JP3407970B2 - Temperature and humidity controller for X-ray equipment - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a temperature / humidity control device for adjusting the temperature and humidity around a sample mounted on an X-ray device.

[0002]

2. Description of the Related Art In the industrial field, there are various devices utilizing X-rays. For example, as one of them, an X-ray diffractometer used for analyzing the crystal structure of a sample is widely known. In the measurement by such an X-ray apparatus, the humidity around the sample may be set to a desired value or the humidity may be changed according to a desired condition. In order to meet such a need, the applicant of the present invention has filed Japanese Patent Application Laid-Open No. 3-2184
In Japanese Patent Publication No. 48, a humidity controller using a so-called shunt type humidity generator was proposed.

In this humidity control device, the humidity-holding air generated by the shunt type humidity generator equipped with a flow meter is introduced into the sample chamber equipped with the humidity sensor through the air transportation pipe equipped with the heater. The flow meter is controlled based on the input of the operation unit, and the humidity is adjusted (that is, set) by this control, and the heater is controlled by the input of the humidity sensor to stabilize the humidity.

[0004]

However, in the above-mentioned conventional apparatus, the humidity in the sample chamber fluctuates subtly according to the temperature in the humidity generator and / or the temperature in the sample chamber. It was not possible to stably and accurately maintain a constant value. Especially, the tendency was remarkable in the high humidity region and the low humidity region. Furthermore, since the humidity was stabilized by controlling the temperature of the air transport pipe with a heater, the sample chamber temperature fluctuates depending on the heater temperature, and again, the humidity in the sample chamber is stably maintained with high accuracy. I couldn't.

The present invention has been made to solve the above problems, and in a temperature and humidity control device using a shunt type humidity generator, the humidity in the sample chamber is stably set to a desired value with high accuracy. The purpose is to be able to maintain.

[0006]

A temperature / humidity control apparatus for an X-ray apparatus according to the present invention is a temperature / humidity control apparatus for adjusting the temperature and humidity around a sample mounted on an X-ray apparatus. A sample chamber for hermetically containing the sample, and a humidity generating means for generating a humidity-holding gas for sending into the sample chamber,
A temperature / humidity control device for an X-ray device having a humidity generating means and a gas transport pipe that hermetically connects a sample chamber. The humidity generating means is composed of a shunt type humidity generating device that adjusts the humidity of the humidity-holding gas by mixing the dry gas and the humidity saturated gas with a mixer.
Then, the temperature inside the humidity generating means and the temperature inside the sample chamber are controlled so as to maintain the same temperature.

[0007]

Since the temperature inside the humidity generating means and the temperature inside the sample chamber are kept equal to each other, the humidity generated by the humidity generating means can be accurately reproduced in the sample chamber without change. Moreover, since the temperature in the sample chamber is controlled to be maintained at a constant temperature, a change in humidity due to a change in temperature is prevented, so that the humidity can be stably and highly accurately maintained.

[0008]

EXAMPLE FIG. 5 shows a horizontal X-ray diffractometer which is an example of an X-ray apparatus using the temperature and humidity controller according to the present invention. This X-ray diffractometer has an X-ray tube 2 installed on a table 1 and a wide-angle goniometer 3. The wide-angle goniometer 3 measures the sample axis ω passing through the X-ray diffraction surface of the sample 4.
And a θ-rotation table 5 that rotates at a predetermined angular velocity, that is, θ-rotation, and a rotation of θ around the sample axis ω.
Rotate in the same direction at double angular velocity, so-called 2θ rotation 2
The rotation table 6 is provided. Rotate the θ turntable 5 by θ,
A rotary drive system for rotating the 2θ rotary table 6 by 2θ is housed inside the gonio base 10.

The sample 4 is removably mounted on the θ rotary table 5, and the circumference of the sample 4 is hermetically surrounded by a sample chamber 7 having an X-ray transmission window 11. A detector arm 8 is fixed to the right end of the 2θ rotary table 6 and extends rightward in the drawing, and a light-receiving slit 9 and an X-ray counter 10 are fixed on the detector arm 8. A divergence slit 13 supported by a stand 12 fixedly installed on the gonio base 10 is arranged between the sample chamber 7 and the X-ray tube 2.

In this X-ray diffractometer, the X-rays emitted from the X-ray focus F in the X-ray tube 2 are extracted as a line-focus X-ray beam, and the divergence slit 1 is used.
The divergence angle in the horizontal direction (that is, in the vertical direction to the paper surface) is limited by 3, and further enters the sample chamber 7 through the window 11 and further enters the sample 4. When the Bragg angle is satisfied between the incident X-ray beam and the crystal lattice plane of the sample 4, X-ray diffraction occurs in the sample 4, and the diffracted X-ray is reflected by the window 1
After passing through 1, the light is taken out of the sample chamber 7, concentrated on the light receiving slit 9 and passed therethrough, and counted by the X-ray counter 10, and the X-ray intensity is calculated from the count result. Here, the θ rotation table 5 and thus the sample 4 are further rotated by θ, and at the same time, the detector arm 8 and thus the light receiving slit 9 and the X-ray counter 10 are rotated by 2θ. As a result, a well-known X-ray diffraction pattern representing the state of changes in the diffracted X-ray intensity with respect to the diffraction angle 2θ is obtained.

In the present embodiment, a temperature / humidity control device 14 is attached to the sample chamber 7, and the operation of the control device 14 causes the inside of the sample chamber 7, that is, around the sample 4 to change accurately according to a constant humidity or a specific condition. Set to humidity. Hereinafter, the humidity control will be described in detail.

As shown in FIG. 4, the sample chamber 7 has a sample case 15 formed of a metal having a high thermal conductivity, such as copper (Cu) or silver (Au), and a uniform inner surface of the sample case 15. It has a heater wire 16 that is distributed in the interior of the sample case 15 and a water pipe 17 as a refrigerant transport path that is evenly distributed in the outer surface of the sample case 15. A gas inlet port 18 and a gas outlet port 19 are provided on the ceiling surface of the sample case 15, and the inner and outer two-layer X-ray transmission windows 11a made of aluminum foil or the like are formed in a portion of the sample case 15 surrounding the sample 4. 11b
Is provided. Also, these X-ray transmission windows 11a
Between 11 and 11b, as shown in FIG. 7, a heater wire 47 is arranged so as to distribute the window frame. Also, θ
A temperature / humidity sensor 20 is provided on the upper end of the turntable 5 near the sample 4.
Is arranged, and the temperature sensor 21 is arranged in contact with or close to the inner surface of the sample case 15.

FIG. 1 shows the construction of an embodiment of the temperature / humidity control device 14 in detail. The temperature / humidity control device 14 includes a humidity generator 22 and a gas transport pipe 23 that hermetically connects the humidity generator 22 and the sample chamber 7. The humidity generator 22 has two gas pipes branched from the dry gas supply pipe 24 and connected again by the mixer 27, that is, a dry gas pipe 25 and a humidity gas pipe 26. A mass flow controller 28 is arranged in the middle of the dry gas pipe 25, and a mass flow controller 29 is provided in the humidity gas pipe 26.
Boiler 30, saturated steam generator 31, and three-way valve 32
Each element of is arranged.

The mixer 27 is, for example, as shown in FIG. 2, a dry gas pipe 25, a humidity gas pipe 26 and a gas transport pipe 2.
3 are connected to each other, and a metal cotton 33 formed of a corrosion resistant metal, for example, a noble metal, stainless steel, or the like is arranged at the connection point. Mass flow controller 28,
Reference numeral 29 denotes, for example, a dry gas pipe 25 and a humidity gas pipe 2 by incorporating an electromagnetic valve and adjusting an opening / closing amount of the electromagnetic valve by a humidity controller 34.
Adjust the flow rate of gas flowing through 6.

The boiler 30 provided in the humidity gas pipe 26 is
Humidity gas pipe 2 according to instructions from the temperature controller 35
The gas flowing through 6 is heated. The saturated steam generator 31 puts the sent gas in a humidity saturated state (humidity 100%) and sends it out to the downstream side. The three-way valve 32 exhausts the output port of the saturated steam generator 31 to the outside in the following two connection modes, that is, a mixed mode in which the saturated steam generator 31 and the mixer 27 are connected to each other, in accordance with an instruction from the host computer 36. Switch to exhaust mode.

In the sample chamber 7, as described, the heater wire 16
Is provided. The heater wire 16 is a temperature controller 3 whose operation is controlled by a host computer 36.
Heat is generated according to the instructions from 7. In addition, a heater wire 39 that generates heat according to an instruction from the temperature controller 38 is provided around the gas transport pipe 23, and a temperature controller 40 whose operation is controlled by the host computer 36.
A heater wire 41 that generates heat according to the instruction from is provided around the humidity generator 22.

The temperature signal S1 and the humidity signal S2 collected by the temperature / humidity sensor 20 arranged near the sample 4 in the sample chamber 7 are processed by the temperature / humidity meter 42,
The temperature signal S1 is sent to the temperature controller 37, and the humidity signal S2 is sent to the humidity controller 34. In addition, if necessary, the temperature and humidity around the sample 4 can be recorded by the recorder 43.
To display. The temperature controller 37 includes a sample case 1
The temperature signal S3 from the temperature sensor 21 arranged near the inner surface of 5 is also sent. The temperature controller 37 uses the two temperature signals S1 and S3 sent in, for example, as shown in FIG.
Well-known PI based on well-known cascade method as shown in FIG.
D control is performed to accurately maintain the temperature inside the sample chamber 7 at a preset temperature.

In FIG. 1, the water pipe 17 is provided in the sample case 15 in the sample chamber 7 as described above, but a water pipe 44 is also provided around the humidity generator 22. Then, the cooling water sent from the cooler 45 is circulated through these water pipes 17 and 44. While this temperature and humidity control device is operating, this cooling water
A fixed amount is always flowed.

The operation of the temperature / humidity control device having the above structure will be described below.

A reference signal Sr corresponding to the target humidity is sent from the host computer 36 to the humidity controller 34, the humidity signal S2 sent from the temperature / humidity meter 42 is compared with the reference signal Sr, and the humidity signal S2 is sent as a reference signal. Sr
The flow rate control by the mass flow controllers 28 and 29 is performed so as to coincide with. At this time, the flow rate control performed by the humidity controller 34 is performed by the forward / backward proportional control in which the total amount is constant as shown in FIG. 3, for example. That is, as shown in the figure, when either the dry gas or the humidity saturated gas is increased, the other is decreased and the total amount thereof is controlled to be always a constant amount. By thus controlling the total amount of the dry gas, for example, the dry air, to be constant, the amount of the gas fed into the sample chamber 7 is always kept constant, so that the pulsation of the gas in the sample chamber 7 is prevented, The atmosphere around the sample 4 is set in a stable state.

During normal temperature and humidity control, the humidity gas pipe 26
The three-way valve 32 provided in the saturated steam generator 31 and the mixer 2
It is set to a mixed mode in which 7 and 7 are connected to each other. The flow rate-controlled dry gas flowing through the dry gas pipe 25 and the flow-rate-controlled humidity saturated gas flowing through the humidity gas pipe 26 are mixed by a mixer 27, thereby generating a gas having a desired humidity. At this time, as shown in FIG. 2, since the metal cotton 33 is arranged in the mixer 27, the mixing of the dry gas and the humidity saturated gas is efficiently promoted, and a mixed gas having a uniform humidity is obtained.

The obtained mixed gas, that is, the humidity-holding gas is fed into the sample chamber 7 through the gas transport pipe 23, and the surroundings of the sample 4 are set to a desired humidity state. In this state, the X-ray diffraction measurement described with reference to FIG. 5 is executed. In general, humidity and temperature are closely related, and if the temperature changes, the humidity changes accordingly. Therefore, even if the humidity of the gas sent into the sample chamber 7 is accurately controlled by the humidity generator 22, it is difficult to keep the humidity constant if the temperature of the sample chamber 7 changes. On the other hand, in this embodiment, the cooling water pipe 17 installed in the sample chamber 7 is used.
Also, due to the function of the heating heater wire 16 whose heat generation is controlled by the temperature controller 37, the inside of the sample chamber 7 is maintained at a desired constant temperature. Therefore, the inside of the sample chamber 7 can be maintained at the target humidity extremely accurately.

The heater 47 provided on the window frame between the inner and outer two layers of the X-ray transmission windows 11a and 11b prevents the X-ray transmission windows 11a and 11b from being condensed.

Furthermore, in addition to the temperature control in the sample chamber 7,
Heater wire 41 and water passage 44 provided in the humidity generator 22
By controlling the temperature inside the humidity generator 22 by the temperature control and simultaneously controlling the temperature of the gas transport pipe 23 by the heater wire 39, the following technical features can be obtained.

First, the humidity generator 22 and the gas transport pipe 23
When the temperatures of the sample chamber 7 are kept equal, the humidity generated by the humidity generator 22 can be exactly reproduced in the sample chamber 7 without changing. When the temperature of the gas transport pipe 23 is kept higher than the temperatures of the humidity generator 22 and the sample chamber 7, dew condensation in the gas transport pipe 23 can be reliably prevented. This phenomenon works particularly advantageously when the inside of the sample chamber 7 is set to high humidity.

When it is desired to set the inside of the sample chamber 7 to an extremely low humidity, the three-way valve 32 is switched to the exhaust mode, that is, the mode in which the output port of the saturated steam generator 31 is exhausted. As a result, the supply of the humidity saturated gas to the mixer 27 is completely cut off, and as a result, low humidity in the sample chamber 7 can be realized.

Although the present invention has been described with reference to one embodiment, the present invention is not limited to the embodiment.
Various modifications can be made within the technical scope described in the claims.

For example, the X-ray diffraction apparatus shown in FIG. 5 is an embodiment of the X-ray apparatus illustrated for the sake of clarity, and the temperature and humidity control apparatus according to the present invention is such an X-ray diffraction apparatus. It can be applied to any X-ray device other than. Further, the means for heating the humidity generator 22, the gas transport tube 23, and the sample chamber 7 is not limited to the heater wires 41, 39, 16 and can be any other heating means.

[0029]

According to the temperature / humidity control device of the first aspect, the temperature inside the sample chamber is kept equal to the temperature inside the humidity generating means, so that the humidity variation due to the temperature variation can be prevented and the sample chamber can be prevented. The humidity of can be stably controlled with high accuracy.

According to the temperature and humidity controller of claim 2,
In particular, when the humidity inside the sample chamber is set to high, it is possible to reliably prevent dew condensation on the gas transport pipe.

According to the temperature and humidity controller of claim 3,
It is possible to reliably prevent pulsation of the gas flow around the sample in the sample chamber.

According to the temperature and humidity controller of claim 4,
By completely shutting off the supply of humidity-saturated gas to the mixer, the sample chamber can be set to extremely low humidity.

According to the temperature and humidity controller of claim 5,
Mixing of the dry gas and the humidity-saturated gas can be promoted, so that a very uniform humidity atmosphere can be set in the sample chamber.

According to the temperature and humidity controller of claim 6,
Uniform temperature control in the sample chamber, and hence humidity control. Further, by cooling the sample case, the temperature of the sample chamber below room temperature can be realized.

According to the temperature and humidity controller of claim 7,
In particular, when the humidity inside the sample chamber is set to high, it is possible to reliably prevent dew condensation from occurring on the X-ray transmission window.

According to the temperature and humidity controller of claim 8,
It is possible to control the temperature in the sample chamber with high accuracy, and thus to control the humidity with high accuracy.

[0037]

[Brief description of drawings]

FIG. 1 is a block diagram of an electric circuit and a piping system showing an embodiment of a temperature / humidity control device for an X-ray device according to the present invention.

FIG. 2 is a side sectional view showing an example of a mixer.

FIG. 3 is a graph showing a preferred example of a method of mixing a dry gas and a humidity saturated gas.

FIG. 4 is a front sectional view showing an example of a sample chamber.

FIG. 5 is a front view showing a horizontal X-ray diffraction device, which is an example of an X-ray device in which the temperature and humidity control device of the present invention is used.

6 is an electrical control block diagram showing an example of a control method used in the temperature controller shown in FIG.

FIG. 7 is a perspective view showing a main part of FIG. 4, particularly an X-ray transmission window.

[Explanation of symbols]

4 samples 7 Sample chamber 14 Temperature and humidity control device 15 sample case 16 heater wire 17 water pipe 18 gas inlet 19 Gas outlet 20 Temperature and humidity sensor 21 Temperature sensor 22 Humidity generator 23 Gas Transport Pipe 24 Dry gas supply pipe 25 Dry gas pipe 26 Humidity gas pipe 28,29 Mass Flow Controller 32 three-way valve 39 heater wire 41 heater wire 44 water pipe

─────────────────────────────────────────────────── ─── Continuation of front page (58) Fields surveyed (Int.Cl. ⁷ , DB name) G01N 23/207 G05D 22/00 B01J 7/02

Claims (8)

(57) [Claims] 1. A temperature-humidity control device for adjusting the temperature and humidity around a sample mounted on an X-ray device, comprising:
X-ray having a sample chamber for hermetically accommodating a sample, a humidity generating means for generating a humidity-holding gas to be sent into the sample chamber, and a gas transport pipe for hermetically connecting the humidity generating means and the sample chamber In the device temperature and humidity control device, the humidity generating means is a shunt type humidity generating device that adjusts the magnitude of humidity of the humidity holding gas by mixing a dry gas and a humidity saturated gas by a mixer, and A temperature / humidity control device for an X-ray device, wherein the temperature inside the humidity generating means and the temperature inside the sample chamber are controlled so as to maintain the same temperature. 2. The temperature / humidity control device for an X-ray apparatus according to claim 1, wherein the temperature of the gas transport pipe is set higher than the temperatures of the humidity generating means and the sample chamber. 3. The temperature / humidity control device for an X-ray apparatus according to claim 1, wherein the flow rate of the dry gas and the flow rate of the humidity-saturated gas are both increased and decreased while maintaining a constant sum. . 4. A three-way valve is provided in the humidity-saturated gas supply path to the mixer, and the humidity-saturated gas is supplied to the mixer and the humidity-saturated gas is exhausted to the outside by switching the three-way valve. The temperature / humidity control device for an X-ray device according to claim 1, wherein 5. The X-ray apparatus according to claim 1, wherein the mixer has a gas flow passage through which a mixed gas flows, and a corrosion-resistant metallic cotton disposed in the gas flow passage. Temperature and humidity controller. 6. The sample chamber has a sample case that surrounds the sample, a heater wire that is uniformly distributed on the inner surface of the sample case, and a refrigerant transfer path that is uniformly distributed on the outer surface of the sample case. The temperature and humidity control device for an X-ray device according to claim 1. 7. The sample chamber has an X-ray transmission window made of two layers, a low X-ray absorption material, inside and outside, and a heater arranged in the X-ray transmission window. X described
Temperature and humidity controller for wire equipment. 8. A temperature and humidity sensor arranged in the vicinity of the sample,
A temperature sensor arranged near the wall surface of the case ,
Input temperature signal from humidity sensor to main controller
The temperature signal from the temperature sensor
Input to the main controller and the sub controller.
The temperature / humidity controller for an X-ray apparatus according to claim 1, wherein the temperature in the sample chamber is controlled in a cascade manner by using rollers .