JP2014002075A - Non-destructive inspection device and method of using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To analyze components generated from an inspection object with high sensitivity by destructing the inspection object.SOLUTION: An inspection chamber 11 has a gas introducing port 12 and a gas discharging port 13, and can house an inspection object 2 therein while keeping an airtight state except for the gas introducing port 12 and the gas discharging port 13. A destroying portion 18 destroys the inspection object 2 housed in the inspection chamber 11 while keeping the airtight state of the inspection chamber 11. A gas supplying portion for supplying predetermined gas from the gas introducing port 12 has gas purifying portions 23 and 26 for lowering impurity density in the predetermined gas to be predetermined concentration or less. A gas analyzing portion 28 analyzes gas flowing in the inspection chamber 11 and discharged from the gas discharging portion 13 when the gas supplying portion supplies the predetermined gas to the gas introducing port 12, at least after the inspection object 2 is destroyed by the destroying portion 18.

Description

  The present invention relates to a destructive inspection apparatus for destroying and inspecting an inspection target (for example, an organic EL display, a packaged semiconductor device, etc.) having an airtight chamber or the like, and a method of using the same.

  In Patent Document 1 below (for example, paragraph [0002] thereof), in order to know the type and concentration of the gas filled in the gas-filled tube body, the gas-filled tube body is broken in a vacuum vessel to obtain a gas chromatograph. A technique for detecting a gas type and a gas concentration by a mass spectrometer is disclosed.

JP 9-318415 A

  However, in the conventional technique, the inspection object is destroyed in the vacuum container, and as a result, the gas generated from the inspection object diffuses in a relatively wide range in the vacuum due to the destruction. The component could not be analyzed with high sensitivity.

  This invention is made in view of such a situation, and provides the destructive inspection apparatus which can analyze with high sensitivity the component which generate | occur | produces from a test target object by destroying a test target object, and its usage method. For the purpose.

  The following aspects are presented as means for solving the problems. The destructive inspection apparatus according to the first aspect has a gas introduction port and a gas discharge port, and can inspect an inspection object inside while being kept airtight except for the gas introduction port and the gas discharge port. A gas supply unit that supplies a predetermined gas from the gas inlet, and a destruction unit that destroys the inspection object stored in the inspection chamber while maintaining the airtight state of the inspection chamber, A gas supply unit having a gas purification unit for reducing an impurity concentration in a predetermined gas to a predetermined concentration or less, and supplying the predetermined gas to the gas inlet by the gas supply unit, thereby flowing through the inspection chamber and A gas analysis unit that analyzes the gas discharged from the gas discharge port after at least the inspection object is destroyed by the destruction unit. The predetermined concentration is preferably 1 ppb, for example.

  In the first aspect, by supplying a predetermined gas to the gas inlet of the examination room by the gas supply unit, the gas discharged through the examination room gas outlet through the examination room is at least the inspection object. After being destroyed by the destruction part, it is analyzed. Therefore, the component generated from the inspection object due to the destruction of the inspection object does not diffuse so much, so to speak, it moves in a lump so as to be supplied to the gas analysis unit. For this reason, according to the first aspect, the component generated from the inspection object is generated with high sensitivity compared to the conventional technology in which the component diffuses in the vacuum, and is generated from the inspection object by destroying the inspection object. The components to be analyzed can be analyzed.

  In the destructive inspection apparatus according to the second aspect, in the first aspect, the destructive portion includes a needle-shaped, sword-shaped, blade-shaped, or other protruding tool. According to the second aspect, the inspection object can be locally destroyed.

  The destructive inspection apparatus according to a third aspect is the destructive inspection apparatus according to the first aspect, wherein the destructive part has a crushing part that is pressurized by a pressurizing means and crushes the inspection object. According to the third aspect, the inspection object can be totally destroyed.

  In the destructive inspection apparatus according to the fourth aspect, in any of the first to third aspects, the pressure in the inspection chamber at the time of destructive inspection of the inspection object is equal to or higher than atmospheric pressure.

  According to the fourth aspect, since the pressure in the examination chamber is equal to or higher than the atmospheric pressure, it is possible to employ a highly sensitive gas analyzer as in the fifth aspect described below.

  In a destructive inspection apparatus according to a fifth aspect, in any one of the first to fourth aspects, the gas analysis unit includes an atmospheric pressure ionization mass spectrometer, a gas chromatograph, a gas chromatograph and a mass spectrometer that do not include a detector. Or a combination of a gas chromatograph having no detector and an atmospheric pressure ionization mass spectrometer. This fifth aspect is an example of a gas analysis unit, but is preferable because these sensitivities are high.

  A destructive inspection apparatus according to a sixth aspect is the apparatus according to any one of the first to fifth aspects, comprising heating means for heating the inspection chamber.

  According to the sixth aspect, since the heating means is provided, the use method as in the following seventh to tenth aspects becomes possible, which is preferable.

  A method of using the destructive inspection apparatus according to the seventh aspect is a method of using the destructive inspection apparatus according to the sixth aspect, wherein after the inspection object is accommodated in the inspection room, the heating means is used to check the inspection room. The inspection chamber and the inspection object are cleaned by supplying the predetermined gas to the gas introduction port by the gas supply unit while flowing the inspection chamber in a state where the temperature is raised to a temperature higher than room temperature. A cleaning stage, a destruction stage for destroying the inspection object by the destruction section after the cleaning stage, and a gas supply section for supplying the predetermined gas to the gas inlet after the destruction stage. And a gas analysis stage for analyzing the gas flowing through the inspection chamber and discharged from the gas outlet.

  When the inspection object is put into the inspection room, substances such as external air and moisture are introduced into the inspection room, and substances such as moisture are also attached to the inspection object itself. If these are left as they are for inspection, they become the background, and the components generated from the inspection object are buried in the background due to the destruction of the inspection object, which hinders analysis of the component. There is a risk.

  On the other hand, according to the seventh aspect, since the cleaning stage for cleaning the examination room and the inspection object is performed, the background is reduced, and components generated from the inspection object are buried in the background. Therefore, the components can be analyzed appropriately.

  According to an eighth aspect of the method for using the destructive inspection apparatus, in the seventh aspect, the destructive stage is performed in a state where the temperature of the inspection chamber is lower than the temperature of the inspection chamber in the cleaning stage. The gas analysis step is performed in a state where the temperature of the examination room is lower than the temperature of the examination room in the cleaning step.

  According to this eighth aspect, among the components generated from the inspection object due to the destruction of the inspection object, relatively many of those that are likely to adhere to the wall of the examination room adhere to the wall, etc. A relatively large amount of what hardly adheres to the wall of the examination room reaches the gas analysis part and is analyzed by the gas analysis part.

  The method for using the destructive inspection apparatus according to the ninth aspect is the method according to the seventh aspect, wherein the destructive stage is performed in a state where the temperature of the inspection room is lower than the temperature of the inspection room in the cleaning stage. The gas analysis step includes a first gas analysis step performed in a state where the temperature of the inspection chamber is lower than the temperature of the inspection chamber in the cleaning step, and then the first gas analysis step. And a second gas analysis stage performed at a higher temperature.

  According to the ninth aspect, in the first gas analysis stage, among the components generated from the inspection object due to the destruction of the inspection object, relatively many of those components that are likely to adhere to the wall of the inspection room are concerned. While adhering to the wall or the like, a relatively large amount of what is difficult to adhere to the wall or the like of the examination room reaches the gas analysis unit and is analyzed by the gas analysis unit. In the second gas analysis stage, the components adhering to the walls of the examination room in the first gas analysis stage are desorbed and reach the gas analysis section and are analyzed by the gas analysis section. become. In this way, in the first gas analysis stage, among the components generated from the inspection object due to the destruction of the inspection object, those that are difficult to adhere to the walls of the inspection room at a relatively low temperature are mainly observed. On the other hand, in the second gas analysis stage, among the components generated from the inspection object due to the destruction of the inspection object, those that are likely to adhere to the walls of the inspection room at a relatively low temperature are mainly used. Can be observed and can be selected and analyzed.

  According to a tenth aspect of the method for using the destructive inspection apparatus, in the seventh aspect, the destructive step is performed in a state where the temperature of the inspection room is higher than room temperature, and the gas analyzing step includes the step of This is performed in a state where the temperature of the examination room is higher than room temperature.

  According to the tenth aspect, among the components generated from the inspection object due to the destruction of the inspection object, not only those that are difficult to adhere to the wall of the inspection room at a relatively low temperature, but also at a relatively low temperature. Even components that are likely to adhere to the wall or the like of the examination room do not adhere to the wall or the like, but both reach the gas analyzer and are analyzed by the gas analyzer. Therefore, in the tenth aspect, when it is desired to analyze both in a lump, components generated from the inspection object due to the destruction of the inspection object adhere to the walls of the inspection room at a relatively low temperature. This is particularly effective in the case where almost no easy-to-treat components are contained in the first place.

  The method for using the destructive inspection apparatus according to the eleventh aspect is the method using the destructive inspection apparatus according to any one of the first to sixth aspects, or the destructive inspection apparatus according to any one of the seventh to tenth aspects. The inspection object that has been subjected to vibration and / or heat cycle in advance as the inspection object is housed in the inspection room.

  In the eleventh aspect, since the inspection object to which vibration and / or heat cycle has been applied in advance is used, the performance deterioration of the inspection object can be accelerated. Therefore, the time required for the performance deterioration test of the inspection object can be significantly shortened. Therefore, for example, when an organic EL display is used as an inspection target, the durability of the sealing material and the performance of the internal dry adsorbent can be confirmed in a short time.

  ADVANTAGE OF THE INVENTION According to this invention, the destructive inspection apparatus which can analyze with high sensitivity the component which generate | occur | produces from a test target object by destroying a test target object, and its usage method can be provided.

1 is a schematic configuration diagram schematically showing a destructive inspection apparatus according to a first embodiment of the present invention. It is a schematic sectional drawing which shows an example of an organic EL display typically. It is a figure which shows typically the mode of the component which generate | occur | produces from a test target object by destroying a test target object. It is a schematic block diagram which shows typically the destructive inspection apparatus by a comparative example. It is a figure which shows an experimental result. It is another figure which shows an experimental result. It is a schematic block diagram which shows typically the destructive inspection apparatus by the 2nd Embodiment of this invention. It is a schematic block diagram which shows typically the destructive inspection apparatus by the 3rd Embodiment of this invention. It is a schematic sectional drawing which shows typically other examples, such as a test room.

  Hereinafter, a destructive inspection apparatus and a method of using the same according to the present invention will be described with reference to the drawings.

[First Embodiment]
FIG. 1 is a schematic configuration diagram schematically showing a destructive inspection apparatus 1 according to a first embodiment of the present invention.

  The destructive inspection apparatus 1 according to the present embodiment has an inspection chamber 11 having a gas inlet 12 and a gas outlet 13. The inspection chamber 11 can accommodate the inspection object 2 inside while being kept airtight except for the gas inlet 12 and the gas outlet 13. In the present embodiment, the examination chamber 11 has a gas inlet 12 and a gas outlet 13 on the side and a cup-shaped container body 14 having an open top and an upper opening of the container body 14 removably closed. The ICF flange 15 is configured. When the inspection object 2 is put in and out of the inspection chamber 11, the ICF flange 15 is removed from the container body 14. A metal packing 16 is provided between the container main body 14 and the ICF flange 15 so that the airtightness of the inspection chamber 11 is maintained. It is preferable to make the inspection chamber 11 small enough to accommodate the inspection object 2 so that components generated from the inspection object 2 do not diffuse as much as possible.

  The ICF flange 15 is provided with a straight line introduction machine 17. At the tip of the straight line introduction machine 17, a protruding tool 18 is provided as a breaking portion that breaks the inspection object 2 accommodated in the inspection room 11 while keeping the airtight state of the inspection room 11. As the protrusion-shaped tool 18, for example, a needle-shaped tool, a sword mountain-shaped tool, a blade-shaped tool, or the like can be used. In the present embodiment, by using the straight line introduction machine 17, while maintaining the airtight state of the inspection room 11, the protruding tool 18 is advanced to the inspection object 2 to locally destroy the inspection object 2. Can be done.

  In the present embodiment, as a heating means for heating the examination room 11, a heating sheet 19 is provided so as to detachably cover the examination room 11. The heating sheet 19 is removed when the inspection object 2 is taken in and out of the inspection room 11. The heating sheet 19 is configured using, for example, a heat insulating material such as glass wool, a heating wire, and the like, and further provided with a temperature detector such as a thermocouple, and can be heated and maintained at a specified constant temperature. Yes. In order to speed up the cooling, a cooling means for cooling the examination room 11 may be provided. The heating means is not limited to the heating sheet 19 as described above, and may be configured using, for example, a Peltier element. In this case, the heating means can also serve as the cooling means.

  In the present embodiment, argon gas as a predetermined gas from a high-pressure cylinder (not shown) containing high-purity argon gas is introduced through the pipe 21. Instead of the high-pressure cylinder, for example, argon gas produced by evaporating liquid argon may be introduced through the pipe 21. The predetermined gas is not limited to argon gas, and may be nitrogen, helium, hydrogen, or the like, for example.

  The pipe 21 is connected to a gas inlet 23 a of a gas purifier 23 such as a getter purifier via an on-off valve 22. The purified gas discharge port 23b of the gas purifier 23 is connected to the gas inlet 12 of the examination room 11 via a gas purifier 26 such as an on-off valve 24, a flow rate controller 25, and molecular sieves. In the present embodiment, the high-pressure cylinder and the elements 21 to 26 constitute a gas supply unit that supplies argon gas from the gas inlet 12 of the inspection chamber 11 into the inspection chamber 11. Further, in the present embodiment, the gas purifiers 23 and 26 constitute a gas purification unit that reduces the impurity concentration in the argon gas supplied into the examination chamber 11 to a predetermined concentration or less (for example, 1 ppb or less). Yes.

  The gas discharge port 13 of the examination chamber 11 is connected to a gas introduction port 28 a of a known atmospheric pressure ionization mass spectrometer 28 via an on-off valve 27 and a pipe 35. The pipe 35 is preferably thin so that the components generated from the inspection object 2 do not diffuse as much as possible. In addition, the gas discharge port 13 of the examination room 11 is opened to the atmosphere via an on-off valve 29. The gas outlet 28 b of the atmospheric pressure ionization mass spectrometer 28 is opened to the atmosphere via the exhaust pipe 30.

  In the present embodiment, the atmospheric pressure ionization mass spectrometer 28 supplies a predetermined gas (argon gas in the present embodiment) to the gas inlet 12 of the inspection chamber 11 by the gas supply unit, whereby the inspection chamber 11. A gas analyzing unit is configured to analyze the gas flowing through the inside and discharged from the gas discharge port 13 of the inspection chamber 11 after at least the inspection object 2 is destroyed by the destruction unit.

  In the present embodiment, the purified gas discharge port 23b of the gas purifier 23 is connected to the gas of the atmospheric pressure ionization mass spectrometer 28 via the open / close valve 31, the flow rate controller 32, and the gas purifier 33 such as molecular sieves. It is connected to the introduction port 28a.

  FIG. 2 is a schematic cross-sectional view schematically showing an example of the organic EL display 41 as an example of the inspection object 2. The organic EL display 41 includes a glass substrate 42, an anode 43 on the glass substrate 42, an organic EL film 44 on the anode 43, a cathode 45 on the organic EL film 44, and a UV adhesive 46 that also serves as a sealing material. And a glass cap (glass plate) 47 which is bonded to the glass substrate 42 to form a hollow portion (airtight chamber) 49, and an adsorption drying agent 48.

  The sealed portion by the UV adhesive 46 is only the peripheral edge portion of the panel, and the hollow portion 49 is filled with dry nitrogen. Moisture and gas intrusion from the outside of the panel is only in the sealing material 46 portion, and the characteristics of the sealing material 46 greatly affect the life of the organic EL. Moisture that enters from the outside of the panel can be blocked by the sealing material 46, but slight residual moisture inside the panel, moisture attached to the glass surface, metal can, and moisture contained in the sealing material volatilize inside the sealing. The cathode is oxidized or the characteristics of the organic film are remarkably deteriorated. Eventually, a non-light emitting portion called a dark spot is generated, resulting in a dark defect. Therefore, the moisture must be kept below a predetermined concentration inside the panel, and an adsorption drying agent 48 is provided. The main component of the adsorption drying agent 48 is BaO or CaO, and the adsorption performance varies depending on the type and shape. For example, sheet-like CaO is widely used. The adsorptive desiccant 48 can adsorb not only moisture entering from the outside but also outgas generated from other constituent materials including the sealing material 46, and contributes to the extension of the life of the organic EL.

  By using the organic EL display 41 as the inspection object 2, for example, confirming the quality of the organic EL display 41, the durability of the sealing material 46, the performance of the adsorptive desiccant 48, and the like from the destructive inspection result. Can do.

  However, the inspection object 2 is not limited to the organic EL display, and may be, for example, a packaged semiconductor device or another article having an airtight chamber.

  The inspection object 2 to be accommodated in the inspection room 11 is an object to which vibration and / or heat cycle has been applied in advance as necessary. In this case, the performance deterioration of the inspection object 2 can be accelerated. Therefore, the time required for the performance deterioration test or the like of the inspection object 2 can be greatly shortened. Therefore, for example, when the organic EL display is used as the inspection object 2, the durability of the sealing material and the performance of the internal dry adsorbent can be confirmed in a short time. When a normal defective organic EL display is destroyed, a large amount of moisture and oxygen in the atmosphere is detected from the organic EL display due to deterioration of the sealing material.

  When performing the destructive inspection of the inspection object 2 using the destructive inspection apparatus 1 according to the present embodiment, first, the on-off valves 24, 27 are closed and the on-off valves 22, 29, 31 are opened. After the ICF flange 15 is removed and the inspection object 2 is accommodated in the inspection chamber 11, the ICF flange 15 is attached to make the inspection chamber 11 airtight, and the heating sheet 19 is attached.

  Next, in a state where the temperature of the examination room 11 is raised to a predetermined temperature (for example, 100 ° C.) higher than room temperature by the heating sheet 19, the opening / closing valves 22, 24, and 29 are opened and the opening / closing valve 27 is closed. A cleaning step of cleaning the inspection chamber 11 and the inspection object 2 is performed by supplying a pure argon gas to the gas inlet 12 of the inspection chamber 11 and flowing it through the inspection chamber 11. In this cleaning stage, the open / close valve 31 is opened and high purity argon gas is allowed to flow through the gas inlet 28a of the atmospheric pressure ionization mass spectrometer 28 so that the atmosphere does not flow into the ion source of the atmospheric pressure ionization mass spectrometer 28. Keep it.

  After this cleaning stage, the on-off valve 29 is closed and the on-off valve 27 is opened, and the gas flowing through the examination chamber 11 is introduced into the atmospheric pressure ionization mass spectrometer 28. At this time, the pressure in the examination room 11 is almost atmospheric pressure.

  At this time, if it is considered that a large amount of impurities are generated when the inspection object 2 is destroyed, the high purity introduced into the atmospheric pressure ionization mass spectrometer 28 via the on-off valve 31, the flow rate controller 32 and the gas purifier 33. The argon gas flow rate is increased to dilute the gas flowing through the examination chamber 11 and measured (analyzed) by the atmospheric pressure ionization mass spectrometer 28. At this time, if a flow rate controller (not shown) is provided in the middle of the exhaust pipe connected to the on-off valve 29, the on-off valve 29 is opened and the exhaust flow rate is adjusted by the flow rate controller, the inspection chamber 11 The variable range of the dilution rate of the gas flowing through the inside can be expanded. On the other hand, when it is considered that the generation of impurities is small when the inspection object 2 is broken, the on-off valve 31 is closed, and measurement (analysis) is performed using only the gas flowing through the inspection chamber 11.

  In this state, the inspection object 2 is destroyed by the protruding tool 18 at the tip of the straight line introduction machine 17. Components generated from the inspection object 2 due to the destruction are included in the argon gas flowing through the inspection chamber 11 and analyzed by the atmospheric pressure ionization mass spectrometer 28.

  In the first example, even after the cleaning step, the temperature of the examination room 11 is set to a temperature higher than room temperature (for example, at the time of destruction of the inspection object 2 and the subsequent gas analysis by the atmospheric pressure ionization mass spectrometer 28 (for example, , 80 ° C.). In this first example, among the components generated from the inspection object 2 due to the destruction of the inspection object 2, not only those that are difficult to adhere to the wall of the inspection room 11 at a relatively low temperature, but also a relatively low temperature. In this case, components that easily adhere to the wall of the examination room 11 do not adhere to the wall or the like, but both reach the atmospheric pressure ionization mass spectrometer 28 and are analyzed by the atmospheric pressure ionization mass spectrometer 28. Will be. Therefore, in this first example, if it is desired to analyze both in a lump, or components generated from the inspection object 2 due to the destruction of the inspection object 2, the walls of the inspection room at a relatively low temperature, etc. This is particularly effective in the case where almost no components that easily adhere to the film are contained in the first place.

  However, the temperature management of the examination room 11 after the cleaning stage is not limited to the first example.

  For example, in the second example, after the cleaning stage, the inspection object 2 is destroyed and then the atmospheric pressure ionization mass spectrometer 28 is set at a temperature lower than the cleaning stage (for example, 40 ° C.). Gas analysis is performed. In this second example, among the components generated from the inspection object 2 due to the destruction of the inspection object 2, a relatively large part of the components that are likely to adhere to the wall of the inspection room 11 adhere to the wall or the like. A relatively large amount that does not easily adhere to the wall of the examination room 11 reaches the atmospheric pressure ionization mass spectrometer 28 and is analyzed by the atmospheric pressure ionization mass spectrometer 28.

  Further, in the third example, after the cleaning stage, the inspection object 2 is destroyed and then the atmospheric pressure ionization mass spectrometer 28 in a state where the temperature is lower than the cleaning stage (for example, 40 ° C.). The first gas analysis is performed by the atmospheric pressure ionization mass spectrometer 28 in a state where the temperature is higher than that at the time of the first gas analysis (for example, 80 ° C.). . In this third example, among the components generated from the inspection object 2 due to the destruction of the inspection object 2 in the first gas analysis stage, relatively many of the components that are likely to adhere to the wall of the inspection room 11 or the like. While relatively attached to the wall or the like of the examination room 11 while adhering to the wall or the like, a relatively large amount reaches the atmospheric pressure ionization mass spectrometer 28 and is analyzed by the atmospheric pressure ionization mass spectrometer 28. Become. In the second gas analysis stage, components adhering to the wall portion of the examination chamber 11 in the first gas analysis stage are desorbed and reach the atmospheric pressure ionization mass spectrometer 28 to be atmospheric pressure ionized. Analysis is performed by the mass spectrometer 28. In this way, in the first gas analysis stage, among the components generated from the inspection object 2 due to the destruction of the inspection object 2, those that are difficult to adhere to the wall portion of the inspection room 11 at a relatively low temperature. On the other hand, in the second gas analysis stage, the components generated from the inspection object 2 due to the destruction of the inspection object 2 can be mainly observed on the wall of the inspection room 11 at a relatively low temperature. What is likely to adhere can be observed mainly, and both can be selected and analyzed.

  In the present embodiment, as described above, high-purity argon gas is supplied to the gas introduction port 12 of the inspection chamber 11, thereby flowing through the inspection chamber 11 and being discharged from the gas discharge port 13 of the inspection chamber 11. The gas to be analyzed is analyzed after at least the inspection object 2 is broken by the protruding tool 18. Therefore, the components generated from the inspection object 2 due to the destruction of the inspection object 2 do not diffuse so much, so to speak, they move in a lump so as to be supplied to the atmospheric pressure ionization mass spectrometer 28. FIG. 3 shows this state. FIG. 3 schematically shows a state of components generated from the inspection object 2 by destroying the inspection object 2 as a state in the pipe 35 connected to the gas inlet 28 a of the atmospheric pressure ionization mass spectrometer 28. It shows. In FIG. 3, 51 schematically shows components in argon gas (components generated from the inspection object 2 due to destruction), and 52 schematically shows the concentration distribution of the components. For this reason, according to the present embodiment, the inspection object 2 is destroyed by destroying the inspection object 2 with higher sensitivity than the conventional technique in which components generated from the inspection object 2 diffuse in a vacuum. The components generated from can be analyzed.

  FIG. 4 is a schematic configuration diagram schematically showing a destructive inspection apparatus 101 according to a comparative example compared with the destructive inspection apparatus 1 according to the present embodiment. The destructive inspection apparatus 101 according to this comparative example conforms to the above-described conventional technique. In FIG. 4, 102 is an inspection object, 103 is an inspection room, 104 is a linear introduction machine, 105 is a protruding tool provided at the tip of the linear introduction machine 104, 106 is an exhaust pipe, 107 is an on-off valve, Reference numeral 108 denotes a mass spectrometer, and 109 denotes an EI ion source. In this destructive inspection apparatus 101, an inspection object 102 is accommodated in an inspection chamber 103 that is evacuated, and the inspection object 102 is destroyed by a protruding tool 105. Since the component generated from the inspection object 102 is diffused in the vacuum due to the destruction, the component cannot be analyzed with high sensitivity by the mass spectrometer 108. On the other hand, in the destructive inspection apparatus 1 according to the present embodiment, as described above, the components generated from the inspection object 2 due to the destruction of the inspection object 2 do not diffuse so much, so to move in a lump. Thus, the components are supplied to the atmospheric pressure ionization mass spectrometer 28, so that the components can be analyzed with high sensitivity. Also in the detector body, the general vacuum mass spectrometer 108 has a sensitivity of ppm (1 / 1,000,000), but the sensitivity of the atmospheric pressure ionization mass spectrometer 28 is usually ppb (1 billion). Therefore, according to the present embodiment, high-sensitivity measurement is possible from this point as well.

  The inventor conducted the following experiment. As a sample of the inspection object 2, a thin hole was processed in an acrylic plate and air was sealed (first sample), and a sample containing a getter material (second sample) was prepared. The volume of these airtight spaces was about 1 microliter. The getter material was encapsulated by activating the getter material by heating it to 400 ° C. in a small quartz heating furnace. Getter materials generally require activation treatment at high temperatures, and activation treatment in glass or metal is available, but activation treatment in resins such as acrylic is difficult, so getter material encapsulation Was performed in a glove box filled with high-purity argon gas.

  The first sample and the second sample were subjected to destructive inspection using the same apparatus as the destructive inspection apparatus 1 according to the present embodiment in the above-described method. At this time, the temperature management of the examination room 11 after the cleaning stage employs the first method. Oxygen and moisture were detected from the first sample containing the atmosphere. Oxygen and moisture were also detected from the second sample encapsulating the getter material, but they were reduced compared to the case of the first sample. Thereby, it turned out that oxygen and a water | moisture content are reduced when a getter material is put. FIG. 5 is a diagram showing the relationship between the time lapse obtained by the destructive inspection of the first sample by this experiment and the oxygen concentration. FIG. 6 is a diagram showing the relationship between the time lapse obtained by the destructive inspection of the first sample and the water concentration by this experiment. The result of FIG. 5 and the result of FIG. 6 were obtained by the experiment conducted simultaneously.

  From the above experimental results, it was confirmed that a gas component of about 1 microliter generated from the inspection object 2 due to destruction can be analyzed with high sensitivity.

[Second Embodiment]
FIG. 7 is a schematic configuration diagram schematically showing a destructive inspection apparatus 61 according to the second embodiment of the present invention. 7, elements that are the same as or correspond to those in FIG. 1 are given the same reference numerals, and redundant descriptions thereof are omitted.

  The destructive inspection apparatus 61 according to the present embodiment differs from the destructive inspection apparatus 1 according to the first embodiment only in that the on-off valves 27 and 29 are removed.

  When performing the destructive inspection of the inspection object 2 using the destructive inspection apparatus 1 according to the present embodiment, first, the on-off valve 24 is closed and the on-off valves 22 and 31 are opened, and then the heating sheet 19 and the ICF flange 15 are temporarily set. Is removed and the inspection object 2 is accommodated in the inspection room 11, and then the ICF flange 15 is attached to make the inspection room 11 airtight, and the heating sheet 19 is attached.

  Next, in a state where the temperature of the examination room 11 is raised to a predetermined temperature (for example, 100 ° C.) higher than room temperature by the heating sheet 19, the on-off valve 31 is closed and the on-off valves 22 and 24 are kept open. A cleaning stage is performed in which the inspection chamber 11 and the inspection object 2 are cleaned by supplying argon gas to the gas inlet 12 of the inspection chamber 11 and flowing it through the inspection chamber 11.

  After this cleaning step, measurement by the atmospheric pressure ionization mass spectrometer 28 is started. At this time, if it is considered that a large amount of impurities are generated when the inspection object 2 is destroyed, the high purity introduced into the atmospheric pressure ionization mass spectrometer 28 via the on-off valve 31, the flow rate controller 32 and the gas purifier 33. The argon gas flow rate is increased to dilute the gas flowing through the examination chamber 11 and measured (analyzed) by the atmospheric pressure ionization mass spectrometer 28. On the other hand, when it is considered that the generation of impurities is small when the inspection object 2 is broken, the on-off valve 31 is closed, and measurement (analysis) is performed using only the gas flowing through the inspection chamber 11.

  In this state, the inspection object 2 is destroyed by the protruding tool 18 at the tip of the straight line introduction machine 17. Components generated from the inspection object 2 due to the destruction are included in the argon gas flowing through the inspection chamber 11 and analyzed by the atmospheric pressure ionization mass spectrometer 28.

  Also in this embodiment, the same advantages as those in the first embodiment can be obtained. This embodiment is particularly effective when there are few impurities generated from the inspection object 2 due to the destruction of the inspection object 2.

[Third Embodiment]
FIG. 8 is a schematic configuration diagram schematically showing a destructive inspection apparatus 71 according to the third embodiment of the present invention. 8, elements that are the same as or correspond to those in FIG. 1 are given the same reference numerals, and redundant descriptions thereof are omitted.

  The destructive inspection apparatus 71 according to the present embodiment is different from the destructive inspection apparatus 1 according to the first embodiment in that a gas chromatograph with a detector (as a gas analysis unit) instead of the atmospheric pressure ionization mass spectrometer 28 ( GC) 72 is used, and the gas chromatograph 72 requires a pressure to be measured that is equal to or higher than the atmospheric pressure. Therefore, a pressure adjusting device 73 for obtaining the pressure is provided immediately before the gas chromatograph 72. It is only a point. The pressure adjusting device 73 may be a device capable of attaching resistance (conductance) to a pipe, such as a thin tube or a pinhole.

  Also in this embodiment, the same advantages as those in the first embodiment can be obtained.

  In this embodiment, instead of the gas chromatograph 72, the gas analysis unit is a combination of a gas chromatograph without a detector and a mass spectrometer, or a gas chromatograph without a detector and atmospheric pressure ionization mass spectrometry. Combinations with devices may also be used.

  By the way, in each said embodiment, as a destruction part which destroys the test target object 2 accommodated in the inspection room 11 while maintaining the airtight state of the inspection room 11, it is not restricted to the protruding tool 18, For example, inspection. A crushing part may be used for the object 2. FIG. 9 shows an example thereof, and is a schematic cross-sectional view schematically showing another example of the examination room 11 and the like. 9, elements that are the same as or correspond to elements in FIG. 1 are given the same reference numerals, and redundant descriptions thereof are omitted.

  In FIG. 9, 81 is a fluid pressure cylinder such as a hydraulic cylinder or a pneumatic cylinder attached to a member that defines the examination chamber 11, and 82 is a collapse member as a collapse portion provided at the tip of the piston 81 a of the fluid pressure cylinder 81. 83 is a table on which the inspection object 2 is placed, 84 is a metal bellows for keeping the inside of the inspection chamber 11 airtight despite the movement of the piston 81a, and 85 and 86 are metal packings. In FIG. 9, the heating sheet 19 that heats the examination room 11 is not shown.

  Thus, if the crushing part is adopted as the destruction part, the inspection object 2 can be totally destroyed.

  As mentioned above, although each embodiment of this invention and its modification were demonstrated, this invention is not limited to these.

DESCRIPTION OF SYMBOLS 1,61,71 Destructive inspection apparatus 2 Inspection object 11 Inspection room 12 Gas inlet 13 Gas outlet 18 Projection-shaped tool 19 Heating sheet 72 Gas chromatograph 82 Collapse member

Claims (11)

An inspection chamber having a gas inlet and a gas outlet, and capable of accommodating an inspection object inside in a state of being kept airtight except for the gas inlet and the gas outlet;
While maintaining the airtight state of the inspection room, a destruction part for destroying the inspection object accommodated in the inspection room,
A gas supply unit that supplies a predetermined gas from the gas introduction port, the gas supply unit having a gas purification unit that reduces an impurity concentration in the predetermined gas to a predetermined concentration or less;
By supplying the predetermined gas to the gas introduction port by the gas supply unit, at least the inspection object is destroyed by the destruction unit in the gas flowing through the inspection chamber and discharged from the gas discharge port. Later, the gas analyzer to analyze,
A destructive inspection apparatus characterized by comprising:   The destructive inspection apparatus according to claim 1, wherein the destructive portion includes a needle-shaped, sword-shaped, blade-shaped or other protruding tool.   The destructive inspection apparatus according to claim 1, wherein the destructive portion includes a crushing portion that is pressurized by a pressurizing unit to crush the inspection object.   The destructive inspection apparatus according to claim 1, wherein a pressure in the inspection chamber at the time of destructive inspection of the inspection object is equal to or higher than atmospheric pressure.   The gas analyzer includes an atmospheric pressure ionization mass spectrometer, a gas chromatograph, a combination of a gas chromatograph without a detector and a mass spectrometer, or a combination of a gas chromatograph without a detector and an atmospheric pressure ionization mass spectrometer. The destructive inspection apparatus according to claim 1, wherein the apparatus is a destructive inspection apparatus.   The destructive inspection apparatus according to claim 1, further comprising a heating unit that heats the inspection chamber. A method of using the destructive inspection apparatus according to claim 6,
After the inspection object is accommodated in the inspection chamber, the gas supply unit supplies the predetermined gas to the gas introduction port in a state where the inspection chamber is heated to a temperature higher than room temperature by the heating means. A cleaning step of cleaning the inspection room and the inspection object by flowing the inspection room;
After the cleaning step, a destruction step of destroying the inspection object by the destruction part,
A gas analysis stage for analyzing the gas discharged from the gas outlet through the inspection chamber by supplying the predetermined gas to the gas inlet by the gas supply unit after the destruction stage;
A method for using a destructive inspection apparatus, comprising: The destruction step is performed in a state where the temperature of the examination room is lower than the temperature of the examination room of the cleaning step,
The gas analysis step is performed in a state where the temperature of the examination room is lower than the temperature of the examination room of the cleaning step.
A method of using the destructive inspection apparatus according to claim 7. The destruction step is performed in a state where the temperature of the examination room is lower than the temperature of the examination room of the cleaning step,
The gas analysis stage includes a first gas analysis stage performed in a state where the temperature of the examination room is lower than the temperature of the examination room in the cleaning stage, and then, from the first gas analysis stage. A second gas analysis stage carried out at a higher temperature,
A method of using the destructive inspection apparatus according to claim 7. The destruction step is performed in a state where the temperature of the examination room is higher than room temperature,
The gas analysis step is performed in a state where the temperature of the examination room is higher than room temperature.
A method of using the destructive inspection apparatus according to claim 7. A method for using the destructive inspection apparatus according to any one of claims 1 to 6, or a method for using the destructive inspection apparatus according to any one of claims 7 to 10,
A method of using a destructive inspection apparatus, wherein an inspection object to which vibration and / or heat cycle has been applied in advance is accommodated in the inspection room as the inspection object.

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