JP2010203842A - X-ray analysis device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an X-ray analysis device capable of suppressing interruption of X-ray measurement to the utmost, and analyzing an acquired measurement results accurately and quickly, when performing X-ray measurement in a prescribed angle range repeatedly in company with a temperature change. <P>SOLUTION: This X-ray analysis device for detecting by an X-ray detector, an X-ray emitted from a sample when irradiating the sample with the X-ray is described as follows: X-ray diffraction measurement is performed, while changing a sample temperature following a temperature changing curve 39, and a plurality of diffraction line profiles 35 are drawn at intervals along longitudinal axes in a range from 2θ=5° to 2θ=40°; X-ray intensity data 35 (→) during movement in the forward direction wherein an angle is increased in a range from 5° to 40° are displayed on a screen from 5° toward 40° on an angle coordinate axis (abscissa of a coordinate display 36), and X-ray intensity data 35 (←) during movement in the reverse direction wherein the angle is reduced are displayed on the screen from 40° toward 5° on the same angle coordinate axis; and the forward/reverse display can be displayed by being switched by a switch icon 43. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to an X-ray analyzer that detects X-rays emitted from a sample when the sample is irradiated with X-rays using an X-ray detector. In particular, the present invention relates to an X-ray analyzer that displays a detection result as an image on a screen.

  The X-ray analyzer determines the crystal structure, molecular structure, etc. of a sample based on the state of secondary X-rays emitted from the sample when the sample is irradiated with X-rays, such as diffraction rays, scattered rays, and fluorescent X-rays. It is a device to analyze. As such an X-ray analyzer, for example, an X-ray diffractometer that measures the diffraction angle and diffraction line intensity of a diffraction line generated from a sample, an X-ray scattering apparatus that measures the angle and intensity of scattered radiation generated from a sample, A fluorescent X-ray apparatus for measuring fluorescent X-rays generated from a sample is known.

  In the above X-ray analysis apparatus, an apparatus is known that performs measurement while changing the environment for a sample. For example, X-ray measurement is performed while changing the temperature of the sample, X-ray measurement is performed while changing the humidity of the sample, or X-ray measurement is performed while changing the pressure applied to the sample. In addition, X-ray measurement may be performed in a state where these environmental changes are combined.

  Conventionally, Patent Document 1 discloses an X-ray analyzer that performs X-ray measurement while changing temperature. In this apparatus, the X-ray capture angle (generally referred to as 2θ angle or 2θ diffraction angle) with respect to the sample axis of the X-ray detector is changed to the first while changing the ambient temperature of the sample under a predetermined condition. The operation of changing between the angle and the second angle (angle measurement operation) is repeatedly performed to measure which angle and size of the secondary X-ray is emitted from the temperature-changing sample.

  The central axis of the X-ray incident on the sample, that is, the incident X-ray is referred to as the X-ray optical axis on the incident side, and the line at which the center of the X-ray inlet of the X-ray detector looks at the center of the sample is the light-receiving side The 2θ angle is an angle formed by the light receiving side X-ray optical axis with respect to the incident side X-ray optical axis.

  In this apparatus, the angle measurement operation from the first angle to the second angle is always performed in one direction, for example, the direction in which the angle increases from a small angle to a large angle. That is, when the angle measurement operation from the first angle to the second angle is finished, the X-ray detector moves back from the second angle position to the first angle position for the next angle measurement operation. Angle measurement is not performed during this return movement.

  Conventionally, Patent Document 2 discloses an X-ray diffractometer that performs an angle measurement operation from a first angle to a second angle continuously in both directions as well as in one direction. In this apparatus, while changing the temperature of the sample, the angle of the X-ray detector is changed between the first angle and the second angle in the forward direction (direction in which the angle increases) and in the reverse direction (direction in which the angle decreases). The X-ray detector detects the X-rays by continuously rotating and repetitively moving.

Japanese Patent Laid-Open No. 11-295244 (pages 2 to 4, FIG. 1) Japanese Examined Patent Publication No. 36-003348 (pages 1 and 2, FIGS. 2, 3 and 4)

  In the X-ray diffraction apparatus disclosed in Patent Document 1, X-ray measurement could not be performed while the X-ray detector was moved back from the second angle to the first angle. Nevertheless, since the sample temperature changed during this return time, the collection of information on the X-ray measurement results was interrupted with respect to the sample temperature change during this return time. For example, when a change occurs in the crystal structure of the sample during the temperature change during the return time, the change in the structure cannot be captured by X-ray measurement.

  In the X-ray diffractometer disclosed in Patent Document 2, the angle measurement of the X-ray detector is alternately and continuously performed in the forward direction and the reverse direction, and is a result of the X-ray measurement in the forward direction and the reverse direction. A diffraction line pattern was continuously drawn on one sheet. In this drawing method, it is very difficult to grasp the relationship between the diffraction peak in the forward direction and the diffraction peak in the reverse direction, and it is difficult to quickly perform accurate analysis.

  The present invention has been made to solve the above-described problems, and interrupts X-ray measurement when X-ray measurement in a predetermined angle range is repeatedly performed with environmental changes such as temperature changes. An object of the present invention is to provide an X-ray diffractometer that can be suppressed as much as possible and that can accurately and quickly analyze the obtained measurement results.

  An X-ray analyzer according to the present invention is an X-ray analyzer that detects X-rays emitted from a sample placed on a sample axis by an X-ray detector when the sample is irradiated with X-rays. Environment changing means for changing the environment, detector rotating device for rotating the X-ray detector around the sample axis, and intensity calculating means for calculating the X-ray intensity based on the output signal of the X-ray detector And image display means for displaying output data of the intensity calculation means as an image on a screen, and a control means for controlling operations of the detector rotating device, the intensity calculation means, and the image display means, The control means measures the angle of the X-ray detector alternately in the forward direction in which the angle increases between the small first angle and the large second angle and in the reverse direction in which the angle decreases by the detector rotating device. While times The X-ray intensity is calculated in both the forward and reverse directions by the intensity calculation means, and the X-ray intensity data during the forward movement is moved from the first angle on the angle coordinate axis to the second angle. The X-ray intensity data when moving in the reverse direction is displayed on the screen from the second angle on the same angular coordinate axis toward the first angle.

  The environment changing means is, for example, a means for changing temperature, a means for changing humidity, or a means for changing pressure. The detector rotating device can be realized by a goniometer used in a general X-ray diffractometer. The intensity calculation means can be constituted by a combination of a CPU that is a component of a computer and calculation program software, for example. The image display means can be constituted by, for example, a combination of a CPU, image forming program software, and an image display driver. A control means can be comprised by the combination of CPU and program software, for example.

  In the conventional X-ray analyzer in which the measurement only in the forward direction is performed a plurality of times with respect to the 2θ diffraction angle of the X-ray detector, the X-ray detector is moved back to the start angle position between each measurement. When the X-ray detector moved back and moved, the X-ray diffraction measurement had to be interrupted, and X-ray diffraction measurement data during the temperature change could not be obtained. On the other hand, according to the present embodiment, since the forward direction measurement and the reverse direction measurement are alternately and continuously repeated, the return time for returning the X-ray detector to the initial position becomes unnecessary, and the X-ray diffraction The measurement is interrupted only for a short time to reverse the measurement direction from the forward direction to the reverse direction. Therefore, the interruption of the X-ray measurement can be suppressed as much as possible.

  Furthermore, in the X-ray analysis apparatus of the present invention, the forward direction data and the backward direction data are displayed on a common angular coordinate axis, so that the data can be analyzed accurately and quickly.

  By the way, in the X-ray analysis apparatus of the present invention, the X-ray detector is moved in the forward direction and the reverse direction while changing the environment such as temperature and humidity, and X-ray diffraction measurement is performed when moving in both directions. Then, the X-ray intensity data at the time of forward movement and the X-ray intensity data at the time of backward movement are displayed on a common angular coordinate axis. In this case, the intensity data related to the 2θ angle of the X-ray intensity data is displayed with the same characteristics in both the forward and reverse directions, but the environmental values of the X-ray intensity data, for example, the characteristics related to temperature, are opposite to those in the forward movement. It differs from the case of moving the direction.

  For example, in FIG. 11 (a), X-ray intensity data 35a, 35c, 35e during forward movement and X-ray intensity data 35b, 35d during backward movement are displayed on the coordinates with the angle coordinate axis 2θ as the horizontal axis. Has been. In each X-ray intensity data, a peak value occurs at the same 2θ angle. As long as the samples are the same, it is natural that a peak occurs at the same angular position in each X-ray intensity data.

  Here, if all the X-ray intensity data are derived from forward movement, the temperature change tendency for each X-ray intensity data is the same. For example, if the temperature is controlled so as to increase at a constant gradient, the temperature gradients for the X-ray intensity data of the forward movement are all constant, for example, a temperature rising gradient that rises to the right. In this case, the difference in temperature at the time of peak occurrence in each X-ray intensity data should be a constant value.

  However, as in the case of the present invention, when the forward movement and the backward movement are continuously repeated with respect to the X-ray detector, the forward data that can be written from the left end in the coordinates of FIG. 35a, 35c, 35e and the reverse direction data 35b, 35d started to be written from the right end, the temperature rising tendency is reverse, and in the temperature change characteristics in the forward movement and the reverse movement The nature of will be different.

  For example, in the case where the temperature gradient of the sample temperature is controlled to be constant, the peak occurrence temperature (112 in the reverse data) from the peak occurrence temperature (eg, 106 ° C. in FIG. 11A) in the forward direction data. Temperature change (6 ° C.) until the peak occurrence temperature (112 ° C.) in the reverse data and the peak change temperature (126 ° C.) in the next forward data (14 ° C.). It is not constant.

  This phenomenon is not a big problem in general analysis, but it can be a factor to confuse judgment when it is desired to conduct an academic and rigorous analysis. Therefore, in a preferred embodiment of the present invention, it further includes display switching means for switching between forward direction display and reverse direction display, and the control means forwards when the forward direction display is selected by the display switching means. X-ray intensity data during movement is displayed on the screen, X-ray intensity data for reverse movement is not displayed, and if reverse display is selected by the display switching means, X-ray intensity data for reverse movement is displayed. It is displayed on the screen, and X-ray intensity data of forward movement is not displayed.

  According to this embodiment, only the forward display or the reverse display can be viewed by operating the display switching means. When forward display and reverse display are mixed, environmental change characteristics such as temperature change characteristics may differ between the displays, but a plurality of X-ray intensity data displayed only in the forward display. In addition, a plurality of pieces of X-ray intensity data displayed in the case of only reverse display are all based on the same environmental change characteristics. Therefore, when it is desired to carry out academic and rigorous analysis, the object can be achieved by selectively performing only the forward display or the reverse display.

  Still another embodiment of the X-ray analyzer of the present invention comprises a forward direction display instruction means for performing only forward display, a reverse direction display instruction means for performing only reverse display, Bi-directional display instructing means for performing display in both reverse directions. And (1) when the bidirectional display instruction means is selected, the control means displays X-ray intensity data at the time of forward movement and backward movement on the screen, and (2) forward display instruction means. Is selected, X-ray intensity data during forward movement is displayed on the screen, X-ray intensity data for backward movement is not displayed, and (3) reverse display instruction means is selected The X-ray intensity data for the backward movement is displayed on the screen, and the forward-movement X-ray intensity data is not displayed.

  The forward direction display instruction means, the backward direction instruction means, and the bidirectional direction instruction means may be a keyboard, a mouse, or other dedicated input device, or may be an icon display displayed on the display screen. . According to this embodiment, since the forward display, the reverse display, and the bidirectional display can be easily selected and displayed on the screen, quick analysis can be performed.

  In a preferred embodiment of the present invention, the detector rotating device has a servo motor as a power source, and the servo motor has an encoder that detects a rotation speed of its output shaft and outputs a signal. The servo motor is a motor that controls the rotation of the output shaft so that the output of the encoder is constant.

  In addition to the above servo motor, a pulse motor can be considered as a power source that moves various mechanisms and that can control the rotation speed or rotation angle of its output shaft. The pulse motor is a motor that controls the rotational speed or line angle of the rotor integral with the output shaft by controlling the pulse current supplied to the stator. When angle measurement and X-ray diffraction measurement are performed in both directions while rotating the X-ray detector in both the forward and reverse directions as in the present invention, accurate angle determination is performed in the forward and forward directions. Must be done.

  When a pulse motor is used, the rotation angle of the output shaft varies between forward rotation and reverse rotation even when a constant pulse current is supplied to the stator due to backlash of the mechanism built in the pulse motor. It may be different. On the other hand, when the servo motor is used, the angle of the output shaft can be accurately matched between the forward rotation and the reverse rotation. Therefore, in the case of the present invention, it is desirable to use a servo motor as a power source.

  In a preferred embodiment of the present invention, the environment changing means includes a temperature control means for changing the temperature of the space including the sample axis, a humidity control means for changing the humidity of the space including the sample axis, and the sample axis. It is at least one of the pressure control means which changes the pressure of the containing space.

  With this configuration, X-ray measurement based on 2θ rotation in both forward and reverse directions is continuously performed on samples exposed to temperature change, humidity change, and pressure change, so that there are few interruptions in the environmental changes. Data can be obtained.

  In a preferred embodiment of the present invention, the image display means displays an environmental change performed by the environment changing means as an image on the screen, and the control means displays an image of output data of the intensity calculating means and the environmental change. Are displayed in association with each other. The environmental change is, for example, a temperature change, a humidity change, a pressure change, or the like. If these environmental changes are displayed simultaneously with the X-ray intensity data, the X-ray intensity data can be accurately analyzed from various viewpoints.

According to the X-ray analyzer according to the present invention, the forward direction measurement and the reverse direction measurement are alternately and continuously repeated, so that a return time for returning the X-ray detector to the initial position becomes unnecessary, and the X-ray analysis is performed. The diffraction measurement is interrupted only for a short period of time to reverse the measurement direction between the forward direction and the reverse direction. Therefore, the interruption of the X-ray measurement accompanying the environmental change such as a temperature change is suppressed as much as possible. It became possible.
Furthermore, in the X-ray analysis apparatus of the present invention, the forward direction data and the backward direction data are displayed on a common angular coordinate axis, so that the data can be analyzed accurately and quickly.

It is a figure which shows the outline of the structure of one Embodiment of the X-ray analyzer which concerns on this invention. It is a block diagram which shows the control system of the X-ray analyzer of FIG. It is a flowchart which shows the flow of control performed by the control system of FIG. It is a figure which shows the example of data storage in the memory used with the control system of FIG. It is a figure which shows the example of a display of the display used with the control system of FIG. It is a figure which shows the example of a display following the example of a display of FIG. It is a figure which shows the example of a display following the example of a display of FIG. It is a figure which shows the example of a display which performed the bidirectional | two-way display of the forward direction and the reverse direction. It is a figure which shows the example of a display which performed only the forward direction display. It is a figure which shows the example of a display which performed only the reverse direction display. It is a figure which shows typically the switching condition of a forward direction display and a reverse direction display.

(First embodiment)
The X-ray analysis apparatus 1 of this embodiment shown in FIG. 1 is an apparatus that performs both X-ray analysis and thermal analysis at the same time. In the present embodiment, analysis using X-ray diffraction is performed as X-ray analysis, and DSC (Differential Scanning Calorimetry) analysis is performed as thermal analysis. Note that it is not an essential requirement to perform DSC measurement in relation to the present invention. And the temperature change and humidity change which are added to a sample with DSC measurement correspond to the environmental change in this invention.

  The X-ray analyzer 1 has a sample chamber 2 that is separated from the outside by a partition wall. The sample chamber 2 is preferably separated from the outside in an air-tight and liquid-tight manner. The sample chamber 2 is formed by a metallic partition such as stainless steel. Around the sample chamber 2, a θ-θ goniometer (θ-θ angle measuring device) 3 is provided as a detector rotating device.

  An X-ray source 6 is provided on one outside of the sample chamber 2 and an X-ray detector 7 is provided on the outside on the opposite side. The X-ray source 6 is supported by an arm installed in the goniometer 3. The X-ray detector 7 is supported by another arm installed in the goniometer 3. As the X-ray detector 7, for example, a zero-dimensional counter having no position resolution such as SC (Scintillation Counter), a semiconductor sensor in which X-ray light receiving elements are linearly arranged in the 2θ angle scanning direction, and the like are used. .

  The θ-θ goniometer 3 supports the sample 4 to be analyzed in a state where it does not rotate on the sample axis ω, that is, in a fixed state. The surface on which the sample 4 is placed is in a horizontal state. The sample axis ω is a virtual line passing through the X-ray irradiation surface of the sample 4, and is a virtual straight line extending in a direction penetrating the paper surface (usually a horizontal direction) in FIG. A straight line connecting the center of the X-ray source 6 and the center of the sample 4 is the X-ray optical axis on the incident side. A straight line connecting the center of the sample 4 and the center of the X-ray capturing area of the X-ray detector 7 is the X-ray optical axis on the light receiving side.

  The θ-θ goniometer 3 rotates the X-ray source 6 and the X-ray detector 7 from the reference 0 ° position (usually in the horizontal direction) about the sample axis ω in the opposite directions by the same angle θ. By these rotations, the X-ray incident angle θ incident on the sample 4 is measured (that is, the angle is positioned), and the X-ray intake port of the X-ray detector 7 looks at the center of the sample 4. The angle 2θ formed with the extension line of the incident side X-ray optical axis is measured. The angle 2θ is twice the X-ray incident angle θ.

  The rotation of the X-ray detector 7 around the sample axis ω is a rotation with the rotation direction opposite to the rotation of the X-ray source 6 and the same rotation angle. Therefore, when the X-ray source 6 rotates by the angle θ, the X-ray detector rotates by the same angle θ in the reverse direction. In this case, the rotation of the X-ray detector 7 is a rotation for detecting a diffraction line generated from the sample 4 at a diffraction angle 2θ by the X-ray inlet of the X-ray detector 7. The rotation of the line detector 7 is referred to as 2θ rotation.

  In the present embodiment, the secondary X-ray is a diffracted ray, but if the X-ray analysis is an analysis using X-ray scattering, the secondary X-ray is a scattered ray, and the X-ray analysis uses a fluorescent X-ray. The secondary X-rays are fluorescent X-rays.

  The goniometer 3 measures the angle θ and the angle 2θ in accordance with a command from the main control device 12 as a control means. The X-ray detector 7 detects a diffraction line emitted from the sample 4 and outputs an X-ray intensity signal S0 which is an electric signal indicating the intensity of the diffraction line. The X-ray intensity signal S0 itself may be a signal indicating the X-ray intensity, or the CPU described later operates according to a measurement control program described later and calculates the X-ray intensity based on the X-ray intensity signal S0. May be.

  The goniometer 3 includes, for example, a servo motor as a power source, power transmission means for converting the rotational power of the servo motor into θ rotation of the X-ray source 6, and the rotational power of the servo motor to 2θ rotation of the X-ray detector 7. Power transmission means for conversion. As the power transmission means, for example, a mechanism composed of a worm and a worm wheel can be used.

  As is well known, a servo motor is a motor that detects the rotation angle or rotation speed of an output shaft with an encoder or the like and feeds back the detection result to an input current to obtain a desired output. In addition to servo motors, pulse motors are known as motors that can control the rotation angle of the output shaft. This pulse motor is a motor that controls the rotation angle of the output shaft and the like by supplying a pulsed current to the motor.

  Both the servo motor and the pulse motor can rotate the output shaft forward and backward, but the pulse motor has a difference between the output shaft angle during forward rotation and the output shaft angle during reverse rotation due to backlash of the internal mechanism. there is a possibility. On the other hand, the servo motor does not cause an output angle shift during forward / reverse rotation. As will be described later, in the present embodiment, the 2θ rotation related to the X-ray detector 7 is performed in both forward and reverse directions. Therefore, a servo motor capable of accurately determining the angle in both directions is advantageous.

  Among the partition walls constituting the sample chamber 2, the material that can allow the X-ray to travel and maintain the internal airtight state and the liquid-tight state at the portion that intersects the traveling path of the incident X-ray and the secondary X-ray An X-ray transmission window having a structure is provided in advance.

  A standard substance 8 is placed adjacent to the sample 4. The sample 4 is a substance whose characteristics change according to the ambient temperature change (for example, a characteristic change due to dissolution), whereas the standard substance 8 is a substance whose characteristics do not change with respect to the temperature change.

  Inside the sample chamber 2, a temperature sensor 9 and a humidity sensor 11 are provided. The temperature sensor 9 detects the temperatures of the sample 4 and the standard substance 8 and outputs them as a temperature signal S1 that is an electrical signal. The humidity sensor 11 detects the humidity around the sample 4 and the standard material 8 and outputs it as a humidity signal S2 which is an electrical signal. The temperature signal S1 and the humidity signal S2 are transmitted to the main controller 12.

  In the sample chamber 2, a DSC measurement circuit 14, a temperature control device 16, and a humidity control device 17 are attached. The DSC measurement circuit 14 has a calorific value detection element (for example, a thermocouple temperature measuring point) disposed in the vicinity of each of the sample 4 and the standard material 8. The DSC measurement circuit 14 detects the difference in the amount of heat (that is, the heat flow rate) flowing into each of the sample 4 and the standard material 8 using these detection elements. The DSC measurement circuit 14 transmits this heat flow rate to the main controller 12 as a heat quantity signal S3 which is an electrical signal.

  The temperature control device 16 operates according to a command from the main control device 12 and controls the temperature inside the sample chamber 2 (that is, the temperature around the sample 4 and the standard material 8). The temperature control device 16 is configured using, for example, a heater that generates heat when energized, a cooler, or the like. In some cases, no cooler is used. The humidity control device 17 operates in accordance with a command from the main control device 12 to control the humidity inside the sample chamber 2 (that is, the humidity around the sample 4 and the standard material 8). A display 23 as an image display device is connected to the output port of the main controller 12. The display 23 is configured by a liquid crystal display device, for example.

  For example, as shown in FIG. 2, the main controller 12 includes a computer having a CPU (Central Processing Unit) 18, a ROM (Read Only Memory) 19, a RAM (Random Access Memory) 21, and a memory 22. Has been. 2 and 1 are denoted by the same reference numerals. The memory 22 includes a semiconductor memory, a mechanical memory such as a CD (Compact Disk), and other storage media having an arbitrary configuration. The memory is not limited to one type of storage medium, and the memory may be composed of a plurality of types of storage media.

  The memory 22 stores a measurement control program 24 that defines the operation of the X-ray analyzer 1 of FIG. 1 and an image display program 26 that generates an image signal for displaying an image on the screen of the display 23. Yes. In the memory 22, various file areas such as a measurement data storage file 28 and an analysis data storage file 29 are provided.

  The measurement data storage file 28 is a file for storing data obtained by X-ray analysis measurement and thermal analysis measurement and not subjected to secondary processing (hereinafter also referred to as raw data). is there. The analysis data storage file 29 is a file for storing data after the analysis processing is added to the raw data (hereinafter, sometimes referred to as analysis data). The analysis processing includes, for example, diffraction profile peak processing, diffraction profile background processing, and the like.

  The measurement conditions of the X-ray analysis measurement are (1) the measurement start angle and measurement end angle of the diffraction angle 2θ in FIG. 1, (2) the moving speed of the scanning movement of the X-ray detector 7 from the start angle to the end angle, (3) There is a sampling time that is a time for which the X-ray detector 7 accumulates X-rays with respect to one 2θ angle.

  The measurement conditions for the thermal analysis measurement include, for example, setting of a target temperature and setting of a temperature increase rate. As other measurement conditions, for example, there are a target humidity setting and a humidity increase rate setting.

  The X-ray analysis measurement is performed by the following procedure, for example. That is, in FIG. 1, the temperature control device 16 is operated to change the temperature around the sample 4 over time in a desired state. On the other hand, the humidity control device 17 is operated to set the humidity around the sample 4 to a desired humidity. Thereby, the sample 4 is placed under a desired temperature and humidity.

  Next, the sample 4 is irradiated with X-rays generated from the X-ray source 6 through an X-ray optical element such as a slit or a monochromator. The X-ray incident angle θ and the diffraction line capture angle 2θ by the X-ray detector 7 are scanned and moved from the start angle to the end angle at a predetermined scanning movement speed. During the scanning movement of the X-ray detector 7, the intensity I (2θ) of the diffraction line is detected at every predetermined sampling time. The diffraction line intensity I (2θ) is an intensity value for each diffraction angle value from the start angle to the end angle of the diffraction angle 2θ. This diffraction line intensity I (2θ) is output from the X-ray detector 7 as an X-ray intensity signal S0.

  The thermal analysis measurement is performed by the following procedure, for example. In FIG. 1, in a state where the sample 4 and the standard material 8 are placed at a desired temperature and humidity, the difference between the amount of heat flowing into the sample 4 and the amount of heat flowing into the standard material 8 is measured over time by the DSC measurement circuit 14. To detect. That is, the difference in heat inflow amount is detected corresponding to the passage of time. The difference in the heat inflow amount is output from the DSC measurement circuit 14 as a heat amount signal S3.

Hereinafter, the measurement realized by the measurement control program 24 and the image display program 26 of FIG. 2 will be described with reference to the flowchart of FIG.
First, in step S1, the apparatus is initialized. The initialization conditions are stored, for example, in a predetermined area in the memory 22 of FIG. Next, in step S2, conditions are set according to the instructions of the measurer as necessary. If the initial value can be left as it is, the condition is not changed in the condition setting step S2.

In this embodiment, measurement is performed under the following conditions.
(1) The temperature in the sample chamber 2 is changed by the temperature control device 16 under predetermined conditions.
(2) The humidity in the sample chamber 2 is changed by the humidity controller 17 under predetermined conditions.
(3) X-ray detector 7 of X St. included angle 2 [Theta] is changed at a predetermined angular velocity or a predetermined stepping angle between the first angle 2 [Theta] _{1 =} 5 ° of the second angle 2 [Theta] _{2 =} 40 °. The direction in which the angle increases is referred to as the forward direction, the direction in which the angle decreases is referred to as the reverse direction, and the forward scan rotation and the reverse scan rotation between 5 ° and 40 ° (ie, reciprocal scan rotation). A) Repeat continuously.

  After the measurement conditions are set, it is determined in step S3 whether or not there has been an instruction to start measurement by the measurer (YES in step S3), and a measurement start command is generated in step S4.

  Then, in FIG. 1, the temperature of the internal region of the sample chamber 2 is controlled according to a predetermined condition by the action of the temperature controller 16, and the humidity of the internal region of the sample chamber 2 is controlled according to a predetermined condition by the action of the humidity controller 17. Is done. Further, by the action of the goniometer 3, the X-ray incident angle θ to the sample 4 and the diffraction line take-in angle 2θ from the sample 4 by the X-ray detector 7 are controlled according to predetermined conditions. As a result of these controls, diffraction line intensity data S0 = I (2θ) is obtained from the X-ray detector 7, and heat flow data (DSC data) S3 is obtained from the DSC measurement circuit 14.

  These obtained data are stored in the measurement data storage file 28 of FIG. 2 in step S5. As shown in FIG. 4, these I (2θ) data and DSC data are stored in relation to the elapsed time t from the start of measurement. Since the elapsed time t is related to the temperature change T of the sample and the change of the diffraction angle 2θ, the diffraction line intensity data I (2θ) is related to the change of the diffraction angle 2θ and the change of the sample temperature T. The DSC calorific data is associated with a change in the sample temperature T. Further, the measured humidity data H is also stored in relation to the elapsed time t.

  Each data is obtained both when the X-ray detector 7 moves in the forward direction and when it moves in the reverse direction. The measurement data storage file 28 distinguishes each data into the forward direction and the reverse direction. Remember. In FIG. 4, data in the forward direction is indicated by “forward”, and data in the reverse direction is indicated by “reverse”.

  When the measurer gives an instruction to display data (YES in step S6), the data obtained by the measurement is displayed on the screen of the display 23 in FIG. Specifically, both forward measurement data and reverse measurement data are displayed simultaneously, only forward measurement data is displayed, and only reverse measurement data is displayed. The display is performed by selecting one of the three types of display modes. In order to make this selection possible, the display selection icon 43 is displayed as an image at a predetermined position on the measurement result screen 34 shown in FIG.

In the measurement result screen 34, the left part 36 is an area for displaying the result of X-ray measurement, and the right part 37 is an area for displaying the result of DSC measurement. In the X-ray measurement result display 36, coordinates with the diffraction angle 2θ on the horizontal axis and the diffraction line intensity I on the vertical axis are displayed. A diffraction line profile 35 that is a result of the X-ray measurement is displayed on the coordinates. Is displayed. The diffraction line profile 35 extends in the horizontal direction over the 2θ angle scanning region from the first angle 2θ ₁ = 5 ° on the horizontal axis scale to the second angle 2θ ₂ = 40 °.

  In the DSC measurement result display 37, the horizontal axis represents heat (Heat Flow / mW), temperature (Temperature / ° C), and humidity (%), and the vertical axis represents the elapsed time (min). A DSC curve 38 as a result of DSC measurement is displayed on the coordinates, and a temperature change curve 39 as a sample temperature condition for DSC measurement and X-ray measurement is further displayed.

  The display selection icon 43 includes a forward direction display icon 43a as a forward direction display instruction means, a backward direction display icon 43b as a backward direction instruction means, and a bidirectional display icon 43c as a bidirectional direction instruction means. These icons can be selected by a pointer display operated by a mouse as an input device. In the initial state, one of the icons, for example, the bidirectional display icon 43c is selected.

  Each of the icons 43a, 43b, and 43c is selected as in the series of processes in steps S7 and S8, the series of processes in S9 and S10, or the series of processes in S11 and S12 in FIG. Corresponding forward data, backward data, or bidirectional data image data is generated, and an image is displayed on the screen based on the data in step S13.

  In this embodiment, as shown in steps S8, S10, and S12, every time measurement data is obtained, the CPU 18 generates image data for image display of the data, and the image data is displayed in step S13. Transmit to the driver. Therefore, in the present embodiment, data obtained by measurement is displayed immediately on the screen of the display 23 of FIG. 1, that is, in real time.

For example, now, in a state where both the display icon 43c is selected, the forward direction of the X-ray diffraction measurement from 2 [Theta] ₁ = 5 ° to 2θ ₂ = 40 °, from the 2 [Theta] ₂ = 40 ° to 2θ ₁ = 5 ° When the X-ray diffraction measurement in the reverse direction is alternately and repeatedly performed, the steps S11, S12, and S13 in FIG. 3 are performed. First, as shown in FIG. The diffraction line profile 35a, the DSC curve 38 and the temperature change curve 39 are displayed simultaneously with the measurement. Next, as shown in FIG. 6, the first diffraction line profile 35b, the DSC curve 38 and the temperature change curve in the reverse direction are displayed. 39 is displayed simultaneously with the measurement, and further, as shown in FIG. 7, a second diffraction line profile 35c, a DSC curve 38, and a temperature change curve 39 in the forward direction are displayed.

  After the measurement as described above is repeatedly performed, when the measurement end condition is reached (for example, when the sample temperature reaches a predetermined temperature) (YES in step S16 in FIG. 3), a measurement end command is issued. Is generated (step S17), and X-ray diffraction measurement and thermal analysis measurement are completed. When all measurements are completed in this way, all measurement data obtained by the measurement are displayed on the measurement result screen 34 as shown in FIG.

  When the measurer desires data analysis, for example, background reduction processing or peak search processing (YES in step S18), the desired analysis is performed on the obtained data, and further obtained by analysis. The obtained data, that is, analysis data is stored in the analysis data storage file 29 of FIG. 2 (step S19). Although not shown in the flowchart of FIG. 3, the obtained analysis data is displayed in the same display form as in FIG. 8 in accordance with an instruction from the measurer.

  When the forward direction display icon 43a is selected instead of selecting the bidirectional display icon 43c of the display selection icons 43, steps S7, S8, and S13 of FIG. 3 are executed, as shown in FIG. Only the measurement data in the forward direction is selectively displayed in the X-ray measurement result display 36, and the display of the measurement data in the reverse direction is omitted. The DSC curve 38 and the temperature change curve 39 are displayed in their entire area.

  On the other hand, when the reverse direction display icon 43b of the display selection icons 43 is selected, steps S9, S10, and S13 in FIG. 3 are executed, and the X-ray measurement result display 36 is displayed as shown in FIG. Only the measurement data in the reverse direction is selectively displayed, and the display of the measurement data in the forward direction is omitted. The DSC curve 38 and the temperature change curve 39 are displayed in their entire area.

Next, the properties of the measurement result screen 34 shown in FIGS. 5 to 10 will be described with reference to FIG. In FIG. 1, X-ray diffraction measurement in the forward direction and the reverse direction between the first angle 2θ ₁ = 5 ° and the second angle 2θ ₂ = 40 ° of the diffraction angle 2θ is continuously repeated. As a result, the diffraction line profiles 35 for each time are drawn in parallel to each other at intervals in the vertical axis direction in the X-ray measurement result display 36 of FIG.

  While each X-ray diffraction measurement is repeatedly performed, that is, while each diffraction line profile 35 is sequentially drawn in FIG. 8, the ambient temperature of the sample 4 is the temperature change curve 39 of the DSC measurement result display 37. Has changed. Therefore, when the temperature change curve 39 is not vertical (a state in which the same temperature is maintained), each X-ray diffraction measurement is performed under different temperature conditions.

  In this embodiment, each diffraction line profile 35, each temperature range when the profile is obtained, and each DSC measurement result corresponding to the temperature range are displayed in association with each other. Specifically, each diffraction line profile 35 is displayed at a horizontal position in a direction along the horizontal axis of the graph with respect to the sample temperature range on the temperature change curve 39 when the diffraction line profile 35 is measured. Yes.

  More specifically, the time on the vertical axis (time axis) of the DSC measurement result display 37 indicates time data of the DSC curve 38 and the temperature change curve 39. The baseline of each diffraction line profile 35 coincides with the measurement start time of each measurement in the forward direction and the reverse direction. That is, when the base line of each diffraction line profile 35 is extended in the right direction as indicated by a broken line, the time at which the extended line intersects the vertical axis (time axis) of the DSC measurement result display 37 is the measurement of each diffraction line profile 35. The start time is shown.

  Since the DSC curve 38 and the temperature change curve 39 are both displayed based on the vertical axis (time axis) of the DSC measurement result display 37, the baseline of each diffraction line profile 35 is the vertical axis of the DSC measurement result display 37. The coincidence with the time on the axis means that the temperature at the start time of each diffraction line profile 35 is a temperature indicated by the intersection of the base line of the diffraction line profile 35 and the temperature change curve 39. . In addition, the DSC measurement data at the start time of each diffraction line profile 35 is a value indicated by the intersection of the base line of the diffraction line profile 35 and the DSC curve 38.

  The temperature change from the start of each diffraction line profile 35 (2θ = 5 ° for forward measurement, 2θ = 40 ° for reverse measurement) to the end is the baseline and temperature of each diffraction line profile 35. This is a part of the temperature change curve 39 for the time from the intersection with the change curve 39 to the end of the diffraction line profile 35. The DSC characteristic from the start to the end of each diffraction line profile 35 is a part of the DSC curve 38 corresponding to the time from the intersection of the base line of each diffraction line profile 35 and the DSC curve 38 to the end of the diffraction line profile 35. It turns out that.

  For example, when considering the eighth diffraction line profile 35 from the bottom indicated by the arrow A in FIG. 8, the predetermined portion C starting from the point where the base line and the temperature change curve 39 intersect is the diffraction line profile 35. It is a temperature change part corresponding to. Further, the predetermined portion D starting from the point where the base line of the diffraction line profile 35 and the DSC curve 38 intersect is the DSC change portion corresponding to the diffraction line profile 35.

  If each angle position between 2θ = 5 ° to 40 ° of each diffraction line profile 35 is exactly matched to the time axis, each diffraction line profile 35 is a profile that rises to the right in the case of a forward profile. (That is, a profile that rises upward by the time elapsed as 2θ increases), and in the case of the reverse profile, it should be a profile that rises to the left (ie, a profile that rises upward by the time elapsed as 2θ decreases). . However, in the display method of the present embodiment, only the measurement start point of each diffraction line profile 35 is made coincident with the time on the time axis, and the base line of each diffraction line profile 35 is displayed in parallel with the horizontal axis (2θ angle axis). is doing. Thereby, the X-ray measurement result display 36 is easy to see.

  Note that the point on each diffraction line profile 35 that coincides with the time on the vertical axis of the DSC measurement result display 37 is not limited to the measurement start point, and may be the center point or an arbitrary intermediate point, or the measurement end point. May be.

  As is apparent from the above description, the DSC curve 38 and the temperature change curve 39 in the DSC measurement result display 37 follow the vertical axis (time axis), and the X-ray measurement result display 36 shows the diffraction line profile 35 in the vertical axis direction. The position also follows the vertical axis (time axis) of the DSC measurement result display 37. Accordingly, each diffraction line profile 35 has a corresponding relationship with an intersection or an intersection region of the temperature change curve 39 and the DSC curve 38 when each profile is horizontally extended in the right lateral direction.

  Therefore, for example, the lowest diffraction line profile 35a is created within a temperature range of 22.0 ° C. to 23.0 ° C., and the second diffraction line profile 35b from the bottom is 23.0 ° C. to 24.0 ° C. If created within the temperature range of ° C., the bottom diffraction line profile 35a is drawn in the horizontal direction of the 22.0 ° C. to 23.0 ° C. portion of the temperature change curve 39, The second diffraction line profile 35b is drawn in the horizontal direction of the portion of the temperature change curve 39 at 23.0 ° C to 24.0 ° C.

  As understood from the above, in the X-ray measurement result display 36, the numerical value of the X-ray intensity (Intensity) graduated on the vertical axis represents each diffraction line profile 35 drawn next to those numerical values. It does not directly indicate the peak intensity value, but indirectly indicates the magnitude of the X-ray intensity corresponding to the peak height of each diffraction line profile 35. In the present embodiment, it is not important to know the exact magnitude of each peak intensity in each diffraction profile 35, but the difference in peak generation position between each diffraction line profile 35 and the difference in approximate peak intensity. Therefore, the display method such as the X-ray measurement result display 36 of this embodiment is very convenient for the measurer.

  Next, in the present embodiment, when the measurer instructs the measurement result screen 34 to perform predetermined screen processing so that the measurer can accurately grasp the measurement result (in FIG. 3). In step S14, YES), the process proceeds to step S15, and a predetermined screen processing program is executed. Specifically, when an operator designates an arbitrary diffraction line profile 35, for example, a diffraction line profile 35 indicated by an arrow A in FIG. 8 with a pointer, and clicks (selects) a mouse button as an input device, The diffraction line profile 35 is displayed with a thicker line (or a different color) than the other diffraction line profiles 35.

  On the right side of the selected diffraction line profile 35, the temperature range when the diffraction line profile 35 is obtained is displayed numerically (arrow B), for example, “108.0-110.2”. At the same time, the corresponding temperature range portion C of the temperature change curve 39 and the corresponding DSC portion D of the DSC curve 38 are also displayed in bold lines (or different colors). If you click again, the selection is canceled, the thick line is removed, and the normal thickness is restored.

  On the other hand, when a portion C of the temperature change curve 39 or a portion D of the DSC curve 38 is clicked, these portions are regarded as selected and are displayed with bold lines (or different colors), and at the same time, corresponding diffraction The line profile 35 is displayed as a thick line (or a different color). Further, the temperature range is displayed numerically on the right side of the selected diffraction line profile.

  As described above, the diffraction line profile 35, the temperature change curve 39, and the DSC curve 38 are visually displayed in association with each other, and a thick line is indicated by clicking on a portion for which a correspondence relationship is desired. Since the correspondence between the curves can be easily, quickly and clearly recognized by display and numerical display, the crystal structure and characteristics of the sample 4 can be easily and accurately determined.

  In the present embodiment, the bidirectional display shown in FIG. 8, the forward display shown in FIG. 9, and the reverse display shown in FIG. 10 can be switched by a switch switching operation using the display selection icon 43. Yes. Hereinafter, this display switching process will be described.

  FIG. 11A schematically shows the case where the bidirectional display is performed in an easily understandable manner. In this example, a sample having a diffraction peak at a diffraction angle 2θ = α is used for measurement. Then, the temperature change is performed with a constant temperature rising gradient from 100 ° C. to 148 ° C., and during the temperature change, the forward X-ray diffraction measurement is performed three times (profiles 35a, 35c, 35e), and the reverse direction. X-ray diffraction measurement is performed twice (profiles 35b and 35d). When reversal is performed in the forward direction and the reverse direction, it is assumed that the temperature rises by 2 ° C. in the time required for the reversal.

  Under the above conditions, the first forward measurement is performed during a temperature change of 100 ° C. to 108 ° C., and then the first reverse measurement is performed when the temperature rises from 108 ° C. to 110 ° C. Started continuously. The reverse measurement is performed during a temperature change of 110 ° C. to 118 ° C., and then the second forward measurement is continuously started when the temperature rises from 118 ° C. to 120 ° C.

  The forward measurement is performed during a temperature change from 120 ° C. to 128 ° C., and then the second backward measurement is continuously started when the temperature rises from 128 ° C. to 130 ° C. The reverse direction measurement is performed during a temperature change of 130 ° C. to 138 ° C., and then the third forward measurement is continuously started when the temperature rises from 138 ° C. to 140 ° C. The forward measurement is performed during a temperature change from 140 ° C to 148 ° C.

  In the conventional measurement method in which the measurement is performed only in the forward direction and the X-ray detector is moved back to the starting angle position between each measurement as in the past, the X-ray diffraction measurement is interrupted when the X-ray detector moves back. Therefore, X-ray diffraction measurement data during the temperature change could not be obtained. On the other hand, according to the present embodiment, since the forward direction measurement and the reverse direction measurement are alternately and continuously repeated, the return time for returning the X-ray detector to the initial position becomes unnecessary, and the X-ray diffraction The measurement is interrupted only for a short time to reverse the measurement direction from the forward direction to the reverse direction. Therefore, the interruption of the X-ray measurement can be suppressed as much as possible.

  By the way, as already explained, the base lines of the diffraction line profiles 35a to 35e are adjusted to the temperature position at the start of measurement. That is, the starting point (left end point) of the first profile 35a in the forward direction is represented at a position indicating 100 ° C. The starting point (right end point) of the first profile 35b in the reverse direction is represented at a position indicating 110 ° C.

  The starting point (left end point) of the second profile 35c in the forward direction is represented at a position indicating 120 ° C. The starting point (right end point) of the second profile 35d in the reverse direction is represented at a position indicating 130 ° C. The start point (left end point) of the third profile 35e in the forward direction is represented at a position indicating 140 ° C.

  The temperature rise between the end of the forward measurement at the right end position of the profile and the start of the reverse measurement and between the end of the reverse measurement at the left end position of the profile and the start of the forward measurement is set to 2 ° C. However, if the time required for folding in the scanning direction of the 2θ angle is set short, the temperature rise at the time of folding can be further reduced.

  The 2θ angular position of the diffraction line peak appearing during forward measurement and the diffraction line peak appearing during reverse measurement are naturally the same angular position because the sample is the same. However, when the forward direction measurement and the reverse direction measurement are continuously performed while being reversed, the temperature condition at the time when the diffraction line peak appears in these measurements changes.

  Specifically, the temperature when the peak occurs in the first profile 35a in the forward direction is 106 ° C., the temperature when the peak occurs in the first profile 35b in the reverse direction is 112 ° C., and the forward direction 2 The temperature when a peak occurs in the second profile 35c is 126 ° C., the temperature when a peak occurs in the second profile 35d in the reverse direction is 132 ° C., and the peak occurs in the third profile 35e in the forward direction. The temperature at which it occurs is 146 ° C.

  Therefore, in the bidirectional display, the temperature difference from the peak in the forward direction to the peak in the reverse direction is 6 ° C. On the other hand, the peak in the forward direction appears after the peak in the reverse direction appears. The temperature difference until is 14 ° C. As described above, the fact that the temperatures at which peaks occur in a plurality of diffraction line profiles 35 are different between adjacent profiles is not a problem in a general analysis, but the structure of the sample with respect to temperature changes. If you want to analyze changes rigorously academically, it is not the best data.

  When performing such a strict analysis, for example, as shown in FIG. 11B, by selecting and clicking the forward display icon 43a, only the forward profiles 35a, 35c, and 35e are displayed as images. The reverse direction profiles 35b and 35d are deleted. Alternatively, for example, as shown in FIG. 11C, by selecting and clicking the reverse display icon 43b, only the reverse profiles 35b and 35d are displayed as images, and the forward profiles 35a, 35c, and 35e are deleted.

  If the graph of FIG.11 (b) or FIG.11 (c) is seen, since the difference of the temperature at the time of the peak generation of each profile will be equal to 20 degreeC in any case, the generation | occurrence | production angle of each peak and temperature environment It becomes possible to analyze the relationship strictly. In other words, it is possible to accurately and quickly analyze the obtained measurement result.

(Other embodiments)
The present invention has been described with reference to the preferred embodiments. However, the present invention is not limited to the embodiments, and various modifications can be made within the scope of the invention described in the claims.

  For example, in the above embodiment, the temperature control device 16 has been described as the environment changing means. However, the humidity control device 17 of FIG. 1 can be considered as an environmental change means, and the structural change of the sample with respect to the humidity change can be analyzed by X-ray diffraction measurement. Furthermore, a pressure control device for changing the pressure in the sample chamber 2 can be attached to the sample chamber 2 and the structural change of the sample with respect to the pressure change can be analyzed by X-ray diffraction measurement. Furthermore, the structural change of the sample with respect to the environmental change of the combination of temperature change, humidity change, and pressure change can be analyzed by X-ray diffraction measurement.

  In the above-described embodiment, the incident side optical system including the X-ray source 6 and the light receiving side optical system including the X-ray detector 7 are moved from the sample 4 while being rotated by the same angle θ in opposite directions around the sample axis ω. A goniometer, that is, a θ-θ goniometer, which is configured to detect the diffraction line of X is detected by the X-ray detector 7. Instead, the incident side optical system including the X-ray source 6 is fixed so as not to rotate, the sample 4 is rotated by θ around the sample axis ω, and the light receiving side optical system including the X-ray detector 7 is set to the sample axis. It is also possible to use a goniometer that is configured to detect the diffraction line from the sample 4 by the X-ray detector 7 while rotating at the angular velocity twice as large as θ rotation around ω, that is, θ-2θ goniometer.

1. 1. X-ray analyzer, 2. sample chamber; Goniometer (detector rotating device), 4. Sample, 6. 6. X-ray source X-ray detector, 8. Reference material, 9. 10. temperature sensor; 11. Humidity sensor 14. Main control device (control means) DSC measurement circuit, 16. Temperature controller, 17. Humidity control device, 18. CPU, 19. ROM, 21. RAM, 22. Memory, 23. Display (image display device), 24. Measurement control program, 26. 27. image display program Measurement data storage file 29. Analysis data storage file, 34. 35. Measurement result screen Diffraction line profile, 36. X-ray measurement result display, 37. DSC measurement result display, 38. DSC curve, 39. Temperature change curve, 43. Display selection icon 43a. Forward display icon, 43b. Reverse display icon, 43c. Bidirectional display icon, ω. Sample axis, S0. X-ray intensity signal, S1. Temperature signal, S2. Humidity signal S3. Heat quantity signal

Claims (6)

In an X-ray analyzer that detects X-rays emitted from a sample placed on the sample axis by an X-ray detector when the sample is irradiated with X-rays,
Environmental change means for changing the environment for the sample;
A detector rotating device for rotating the X-ray detector around the sample axis;
Intensity calculating means for calculating the X-ray intensity based on the output signal of the X-ray detector;
Image display means for displaying output data of the intensity calculation means as an image on a screen;
Control means for controlling the operation of the detector rotation device, the intensity calculation means and the image display means,
The control means includes
The X-ray detector is rotated by the detector rotating device while measuring the angle alternately in the forward direction in which the angle increases and in the reverse direction in which the angle decreases between a small first angle and a large second angle. Let
The X-ray intensity is calculated both in the forward direction and in the reverse direction by the intensity calculation means,
X-ray intensity data during forward movement is displayed on the screen from the first angle to the second angle on the angle coordinate axis, and X-ray intensity data during reverse movement is displayed on the second angle on the same angle coordinate axis. An X-ray analyzer that displays on the screen from an angle toward the first angle. It further has display switching means for switching between forward display and reverse display,
The control means includes
When the forward switching is selected by the display switching means, the X-ray intensity data at the time of forward movement is displayed on the screen, and the X-ray intensity data of the backward movement is not displayed,
2. The reverse movement X-ray intensity data is displayed on the screen when the reverse display is selected by the display switching means, and the forward movement X-ray intensity data is not displayed. X-ray analyzer. Forward direction display instruction means for performing only forward direction display, reverse direction display instruction means for performing only reverse direction display, and bidirectional display instruction means for performing both forward and reverse display And
The control means includes
When the bidirectional display instruction means is selected, the X-ray intensity data at the time of forward movement and backward movement is displayed on the screen,
When the forward direction display instruction means is selected, the X-ray intensity data at the time of forward movement is displayed on the screen, and the X-ray intensity data of the backward movement is not displayed.
2. The X-ray intensity data at the time of reverse movement is displayed on the screen when the reverse direction display instruction means is selected, and the X-ray intensity data for the forward movement is not displayed. X-ray analyzer. The detector rotating device has a servo motor as a power source, the servo motor has an encoder that detects a rotation speed of its output shaft and outputs a signal, and the servo motor outputs an output of the encoder. 4. The X-ray analysis apparatus according to claim 1, wherein the X-ray analysis apparatus is a motor that controls the rotation of the output shaft so that is constant. The environment changing means is
Temperature control means for changing the temperature of the space including the sample axis;
The humidity control means for changing the humidity of the space including the sample axis, and the pressure control means for changing the pressure of the space including the sample axis, respectively. 5. The X-ray analyzer according to any one of the above. The image display means displays an environmental change performed by the environmental change means as an image on a screen,
6. The X according to claim 1, wherein the control unit displays an image display of output data of the intensity calculation unit and an image display of the environmental change in association with each other. Line analyzer.

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