A precise test method for material outgassing rate based on torsion balance technology
Through the material air effluent measurement system based on torsion scale technology, the problem of difficulty in measuring the air effluent in the prior art is solved, and high-precision and real-time air effluent measurement are achieved.
Patent Information
- Application Number
- CN202311359848.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-19
- Publication Date
- 2025-02-07
- Estimated Expiration
- 2043-10-19
AI Technical Summary
The prior art is difficult to measure the material air effluent of small volume samples with high accuracy, and it is impossible to observe the instantaneous air effluent of the material in real time.
The material air outlet measurement system based on torsion scale technology is adopted, including a torsion swing device, an angle detection device and a sample placement device. By closing the sample chamber to accumulate gas and measuring the deflection angle of the inspection mass module, the air outlet of the sample is calculated.
The air effluent measurement of small volume samples is achieved, the measurement efficiency is improved, and the continuous air effluent fluctuations of the material can be observed in real time.
Smart Images

Figure CN117630282B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of material outgassing rate testing, and in particular to a method for accurately testing the material outgassing rate based on a torsion balance technology. Background Art
[0002] The outgassing effect of materials is a common problem in the vacuum field. The ultimate vacuum degree of the vacuum system is limited by the outgassing rate level of the materials in the system. At present, the main testing methods for material outgassing rate are the static pressure increase method and the small hole conductance method. The former realizes the internal outgassing rate evaluation by monitoring the internal pressure changes of the vacuum system, so an extremely high-resolution vacuum gauge is indispensable. The latter realizes the outgassing rate test by comparing the pressure difference on both sides of the small hole with known conductance. In order to achieve high-precision outgassing rate testing, it is necessary to provide an extremely high vacuum or even an extreme vacuum experimental environment. The lower limit of the measurement of the typical domestic outgassing rate test system measured by the static pressure increase method is about 10 -9 Pa.m / s level [1] , the measurement limit of the small hole conductivity method reaches 10 -10 Pa m / s [2] Under the demand for high-resolution measurement, the current mainstream test methods have high requirements for the vacuum system environment and are difficult to operate. In addition, the test methods used in the vacuum field focus on the average value of the material outgassing rate within a period of test time, and cannot observe the instantaneous outgassing rate fluctuations of the material.
[0003] Gravitational wave detection has been one of the hot topics in physics in recent years. Inertial sensors, one of the core payloads of space gravitational wave detection technology, need to maintain a free fall state in scientific mode, so the residual acceleration caused by various non-conservative forces must be suppressed within a certain noise level. In the vacuum environment of space, the outgassing effect of materials becomes an interference that affects the residual acceleration of inertial sensors, so it is necessary to test and evaluate it.
[0004] The traditional methods currently used can only measure the average outgassing rate of the material over a period of time, and cannot study the fluctuation of the outgassing rate of the sample. In addition, most traditional testing methods are applied to the outgassing rate test of the vacuum container body or large-volume samples, and it is difficult to test small-volume samples with small outgassing volume. Summary of the invention
[0005] In order to overcome the above-mentioned defects of the prior art, the present invention provides a method for accurately testing the gas outflow rate of materials based on torsion balance technology, which can realize the gas outflow rate measurement of small volume samples and improve the measurement efficiency.
[0006] An embodiment of the present invention provides a material outgassing rate measurement system, comprising a container, and further comprising: a torsion pendulum device, an angle detection device, and a sample placement device;
[0007] The torsion pendulum device comprises a mass inspection module, and the mass inspection module is suspended in the container;
[0008] The angle detection device is used to detect the deflection angle of the inspection mass module;
[0009] The sample placement device is arranged in the container, and the sample placement device comprises a sample air outlet pipeline, and the output port of the sample air outlet pipeline is directly facing the inspection mass module.
[0010] Furthermore, the torsion pendulum device also includes: vacuum guidance, magnetic damping and torsion wire;
[0011] The vacuum guide is arranged on the container, and the vacuum guide is connected to the magnetic damper;
[0012] The magnetic damper is arranged in a closed space inside the container, the magnetic damper is located between the vacuum guide and the inspection mass module, and the magnetic damper is connected to the inspection mass module through a torsion wire.
[0013] Furthermore, the angle detection device includes an autocollimator, and the angle detection device observes the inspection mass module through the autocollimator.
[0014] Further, the inspection quality module includes a glass sheet, a reflector and a sleeve;
[0015] The glass sheet is an I-shaped quartz glass sheet, including glass sheets at both ends and a middle connecting rod;
[0016] The reflectors are arranged on both sides of the sleeve and are used to reflect the light beam emitted by the angle detection device;
[0017] The sleeve is arranged on the middle connecting rod and is used to connect the torsion wire and the inspection mass module.
[0018] Furthermore, the sample placement device also includes a sample chamber and a valve;
[0019] The sample chamber is arranged in the container, connected to the valve, and used for placing the sample to be tested;
[0020] The valve is connected to the sample chamber and the sample gas outlet pipeline.
[0021] Further, the system also includes a control device;
[0022] The control device comprises a control chamber, a control valve and a control pipeline; wherein the control chamber has the same structure as the sample chamber;
[0023] The control chamber is arranged in the container and connected to the control valve; wherein the control valve has the same structure as the valve;
[0024] The control valve connects the control chamber and the control pipe; wherein the control pipe has the same structure as the sample outlet pipe and the output port of the control pipe faces the inspection quality module. Furthermore, the system also includes a gas analyzer;
[0025] The input end of the gas analyzer is placed in the container and is used to detect the gas composition in the container.
[0026] Another embodiment of the present invention provides a method for measuring the gas outflow rate of a material, comprising the following steps:
[0027] After placing the sample to be tested in the sample chamber, closing the sample chamber door and opening the valve, and then evacuating the container to a vacuum environment;
[0028] After confirming that the inspection mass module is in a small-amplitude free oscillation state, closing the valve to make the sample chamber in a sealed state; wherein the inspection mass module is suspended in the container;
[0029] When the sample chamber remains sealed for a predetermined time, the valve is opened, and the gas in the sample chamber is released through the sample outlet pipe and collides with the inspection mass module;
[0030] The inspection mass module is detected by an angle detection device to obtain a deflection angle of the inspection mass module, and the gas emission rate of the sample to be tested is calculated based on the deflection angle.
[0031] Furthermore, before placing the sample to be tested in the sample chamber, the method further comprises:
[0032] The output port of the sample gas outlet pipe is adjusted to face the glass sheet, and the distance between the output port and the glass sheet is less than a preset distance threshold.
[0033] Furthermore, before measuring the gas outflow rate of the sample, the method further includes: performing a control test; wherein the control test specifically includes:
[0034] Close the control chamber and open the control valve;
[0035] After the container is evacuated to a vacuum state and the inspection quality module is confirmed to be in a state of small-amplitude free oscillation, the control valve is closed to seal the control chamber;
[0036] When the control chamber remains sealed for a predetermined time, the control valve is opened, and the gas in the control chamber is released through the sample outlet pipe and collides with the inspection quality module;
[0037] The inspection mass module is detected by an angle detection device to obtain a deflection angle of the inspection mass module, and the background gas outflow rate of the control chamber is calculated based on the deflection angle.
[0038] Compared with the prior art, the present invention has the following beneficial effects:
[0039] The present invention can measure the average gas outflow rate of the material over a period of time and the gas outflow rate of a small volume sample by accumulating gas in a closed sample chamber. In addition, the present invention also provides a set of control chambers to deduct the background gas outflow effect of the sample chamber, thereby improving the measurement efficiency. At the same time, keeping the valve open can also measure the gas outflow rate fluctuation of the material continuously outflowing. BRIEF DESCRIPTION OF THE DRAWINGS
[0040] Figure 1 A schematic structural diagram of a material outgassing rate measuring device provided in one embodiment of the present invention.
[0041] Figure 2 A schematic structural diagram of a preferred embodiment of a material outgassing rate measuring device provided by the present invention.
[0042] Figure 3 A structural schematic diagram of a quality inspection module provided in an embodiment of the present invention.
[0043] Figure 4 A schematic flow chart of a material outgassing rate measurement method provided in accordance with another embodiment of the present invention.
[0044] Figure 5 A schematic flow chart of a preferred embodiment of a material outgassing rate measurement method provided by the present invention.
[0045] Explanation of the meaning of the accompanying symbols: 1. Container; 2. Vacuum guide; 3. Magnetic damping; 4. Torsion wire; 5. Angle detection device; 6. Sample chamber; 6a. Valve; 7. Control chamber; 7a. Control valve; 9. Glass sheet; 10. Reflector; 11. Sleeve; 12. Gas analyzer. DETAILED DESCRIPTION
[0046] The drawings are for illustrative purposes only and should not be construed as limiting the present patent;
[0047] It is understandable to those skilled in the art that some well-known structures and their descriptions may be omitted in the drawings.
[0048] The technical solution of the present invention is further described below in conjunction with the accompanying drawings and embodiments.
[0049] Reference Figure 1, is a schematic structural diagram of a material outgassing rate measuring device provided by an embodiment of the present invention, comprising a container 1, and further comprising: a torsion pendulum device, an angle detection device 5 and a sample placement device;
[0050] The torsion pendulum device comprises a mass inspection module, and the mass inspection module is suspended in the container 1;
[0051] The angle detection device 5 is used to detect the deflection angle of the inspection mass module;
[0052] The sample placement device is arranged in the container 1, and the sample placement device comprises a sample air outlet pipeline, and the output port of the sample air outlet pipeline is directly facing the inspection mass module.
[0053] Furthermore, the torsion pendulum device further comprises: a vacuum guide 2, a magnetic damper 3 and a torsion wire 4;
[0054] The vacuum guide 2 is arranged on the container 1, and the vacuum guide 2 is connected to the magnetic damper 3;
[0055] The magnetic damper 3 is disposed in a closed space inside the container 1 , the magnetic damper 3 is located between the vacuum guide 2 and the inspection mass module, and the magnetic damper 3 is connected to the inspection mass module through a torsion wire 4 .
[0056] Furthermore, the angle detection device 5 includes an autocollimator, and the angle detection device 5 observes the inspection mass module through the autocollimator.
[0057] In a preferred embodiment, referring to Figure 2 , is a schematic diagram of the structure of a material outgassing rate measuring device provided by a preferred embodiment of the present invention. Figure 2 It can be seen that the device includes a container 1, a vacuum guide 2, a magnetic damper 3, a torsion wire 4 and an angle detection device 5.
[0058] The vacuum guide 2 and the magnetic damper 3 are connected through a torsion wire 4. The vacuum guide 2 is arranged on the container 1, and the magnetic damper 3 is arranged in a closed space inside the container 1. The upper end of the magnetic damper 3 is connected to the vacuum guide 2, and the lower end is connected to the inspection mass module through the torsion wire 4. The vacuum guide 2, the magnetic damper 3, the torsion wire 4 and the inspection mass module together constitute a torsion pendulum system.
[0059] In addition, an angle detection device 5 is provided outside the container 1. The angle detection device 5 is actually a high-resolution autocollimator for detecting the deflection angle of the inspection mass module. To prevent the deflection angle from being too large and exceeding the measurement range of the autocollimator, the range of the angle detection device 5 needs to be large enough.
[0060] The torsion pendulum system and the angle detection device 5 together form a torsion balance platform, which can be regarded as a torque sensor.
[0061] Preferably, the inspection quality module comprises a glass sheet 9, a reflector 10 and a sleeve 11;
[0062] The glass sheet 9 is an I-shaped quartz glass sheet, including glass sheets at both ends and a middle connecting rod;
[0063] The reflectors 10 are arranged on both sides of the sleeve 11 and are used to reflect the light beam emitted by the angle detection device;
[0064] The sleeve 11 is arranged on the middle connecting rod and is used to connect the torsion wire 4 and the inspection mass module.
[0065] In a preferred embodiment, referring to Figure 3 , which is a structural front view of a quality inspection module provided in an embodiment of the present invention, including a glass sheet 9, a reflector 10 and a sleeve 11.
[0066] The glass sheet 9 is an I-shaped quartz glass sheet, which is composed of large glass sheets at both ends and a connecting rod in the middle. Figure 2 From the side view of the inspection quality module (the lower end connection part of the torsion wire 4), it can be seen that there are actually two reflectors 10, which are respectively arranged on both sides of the sleeve 11 to reflect the light beam emitted by the angle detection device 5 ( Figure 2 The dotted line portion is a schematic diagram of the light beam. The sleeve 11 is disposed on the middle connecting rod and is used to connect the torsion wire 4 and the inspection mass module, so that the inspection mass module is suspended in the container 1 through the torsion wire 4.
[0067] Furthermore, the sample placement device also includes a sample chamber 6 and a valve 6a;
[0068] The sample chamber 6 is disposed in the container 1 and connected to the valve 6a, and is used to place the sample to be tested;
[0069] The valve 6a connects the sample chamber 6 with the sample outlet pipe.
[0070] Preferably, the system further comprises a control device;
[0071] The control device comprises a control chamber 7, a control valve 7a and a control pipeline; wherein the control chamber 7 has the same structure as the sample chamber 6;
[0072] The control chamber 7 is disposed in the container 1 and is connected to the control valve 7a; wherein the control valve 7a has the same structure as the valve 6a;
[0073] The control valve 7a connects the control chamber 7 with the control pipeline; wherein the control pipeline has the same structure as the sample outlet pipeline and the output port of the control pipeline faces the inspection mass module.
[0074] In a preferred embodiment, referring to Figure 2 , the container 1 is also provided with a sample chamber 6 and a control chamber 7. In order to reduce the influence of the background gas outflow rate of the sample chamber on the sample test, both use low gas outflow rate alloys as processing materials, such as 6061 aluminum alloy, 316 stainless steel, etc., and perform high temperature baking and polishing. The sample chamber 6 is connected with a valve 6a and a sample gas outlet pipe, and the control chamber 7 is also connected with a control valve 7a and a control pipe. The control valve 7a is exactly the same as the valve 6a, and the control pipe is exactly the same as the sample gas outlet pipe.
[0075] The purpose of setting up the control chamber 7 is to eliminate the background gas outflow rate. In actual measurement, the output ports of the control pipe and the sample gas outlet pipe are aligned with the same glass sheet. In order to make all the released gas molecules hit the test mass, the gas outlet pipe is placed within 5mm parallel to the test mass, and the center of the pipe is coaxial with the center of the large glass sheet at one end of the test mass.
[0076] Further, the system also includes a gas analyzer 12;
[0077] The input end of the gas analyzer 12 is placed in the container 1 and is used to detect the gas composition in the container 1 .
[0078] Reference Figure 4 , is a flow chart of a material outgassing rate measurement method provided by another embodiment of the present invention, comprising the following steps:
[0079] S1: After placing the sample to be tested in the sample chamber 6, the sample chamber 6 is closed and the valve 6a is opened, and then the container 1 is evacuated to a vacuum environment;
[0080] S2: After confirming that the inspection mass module is in a small-amplitude free oscillation state, closing the valve 6a to make the sample chamber 6 in a sealed state; wherein the inspection mass module is suspended in the container 1;
[0081] S3: When the time duration for which the sample chamber 6 remains sealed reaches a preset time threshold, the valve 6a is opened, and the gas in the sample chamber 6 is released through the sample outlet pipe and collides with the inspection mass module;
[0082] S4: Detecting the inspection mass module through the angle detection device 5 to obtain the deflection angle of the inspection mass module, and calculating the gas emission rate of the sample to be tested according to the deflection angle.
[0083] Regarding step S1, specifically, before placing the sample to be tested in the sample chamber 6, it also includes:
[0084] The output port of the sample gas outlet pipe is adjusted to face the glass sheet 9, and the distance between the output port and the glass sheet 9 is less than a preset distance threshold.
[0085] Preferably, before measuring the gas outflow rate of the sample, the method further comprises: performing a control test; wherein the control test specifically comprises:
[0086] Close the control chamber 7 and open the control valve 7a;
[0087] After the container 1 is evacuated to a vacuum state and the quality inspection module is confirmed to be in a small-amplitude free oscillation state, the control valve 7a is closed to make the control chamber 7 in a sealed state;
[0088] When the time for which the control chamber 7 remains sealed reaches a preset time threshold, the control valve 7a is opened, and the gas in the control chamber 7 is released through the sample outlet pipe and collides with the inspection mass module;
[0089] The inspection mass module is detected by an angle detection device 5 to obtain a deflection angle of the inspection mass module, and the background gas outflow rate of the control chamber 7 is calculated based on the deflection angle.
[0090] In a preferred embodiment, referring to Figure 5 , the measurement method of material outgassing rate is as follows:
[0091] Before the measurement begins, build the torsion balance platform, install the sample chamber 6 and the control chamber 7, and adjust the outlet of the sample chamber and the control chamber gas outlet valve to the center of the large glass plate of the inspection mass, within 5 mm from the surface of the inspection mass;
[0092] After placing the sample in the sample chamber 6, close the sample chamber door, keep valve 6a open, and evacuate the vacuum container 1 to a vacuum state with a vacuum degree of 1×10 -5 Pa and maintained by an ion pump, the torsion pendulum is adjusted to a torsion amplitude of the proof mass module within 10 μrad (i.e., the torsion pendulum is in a small-amplitude free oscillation state), and the background noise curve spectrum of the torsion balance is measured;
[0093] After confirming that the torsion pendulum is in a state of free oscillation with a small amplitude, close valve 6a to seal the sample chamber and allow the gas to accumulate;
[0094] Sealing time t seal After that, the valve 6a is opened, the mass inspection module receives the gas collision vibration, reads the deflection angle spectrum through the angle detection device 5 and obtains the residual gas component ratio in the container 1 through the gas analyzer 12, and finally obtains the total collision gas molecular weight and the total gas outflow rate of the sample in the sample chamber.
[0095] When multiple measurements are required, the torsion pendulum can be adjusted back to a small amplitude state after the vacuum system is stable, and the above experimental process can be repeated to measure again. In addition, after the average gas outflow rate measurement is completed, the valve 6a is kept open, and the torsion balance noise spectrum over a period of time is measured to obtain the sample gas outflow rate fluctuation noise.
[0096] Furthermore, before formally measuring the sample outgassing rate, a control test is required to obtain the background outgassing rate of the sample chamber, thereby reducing the test error. The control test is similar to the formal test process, except that the control chamber 7 is used instead of the sample chamber 6, and the sample to be tested is not placed in the control chamber 7. After the background noise is obtained in the control test, the background noise is deducted in the subsequent calculation, which can improve the accuracy of the measurement.
[0097] As an optional embodiment, after placing the sample in the sample chamber 6 during the formal test, the opening and closing of the sample chamber 6 and the control chamber 7, valve 6a and control valve 7a can be synchronously controlled, which can also eliminate background noise and improve measurement accuracy.
[0098] Finally, the measuring principle of the material outgassing rate measuring method provided by the present invention is as follows:
[0099] When gas molecules collide with the test mass module, momentum exchange occurs, and the macroscopic force can be measured by the torsion balance. Therefore, when the valve of the sample chamber is opened, the gas released from the sample chamber quickly hits the test mass, and the corresponding amount of gas released can be obtained by measuring the magnitude of the force during the process.
[0100] When the test mass is subjected to an external torque τ at a certain point, the motion equation of the torsion pendulum that produces the corresponding deflection around the suspension wire is:
[0101]
[0102] where θ is the deflection angle of the torsion pendulum around the suspension wire, is the first-order differential of θ, is the second-order differential of θ, I is the moment of inertia of the torsion pendulum, γ is the damping coefficient, k is the torsional elastic coefficient of the torsion wire, φ is the dissipation angle of the torsion wire, the second term on the left side of the formula represents the torque generated by the gas damping of the torsion pendulum, and the third term represents the restoring torque of the suspension wire deformation. Under high vacuum conditions (such as 10 -5 Pa), the gas damping effect can generally be ignored.
[0103] By Fourier transforming the above motion equation, we can get the transfer function of the torsion pendulum deflection angle and torque:
[0104]
[0105] in, is the eigenfrequency of the torsion balance, is the torsion wire quality factor.
[0106] When the preparation is completed, the sample is placed in the sample chamber and the whole system is in the expected vacuum state, and the valves of the sample chamber and the control chamber are open. seal , gas accumulation in the sample chamber. t seal Then the sample chamber valve is opened, the gas is released rapidly and collides with the inspection mass module, causing the inspection mass module to twist around the torsion wire.
[0107] After the valve is opened, the gas is released very quickly. The pressure change in the sample chamber is used as the judgment of the gas release amount. The time to reach 95% of the equilibrium pressure drop is:
[0108]
[0109] Among them, V SC (m 3 ) is the internal volume of the sample chamber, C (m 3 / s) is the molecular conductance at the outlet of the vent valve. For this device, the time t c <6s, compared with the response time of the torsion balance of hundreds of seconds, it can be considered that an impulse response is generated on the torsion balance, from which the deflection angle of the torsion balance can be calculated as:
[0110]
[0111] Among them, Q outgassing (molecules / s) is the sample outgassing rate, I molecule (kg*m / s) is the momentum exchange caused by the collision of a single gas molecule, L(m) is the torsion balance arm, I(kg*m 2 ) is the moment of inertia of the torsion pendulum, and k (N*m / rad) is the torsional stiffness of the torsion wire.
[0112] Therefore, the corresponding sample outgassing rate Q is calculated by reading the change in the torsion angle caused by the gas impact outgassmg ,Right now:
[0113]
[0114] Because a control room is set up, the background gas outflow of the sample room is theoretically equal to that of the control room, and the effect is offset. Therefore, only a set of blank control experiments without samples need to be performed before starting the experiment. It is not necessary to perform a control experiment every time to deduct the background. For samples with extremely low gas outflow rate, it is necessary to increase the sealing time t seal , making the impulse response of the torsion balance to be measured significantly larger than the background.
[0115] Among them, I in the above formula moleculeIt is the average value of impulse generated by each gas component. For different gases, the impulse ratio depends on the molecular mass ratio. For example, the impulse ratio between type I gas and type J gas is specifically reflected as follows:
[0116]
[0117] The gases released by metal materials under high vacuum conditions are mainly hydrogen and water vapor. The specific gas components are measured by the gas analyzer 12. Assuming that the molecular weight of type i gas accounts for ni of the total molecular weight, the average molecular impulse I molecule The calculation formula is:
[0118]
[0119] The above is the measurement process of the average gas outflow rate of the sample. This method can also evaluate the gas outflow rate fluctuation of the sample. The specific method is:
[0120] After the average gas outflow rate test is completed, the sample chamber vent valve is kept open. The torsion balance is continuously acted upon by the gas released from the sample chamber. The gas outflow rate fluctuates during the continuous gas release process of the sample. The fluctuation noise is Q fluctuation , the fluctuation noise can be read out from the torsion balance torque noise spectrum:
[0121]
[0122] in, is the torsion balance torque noise, and the specific calculation formula is as follows:
[0123]
[0124] in, is the power spectral density of the torsion balance deflection angle.
[0125] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the embodiments here. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the claims of the present invention.
Claims
1. A material outgassing rate measurement system, comprising a container (1), characterized in that: Also includes: Vacuum guide (2), magnetic damping (3), torsion wire (4), torsion pendulum device, angle detection device (5) and sample placement device; The torsion pendulum device comprises a mass inspection module, and the mass inspection module is suspended in the container (1); wherein the mass inspection module comprises a glass sheet (9), a reflector (10) and a sleeve (11); The glass sheet (9) is an I-shaped quartz glass sheet, comprising glass sheets at both ends and a middle connecting rod; The reflectors (10) are arranged on both sides of the sleeve (11) and are used to reflect the light beam emitted by the angle detection device (5); The sleeve (11) is arranged on the middle connecting rod and is used to connect the torsion wire (4) and the inspection mass module; The vacuum guide (2) is arranged on the container (1), and the vacuum guide (2) is connected to the magnetic damper (3); The magnetic damper (3) is arranged in a closed space inside the container (1), the magnetic damper (3) is located between the vacuum guide (2) and the inspection mass module, and the magnetic damper (3) is connected to the inspection mass module through a torsion wire (4); The angle detection device (5) comprises an autocollimator, and the angle detection device (5) observes the inspection mass module through the autocollimator to detect the deflection angle of the inspection mass module; The sample placement device is arranged in the container (1), and comprises a sample air outlet pipeline, wherein the output port of the sample air outlet pipeline faces the mass inspection module.
2. A material outgassing rate measurement system according to claim 1, characterized in that: The sample placement device also includes a sample chamber (6) and a valve (6a); The sample chamber (6) is arranged in the container (1), connected to the valve (6a), and is used for placing the sample to be tested; The valve (6a) connects the sample chamber (6) with the sample outlet pipe.
3. A material outgassing rate measurement system according to claim 2, characterized in that: The system also includes a control device; The control device comprises a control chamber (7), a control valve (7a) and a control pipeline; wherein the control chamber (7) has the same structure as the sample chamber (6); The control chamber (7) is arranged in the container (1) and is connected to the control valve (7a); wherein the control valve (7a) has the same structure as the valve (6a); The control valve (7a) connects the control chamber (7) with the control pipeline; wherein the control pipeline has the same structure as the sample outlet pipeline and the output port of the control pipeline faces the inspection mass module.
4. A material outgassing rate measurement system according to claim 1, characterized in that: The system also includes a gas analyzer (12); The input end of the gas analyzer (12) is placed in the container (1) and is used to detect the gas composition in the container (1).
5. A material outgassing rate measurement method based on the material outgassing rate measurement system according to claim 3, characterized in that: The following steps are involved: After placing the sample to be tested in the sample chamber (6), the sample chamber (6) is closed and the valve (6a) is opened, and then the container (1) is evacuated to a vacuum environment; After confirming that the inspection mass module is in a small-amplitude free oscillation state, the valve (6a) is closed to put the sample chamber (6) in a sealed state; wherein the inspection mass module is suspended in the container (1); When the time for which the sample chamber (6) remains sealed reaches a preset time threshold, the valve (6a) is opened, and the gas in the sample chamber (6) is released through the sample outlet pipe and collides with the inspection mass module; The inspection mass module is detected by an angle detection device (5) to obtain the deflection angle of the inspection mass module, and the gas emission rate of the sample to be tested is calculated based on the deflection angle.
6. A material outgassing rate measurement method according to claim 5, characterized in that: Before placing the sample to be tested in the sample chamber (6), the method further comprises: The output port of the sample air outlet pipe is adjusted to face the glass sheet (9), and the distance between the output port and the glass sheet (9) is less than a preset distance threshold; wherein the output ports of the control pipe and the sample air outlet pipe are aligned with the same glass sheet.
7. A material outgassing rate measurement method according to claim 5, characterized in that: Before measuring the gas outflow rate of the sample, the method further includes: performing a control test; wherein the control test specifically includes: Close the control chamber (7) and open the control valve (7a); After the container (1) is evacuated to a vacuum state and it is confirmed that the inspection mass module is in a small-amplitude free oscillation state, the control valve (7a) is closed to put the control chamber (7) in a sealed state; When the time for which the control chamber (7) remains sealed reaches a preset time threshold, the control valve (7a) is opened, and the gas in the control chamber (7) is released through the sample outlet pipe and collides with the inspection mass module; The inspection mass module is detected by an angle detection device (5) to obtain the deflection angle of the inspection mass module, and the background gas outflow rate of the control chamber (7) is calculated based on the deflection angle.
Citation Information
Patent Citations
System and method for measuring partial pressure outgassing rate of material
CN103267705A
Procedure for analyzing an adhering surface film on a specimen
DE102014222483A1