JPH03218448A - Humidity controller for x-ray device - Google Patents

Abstract

PURPOSE:To measure X-ray diffraction with relative humidity as a parameter by changing humidity around a sample by a branch type humidity generating means with satisfactory change accuracy and holding an accuracy value constant after the change. CONSTITUTION:Supplied dry air is branched to two ducts 20a and 20b of a branch type humidity generating means 17. The humidity of the air in the duct 20a is made 100% in a saturation tank and on the other hand, the air in the duct 20b is fed into a mixing tank 24 and mixed while maintaining 0% humidity. Corresponding to the rate of the mixture, humidity air is generated. The rate of the mixture is controlled based on flow-meters 21 and 23 provided at the both ducts 20a and 20b and the air with desired humidity is fed from an air transport pipe 24 through an absorption nozzle 15 to the internal part of an internal case 8, namely, around a sample 5. Next, the air is passed through a hole 26 and a space between cases 8 and 9 and discharged from an exhaust nozzle to an external part. In the internal part of the case 8, a humidity sensor 27 is arranged and the humidity is held constant by a controller 18. Thus, the surrounding part of the sample 5 is measured under the fixed and desired humidity.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a humidity control device for adjusting the humidity around a sample attached to an X-ray apparatus.

[Conventional Technology] Among the minerals existing on the earth, there are some whose internal crystal structures change when the humidity around them changes. The mode of change in the crystal structure is as follows:
There are various differences depending on the type of minerals that make up the mineral, so if you measure the state of the crystal structure while changing humidity as a parameter, you can learn about the elements that make up the mineral. It becomes possible to obtain information on

For example, in a clay mineral called smectite, the bottom rIn spacing of the layered M@ structure changes depending on the relative humidity of the surrounding atmosphere. In this case, the clay mineral is a layered silicate, and the change in the basal spacing in E is due to differences in the type of cations that enter between the layers and the crystal chemical properties of the silicate layer itself. Therefore, if we measure the change in the basal spacing of smectite without changing the relative humidity, we can determine the interlayer cations and silicates that make up the smectite. Information about the charge of - can be obtained.

Incidentally, the crystal structure of smectite, such as the basal spacing, can be read from an X-ray diffraction pattern obtained by X-ray diffraction. Therefore, when conducting mineral tests such as those mentioned above. An X&I diffractometer can be used. However, in such an XM diffraction experiment,
The relative humidity around the sample attached to the X-ray diffraction device is
It becomes necessary to make changes 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 hygroscopic property of a sulfuric acid solution, and attempts to control 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 in L, various experimental difficulties were encountered because the sulfuric acid solution is highly hygroscopic. especially. There were considerable errors at relative humidity between 0 and 20% and between 80 and 100%. The present invention has been made in view of the above-mentioned problems in conventional humidity control methods, and provides a humidity control method for an X-ray apparatus that enables accurate X-ray diffraction measurements using relative humidity as a parameter. The purpose is to provide a control device.

[Means for solving the problem] In order to achieve the above object, the humidity control device according to claim J includes a sample case that seals around the sample, and humid air to be sent into the sample case. The humidity generating means is constituted by a branch type humidity generating device. This split-flow humidity generator generates humidity by mixing dry air and humidity-saturated air, and by changing the mixing ratio of both types of air, the amount of humidity generated can be adjusted. This is a device that can do this.

The humidity control device of Jff requirement 2 is one in which the connection state between the sample case and the humidity generating means is limited. The humidity generating means can be directly attached to the case, but in the device of Item 2, the two are connected to each other via a long flexible tube.

The humidity control device of Jt1 requirement 3 has limitations added to the sample case. Essentially, the sample case is not limited to any particular configuration as long as it can seal the sample attached to the X-ray device. In the apparatus of requirement 3, the sample case is particularly constructed of a double 4iI case.

! +'tThe humidity control device of requirement 4 is one in which the sample case is modified. Specifically, the sample case is −
The lower part is divided into two parts, and the upper part can be attached and removed.

A humidity control device according to a fifth aspect of the present invention specifies how to flow humidity-containing air when a case with a two-hole structure as described above is used as a sample case. In this device, the air sent from the humidity generating means first enters the inner case,
Thereafter, it is discharged to the outside via the outer case.

The humidity control device according to claim 6 is a further modification of the device according to claim 2, which uses an air transport pipe. In this device, a heater is provided around the air supply pipe, a humidity detection 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 detection means.

[Function] In the humidity control device according to claim 1, the humidity generating means (17
) The air having the desired humidity (humidity air) generated in the sample case (7) is sent into the sample case (7). As a result, the sample (5) in the sample case is placed under the desired humidity. In this state, measurement is performed using an X-ray device, for example, an X-ray diffraction device.

Since the humidity generating means has a branch type humidity generating structure, the humidity setting can be changed precisely and the set thirst level can be maintained accurately and constant.

In the apparatus of Jff requirement 2, the humidity-containing air generated by the humidity generating means (17) is sent into the sample case (7) through the air transport pipe (25). By providing this air transport pipe, the humidity generating means can be installed at a separate location away from the sample case.

Jl? In the Xf13 device, 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 claim 4, the L portion of the sample case is opened during attachment and detachment of the sample or other maintenance work.

In the apparatus of claim 5, the humidity-laden air is discharged to the outside after flowing evenly inside the double case.

In the apparatus of claim 6, the humidity of the air sent into the sample case is controlled by the heater (19), thereby maintaining the humidity inside the sample case constant.

[Example] FIG. 1 shows an X-ray diffraction device that is an example of an X-ray device equipped with a humidity control device according to the present invention. This 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 above the goniometer 1. A sample 5 is mounted on the sample holder 3, and an X&1-intensity detector 6 is mounted on the right end of the detector holder 4. The sample holder 3 rotates O around the axis ω, and at the same time the detector holder 4 rotates 20 times (twice 0) around the axis ω.

The X-rays emitted from the X-ray generator 2 are diffracted by the sample 5,
The diffracted X-rays are received by the X-ray detector 6 and their intensity is measured. During this measurement, the sample 5 is held in the sample holder 3.
The X-ray detector 86 rotates 20 times together with the detector holder 4. As a result, a well-known X-ray diffraction pattern is obtained in which the vertical axis represents the X-ray intensity and the horizontal axis represents the sample rotation angle (usually 20 degrees).

In this embodiment, when performing the above-described X-ray diffraction, the atmospheric humidity of the sample 5 can be changed as appropriate. The configuration for this purpose will be described below.

In FIG. 1, sample holder 3 and sample 5 are surrounded by sample case 7. In FIG. 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. Both 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. 0 ring 10, inner case 8
The interior of the sample 5, 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 are provided with X-ray entrance windows 11 and 12 and X-ray exit windows 13 and l4. Each of these layers is made of, for example, a polyester film.

As shown in FIG. 2, the inner case 8 has an intake nozzle 15.
is attached, and the exhaust nozzle 1 is attached to the outer case 9.
6 is installed.

FIG. 4 shows an example of a device for generating relative humidity and controlling the humidity value.

This device includes a humidity generating means 17, a control device i18, and a heater [9].

The humidity generating means 17 has a so-called branch type humidity generating structure. That is, the supplied dry air (humidity O%
) is divided into two conduits 20a and 20b. A flow meter 21 and a saturation tank 22 are arranged in one pipe 20a, and only a flow meter 23 is arranged in the other pipe 20b. The saturation tank 22 functions to bring the sent air into a humidity saturated state (Il degree 100%) and send it out to the next process.

The humidity saturated air sent by the pipe 20a and the pipe 20
The dry air sent by b is sent together to the air mixing section 24, where they are mixed with each other. This generates air with a humidity that corresponds to the mixing ratio. The amount of humidity generated, that is, the mixing ratio of dry air (0%) and humidity saturated air (100%) is determined by each pipe 20a.
, 2Ob can be set to a desired value by adjusting the amount of air flowing through the flowmeters 21.23.

The air that has reached the desired humidity via the air mixing section 24 (humidity-containing air) is sent to the intake nozzle 15 through an air transport pipe 25 that connects the humidity generating means 17 and the intake nozzle 15 of the sample case 7. Supplied.

The air that has reached the intake nozzle 15 is sent into the inner case 8, that is, around the sample 5, as shown in FIG. The air sent into the inner case 8 is then sent out to the space between the outer case 9 and the inner case 8 through the hole 26 provided in the upper part of the inner case 8, and then through the exhaust nozzle 16. is discharged to the outside through the

In this way, the area around the sample 5 can be kept under desired humidity during the X-ray diffraction measurement.

During the measurement, the inside of the inner case 8 needs to be kept at a constant humidity. Therefore, in this embodiment, a humidity sensor 27 is arranged inside the inner case 8. This 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. 4.

The controller 18 controls the air transport pipe 2 based on the humidity signal.
The heater 19 placed near the heater 5 is controlled on/off or the amount of power supplied to the heater is adjusted. By adjusting the humidity of the air supplied to the sample case 7 in this way, the humidity inside the inner case 8 is kept constant.

In this embodiment, in addition to the humidity control of maintaining the humidity at a constant level 1α as described above, the relative humidity value itself within the inner case 8 is controlled to 0%, 20%, etc. ...The settings can be changed step by step, such as 80%. When changing the humidity as described above, in FIG. 4, the measurer inputs the desired relative humidity 11' to the control device 18 via the operating section 28 such as a keyboard. Control device 18
controls the flowmeter 21 or 23 accordingly to adjust the amount of air flowing therethrough. As a result, the mixing ratio of dry air and humidity-saturated air in the air mixing section 24 changes, and the level of generated humidity can be changed to a desired value.

As described in I- below, according to this example, the relative humidity around the sample 5 is changed to a desired value, and the X-ray diffraction measurement is performed while the changed relative humidity is held constant. I can do it. As a result, as shown in Fig. 5, sample 5
The relative humidity around O%, 20%,...80
The X&1 diffraction pattern can be expressed as %. In these diffraction patterns, curve a is an enlarged version of curve b.

Now, consider the case where a clay mineral called smectite is used as sample 5. In this case, based on the X-ray diffraction patterns at each relative humidity shown in FIG. 5, the basal spacing of the clay mineral when the clay mineral is at a relative humidity close to each relative humidity can be calculated.

Since this calculation method itself is already a well-known technique, detailed explanation will be omitted. In this way, when the basal spacing of a clay mineral under different relative humidities is determined, it becomes possible to infer various information regarding the elements constituting the clay mineral based on it. For example, it is possible to determine what kind of interlayer ions make up a clay mineral, and how the formation of a water molecule layer differs depending on the difference in the interlayer ions.

In addition, in FIG. 2, the upper parts 8a and 9a of the inner case 8 and the outer case 9 can be attached and removed using screws, respectively. This is to facilitate mounting and maintenance of the sample 5.

Although the present invention has been described above with reference to one embodiment, the present invention is not limited to that embodiment.

For example, in the above embodiment, a double structure case consisting of an inner case 8 and an outer case 9 was used as the sample case 7, but if the sample case 5 is of a flt structure that can be sealed tightly, a single layer like an insect can be used. case or any other structured case can be used. However, if a case with a double structure is used, the heat retention inside the sample chamber, that is, inside the inner case 8 can be improved.

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

[Effects of the Invention] According to the present invention, the atmosphere of the sample is improved by using a separate flow type humidity generation means. Since the temperature is changed, it is possible to change the humidity value with high precision, and it is also possible to accurately maintain the humidity value after the change at a constant value. As a result, it has become possible to perform extremely accurate X-ray diffraction measurements using relative humidity as a parameter.

According to the invention of claim 2 of J17, the shape, structure, etc. 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, so that the inside of the inner case,
In other words, the ability to maintain constant humidity around the sample, so-called heat retention, was improved.

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

According to the invention of claim 5, when a double-structured sample case is used, the heat retention inside the inner case, that is, the heat retention inside the sample chamber, can be further improved by -WII.

According to the invention of item 6, the humidity inside the sample case can be kept extremely accurately at a constant value {+il.

[Brief explanation of drawings]

FIG. 1 is a side view showing an example of an X-ray diffraction apparatus using the humidity control device according to the present invention, FIG. 4 is a schematic diagram showing an example of a means for humidity control used in the device shown in FIG. 1, and FIG. 5 is a plan view taken along the line ■-■ 2 is a graph showing an X-ray diffraction pattern showing the results of measurements performed using this method. 5... Sample 7... Sample case 8... Inner case 9... Outer case 17... Humidity generating means 25... Air transport pipes 8a, 9a... Case upper part 19... Heater 27... Humidity sensor 18... Control device 1 Fig. 1 Fig. 2 xa x*i Fig. 5 2 10 20 30 40 2θ (@)

Claims (1)

[Scope of Claims] (1) A humidity control device for adjusting the humidity around a sample attached to an X-ray apparatus, which comprises a sample case that seals around the sample, and a device for feeding the sample into the sample case. and a humidity generating means that generates humidity-containing air, and the humidity generating means is of a split flow type that adjusts the level of humidity of the humidity-containing air by mixing dry air and humidity-saturated air. A humidity control device characterized by being a humidity generation device. (2) The humidity control device according to claim 1, wherein the sample case and the humidity generating means are communicated with each other 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. Control device. (4) The humidity control device according to claim 1 or 3,
A humidity control device characterized in that the upper part of the sample case is removable. (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 passes through the space between the outer case and the inner case. A humidity control device characterized in that humidity is discharged to the outside. (6) The humidity control device according to claim 2, wherein the humidity is detected by a heater provided around the air transport pipe, a humidity detection means disposed within the sample case, and a humidity detected by the humidity detection means. A humidity control device comprising: a control means for controlling the amount of heat generated by the heater based on humidity.