JPH05188016A - Sample heating device of x-ray diffraction device - Google Patents

Abstract

PURPOSE:To obtain a sample heating device of an X-ray diffraction device which is capable of obtaining correctly measured data, and of preventing pollution of the atmosphere around the sample. CONSTITUTION:A sample heating device is used in an X-ray diffraction device where the X-ray is made incident on a sample 8, and the X-ray diffracted by the sample 8 is detected. The sample heating device is provided with a light source 13, an elliptical inner surface reflecting mirror 12 to converge the light from the light source 13, and a photo-conductor 14 to guide the light converged by the elliptical inner surface reflecting mirror 12 to the sample 8.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a sample heating device used in an X-ray diffraction device.

[0002]

2. Description of the Related Art In a general X-ray diffractometer, measurement is performed by irradiating a sample with X-rays and detecting X-rays diffracted by the sample. In addition, when the X-ray diffraction measurement is performed, the sample may be heated to analyze the sample under a high temperature condition.

[0003] Conventionally, as an apparatus for heating a sample used for X-ray diffraction measurement, a heating wire such as a coil is wound around the sample at intervals and the sample and the heating wire are covered with a heat shield cover. Things are known. In this heating device, the heating wire is energized to generate heat, and the heat is used to heat the sample.

[0004]

However, in the above-mentioned conventional heating device, since the X-rays incident on the sample and the diffracted X-rays diffracted by the sample are transmitted through the heating line, the obtained X-ray diffraction There is a problem in that accurate measurement data cannot be obtained because the diffraction data of the heating line is included in the data. In addition, there is a problem that a pollutant component is emitted from the heating line that generates heat, and the atmosphere around the sample is polluted.

The present invention has been made in view of the above problems in the conventional apparatus, and it is an X-ray generator that can obtain accurate measurement data and does not contaminate the atmosphere around the sample. An object is to provide a sample heating device.

[0006]

In order to achieve the above object, a sample heating apparatus for an X-ray diffraction apparatus according to the present invention comprises a light source, a light focusing means for focusing light from the light source, and a light focusing means. And a light guide for guiding the collected light to the sample.

[0007]

The light from the light source is converged at one point by the light converging means and then guided to the sample by the light guide, and the sample absorbs the light to heat the sample to raise its temperature. The sample heats up when exposed to light,
There are no obstacles on the traveling path of the X-rays incident on the sample and the X-rays diffracted from the sample. Therefore, the inconvenience that the obtained X-ray diffraction data contains an unnecessary component is eliminated. Further, since the sample is heated by light, no pollutant component is generated and the atmosphere around the sample is maintained in a clean state.

[0008]

EXAMPLE FIG. 2 shows X using the sample heating apparatus according to the present invention.
An example of a line diffraction device is shown. Prior to describing the sample heating apparatus, first, the entire X-ray diffraction apparatus will be briefly described.

A goniometer 2 is fixedly arranged on the table 1. The goniometer 2 includes a source arm 3 and a detector arm 4 that extend radially from the center. An X-ray tube 5 equipped with an X-ray source P is fixed to the tip of the radiation source arm 3, while a scintillation counter (SC) and other X-ray detectors 6 are fixed to the tip of the detector arm 4. ing. A sample support device 7 which also functions as a sample heating device is arranged in front of the goniometer 2, and a sample 8 to be measured is fixedly supported by the sample support device 7.

The X-rays emitted from the X-ray source P in the X-ray tube 5 are incident on the sample 8 and when the X-ray diffraction condition is satisfied between the X-ray source P and the crystal lattice plane in the sample 8. Diffract on the sample. The diffracted X-rays are detected by the X-ray detector 6.
An X-ray intensity measurement circuit (not shown) is connected to the X-ray detector 6, and the intensity of the X-ray detected by the X-ray detector 6 is measured by the X-ray intensity measurement circuit.

The goniometer 2 drives the radiation source arm 3 to rotate in the direction of arrow A intermittently or continuously at a constant angular velocity, and further intermittently or continuously drives the detector arm 4 at the same angular velocity in the opposite direction, that is, the arrow. It is driven to rotate in the B direction. These rotations are usually called θ rotations.
Due to this θ rotation, the incident angle of the incident X-rays that emerge from the X-ray tube 5 and enter the sample 8 changes with time,
The intensity of the diffracted X-ray with respect to each individual X-ray incident angle was measured, and as a result, a graph showing the intensity change of the diffracted X-ray with respect to the incident angle change of the X-ray incident on the sample 8, that is, a so-called X-ray diffraction pattern was obtained. Be done. From this X-ray diffraction pattern, the internal structure of the sample 8 is analyzed.

In the above X-ray diffraction measurement, the measurement may be performed with the sample 8 being heated. Sample support device 7
Also acts as a sample heating device therefor. Hereinafter, it will be described in detail.

As shown in FIG. 1, the sample support and heating device 7 has a cylindrical casing 9 and a heat shield cover 10 fixedly mounted on the casing 9. A thin film 11 made of a material that allows X-rays to freely pass through is attached to the upper portion of the heat shield cover 10. An ellipsoidal inner reflecting mirror 12 is provided inside the housing 9, and a tungsten lamp 13 as a light source is arranged at one of two focal positions of the inner reflecting mirror 12. The light introducing end 14a of the light guide 14 which is a cylindrical rod is arranged at the other focal position. A current supply circuit 16 is connected to the lamp 13, and the lamp 13 emits light by the current supplied from the current supply circuit. Light guide 14
Is a material that can efficiently transmit light, such as quartz (SiO 2
₂ ), made of transparent sapphire (Al ₂ O ₃ ), and fixed by the housing 9 immovably.

The upper end of the light guide 14, that is, the light emitting end 14
A sample mounting table 15 is fitted and attached to the sample b.
Then, the sample 8 is placed on the sample placing table 15. The X-rays pass through the thin film 11 and enter the sample 8, and the diffracted X-rays from the sample 8 pass through the thin film 11 and proceed.

A temperature detecting element, for example, a thermocouple 17 is embedded in the sample mounting table 15, and a temperature signal of the thermocouple, that is, a thermoelectromotive force is guided to a temperature control circuit 18.
The temperature control circuit 18 determines whether the sample 8
The current supplied by the current supply circuit 16 is controlled so that the temperature of 1 is maintained at the target predetermined temperature.

Since the sample supporting and heating device 7 is constructed as described above, all the light emitted from the lamp 13 is collected by the inner reflecting mirror 12 at the light incident end 14a of the light guide 14. Then, the condensed light propagates through the light guide 14 and is applied to the sample 8 from the light emitting end 14b. The light irradiation heats the sample 8 to a target temperature.
In this state, X-ray diffraction measurement is performed.

In the sample heating device 7 described above,
No heating line such as a coil exists on the X-ray irradiation surface side of the sample 8. Therefore, unnecessary X-ray diffraction lines are not generated, and accurate X-ray diffraction measurement can be performed. Further, since no heating line is used, no pollutant component is generated even at high temperatures, and X-ray diffraction measurement can be performed in a clean atmosphere. Therefore, the sample 8 is not adversely affected, and accurate measurement results can be obtained.

As described above, quartz, transparent sapphire, etc. can be applied as the material of the light guide 14, but the heat resistant temperature of the transparent sapphire is as high as about 2000 degrees, and therefore the sample 8 is heated to a high temperature. If desired, it is convenient to use the transparent sapphire as a light guide.

Further, the sample mounting table 15 can be made of either a material such as a black material which easily absorbs light to generate heat or a transparent material. However, when a highly transparent sample is used as the sample, it is preferable to configure the sample mounting table with a light absorbing material such as black in order to increase the heat generation efficiency.

FIG. 3 shows another embodiment of the sample heating apparatus according to the present invention. Sample heating device 20 according to this embodiment
Is an ellipsoidal internal reflection mirror 12, a tungsten lamp 13 as a light source arranged at the first focal point of the internal reflection mirror 12, and a total reflection capillary tube 21 as a light guide.
And have. The total reflection capillary tube 21 is a cylindrical round bar made of quartz with a through hole 22 having a minute diameter formed in the center thereof. For example, the outer diameter of the cylindrical rod is about 8 mm, and the inner diameter of the through hole 22 is 30 to 50 μm. The total reflection capillary tube 21 has a light introduction end at the inner reflection mirror 1.
The second focal point position is set to 2.

The sample heating device 20 is an X-ray diffraction device for obtaining an X-ray diffraction image of a micro sample or a micro region of the sample.
For example, it is suitable as a heating device for heating a sample to be used in a so-called minute area X-ray diffractometer, a four-axis goniometer, or the like.

FIG. 5 shows an example in which the sample heating device 20 is installed in a microscopic area X-ray diffractometer. The small area X-ray diffractometer is an axis line orthogonal to the optical axis of the X-ray R.
An ω holder 23 that is rotatable about an axis, and a χ holder 24 that is connected to the tip of the ω holder and is rotatable about an χ (chi) axis that is an axis orthogonal to the ω axis. The sample holder 25 is connected to the tip of the holder 24 and is capable of rotating and swinging around a φ axis line orthogonal to both the ω axis line and the χ axis line.

The ω holder 23 is driven by a pulse motor 26 arranged on the ω axis to oscillate, and the χ holder 24
Is swung by being driven by a pulse motor 27 arranged on the χ axis, and the sample holder 25 is swung by being driven by a pulse motor 28 arranged on the φ axis.

The sample 8 is held at the tip of a sample holder 25, and the holders 23 and 2 described above with respect to the sample 8 are held.
Position sensitive X-ray detector (PSP
C) 29 is installed. The PSPC 29 is an X-ray detector known per se, and takes in X-rays from an opening 30 extending in an arc shape, and simultaneously measures the X-ray intensity at each position in the arc area. That is, the intensity of the diffracted X-ray is simultaneously detected over a wide range of the diffraction angle 2θ.

A collimator 31 is provided on the optical axis of the X-ray R, and the X-ray incident on the sample 8 is limited by the collimator 31 to a very narrow cross section, for example, a diameter of several μm. The X-ray beam irradiated on the sample 8 through the collimator 31 is diffracted by the sample 8 when the diffraction condition is satisfied with the crystal lattice plane in the sample. The diffracted X-rays enter the PSPC 29 through the opening 30, and their intensities are simultaneously measured over a wide range of the diffraction angle 2θ.

Since the X-ray beam is limited by the collimator 31 to have a very small cross-sectional area and is incident on the sample 8,
It is possible to obtain X-ray information of a minute sample or a minute area of the sample. When the X-ray irradiation area becomes minute as described above, the number of crystals existing in the X-ray irradiation area decreases, and the reproducibility of the measurement result may deteriorate. In order to avoid this, the ω holder 23, the χ holder 24, and the sample holder 25 are respectively attached to the ω axis, χ axis, and φ.
The sample 8 is oscillated about the axis to rotate and oscillate in all directions, and more crystals in the sample are surely put in the X-ray irradiation region.

In the case of the embodiment shown in FIG. 5, the sample heating device 20 attached to the above-mentioned minute region X-ray diffraction device is
The sample 8 is fixed to the opposite side of the ω-axis pulse motor 26. Since the heating device 20 has the configuration shown in FIG. 3 as described above, the light emitted from the lamp 13 is collected at the light incident end of the total reflection capillary tube 12 by the internal reflection mirror 12. The light collected in this manner travels while being totally reflected in the minute through hole 22, exits from the light exit end, and enters the sample 8. The sample 8 is heated by this light irradiation. Since the total reflection capillary tube 21 can emit spot-like light having a small cross section and high intensity, even if the sample 8 is a minute sample, it can be reliably heated. Further, when the sample 8 is relatively large, it is possible to reliably heat only the minute region of the sample. The light emitting end of the total reflection capillary tube 21 and the sample 8
By arranging the condenser lens 32 between and, it becomes possible to further narrow the light irradiation area to the sample 8 and heat an extremely small area.

FIG. 4 shows still another embodiment of the sample heating apparatus. This sample heating device has a xenon lamp 33 as a light source, an ellipsoidal internal reflection mirror 12, and an optical fiber 34 as an optical conductor. The light emitting portion 33a of the xenon lamp 33 is arranged at the first focal position of the inner reflecting mirror 12. The optical fiber 34 is a known photoconductive member, and is formed by bundling a large number of thin linear members capable of conducting light while totally reflecting the light. The optical fiber 34 has flexibility and can be freely deformed. Light incident part 34 of optical fiber 34
a is located at the second focal position of the inner reflecting mirror 12.
The condenser lens 32 is fixed to the light emitting portion 34b of the optical fiber 34.

The lamp 33 is powered by the power source 35 and emits light. The light from the lamp 33 is condensed by the inner reflecting mirror 12 on the light incident portion 34 a of the optical fiber 34. The condensed light travels while being totally reflected in the optical fiber 34, is emitted from the light emitting portion 34b, and is further irradiated by the condenser lens 32 while being converged on the minute sample 8 or the minute region of the sample 8. It In this way, the area irradiated with light is heated. The shutter 36 arranged between the lamp 33 and the light incident part 34a of the optical fiber 34 blocks the optical path of the reflected light from the internal reflection mirror 12 when it is not necessary to irradiate the sample 8 with light. Acts like. When heating the sample, the shutter 36 opens the optical path.

In the embodiment shown in FIG. 4 as well, light can be condensed in a minute region, so that a sample used in an X-ray diffraction device for a minute region such as a minute region X-ray diffraction device is heated. It is suitable for Further, in particular, since the flexible optical fiber 34 is used to transmit the light, and the light emitting portion 34b is a very small member, even if the spatial margin around the sample 8 is small, the The sample heating device can be installed easily.

Although the present invention has been described with reference to the preferred embodiment, the present invention is not limited to the embodiment. For example, referring to FIG.
As the condensing means for condensing the light on the surface 4, a condensing lens may be used in addition to the ellipsoidal inner reflecting mirror 12.

In the embodiment shown in FIG. 1, the light guide 14 itself is used as a structural element for supporting the sample 8.
However, it is also possible to provide a separate structural element for supporting the sample and use the light guide 14 only as an element for heating the sample.

In the embodiment shown in FIG. 1, the sample 8 is heated from the back side of the X-ray irradiation surface. However, the heating point is not necessarily limited to the back side of the X-ray irradiation surface. For example, heating the sample from the lateral direction. You can also

[0034]

According to the present invention, when the X-ray diffraction measurement is performed while the sample is kept at a high temperature, it is not necessary to provide a heating line around the sample, so that accurate X-ray diffraction that does not include a noise component is obtained. Data is obtained. In addition, the atmosphere around the sample can be maintained in a clean state.

[Brief description of drawings]

FIG. 1 is a side sectional view showing an embodiment of a sample heating apparatus according to the present invention.

FIG. 2 is a perspective view showing an example of an X-ray diffraction apparatus using the sample heating apparatus.

FIG. 3 is a plan sectional view showing another embodiment of the sample heating apparatus according to the present invention.

FIG. 4 is a cross-sectional plan view showing still another embodiment of the sample heating apparatus according to the present invention.

FIG. 5 is a perspective view showing a case where the sample heating device shown in FIG. 3 is attached to a minute region X-ray diffraction device.

[Explanation of symbols]

 8 sample 12 internal reflecting mirror 13 lamp 14 optical conductor 15 sample mounting table 21 total reflection capillary tube 32 condensing lens 33 xenon lamp 34 optical fiber

Claims (7)

[Claims] 1. A sample heating apparatus used in an X-ray diffraction apparatus for injecting X-rays into a sample and detecting the X-rays diffracted by the sample, a light source, and a light focusing means for focusing the light from the light source, A sample heating device, comprising: a light guide for guiding the light collected by the light focusing means to the sample. 2. The sample heating apparatus according to claim 1, wherein the light guide is a cylindrical rod made of quartz (SiO ₂ ) or transparent sapphire (Al ₂ O ₃ ). 3. The sample heating apparatus according to claim 1, wherein the light guide is a total reflection capillary tube provided with a through hole having a fine diameter for advancing while totally reflecting the light. 4. The sample heating apparatus according to claim 1, wherein the optical conductor is a flexible optical fiber bundle. 5. The sample heating apparatus according to claim 1, further comprising a condenser lens disposed between the light emitting end of the light guide and the sample. 6. The sample heating apparatus according to claim 1, further comprising a light absorbing member provided between the light emitting end of the light guide and the sample. 7. The sample heating apparatus according to claim 1, wherein the light focusing means is a reflecting mirror formed in an ellipsoidal shape.