JP3659943B2 - Apparatus and method for analyzing surface reaction process of diffusion material - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a diffusion material surface reaction process analysis apparatus and method for observing and analyzing the reaction state of a diffusion sample when hydrogen or deuterium permeates into the diffusion material while permeating.
[0002]
[Prior art]
As a conventional technique for reacting a sample with hydrogen or deuterium, there is a technique disclosed in Japanese Patent Application Laid-Open Nos. 8-166476 and 8-166477. JP-A-8-166476 (hereinafter referred to as “first prior art”) describes a sample prepared by including one of light hydrogen and deuterium in a solid such as a metal such as palladium or an alloy thereof. Is heated by a heater in a vacuum vessel to move any one of the gases in the sample to artificially cause a nuclear fusion reaction.
[0003]
In addition, in the above-mentioned JP-A-8-166477 (hereinafter referred to as “second prior art”), the space between the electrolytic cell on the electrolytic solution side, the vacuum vessel, and the cathode electrode as a sample made of palladium or the like is airtight. The device is configured to be closed, and the electrolytic solution is electrolyzed with the cathode electrode and the anode electrode, so that charged particles and X-rays generated by the nuclear reaction at that time cannot pass through the electrolyte solution. A technique for enabling detection is disclosed.
However, although the first conventional technique uses a vacuum vessel to induce a fusion reaction therein, it cannot diffuse hydrogen or deuterium continuously for a long time. Moreover, this prior art measures the radiation generated as a result of the fusion reaction, and does not measure each reaction product (element conversion). On the other hand, in the second conventional technique, since electrolytic storage is used, there is a possibility that impurities may be mixed in unless the nuclear reaction product is produced in large quantities, and there is a problem that measurement accuracy is lacking.
[0004]
[Problems to be solved by the invention]
Japanese Patent Laid-Open No. 2001-165851 proposes a method for analyzing the surface reaction process of a diffusion material and an apparatus for solving such a problem.
In this technique, deuterium is injected into the sample by utilizing the pressure difference between the storage chamber and the discharge chamber. However, deuterium that has passed through the sample is removed from the discharge chamber, while Need to continue to supply deuterium. Therefore, there is a problem that the cost of relatively expensive deuterium increases. In addition, when tritium is used as hydrogen, it is necessary to perform a safe exhaust treatment, and thus there is a problem that costs are increased in order to ensure safety.
[0005]
The present invention has been made in view of the above circumstances, and an object thereof is to provide an apparatus and method for analyzing the surface reaction process of a diffusion material that can reduce the cost.
[0006]
[Means for Solving the Problems]
According to the first aspect of the present invention, there is provided a surface of a diffusing material comprising: an occlusion chamber and a discharge chamber in which a diffusing material capable of diffusing hydrogen gas is sandwiched between each other in an airtight state; In the reaction process analysis device, the circulation device includes a hydrogen supply system that supplies hydrogen into the storage chamber, and a circulation device that returns the gas that has permeated the diffusion material and flowed from the storage chamber into the discharge chamber. Comprises a flow passage communicating the discharge chamber and the storage chamber, and a circulation pump provided in the middle of the flow passage for sending gas from the discharge chamber side to the storage chamber side. A machine is provided .
[0007]
In the present invention, the hydrogen gas that has permeated the diffusion material and flowed from the storage chamber into the discharge chamber is returned to the storage chamber again. Thus, hydrogen gas can be reused. In addition, when tritium is used as hydrogen, high safety can be obtained by recycling tritium without being discharged to the outside.
Further, since the pressurizing compressor is provided in the middle of the flow path, the gas after being pressurized in accordance with the pressure in the storage chamber is returned to the storage chamber.
[0008]
According to a second aspect of the present invention, in the diffusion material surface reaction process analyzing apparatus according to the first aspect, a filter for removing impurities is provided in the middle of the flow path.
[0009]
In this invention, the hydrogen gas is returned to the storage chamber after impurities generated from the circulation pump and the piping system are removed by the filter.
[0012]
According to a third aspect of the present invention, in the diffusion material surface reaction process analyzer according to the first or second aspect , tritium is used as the hydrogen, and tritium detection means for detecting the amount of tritium in the storage chamber is provided. It is characterized by.
[0013]
In the present invention, when a gas containing tritium is used as hydrogen, the increase or decrease of tritium in the system is monitored. Thereby, it is possible to detect when there is a nuclide conversion, leakage or the like.
[0014]
According to a fourth aspect of the present invention, there is provided the diffusion material surface reaction process analyzing apparatus according to the third aspect , wherein the tritium detecting means includes a flow path that exits the storage chamber and returns to the storage chamber, And a tritium monitor.
[0015]
In the present invention, the gas in the storage chamber is taken into the flow path by the circulation pump, and the amount of tritium contained in the gas is detected by the tritium monitor.
[0016]
The invention according to claim 5, the boundary position between the storage chamber and the discharge chamber, a diffusion material capable of diffusing hydrogen and sandwiching airtightly to each other, releasing chamber gas from the storage chamber through the in diffusing material The surface reaction process analysis method of the diffusion material for analyzing the surface of the diffusion material, the step of injecting hydrogen into the diffusion material exposed in a vacuum storage chamber, and the permeation of the diffusion material And a step of compressing hydrogen and returning it to the storage chamber again.
[0017]
In the present invention, the hydrogen gas that has permeated the diffusion material and flowed from the storage chamber into the discharge chamber is returned to the storage chamber again. Thus, hydrogen gas can be reused.
[0018]
A sixth aspect of the present invention is the diffusion material surface reaction process analysis method according to the fifth aspect , wherein tritium is used as the hydrogen, and the tritium detection step of detecting the amount of tritium in the storage chamber is provided. And
[0019]
In the present invention, when a gas containing tritium is used as hydrogen, the increase or decrease of tritium in the system is monitored. Thereby, it is possible to detect when there is a nuclide conversion, leakage or the like.
[0020]
DETAILED DESCRIPTION OF THE INVENTION
Next, embodiments of the present invention will be described with reference to the drawings.
In FIG. 1, reference numeral 1 denotes a sample that is a hydrogen diffusion material, 2 denotes an occlusion chamber, 3 denotes an emission chamber, and the sample 1 is disposed at the boundary position between the occlusion chamber 2 and the emission chamber 3. The space is kept airtight so that impurities are not mixed.
[0021]
The sample 1 may be anything as long as it is a material that allows hydrogen to permeate while diffusing, such as palladium, titanium, vanadium, and the like. In addition, the constituent materials of the storage chamber 2 and the discharge chamber 3 are made of a material that does not adversely affect even if it comes into contact with hydrogen or a diffusion material.
In the present embodiment, the deuterium is used for explanation. However, the present invention is not limited to this, and light hydrogen can be substituted.
[0022]
In this apparatus, an evacuation system 7, a hydrogen supply system 8, and a pressure gauge 19 are provided, and the discharge chamber 3 is provided with an evacuation system (circulation device) 9 and an evacuation system gauge 20. It has been.
The evacuation system 7 is for maintaining the storage chamber 2 in a high vacuum state in advance when supplying deuterium gas, and is provided between the rotary pump 7a, the vacuum valve 7b, and the rotary pump 7a and the vacuum valve 7b. A turbo molecular pump 7c, a vacuum gauge 7d for the storage chamber provided between the vacuum valve 7b and the storage chamber 2 is provided.
The hydrogen supply system 8 fills the storage chamber 2 in a vacuum state with deuterium gas, and includes a deuterium gas cylinder 8a and a variable leak valve 8b.
The evacuation system 9 always keeps the discharge chamber 3 in a vacuum state, and includes a flow path 9 a that exits from the discharge chamber 3 and returns to the storage chamber 2. Further, a turbo molecular pump 9b for evacuating the discharge chamber 3 with respect to the flow path 9a, a circulation pump 9c for sending gas from the discharge chamber 3 side to the storage chamber 2 side, and a gas sent from the circulation pump 9c A compressor 9d for compressing the gas, an external exhaust valve 9e for switching the flow of gas boosted by the compressor 9d to the storage chamber 3 and a flow path for sending it to a separate discharge system, and a filter 9f for removing impurities Are provided in this order from the discharge chamber 3 toward the storage chamber 2. The filter 9f removes impurities generated from the circulation pump 9c and the piping system by cooling the flow path 9a with liquid nitrogen or the like. If the pressure in the storage chamber 2 is not high, the compressor 9d may not be provided. Similarly, the filter 9f may not be provided when impurities generated from the circulation pump 9c and the piping system are extremely small.
[0023]
As shown in the figure, the sample 1 is disposed at a boundary position between the storage chamber 2 and the discharge chamber 3 while being in an airtight state. At that time, the sample 1 is set so that the film formation surface side of the sample 1 faces the storage chamber 2 as shown in FIG. In the figure, reference numeral 4 is a vacuum flange, and 6 is an O-ring.
[0024]
The storage chamber 2 is provided with an XPS measuring device including an electrostatic analyzer 21 and an X-ray gun 22 as analysis means, and an X-ray detector 14 as a radiation measuring instrument.
[0025]
Since the X-ray detector 14 is installed in the atmosphere, a beryllium window 14a is provided between the X-ray source and the storage chamber 2 so as to partition the vacuum and the atmosphere and allow X-rays to pass therethrough. ing.
[0026]
In the present embodiment, first, the sample 1 is set between the storage chamber 2 and the discharge chamber 3. After the sample 1 is set, the vacuum evacuation system 7 on the storage chamber 2 side and the evacuation system 9 on the discharge chamber 3 side are driven to bring both chambers into a high vacuum state at a predetermined pressure. The vacuum exhaust system 9 is exhausted by a turbo molecular pump 9b and exhausted to the outside through an external exhaust valve 9e.
Next, when a predetermined high vacuum state is reached, the state of the sample surface in the storage chamber 2 is measured by the XPS measurement device, and the substances present on the sample surface are measured. After such measurement, the vacuum valve 7 b of the vacuum exhaust system 7 in the storage chamber 2 is closed, while deuterium gas is introduced into the storage chamber 2 by the hydrogen supply system 8. After the introduction of the predetermined amount, the supply of hydrogen is stopped, and the operation of returning the hydrogen permeated to the discharge chamber 3 by the vacuum exhaust system 9 to the storage chamber 2 is performed. At this time, the external exhaust valve 9e is switched to the storage chamber 2 side so that the hydrogen gas sent by the circulation pump 9c is introduced to the storage chamber 2 side.
[0027]
Since the XPS measurement device is a device that can measure only at high vacuum, the X-ray detector 14 is operated without being operated within this time, and the X-ray detector 14 releases X from the sample 1. The dose can be detected.
[0028]
The discharge chamber 3 is exhausted by the turbo molecular pump 9b. Accordingly, the gas that has permeated through the sample 1 is sucked by the turbo molecular pump 9b and sent to the storage chamber 2 side by the circulation pump 9c. At this time, the gas is first pressurized by the compressor 9d in accordance with the pressure in the storage chamber 2, and then impurities are removed by the filter 9f, and then introduced into the storage chamber 2.
Thereafter, after a predetermined time has elapsed, the storage chamber 2 is evacuated again by opening the vacuum valve 7b of the evacuation system 7. Further, the external exhaust valve 9e is switched to the exhaust side.
Then, after the inside of the storage chamber 2 becomes a high vacuum, the XPS measuring device is driven again to perform elemental analysis on the surface side of the sample 1.
[0029]
In this way, the gas in the discharge chamber 3 is returned to the storage chamber 2 by the vacuum exhaust system 9, and deuterium circulates between the storage chamber 2 and the discharge chamber 3. Therefore, deuterium can be used repeatedly, and the effect that cost can be suppressed can be obtained. In addition, when tritium is used as hydrogen, it is possible to circulate and use tritium, which requires high safety for exhaust processing and is costly, and this can also reduce the cost.
Moreover, by compressing with the compressor 9d, the hydrogen gas returned to the storage chamber 2 can be matched with the pressure of the storage chamber 2, and impurities can be removed by passing through the filter 9f.
Moreover, since the state of the sample surface before permeating deuterium and the state of the sample surface after permeating deuterium are measured, the state of the sample 1 before and after the reaction can be analyzed. It is possible to reliably elucidate that the substance was generated. Moreover, since the storage chamber 2, the sample 1, and the discharge chamber 3 are kept airtight for a long time, and the sample 1 is not taken out between them, there is no possibility that impurities are mixed from the outside during the experiment. The substance generated on the surface of the sample 1 can be analyzed accurately and accurately.
[0030]
Next, a second embodiment of the present invention will be described. In addition, about the structure same as the said 1st Embodiment, the same code | symbol is used and the description is abbreviate | omitted.
FIG. 3 is a diagram showing the configuration of the present embodiment. In this embodiment, the deuterium gas cylinder 8a contains tritium as hydrogen.
Tritium detection means 20 is provided. The tritium detection means 20 includes a circulation channel 20a that exits from the storage chamber 2 and returns to the storage chamber 2. The circulation channel 20a includes a tritium monitor 20b and a circulation pump 20c from upstream to downstream. And the filter 20d are provided in this order.
The tritium monitor 20b is a device that detects the amount of tritium, and the filter 20d is a device that removes impurities generated from the circulation pump 20c and the piping system by cooling the circulation channel 20a with liquid nitrogen or the like. Note that the filter 20d may not be provided when impurities generated from the circulation pump 20c and the piping system are extremely small.
[0031]
Next, the operation of this embodiment will be described.
In the present embodiment, as in the first embodiment, hydrogen is supplied from the hydrogen supply system 8 to the storage chamber 2 and permeates through the sample 1 while diffusing. At this time, the gas in the discharge chamber 3 is returned to the storage chamber 2 by the vacuum exhaust system 9 in the same manner as described above, and deuterium circulates between the storage chamber 2 and the discharge chamber 3. Therefore, deuterium can be used repeatedly, and costs can be reduced.
In addition, after stopping the hydrogen supply from the hydrogen supply system 8, the circulation pump 20c is driven to measure the gas in the storage chamber 2 with the tritium monitor 20b. The tritium monitor 20b detects the amount of tritium contained in the gas. Therefore, fluctuations in the amount of tritium in the system (occlusion chamber 2 and release chamber 3) can be detected, and can be detected when there is a nuclide conversion or leakage.
Thus, high safety and low cost can be realized by recycling tritium without exhausting it to the outside.
[0032]
In the illustrated embodiments so far, the configuration in which various analyzers are provided in the storage chamber 2 is shown, but it is needless to say that the analyzer may be provided on the discharge chamber 3 side. Moreover, if these nuclear analysis means are used according to the purpose of analysis, various analysis purposes can be realized. Therefore, not only the examples given in the above-described embodiment, but also those according to at least the contents to be analyzed can be installed and used.
Further, the analyzing means is not necessarily integral with the storage chamber 2 or the discharge chamber 3, and may be provided separately from the storage chamber 2 and the discharge chamber 3. That is, after allowing hydrogen to pass through the sample 1, the sample 1 may be taken out from the storage chamber 2 and the discharge chamber 3, and the sample 1 may be transferred to an analysis means provided outside to perform analysis.
[0033]
【The invention's effect】
As described above, according to the present invention, the gas that permeates the diffusion material and flows from the storage chamber into the discharge chamber is returned to the storage chamber again. As a result, hydrogen gas can be reused and costs can be reduced. In addition, when tritium is used as hydrogen, high safety can be obtained by recycling the tritium without recycling it to the outside.
Further, by providing a filter, impurities coming out of the circulation pump and the piping system can be removed.
Moreover, since the compressor is provided, the hydrogen compressed according to the pressure of the storage chamber can be introduced into the storage chamber.
Furthermore, when tritium is used as hydrogen, it is possible to detect nuclide conversion, leakage, etc. by using tritium detection means.
[Brief description of the drawings]
FIG. 1 is a configuration diagram showing a surface reaction process analyzer according to a first embodiment of the present invention.
2 is a cross-sectional view showing a security maintaining structure among the storage chamber, the sample, and the discharge chamber in FIG. 1. FIG.
FIG. 3 is a configuration diagram illustrating a surface reaction process analyzer according to a second embodiment of the present invention.
[Explanation of symbols]
1 Sample (diffusion material)
2 Storage chamber 3 Release chamber 9 Vacuum exhaust system (circulation device)
9a Channel 9c Circulation pump 9d Compressor 9f Filter 20 Tritium detection means 20a Channel 20b Tritium monitor 20c Circulation pump 20d Filter

Claims (6)

In a diffusion material surface reaction process analysis device comprising an occlusion chamber and a discharge chamber in which a diffusion material capable of diffusing hydrogen gas is sandwiched between each other in an airtight state, and an analysis means for analyzing the surface of the diffusion material.
A hydrogen supply system that supplies hydrogen into the storage chamber, and a circulation device that returns the gas that has passed through the diffusion material and flows from the storage chamber into the discharge chamber, and returns to the storage chamber.
The circulation device includes a flow path that connects the discharge chamber and the storage chamber, and a circulation pump that is provided in the middle of the flow path and sends gas from the discharge chamber side to the storage chamber side .
An apparatus for analyzing a surface reaction process of a diffusing material, characterized in that a pressurizing compressor is provided in the middle of the flow path . In the surface reaction process analyzer of the diffusing material according to claim 1,
A diffusion material surface reaction process analyzer characterized in that a filter for removing impurities is provided in the middle of the flow path. In the surface reaction process analyzer of the diffusing material according to claim 1 or 2 ,
An apparatus for analyzing a surface reaction process of a diffusing material, wherein tritium is used as the hydrogen, and tritium detection means for detecting the amount of tritium in the storage chamber is provided. The surface reaction process analyzer for a diffusing material according to claim 3 ,
The tritium detection means includes a flow path that exits from the storage chamber and returns to the storage chamber, a circulation pump provided in the middle of the flow path, and a tritium monitor. Process analyzer. The boundary position between the storage chamber and the discharge chamber, placed sandwiching the diffusion material capable of diffusing hydrogen airtightly to each other, to release the gas release chamber through the diffusion material from the storage chamber, the surface of the diffusing material A method for analyzing the surface reaction process of a diffusion material
A surface of the diffusion material comprising the steps of injecting hydrogen into the diffusion material exposed in the vacuum storage chamber, and compressing the hydrogen that has permeated the diffusion material and returning it to the storage chamber again. Reaction process analysis method. The surface reaction process analysis method for a diffusing material according to claim 5 ,
A method for analyzing a surface reaction process of a diffusing material, characterized in that tritium is used as the hydrogen and has a tritium detection step of detecting the amount of tritium in the storage chamber.

Images