of two sample holders for sampling at a time. Each sample holder storage rack adopts a three-piece stainless steel stacking design, which is convenient for material processing and easy for later maintenance; in addition, the back of the sample holder storage rack adopts a spring top bead lock-like structure design, so that the sample holder will not fall off due to the rotation of the sample holder. During the connection and debugging process between the rapid sampling chamber and the UFO cavity, the length of the four pillars connecting the sample holder structure and the top flange in the rapid sampling chamber can be adjusted (such as Figure 3 ), for a high degree of matching.

[0044] Another aspect of the present invention provides a method for using an ultra-high vacuum rapid sample introduction device, comprising the steps of:

[0045] S1: Preparations before chamber degassing: Confirm that the gate valve connecting the rapid injection chamber to the first 100CF flange port 1 is closed; close the vacuum gauge connected to the second 35CF flange port 6; release the shutter 10 buckle; turn off the pump group connected to the third 100CF flange port 3 until the molecular pump speed drops to 0 rpm;

[0046] S2: Deflate the rapid injection chamber through the air inlet of the molecular pump 8 until the shutter 10 can be opened;

[0047] S3: Open the shutter 10, place the sample holder containing the sample on the sample holder 9, and close the shutter 10;

[0048] S4: Turn on the pump group to evacuate the fast injection chamber, and then turn on the vacuum gauge to check the vacuum degree;

[0049] S5: Wait until the vacuum degree is greater than 10 -8 mbar, open the valve between the fast sampling chamber and the UFO to transfer the sample into the UFO cavity.

[0050] For ease of description, spatially relative terms such as "above", "above", "on the upper surface of", "above", etc. may be used herein to describe the spatial positional relationship of a device or feature to other devices or features as shown in the figures. It should be understood that spatially relative terms are intended to include different orientations of the device in use or operation in addition to the orientation described in the figures. For example, if the device in the drawings is inverted, the device described as "above other devices or structures" or "above other devices or structures" will be positioned as "below other devices or structures" or "below other devices or structures". Thus, the exemplary term "above" can include both "above" and "below". The device can also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatially relative descriptions used here are interpreted accordingly.

[0051] In addition, it should be noted that the use of terms such as "first" and "second" to limit components is only for the convenience of distinguishing the corresponding components. Unless otherwise stated, the above terms have no special meaning and therefore cannot be understood as limiting the scope of protection of the present invention.

[0052] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations of the present invention are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. An ultra-high vacuum rapid sample introduction device, characterized in that: The invention comprises a sampling device body, a rapid sampling chamber arranged inside the sampling device body, and a first 100CF flange opening (1), a second 100CF flange opening (2), a third 100CF flange opening (3), a first 63CF flange opening (4), a first 35CF flange opening (5), a second 35CF flange opening (6) and a second 63CF flange opening (7) arranged on the sampling device body.

2. The ultra-high vacuum rapid sample introduction device according to claim 1, characterized in that: The rapid injection chamber is made of 304 stainless steel, and the cavity size is 108 mm in diameter and 225 mm in height.

3. The ultra-high vacuum rapid sample introduction device according to claim 1, characterized in that: The interior of the rapid injection chamber is a cylindrical cavity.

4. The ultra-high vacuum rapid sample introduction device according to claim 3, characterized in that: The cylindrical cavity volume of the rapid injection chamber is less than or equal to 1.2L, and a molecular pump (8) with a pumping speed of 300L / s and a dry pump with a pumping speed of 15L are used to evacuate the rapid injection chamber to achieve a vacuum of 10 within 30 minutes. -6 The purpose of mbar.

5. The ultra-high vacuum rapid sample introduction device according to claim 3, characterized in that: A sample holder (9) is provided on the second 100CF flange port (2), and the sample holder (9) is connected to a magnetic coupling rotator.

6. The ultra-high vacuum rapid sample introduction device according to claim 5, characterized in that: In the cavity of the rapid sampling chamber, the sample holder (9) uses two silicon nitride bearings as rotation and axial support, and the ends of the sample holder are placed facing each other.

7. The ultra-high vacuum rapid sample introduction device according to claim 5, characterized in that: The sample holder is made of three pieces of stainless steel stacked together.

8. The ultra-high vacuum rapid sample introduction device according to claim 1, characterized in that: The first 63CF flange opening (4) is provided with a shutter (10) having a first glass observation window (11); the first 35CF flange opening (5) is provided with a second observation window (12); and the second 63CF flange opening (7) is provided with a third observation window (13).

9. A method for using an ultra-high vacuum rapid sampling device, characterized in that: Including steps: S1: Preparation work before chamber degassing: confirm that the plug valve connecting the rapid injection chamber to the first 100CF flange port (1) is closed; close the vacuum gauge connected to the second 35CF flange port (6); release the shutter (10) buckle; turn off the pump group connected to the third 100CF flange port (3) until the molecular pump speed drops to 0 rpm; S2: Deflate the rapid injection chamber through the air inlet of the molecular pump (8) until the shutter (10) can be opened; S3: Open the shutter (10), place the sample holder containing the sample on the sample holder (9), and close the shutter (10); S4: Turn on the pump group to evacuate the fast injection chamber, and then turn on the vacuum gauge to check the vacuum degree; S5: Wait until the vacuum degree is greater than 10 -8 mbar, open the valve between the fast sampling chamber and the UFO to transfer the sample into the UFO cavity.

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