JPH06103960A - Spectrometry for infinitesimal amount of gas emitted from deformed and ruptured material - Google Patents

Abstract

PURPOSE:To enable the infinitesimal amount of gas to be analyzed, which is emitted out of material when the material is deformed and ruptured, and thereby verify a cause for brittle tendency by integrally arranging a material testing machine, an ultra high vacuum chamber, an exhaust means and a mass spectrometry in an ultra high vacuum system. CONSTITUTION:A material testing machine 1 capable of making tests for tension, compression and fatigue, a high performance mass spectrometry 4 and a non-volatile getter pump 8 are connected to an ultra high vacuum chamber 2 whose vacuum level. is less than 10<-7>pa. Next, turbo molecular pumps 9a and 9b are connected to an exhaust pipe 6 connected to the chamber 2 via a sputter ion pump 7 and a cut-off valve, and a specimen take-in/out cover 11 is provided for the chamber 2. Namely the machine 1, the chamber 2, the device 3 and the mass spectrometry 4 are integrally arranged in an ultra vacuum system. By this constitution, the ultra trace amount of gas emitted when material is deformed and ruptured, can be analyzed with high accuracy, and concurrently the results of tests are so devised as to be indicated and recorded by a data processing means.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an analyzer for an extremely small amount of gas released from a material when it is deformed or destroyed.
It plays a great role in elucidating the relationship between destruction and gas elements.
The device of the present invention can be applied to basic fields of material physical properties such as elucidation of interactions between hydrogen atoms and dislocations. Also, by using isotopes, it can be mixed from any of the manufacturing, heat treatment, and use environments of materials. It is possible to elucidate whether or not the generated gas adversely affects, and it is a device that gives useful knowledge not only for new materials and other material design but also for safe use of structures.

[Prior art]

An outline of related conventional techniques is as follows. (1) Tensile / compression / fatigue tests of materials under ultra-high vacuum have been performed by separate devices, and the effects of water vapor and hydrogen in the test environment are reported by comparison with the test results in the atmosphere. It has been. However, there is no example of direct analysis of a very small amount of hydrogen gas released from a sample when it is deformed or fractured.

(2) Regarding the gas analysis in the material, there is a thermal desorption gas analyzer for heating the material under high vacuum and analyzing various gas elements released from the material, such as a quadrupole mass spectrometer. It is used to study chamber materials, etc. by the method of analyzing hydrogen gas, etc. However, it is not possible to clarify what gas element is directly involved in the embrittlement of the material because it is not a gas analysis at the time of deformation / breakage.

(3) Detection of hydrogen released when a material is deformed or ruptured can be performed by, for example, Skamanz et al. (Corrosion Science, V
ol.16 (1976), pp.443-459.). Here, a tensile test under 10 ^-3 Pa with an oil diffusion pump and a liquid nitrogen trap was conducted on a sample that had been left in saturated steam for several days to absorb excess hydrogen, and the released hydrogen was measured. It is detecting. However, since hydrogen is not detected when it is not left in water vapor, it is not suitable for detecting a very small amount of hydrogen and other gases already present in the material.

[0005]

As described above, there is no test device for deforming / breaking a material under ultrahigh vacuum and analyzing a gas such as hydrogen gas released at that time. above
It seems that releasing hydrogen released when a material is deformed or broken can be achieved by combining (1) and (2) and developing (3), but this has not been done in the past. The reason is that if there is an operating part such as a tester, it is difficult to achieve an ultra-high vacuum, and even if an ultra-high vacuum is achieved, it is difficult to detect an extremely small amount of gas released from the material. Probably because it was thought.

In reality, however, hydrogen diffuses during the deformation of the material and is segregated at a high concentration in the region where the dislocation density is high, so that it is detected even during the deformation, and at the moment of fracture, an extremely high partial pressure (~ 10
^-6 Pa) was detected. However, the device used by Skamanz et al. Has a low degree of vacuum (10 ^-3 P
a), because of the high sensitivity of the mass spectrometer, etc., it was completely impossible to analyze commercially available materials containing only a very small amount of gas. Therefore, the emergence of a device that can elucidate the embrittlement mechanism of a material and obtain knowledge for preventing the embrittlement has been long awaited.

[0007] Conventional analyzers for trace amounts of gas released from materials during deformation and destruction include a material testing machine equipped with an ultra-high vacuum chamber, a thermal desorption gas analyzer equipped with a high vacuum chamber and a mass spectrometer,
There is a material testing machine equipped with a high vacuum chamber and a mass spectrometer. Gas analysis is not possible, and gas analysis is possible, but it is not an analysis of the gas directly involved in deformation / rupture, but is an analysis of the gas released from the material while raising the temperature. Aims to conduct a material test in a high vacuum of 10 ^-3 Pa created by an oil diffusion pump, and detect a large amount of released hydrogen from a sample exposed to saturated water vapor with a mass spectrometer of ordinary sensitivity. It was done. Therefore, it is impossible for the conventional device to detect the very small amount of hydrogen and other gases already contained in the commercially available material when the material is deformed or ruptured. In fact, hydrogen is not extracted from the sample not exposed to saturated steam. It reports that it was not detected.

[0008]

The present invention relates to an apparatus for analyzing a gas emitted from a material by a high-sensitivity mass spectrometer while deforming or breaking the material in an ultra-high vacuum chamber. Is essentially different from, and enables analysis of a very small amount of gas in a normal material that could not be detected by (is not targeted for detection).

According to the present invention, an ultrahigh vacuum chamber of 10 ^-7 Pa or less is connected to a material tester capable of performing tensile, compression and fatigue tests, a high performance mass spectrometer and a non-evaporating getter pump, and an ultrahigh vacuum is provided. A sputter ion pump was connected to an exhaust pipe connected to the vacuum chamber, and a turbo molecular pump was connected via a shutoff valve, and a lid for sample exchange was provided on the ultra-high vacuum chamber. It is in the analyzer of the trace amount of gas released.

In the analyzer of the present invention, the mass spectrometer 4 preferably has a sample piece, an ion source, an analysis section, and an ion detection section arranged in a linear relationship.

The mass spectrometer of the present invention is close to the connection between the exhaust pipe and the ultra high vacuum chamber, and is about 30 to 60 degrees, preferably 45 degrees.
It is good to install it at a reasonable rate.

[Action]

Embrittlement and fracture due to the interaction between the material and the gas element, such as delayed fracture of steel and environmental embrittlement of ceramics and intermetallic compounds, often cause problems, and are also greatly related to the reliability of structural materials. . However, in the past, it was difficult to analyze the gas at the time of deformation / breakage, so sufficient recognition was not obtained, and there was a problem in its safety and the like. The device of the present invention enables analysis of an extremely small amount of gas released from a material when it is deformed or ruptured by applying compression, tension or fatigue to the material, and directly analyzes the released gas at the time of deformation or rupture. Therefore, the purpose is to demonstrate the cause of embrittlement. Also, whether the gas in question entered during the material preparation stage, the heat treatment stage, or the environment where it was used was identified by using an isotope as a tracer and can be measured. .

An embodiment of the device of the present invention will be described below with reference to the drawings. As shown in FIG. 1, the apparatus of the present invention comprises a material testing machine 1, an ultra-high vacuum chamber 2, an exhaust device 3,
It comprises a quadrupole mass spectrometer 4 and a data analysis processor 5.

In the apparatus of the present invention, an ultrahigh vacuum chamber 2 is attached to surround a test piece held by a jig of a material testing machine 1, and an exhaust device 3 and a quadrupole mass spectrometer 4 are attached to the chamber 2. It is configured by connecting with the data analysis device processing 5.

(1) Material testing machine: As shown in FIG. 3, the material testing machine 1 has a cross head 14 supported by two columns 13 erected on the left and right sides of a base 12 supported by a lifting cylinder 15. A test piece 19 is held between a load cell 17 mounted on the upper crosshead 14 and a piston 18 mounted on the lower table 16 so that the test piece 19 can be moved up and down with respect to a table 16 mounted below the column 13. When the jigs 20 and 20 are attached and the actuator 21 attached to the piston 18 is operated, the test piece 19
It is configured so that it can be deformed or broken by compression or tension. 22 is a clamp cylinder for fixing the crosshead 14, 23 is a vibration-proof pad, and 24 is a door. In the material testing method using the material testing machine 1 shown in FIG. 3, the test piece is mounted between the load cell and the piston via a test piece mounting jig. When hydraulic pressure is applied to the actuator, the piston and lower jig move up or down, pulling and pulling against the test piece.
A compression / fatigue test can be performed.

FIG. 4 is a view showing a state in which the ultrahigh vacuum chamber 2 is attached to the material testing machine 1 used in the present invention.

FIG. 5 is an enlarged view of the main part of FIG.
The jig 20 for holding the test piece 19 is surrounded, the ultra-high vacuum chamber 2 is attached, and the mass spectrometer 4 is attached to the flange 2A provided on one side of the ultra-high vacuum chamber 2.

Since the material testing machine 1 is for deforming and breaking the material, it is sufficient that it can be deformed according to the purpose.
Fatigue fracture also poses a problem in structures, so a servo pulsar from Shimadzu was selected to enable gas analysis during fatigue tests as well as tension and compression (EHF-EB5-10L).
Type). There is no particular problem with the model of the testing machine, and it is considered that the strain rate should be within the range of those normally used. However, when high speed deformation is a problem, such a testing machine may be selected. The capacity of the testing machine should be up to 10 tons.
The larger the cross-sectional area of the test piece is, the larger the amount of released gas is. Therefore, in principle, the larger the diameter of the test piece is, the more convenient it is to analyze a very small amount of gas. However, if the analyzer described below is used with a test piece with a capacity of up to 10 tons that can be tested with normal specifications, there is no particular problem.

(2) Ultra-high vacuum chamber: The ultra-high vacuum chamber 2 is a test piece held by the jigs 20, 20 of the material testing machine 1.
A test piece which is mounted so as to surround 19 and has a mass spectrometer 4 and a data analysis processing device mounted on one side thereof and which is in a vacuum.
It is designed to allow direct analysis of the gas released when deformed, stretched, or broken. The ultra-high vacuum chamber 2 containing the sample to be deformed was made of stainless steel (SUS304) whose surface was electrolytically polished. Although it is conceivable to use an aluminum alloy that emits less gas, stainless steel was used here in consideration of baking and other conditions. The smaller the internal volume of the chamber 2, the higher the partial pressure of the gas released from the sample, which is advantageous for gas analysis using a mass spectrometer. However, we decided to select a larger size here (internal volume: 0.05 m ³ ) so that the sample could be heated and cooled in the future.

(3) Vacuum exhaust device: Ultra-high vacuum chamber 2
The exhaust gas inside is at least 10 ^-5 Pa so that gas analysis can be performed.
Since the degree of vacuum needs to be as follows, the sputtering ion pump 7, the getter pump 8 and the turbo molecular pump 9 are used to obtain an ultrahigh vacuum. In the present invention, the exhaust pipe 6 (electrolytic polishing SU
Two turbo molecular pumps 9 are directly connected to each other via S304 (made by S304) (Shimadzu TMP-550, TMP-50 type), and a non-evaporable getter pump 8 (made by ULVAC SORB-AC 50-
The vacuum degree of 1.3 × 10 ⁻⁷ Pa is constantly obtained by using D type). In this case, it is preferable to use the sputter ion pump 7 because the higher the ultimate vacuum is, the more convenient it is for the analysis of a very small amount of gas. The drawing shows the case where ULVAC PST-8AM type or the like is attached to the ion pump. However, in the case of a material that releases a large amount of gas, the level of 10 ⁻⁵ Pa may be sufficient. Here, the non-evaporable getter pump 8 having a high hydrogen exhaust rate was provided immediately below the mass spectrometer 4 described later so that the released hydrogen gas was directed to the mass spectrometer 4.

(4) Mass spectrometer 4: As shown in FIG. 5, the mass spectrometer 4 has an ion source 4 of the mass spectrometer 4 for the test piece 19 held by the jigs 20, 20 in the ultrahigh vacuum chamber 2.
A, the analysis unit 4B, and the ion detection unit 4C are arranged in a linear relationship, the data analysis processing device 5 is connected to the ion detection unit 4C, and the data obtained by the mass spectrometer 4 is analyzed and processed or recorded or Configure to display.

Considering the analysis of hydrogen, which causes embrittlement of many materials, and the use of deuterium ( ² H) as an isotope, an analyzer with high analysis accuracy is selected in the region of light elements. Is preferred. In the present invention, an MSQ-400 type quadrupole trace mass spectrometer manufactured by ULVAC is used as the mass spectrometer. The analysis mass number (m / e) is 1 to 400, and it is possible to analyze polymer gas. The mass spectrometer 4 is perpendicular to the longitudinal direction of the sample and at the same height as the center of the parallel part of the sample so that the sample, the ion source, the analysis part, and the ion detection part are arranged in a straight line. It was placed at a position inclined at 45 degrees and directly above the non-evaporable getter pump.

(5) Data processing device 5 In the measurement by the mass spectrometer 4, a method of sweeping m / e = 1 to 50 is usually adopted in consideration of the residual gas species in the chamber, but the resolution is increased. For each sweep, 1 ~
It takes a few seconds. When such an analysis method is applied to the mass spectrometer attached to the present material testing machine, there is a possibility that intermittent gas emission during deformation or gas analysis at the moment of breakage cannot be performed. Therefore, the present invention incorporates a 10-channel high-speed multi-peak data processing device 5 developed by ULVAC. In this device 5, 10 selected from m / e = 1-50
It is possible to analyze up to 10 types of gas almost simultaneously (10 msec / ch).

The mass spectrometer used in the analyzer of the present invention is ULVAC quadrupole mass spectrometer MSQ-400 type, and its parts are described as follows. The mass spectrometer 4 is roughly divided into three parts, that is, an ion source 4A, an analysis part 4B, and an ion detection part 4C, which are linearly arranged. The interior of the mass spectrometer 4 is designed and assembled so that all parts can withstand repeated bake below 300 ° C.

(1) Ion Source 4A The ion source 4A is composed of an ionization box, a filament, and various electrodes (lens system). Each of them is insulated by high purity alumina. The vacuum residual gas is ionized by the emission current from the filament in the ionization chamber. Two filaments are attached,
Even if one of them is broken, the ion source 4A can be used by switching to the other without being taken out. The gas ionized in the ionization box is extracted in the direction perpendicular to the emission current, converged by the lens system, and becomes a thin ion beam, which is ejected near the center of the analysis electrode section.
Even if two filaments are both broken, replacement can be performed very easily.

(2) Analysis part (quadrupole electrode) 4B This part is the most important part of the mass filter type mass spectrometer. Therefore, it is made by carefully assembling precision-machined parts. The MSQ-400 type is characterized by using four hyperboloidal column electrodes to create an ideal theoretically correct electric field. These electrodes are accurately arranged in parallel via a spacer.

Two sets of electrodes facing each other are respectively connected inside the analysis tube. A voltage obtained by superimposing an AC voltage V and a DC voltage U is applied to this electrode. Ions that enter the central axis from the ion source oscillate, and only those that oscillate with a certain specific value pass, and other ions collide with the electrode and cannot pass. Since this is an electrode that functions in this way, this portion is also called a filter electrode.

(3) Detecting section 4C This is a section for detecting ions that have passed through the analyzing section 4B, and usually a box-and-grid type secondary electron multiplier is used. There are 17 stages of electrodes, and there is a (ion entrance) grid in front of the first electrode so that secondary electrons can be efficiently sent to the next stage electrode. Copper and beryllium (Cu-Be) are used as the electrode material. As an option, a channel type secondary electron multiplier may be used.
Also, to check the amplification factor of the secondary electron multiplier,
Only the first electrode can detect the ion current independently. The ion current amplified by the secondary electron multiplier enters the minute current amplifier through the low noise ion code, is detected with high sensitivity as an ion current, and is 10 ^-10 Pa (about 10 ^-12 Torr).
It is configured so that the following partial pressures can be measured.

FIG. 6 is a sectional view for explaining the construction principle of the turbo molecular pump used in the analytical tester of the present invention. The built-in induction motors 27, 28 are accelerated to a specified rotation speed by a dedicated high frequency power source. A rotor blade 30 is attached to the electric motor shaft 29, and a stator 31 is arranged between the rotor blades. A spacer 32 is inserted for positioning the stator.

The motor shaft 29 has bearings 33, 33 on the upper and lower sides,
A nozzle 34 for supplying lubricating oil to this bearing is provided at the lowermost end. Lubricating oil is stored in tank 35 and oil gauge 36
According to the configuration, the amount of oil and the deterioration state of oil can be observed.

The tank is cooled by a fan 37 whose fan cover 38 effectively cools the tank. The lubricating oil passes through the filter 39 and returns to the tank.
A protective net 40 is provided in the pump at the intake port to prevent dust and the like from entering. 41 indicates a magnet for removing dust mixed in oil.

The arrangement and shape of the rotor blades and stator blades are designed so that various performances such as exhaust speed and compression ratio can be exhibited most efficiently. The rotor blades and the stator blades in the upper stage are designed mainly to improve the exhaust performance, and the compression performance increases in the lower stage.
The shape of the stator blade is changed by its main action.

The principle of exhausting the turbo molecular pump 9 is roughly as follows. The distance until the gas molecules collide with each other, that is, the space where the mean free path is increased (generally, a vacuum region of 10 ^-4 Torr or less), the gas molecules collide with the wall (that is, the rotor) moving at high speed. Therefore, when the gas molecules fly out of the rotor, they have a maximum probability of 180
Reflects at a solid angle of °.

If there is no heat exchange on the rotor surface, the gas molecules that have jumped out are the vector of the thermal motion velocity of itself and the velocity of the rotor. The velocity given to the gas molecules of the rotor is determined by its geometrical shape and rotation speed, so that the gas molecules move from a non-directional thermal motion to a directional motion.

FIG. 7 is a sectional view for explaining the operating principle of the non-evaporable getter pump. In FIG. 7, 42 is a cylindrical getter material made of a Zn-Al alloy, 43 is a heater housed inside, and the getter material 42 has both ends thereof pressed by pressing plates 44 and fixed by bolts and nuts 45. 46 is a heater terminal metal fitting, and this non-evaporable getter pump is inserted in the vacuum chamber 2 and the getter material 42 is heated by the heater 43.
When is heated to 400 ° C., the gas is absorbed by the getter material 42 and the inside of the vacuum chamber 2 is exhausted.

The standard usage of the device of the present invention is as follows. First, set a test piece with a total length of 50 to 60 mm and a parallel portion length of 10 to 30 mm in the grip of the tester, seal the sample insertion port with an oxygen-free copper gasket, and after rough evacuation with the rotary pump 7, then use the turbo molecular pump. Exhaust by 9A and 9B is started. After evacuation for about 30 minutes to reach the level of 10 ⁻⁵ Pa, the vacuum chamber 2, the exhaust pipe 6 and the turbo molecular pumps 9A and 9B are heated and held at 120 to 200 ° C. for baking for 24 hours. After the baking is completed, natural cooling is performed to obtain an ultrahigh vacuum of 1 × 10 ⁻⁷ Pa. At this stage, the non-evaporable getter pump 8 is operated, but the pump
Since it is heated to 400 ° C, depending on how the pump is installed, the temperature in the surrounding chamber will rise and the degree of vacuum will drop.
Therefore, the voltage applied to the pump is lowered to lower the temperature and the chamber is cooled. However, for hydrogen,
The pumping speed does not change much at 400 ° C and room temperature (when no voltage is applied).

The material test is performed while exhausting with the turbo molecular pump 9 and the non-evaporable getter pump 8, and the load-displacement curve, the total pressure change, and the ion current change from the mass spectrometer 4 are measured. Then, by correlating the load-displacement curve with the total pressure / ion current change, information on the gas release characteristics at the time of deformation / breakage is obtained. An analog recorder or a personal computer can be used to measure the load-displacement curve and total pressure.
For mass spectrometry, a high speed multi-peak data processing system 5 is used. With this system, it is possible to measure up to 10 kinds of gas in a short time, such as a measurement interval between gas species of 10 msec and a measurement interval of the same gas species of 100 msec or less. It is possible to measure a fast partial pressure change called outgassing. The gas species are H ₂ (mass number 2), H ₂ O (18), which is the main residual gas in the chamber,
In addition to N ₂ + CO (28), C for distinguishing N ₂ from CO
HD (3), D ₂ (4) when stable isotopes such as (12), N (14), O (16) and deuterium ( ² H (D), mass number 2) are used as tracers , HDO (19), D ₂ O (20), etc., but 10 types will be selected from these (the measurable mass number is 1 to 400). Of course, isotopes other than hydrogen (such as ¹⁵ N and O ¹⁸ ) can be used,
Radioactive materials (such as ³ H) must be used in dedicated handling facilities. After the test is completed, the gate valve 10 is closed, the inside of the chamber 2 is leaked by high-purity argon gas, and the test piece is taken out from the sample taking-out lid 11.

In the embodiment of the present invention, a turbo molecular pump,
An ultra-high vacuum of 10 ^-7 Pa is obtained by exhausting with a non-evaporating getter pump and a sputter ion pump. However, in order to obtain such an ultra-high vacuum, it is not always necessary to combine the pumps described above. Achievements are possible with numerous other pumps not mentioned. For example, an oil diffusion pump (for high vacuum, approx. 10 ^-3
Even in Pa), if a liquid nitrogen trap is used, an ultrahigh vacuum of 10 ⁻⁷ Pa can be obtained. Therefore, in the present invention, it was decided to obtain an ultra-high vacuum by the pumps used in the examples, but the combination of the pumps used is not necessarily an essential condition, and the point is that an ultra-high vacuum of 10 ^-5 Pa or less is necessary. It is essential and it should be carried out as such.

[0039]

【Example】

Experimental method: 7 provided by a domestic aluminum manufacturer
From extruded material of NO1 alloy (international standard 7005 alloy) φ14 × 40
A mm sample was cut out and processed into a round bar tensile test piece having a parallel portion φ8 × 10 mm, and then subjected to solution heat treatment at 470 ° C. for 3.6 ks, water quenching, and artificial aging treatment at 120 ° C. for 86.4 ks. After sufficiently degreasing with acetone, put it in the ultra-high vacuum chamber,
79ks at 150 ℃ in the chamber containing the sample in about 10 ^-5 Pa
After the baking treatment of 5 × 10 ^-7
The pressure was Pa. Tensile test is performed at a constant crosshead speed (0.5 mm / min), and during the test, m / e = 2, 12, 14,
Mass spectrometric analyzes were carried out on 16, 18, 28, 32, 40 and 44.

Experimental results: FIG. 8 shows the results of residual gas analysis, showing the ion current characteristics of H ₂ , H ₂ O, (N ₂ + CO), and CO ₂ . FIG. 9 shows a load-displacement curve diagram in the tensile test, and FIGS. 10 to 18 are ion current characteristic diagrams showing the results of mass spectrometry. Approximately 390 s after the start of the test, the test piece broke, but at this time, m / e = 2, 14, 16, 2
8, 40 and 44 peaks were detected. That is, H ₂ , N
_{It was found that 2} + CO, Ar and CO ₂ were released from the fracture surface, and the most released gas was H ₂ . In addition, the ion current of monatomic N and O was also changed,
This is a result of breaking the interatomic bond by the ion source of the mass spectrometer, and N is a part of N ₂ dissociated. It is unknown at this stage whether O originates from CO or CO ₂ .
In any case, it was revealed that a large amount of H ₂ was released from the fracture surface of the 7NO1 alloy used in the experiment of the present invention, and hydrogen was involved in the destruction even in the industrially sufficiently degassed sample. It was proved that.

Experimental considerations: (1) Tensile pulling of material under ultra high vacuum
In the compression / fatigue test, the effects of water vapor and hydrogen in the test atmosphere have been reported by comparing with the test results in air (mainly ductility and toughness) as described above. At this time,
It has been considered that the test under ultra-high vacuum has no or negligible influence of water vapor in the atmosphere. However, when a mass spectrometer was attached to the ultra-high vacuum chamber in the present invention, it was found that most of the residual gas in the ultra-high vacuum of 10 ⁻⁷ Pa was hydrogen and water vapor, and the environment was maintained even under the ultra-high vacuum. It is considered that it has become necessary to consider the embrittlement of the material due to hydrogen and water vapor.

(2) In the study according to the present invention, the released gas was detected even in the initial stage of deformation (elastic range) of the material. It is considered that this is because the oxide film on the surface of the sample was destroyed and gas just below the film was released. The results of this experiment are one of the important points in the study of vacuum chamber materials by conventional temperature-dependent desulfurization test equipment, and suggest that the effect of the oxide film on the surface is important in addition to the gas release accompanying the heating of the sample. To do.

(3) The apparatus of Skamanz et al. Could not detect hydrogen released from a sample not exposed to saturated steam. Therefore, in order to demonstrate hydrogen embrittlement, it was necessary to introduce a large amount of hydrogen into the sample, and therefore a phenomenon different from the phenomenon that could actually occur was observed. However, the present invention has made it possible to detect an extremely small amount of gas already present in the material, and thus greatly contributes to the demonstration of embrittlement due to the amount of gas whose influence has been neglected so far. It is possible to measure.

[0044]

In the ultratrace gas analyzer of the present invention, the material testing machine 1, the ultra-high vacuum chamber 2, the exhaust device 3, and the mass spectrometer 4 are integrally arranged in the ultra-high vacuum system. The extremely small amount of gas released from the material when the material is deformed or destroyed can be analyzed with high accuracy, and the test results can be instructed and recorded by the data processing device with high accuracy and speed. There is.

[Brief description of drawings]

FIG. 1 is a front view of an analyzer of the present invention.

FIG. 2 is a plan view of the analyzer of the present invention.

FIG. 3 is a front view of the material testing machine of the present invention.

FIG. 4 is a cross-sectional view showing a state in which an ultrahigh vacuum chamber is attached to the material testing machine of the present invention.

FIG. 5 is an explanatory diagram in which a part of FIG. 4 is enlarged.

FIG. 6 is a cross-sectional view showing the basic structure of a turbo molecular pump used in the present invention.

FIG. 7 is a sectional view showing the structure of a non-evaporable getter pump used in the present invention.

FIG. 8 is an ionic current characteristic diagram of each element and compound showing a residual gas analysis result analyzed by the test apparatus of the present invention.

FIG. 9 is a load-displacement curve diagram in the testing machine of the present invention.

FIG. 10 is an ion current curve diagram of carbon (C) showing the results of mass spectrometry by the tester of the present invention.

FIG. 11 is an oxygen (O ₂ ) ion current curve diagram showing the results of mass spectrometry by the tester of the present invention.

FIG. 12 is an ion current curve diagram of CO ₂ showing the results of mass spectrometry by the tester of the present invention.

FIG. 13 is an ion current curve diagram of N ₂ + CO showing the results of mass spectrometry by the tester of the present invention.

FIG. 14 is an ion current curve diagram of H ₂ O showing the result of mass spectrometry by the tester of the present invention.

FIG. 15 is an ion current curve diagram of H ₂ showing the results of mass spectrometry by the tester of the present invention.

FIG. 16 is an ion current curve diagram of N showing the results of mass spectrometry by the tester of the present invention.

FIG. 17 is an Ar ion current curve diagram showing the results of mass spectrometry by the tester of the present invention.

FIG. 18 is an O ion current curve diagram showing mass spectrometry results by the tester of the present invention.

[Explanation of symbols]

 1 Material Testing Machine 2 Ultra High Vacuum Chamber 2A Mass Spectrometer Intake Flange 3 Exhaust Device 4 Mass Spectrometer 5 Data Analysis Processing Device 6 Exhaust Pipe 7 Sputter Ion Pump 8 Non-evaporable Getter Pump 9 Turbo Molecular Pump 10 Gate Valve 11 Sample Entry / Exit Lid 12 Base 13 Strut 14 Crosshead 15 Lifting cylinder 16 Table 17 Load cell 18 Piston 19 Test piece 20 Jig 21 Actuator 22 Clamp cylinder 23 Anti-vibration pad 24 Door 25 Lifting manifold 26 Clamp manifold 27, 28 Induction motor 29 Electric motor shaft 30 Rotor blade 33 Bearing 34 Nozzle 35 Tank 36 Oil Gauge 39 Filter 40 Protective Net 41 Magnet 42 Getter Material 43 Heater 44 Holding Plate 45 Bolt Nut 46 Heater Terminal Metal

Claims (3)

[Claims] 1. An ultra-high vacuum chamber of 10 ⁻⁷ Pa or less,
A material testing machine that can perform tensile, compression, and fatigue tests, a high-performance mass spectrometer, and a non-evaporable getter pump are connected, and an exhaust pipe connected to an ultra-high vacuum chamber is connected to a sputter ion pump and a shut-off valve. An analyzer for an extremely small amount of gas released from a material at the time of deformation or destruction, which is connected to a turbo molecular pump and is provided with a lid for sample exchange in the ultra-high vacuum chamber. 2. The analyzer according to claim 1, wherein the mass spectrometer has a sample parallel part, an ion source, an analysis part, and an ion detection part arranged in a linear relationship. 3. The analyzer according to claim 1, wherein the mass spectrometer is mounted close to a connecting portion between the exhaust pipe and the ultra-high vacuum chamber so as to form an angle of about 30 to 45 degrees.