Device and method for testing gas components of wide-temperature-range ultrahigh vacuum system

Abstract

The invention discloses a wide-temperature-range ultrahigh vacuum system gas component testing device and method, the device comprises an inner vacuum cavity, an outer vacuum cavity, a sample supporting plate, a quadrupole mass spectrometer, a vacuum system, a vacuum coupling sample transfer rod and a control device, the outer vacuum cavity is used for loading, unloading and transferring a sample, and the inner vacuum cavity is used for maintaining and testing the ultrahigh vacuum system. The vacuum system adopts a mechanical pump, a molecular pump, an ion pump and other multi-stage vacuum pumps to vacuumize, and adopts multiple groups of vacuum gauges to measure different vacuum degrees. A quadrupole mass spectrometer is adopted to analyze and detect gas components generated by the parts.

Description

Technical Field

[0001] The present invention relates to a gas component testing device and method for a wide-temperature ultra-high vacuum system, belonging to the field of non-destructive detection of gas content of parts with high-precision and high-stability requirements in aerospace equipment. Background Art

[0002] Space microwave components are widely used in satellite payload products such as antennas, and their quality and reliability have an important impact on the performance and on-orbit stable operation of the entire satellite. During the processes of material smelting, part machining, and surface treatment, gases such as hydrogen will be generated, and these gases will be stored in the base material or coating. In multiple processes of part surface treatment such as pickling, nickel plating, and gold plating, the generation and residue of hydrogen and water vapor are involved. These gases not only remain on the shell, but also penetrate into the metal coating. Excessive hydrogen content will cause "hydrogen poisoning" problems such as material deformation, performance degradation, and loss of original functions of the circuit in gallium arsenide chips. In addition, moisture will adsorb on the metal material of the parts, causing the material to absorb water and the metal electrode potential to change, resulting in the formation of a primary battery reaction in the device and causing electrochemical corrosion. The gases in these devices will directly affect the service performance and service life of the payload. Therefore, in the production of microwave devices, it is often necessary to analyze the gas components contained in the devices to ensure that no impurities such as hydrogen and water vapor are introduced into the electronic circuit packaging, so as not to affect the service life of the microwave devices.

[0003] In addition, after the shell plating layer undergoes degassing treatments such as normal pressure baking and vacuum dehydrogenation, most of the gases in the shell can be released, but there are still certain residual gases trapped inside the shell and difficult to discharge. During the subsequent service process of the product in orbit, affected by factors such as temperature changes, they will be slowly released, thus affecting the performance of sensitive chips and other devices. In order to analyze the changes of hydrogen and water vapor inside the microwave device under different baking processes, it is necessary to monitor the gas changes in the vacuum environment in real time, effectively analyze and judge the influence law of degassing, so as to obtain a reasonable degassing process. Currently, the main method for testing hydrogen in the shell plating layer and packaging components is the "small box method", in which the test sample is placed in a standard box body, sealed and after experiencing certain temperature and time conditions, the gas content in the box body is tested by a destructive method of puncture extraction. Summary of the Invention

[0004] The technical problem solved by the present invention is: aiming at the problem in the current existing technology that during the service process of the product in orbit, it is affected by factors such as temperature changes and affects the performance of sensitive chips and other devices, a gas component testing device and method for a wide-temperature ultra-high vacuum system are proposed.

[0005] The present invention solves the above technical problem through the following technical solutions:

[0006] A wide temperature range ultra-high vacuum system gas component testing device, comprising an inner vacuum chamber, an outer vacuum chamber, a sample support plate, a quadrupole mass spectrometer, a vacuum system, a vacuum coupling sample transfer rod, and a control device, wherein:

[0007] The outer vacuum chamber is arranged between the inner vacuum chamber and the atmospheric environment to provide an air pressure buffer space for the inner vacuum chamber. The outer vacuum chamber is used for loading and unloading and transferring the samples to be tested, and the inner vacuum chamber is used to maintain the vacuum environment and the test state; the quadrupole mass spectrometer is arranged on the side wall of the inner vacuum chamber, and is used to analyze and detect only the gas components generated by the samples to be tested; the sample holder is arranged in the inner vacuum chamber or the outer vacuum chamber for carrying and heating or cooling the samples to be tested, and the inner vacuum chamber and the outer vacuum chamber are both provided with reserved spaces for the sample holders, and the sample holders are switched between the reserved spaces for the sample holders according to the requirements of loading and unloading and transferring the samples to be tested; the inner vacuum chamber and the outer vacuum chamber are both connected to the vacuum system through gas pipelines to realize vacuum processing; the vacuum coupling sample transfer rod is arranged on the side wall of the outer vacuum chamber to realize the transfer of the samples to be tested or the sample holder of the outer vacuum chamber; the quadrupole mass spectrometer, the vacuum system, and the vacuum coupling sample transfer rod are all connected to the control device and operated by the control device.

[0008] The inner walls of the inner vacuum chamber and the outer vacuum chamber are both provided with vacuum gauges for measuring the vacuum degree; the inner vacuum chamber is provided with a plug valve, and when the outer vacuum chamber is supplied with the sample to be tested by the vacuum coupling transfer rod, the sample to be tested or the sample support plate is transferred into the inner vacuum chamber by operating the plug valve and the vacuum coupling transfer rod.

[0009] The sample support plate includes a platform, a liquid nitrogen cold plate, and an electric heating device, wherein:

[0010] The platform is used to carry the samples to be tested introduced from the external vacuum chamber. A liquid nitrogen cold plate and an electric heating device are pre-buried under the platform. The liquid nitrogen cold plate is used to cool the samples to be tested, and the electric heating device is used to heat the samples to be tested. Both the liquid nitrogen cold plate and the electric heating device execute corresponding sample processing through the control instructions sent by the control device.

[0011] The vacuum system uses a mechanical pump, a molecular pump, and an ion pump to form a multi-stage vacuum pump, which is directly controlled by a control device to achieve vacuum processing of the inner vacuum chamber and the outer vacuum chamber; the type of pump used in the vacuum system is determined according to the vacuum degree required for vacuuming.

[0012] The outer vacuum chamber adopts a stainless steel top cover and a stainless steel vacuum chamber to meet the vacuum requirements; the sample to be tested is heated and degassed through a sample support plate in the inner vacuum chamber or cooled and adsorbed through a sample support plate in the outer vacuum chamber, and a quadrupole mass spectrometer is used to detect the gas components generated by the sample to be tested after the heating treatment.

[0013] The surface of the platform adopts a condensation adsorption structure with analytical adsorption function to improve the condensation concentration adsorption efficiency in the outer vacuum chamber; the condensation adsorption structure is formed on the surface of the platform by laser or wet etching, which is used to improve the detection sensitivity of the quadrupole mass spectrometer.

[0014] A gas component testing method implemented according to a gas component testing device for a wide-temperature ultra-high vacuum system, including:

[0015] Arrange the sample to be tested in the outer vacuum chamber and perform sealed vacuum chamber treatment on the outer vacuum chamber;

[0016] Evacuate the outer vacuum chamber until the vacuum degree of the outer vacuum chamber reaches the first preset vacuum degree;

[0017] Open the gate valve between the outer vacuum chamber and the inner vacuum chamber to make the inner vacuum chamber and the outer vacuum chamber communicate with each other;

[0018] Cool and adsorb the sample to be tested through the condensation adsorption structure of the sample carrier in the outer vacuum chamber;

[0019] Control the vacuum coupling sample transfer rod through the control device to transfer the sample to be tested and the sample carrier after cooling and adsorption treatment onto the reserved space of the sample carrier in the inner vacuum chamber;

[0020] Control the sample carrier through the control device to heat the sample to be tested before the inner vacuum to achieve thermal excitation;

[0021] Collect various gases generated after thermal excitation of the sample to be tested by the quadrupole mass spectrometer for test analysis;

[0022] Determine the partial pressure of various gases generated after thermal excitation of the sample to be tested according to the test analysis results, and determine the content of various gases after thermal excitation of the sample to be tested according to the partial pressure.

[0023] After the inner vacuum chamber and the outer vacuum chamber communicate with each other, the gate valve between the outer vacuum chamber and the inner vacuum chamber remains open, and the gas in the outer vacuum chamber and the inner vacuum chamber is exchanged and the sample to be tested is sent to the sample carrier in the inner vacuum chamber. The vacuum system pumps out the gas in the vacuum system through a multi-stage vacuum pump to reach the second preset vacuum degree. When the gas in the vacuum system reaches the second preset vacuum degree, it is regarded that the vacuum degree required for the heating treatment of the inner vacuum chamber meets the standard.

[0024] After the sample to be tested undergoes heating and degassing treatment, the water vapor content in the inner vacuum chamber is reduced to avoid contamination of the quadrupole mass spectrometer by water vapor; the gate valve is used to block the gas exchange between the outer vacuum chamber and the inner vacuum chamber in the closed state; the vacuum coupling sample transfer rod is used to realize the switching of the sample to be tested between the outer vacuum chamber and the inner vacuum chamber to prevent each part of the component from being exposed to the atmosphere during loading, unloading or transfer.

[0025] The advantages of the present invention compared with the prior art are:

[0026] (1) The present invention provides a wide temperature range ultra-high vacuum system gas component testing device and method. The device is simple to operate, and its double-layer buffered vacuum chamber structure is easy to maintain ultra-high vacuum. The equipment cost and maintenance cost are relatively low, and non-destructive dynamic detection can be achieved. The measurement results are accurate, and the device can provide a basis for hydrogen and water vapor control of devices such as tube shell coating layers, redundant design of hydrogen sensitive components, and device service life evaluation, so as to ensure the stability of hydrogen content in the tube shell throughout the life cycle and avoid quality problems such as device performance failure.

[0027] (2) The present invention proposes a method of switching between a primary vacuum chamber and a high vacuum chamber to avoid gas adsorption and difficulty in re-vacuuming caused by direct contact of the ultra-high vacuum chamber with the atmosphere, and to avoid exposure of the test probe and the ultra-high vacuum chamber to the atmosphere during the loading and unloading of parts, thereby reducing the ultra-high vacuum evacuation time and greatly improving the test efficiency. At the same time, the sample support plate is pre-buried with heating and cooling pipelines to meet the gas content detection requirements of the sample under different temperature conditions;

[0028] (3) The present invention can perform degassing by preheating in the outer vacuum chamber to prevent water vapor and other gases from contaminating precision equipment such as a mass spectrometer in the inner vacuum chamber, and can concentrate and adsorb the gas in the sample by pre-condensing it using a liquid nitrogen pipeline in the outer vacuum chamber, and then analyze the gas in the sample using a heating pipeline in the inner vacuum chamber, thereby improving the signal level of gas detection, thereby improving the sensitivity of back-end mass spectrometry and other detection methods. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 Schematic diagram of the gas composition testing device for the wide temperature range ultra-high vacuum system provided by the present invention. DETAILED DESCRIPTION

[0030] A wide temperature range ultra-high vacuum system gas component testing device includes an inner vacuum chamber, an outer vacuum chamber, a sample support plate, a quadrupole mass spectrometer, a vacuum system, a vacuum coupling sample transfer rod, and a control device. The outer vacuum chamber is used for sample loading and unloading and transfer, and the inner vacuum chamber is used for maintaining and testing the ultra-high vacuum system. The vacuum system uses multi-stage vacuum pumps such as mechanical pumps, molecular pumps, and ion pumps for vacuuming, and uses multiple sets of vacuum gauges to measure different vacuum degrees. A quadrupole mass spectrometer is used to analyze and detect the gas components generated by the parts.

[0031] In the wide temperature range ultra-high vacuum system gas composition test device:

[0032] The outer vacuum chamber is arranged between the inner vacuum chamber and the atmospheric environment to provide an air pressure buffer space for the inner vacuum chamber. The outer vacuum chamber is used for loading and unloading and transferring the samples to be tested, and the inner vacuum chamber is used to maintain the vacuum environment and the test state; the quadrupole mass spectrometer is arranged on the side wall of the inner vacuum chamber, and is used to analyze and detect only the gas components generated by the samples to be tested; the sample holder is arranged in the inner vacuum chamber or the outer vacuum chamber for carrying and heating or cooling the samples to be tested, and the inner vacuum chamber and the outer vacuum chamber are both provided with reserved spaces for the sample holders, and the sample holders are switched between the reserved spaces for the sample holders according to the requirements of loading and unloading and transferring the samples to be tested; the inner vacuum chamber and the outer vacuum chamber are both connected to the vacuum system through gas pipelines to realize vacuum processing; the vacuum coupling sample transfer rod is arranged on the side wall of the outer vacuum chamber to realize the transfer of the samples to be tested or the sample holder of the outer vacuum chamber; the quadrupole mass spectrometer, the vacuum system, and the vacuum coupling sample transfer rod are all connected to the control device and operated by the control device.

[0033] Vacuum gauges are provided on the inner walls of the inner vacuum chamber and the outer vacuum chamber to measure the vacuum degree; the inner vacuum chamber is provided with a plug valve. When the outer vacuum chamber transfers the sample to be tested into the inner vacuum chamber by the vacuum coupling sample transfer rod, the sample to be tested or the sample support plate is transferred into the inner vacuum chamber by operating the plug valve and the vacuum coupling sample transfer rod.

[0034] The sample support plate includes a platform, a liquid nitrogen cold plate, and an electric heating device, wherein:

[0035] The platform is used to carry the samples to be tested introduced from the external vacuum chamber. A liquid nitrogen cold plate and an electric heating device are pre-buried under the platform. The liquid nitrogen cold plate is used to cool the samples to be tested, and the electric heating device is used to heat the samples to be tested. Both the liquid nitrogen cold plate and the electric heating device execute corresponding sample processing through the control instructions sent by the control device.

[0036] The vacuum system uses a multi-stage vacuum pump composed of a mechanical pump, a molecular pump, and an ion pump, which is directly controlled by a control device to realize the vacuuming of the inner vacuum chamber and the outer vacuum chamber; the type of pump used in the vacuum system is determined according to the vacuum degree required for vacuuming.

[0037] The outer vacuum chamber adopts a stainless steel top cover and a stainless steel vacuum chamber to meet the vacuum requirements; the sample to be tested is heated and degassed through the sample support plate in the inner vacuum chamber or cooled and adsorbed through the sample support plate in the outer vacuum chamber, and the quadrupole mass spectrometer is used to detect the gas components generated by the sample to be tested after the heating treatment.

[0038] The platform surface adopts a condensation adsorption structure with analytical adsorption function to improve the condensation concentration adsorption efficiency in the external vacuum chamber; the condensation adsorption structure is formed on the platform surface by laser or wet etching to improve the detection sensitivity of the quadrupole mass spectrometer.

[0039] Gas composition testing method, the steps include:

[0040] Place the sample to be tested in the outer vacuum chamber and seal the outer vacuum chamber for vacuum treatment;

[0041] Evacuate the outer vacuum chamber until the vacuum degree of the outer vacuum chamber reaches the first preset vacuum degree;

[0042] Open the gate valve between the outer vacuum chamber and the inner vacuum chamber to connect the inner vacuum chamber and the outer vacuum chamber to each other;

[0043] In the outer vacuum chamber, cool and adsorb the sample to be tested through the condensation adsorption structure of the sample tray;

[0044] Through the control device, control the vacuum coupling sample transfer rod to transfer the sample to be tested and the sample tray after the cooling adsorption treatment onto the reserved space of the sample tray in the inner vacuum chamber;

[0045] Through the control device, control the sample tray to heat-treat the sample to be tested before the inner vacuum to achieve thermal excitation;

[0046] Collect various gases generated after the thermal excitation of the sample to be tested by the quadrupole mass spectrometer for test analysis;

[0047] Determine the partial pressure of various gases generated after the thermal excitation of the sample to be tested according to the test analysis results, and determine the content of various gases after the thermal excitation of the sample to be tested according to the partial pressure of the gases.

[0048] After the inner vacuum chamber and the outer vacuum chamber are connected to each other, the gate valve between the outer vacuum chamber and the inner vacuum chamber remains open. After the gas exchange between the outer vacuum chamber and the inner vacuum chamber, the sample to be tested is sent to the sample tray in the inner vacuum chamber. The vacuum system evacuates the gas in the vacuum system through a multi-stage vacuum pump to reach the second preset vacuum degree. When the gas in the vacuum system reaches the second preset vacuum degree, it is considered that the vacuum degree required for the heating treatment of the inner vacuum chamber meets the standard.

[0049] After the sample to be tested undergoes heating and degassing treatment, the water vapor content in the inner vacuum chamber decreases to avoid the contamination of the quadrupole mass spectrometer by water vapor; the gate valve is used to block the gas exchange between the outer vacuum chamber and the inner vacuum chamber in the closed state; the vacuum coupling sample transfer rod is used to realize the switching of the sample to be tested between the outer vacuum chamber and the inner vacuum chamber to prevent each component from being exposed to the atmosphere during the loading, unloading or transfer process.

[0050] The following is further described in conjunction with the specification drawings and preferred embodiments:

[0051] In the current embodiment, the gas component testing device for the wide-temperature ultra-high vacuum system, such as Figure 1As shown, it includes: an inner vacuum chamber, an outer vacuum chamber, a sample holder that can be heated and cooled, a vacuum system, a quadrupole mass spectrometer and a control system. The vacuum chamber of this device includes an outer vacuum chamber 1 and an inner vacuum chamber 2. The outer vacuum chamber 1 is between the inner vacuum chamber 2 and the atmosphere, and plays a role in air pressure buffering. The outer vacuum chamber 1 is used for sample loading and unloading and transfer, and the inner vacuum chamber 2 is used for the maintenance and testing of the ultra-high vacuum system. There are two sets of sample holders 3, which are respectively arranged inside the outer vacuum chamber 1 and the inner vacuum chamber 2. The liquid nitrogen cold plate 4 and the electric heating device 5 are installed at the bottom of the sample holder 3. The sample holder 3 is detachable and can be transferred between the outer vacuum chamber 1 and the inner vacuum chamber 2. The quadrupole mass spectrometer 6 is connected to the inner vacuum chamber 2 to analyze and detect the gas components generated by the parts. The vacuum system 7 uses multi-stage vacuum pumps such as mechanical pumps, molecular pumps, and ion pumps for vacuuming. The vacuum measurement system 8 uses multiple sets of vacuum gauges to measure different vacuum degrees. The plug valve 9 is located between the outer vacuum chamber 1 and the inner vacuum chamber 2, and is used to control and block the gas exchange between the outer vacuum chamber 1 and the inner vacuum chamber 2. The vacuum coupling sample transfer rod 10 is installed in the outer vacuum chamber 1, and is used to transfer the sample support plate 3 or the sample between the outer vacuum chamber 1 and the inner vacuum chamber 2. The control system 11 is connected to the liquid nitrogen cold plate 4, the electric heating device 5, the quadrupole mass spectrometer 6, the vacuum system 7, the vacuum measurement system 8, the vacuum coupling sample transfer rod 10 and other components, and is used to read data and control the switching and adjustment of the components.

[0052] The device has the following characteristics: (1) By switching between the primary vacuum chamber and the high vacuum chamber, the test probe and the ultra-high vacuum chamber are prevented from being exposed to the atmosphere during the loading and unloading of parts, which reduces the ultra-high vacuum pumping time and greatly improves the test efficiency. In addition, heating and cooling pipelines are pre-buried under the sample support plate to meet the gas content detection requirements of the sample under different temperature conditions. (2) The following working mode can be used to have the function of pre-degassing: degassing is performed by pre-heating in the outer vacuum chamber to prevent water vapor and other gases from contaminating precision equipment such as mass spectrometers in the inner vacuum chamber. (3) The following working mode can be used to have the function of concentrating gas to improve detection sensitivity: the gas in the sample is concentrated and adsorbed by pre-condensing in the outer vacuum chamber using a liquid nitrogen pipeline, and then the gas in the sample is analyzed by a heating pipeline in the inner vacuum chamber. The sample support plate surface adopts a condensation adsorption structure with molecular adsorption, which can improve the condensation concentration adsorption efficiency in the outer vacuum chamber, and can further improve the subsequent gas detection signal level in the inner vacuum chamber and the sensitivity of detection methods such as mass spectrometry. The condensation adsorption structure is formed on the surface by laser or wet etching. After adopting this method, the signal level of gas detection is greatly improved, thereby improving the sensitivity of back-end mass spectrometry detection.

[0053] The gas composition test method process is as follows:

[0054] Step 1: After the sample is placed in the outer vacuum chamber, the vacuum chamber is sealed and initially evacuated.

[0055] Step 2: When the vacuum degree of the outer vacuum chamber reaches the initial vacuum degree, open the gate valve between the outer vacuum chamber and the inner vacuum chamber to connect the primary vacuum chamber and the high vacuum chamber, send the sample into the inner vacuum chamber, and close the gate valve.

[0056] Step 3: Use a multi-stage vacuum pump to evacuate the gas in the vacuum system to reach the required ultra-high vacuum.

[0057] Step 4: Thermally excite the sample on the workbench at different set temperatures to release gases such as hydrogen.

[0058] Step 5: Test the gas inside the vacuum chamber with a quadrupole mass spectrometer to obtain the partial pressure of each gas, and thus obtain the gas content.

[0059] Step 6: Transfer the sample from the inner vacuum chamber to the outer vacuum chamber, close the gate valve, and after the outer vacuum chamber returns to atmospheric pressure, replace the new sample.

[0060] Example 1:

[0061] The vacuum chamber consists of a stainless steel top cover and a stainless steel vacuum container. The test device includes 1 outer vacuum chamber, 2 inner vacuum chamber, 3 sample tray, 4 liquid nitrogen cold plate, 5 electric heating device (embedded), 6 quadrupole mass spectrometer, 7 vacuum system, 8 vacuum gauge, 9 gate valve, 10 vacuum coupling sample transfer rod, 11 control system;

[0062] Step 1: After the sample is placed in the outer vacuum chamber, the vacuum chamber is sealed and initially evacuated.

[0063] Step 2: When the vacuum degree of the outer vacuum chamber reaches 3.1×10 -3 Pa, open the gate valve between the outer vacuum chamber and the inner vacuum chamber to connect the primary vacuum chamber and the high vacuum chamber, and send the sample into the inner vacuum chamber.

[0064] Step 3: Use a multi-stage vacuum pump to evacuate the gas in the vacuum system to reach 2.1×10 -8 Pa.

[0065] Step 4: Thermally excite the sample on the workbench at 100 °C to release hydrogen.

[0066] Step 5: Test the gas inside the vacuum chamber with a quadrupole mass spectrometer to obtain the partial pressure of each gas, and thus obtain the gas content.

[0067] The comparison of the gas content results obtained in this example with the gas content results measured by the standard small box method is shown in the following table:

[0068] Table 1 Comparison of Gas Content Detection Data between the Device in Example 1 and the Standard Small Box Method (Gas Content: ppm)

[0069]

[0070] Step 6: Transfer the sample from the inner vacuum chamber to the outer vacuum chamber. After closing the gate valve and the outer vacuum chamber returns to normal pressure, replace the sample with a new one.

[0071] Example 2:

[0072] Use the same wide-temperature ultra-high vacuum system gas component testing device as in Example 1. The gas detection method of the device includes the following steps:

[0073] Step 1: After placing the sample in the outer vacuum chamber, seal the vacuum chamber and perform a preliminary evacuation.

[0074] Step 2: When the vacuum degree of the outer vacuum chamber reaches 2.8×10 -3 Pa, open the gate valve between the outer vacuum chamber and the inner vacuum chamber to connect the primary vacuum chamber and the high vacuum chamber, and send the sample into the inner vacuum chamber.

[0075] Step 3: Use a multi-stage vacuum pump to pump out the gas in the vacuum system until it reaches 3.3×10 -8 Pa.

[0076] Step 4: Thermally excite the sample on the workbench at a temperature of 220°C to release hydrogen.

[0077] Step 5: Test the gas inside the vacuum chamber with a quadrupole mass spectrometer to obtain the partial pressure of each gas, and thus obtain the gas content.

[0078] The comparison of the gas content results obtained in this example with the gas content results measured by the standard small box method is as follows in the table:

[0079] Table 2 Comparison of Gas Content Detection Data between the Device in Example 2 and the Standard Small Box Method (Gas Content: ppm)

[0080]

[0081] Step 6: Transfer the sample from the inner vacuum chamber to the outer vacuum chamber. After closing the gate valve and the outer vacuum chamber returns to normal pressure, replace the sample with a new one.

[0082] Example 3:

[0083] Use the wide-temperature ultra-high vacuum system gas component testing device. The following working mode can have the function of pre-degassing: Evacuate the outer vacuum chamber to a vacuum degree of 6.3×10 -3Pa was heated to 110 °C and held for 24 h for degassing. After the degassing treatment, the water vapor content was reduced to 23% of the original level, avoiding the contamination of precision equipment such as mass spectrometers in the inner vacuum chamber by gases such as water vapor.

[0084] Example 4:

[0085] Using a gas component testing device for a wide-temperature-range ultra-high vacuum system, the following working mode can have the function of concentrating gases to improve detection sensitivity: By using a liquid nitrogen pipeline in the outer vacuum chamber to pre-condense and adsorb the gases in the sample in advance, and then using a heating pipeline in the inner vacuum chamber to desorb the gases in the sample. The upper surface of the sample holder adopts a condensation adsorption structure with molecular adsorption effect, which can improve the condensation and concentration adsorption efficiency in the outer vacuum chamber, and can further improve the gas detection signal level in the subsequent inner vacuum chamber and the sensitivity of detection means such as mass spectrometry. The condensation adsorption structure is formed into a micro-nano structure on the surface by laser: The parameters of the laser are as follows: femtosecond laser pulses with a wavelength of 800 nm, a pulse width of 200 fs, a repetition frequency of 50 Hz, an energy density of 6 J / cm 2 ², a scanning speed of 3 mm / s, and a scanning pitch of 30 μm. After laser treatment, a condensation adsorption structure with molecular adsorption effect is formed on the surface of the sample holder. After adopting this method, the signal level of gas detection is increased to 8.3 times of the original, thus improving the sensitivity of the subsequent mass spectrometry detection.

[0086] Although the present invention has been disclosed above with preferred embodiments, it is not used to limit the present invention. Any person skilled in the art can make possible changes and modifications to the technical solution of the present invention by using the methods and technical contents disclosed above without departing from the spirit and scope of the present invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention all belong to the protection scope of the technical solution of the present invention.

[0087] The content not described in detail in the specification of the present invention belongs to the well-known technology of those skilled in the art.

Claims

1. A wide temperature range ultra-high vacuum system gas component testing device, characterized by: It includes an inner vacuum chamber, an outer vacuum chamber, a sample support plate, a quadrupole mass spectrometer, a vacuum system, a vacuum coupling sample transfer rod, and a control device, wherein: The outer vacuum chamber is arranged between the inner vacuum chamber and the atmospheric environment to provide an air pressure buffer space for the inner vacuum chamber. The outer vacuum chamber is used for loading and unloading and transferring the samples to be tested, and the inner vacuum chamber is used to maintain the vacuum environment and the test state; the quadrupole mass spectrometer is arranged on the side wall of the inner vacuum chamber, and is used to analyze and detect only the gas components generated by the samples to be tested; the sample holder is arranged in the inner vacuum chamber or the outer vacuum chamber for carrying and heating or cooling the samples to be tested, and the inner vacuum chamber and the outer vacuum chamber are both provided with reserved spaces for the sample holders, and the sample holders are switched between the reserved spaces for the sample holders according to the requirements of loading and unloading and transferring the samples to be tested; the inner vacuum chamber and the outer vacuum chamber are both connected to the vacuum system through gas pipelines to realize vacuum processing; the vacuum coupling sample transfer rod is arranged on the side wall of the outer vacuum chamber to realize the transfer of the samples to be tested or the sample holder of the outer vacuum chamber; the quadrupole mass spectrometer, the vacuum system, and the vacuum coupling sample transfer rod are all connected to the control device and operated by the control device.

2. A wide temperature range ultra-high vacuum system gas component testing device according to claim 1, characterized in that: The inner walls of the inner vacuum chamber and the outer vacuum chamber are both provided with vacuum gauges for measuring the vacuum degree; the inner vacuum chamber is provided with a plug valve, and when the outer vacuum chamber is supplied with the sample to be tested by the vacuum coupling transfer rod, the sample to be tested or the sample support plate is transferred into the inner vacuum chamber by operating the plug valve and the vacuum coupling transfer rod.

3. The wide temperature range ultra-high vacuum system gas component testing device according to claim 2, characterized in that: The sample support plate includes a platform, a liquid nitrogen cold plate, and an electric heating device, wherein: The platform is used to carry the samples to be tested introduced from the external vacuum chamber. A liquid nitrogen cold plate and an electric heating device are pre-buried under the platform. The liquid nitrogen cold plate is used to cool the samples to be tested, and the electric heating device is used to heat the samples to be tested. Both the liquid nitrogen cold plate and the electric heating device execute corresponding sample processing through the control instructions sent by the control device.

4. The wide temperature range ultra-high vacuum system gas component testing device according to claim 1, characterized in that: The vacuum system uses a mechanical pump, a molecular pump, and an ion pump to form a multi-stage vacuum pump, which is directly controlled by a control device to achieve vacuum processing of the inner vacuum chamber and the outer vacuum chamber; the type of pump used in the vacuum system is determined according to the vacuum degree required for vacuuming.

5. The wide temperature range ultra-high vacuum system gas component testing device according to claim 3, characterized in that: The outer vacuum chamber adopts a stainless steel top cover and a stainless steel vacuum chamber to meet the vacuum requirements; the sample to be tested is heated and degassed through a sample support plate in the inner vacuum chamber or cooled and adsorbed through a sample support plate in the outer vacuum chamber, and a quadrupole mass spectrometer is used to detect the gas components generated by the sample to be tested after the heating treatment.

6. The wide temperature range ultra-high vacuum system gas component testing device according to claim 5, characterized in that: The surface of the platform adopts a condensation adsorption structure with analytical adsorption effect to improve the condensation concentration adsorption efficiency in the outer vacuum chamber; the condensation adsorption structure is formed on the surface of the platform by laser or wet etching, which is used to improve the detection sensitivity of the quadrupole mass spectrometer.

7. A gas component testing method implemented by the gas component testing device of the wide-temperature-range ultra-high vacuum system according to claim 6, characterized in that It includes: Arrange the sample to be tested in the outer vacuum chamber and perform a sealed vacuum chamber treatment on the outer vacuum chamber; Evacuate the outer vacuum chamber until the vacuum degree of the outer vacuum chamber reaches the first preset vacuum degree; Open the gate valve between the outer vacuum chamber and the inner vacuum chamber to make the inner vacuum chamber and the outer vacuum chamber communicate with each other; In the outer vacuum chamber, cool and adsorb the sample to be tested through the condensation adsorption structure of the sample tray; Through the control device, control the vacuum coupling sample transfer rod to transfer the sample to be tested and the sample tray after the cooling and adsorption treatment to the reserved space of the sample tray in the inner vacuum chamber; Through the control device, control the sample tray to heat-treat the sample to be tested before the inner vacuum to achieve thermal excitation; Collect various gases generated after the thermal excitation of the sample to be tested by the quadrupole mass spectrometer for test analysis; Determine the partial pressure of various gases generated after the thermal excitation of the sample to be tested according to the test analysis results, and determine the content of various gases after the thermal excitation of the sample to be tested according to the partial pressure of the gases.

8. The gas component testing method according to claim 6, wherein: After the inner vacuum chamber and the outer vacuum chamber communicate with each other, the gate valve between the outer vacuum chamber and the inner vacuum chamber remains open. After the gas exchange between the outer vacuum chamber and the inner vacuum chamber, the sample to be tested is sent to the sample tray in the inner vacuum chamber. The vacuum system evacuates the gas in the vacuum system through a multi-stage vacuum pump to reach the second preset vacuum degree. When the gas in the vacuum system reaches the second preset vacuum degree, it is considered that the vacuum degree required for the heating treatment of the inner vacuum chamber meets the standard.

9. The gas component testing method according to claim 6, wherein: After the sample to be tested undergoes heating and degassing treatment, the water vapor content in the inner vacuum chamber decreases to avoid contamination of the quadrupole mass spectrometer by water vapor; the gate valve is used to block the gas exchange between the outer vacuum chamber and the inner vacuum chamber in the closed state; The vacuum coupling sample transfer rod is used to realize the switching of the sample to be tested between the outer vacuum chamber and the inner vacuum chamber to prevent each part of the component from being exposed to the atmosphere during the loading, unloading or transfer process.

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