JP2859910B2 - Humidity control device for X-ray equipment - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a humidity control device for adjusting the humidity around a sample mounted on an X-ray apparatus.

[Related Art] Among minerals existing on the earth, there are some minerals which change due to a change in humidity around the minerals. The manner of such a change in the crystal structure varies depending on the type of elements constituting the mineral and the like.Therefore, if the state of the crystal structure is measured while changing the humidity as a parameter, It is possible to obtain information on elements constituting the mineral.

For example, in clay minerals called smectite, the distance between the bottom surfaces of the layered structure changes with the relative humidity of the atmosphere. In this case, the clay mineral is a layered silicate, and the above-mentioned change in the spacing between the bottom surfaces is caused by a difference in the kind of a cation interposed between layers and a difference in crystal chemical properties of the silicate layer itself. Therefore, by measuring the change in the distance between the bottom surfaces of the smectite while changing the relative humidity, it is possible to obtain information on the interlayer cations constituting the smectite and the charge of the silicate layer.

By the way, the crystal structure such as the interval between the bottom surfaces of smectite can be read from an X-ray diffraction pattern obtained by X-ray diffraction. Therefore, an X-ray diffractometer can be used when performing the above mineral test. However, in such an X-ray diffraction experiment, it becomes necessary to change the relative humidity around the sample mounted on the X-ray diffraction apparatus according to preset conditions. In this case, some means of creating relative humidity is required.

Conventionally, a simple method using a sulfuric acid solution has been known as a means for creating relative humidity. This method utilizes the hygroscopicity of the sulfuric acid solution, and attempts to adjust the humidity by appropriately changing the concentration of the sulfuric acid solution.

[Problems to be Solved by the Invention] In the humidity control method using a sulfuric acid solution as described above, various difficulties have been involved in experiments due to the strong hygroscopicity of the sulfuric acid solution. In particular, there was considerable error at relative humidities of 0-20% and 80-100%.

The present invention has been made in view of the above problems in the conventional humidity control method, and has been made in consideration of a humidity for an X-ray apparatus that enables accurate X-ray diffraction measurement with relative humidity as a parameter. It is an object to provide a control device.

Means for Solving the Problems In order to achieve the above object, a humidity control device according to claim 1 includes a sample case that seals around a sample, and air having humidity for sending the sample case into the sample case. And a humidity generating means for generating the humidity. The humidity generating means is constituted by a split-flow type humidity generating device. This split-flow type humidity generator generates humidity by mixing dry air and humidity-saturated air with each other, and adjusts the magnitude of the generated humidity by changing the mixing ratio of the two airs. It is a device that can be used.

According to a second aspect of the present invention, there is provided a humidity control device in which a connection state between the sample case and the humidity generating means is limited. The humidity generating means can be directly attached to the sample case, but in the device of the second aspect, the two are connected to each other via a long flexible tube.

The humidity control device according to claim 3 is one in which the sample case is limited. The configuration of the sample case is not limited to a special one as long as the sample case can essentially seal the sample mounted on the X-ray apparatus. In particular, it is constituted by a case having a double structure.

The humidity control device according to claim 4 is a device in which the sample case is modified. More specifically, the sample case is divided into upper and lower parts, and the upper part thereof can be attached and detached.

According to a fifth aspect of the present invention, there is provided a humidity control device which specifies a flow of the humidity holding air when the above-described double-structure case is used as a sample case. In this device, the air sent from the humidity generating means first enters the inner case,
Then, it is discharged to the outside via the outer case.

The humidity control device according to claim 6 is obtained by further modifying the device according to claim 2 using an air transport pipe. In this device, a heater is provided around the air supply pipe,
Humidity detecting means is provided in the sample case, and the amount of heat generated by the heater is controlled based on the humidity detected by the humidity detecting means.

[Operation] In the humidity control device according to claim 1, the humidity generation means (1
The air having the desired humidity (humidity holding air) generated in 7) is sent into the sample case (7). As a result, the sample (5) in the sample case is placed under a desired humidity. In this state, measurement is performed by an X-ray device, for example, an X-ray diffraction device.

Since the humidity generating means has a split-flow type humidity generating structure, it is possible to change the humidity setting precisely and to keep the set humidity accurately and constant.

In the apparatus according to the second aspect, the humidity holding air generated by the humidity generating means (17) is sent to the sample case (7) through the air transport pipe (25). By providing this air transport pipe, the humidity generating means can be installed at another place away from the sample case.

Device according to claim 3, wherein the sample (5) is placed in a sample chamber surrounded by an inner case (8). Since this sample chamber is further surrounded by the outer case (9), the heat retention of the sample chamber is improved.

In the apparatus according to the fourth aspect, the upper part of the sample case is opened during attachment and detachment of the sample or other maintenance work.

In the apparatus according to claim 5, the humidity holding air is discharged to the outside after flowing evenly inside the double case.

7. The apparatus according to claim 6, wherein the temperature of the air fed into the sample case is adjusted by the heater (19), whereby the humidity inside the sample case is kept constant.

[Embodiment] FIG. 1 is a view showing an X having a humidity controller according to the present invention.
1 shows an X-ray diffraction apparatus which is an example of a X-ray apparatus. This X
The X-ray diffraction apparatus has a goniometer 1 and an X-ray generator 2 provided on the left side thereof. A sample holder 3 and a detector holder 4 are provided on the goniometer 1. A sample 5 is mounted on the sample holder 3, and an X-ray intensity detector 6 is mounted on a right end of the detector holder 4. The sample holder 3 moves around the axis ω by θ.
And at the same time, the detector holder 4 also rotates about the axis ω by 2θ (twice θ).

The X-rays emitted from the X-ray generator 2 are diffracted by the sample 5, and the diffracted X-rays are received by the X-ray detector 6 and the intensity is measured. During this measurement, the sample 5 rotates θ with the sample holder 3 and the X-ray detector 6 rotates 2θ with the detector holder 4. As a result, a well-known X-ray diffraction pattern with the X-ray intensity on the vertical axis and the sample rotation angle (usually 2θ) on the horizontal axis is obtained.

In the present embodiment, in performing the X-ray diffraction as described above, the atmospheric humidity of the sample 5 can be appropriately changed. Hereinafter, the configuration for that will be described.

In FIG. 1, the sample holder 3 and the sample 5 are surrounded by a sample case 7. As shown in FIG. 2, the sample case 7 has an inner case 8 surrounding the sample 5 and an outer case 9 surrounding the inner case 8. The two cases 8 and 9 are integrated at the bottom of the case, and the bottom of the case is fitted into the sample holder 3 via an O-ring 10. O-ring 10 allows inner case 8
, That is, the sample chamber around the sample 5 is sealed.

As shown in FIG. 3, the inner case 8 and the outer case 9 have X-ray entrance windows 11 and 12 and an X-ray exit window 13 respectively.
And 14 are provided. Each of these windows is formed of, for example, a polyester film.

As shown in FIG.
The outer case 9 has an exhaust nozzle 16
Is attached.

FIG. 4 shows an example of an apparatus for generating a relative humidity and controlling the humidity value. This device is
It has a humidity generating means 17, a control device 18, and a heater 19.

The humidity generating means 17 has a so-called split flow type humidity generating structure. That is, the supplied dry air (humidity 0
%) Is diverted to two conduits 20a and 20b. A flow meter 21 and a saturation tank 22 are arranged in one pipeline 20a, and only a flow meter 23 is arranged in the other pipeline 20b. The saturation tank 22 functions to make the sent air in a humidity saturated state (100% humidity) and send it to the next process.

The humidity-saturated air sent by the line 20a and the dry air sent by the line 20b are both sent to the air mixing section 24, where they are mixed with each other. As a result, air having a humidity corresponding to the mixing ratio is generated. The magnitude of the generated humidity, that is, the mixing ratio of the dry air (0%) and the humidity-saturated air (100%) is adjusted by the flow meters 21 and 23 by controlling the amount of air flowing in each of the pipes 20a and 20b. Thus, the desired value can be set.

The air having the desired humidity (humidity holding air) via the air mixing section 24 is sent to the suction nozzle 15 by an air transport pipe 25 connecting the humidity generating means 17 and the suction nozzle 15 of the sample case 7. Supplied.

The air that has reached the suction nozzle 15 is sent into the inside of the inner case 8, that is, around the sample 5, in FIG. The air sent into the inner case 8 then passes through a hole 26 provided in the upper part of the inner case 8,
The air is sent out to the space between the outer case 9 and the inner case 8, and further discharged to the outside via the exhaust nozzle 16. Thus, the sample 5 can be placed under a desired humidity during the X-ray diffraction measurement.

During the measurement, the inside of the inner case 8 needs to be always kept at a constant humidity. Therefore, in the present embodiment, the humidity sensor 27 is disposed inside the inner case 8. The humidity sensor 27 detects the humidity inside the inner case 8 and sends the detection result as a humidity signal to the control device 18 in FIG. The control device 18 controls ON / OFF of the heater 19 disposed near the air transport pipe 25 or controls the amount of power supplied to the heater based on the humidity signal. By adjusting the temperature of the air supplied to the sample case 7 in this way, the humidity in the inner case 8 is kept constant.

In the present embodiment, in addition to the humidity control of maintaining the humidity at a constant value as described above, the relative humidity value in the inner case 8 itself is gradually changed to 0%, 20%,. Settings can be changed. To make such a humidity change, in FIG. 4, the measurer instructs the controller 18 via the operation unit 28 such as a keyboard to a desired relative humidity value. The controller 18 controls the flow meter 21 or the flow meter 23 accordingly to adjust the amount of air flowing therethrough.
Accordingly, the mixing ratio of the dry air and the humidity-saturated air in the air mixing unit 24 changes, and the magnitude of the generated humidity can be changed to a desired value.

As described above, according to this embodiment, the relative humidity around the sample 5 can be changed to a desired value, and the X-ray diffraction measurement can be performed with the changed relative humidity kept constant. . As a result, as shown in FIG.
X-ray diffraction patterns can be obtained when the relative humidity around is changed to 0%, 20%,..., 80%. In these diffraction patterns, the curve a is an enlarged view of the curve b.

Now, consider the case where a clay mineral called smectite is applied as sample 5. In this case, based on the X-ray diffraction pattern at each relative humidity shown in FIG. 5, the bottom interval of the clay mineral when the clay mineral is placed at each relative humidity can be calculated. Since the calculation method itself is a well-known technique, a detailed description thereof will be omitted. As described above, when the bottom surface interval of the clay mineral under different relative humidity is obtained, it is possible to infer various information on the elements constituting the clay mineral based on the obtained distance. For example, it is possible to determine what interlayer ions are included in the clay mineral, how the water molecule layer is formed depending on the difference between the interlayer ions, and the like.

In FIG. 2, upper portions 8a and 9a of the inner case 8 and the outer case 9 can be attached and detached by screws, respectively. This is for facilitating mounting and maintenance of the sample 5.

The present invention has been described with reference to one embodiment, but the present invention is not limited to the embodiment.

For example, in the above-described embodiment, a double case composed of the inner case 8 and the outer case 9 is used as the sample case 7, but if the structure around the sample 5 can be sealed, a simple single case is used. Alternatively, a case having any other structure can be used. However, if a case having a double structure is used, the heat retention in the sample chamber, that is, the inside of the inner case 8 can be enhanced.

In this embodiment, the humidity generating means 17 and the sample case 7 are connected to each other via the air transport pipe 25. However, it is also possible to directly connect both without using the air transport pipe 25. .

[Effects of the Invention] According to the present invention, the atmosphere humidity of the sample is changed by using the split-flow type humidity generating means, so that the humidity value can be changed with high accuracy, and the humidity after the change is changed. It has become possible to keep the value exactly constant. As a result, X-ray diffraction measurement using relative humidity as a parameter can be performed very accurately.

According to the second aspect of the invention, the shape and structure of the humidity generating means can be freely set regardless of the X-ray apparatus.

According to the invention of claim 3, a space is formed between the outer case and the inner case, and thereby, the ability to maintain a constant temperature inside the inner case, that is, around the sample,
The so-called heat retention could be improved.

According to the invention of claim 4, attachment and detachment of the sample in the sample case or other maintenance work can be easily performed.

According to the fifth aspect of the present invention, it is possible to further improve the heat retaining property in the inner case, that is, the heat retaining property in the sample chamber when the sample case having the double structure is used.

According to the invention of claim 6, the humidity in the sample case can be maintained very accurately at a constant value.

[Brief description of the drawings]

FIG. 1 is a side view showing an example of an X-ray diffractometer using a humidity control device according to the present invention, FIG. 2 is a sectional view taken along the line II-II of FIG. 1, and FIG. FIG. 4 is a schematic sectional view showing an example of a means for controlling humidity used in the apparatus shown in FIG. 1, and FIG. 5 is a sectional view taken using the apparatus shown in FIG. 7 is a graph showing an X-ray diffraction pattern showing the result of the measurement. 5 ... Sample 7 ... Sample case 8 ... Inner case 9 ... Outer case 17 ... Humidity generating means 25 ... Air transport tube 8a, 9a ... Top case 19 ... Heater 27 ... Humidity sensor 18 ... Control device

Claims (6)

(57) [Claims] 1. A humidity control device for adjusting the humidity around a sample mounted on an X-ray apparatus, comprising: a sample case for hermetically sealing around the sample; and a humidity holding air for sending the sample case into the sample case. Humidity generating means for generating the humidity, the humidity generating means is a split-flow type humidity generating apparatus that adjusts the humidity of the humidity holding air by mixing the dry air and the humidity saturated air. A humidity control device, comprising: 2. A humidity control apparatus according to claim 1, wherein said sample case and said humidity generating means are communicated by a flexible air transport pipe. . 3. The humidity control device according to claim 1, wherein the sample case is a double case having an inner case that seals the sample and an outer case that seals the inner case. Humidity controller. 4. The humidity control device according to claim 1, wherein an upper portion of the sample case is detachable. 5. The humidity control device according to claim 3, wherein the humidity-containing air sent from the humidity generating means first enters the inner case, and then divides the space between the outer case and the inner case. Humidity control device characterized by being discharged to the outside via 6. The humidity control device according to claim 2, wherein the heater is provided around the air transport pipe, humidity detection means disposed in the sample case, and the humidity is detected by the humidity detection means. Control means for controlling the amount of heat generated by the heater based on the humidity.