Patent Description:
When an anaerobic substance that easily chemically reacts with components in the atmosphere (oxygen, nitrogen, water, etc.) is used as a sample, it is necessary to place the sample in a closed space that does not come into contact with the atmosphere and perform measurement and analysis on the sample. Further, even when a substance that is dangerous to a measurer and requires the measurer to exercise caution when handling it is used as a sample, it is also necessary to place the sample in a closed space and perform measurement and analysis on the sample while the sample is prevented from scattering or leaking to the outside.

<CIT> describes an X-ray diffraction chamber that is attachable to an X-ray diffraction apparatus. The chamber comprises a housing, a first X-ray window and a second X-ray window. X-rays of the X-ray diffraction apparatus can pass through the windows so that a sample within the housing can be analyzed.

<CIT> describes a sample holder for an ion milling apparatus. The sample holder comprises a holder body having a sample holding portion for holding the sample, and a cover member detachably mounted to the holder body and hermetically sealing the sample held on the sample holding portion. The holder body has a shield plate for shielding a part of the sample against the ion beam, and a field correcting plate for correcting electrical fields around the sample.

<CIT> (Patent Literature <NUM>) discloses an atmosphere control glove box apparatus integrated with an X-ray diffraction apparatus that enables this kind of measurement and analysis.

In the conventional apparatus disclosed in Patent Literature <NUM> includes a biaxial diffractometer (<NUM>) as an X-ray diffraction apparatus and a glove box (<NUM>) which are connected to each other via an intermediary chamber (<NUM>). A sample table (<NUM>) of the X-ray diffraction apparatus is arranged in the intermediary chamber (<NUM>). The sample is manually set on the sample table (<NUM>) in the intermediary chamber (<NUM>) via an internal space of the glove box (<NUM>) by using a glove (3b).

In the intermediary chamber (<NUM>), for example, an atmosphere in which an inert gas circulates is formed through the glove box (<NUM>). The measurement by the X-ray diffraction apparatus is performed while the sample is placed inside this intermediary chamber (<NUM>).

The conventional apparatus disclosed in Patent Literature <NUM> has a configuration in which the X-ray diffraction apparatus and the intermediary chamber are integrated with each other and the periphery of the sample table of the X-ray diffraction apparatus is covered by the intermediary chamber. Therefore, the sample must be manually loaded and unloaded onto and from the sample table fixed to the X-ray diffraction apparatus via the inside of the glove box as described above, which has posed a problem in workability.

The present invention has been made in view of the above circumstances, and has an object to provide an airtight apparatus, and a measurement system that are capable of easily measuring an anaerobic sample without exposing to the atmosphere.

In order to attain the above object, according to the present invention, an airtight apparatus comprises an airtight box for measurement for placing therein a sample to be measured by an X-ray analysis apparatus installed outside; and a glove box connected to the airtight box for measurement, wherein the airtight box for measurement comprises a housing that is hollow therein and has a connecting unit for connecting the housing to the glove box; a sample stage including a sample loading portion; a measurement window that is provided in the housing to measure a sample loaded on the sample stage from the outside by the X-ray analysis apparatus, wherein the connecting unit of the housing is designed for connection to the glove box which is arranged outside side by side together with the airtight
box for measurement such that the inside of the housing communicates with the inside of the glove box, and the inside of each of the housing and the glove box is put into an airtight state; and an X-ray shielding member arranged for shielding intrusion of X-rays from the inside of the housing into the glove box.

According to the airtight box for measurement having the above-described configuration, it is possible to easily realize the measurement of an anaerobic sample in combination with an X-ray analysis apparatus without exposing to the atmosphere.

The airtight box of the airtight apparatus may comprise a transport stage that is installed in the housing and configured to transport the sample stage, and the transport stage may be configured to extend a transport track of the sample stage up to the inside of the glove box connected to the housing.

By providing the transport stage for transporting the sample stage in the housing, the sample can be placed inside the housing without requiring an operator to insert his or her hand deeply inside the housing, so that workability can be enhanced.

Further, in the airtight box of the airtight apparatus , a measurement position is set inside the housing. Therefore, the airtight box for measurement according to the present invention is preferably configured to further comprise a sample position adjustment mechanism for positioning the sample loaded on the sample stage at the measurement position.

By providing such a sample position adjustment mechanism, it is possible to accurately position the sample at the measurement position of the measurement apparatus and realize highly accurate measurement.

The airtight apparatus may further comprise a pipe communicating with the inside of the housing, and the pipe may be configured to connect with at least one of a vacuum suction pipe and an inert gas supply source.

As a result, it is possible to quickly set the inside of the housing to a vacuum atmospheric state or an inert gas atmospheric state.

Further, in the airtight box of the airtight apparatus X-rays are incident and emitted through the measurement window, the housing is formed of a material that shields X-rays. For example, it is preferable that the housing is configured to prevent scattered X-rays in the airtight box for measurement from leaking to the outside. Note that the measurement window is formed of a material that transmits X-rays.

As mentioned above, the airtight box for measurement further comprises an X-ray shielding member for shielding intrusion of X-rays from the inside of the housing into the glove box.

By providing the X-ray shielding member, a work in the glove box can be performed in parallel with measurement by the X-ray analysis apparatus, so that the efficiency of the work can be enhanced.

Since the airtight box for measurement is provided with the sample stage in the housing, the thus-configured airtight apparatus can be also used for measurement to be performed by using various measurement apparatuses without being integrated with each measurement apparatus, and thus it is highly versatile.

The glove box of the airtight apparatus may be configured to include a blocking member configured to block an opening portion communicating with the inside of the housing to partition off the inside of the glove box from the inside of the housing, thereby
putting the inside of the glove box into an airtight state.

The inside of the glove box is partitioned off from the inside of the housing by this blocking member, so that a work environment that should be performed independently inside each of the glove box and the airtight box for measurement can be prepared in such a case that maintenance of the glove box or the airtight box for measurement is performed.

Further, a measurement system according to the present invention comprises an X-ray analysis apparatus and the airtight apparatus having the foregoing configuration; the X-ray analysis apparatus is configured to measure a sample loaded on the sample stage through the measurement window.

According to the thus-configured measurement system, since the airtight apparatus is provided with the sample stage in the housing, various measurements can be performed by combining an appropriately selected measurement apparatus with the airtight apparatus.

Further, the measurement system according to the present invention may be configured so that the X-ray analysis apparatus includes a controller for outputting a control signal for controlling the sample position adjustment mechanism for positioning the sample loaded on the sample stage at a measurement position.

Further, the measurement system according to the present invention may be configured such that the X-ray analysis apparatus includes a goniometer, and the measurement system further comprises a positioning member for fixing and positioning the airtight box for measurement to the goniometer.

The positioning member makes it possible to position the sample stage provided in the airtight box for measurement at the measurement position of the X-ray analysis apparatus with higher accuracy.

The measurement system according to the present invention may be configured such that that the X-ray analysis apparatus comprises
an opening/closing door, the measurement position is set inside the opening/closing door, and the opening/closing door includes a cutout through which a part of the housing is inserted to arrange the measurement window at a position corresponding to the measurement position.

By providing such a cutout in the opening/closing door, the measurement window of the airtight box for measurement can be arranged at a position corresponding to the measurement position with a simple configuration.

Here, the cutout formed in the opening/closing door allows a part of the housing having a flange at an intermediate portion thereof to pass through the cutout, and is formed to be smaller than an outer shape of the flange, and a mount portion of the flange is provided near the inside of the opening/closing door.

The inside and outside of the opening/closing door can be partitioned by the flange.

Further, the X-ray analysis apparatus of the above-described measurement system is preferably provided with a sensor for detecting a state where the opening/closing door is closed and the flange is mounted at the mount portion.

This sensor makes it possible to check the closed state of the opening/closing door and the state where the cutout is partitioned by the flange.

As described above, according to the present invention, desired measurement for an anaerobic sample can be easily realized without exposing to the atmosphere.

<FIG> is a partially cross-sectional front view showing a schematic structure of a measurement system according to an embodiment of the present invention. First, the schematic structure of the measurement system according to the embodiment of the present invention will be described with reference to <FIG>.

The measurement system is configured by the combination of a measurement apparatus <NUM>, a glove box <NUM>, and an airtight box <NUM> for measurement. Further, the combination of the glove box <NUM> and the airtight box <NUM> for measurement constitutes the airtight apparatus.

The measurement apparatus <NUM> is an apparatus capable of irradiating a sample as a measurement target in the airtight box <NUM> for measurement with an electromagnetic wave from an energy source (a light source on an incident side) installed in the atmosphere, detecting photons emitted from the sample by a detector which is outside the airtight box <NUM> for measurement and installed in the atmosphere and performing analysis. A non-destructive inspection machine that uses X-rays , ultraviolet rays, visible rays, terahertz waves, or the like can be arbitrarily selected and applied as the measurement apparatus <NUM> according to the purpose of measurement. For example, when a substance constituting a sample or a crystal structure of the substance or morphological analysis of the inside and outside of the sample is determined, an X-ray diffraction apparatus, a fluorescent X-ray apparatus, and an X-ray CT apparatus using an X-ray wavelength can be applied as the measurement apparatus <NUM>.

As is well known, the glove box (GB) <NUM> is a physical and chemical apparatus that has an internal space having a closed structure and is capable of performing various operations in the internal space in a state where it is shielded from the outside air. Rubber gloves that can be inserted into the internal space are provided on the front of the glove box <NUM> so that an operator can wear these rubber gloves on both hands and operates samples, tools, etc. inside the glove box <NUM>.

The glove box <NUM> is also provided with an auxiliary box called an antechamber <NUM> (pass box) which is arranged side by side together with the glove box <NUM> and used to insert/remove articles into/from the glove box <NUM>, and samples, tools, etc. are inserted into the glove box <NUM> via the antechamber <NUM>. After operations have been finished, the samples, the tools, and the like in the glove box <NUM> can be removed to the outside via the antechamber <NUM>.

The airtight box <NUM> for measurement includes a housing <NUM> having a hollow therein. The housing <NUM> has a laterally elongated shape, and one side end surface 31a (right end surface in <FIG>) thereof is opened. The opened side end surface 31a is connected to a side wall of the glove box <NUM> which is arranged outside side by side together with the airtight box <NUM> for measurement. The glove box <NUM> is provided with an opening portion 20a at a side wall portion thereof to which the housing <NUM> is connected, and this opening portion 20a is aligned with the opening of the side end surface 31a in the housing <NUM>, whereby the inside of the housing <NUM> can be caused to communicate with the inside of the glove box <NUM>.

Here, the inside of the housing <NUM> is configured to have no gap except for the opening of the side end surface 31a. Therefore, the inside of the housing <NUM> and the inside of the glove box <NUM> which are connected to each other are put into an airtight state.

Note that known connecting means can be appropriately selected and used as a method of connecting the housing <NUM> to the glove box <NUM>. For example, it is possible to construct a connecting structure by providing a flange on a side end edge of the housing <NUM>, bringing the flange into close contact with the side wall of the glove box <NUM> via packing, and fixing the flange to the side wall of the glove box <NUM> with fasteners such as bolts and nuts or the like.

A sample stage <NUM> and a transport stage <NUM> are provided inside the housing <NUM>. The sample stage <NUM> is mounted on the transport stage <NUM>. The transport stage <NUM> is transport means for transporting the sample stage <NUM> in an axial direction (right-and-left direction in <FIG>) of the housing <NUM>. The transport stage <NUM> can be configured by using, for example, a known slider mechanism.

Here, the transport stage <NUM> is configured to be able to transport the sample stage <NUM> to the inside of the glove box <NUM>. By extending a transport track of the sample stage <NUM> to the inside of the glove box <NUM> as described above, it is possible to load a sample onto the sample stage <NUM> in the glove box <NUM> and easily transport the sample stage <NUM> into the housing <NUM> as it is, thereby enhancing workability.

The sample stage <NUM> is provided with a sample loading portion, and the sample is loaded onto the loading portion. The work of loading the sample onto the sample stage <NUM> is performed inside the glove box <NUM> as described above.

Further, the housing <NUM> is provided with a measurement window <NUM>. The measurement window <NUM> is a component for measuring the sample loaded on the sample stage <NUM> from the outside of the housing <NUM> by the measurement apparatus <NUM>. The position at which the measurement window <NUM> is formed adjusted so that the sample placed inside the housing <NUM> can be measured by the measurement apparatus <NUM> to be used in combination.

Further, the measurement window <NUM> is closed by a window member to keep the inside of the housing <NUM> in an airtight state. A material to be applied to the window member is selected according to the measurement apparatus <NUM> to be used in combination. It is possible to perform analysis with the measurement apparatus <NUM> using X-rays, ultraviolet rays, visible rays, or terahertz waves by using, for example, a material such as beryllium, silicon nitride, glassy carbon, Ge (germanium), Si (silicon), diamond, sapphire, CaF2 (calcium fluoride), ZnSe (zinc selenide), ZnS (zinc sulfide), chalcogenide glass or quartz as the material for the window member.

Further, by using a material (transmitting therethrough light or the like) having a wavelength common to a plurality of measurement apparatuses <NUM> for the window member, it is also possible to configure the airtight box <NUM> for measurement with which measurements can be performed by the plurality of measurement apparatuses <NUM>.

A measurement position A is preset inside the housing <NUM>. The measurement position A preset inside the housing <NUM> is positionally adjusted so as to coincide with a measurement position (not shown) set in the measurement apparatus <NUM> when the measurement system is constructed by combining the airtight box <NUM> for measurement with the measurement apparatus <NUM>.

Further, when a measurement is performed, a sample loaded on the sample stage <NUM> is positioned at the measurement position A set inside the housing <NUM>. In order to perform this positioning, the airtight box <NUM> for measurement is provided with a sample position adjustment mechanism <NUM>. Various moving mechanisms capable of moving and adjusting the sample so that the measurement position coincides with the measurement position A can be applied to the sample position adjustment mechanism <NUM>.

For example, the positioning in the axial direction of the housing <NUM> can be realized by a configuration in which the transport stage <NUM> is provided with a stopper <NUM>, and the movement of the transport stage <NUM> is stopped by the stopper <NUM> when the sample loaded on the sample stage <NUM> has reached the measurement position A. Further, the positioning in the height direction can be realized by incorporating an elevating mechanism <NUM> into the sample stage <NUM> and adjusting the height position of the sample by driving the elevating mechanism <NUM>.

Note that with respect to a front-and-rear direction (a direction vertical to the paper surface of <FIG>), the front-and-rear positions of the sample stage <NUM> and the transport stage <NUM> may be adjusted in advance according to the measurement position A. Further, if necessary, a front-and-rear drive mechanism may be incorporated in the sample stage <NUM>.

Here, the elevating mechanism <NUM> incorporated in the sample stage <NUM> is controlled to be driven based on a control signal from a controller <NUM> installed in the measurement apparatus <NUM>, and positions the sample loaded on the sample stage <NUM> at the measurement position A.

The measurement window <NUM> described above is formed at a place corresponding to the measurement position A set inside the housing <NUM>. In other words, the measurement window <NUM> is formed in the housing <NUM> while positionally adjusted so that the measurement apparatus <NUM> can measure the sample placed at the measurement position A set inside the housing <NUM> through the measurement window <NUM>.

Further, a pipe <NUM> is connected to each of the glove box <NUM> and the housing <NUM> of the airtight box <NUM> for measurement. The pipe <NUM> is configured to be connectable to any one of a vacuum suction pump <NUM> and an inert gas supply source <NUM> by switching a valve <NUM>. As described above, the measurement system (and the airtight apparatus) of the present embodiment connects the pipe <NUM> to not only the glove box <NUM>, but also the housing <NUM> of the airtight box <NUM> for measurement, whereby the inside of the housing <NUM> can be directly evacuated and an inert gas can be directly supplied into the housing <NUM>. Therefore, the inside of the housing <NUM> can be quickly set to the same atmospheric state as the inside of the glove box <NUM>.

Note that the glove box <NUM> is provided with a blocking member <NUM> for blocking the opening portion 20a. The blocking member <NUM> is configured so as to be manually operated from the inside of the glove box <NUM> to be moved to and fixed at a position where the opening portion 20a is blocked.

The inside of the glove box <NUM> is partitioned off from the inside of the housing <NUM> by the blocking member <NUM>, whereby it is possible to prepare a work environment to be independently performed in each of the boxes <NUM> and <NUM> when maintenance of the glove box <NUM> and the airtight box <NUM> for measurement is performed or the like. For example, a maintenance work in the glove box <NUM> can be performed while maintaining the atmosphere inside the glove box <NUM>. Further, the maintenance of the airtight box <NUM> for measurement can be performed independently while maintaining the atmosphere inside the glove box <NUM>.

Next, a specific configuration example of the measurement system according to the embodiment of the present invention in which the measurement apparatus is an X-ray diffraction apparatus will be described in detail with reference to <FIG>.

<FIG> is a perspective view showing the appearance of the measurement system according to the present embodiment in which the measurement apparatus is an X-ray diffraction apparatus, <FIG> is a plan view showing the appearance of the measurement system according to the present embodiment, and <FIG> is a front view showing the appearance of the measurement system according to the present embodiment.

Note that the same parts as or corresponding parts to those of the schematic structure shown in <FIG> are represented by the same reference signs.

The measurement system according to the present embodiment is configured by the combination of the X-ray diffraction apparatus <NUM> as the measurement apparatus, the glove box <NUM>, and the airtight box <NUM> for measurement.

The X-ray diffraction apparatus <NUM> is an apparatus often used in material study because it can provide information on the crystallinity, crystal structure, and crystal orientation of a material in a non-destructive and non-contact manner and can identify unknown substances. In general, the X-ray diffraction apparatus <NUM> includes an X-ray source for generating X-rays, a goniometer for accurately measuring an angle, and an X-ray detector for measuring X-ray intensity, and data processing system for controlling these components and calculates count values.

Generally, examples of the goniometer include a θ-2θ type goniometer in which the position of the X-ray source is fixed and the sample is rotated by an angle of θ at the same time when the X-ray detector is rotated by an angle of 2θ, and a θ-θ type goniometer in which the X-ray source and the X-ray detector operate while keeping the same angle with respect to a horizontally arranged sample.

In this embodiment, since it is necessary to deal with a sample having high fluidity and the sample stage <NUM> for loading the sample is installed in the airtight box, a configuration in which an X-ray diffraction apparatus <NUM> adopting the θ-θ type goniometer for the horizontally arranged sample is used as the measurement apparatus will be described.

These components constituting the X-ray diffraction apparatus <NUM> are accommodated and arranged inside an X-ray shielding cover <NUM>, and a safety measure is taken to prevent X-rays from leaking to the outside during measurement.

Further, the X-ray shielding cover <NUM> shown in the figure is provided with opening/closing doors <NUM> on the front surface thereof. In the present embodiment, a part of the housing <NUM> of the airtight box <NUM> for measurement is inserted into the X-ray shielding cover <NUM> so that the part of the housing <NUM> penetrates through the opening/closing doors <NUM>.

<FIG> is a perspective view showing the appearance of the airtight box for measurement connected to the side wall of the glove box. The airtight apparatus of the present embodiment is constructed by the combination of the glove box <NUM> and the airtight box <NUM> for measurement as shown in figures.

The airtight box <NUM> for measurement includes a housing <NUM>, a transport stage <NUM>, and a sample stage <NUM>. The housing <NUM> is connected to the side wall of the glove box <NUM>, and the inside of the housing <NUM> communicates with the inside of the glove box <NUM>. The housing <NUM> is made of a material that shields X-rays, and X-rays do not intrude into the housing <NUM> from portions other than the measurement window <NUM>. The transport stage <NUM> transports the sample stage <NUM> in the axial direction of the housing <NUM>, and further extends the transport path thereof to the inside of the glove box <NUM>.

<FIG> is a perspective view showing the appearance of the housing constituting the airtight box for measurement, and <FIG> is a perspective view showing the two-divided structure of the housing.

The housing <NUM> is hollow therein and has a laterally elongated shape, and one side end surface 31a thereof is opened. A flange (side end flange <NUM>) is formed on the side end edge of the housing <NUM> which is a peripheral edge of the opening. A connection structure is constructed in the housing <NUM> by bringing the side end flange <NUM> into contact with the side wall of the glove box <NUM> via a packing (not shown) and fixing the side end flange <NUM> to the side wall of the glove box <NUM> with fasteners such as bolts and nuts or the like (see <FIG>).

As shown in <FIG>, the housing <NUM> is divided into two parts at a middle portion in the axial direction, and a housing element (a housing base end portion 31A) on a base end portion side with respect to the middle portion is kept to be connected to the side wall of the glove box <NUM> whereas a housing element (a housing tip portion 31B) on a tip portion side with respect to the middle portion is freely detachable. In other words, flanges (middle flanges <NUM>) are formed at joint portions of the housing base end portion 31A and the housing tip end portion 31B, and the middle flanges <NUM> are brought into contact with each other via a packing (not shown) and fastened to each other by using fasters such as bolts and nuts or the like, thereby constructing an integrated housing <NUM>.

Further, the housing tip portion 31B can be easily separated from the housing base end portion 31A by merely removing the fasteners. By removing the housing tip portion 31B in this way, operations such as maintenance and adjustment of the sample stage <NUM> and the transport stage <NUM> provided inside the housing <NUM> or change of the configuration of the sample stage <NUM> can be easily and quickly performed.

As shown in <FIG>, the measurement position A is set inside the housing <NUM>. The housing <NUM> is arranged relatively to the X-ray diffraction apparatus <NUM> in a state where the measurement position A is positioned at a measurement position set in the X-ray diffraction apparatus <NUM> (hereinafter may be referred to as an X-ray irradiation position). The sample is loaded on the sample stage <NUM> and is arranged at the measurement position A through the transport operation by the transport stage <NUM> and the elevating operation by the sample stage <NUM>.

The X-ray diffraction apparatus <NUM> irradiates the sample placed at the measurement position A inside the housing <NUM> with X-rays, and detects diffracted X-rays reflected from the sample by the X-ray detector.

<FIG> is a side cross-sectional view showing the measurement window provided in the housing.

The measurement window <NUM> includes an incidence-side measurement window 40a and an emission-side measurement window 40b. As described above, the sample is placed at the measurement position A set in the housing <NUM>. The incidence-side measurement window 40a is provided at a place where X-rays from the X-ray source <NUM> can be incident therethrough and the surface of the sample placed at the measurement position A can be irradiated with the X-rays. Further, the emission-side measurement window 40b is provided at a place where diffracted X-rays reflected from the surface of the sample placed at the measurement position A can be emitted to the X-ray detector <NUM> provided outside.

The measurement window <NUM> is blocked by a window member made of a material (for example, beryllium) having a characteristic of blocking the atmosphere, but transmitting X-rays therethrough.

Note that the measurement window <NUM> can be formed in a continuous linear shape extending from an upper portion of the front surface to an upper portion of the back surface through the upper surface, for example.

<FIG> is a front view showing the appearance of the transport stage.

The transport stage <NUM> is configured so that a slider <NUM> slides along a guide rail <NUM> fixed to the floor surface of the housing <NUM> to enable the sample stage <NUM> to be transported to the inside of the glove box <NUM>. The sample stage <NUM> is mounted on the upper surface of the slider <NUM>.

The slider <NUM> is provided with an operating handle <NUM> at an end portion thereof on the glove box <NUM> side. The operator can grasp the operating handle <NUM> from the inside of the glove box <NUM> and easily move the slider <NUM>. Note that although not shown in <FIG>, the slider <NUM> includes an intermediate slider and an upper slider, and the intermediate slider engages with the upper slider and moves integrally with the upper slider in a process of moving the upper slider to the tip portion of the housing <NUM>. As a result, the sample stage <NUM> can be pulled out from the housing <NUM> and moved to the inside of the glove box <NUM>.

Note that it is also possible to install a drive motor for driving the transport stage <NUM> in the airtight box <NUM> for measurement and control the drive motor based on a control signal from the controller <NUM> (see <FIG>) provided in the measurement apparatus (X-ray diffraction apparatus) <NUM> to move the transport stage <NUM>.

The slider <NUM> of the transport stage <NUM> is provided with an X-ray shielding member <NUM> at a position where the X-ray shielding member <NUM> is closer to the glove box <NUM> than the sample stage <NUM>. The X-ray shielding member <NUM> is formed in a plate-like shape with a material capable of shielding X-rays, and arranged along the cross-section of the housing <NUM>. The internal space of the housing <NUM> is partitioned off by the X-shielding member <NUM>. Therefore, scattered X-rays generated around the sample stage <NUM> during the X-ray diffraction measurement are shielded by the housing <NUM> and the X-ray shielding member <NUM>, so that leakage of the X-rays to the glove box <NUM> side can be prevented.

<FIG> are front views showing the sample position adjustment mechanism to the measurement position.

Like the schematic structure described above, the measurement position A is preset inside the housing <NUM>.

The stopper <NUM> is fixedly provided inside the housing <NUM> and on the floor surface near the tip of the housing <NUM>. The stopper <NUM> abuts against the sample stage <NUM> that has been moved to the tip of the housing <NUM> by the transport stage <NUM>, thereby restricting the movement of the sample stage <NUM>. The setup position of the stopper <NUM> is adjusted so that when the sample stage <NUM> abuts against the stopper <NUM>, the sample loaded on the sample stage <NUM> is positioned at the same position in the axial position as the measurement position A set in the housing <NUM>.

Further, the sample stage <NUM> is incorporated with the elevating mechanism <NUM> for adjusting the height position of the sample. The position adjustment in the height direction with respect to the measurement position A set in the housing <NUM> is performed by the elevating mechanism <NUM>. The stopper <NUM> and the elevating mechanism <NUM> constitute the sample position adjustment mechanism <NUM> for positioning the sample loaded on the sample stage <NUM> at the measurement position A.

<FIG> is a perspective view showing a structure in which the tip portion of the housing is fixed to the goniometer of the X-ray diffraction apparatus, and <FIG> is an enlarged front view showing a fixed structure of the tip portion.

The measurement position A set inside the housing <NUM> is positionally adjusted so as to coincide with the X-ray irradiation position (not shown) set in the X-ray diffraction apparatus <NUM> when the measurement system is constructed by combining the airtight box <NUM> for measurement with the X-ray diffraction apparatus <NUM>. However, in a case where the X-ray diffraction apparatus <NUM> and the airtight box <NUM> for measurement are arranged independently of each other, the tip portion of the housing <NUM> is likely to sag downward because the sample stage <NUM> is mounted inside the housing <NUM> extending in the axial direction, so that there is a risk that the measurement position A set inside the housing <NUM> may deviate from the X-ray irradiation position set in the X-ray diffraction apparatus <NUM>.

Therefore, in the present embodiment, as shown in <FIG>, the tip portion of the housing <NUM> is fixed to the goniometer <NUM> of the X-ray diffraction apparatus <NUM> by a positioning member <NUM>, whereby the housing <NUM> of the airtight box <NUM> for measurement is positioned with respect to the goniometer <NUM>.

Specifically, the tip portion of the housing <NUM> is fixed to the goniometer <NUM> by using the positioning member <NUM> with the transport stage <NUM> abutting against the stopper <NUM> so as to cause the measurement position A set inside the housing <NUM> to coincide with the X-ray irradiation position set in the X-ray diffraction apparatus <NUM>.

As a result, the tip portion of the housing <NUM> is prevented from sagging, and the measurement position A can be stably positioned at the X-ray irradiation position. Further, by removing the positioning member <NUM>, the X-ray diffraction apparatus (measurement apparatus) <NUM> and the airtight apparatus (including the airtight box <NUM> for measurement and the glove box <NUM>) can be easily separated from each other, so that each of the X-ray diffraction apparatus <NUM> and the airtight apparatus can be used as a single apparatus.

<FIG>, <FIG> are diagrams showing an X-ray shielding structure provided between the opening/closing door of the X-ray diffraction apparatus and an intermediate flange of the housing. Specifically, <FIG> are perspective views that give a bird's-eye view of the appearance of the X-ray diffraction apparatus and the airtight box for measurement. <FIG> is a perspective view of cutouts formed in the opening/closing door as viewed from the back surface side. <FIG> is a perspective view of the X-ray shielding structure as viewed from the back surface side of the opening/closing door (that is, the inside of an X-ray shielding cover).

As shown in <FIG>, and <FIG>, cutouts <NUM> and <NUM> are formed in the opening/closing doors <NUM> provided on the front surface of the X-ray shielding cover <NUM>. These cutouts <NUM> and <NUM> form an opening for inserting a part of the housing <NUM> into the X-ray shielding cover <NUM>. These cutouts <NUM> and <NUM> mate with each other while the opening/closing doors <NUM> are closed, thereby forming one opening (see <FIG>).

In the housing <NUM> of the airtight box <NUM> for measurement, the housing tip end portion 31B shown in <FIG> is inserted from the cutouts <NUM> into the X-ray shielding cover <NUM> and arranged there. Here, as shown in <FIG>, the intermediate flange <NUM> of the housing <NUM> is arranged so as to cover the peripheral edge portions of the cutouts <NUM> from the back surface side of the opening/closing doors <NUM>. As a result, it is possible to prevent X-rays from leaking from the internal space of the X-ray diffraction apparatus <NUM> covered by the X-ray shielding cover <NUM> through the cutouts <NUM> to the outside. In other words, the intermediate flange <NUM> of the housing <NUM> constitutes the X-ray shielding structure for the cutouts <NUM>.

Further, as shown in <FIG>, a closing check sensor <NUM> is installed on the opening/closing doors <NUM>, and the closing check sensor <NUM> detects a closed state of the opening/closing doors <NUM>. Further, an X-ray shielding check sensor <NUM> is installed to be shared to the opening/closing door and the intermediate flange <NUM>, and the X-ray shielding check sensor <NUM> detects that the peripheral edge portions of the cutouts <NUM> are covered by the intermediate flange <NUM> of the housing <NUM> from the back surface side.

Based on a detection signal from each of the proximity sensors <NUM> and <NUM>, it is possible to prevent any operation of the X-ray diffraction apparatus <NUM> under a state where the opening/closing doors <NUM> are left open or the housing <NUM> is not arranged before the operation is executed.

Note that the foregoing configuration may be modified so that the closed state of the opening/closing doors <NUM> can be also detected by the sensor (X-ray shielding check sensor <NUM>) provided to be shared to the opening/closing door <NUM> and the intermediate flange <NUM>. In this case, the sensor (closing check sensor <NUM>) provided to be shared to the opening/closing doors <NUM> may be omitted.

<FIG> is a perspective view showing the pipes connected to the glove box and the housing of the airtight box for measurement, and the blocking member for blocking the opening portion of the glove box. As shown in <FIG>, the pipe <NUM> is connected to each of the glove box <NUM> and the housing <NUM> of the airtight box <NUM> for measurement. Like the schematic structure shown in <FIG>, these pipes <NUM> are configured to be connectable to any one of the vacuum suction pump <NUM> and the inert gas supply source <NUM> by switching the valve <NUM>.

Further, the blocking member <NUM> is freely attachable to and detachable from the opening portion 20a of the glove box <NUM>.

The connection of the pipes <NUM> to the glove box <NUM> and the housing <NUM> as described above makes it possible to set the inside of the airtight box <NUM> for measurement to the same atmospheric state as the inside of the glove box <NUM> even when the opening portion 20a of the glove box <NUM> is blocked by the blocking member <NUM> during maintenance of the airtight box <NUM> for measurement.

Further, the connection of the pipe <NUM> to the airtight box <NUM> for measurement makes it possible to uniformly and quickly set the inside of the airtight box <NUM> for measurement to the same atmospheric state as the inside of the glove box <NUM>.

According to the following procedure, the measurement system having the specific configuration described above can measure an anaerobic sample under an environment where the atmosphere is blocked.

A required atmosphere such as a vacuum atmosphere or an inert gas atmosphere is formed inside the glove box <NUM> and the housing <NUM>. In other words, the inside of the housing <NUM> connected to the glove box <NUM> can be forcibly exhausted in a short time by a vacuum suction pump. Further, after the forced exhaust by the vacuum suction pump, inert gas can be purged and enclosed to form a required atmosphere.

The X-ray diffraction apparatus <NUM> is operated while the sample stage <NUM> in the housing <NUM> is caused to abut against the stopper <NUM> (see <FIG>), thereby performing a height adjustment operation for the sample loading portion called half-split. Through this operation, the height of the sample loading portion is adjusted to the measurement position A in the housing <NUM>.

Thereafter, as shown in <FIG> and <FIG>, a measurement target sample and necessary tools and the like are inserted into the glove box <NUM> via the antechamber <NUM> which is arranged side by side together with the glove box <NUM>.

Next, the operator puts on the rubber gloves provided in the glove box <NUM> and operates the sample in the glove box <NUM> from the outside to execute a pretreatment for X-ray diffraction measurement. Then, as shown in <FIG>, the sample stage <NUM> installed inside the housing <NUM> is moved to the inside of the glove box <NUM>, and the sample is loaded onto the sample stage <NUM>. Subsequently, the sample stage <NUM> is moved into the housing <NUM>, and stopped when it abuts against the stopper <NUM> (see <FIG>). As described above, since the height has already been adjusted, the sample is placed at the measurement position A by stopping the sample stage <NUM> at a position where the sample stage <NUM> abuts against the stopper <NUM>.

Thereafter, the X-ray diffraction apparatus <NUM> is operated to perform X-ray diffraction measurement on the sample in the housing <NUM>. After the measurement is completed, the sample stage <NUM> in the housing <NUM> is moved to the inside of the glove box <NUM> again (see <FIG>), and the measured sample is removed from the sample stage <NUM>. Subsequently, after a necessary post-treatment is completed in the glove box <NUM>, the sample is taken out to the outside via the antechamber <NUM>.

Note that the present invention is not limited to the above-described embodiment, and it goes without saying that various modifications and applications can be implemented.

For example, the airtight box for measurement according to the present invention can be configured by using a well-known glove box. In that case, an existing glove box may be provided with a connecting unit to be connected to a connecting unit of the housing <NUM>.

Since an energy source (a light source on the incident side) and the detector of the measurement apparatus can be installed in the atmosphere, these units of a general-purpose measurement apparatus can be used in combination with the airtight apparatus of the present invention to configure the measurement system according to the present invention.

In that case, a sample stage (a component for placing the sample at the measurement position) which has been provided in the existing measurement apparatus is removed in advance, and the sample stage which has been provided inside the airtight box for measurement is used.

When an existing X-ray diffraction apparatus is provided with an opening/closing door for shielding X-rays, a cutout corresponding to the cutout <NUM> described above is formed in the opening/closing door, and a part of the housing of the airtight box for measurement is inserted into the inside of the opening/closing door through the cutout.

The sample position adjustment mechanism for positioning the sample loaded on the sample stage to the measurement position may be configured by incorporating the sample stage with an XYZ table capable of performing not only position adjustment in an up-and-down direction (Z direction), but also position adjustment in an axial direction (Y direction) and a front-and-rear or lateral direction (X direction) of the housing.

<FIG> and <FIG> show the configuration in which the branched pipes <NUM> are connected to the glove box <NUM> and the housing <NUM> of the airtight box <NUM> for measurement so that the glove box <NUM> and the housing <NUM> of the airtight box <NUM> for measurement communicate with the vacuum suction device and the inert gas supply source. However, the present invention is not limited to the above configuration, and the pipes may be configured as follows.

For example, pipes may be independently connected to the glove box <NUM> and the housing <NUM> of the airtight box <NUM> for measurement respectively so that each of the glove box <NUM> and the housing <NUM> of the airtight box <NUM> for measurement individually communicates with the vacuum suction device and the inert gas supply source.

The pipes to communicate with the vacuum suction device and the inert gas supply source may be connected to a plurality of places in the glove box <NUM> and the housing <NUM> of the airtight box <NUM> for measurement, if necessary.

Further, the pipes communicating with the vacuum suction device and the inert gas supply source may be connected to not only the glove box <NUM> and the housing <NUM> of the airtight box <NUM> for measurement, but also, for example, the antechamber <NUM> (pass box) attached to the glove box <NUM>.

Claim 1:
An airtight apparatus comprising:
an airtight box (<NUM>) for measurement for placing therein a sample to be measured by an X-ray analysis apparatus (<NUM>) installed outside; and
a glove box (<NUM>) connected to the airtight box (<NUM>) for measurement,
wherein the airtight box (<NUM>) for measurement comprises:
a housing (<NUM>) that is hollow therein and has a connecting unit for connecting the housing (<NUM>) to the glove box (<NUM>);
a sample stage (<NUM>) including a sample loading portion;
a measurement window (<NUM>) that is provided in the housing (<NUM>) to measure a sample loaded on the sample stage (<NUM>) from the outside by the X-ray analysis apparatus (<NUM>), wherein the connecting unit of the housing (<NUM>) is designed for connection to the glove box (<NUM>) which is arranged outside side by side together with the airtight box (<NUM>) for measurement, such that the inside of the housing (<NUM>) communicates with the inside of the glove box (<NUM>), and the inside of each of the housing (<NUM>) and the glove box (<NUM>) is put into an airtight state;
characterised by
an X-ray shielding member (<NUM>) arranged for shielding intrusion of X-rays from the inside of the housing (<NUM>) into the glove box (<NUM>).