CN114113285A - Mechanism and method for measuring air release rate of metal material - Google Patents
Mechanism and method for measuring air release rate of metal material Download PDFInfo
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- 230000007246 mechanism Effects 0.000 title claims abstract description 36
- 239000007769 metal material Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 238000010943 off-gassing Methods 0.000 claims abstract description 27
- 238000002955 isolation Methods 0.000 claims abstract description 23
- 230000008859 change Effects 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 108
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 230000000630 rising effect Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 17
- 238000012360 testing method Methods 0.000 abstract description 14
- 230000009471 action Effects 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 154
- 238000001514 detection method Methods 0.000 description 14
- 238000005259 measurement Methods 0.000 description 7
- 238000007872 degassing Methods 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 230000000740 bleeding effect Effects 0.000 description 3
- 238000009529 body temperature measurement Methods 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 230000005469 synchrotron radiation Effects 0.000 description 1
- 230000007723 transport mechanism Effects 0.000 description 1
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention discloses a mechanism for measuring the outgassing rate of a metal material, which belongs to the technical field of outgassing rate testing devices and comprises a vacuum chamber and a gas measuring device, wherein a sample table is arranged in the vacuum chamber; also discloses a method for measuring the air release rate of the metal material, which comprises the following steps: s1, baking the vacuum chamber, vacuumizing the vacuum chamber, and cooling to obtain ultrahigh vacuum; s2, placing the sample on the sample table, and enabling the air inlet hole to be close to the surface of the sample; s3, heating or refrigerating the sample as required, starting the gas measuring device to collect the gas desorbed from the sample, recording the change of the gas release amount of the sample at a specific temperature along with the time, or the trend of the gas release amount of the sample at a specific temperature rise rate along with the temperature change, and under the action of the isolation sleeve, ensuring that the gas inlet of the gas inlet hole is only the gas released by the sample, thereby accurately measuring the gas release rate of the surface or bulk phase of the material.
Description
Technical Field
The invention relates to the technical field of air bleeding rate testing devices, in particular to a mechanism and a method for testing the air bleeding rate of a metal material.
Background
Some high-precision analysis and detection equipment such as synchrotron radiation, electron microscope, XPS and the like all need an ultrahigh vacuum environment when in use, and one of the very important conditions for achieving the ultrahigh vacuum environment is that the material outgassing rate of the manufactured analysis and detection equipment is required to be low enough to avoid the self outgassing of the material for manufacturing the analysis and detection equipment from influencing the vacuum degree of the analysis and detection equipment, so that the resolution of a detection result is reduced. At present, special stainless steel materials are often adopted for manufacturing the analysis and detection equipment, and the method for detecting the gas release rate of the stainless steel materials at present generally comprises the steps of rolling a stainless steel plate into a cylinder, welding a round bottom on the bottom surface of the cylinder, welding a standard knife edge flange with the diameter of CF200 on the top surface of the cylinder, forming a sealed cavity by the components, and arranging a plurality of knife edge flanges with the size of CF35 on the cavity, wherein the flanges are used for connecting various pump sets, precise vacuum meters, valves, residual gas analyzers and the like. When the detection is carried out, the interior of the cavity is firstly vacuumized by a vacuum pump, after the vacuumization is finished, the whole system is subjected to degassing treatment, and then bulk gas is driven out by baking at a higher temperature and enters a cavity where the residual gas analyzer is located through a leak hole for detection.
However, in the above detection method, although the oven is used to bake and degas the detection equipment, the abandonment rate of two different materials is often increased, and the two different materials need to be made into a cavity, the smoothness inside the cavity needs to be ensured to be consistent in the process, the whole large cavity needs to be heated in a laboratory, the heating speed is low, and the highest temperature is limited. In addition, because the leakage detection of a new cavity at this time is needed every time, all flanges and interfaces are ensured to be well sealed. In addition, in the detection process, gas outside the cylinder may permeate into the steel, and under the condition of vacuumizing the inside of the steel cylinder, the speed of permeating external gas into the cylinder material is increased, so that the gas release rate of the inside of the steel cylinder is actually higher than the original gas release rate of the steel cylinder. In order to avoid the problem, the invention patent with the patent number of '201810283087.6' and the name of 'a material air suction and air discharge rate testing device' discloses a material air discharge rate testing device, which comprises an air discharge testing system, an inlet and outlet sample chamber and a molecular pump, wherein the inlet and outlet sample chamber is communicated with an air discharge performance testing chamber of the air discharge testing system, the air discharge testing system and the inlet and outlet sample chamber are vacuumized by the molecular pump during testing, then a sample is sent into the air discharge performance testing chamber by an air discharge sample sending rod in the sample outlet chamber for testing, and the air discharge rate of the tested sample can be prevented from being interfered by external air by vacuumizing the air discharge testing system. However, although the above patent provides a vacuum environment for the sample to avoid the interference of the outside air, the outgassing rate of the outgassing test system, the chamber for entering and exiting the sample and the material of the molecular pump itself also exists, even if the whole device is dried and degassed, it is impossible to degas a hundred percent of the outgassing, and the residual gas is still remained, and after the evacuation, the residual gas is released, which affects the final measurement result.
Disclosure of Invention
The present invention is directed to solve the above problems, and an object of the present invention is to provide a mechanism and a method for measuring a outgassing rate of a metal material, wherein under the action of an isolation sleeve, gases in a vacuum chamber except for a sample can be isolated, and after an air inlet is close to the surface of the sample, it can be ensured that all the gases come from the sample, so as to avoid the interference of external gases, and improve the accuracy of the outgassing rate.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a mechanism for measuring the gas release rate of a metal material, which comprises a vacuum chamber and a gas measuring device, wherein a sample table for fixing a sample is arranged in the vacuum chamber, the gas inlet end of the gas measuring device is hermetically connected with an isolating sleeve extending into the vacuum chamber, and the end of the isolating sleeve is provided with a gas inlet hole for being close to the surface of the sample and collecting the gas released by the sample.
Preferably, the gas measuring device comprises a quadrupole mass spectrometer, and the isolation sleeve is hermetically connected to an ionizer of the quadrupole mass spectrometer.
Preferably, the end of the isolation sleeve close to the sample is a conical head, and the air inlet hole is arranged at the tip of the conical body.
Preferably, be equipped with the confession on the vacuum chamber the admission line that isolation sleeve stretched into, the admission line with all be equipped with flange on the quadrupole mass spectrometer, two sealing connection has the bellows between the flange, the ionization ware is located inside the bellows.
Preferably, the quadrupole mass spectrometer is mounted on a position adjustment mechanism by which the distance of the gas inlet from the sample surface can be adjusted.
Preferably, a heater and a liquid nitrogen tube are arranged in the sample stage, and a connecting pipeline for connecting the heater and the liquid nitrogen tube with an external temperature control system and an air guide pipeline communicated with an external air guide device are arranged on the vacuum chamber.
Preferably, a temperature measuring probe connected with the sample is arranged on the sample stage, the temperature measuring probe is connected with the external temperature control system, and real-time temperature information of the sample is obtained through the temperature measuring probe.
Preferably, the external temperature control system is connected to a computer, the computer can process the temperature information measured by the temperature measuring probe, and the external temperature control system controls the heating power of the heater and the like to control the heating temperature, the heating rate and the heating time of the sample.
Preferably, the vacuum chamber is provided with a vacuum pump for evacuating the inside thereof and a vacuum gauge extending into the inside of the vacuum chamber.
Preferably, a sample conveying pipeline for being hermetically connected with the sample conveying mechanism is arranged on the vacuum chamber.
Preferably, the vacuum chamber is further provided with an observation window for observing the sample.
The method for measuring the air release rate of the metal material is also disclosed, and the mechanism for measuring the air release rate of the metal material comprises the following steps:
s1, vacuumizing the vacuum chamber, heating and baking the vacuum chamber, wherein the baking temperature is at least 120 ℃, and the baking is stopped after at least 48 hours, so that the baking is carried out for 10-10Vacuum degree in mbar magnitude;
s2, placing a sample to be measured on the sample stage, and adjusting the position of the gas measuring device to enable the gas inlet hole to be close to the surface of the sample;
and S3, heating the sample as required, starting the gas measuring device to collect the sample gas, and recording the change of the outgassing gas and the type of the sample at a specific temperature and the outgassing amount of the sample along with time, or the trend of the outgassing amount of each gas of the sample along with the change of the temperature at a specific temperature rising rate.
Compared with the prior art, the invention has the following technical effects:
1. according to the invention, an ultrahigh vacuum environment can be provided for the sample through the vacuum chamber, so that the interference of external gas can be avoided, and meanwhile, conditions are created for sample deflation; the gas inlet end of the gas measuring device is sealed with the isolation sleeve, so that the gas except the sample in the vacuum chamber can be isolated, and when the gas inlet hole of the isolation sleeve is close to the surface of the sample, the gas entering the isolation sleeve from the gas inlet hole can be completely released from the sample, so that the measuring accuracy of the gas release rate of the sample is improved.
2. In the invention, a heater, a liquid nitrogen tube and a temperature measuring probe are arranged in a sample stage, and a gas inlet device arranged on the device is combined, so that a measuring mechanism has two measuring functions of material gas release rate and gas suction rate; when the gas release rate is measured, under the ultra-vacuum environment, according to the material of the sample, the sample is heated by the heater, so that the gas in the sample is released, the accurate measurement of the gas release rate of the sample body along with the temperature change can be realized, when the gas suction rate is measured, under the ultra-vacuum environment, the sample is firstly refrigerated to the liquid nitrogen temperature by the liquid nitrogen pipe, then the sample is clung to the sample by the external gas guide equipment and the telescopic gas guide pipeline, the gas is supplied to the room, so that the sample adsorbs the supplied gas, the gas supply is stopped after a certain time, the sample is vacuumized again, and then the sample is heated again, and meanwhile, the gas released by the sample is collected and analyzed by the gas measuring device, so that the gas desorption rate, namely the gas suction rate of the sample is measured.
3. According to the invention, the vacuum chamber is hermetically connected with the sample conveying mechanism through the sample conveying pipeline, so that after the vacuum chamber is vacuumized, the ultrahigh vacuum environment in the vacuum chamber is not damaged when the sample conveying mechanism conveys the sample, and the vacuum chamber is ensured to be always kept in ultrahigh vacuum.
4. In the invention, the vacuum chamber is heated and baked firstly, so that the vacuum chamber and other devices in the vacuum chamber can be baked and degassed, and the degassing interference of other mechanisms on the measurement of the sample degassing rate is avoided; after the sample is vacuumized, the sample needs to be heated, refrigerated or kept at normal temperature according to the characteristics of the sample material, the deep gas in the sample can be promoted to be released by heating, the gas on the surface can be not only used for measuring the gas release rate of the material body, the gas suction property on the surface of the sample and the adsorption temperature of the gas adsorbed on the surface can be measured by refrigerating, and the trend that the gas release amount of the sample changes along with the temperature at different heating rates can be measured.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic structural view of a mechanism for measuring a outgassing rate of a metallic material;
FIG. 2 is a sectional view of a mechanism for measuring a gas release rate of a metal material;
FIG. 3 is a schematic view of the spacer sleeve;
FIG. 4 is a cross-sectional view of a distance tube.
Description of reference numerals: 1. a vacuum chamber; 2. a sample stage; 3. a quadrupole mass spectrometer; 4. an isolation sleeve; 5. an air inlet; 6. a connecting flange; 7. a bellows; 8. a liquid nitrogen pipe; 9. connecting a pipeline; 10. a connecting member; 11. a vacuum pump; 12. a vacuum gauge; 13. an observation window; 14. a sample delivery pipeline; 15. a standby pipeline; 16. an air guide duct.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a metal material outgassing rate measuring mechanism, as shown in fig. 1 to 4, which comprises a vacuum chamber 1 and a gas measuring device, wherein a sample stage 2 for fixing a sample is arranged in the vacuum chamber 1, the gas inlet end of the gas measuring device is hermetically connected with a separation sleeve 4, the end of the separation sleeve 4 is provided with a gas inlet 5, and the shape and the size of the gas inlet 5 can be flexibly selected, preferably 2 to 4mm, and can be in other sizes; the separating sleeve 4 extends into the vacuum chamber 1, the air inlet holes 5 need to be close to the surface of the sample as much as possible during detection, and preferably the air inlet holes 5 need to be close to the surface of the sample within 1mm during detection, so that the interference of air release of other components and devices in the vacuum chamber 1 can be eliminated through the separating sleeve 4 and the air inlet holes 5, and the measured gas is ensured to come from the sample. As a preferable arrangement, referring to fig. 1 and 2, the vacuum chamber 1 is a cylindrical structure, the sample stage 2 is vertically suspended at the center of the vacuum chamber 1, the fixing surface of the sample stage 2 for fixing the sample is perpendicular to the horizontal plane, the gas measuring device is located at one side of the vacuum chamber 1, the separation sleeve 4 is horizontally extended into the vacuum chamber 1, and the gas inlet 5 is perpendicular to the fixing surface of the sample stage 2. The sample is small, preferably 10mm x 10mmm x 1mm (length x width x thickness), because the sample is small in size, the air release rate of different positions of the same sample can be measured, a plurality of samples can be arranged at the same time, and the like, and the size of the sample is not limited to the above size. Of course, the vacuum chamber 1, the gas measuring device, the isolation sleeve 4, and the like are only used as a reference in a preferred manner, and are not limited to this arrangement manner, if other manners can measure the gas release rate of the sample, for example, the fixing surface of the sample stage 2 is arranged upward, i.e., parallel to the horizontal plane, and the isolation sleeve 4 extends downward from the top to the top of the fixing surface of the sample stage 2, and of course, other arrangement manners are provided, which are not described herein again.
In this embodiment, as shown in fig. 1 to 4, the gas measuring apparatus includes a quadrupole mass spectrometer 3, and the isolation sleeve 4 is hermetically connected to an ionizer of the quadrupole mass spectrometer 3, and when a sample is measured, differential pumping is formed in the isolation sleeve 4, so that gas released from the sample is sucked into the ionizer, and after being processed by the ionizer, the gas is sent into the quadrupole mass spectrometer 3 for analysis.
Further, in this embodiment, as shown in fig. 1 to 4, the end of the isolation sleeve 4 close to the sample is a conical head, the air inlet hole 5 is disposed at the tip of the conical head, the conical head can effectively isolate the gas except the sample, and meanwhile, the conical head is also easy to form a pressure difference, so that the gas of the sample outside the air inlet hole 5 can more easily enter the isolation sleeve 4.
In this embodiment, as shown in fig. 1 to 4, a gas inlet pipe is arranged on the vacuum chamber 1, the pipe orifice of the gas inlet pipe and the quadrupole mass spectrometer 3 are respectively and hermetically connected with a connecting flange 6, a corrugated pipe 7 is hermetically connected between the two connecting flanges 6, the ionizer of the quadrupole mass spectrometer 3 and the isolation sleeve 4 of the front section of the ionizer are both located in the corrugated pipe 7, and the end of the isolation sleeve 4 extends into the vacuum chamber 1. The two connecting flanges 6 and the corrugated pipe 7 form a telescopic sealing channel, when the quadrupole mass spectrometer 3 is moved back and forth, the corrugated pipe 7 can be compressed or stretched, so that the distance between the air inlet hole 5 of the isolation sleeve 4 and the surface of the sample can be adjusted, and meanwhile, the corrugated pipe 7 can ensure the sealing property between the vacuum chamber 1 and the quadrupole mass spectrometer 3.
Further, in the present embodiment, the quadrupole mass spectrometer 3 is mounted on a position adjusting mechanism, and the distance between the gas inlet 5 and the sample surface can be adjusted by the position adjusting mechanism. If quadrupole mass spectrometer 3 sets up in one side of vacuum chamber 1, then can set up a one-dimensional platform on the position control mechanism, install quadrupole mass spectrometer 3 after on the one-dimensional platform, can drive quadrupole mass spectrometer 3 back-and-forth movement through the one-dimensional platform to the distance of 5 distance sample surfaces of inlet port of adjustment isolating sleeve 4. A positioning system can be arranged on the one-dimensional platform, so that the distances between the air inlet 5 and the surface of the sample are consistent during each measurement.
In this embodiment, as shown in fig. 1 to 4, a heater and a liquid nitrogen tube 8 are arranged in a sample stage 2, a connecting pipeline 9 is arranged at the top of a vacuum chamber 1, a connecting piece 10 is hermetically connected in the connecting pipeline 9, one end of the connecting piece 10 is connected with the heater and the liquid nitrogen tube 8, and the other end is connected with an external temperature control system; the vacuum chamber 1 is further provided with an air guide duct 16, which is communicated with an external air guide device through the air guide duct 16. After a heater and a liquid nitrogen tube 8 are arranged on the sample platform 2, the measuring device has two measuring functions of air release rate and air suction rate.
Firstly, air bleeding rate measurement:
and (3) measuring the gas release rate of the sample: after vacuum chamber 1 is vacuumized, the heater is controlled by an external temperature control system to rapidly heat the sample on sample stage 2 to remove gas adsorbed on the surface of the sample, then the temperature is reduced to room temperature or other required temperatures, the sample is heated at a certain rate of heating speed as required, and the change of the outgassing amount of various gases along with the temperature is measured while heating. Finally, the difference of the air release amount among different samples can be compared by integrating the air release amount of all different temperatures. In addition, the gas release conditions of different gases at different temperatures are recorded, so that the gas release amounts of different gases at different temperatures can be compared, and more information can be obtained.
Secondly, measuring the air suction rate: after vacuum chamber 1 evacuation, supply liquid nitrogen in liquid nitrogen pipe 8 through external temperature control system, cool the sample to the liquid nitrogen temperature, and simultaneously through external gas guide equipment, gas guide pipeline 16 supplies gas in vacuum chamber 1, the gas guide pipeline is pressed close to the sample, make the sample can breathe in fast and do not destroy the vacuum of super high vacuum wall, after breathing in the completion, can heat the sample again under external temperature control system control, make the gaseous release of absorption in the sample, and be collected and the analysis by the gas survey device, thereby can measure the desorption condition of gas on the sample along with temperature variation, can obtain the suction rate of sample.
Preferably, the heater can adopt a resistance heating mode or an electron bombardment heating (E-beam) mode, and can realize large-range accurate temperature control by combining with PID (proportion integration differential) algorithm control: the temperature range is from the lowest temperature of 100K (173 ℃ below zero) to the highest temperature of 2000 ℃, the temperature precision is 0.1 ℃, and the maximum temperature rise speed can be more than 4 ℃ per second.
Further, in this embodiment, a temperature measurement probe connected to the sample is disposed on the sample stage 2, the temperature measurement probe is connected to an external temperature control system, and the temperature measurement probe obtains real-time temperature information of the sample.
Further, in this embodiment, the external temperature control system is connected to the computer, the computer can process the temperature information measured by the temperature measuring probe, and the external temperature control system controls the heating power of the heater to control the heating temperature, the heating rate, the heating time, and the like of the sample.
In the present embodiment, as shown in fig. 1 to 4, the vacuum chamber 1 is provided with a vacuum pump 11 and a vacuum gauge 12, and one or more sets of vacuum pumps 11 may be provided. Referring to fig. 1, the present embodiment employs a set of vacuum pumps 11, and the vacuum pump 11 is disposed at the bottom of the vacuum chamber 1, and a vacuum gauge 12 is disposed at the top of the vacuum chamber 1 and extends into the vacuum chamber 1, and the vacuum degree inside the vacuum chamber 1 can be constantly monitored by the vacuum gauge 12. Preferably, the vacuum degree in the vacuum chamber 1 is 10 before the sample measurement is performed-10In the mbar range.
In this embodiment, as shown in fig. 1 to 4, a sample feed pipe 14 for hermetically connecting to a sample transport mechanism is provided on a side wall of the vacuum chamber 1. After the vacuum chamber 1 is vacuumized, the sample can be conveyed to the sample stage 2 by the sample conveying mechanism, and the sample is fixed on the sample stage 2.
In the present embodiment, as shown in fig. 1 to 4, an observation window 13 for observing the sample is further provided on the side wall of the vacuum chamber 1 to observe the inside condition of the vacuum chamber 1 at any time and whether the sample is mounted in place when the sample is mounted on the sample stage 2 by the sample conveying mechanism.
In this embodiment, as shown in fig. 1 to 4, the side wall of the vacuum chamber 1 is further provided with a spare pipe 15, which can be upgraded for other applications, and can perform other functions, such as connecting other devices, and it is necessary to seal the vacuum chamber before it is disconnected.
Example 2
The embodiment discloses a method for measuring the outgassing rate of a metal material, as shown in fig. 1 to 4, the method for measuring the outgassing rate of the metal material adopts the mechanism for measuring the outgassing rate of the metal material, and comprises the following steps:
s1, vacuumizing the vacuum chamber 1, heating the baking vacuum chamber 1 for degassing, wherein the baking temperature is at least 120 ℃, and stopping baking after at least 48 hours until 10 min is obtained-10Vacuum degree in mbar magnitude;
s2, placing a sample to be detected on the sample table 2, and adjusting the position of the quadrupole mass spectrometer 3 to enable the air inlet 5 of the isolation sleeve 4 to be close to the surface of the sample, wherein the distance between the air inlet 5 and the surface of the sample is required to be within 1 mm;
and S3, heating the sample (or not heating) according to the requirement, starting the quadrupole mass spectrometer 3 at the same time, collecting the sample gas, and recording the outgassing gas and the type of the sample at a specific temperature and the variation of the outgassing amount of the sample with time, or the variation trend of the outgassing amount of each gas of the sample with the temperature at a specific temperature rising rate.
By the method, the measurement of the material content of the metal sample bulk gas (mainly hydrogen, helium and the like) can be obtained, and the degassing rate of the material can be influenced by the content. The purpose of heating is mainly to release gas in the sample material, so that the gas release rate of the material phase can be measured.
Further, this embodiment also discloses a method for measuring the air intake rate of a metal material, as shown in fig. 1 to 4, the method using the mechanism for measuring the air discharge rate of a metal material includes the following steps:
s1, vacuum chamber 1 is pumpedVacuum and heating the baking vacuum chamber 1 for degassing at a baking temperature of at least 120 ℃ and stopping baking after at least 48 hours until 10-10Vacuum degree in mbar magnitude;
s2, placing a sample to be detected on the sample table 2, performing liquid nitrogen refrigeration on the sample as required, controlling the sample to be at a proper temperature through external PID, enabling an air guide pipe of an air guide device to be close to the sample through a one-dimensional translation table, starting an external air guide device, supplying air to the surface of the sample through an air guide pipeline 16, stopping supplying air after a certain time, moving out the air guide pipe and vacuumizing again when the vacuum degree of a vacuum chamber is obviously increased;
s3, adjusting the position of the quadrupole mass spectrometer 3 to enable the air inlet 5 of the isolation sleeve 4 to be close to the surface of the sample, wherein the distance between the air inlet 5 and the surface of the sample is required to be within 1 mm;
and S4, heating the sample at a certain heating rate according to the requirement, starting the quadrupole mass spectrometer 3 at the same time, collecting the concerned sample gas, and recording the desorption condition of the gas on the sample measured along with the temperature change, thus obtaining the gas absorption rate of the sample.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. The utility model provides a metal material outgassing rate survey mechanism, its characterized in that includes vacuum chamber, gaseous survey device, be provided with the sample platform that is used for fixed sample in the vacuum chamber, the inlet end of gaseous survey device is equipped with additional and stretches into the inside isolating sleeve of vacuum chamber, the inlet port that is used for being close to is seted up to the end of isolating sleeve the sample surface is collected the sample releases gaseously.
2. The mechanism of claim 1, wherein the gas measuring device comprises a quadrupole mass spectrometer, and the isolation sleeve is hermetically connected to an ionizer of the quadrupole mass spectrometer.
3. The mechanism as claimed in claim 2, wherein the end of the isolation sleeve close to the sample is a cone, and the air inlet is disposed at the tip of the cone.
4. The mechanism of claim 2 or 3, wherein the vacuum chamber is provided with a gas inlet pipe into which the isolation sleeve extends, the gas inlet pipe and the quadrupole mass spectrometer are provided with connecting flanges, a bellows is hermetically connected between the two connecting flanges, and the ionizer is located inside the bellows.
5. A mechanism according to claim 4, wherein said quadrupole mass spectrometer is mounted on a position adjusting mechanism, and the distance between said gas inlet and the surface of said sample can be adjusted by said position adjusting mechanism.
6. The mechanism of claim 1, wherein a heater and a liquid nitrogen tube are disposed in the sample stage, and the vacuum chamber is provided with a connecting pipe for connecting the heater and the liquid nitrogen tube with an external temperature control system and an air guide pipe for communicating with an external air guide device.
7. The mechanism of claim 1, wherein the vacuum chamber is provided with a vacuum pump for evacuating the inside thereof and a vacuum gauge extending into the vacuum chamber.
8. The mechanism of claim 7, wherein the vacuum chamber is provided with a sample delivery pipe for hermetically connecting to the sample delivery mechanism.
9. The mechanism of claim 7, wherein the vacuum chamber further has an observation window for observing the sample.
10. A method for measuring a metal material outgassing rate, using a metal material outgassing rate measuring mechanism according to any one of claims 1 to 9, comprising the steps of:
s1, vacuumizing the vacuum chamber, heating and baking the vacuum chamber, wherein the baking temperature is at least 120 ℃, and the baking is stopped after at least 48 hours, so that the baking is carried out for 10-10Vacuum degree in mbar magnitude;
s2, placing a sample to be measured on the sample stage, and adjusting the position of the gas measuring device to enable the gas inlet hole to be close to the surface of the sample;
and S3, heating the sample as required, starting the gas measuring device to collect the sample gas, and recording the change of the outgassing gas and the type of the sample at a specific temperature and the outgassing amount of the sample along with time, or the trend of the outgassing amount of each gas of the sample along with the change of the temperature at a specific temperature rising rate.
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