JP4526099B2 - Method for manufacturing sample support and sample high temperature apparatus - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a connection method for connecting tungsten members to each other by welding. The present invention also relates to a sample high temperature apparatus for heating a sample.
[0002]
[Prior art]
X-ray diffractometers that measure the crystal structure and the like of a sample using the X-ray diffraction phenomenon have been widely known. In this X-ray diffractometer, a sample high temperature apparatus that supports a sample in a heated state may be used in order to measure a change in the crystal structure or the like of the sample at a high temperature.
[0003]
Conventionally, as this sample high temperature apparatus, as shown in FIG. 5, a connection structure constituted by connecting members formed of tungsten or a tungsten alloy (hereinafter referred to as tungsten members) to each other is often used. In this connection structure, a thermocouple 54 in which a tungsten wire 52 and a tungsten / rhenium wire 53 are connected at a temperature measuring point P is connected to the heater plate 51 in order to detect the temperature of the heater plate 51 formed of tungsten. Is done.
[0004]
In this case, the heater plate 51 corresponds to one tungsten member, the thermocouple 54 corresponds to the other tungsten member, and the sample is placed on the heater plate 51. When the heater plate 51 is energized, the heater plate 51 generates heat and the sample placed thereon can be heated.
[0005]
In general, since it is difficult to weld two tungsten members, conventionally, one tungsten member, for example, a member 55 formed of, for example, Ta (tantalum), Pt (platinum), Mo (molybdenum) or the like is used. The thermocouple 54 is pressed against the other tungsten member, for example, the heater plate 51, and in this state, the thermocouple 54 is welded to the heater plate 51 by spot welding or the like, thereby connecting the thermocouple 54 and the heater plate 51, that is, the tungsten member. We had achieved a connection between each other.
[0006]
[Problems to be solved by the invention]
Incidentally, in recent years, there has been a demand to use a connection structure (hereinafter referred to as a tungsten structure) between tungsten members as described above in an N ₂ (nitrogen) gas atmosphere. In this case, tungsten can be used without any trouble even in an N ₂ gas atmosphere, but Ta (tantalum), Pt (platinum), Mo (molybdenum), etc. may not be used due to changes in physical properties in the N ₂ atmosphere. There is. For this reason, conventionally, the tungsten structure cannot be used in an N ₂ gas atmosphere.
[0007]
The present invention has been made in view of the above problems, and an object of the present invention is to enable a tungsten structure to be used without any trouble even in an N ₂ atmosphere.
[0008]
[Means for Solving the Problems]
To achieve the above Symbol purpose of the method of manufacturing a sample holder according to the present invention, on a base formed by tungsten or a tungsten alloy, formed by joining the sample holding member formed of tungsten or a tungsten alloy sample A method of manufacturing a support base , wherein a welded portion of the sample holding member is placed on the base with a rhenium foil interposed therebetween, and the base, the rhenium foil, and the welded portion of the sample holding member are placed by a pair of spot electrodes. A process of welding the base, the rhenium foil, and the welded portion of the sample holding member at a plurality of locations by energizing those electrodes in a pressed state and fixing the sample holding member on the base. Features.
In the method of manufacturing a sample support with the above configuration, the sample holding member can be a partition member having an L-shaped cross section, and one piece of the L-shape is a welded portion, and the other piece is It can be used as a screen part for holding the sample.
[0009]
In the following, the manufacturing method of the sample holder according to the present invention, on a base formed by tungsten or a tungsten alloy, placing the temperature measuring point of the thermocouple formed by tungsten or a tungsten alloy, rhenium surveying temperature point pressing a foil to the base, a plurality of points around the base and the rhenium foil by energizing their electrodes while pressing the base and said the process of welding the rhenium foil temperature measuring points by a pair of spot electrodes And the temperature measuring point of the thermocouple is connected to the base .
[0010]
According to the method for manufacturing the sample support of the above configuration, the rhenium member is used as the interposition member when the tungsten members are connected to each other by welding. This rhenium member has physical properties in the N ₂ atmosphere is stable, tungsten structure that is configured to include a also now available without hindrance in N ₂ atmosphere.
[0011]
In the method for manufacturing a sample support, the welding is spot welding in which welding is performed by applying a current to the dotted region while pressing the dotted region.
[0012]
In the following, the sample temperature apparatus according to the present invention includes: a base formed by tungsten or a tungsten alloy, is formed by a tungsten or tungsten alloy, and the sample holding member provided on the base, connected to the base It has energizing means for energizing the said base Te, the base and welded parts of the sample holding member, to each other by being spot welded to a plurality of points in a state sandwiching the rhenium foil therebetween The spot welding is performed by energizing the base, the rhenium foil, and the welded portion of the sample holding member with a pair of spot electrodes while energizing the electrodes. And
[0013]
According to the sample high temperature apparatus having this configuration, the sample can be heated by causing the base to generate heat by energization. In addition, since the tungsten or tungsten alloy constituting the base and the sample holding member and the rhenium member interposed therebetween do not deteriorate in characteristics even in a high-temperature N ₂ gas atmosphere, the sample high-temperature apparatus according to the present invention has a high temperature. The sample can be held without any trouble under the N ₂ atmosphere.
[0014]
(5) Next, another sample high-temperature apparatus according to the present invention includes a base formed of tungsten or a tungsten alloy, a thermocouple formed of tungsten or a tungsten alloy and bonded to the base, and connected to the base. Energizing means for energizing the base, and the temperature measuring point of the thermocouple is welded to the base with the rhenium member and the base sandwiching the temperature measuring point of the thermocouple. By doing so, the base is brought into close contact with the base.
[0015]
According to the sample high temperature apparatus having this configuration, the sample can be heated by causing the base to generate heat by energization, and the temperature of the sample at that time can be detected by the thermocouple. In addition, since the tungsten or tungsten alloy constituting the base and the thermocouple and the rhenium member that presses the thermocouple against the base do not deteriorate in characteristics even in a high-temperature N ₂ gas atmosphere, according to the sample high-temperature apparatus of the present invention, The sample can be held without any trouble under an N ₂ atmosphere.
[0016]
(6) Next, still another sample high-temperature apparatus according to the present invention includes a base formed of tungsten or a tungsten alloy, and is formed of tungsten or a tungsten alloy and joined to the base, thereby being integrated with the base. A sample holding member for holding the sample, a thermocouple formed of tungsten or a tungsten alloy and joined to the base, and an energization means connected to the base and energizing the base, the base And the sample holding member are joined to each other by welding the base and the sample holding member with a rhenium member sandwiched therebetween, and the temperature measuring point of the thermocouple is determined by the rhenium member and the base. By welding the rhenium member to the base with the temperature measuring point of the thermocouple sandwiched therebetween, the rhenium member is brought into close contact with the base. It is characterized by being joined together.
[0017]
DETAILED DESCRIPTION OF THE INVENTION
(First embodiment)
FIG. 1 shows a sample heating support 1 which is a connection structure of tungsten members formed by using the method for connecting tungsten members according to the present invention to configure a sample high temperature apparatus of an X-ray diffraction apparatus. In this case, the embodiment is shown. The X-ray diffractometer shown here detects an X-ray source F that generates X-rays that irradiate the sample S, a container 2 that hermetically surrounds the sample heating support 1, and diffracted X-rays generated from the sample S. And an X-ray detector 3.
[0018]
The container 2 is formed of, for example, Al (aluminum), and a viewing window 4 made of a transparent material such as heat-resistant glass is provided at a position where the sample S can be expected from the outside. Through this window 4, the temperature of the sample S can be measured by an optical thermometer. Further, the container 2, are connected N ₂ gas supply system for supplying N ₂ gas therein. In addition, an X-ray passage window 13 is provided on the side surface of the container 2 with a material that allows X-rays to pass therethrough, for example, Be (beryllium). Even when the X-ray passage window 13 is provided, the airtightness inside the container 2 is not impaired.
[0019]
The sample heating support 1 is made by welding, for example, spot welding, a pair of partition members 8 and 8 having an L-shaped cross section, which is also formed of tungsten, to a base plate 7 formed of tungsten in a generally rectangular thin plate shape. Is formed by. The screen member 8 functions as a sample holding member for holding a sample. The end on the long side of the base plate 7 is bent to increase the strength of the base plate 7. Further, a power source 12 as an energizing means is connected to both ends of the base plate 7. When a predetermined voltage is applied to both ends of the base plate 7 by the power source 12, the base plate 7 generates heat by energization.
[0020]
When the partition member 8 is welded to the base plate 7, as shown in FIG. 2, the rhenium foil 9, that is, the rhenium member is sandwiched between the base plate 7 and the partition member 8. The partition member 8 is pressed from both sides by the spot electrodes 11a and 11b, and further energized, whereby the base plate 7 and the partition member 8 are welded to each other and connected to each other.
[0021]
In addition, it seems that about 5 to 6 welding locations by spot welding indicated by “x” in FIG. 2 are sufficient. Further, the spot electrodes 11a and 11b are formed of, for example, molybdenum or tungsten, and the tip diameters for welding are set to about φ1 mm, for example. Moreover, the welding power at the time of spot welding is set to 35 WS (watts / second), for example.
[0022]
In general, the base plate 7 and the partition member 8, which are tungsten members, cannot be easily welded. However, if the rhenium foil 9 is interposed between them as in the present embodiment, the tungsten members are securely connected to each other. Can be welded. In addition, the long hole 14 provided in the partition member 8 is for adjusting the clamping force with respect to the sample S to a desired value.
[0023]
In FIG. 1, the distance between the pair of partition members 8 and 8 is set to be slightly wider than the width of the sample S, and the sample S is inserted between them to support the sample S in an upright state. Can do. The sample S is a substance formed of, for example, ceramic glass, and it is considered desirable to receive an X-ray measurement in an upright state.
[0024]
Since the X-ray diffraction apparatus of the present embodiment is constructed as described above, the interior of the container 2 is set to N ₂ gas atmosphere by N ₂ gas supplied from N ₂ gas supply system 6. Then, a voltage is applied to the base plate 7 of the sample heating support 1 by the power source 12 to heat the base plate 7, thereby heating the sample S to a desired temperature, for example, about 1700 ° C. to 1800 ° C. The temperature of the heated sample S is detected by an optical thermometer through the observation window 4.
[0025]
In the high temperature and N ₂ atmosphere as described above, the X-ray emitted from the X-ray source F enters the sample S through the X-ray passage window 13 of the container 2. At this time, when the Bragg diffraction condition is satisfied between the incident X-ray and the crystal lattice plane of the sample S, a diffracted X-ray is generated from the sample S, and the diffracted X-ray passes through the X-ray passage window 13. Then, it proceeds to the outside and is detected by the X-ray detector 3. In this way, diffraction X-ray information from the sample S in a high temperature and N ₂ atmosphere can be collected.
[0026]
During the X-ray diffraction measurement as described above, the base plate 7 made of tungsten and the partition member 8 made of tungsten can be used without any trouble even in an N ₂ atmosphere. Also, the rhenium foil 9 interposed between the base plate 7 and the partition member 8 does not cause a significant change in characteristics in the N ₂ atmosphere, and can be used without any trouble.
[0027]
(Second Embodiment)
FIG. 3 shows a sample heating support base 1 which is an example of a connection structure between tungsten members formed by using the method for connecting tungsten members according to the present invention to configure a sample high temperature apparatus of an X-ray diffraction apparatus. An embodiment when used is shown. In FIG. 3, the same members as those in FIG. 1 are denoted by the same reference numerals, and description thereof will be omitted.
[0028]
In the embodiment shown in FIG. 1, the sample temperature is measured by the optical thermometer through the observation window 4, but in the present embodiment shown in FIG. 3, the sample temperature is measured using a thermocouple. Specifically, the temperature measuring point P of the thermocouple 22 is connected to the back surface of the base plate 7. Further, no partition member (see reference numeral 8 in FIG. 1) is provided on the upper surface of the base plate 7, and the sample S is simply placed on the base plate 7 in a planar manner.
[0029]
The thermocouple 22 is formed by connecting a tungsten wire 23 and a tungsten / rhenium wire 24 at a temperature measuring point P. The connection of the temperature measuring point P of the thermocouple 22 to the base plate 7 is achieved by a welding process. For example, as shown in FIG. 4, the temperature measuring point P of the thermocouple 22 is connected to the base plate 7 by a rhenium foil 19. Further, it can be achieved by welding to the back surface of the base plate 7 with spot electrodes 11a and 11b at appropriate positions of the rhenium foil 19, for example, four corners indicated by “x” marks.
[0030]
Even in X-ray diffraction apparatus of the present embodiment, in FIG. 3, the interior of the container 2 is set to N ₂ gas atmosphere by N ₂ gas supplied from N ₂ gas supply system 6. Then, a voltage is applied to the base plate 7 of the sample heating support 1 by the power source 12 to heat the base plate 7, thereby heating the sample S to a desired temperature, for example, about 1700 ° C. to 1800 ° C. The temperature of the heated sample S is detected by the thermocouple 22.
[0031]
In the high temperature and N ₂ atmosphere as described above, the X-ray emitted from the X-ray source F enters the sample S through the X-ray passage window 13 of the container 2. At this time, when the Bragg diffraction condition is satisfied between the incident X-ray and the crystal lattice plane of the sample S, a diffracted X-ray is generated from the sample S, and the diffracted X-ray passes through the X-ray passage window 13. Then, it proceeds to the outside and is detected by the X-ray detector 3. In this way, diffraction X-ray information from the sample S in a high temperature and N ₂ atmosphere can be collected.
[0032]
During the X-ray diffraction measurement as described above, the base plate 7 made of tungsten and the thermocouple 22 containing tungsten can be used without any trouble even in an N ₂ atmosphere. Further, the rhenium foil 19 connecting the temperature measuring point P of the thermocouple 22 to the base plate 7 does not cause a significant change in characteristics in the N ₂ atmosphere, and can be used without any trouble.
[0033]
(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.
[0034]
For example, in the above embodiment, the method for connecting the tungsten members according to the present invention is applied to the case where the sample heating support 1 used in the X-ray diffractometer is manufactured, but the present invention connects the tungsten members to each other. The present invention can be applied to the production of a tungsten structure having any other structure configured as described above.
[0035]
【The invention's effect】
As described above, according to the method for manufacturing a sample support base according to the present invention, since rhenium foil is used as an intervening member when the base and the sample holding member , which are tungsten members , are connected by welding, the welding is performed. The connection structure of tungsten members produced by the above can be used without any trouble in the N ₂ atmosphere.
[0036]
Further, according to the sample high temperature apparatus of the fourth aspect, the temperature of the sample can be raised by causing the base to generate heat by energization. In addition, since the tungsten or tungsten alloy constituting the base and the sample holding member and the rhenium member interposed therebetween do not deteriorate in characteristics even in a high-temperature N ₂ gas atmosphere, the sample high-temperature apparatus according to the present invention has a high temperature. The sample can be held without any trouble under the N ₂ atmosphere.
[0037]
According to the sample high temperature apparatus of the fifth aspect, the sample can be heated by causing the base to generate heat by energization, and the temperature of the sample at that time can be detected by the thermocouple. In addition, since the tungsten or tungsten alloy constituting the base and the thermocouple and the rhenium member that presses the thermocouple against the base do not deteriorate in characteristics even in a high-temperature N ₂ gas atmosphere, according to the sample high-temperature apparatus of the present invention, The sample can be held without any trouble under an N ₂ atmosphere.
[Brief description of the drawings]
FIG. 1 is a view showing an embodiment of a high temperature sample apparatus manufactured by using a method for connecting tungsten members according to the present invention.
FIG. 2 is a perspective view showing an embodiment of a method for connecting tungsten members according to the present invention.
FIG. 3 is a diagram showing another embodiment of a high temperature sample apparatus manufactured by using the method for connecting tungsten members according to the present invention.
FIG. 4 is a perspective view showing another embodiment of a method for connecting tungsten members according to the present invention.
FIG. 5 is a perspective view showing an example of a conventional tungsten structure.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Sample heating support stand 2 Airtight container 3 X-ray detector 4 Viewing window 7 Base plate 8 Screen member 9 Rhenium foil 11a, 11b Spot welding electrode 13 X-ray passage window 19 Rhenium foil 21 Sample heating support stand (of tungsten members) Connection structure)
22 Thermocouple 23 Tungsten wire 24 Tungsten rhenium wire

Claims (8)

A method for manufacturing a sample support, comprising a sample holding member formed of tungsten or a tungsten alloy joined to a base formed of tungsten or a tungsten alloy,
Place the welded part of the sample holding member on the base with a rhenium foil in between ,
In a state where the welded portions of the base, the rhenium foil, and the sample holding member are pressed by a pair of spot electrodes, the electrodes are energized to weld the welded portions of the base, the rhenium foil, and the sample holding member. Perform processing at multiple locations,
The method for producing a sample support , wherein the sample holding member is fixed on the base . The sample holding member is a partition member having an L-shaped cross section, wherein one part of the L shape is a welded part, and the other part is a partition part for holding the sample. The manufacturing method of the sample support stand of Claim 1. On the base formed of tungsten or tungsten alloy , place the temperature measuring point of the thermocouple formed of tungsten or tungsten alloy ,
Press the temperature measuring point against the base with rhenium foil ,
In a state where the base and the rhenium foil are pressed by a pair of spot electrodes, a process for welding the base and the rhenium foil by energizing those electrodes is performed at a plurality of locations around the temperature measuring point,
A temperature measuring point of the thermocouple is connected on the base . A method for manufacturing a sample support base . A base formed of tungsten or tungsten alloy;
A sample holding member formed of tungsten or a tungsten alloy and provided on the base;
Has energizing means for energizing the said base being connected to said base,
The base and the welded portion of the sample holding member are joined together by spot welding at a plurality of locations with a rhenium foil sandwiched between them ,
The spot welding is performed by energizing the base, the rhenium foil, and the welded portion of the sample holding member with a pair of spot electrodes while energizing those electrodes. Sample high-temperature equipment. A base formed of tungsten or tungsten alloy;
A thermocouple formed of tungsten or a tungsten alloy and connected to the base;
Has energizing means for energizing the said base being connected to said base,
The thermocouple temperature measurement point is obtained by spot welding the rhenium foil to the base at a plurality of locations around the temperature measurement point with the temperature measurement point of the thermocouple sandwiched between the rhenium foil and the base. , Closely connected to the base,
The sample high-temperature apparatus , wherein the spot welding is performed by energizing the base and the rhenium foil while the base and the rhenium foil are pressed by a pair of spot electrodes . A base formed of tungsten or tungsten alloy;
A sample holding member formed of tungsten or a tungsten alloy and provided on the base;
A thermocouple formed of tungsten or a tungsten alloy and connected to the base;
Has energizing means for energizing the said base being connected to said base,
The base and the welded portion of the sample holding member are joined to each other by applying first spot welding at a plurality of locations with a rhenium foil sandwiched between them .
The first spot welding is performed by energizing the base, the rhenium foil, and the welded portion of the sample holding member with a pair of spot electrodes while energizing those electrodes.
Temperature measuring point of the thermocouple, the base to the second spot welding at a plurality of locations around the temperature measuring point the rhenium foil in a state sandwiching the temperature measuring point of the thermocouple by the said base and rhenium foil by the applied, is connected in close contact with the base,
The sample high-temperature apparatus, wherein the second spot welding is performed by energizing the base and the rhenium foil while the base and the rhenium foil are pressed by a pair of spot electrodes . The sample holding member is a partition member having an L-shaped cross section, wherein one part of the L shape is a welded part, and the other part is a partition part for holding the sample. The sample high temperature apparatus according to claim 4 or 6. A container covering the base, and N into the container ₂ The sample high-temperature apparatus according to any one of claims 4 to 7, further comprising a gas supply system for supplying a gas.

Images