CN114113285B - Metal material gassing rate measuring mechanism and measuring method thereof - Google Patents

Metal material gassing rate measuring mechanism and measuring method thereof Download PDF

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CN114113285B
CN114113285B CN202111491730.2A CN202111491730A CN114113285B CN 114113285 B CN114113285 B CN 114113285B CN 202111491730 A CN202111491730 A CN 202111491730A CN 114113285 B CN114113285 B CN 114113285B
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sample
gas
vacuum chamber
rate
metal material
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CN114113285A (en
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赵萍
张建阳
陈克琳
郝亚伟
陈军
石岩
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Institute of Materials of CAEP
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating 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
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/30Nuclear fission reactors

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  • General Health & Medical Sciences (AREA)
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  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses a metal material gassing rate measuring mechanism, which belongs to the technical field of gassing rate measuring devices, and comprises a vacuum chamber and a gas measuring device, wherein a sample table is arranged in the vacuum chamber; the invention also discloses a method for measuring the gassing 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 a sample table, and enabling the air inlet hole to be close to the surface of the sample; s3, heating or refrigerating the sample according to the requirement, starting a gas measuring device to collect gas desorbed from the sample, recording the time change condition of the gas release amount of the sample at a specific temperature or the trend of the gas release amount of the sample at a specific temperature rising rate along with the temperature change, and ensuring that the gas inlet of the gas inlet is only the gas released by the sample under the action of the isolating sleeve, so that the gas release rate of the surface or bulk phase of the material is accurately measured.

Description

Metal material gassing rate measuring mechanism and measuring method thereof
Technical Field
The invention relates to the technical field of deflation rate testing devices, in particular to a metal material deflation rate measuring mechanism and a metal material deflation rate measuring method.
Background
Some high-precision analysis and detection equipment such as synchronous radiation, an electron microscope and XPS all need an ultrahigh vacuum environment when in use, and one of the important conditions for achieving the ultrahigh vacuum environment is that the material deflation rate for manufacturing the analysis and detection equipment is required to be low enough so as to avoid that the vacuum degree is influenced by the deflation of the material for manufacturing the analysis and detection equipment, and the resolution of detection results is reduced. The present method for detecting the gassing rate of the stainless steel material is to roll the stainless steel plate into a cylinder, then weld a round bottom on the bottom surface of the cylinder, weld a standard knife edge flange with a diameter CF200 on the top surface of the cylinder, and form a sealed cavity, then open a plurality of knife edge flanges with a CF35 size on the cavity, and the flanges are used for connecting various pump sets, precise vacuum gauges, valves, residual gas analyzers and the like. When the detection is carried out, the vacuum pump is used for vacuumizing the cavity, after the vacuumizing is finished, the whole system is subjected to degassing treatment, then the gas in the bulk phase is removed through higher-temperature baking, and the gas enters the cavity where the residual gas analyzer is located through the leak hole for detection.
However, in the above detection method, although the baking oven is used to bake and degas the detection device, the discard rate of two different materials is compared, so that a lot of materials are needed, and the materials are needed to be made into a cavity, the smoothness of the interior of the cavity is required to be ensured to be consistent in the process, the whole large cavity is required to be heated in a laboratory, the heating speed is slow, and the highest temperature is limited. In addition, as the leak detection is needed to be carried out on the new cavity every time, the sealing of all flanges and interfaces is ensured to be good. In addition, in the detection process, the gas outside the cylinder can possibly infiltrate into the steel, and under the condition that the inside of the steel cylinder is vacuumized, the rate of the external gas infiltrating into the cylinder material can be accelerated, so that the gas release rate detected inside 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, named as 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, a sample inlet and outlet chamber and a molecular pump, wherein the sample inlet and outlet chamber is communicated with an air discharge performance testing chamber of the air discharge testing system, the air discharge testing system and the sample inlet and outlet chamber are vacuumized through the molecular pump during testing, and then a sample is sent into the air discharge performance testing chamber to be tested by an air discharge sample sending rod in the sample inlet and outlet chamber, and the air discharge rate of the tested sample can be prevented from being interfered by external air through vacuumizing the air discharge testing system. However, although the above patent provides a vacuum environment for the sample to avoid the interference of external air, the material of the deflation test system, the sample inlet and outlet chamber and the molecular pump has a deflation rate, and even if the whole device is dried and degassed, the gas is still remained, and after the vacuum is pumped, the residual gas is released, so that the final measurement result is affected.
Disclosure of Invention
The invention aims to solve the technical problems, and provides a metal material gassing rate measuring mechanism and a measuring method thereof, wherein under the action of an isolating sleeve, gas except a sample in a vacuum chamber can be isolated, and after an air inlet hole is close to the surface of the sample, the gas can be ensured to come from the sample completely, so that the interference of external gas is avoided, and the gassing rate accuracy is improved.
In order to achieve the above object, the present invention provides the following solutions: the invention provides a metal material gassing rate measuring mechanism which comprises a vacuum chamber and a gas measuring device, wherein a sample table for fixing a sample is arranged in the vacuum chamber, an air inlet end of the gas measuring device is connected with an isolation sleeve extending into the vacuum chamber in a sealing manner, and an air inlet hole for collecting gas released by the sample and approaching to the surface of the sample is formed in the end of the isolation sleeve.
Preferably, the gas measurement 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, which is close to the sample, is a conical head, and the air inlet hole is arranged on the tip end of the conical body.
Preferably, the vacuum chamber is provided with an air inlet pipeline into which the isolation sleeve extends, the air inlet pipeline and the quadrupole mass spectrometer are respectively provided with a connecting flange, a corrugated pipe is connected between the two connecting flanges in a sealing way, and the ionizer is positioned inside the corrugated pipe.
Preferably, the quadrupole mass spectrometer is mounted on a position adjustment mechanism by which the distance of the inlet aperture from the sample surface can be adjusted.
Preferably, the sample stage is internally provided with a heater and a liquid nitrogen pipe, and the vacuum chamber is provided with a connecting pipeline for connecting the heater and the liquid nitrogen pipe with an external temperature control system and an air guide pipeline communicated with external air guide equipment.
Preferably, a temperature measuring probe connected with the sample is arranged on the sample table, 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 with 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 and the like of the heater so as 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 vacuumizing the interior of the vacuum chamber and a vacuum gauge extending into the interior of the vacuum chamber.
Preferably, the vacuum chamber is provided with a sample delivery pipeline for sealing connection with the sample delivery mechanism.
Preferably, an observation window for observing the sample is further arranged on the vacuum chamber.
The invention also discloses a metal material gassing rate measuring method, which adopts the metal material gassing rate measuring mechanism and comprises the following steps:
s1, vacuumizing the vacuum chamber, heating and baking the vacuum chamber, wherein the baking temperature is at least 120 ℃ for at least 48 hoursAfter stopping baking, realize 10 -10 Vacuum degree of mbar magnitude;
s2, placing a sample to be detected on the sample table, and adjusting the position of the gas measuring device to enable the air inlet hole to be close to the surface of the sample;
s3, heating the sample according to the need, starting the gas measuring device to collect the sample gas, and recording the gas release quantity of the sample at a specific temperature, the type and the time change condition of the gas release quantity of the sample, or the trend of the gas release quantity of the sample at a specific temperature rise rate along with the temperature change.
Compared with the prior art, the invention has the following technical effects:
1. according to the invention, the vacuum chamber can provide an ultrahigh vacuum environment for the sample, so that the interference of external gas can be avoided, and conditions are created for sample deflation; the gas inlet end of the gas measuring device is sealed with the isolation sleeve, gas except the sample in the vacuum chamber can be isolated outside, 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 released from the sample, so that the measuring accuracy of the sample gassing rate is improved.
2. According to the invention, the heater, the liquid nitrogen pipe and the temperature measuring probe are arranged in the sample table, and the air inlet equipment arranged on the equipment is combined, so that the measuring mechanism has two measuring functions of material air release rate and air suction rate; when the gas release rate is measured, the sample is heated by a heater according to the material of the sample in the ultra-vacuum environment so as to promote the gas in the sample to be released, the accurate measurement of the gas release rate of the sample phase along with the temperature change can be realized, when the gas release rate is measured, the sample is firstly refrigerated to the liquid nitrogen temperature by a liquid nitrogen pipe in the ultra-vacuum environment, then the gas is closely attached to the sample by an external gas guide device and a telescopic gas guide pipeline, the gas is fed into a room so as to promote the sample to adsorb the fed gas, the gas is stopped after a certain time, the gas is pumped again, then the gas is heated again, and meanwhile, the gas released by the sample is collected and analyzed by a gas measuring device, so that the gas release rate, namely the gas release rate of the sample, is measured.
3. According to the invention, the vacuum chamber is in sealing connection with the sample conveying mechanism through the sample conveying pipeline, and 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, so that the vacuum chamber is ensured to always maintain ultrahigh vacuum.
4. In the invention, the vacuum chamber is heated and baked firstly, the vacuum chamber and other devices in the vacuum chamber can be baked and degassed, and the measurement of the sample deflation rate by the deflation interference of other mechanisms is avoided; then after vacuumizing, the sample is heated, refrigerated or kept at normal temperature according to the characteristics of the sample material, and the gas in the deep layer inside the sample is heated and can be promoted to be released instead of the gas on the surface, so that the gas release rate of the bulk phase of the material can be measured, the gas suction property of the surface of the sample, the adsorption temperature of the gas adsorbed on the surface and the like can be measured through refrigeration, and the trend of the gas release amount of the sample along with the temperature change under different heating rates can be measured.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a metal material gassing rate measuring mechanism;
FIG. 2 is a cross-sectional view of a metal material gassing rate measuring mechanism;
FIG. 3 is a schematic view of the construction of an isolation sleeve;
fig. 4 is a cross-sectional view of the spacer sleeve.
Reference numerals illustrate: 1. a vacuum chamber; 2. a sample stage; 3. a quadrupole mass spectrometer; 4. an isolation sleeve; 5. an air inlet hole; 6. a connecting flange; 7. a bellows; 8. a liquid nitrogen pipe; 9. a connecting pipe; 10. a connecting piece; 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 pipeline.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a metal material gassing rate measuring mechanism, as shown in fig. 1 to 4, which comprises a vacuum chamber 1 and a gas measuring device, wherein a sample table 2 for fixing a sample is arranged in the vacuum chamber 1, the gas inlet end of the gas measuring device is connected with a separation sleeve 4 in a sealing way, the end of the separation sleeve 4 is provided with an air inlet hole 5, the shape and the size of the air inlet hole 5 can be flexibly selected, and the shape and the size of the air inlet hole 5 can be preferably 2-4 mm, and can also be of other sizes; the isolation sleeve 4 stretches into the vacuum chamber 1, the air inlet hole 5 needs to be close to the surface of the sample as much as possible during detection, preferably the air inlet hole 5 needs 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 discharged through the isolation sleeve 4 and the air inlet hole 5, and the measured air is ensured to come from the sample. As a preferred arrangement, referring to fig. 1 and 2, the vacuum chamber 1 is in a cylindrical structure, the sample stage 2 is vertically suspended in the center of the vacuum chamber 1, the fixing surface of the sample stage 2 for fixing the sample is vertical to the horizontal plane, the gas measuring device is located at one side of the vacuum chamber 1, the isolation sleeve 4 horizontally extends into the vacuum chamber 1, and the air inlet hole 5 is vertical to the fixing surface of the sample stage 2. The sample is small, and the size is preferably 10mm x 1mm (length x width x thickness), because the sample size is small, the air release rate of different positions of the same sample can be measured, and a plurality of samples can be simultaneously arranged, and the like, and the sample size 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 preferred mode, and are not limited to this mode, if other modes can realize the measurement of the sample deflation rate, for example, the fixing surface of the sample stage 2 is arranged upwards, that is, parallel to the horizontal plane, and the isolation sleeve 4 extends downwards from the top to the top of the fixing surface of the sample stage 2, and of course, other modes are not described herein.
In this embodiment, as shown in fig. 1 to 4, the gas measurement device includes a quadrupole mass spectrometer 3, the isolation sleeve 4 is hermetically connected to an ionizer of the quadrupole mass spectrometer 3, and when a sample is measured, a differential pump is formed in the isolation sleeve 4, so that the gas released from the sample is sucked into the ionizer, and after being processed by the ionizer, 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 on the tip of the conical head, the conical head can effectively isolate the gas except the sample, and meanwhile, the conical head is 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, an air inlet pipe is disposed on the vacuum chamber 1, a pipe orifice of the air inlet pipe and the quadrupole mass spectrometer 3 are respectively and hermetically connected with a connecting flange 6, a bellows 7 is hermetically connected between the two connecting flanges 6, an ionizer of the quadrupole mass spectrometer 3 and an isolation sleeve 4 at the front section of the ionizer are both disposed in the bellows 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, and 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 a sample can be adjusted, and the corrugated pipe 7 can ensure the tightness 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 by which the distance between the air inlet aperture 5 and the sample surface can be adjusted. If the quadrupole mass spectrometer 3 is arranged at one side of the vacuum chamber 1, a one-dimensional platform can be arranged on the position adjusting mechanism, and after the quadrupole mass spectrometer 3 is arranged on the one-dimensional platform, the quadrupole mass spectrometer 3 can be driven to move back and forth by the one-dimensional platform, so that the distance between the air inlet hole 5 of the isolation sleeve 4 and the surface of the sample can be adjusted. A positioning system can be arranged on the one-dimensional platform to ensure that the distance between the air inlet 5 and the surface of the sample is consistent during each measurement.
In this embodiment, as shown in fig. 1 to 4, a heater and a liquid nitrogen pipe 8 are arranged in the sample stage 2, a connecting pipe 9 is arranged at the top of the vacuum chamber 1, a connecting piece 10 is connected in the connecting pipe 9 in a sealing manner, one end of the connecting piece 10 is connected with the heater and the liquid nitrogen pipe 8, and the other end is connected with an external temperature control system; the vacuum chamber 1 is also provided with an air guide pipeline 16, and is communicated with external air guide equipment through the air guide pipeline 16. After the heater and the liquid nitrogen pipe 8 are arranged on the sample table 2, the measuring device has two measuring functions of the deflation rate and the aspiration rate.
1. And (3) measuring the air release rate:
sample phase gassing rate determination: after the vacuum chamber 1 is vacuumized, the external temperature control system controls the heater to rapidly heat the sample on the sample table 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 temperature rise speed according to the requirements, and the change condition of the gassing amount of various gases along with the temperature is measured while the sample is heated. Finally, by integrating all the gassing amounts at different temperatures, the difference in gassing amounts between different samples can be compared. In addition, the deflation conditions of different gases with different temperatures are recorded, so that the deflation amounts of different gases at different temperatures can be compared, and more information can be obtained.
2. Measurement of the inspiration rate: after the vacuum chamber 1 is vacuumized, liquid nitrogen is supplied into the liquid nitrogen pipe 8 through an external temperature control system, the sample is cooled to the liquid nitrogen temperature, and gas is supplied into the vacuum chamber 1 through external gas guide equipment and a gas guide pipeline 16, the gas guide pipeline is close to the sample, so that the sample can be quickly sucked without damaging the vacuum of an ultrahigh vacuum wall, after the suction is completed, the sample can be heated again under the control of the external temperature control system, adsorbed gas in the sample is promoted to be released, and the gas is collected and analyzed by a gas measuring device, so that the desorption condition of the gas on the sample along with the temperature change can be measured, and the suction rate of the sample can be obtained.
Preferably, the heater can adopt a resistance heating mode or an electron bombardment heating (E-beam) mode, and can realize a wide range of temperature accurate control by combining PID (Proportion Integral Differential) algorithm control: the temperature ranges from a minimum temperature of 100K (minus 173 ℃ C.) to a maximum temperature of 2000 ℃ C. With a temperature accuracy of 0.1 ℃ C. And a maximum heating rate of greater than 4 ℃ per second.
Further, in this embodiment, a temperature measurement probe connected to the sample is disposed on the sample stage 2, and the temperature measurement probe is connected to an external temperature control system, so as to obtain real-time temperature information of the sample.
Further, in this embodiment, the external temperature control system is connected to the computer, and the computer is capable of processing the temperature information measured by the temperature measurement probe, and controlling the heating power of the heater by the external temperature control system, so as to control the heating temperature, the heating rate, the heating time, and the like of the sample.
In this embodiment, as shown in fig. 1 to 4, a vacuum pump 11 and a vacuum gauge 12 are provided on the vacuum chamber 1, 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 sets the vacuum pumps 11 at the bottom of the vacuum chamber 1, and a vacuum gauge 12 is provided 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 monitored at all times by the vacuum gauge 12. Preferably, the vacuum in the vacuum chamber 1 is 10 before the sample measurement is performed -10 In the order of mbar.
In this embodiment, as shown in fig. 1 to 4, a sample feeding pipe 14 for sealing connection with a sample feeding mechanism is provided on a side wall of the vacuum chamber 1. After the vacuum chamber 1 is evacuated, a sample can be transported to the sample stage 2 by the sample transport mechanism, and the sample is fixed on the sample stage 2.
In this 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 internal condition of the vacuum chamber 1 at any time, and whether the sample is mounted in place when mounted on the sample stage 2 by the sample conveying mechanism.
In this embodiment, as shown in fig. 1 to 4, a standby pipe 15 is further provided on the side wall of the vacuum chamber 1, which can be used for other applications to upgrade, and to realize other functions, such as connecting other devices, etc., and sealing is required before disconnection.
Example 2
The embodiment discloses a metal material gassing rate measuring method, as shown in fig. 1 to 4, adopting the metal material gassing rate measuring mechanism, comprising the following steps:
s1, vacuumizing the vacuum chamber 1, heating and baking the vacuum chamber 1 to degas, baking at a temperature of at least 120 ℃ and stopping baking after at least 48 hours until 10 is obtained -10 Vacuum degree of 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 an air inlet hole 5 of the isolation sleeve 4 to be close to the surface of the sample, wherein the distance between the air inlet hole 5 and the surface of the sample is required to be within 1 mm;
and S3, heating the sample according to the need (or not), starting the quadrupole mass spectrometer 3 at the same time, collecting the sample gas, and recording the gas release and the type of the sample at a specific temperature and the change condition of the gas release amount of the sample with time, or the trend of the gas release amounts of the sample at a specific temperature rise rate with the change of the temperature.
By the method, the measurement of the content of the bulk gas (mainly hydrogen, helium and the like) of the metal sample in the material can be obtained, and the content of the bulk gas can influence the degassing rate of the material. The heating purpose is mainly to release the gas inside the sample material, so as to realize the measurement of the gassing rate of the material phase.
Further, this embodiment also discloses a method for measuring the air suction rate of a metal material, as shown in fig. 1 to 4, using the above-mentioned mechanism for measuring the air discharge rate of a metal material, comprising the following steps:
s1, vacuumizing the vacuum chamber 1, heating and baking the vacuum chamber 1 to degas, baking at a temperature of at least 120 ℃ and stopping baking after at least 48 hours until 1 is obtained0 -10 Vacuum degree of mbar magnitude;
s2, placing a sample to be tested on a sample table 2, refrigerating the sample by liquid nitrogen according to the requirement, controlling the sample to a proper temperature by an external PID (proportion integration differentiation), enabling an air duct of an air guide device to be close to the sample by a one-dimensional translation table, starting the external air guide device, supplying air to the surface of the sample by an air duct 16, stopping air supply when the vacuum degree of a vacuum chamber is found to be obviously increased after a certain time, removing the air duct, and vacuumizing again;
s3, adjusting the position of the quadrupole mass spectrometer 3 to enable the air inlet hole 5 of the isolation sleeve 4 to be close to the surface of the sample, wherein the distance between the air inlet hole 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 gas of the sample of interest, and recording the desorption condition of the gas on the sample measurement sample along with the temperature change, so that the air suction rate of the sample can be obtained.
The principles and embodiments of the present invention have been described in detail with reference to specific examples, which are provided to facilitate understanding of the method and core ideas of the present invention; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.

Claims (7)

1. The utility model provides a metal material gassing rate survey mechanism, its characterized in that includes vacuum chamber, gas measuring device, be provided with the sample platform that is used for fixed sample in the vacuum chamber, gas measuring device's inlet end adds to be equipped with and stretches into the inside isolation sleeve of vacuum chamber, the end of isolation sleeve is offered and is used for being close to the sample surface and collect the inlet port of sample release gas, gas measuring device includes the quadrupole mass spectrometer, isolation sleeve sealing connection is in on the ionizer of quadrupole mass spectrometer, be equipped with on the vacuum chamber and supply the admission line that the 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 ionizer is located inside the bellows, the quadrupole mass spectrometer is installed on position adjustment mechanism, through position adjustment mechanism can adjust the inlet port with the distance of sample surface, the quadrupole mass spectrometer is installed on position adjustment mechanism can be adjusted through position adjustment mechanism the inlet port with the distance of sample surface, the position adjustment mechanism can be passed through on the position adjustment mechanism.
2. The mechanism of claim 1, wherein the end of the isolating sleeve adjacent to the sample is a conical head, and the air inlet is arranged on the tip of the conical head.
3. The metal material gassing rate measuring mechanism according to claim 1, wherein the sample stage is internally provided with a heater and a liquid nitrogen pipe, and the vacuum chamber is provided with a connecting pipeline for connecting the heater and the liquid nitrogen pipe with an external temperature control system and an air guide pipeline communicated with an external air guide device.
4. The mechanism for measuring the gassing rate of metal materials according to claim 1, wherein the vacuum chamber is provided with a vacuum pump for evacuating the inside of the vacuum chamber and a vacuum gauge extending into the inside of the vacuum chamber.
5. The mechanism for measuring the gassing rate of metal materials according to claim 4, wherein the sample feeding pipeline for sealing connection with the sample feeding mechanism is arranged on the vacuum chamber.
6. The mechanism for measuring the gassing rate of a metal material according to claim 4, wherein the vacuum chamber is further provided with an observation window for observing the sample.
7. A metal material outgassing rate measurement method, employing a metal material outgassing rate measurement mechanism according to any one of claims 1-6, characterized by comprising the steps of:
s1, vacuumizing the vacuum chamber, heating and baking the vacuum chamber, wherein the baking temperature is at least 120 ℃, and stopping baking after at least 48 hours to realize the vacuum degree of 10-10 mbar;
s2, placing a sample to be detected on the sample table, and adjusting the position of the gas measuring device to enable the air inlet hole to be close to the surface of the sample;
s3, heating the sample according to the need, starting the gas measuring device to collect the sample gas, and recording the gas type of the sample at a certain temperature and the change condition of the gas discharge amount of the sample with time, or the trend of the gas discharge amounts of the sample at a certain temperature rising rate with the change of the temperature.
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Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06273383A (en) * 1993-03-17 1994-09-30 Denshi Kagaku Kk Temperature-programmed desorption gas analyzer
JPH09222419A (en) * 1995-12-11 1997-08-26 Toyota Central Res & Dev Lab Inc Device and method for reaction analysis
JPH1183802A (en) * 1997-09-04 1999-03-26 Oki Electric Ind Co Ltd Desorption gas by temperature rise analysis method and apparatus
US5955886A (en) * 1997-07-10 1999-09-21 Pcp, Inc. Microliter-sized ionization device and method
JP2000260750A (en) * 1999-03-08 2000-09-22 Denshi Kagaku Kk Gas analyzer for heated and separated gas
WO2001096852A1 (en) * 2000-06-14 2001-12-20 Mitsubishi Heavy Industries, Ltd Device for detecting chemical substance and method for measuring concentration of chemical substance
JP2002174606A (en) * 2000-12-05 2002-06-21 Rigaku Corp Temperature-programmed desorption analyzer and its method
CN1786704A (en) * 2004-12-08 2006-06-14 上海永新彩色显像管股份有限公司 Method for testing performance of scanning gassing of colour display tube
JP2011232108A (en) * 2010-04-26 2011-11-17 Ngk Insulators Ltd Generated gas analyzing apparatus
DE102013009177A1 (en) * 2012-07-26 2014-01-30 Rigaku Corporation Skimmer type connection structure for use as gas supply structure for differential thermal balance, has tubular body with skimmer portion and arranged extending in direction of flow of carrier gas stream and opening at upstream side end
CN106814125A (en) * 2016-12-08 2017-06-09 中国科学院光电研究院 A kind of material radiation causes the online testing device and method of testing deflated
CN110865002A (en) * 2019-11-17 2020-03-06 北京东方计量测试研究所 High-precision material outgassing rate testing system and testing method thereof
CN112505335A (en) * 2019-09-16 2021-03-16 中国科学院苏州纳米技术与纳米仿生研究所 Ultrahigh vacuum sample transfer equipment and method

Family Cites Families (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3298974B2 (en) * 1993-03-23 2002-07-08 電子科学株式会社 Thermal desorption gas analyzer
JP2002372483A (en) * 2001-04-09 2002-12-26 Toshiba Microelectronics Corp Elimination gas analysis apparatus and method
JP3846800B2 (en) * 2003-08-18 2006-11-15 株式会社リガク Evolved gas analysis method and apparatus
DE10350686A1 (en) * 2003-10-30 2005-06-16 Infineon Technologies Ag Apparatus and method for detecting outgassing products
CN2757131Y (en) * 2004-12-17 2006-02-08 上海永新彩色显像管股份有限公司 High temperature gas discharging property detector for material in display tube
JP4731359B2 (en) * 2006-03-03 2011-07-20 株式会社堀場製作所 Sample vaporizer and ICP analyzer for analyzer
CN104569228B (en) * 2014-12-31 2016-03-16 同方威视技术股份有限公司 A kind of sampling device
RU160431U1 (en) * 2015-05-29 2016-03-20 Общество с ограниченной ответственностью "Энергомаштехника" (ООО "ЭМТ") INSTALLATION FOR MASS-SPECTROMETRIC DETERMINATION OF CHEMICAL COMPOUNDS
CN106404592A (en) * 2016-08-31 2017-02-15 浙江大学 Heat insulation material outgassing rate test device
CN206208685U (en) * 2016-09-22 2017-05-31 南京益东惠电子科技有限公司 A kind of use Dynamic flow methed measures the vacuum measurement system of material outgassing performance
CN206074511U (en) * 2016-09-22 2017-04-05 南京益东惠电子科技有限公司 A kind of Dynamic flow methed measures vacuum device rga system and device
JP6934239B2 (en) * 2017-02-27 2021-09-15 国立大学法人東京工業大学 High-sensitivity temperature rise desorption gas analyzer
CN208091767U (en) * 2017-12-22 2018-11-13 深圳迈瑞生物医疗电子股份有限公司 Sampling probe and sampling needle assemblies
CN208208713U (en) * 2018-06-19 2018-12-07 中国科学院光电研究院 A kind of detection device of high-precision mass spectrum detection limit
JP6919630B2 (en) * 2018-07-30 2021-08-18 三菱電機株式会社 Gas analyzer and gas analysis method
CN112683726A (en) * 2020-12-01 2021-04-20 中国科学院近代物理研究所 Device and method for testing air yield of material
CN112595562B (en) * 2020-12-11 2022-12-06 中国科学院工程热物理研究所 Mass spectrum homothermal in-situ sampling interface capable of being flexibly arranged and mass spectrum homothermal in-situ sampling method
CN113270308B (en) * 2021-05-20 2024-03-12 中国科学院工程热物理研究所 Sampling sleeve capable of preventing dust and removing dust, mass spectrum sampling interface and mass spectrum sampling method

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06273383A (en) * 1993-03-17 1994-09-30 Denshi Kagaku Kk Temperature-programmed desorption gas analyzer
JPH09222419A (en) * 1995-12-11 1997-08-26 Toyota Central Res & Dev Lab Inc Device and method for reaction analysis
US5955886A (en) * 1997-07-10 1999-09-21 Pcp, Inc. Microliter-sized ionization device and method
JPH1183802A (en) * 1997-09-04 1999-03-26 Oki Electric Ind Co Ltd Desorption gas by temperature rise analysis method and apparatus
JP2000260750A (en) * 1999-03-08 2000-09-22 Denshi Kagaku Kk Gas analyzer for heated and separated gas
WO2001096852A1 (en) * 2000-06-14 2001-12-20 Mitsubishi Heavy Industries, Ltd Device for detecting chemical substance and method for measuring concentration of chemical substance
JP2002174606A (en) * 2000-12-05 2002-06-21 Rigaku Corp Temperature-programmed desorption analyzer and its method
CN1786704A (en) * 2004-12-08 2006-06-14 上海永新彩色显像管股份有限公司 Method for testing performance of scanning gassing of colour display tube
JP2011232108A (en) * 2010-04-26 2011-11-17 Ngk Insulators Ltd Generated gas analyzing apparatus
DE102013009177A1 (en) * 2012-07-26 2014-01-30 Rigaku Corporation Skimmer type connection structure for use as gas supply structure for differential thermal balance, has tubular body with skimmer portion and arranged extending in direction of flow of carrier gas stream and opening at upstream side end
CN106814125A (en) * 2016-12-08 2017-06-09 中国科学院光电研究院 A kind of material radiation causes the online testing device and method of testing deflated
CN112505335A (en) * 2019-09-16 2021-03-16 中国科学院苏州纳米技术与纳米仿生研究所 Ultrahigh vacuum sample transfer equipment and method
CN110865002A (en) * 2019-11-17 2020-03-06 北京东方计量测试研究所 High-precision material outgassing rate testing system and testing method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Gas discharge plasma treatment of poly(ethylene glycol-co-1,3/1,4 cyclohexanedimethanol terephthalate) for enhanced paint adhesion;Salapare, HS 等;JOURNAL OF VACUUM SCIENCE & TECHNOLOGY A;第34卷(第4期);第041303页 *
GIC-4117串列加速器***及应用研究;何俊;中国优秀博士学位论文全文数据库工程科技Ⅱ辑(第04期);第C040-1页 *
SECONDARY ION QUADRUPOLE MASS-SPECTROMETER FOR DEPTH PROFILING-DESIGN AND PERFORMANCE EVALUATION;MAGEE, CW 等;REVIEW OF SCIENTIFIC INSTRUMENTS;第49卷(第4期);第477-485页 *

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