WO2006085405A1

WO2006085405A1 - Method of quantitative determination of atomic hydrogen, apparatus therefor, method of adsorption removal of atomic hydrogen and apparatus therefor

Info

Publication number: WO2006085405A1
Application number: PCT/JP2005/017266
Authority: WO
Inventors: Akira Namiki; Akira Izumi; Hiroshi Tsurumaki
Original assignee: National University Corporation Kyushu Insutituteof Technology
Priority date: 2005-02-14
Filing date: 2005-09-20
Publication date: 2006-08-17
Also published as: JPWO2006085405A1; JP4072627B2

Abstract

A method of quantitative determination of atomic hydrogen, in which the quantitative determination of atomic hydrogen can be carried out easily and accurately; an apparatus therefor; a method of removal of atomic hydrogen, in which any atomic hydrogen can be removed; and an apparatus therefor. There is provided apparatus (10) for quantitative determination of atomic hydrogen, comprising sensor chamber (12), sensor substrate (14), heating means (16), atomic deuterium emission unit (24) and mass spectrometer (26). The sensor substrate (14) is irradiated with atomic deuterium, and the sensor substrate (14) is exposed to a measuring object gas containing atomic hydrogen. The intensities of HD and deuterium desorbed from the sensor substrate (14) are measured, from which the amount of atomic deuterium remaining on the sensor substrate (14) is computed. On the basis of an intensity correlationship by mass spectrometry between the in-advance determined atomic hydrogen irradiation amount to the sensor substrate (14) and amount of atomic deuterium remaining on the sensor substrate (14), there is accomplished the quantitative determination of atomic hydrogen in the measuring object gas.

Description

Specification

Atomic hydrogen determination method and apparatus, and atomic hydrogen adsorption and removal method and apparatus

Technical field

[0001] The present invention mainly relates to a technique for quantitative determination of atomic hydrogen.

Background art

[0002] In recent years, substrate surface cleaning technology using atomic hydrogen has attracted attention mainly in the semiconductor industry. It has also been clarified that atomic hydrogen generated from raw materials determines the performance of semiconductor devices during thin film deposition. Therefore, there is a need for a technique for quantifying the amount of atomic hydrogen generated and a technique for removing atomic hydrogen to control the amount of atomic hydrogen.

[0003] As a simple method that has been known for a long time for quantitative determination of atomic hydrogen, a special glass is irradiated with atomic hydrogen and the amount of atomic hydrogen is measured by the fact that the glass is colored. There is a method force S (see Non-Patent Document 1, for example). However, with this method, it is difficult to accurately measure the amount of atomic hydrogen.

On the other hand, as a method for accurately measuring the atomic hydrogen amount, there is a 2-photon laser induced fluorescence or vacuum ultraviolet absorption method (for example, Non-Patent Document 2 referred to.) With ₀ tooth force, these methods are all large Therefore, there is a problem that the apparatus configuration becomes complicated and the apparatus cost increases.

There is also a quantitative method using the atomic hydrogen extraction (D) on crystalline silicon by atomic hydrogen. This method is characterized by the ability to measure the amount of atomic hydrogen relatively correctly because it can be distinguished from the hydrogen present in the knock ground by using atomic deuterium. (For example, see Non-Patent Document 3 and Non-Patent Document 4.) ₀ However, in this case, it is difficult to handle such as crystalline silicon must be cleaned in an ultra-high vacuum. It is also used only for some scientific research purposes where quantitative reproducibility is very poor.

Non-Patent Document 1: Takashi Morimoto, Koji Yoneyama, Hironobu Umemoto, Satoshi Masuda, Eiji Matsumura, Keiji Ishibashi, Kashiyama Hiroshi, Hiroshi Kawade, Quantitative determination of H atom density using glass containing tungsten oxide, Spring 5th

1st Conference on Applied Physics (Tokyo), 28P-ZE-1, March 2004

Non-Patent Document 2: H. Umemoto, K. Ohara, D. Morita, Y. Nozaki, A. Masuda, and H. Mat sumura, Direct Detection of Atomic Hydrogen in the Catalytic Chemical Vapor Deposition of the SiH4 / H2 System, J. Appl. Phys., 91, 3, 1650, 2002.

Non-Patent Document 3: H. N. Waltenburug, J. T. Yates, Surface-chemistry ofsilicon, Chem. Reviews, 95, 5, 1589 (1995).

Non-Patent Document 4: S. Shimokawa, A. Namiki, T. Ando, Y. Sato, J. Lee, J. Chem. Phys., 1 12, 356 (2000).

Disclosure of the invention

Problems to be solved by the invention

[0004] The problem to be solved is that there is no simple and accurate method for quantitative determination of atomic hydrogen and no method for removing atomic hydrogen.

[0005] The present invention has been made in view of the above problems, and has as its object to provide an atomic hydrogen quantification method and apparatus capable of easily and accurately quantifying atomic hydrogen. To do.

Another object of the present invention is to provide an atomic hydrogen adsorption / removal method and apparatus capable of removing atomic hydrogen.

Means for solving the problem

[0006] The atomic hydrogen determination method according to the present invention comprises:

A sensor preparation process for preparing the sensor material under initial conditions;

A sensor exposure step for exposing the sensor to a gas to be measured containing atomic hydrogen (H);

Heating the sensor;

An intensity measuring step for measuring the intensity of hydrogen (H) desorbed from the sensor;

2

Based on the correlation between the irradiation time of atomic hydrogen (H) on the sensor and the intensity of hydrogen (H) desorbed from the sensor by mass spectrometry, the measurement target gas is measured.

2

Atomic hydrogen quantification process for quantifying atomic hydrogen (D) in It is characterized by having.

[0007] Further, the atomic hydrogen determination method according to the present invention includes:

During the sensor preparation step, the sensor material is irradiated with atomic deuterium (D) to prepare a sensor,

In the intensity measurement step, the strength of HD and deuterium (D) desorbed from the sensor

Measure twice and use this to calculate the amount of atomic deuterium (D) remaining in the sensor,

In the atomic hydrogen determination step, the intensity correlation obtained by mass spectrometry between the atomic hydrogen (H) irradiation amount for the sensor and the atomic deuterium (D) amount remaining in the sensor previously obtained is determined. Based on this, the atomic hydrogen (D) in the gas to be measured is quantified.

[0008] Further, in the atomic hydrogen determination method according to the present invention, the sensor material includes Ni, Cr, Al, Mn, Fe, Co, Be, W, V, Si, C, Nb, Ta, Cu, and Ti. It is an alloy composed of at least two or more kinds of metal members selected from the above.

[0009] Further, the atomic hydrogen quantification method according to the present invention is characterized in that it is the alloy strength Nconel.

[0010] Further, the atomic hydrogen quantification method according to the present invention is characterized in that mass spectrometry is performed using a quadrupole mass spectrometer during the intensity measurement step.

[0011] Further, an atomic hydrogen quantification device according to the present invention includes a sensor chamber that houses a sensor substrate and a heating mechanism that heats the sensor substrate, and the sensor chamber that is provided in connection with the sensor chamber. Atomic deuterium introduction part that introduces atomic deuterium so that the flow can be shut off, measurement target gas introduction part that introduces the gas to be measured into the sensor chamber so that the flow can be shut off, and gas in the sensor chamber that can shut off the flow mass analysis It is characterized by comprising at least a sensor chamber gas lead-out section leading to the apparatus.

[0012] In addition, the atomic hydrogen quantification device according to the present invention includes an atomic deuterium generator connected to the atomic deuterium introduction unit, and a mass spectrometer connected to the sensor chamber gas outlet unit. It is further provided with the feature.

[0013] In addition, the atomic hydrogen quantification device according to the present invention is characterized in that the mass spectrometer is a quadrupole mass spectrometer. [0014] In addition, the method for adsorbing and removing atomic hydrogen according to the present invention includes a desorption step of desorbing atomic hydrogen adsorbed on the material by heating a material capable of adsorbing and desorbing atomic hydrogen, An adsorption removal step of adsorbing and removing atomic hydrogen in the target gas by exposing the material to the target gas containing atomic hydrogen.

[0015] Further, in the atomic hydrogen adsorption and removal method according to the present invention, the material is Ni, Cr, Al, Mn, Fe, Co, Be, W, V, Si, C, Nb, Ta, Cu, and Ti. Among these, it is an alloy composed of at least two kinds of metals whose forces are also selected.

[0016] Further, the atomic hydrogen adsorption / removal method according to the present invention is characterized by the alloy power Nconel.

[0017] The atomic hydrogen adsorption / removal device according to the present invention includes a material capable of adsorbing and desorbing atomic hydrogen and a heating mechanism for heating the material to desorb atomic hydrogen, and It is characterized in that the material in a state in which is desorbed is exposed to a target gas containing atomic hydrogen.

The invention's effect

[0018] In the present invention, a sensor prepared under initial conditions is exposed to an atmosphere containing atomic hydrogen to desorb atomic deuterium and the like, and the atomic state in the atmosphere is determined based on the determination result of atomic deuterium and the like. Since hydrogen is quantified, atomic hydrogen in the atmosphere can be quantified easily and accurately.

In addition, atomic hydrogen in the target gas can be removed using a material that can significantly adsorb and desorb atomic hydrogen.

Brief Description of Drawings

FIG. 1 is a diagram showing a schematic configuration of an atomic hydrogen quantification apparatus.

[Fig. 2-1] A graph showing the relationship between the irradiation time of atomic hydrogen and the intensity of deuterium desorbed when Inconel is used for the sensor when atomic deuterium is irradiated to the sensor material. .

[Fig. 2-2] A graph showing the relationship between the irradiation time of atomic hydrogen and the intensity of desorbed HD when Inconel is used for the sensor when atomic deuterium is irradiated to the sensor material.

[Fig.3-1] When irradiating sensor material with atomic deuterium, stainless steel FIG. 6 is a graph showing the relationship between the irradiation time of atomic hydrogen and the strength of deuterium desorbed when used in the above.

[Fig. 3-2] A graph showing the relationship between the atomic hydrogen irradiation time and the desorption HD intensity when stainless steel is used for the sensor when atomic deuterium is irradiated to the sensor material. [4] 4-1] A graph showing the relationship between the irradiation time of atomic hydrogen and the strength of deuterium desorption when crystalline silicon is used as the sensor when atomic deuterium is irradiated to the sensor material.

圆 4-2] When irradiating sensor material with atomic deuterium, it is a diagram showing the relationship between the irradiation time of atomic hydrogen and the desorption HD intensity when crystalline silicon is used as the sensor.

FIG. 5-1 is a diagram showing the relationship between the irradiation time of atomic hydrogen and the intensity of deuterium desorbed when aluminum is used as a sensor when atomic deuterium is irradiated to the sensor material. .

[Fig. 5-2] When irradiating the sensor material with atomic deuterium, it is a diagram showing the relationship between the irradiation time of atomic hydrogen and the desorption HD intensity when aluminum is used as the sensor. 6] A graph showing the relationship between deuterium intensity when thermal desorption is performed on Inconel with varying atomic deuterium irradiation time when atomic deuterium is irradiated onto the sensor material. is there.

Explanation of symbols

10 Atomic hydrogen determination system

12 Sensor room

14 Sensor board

16 Heating mechanism

18 Atomic deuterium inlet

20 Measurement target gas introduction part

22 Sensor room gas outlet

24 Atomic deuterium generator 26 Mass spectrometer

BEST MODE FOR CARRYING OUT THE INVENTION

A preferred embodiment of the present invention will be described below with reference to the drawings.

[0022] First, the atomic hydrogen determination method according to the present invention will be described.

In the atomic hydrogen quantification method according to the present invention, after preparing the sensor material under the initial conditions (sensor preparation step), the sensor is exposed to a measurement target gas containing atomic hydrogen, in other words, the sensor is exposed to atomic hydrogen. Is irradiated (sensor exposure process), and the sensor is further heated (heating process) to desorb the hydrogen produced on the sensor. Next, the intensity of the desorbed hydrogen is measured by mass spectrometry (strength measurement process), and the correlation between the irradiation time of atomic hydrogen on the sensor material previously determined and the intensity by mass spectrometry of hydrogen desorbed from the sensor material Based on the above, the atomic hydrogen in the measurement target gas is quantified (atomic hydrogen quantification process).

Here, as a method for preparing the sensor material under the initial conditions, a method of performing initial cleaning by removing hydrogen at a high temperature can be used. However, the method is not limited to this as long as reproducibility can be ensured.

[0023] Further, in the atomic hydrogen quantification method according to the present invention, more preferably, in the sensor preparation step, atomic deuterium (D) is irradiated to the sensor material to irradiate atomic deuterium (D). Capture (capture) deuterium termination. As a result, in the sensor exposure process, deuterium (D) and deuterium generated by atomic hydrogen (D) are irradiated by irradiating the sensor with atomic hydrogen.

2

An extraction reaction of compound (HD) occurs. Next, after heating the sensor (heating process), the intensity measurement process is performed to measure the deuterium compound (HD) and deuterium (D) intensity desorbed from the sensor, and from this, the atoms remaining in the sensor are measured. Calculate the amount of deuterium (D).

2

Next, in the atomic hydrogen determination step, the correlation between the intensity of the atomic hydrogen (H) irradiation with respect to the sensor determined in advance and the amount of atomic deuterium (D) remaining on the sensor by mass spectrometry (deuterium Quantitative determination of atomic hydrogen (D) in the measurement target gas based on the calibration curve)

In the method of irradiating atomic deuterium, mass analysis is performed on a gas containing a desorbed component that is desorbed by the sensor force during irradiation of atomic hydrogen in the sensor exposure step, and then deuterium or heavy water is used. Measure the strength of the elemental compound (strength measurement step A). In addition, a method of measuring the strength of deuterium or deuterium compounds by mass spectrometry of a gas containing a desorbed component that is directly desorbed from the sensor by an extraction reaction may be used (strength measurement step B).

In the case of the quantitative method using the extraction reaction of atomic deuterium on crystalline silicon by atomic hydrogen as described in the prior art, it is difficult to handle because crystalline silicon must be washed in an ultra-high vacuum. It is. Also, quantitative reproducibility is very poor. On the other hand, according to the present invention, since a large amount of drawn gas can be obtained by using a sensor irradiated with a large amount of atomic deuterium, complicated handling such as applying a high degree of cleaning to the sample is required. Atomic hydrogen can be quantified with much higher accuracy. According to this method, atomic deuterium can also be quantified.

[0024] In the operations described above, when atomic deuterium is not irradiated, for example, in the sensor ^preparation process, under an ultrahigh vacuum condition of about 10 ^_8 Pa or less and a temperature condition of about 50 ° C or less. To do. The sensor exposure process is performed under an ultrahigh vacuum condition of about 10 ^_8 Pa or less and a temperature condition of about 20 to 500 ° C. The strength measurement process is performed under ultra-high vacuum conditions of about 10 ^_8 Pa or less. In the strength measurement process B, it is performed under an ultra-high vacuum condition of about 10 ^_8 Pa or less and a temperature condition of about ^20-500 ° C.

In contrast, when irradiating the atomic deuterium, for example, in the sensor preparing step, 10 ^_4 P _a ^~10 ^_8 Pa about ultra-high vacuum conditions, at a temperature of room temperature to about 100 ° C Do. In the sensor exposure process, it is performed under an ultrahigh vacuum condition of about ¹ Pa to: L0 ^_8 Pa and under a temperature condition of about 269 to 100 ° C. In the strength measuring step A, in ultra-high vacuum conditions of about 10 ^_4 P _a ~10 ^_8 Pa, carried out at a temperature of about 100 to 500 ° C. In the strength measuring step B, 10 _ ⁴ at P _a to 10 ^_8 Pa about ultra-high vacuum conditions, carried out at a temperature of room temperature to about 100 ° C

In the present invention, as long as the sensor material satisfies the determination of atomic hydrogen, the sensor material takes in a sufficient amount of atomic deuterium, particularly in the case of irradiation with atomic deuterium, and The material type is not particularly limited as long as it generates a sufficient amount of extraction gas when irradiated with gaseous hydrogen. For example, an appropriate material such as crystalline silicon, stainless steel, or aluminum may be used. it can. However, the above action is more From the viewpoint of effective expression, at least two kinds of metals selected from Ni, Cr, Al, Mn, Fe, Co, Be, W, V, Si, C, Nb, Ta, Cu and Ti are used. It is more preferable to use a configured alloy. As such an alloy, it is more preferable to use Inconel, and Invar, Northello and the like are also preferable.

[0026] In the present invention, mass spectrometry can be performed using an appropriate apparatus, but a quadrupole mass spectrometer is more preferable.

[0027] An atomic hydrogen quantification apparatus according to the present invention that can suitably realize the atomic hydrogen quantification method according to the present invention will be described with reference to FIG.

In the atomic hydrogen determination device (atomic hydrogen monitoring device) 10 shown in FIG. 1, a sensor chamber (sensor) 14 and a heating mechanism 16 for heating the sensor substrate 14 are provided (accommodated) in the sensor chamber 12. O) The heating mechanism 16 includes, for example, a heating plate that also serves as a mounting table for the sensor substrate 14 and a heat source that heats the heating plate.

Connected to the sensor chamber 12, an atomic deuterium introduction section 18, a measurement target gas introduction section 20, and a sensor chamber gas outlet section 22 are provided. The measurement target gas introduction unit 20 includes a valve mechanism such as a gate valve that connects the sensor chamber 12 and the outside so as to be able to shut off the flow. Each of the atomic deuterium introduction section 18 and the sensor chamber gas outlet section 22 is also provided with an appropriate blocking mechanism. If atomic deuterium is not used, the atomic deuterium introduction section 18 is not necessary.

The apparatus configured as described above can be used, for example, as a portable type, transported to a measurement place, and connected to an atomic deuterium generator, a measurement object gas, and a mass spectrometer, respectively.

[0029] The apparatus configured as described above can also be used as a portable atomic hydrogen removing apparatus (portable atomic hydrogen monitoring apparatus). In this case, the measurement target gas introduction part (target gas introduction part) 20 is connected to an atmosphere containing atomic hydrogen to be removed. Further, the sensor chamber gas deriving unit 22 is unnecessary, and further, if the atomic deuterium is previously taken into the sensor substrate 14, the atomic deuterium introducing unit 18 is also unnecessary.

In this case, it is simpler to adopt a method in which atomic deuterium is taken in and the heated sensor substrate 14 is placed in an atmosphere containing the atomic hydrogen to be removed. is there.

In addition, as shown in FIG. 1, the atomic hydrogen quantification apparatus 10 includes an atomic deuterium generator 24 in the atomic deuterium introduction section 18 and a mass spectrometer 26 in the sensor chamber gas outlet section 22. Can also be connected to each other. When atomic deuterium is not used, the atomic deuterium introduction part 18 and the atomic deuterium generator 24 are not necessary.

[0031] A method of using the atomic hydrogen quantification apparatus 10 will be described.

Atomic deuterium generated from the atomic deuterium generator 24 is introduced into the sensor chamber 12, and the sensor substrate 14 is irradiated with atomic hydrogen. In a state where the sensor substrate 14 is heated by the heating mechanism 16, there is a measurement target gas containing atomic deuterium! Or an atmospheric gas containing atomic hydrogen to be removed is introduced into the sensor chamber 12.

The measurement target gas containing atomic deuterium or the atmosphere gas containing atomic hydrogen to be removed is generated, for example, in a thin film deposition apparatus, a dry etching apparatus, or the like.

These so-called atomic hydrogen generators and atomic hydrogen quantification apparatus 10 are connected via gas introduction unit 20 to be measured, and the gas containing atomic hydrogen from the atomic hydrogen generator enters sensor chamber 12. The introduced and heated sensor substrate 14 is exposed to this gas. Atomic hydrogen is consumed in the reaction with atomic deuterium.

[0032] The sensor substrate 14 irradiated with atomic hydrogen is heated by the heating mechanism 16 to a temperature higher than the temperature at the time of irradiation, and the intensity of deuterium or deuterium compound (HD) desorbed is mass analyzed. The amount of atomic deuterium remaining in the sensor is calculated from the measurement with the device 26. Intensity correlation data obtained by mass spectrometry between the atomic hydrogen irradiation amount on the sensor substrate 14 and the atomic deuterium amount remaining on the sensor substrate 14 previously incorporated in the mass spectrometer 26. Based on this, atomic hydrogen is quantified.

[0033] The results of an experiment of extracting deuterium with atomic hydrogen will be described below.

[0034] Figure 2-1 shows that an alloy composed of Ni, Cr, Al, Mn, Fe, and Co (Inconel) is the sensor, and atomic hydrogen (H ) Shows the experimental results of the pull-out reaction. At the same time, instead of this alloy, stainless steel, crystalline silicon, and aluminum were used as sensors, and the results are also shown in Fig. 3-1 to Fig. 5-1. Figures 2-1 to 51 show the relationship between the irradiation time of atomic hydrogen and the deuterium (D) intensity desorbed, respectively. is doing. Figures 2-2 to 5-2 show the relationship between atomic hydrogen irradiation time and desorbed HD intensity.

All materials (sensors) used in this experiment were only organically cleaned. From this result, it is clear that each material takes in a lot of atomic hydrogen and causes a reaction with atomic deuterium!

It can also be seen that Inconel takes in more atomic hydrogen, which has a stronger initial deuterium strength than other materials, and causes a reaction with atomic deuterium. In addition, it can be seen that the deuterium intensity of the Incone decreases rapidly with respect to the atomic hydrogen irradiation time compared to other materials. This shows that the amount of atomic hydrogen can be determined more accurately by using Inconel. The results also show that Inconel plays the most efficient role in removing atomic hydrogen.

[0035] Fig. 6 shows the relationship between the deuterium intensity when deuterium is heated and desorbed from Inconel with different atomic deuterium irradiation time after sufficient irradiation with deuterium atoms (atomic deuterium). Indicates. The pressure when irradiating atomic deuterium (corresponding to the flux of atomic deuterium) is 0.5 X 10 ^_5 Pa.

2. Two results of 5 X 10 ^_5 Pa are shown.

This result shows that when the pressure is 0.5 X 10 ^_5 Pa, there is a linear relationship between the irradiation time of atomic deuterium and the deuterium intensity in the range of 300 seconds. Compared Further, if the pressure is 2. ⁵ X 10- 5 Pa, is related in the same straight line as the previous to initial irradiation of about 50 seconds, deuterium strength pressure as in 0. 5 X 10 ^_5 Pa Therefore, it is 5 times the same as the increase in pressure. This result shows that atomic hydrogen can be measured correctly.

The above experiment was repeated. Compared to stainless steel, crystalline silicon, and aluminum, Inconel achieved the same results with good reproducibility.

[0036] Next, the method for adsorbing and removing atomic hydrogen according to the present invention will be described.

The method for adsorbing and removing atomic hydrogen according to the present invention is an adsorbing and removing method in which atomic hydrogen in a target gas is adsorbed and removed by exposing a material capable of adsorbing and desorbing atomic hydrogen to the target gas containing atomic hydrogen. And a desorption step of desorbing atomic hydrogen adsorbed on the material.

[0037] Here, the material capable of adsorbing and desorbing atomic hydrogen is described in the explanation of the atomic hydrogen determination method. The materials mentioned can be used.

That is, the material capable of adsorbing and desorbing atomic hydrogen is not particularly limited as long as it exhibits the effects of the present invention. For example, an appropriate material such as crystalline silicon, stainless steel, aluminum or the like can be used. Can be used. However, from the viewpoint of more effectively expressing the above action, Ni ゝ Cr のうち Al, Mn, Fe ゝ Co, Be ゝ W, V, Si ゝ C, Nb ゝ Ta ゝ Cu and Ti It is more preferable to use an alloy composed of at least two kinds of metal chains selected from the above. Furthermore, it is more preferable to use Inconel as such an alloy.

[0038] In the adsorption removal step, for example, the material is exposed to a target gas containing atomic hydrogen.

Thereby, the atomic hydrogen in the target gas can be adsorbed and removed.

In the desorption step, for example, the material is heated to a temperature of 100 to 500 ° C. under atmospheric pressure or reduced pressure. At this time, the sensor irradiated with atomic deuterium described in the explanation of the atomic hydrogen determination method can also be used. By this step, atomic hydrogen adsorbed on the material can be removed, so that the same material can be used repeatedly.

[0040] The atomic hydrogen adsorption / removal device according to the present invention, which can suitably implement the atomic hydrogen adsorption / removal method according to the present invention, heats a material capable of adsorbing and desorbing atomic hydrogen and the material. And a heating mechanism that desorbs atomic hydrogen, and the material in a state where atomic hydrogen is desorbed is exposed to a target gas containing atomic hydrogen. Note that the heating mechanism is not required depending on the method used by exchanging materials.

As such an apparatus, for example, the apparatus shown in FIG. 1 described in the explanation of the atomic hydrogen quantification apparatus can be used. Alternatively, an apparatus consisting only of a material and a heating mechanism may be used as it is in a target gas containing atomic hydrogen. Alternatively, a device having only material power may be used as it is in a target gas containing atomic hydrogen.

Claims

The scope of the claims

[1] A sensor preparation process for preparing the sensor material under initial conditions;

A sensor exposure step of exposing the sensor to a measurement target gas containing atomic hydrogen; and a heating step of heating the sensor;

An intensity measuring step for measuring the intensity of hydrogen desorbed from the sensor;

Atomic hydrogen quantification step for quantifying atomic hydrogen in the gas to be measured based on the correlation between the irradiation time of atomic hydrogen on the sensor determined in advance and the intensity of hydrogen desorbed from the sensor by mass spectrometry When,

A method for determining atomic hydrogen, comprising:

[2] During the sensor preparation step, the sensor material is prepared by irradiating the sensor material with atomic deuterium,

In the intensity measurement step, the intensity of HD and deuterium desorbed from the sensor is measured, and from this, the amount of atomic deuterium remaining in the sensor is calculated,

In the atomic hydrogen determination step, based on the correlation between the atomic hydrogen irradiation amount for the sensor obtained in advance and the atomic deuterium amount remaining in the sensor by mass spectrometry, 2. The atomic hydrogen quantification method according to claim 1, wherein atomic hydrogen is quantified.

[3] The sensor material includes at least two kinds of metal forces selected from Ni, Cr, Al, Mn, Fe, Co, Be, W, V, Si, C, Nb, Ta, Cu and Ti. The atomic hydrogen determination method according to claim 1 or 2, wherein the alloy is an alloy.

4. The atomic hydrogen determination method according to claim 3, wherein the alloying force is S inconel.

5. The atomic hydrogen determination method according to claim 1 or 2, wherein in the intensity measurement step, mass spectrometry is performed using a quadrupole mass spectrometer.

[6] A sensor chamber that houses a sensor substrate and a heating mechanism that heats the sensor substrate, and an atomic device that is provided in connection with the sensor chamber and introduces atomic deuterium into the sensor chamber so that the flow of the deuterium can be interrupted. Deuterium introduction section, measurement target gas introduction section for introducing the measurement target gas into the sensor chamber so as to be shut off, and mass so that the gas in the sensor chamber can be shut off. An atomic hydrogen quantification device comprising at least a sensor chamber gas deriving unit for deriving to an analyzer.

7. The atom according to claim 6, further comprising an atomic deuterium generator connected to the atomic deuterium introduction part, and a mass spectrometer connected to the sensor chamber gas outlet part. Hydrogen determination device.

8. The atomic hydrogen quantification device according to claim 7, wherein the mass spectrometer is a quadrupole mass spectrometer.

[9] A desorption step of desorbing atomic hydrogen adsorbed on the material by heating the material capable of adsorbing and desorbing atomic hydrogen, and exposing the material to a target gas containing atomic hydrogen. And an adsorption removal step of adsorbing and removing atomic hydrogen in the target gas.

[10] The material is composed of at least two metal forces selected from Ni ゝ Cr ゝ Al, Mn, Fe ゝ Co, Be ゝ W, V, Si ゝ C, Nb ゝ Ta ゝ Cu and Ti. 10. The method for adsorbing and removing atomic hydrogen according to claim 9, wherein the method is an alloy.

11. The method for adsorbing and removing atomic hydrogen according to claim 10, wherein the alloying force is S Inconel.

[12] A material that can absorb and desorb atomic hydrogen, and a heating mechanism that desorbs atomic hydrogen by heating the material, and includes the atomic hydrogen in a state in which the atomic hydrogen is desorbed. An atomic hydrogen adsorption and removal device characterized by being exposed to gas.