JPH11211642A - High-temperature high-pressure atmosphere testing device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To achieve the fatigue/creep test and the pull/compression test of a sample under the atmosphere of a gas, a steam, or the like and under high- temperature and high-pressure condition by forming a container in an inner/outer double structure and reducing the annular space between an inner container, the support member of the sample, or the like. SOLUTION: When the inside of an internal container 50 is set to a desired gas atmosphere, a valve is adjusted and an active gas and/or an inactive gas is supplied to an annular space 62 of the internal container 50 by a compressor 96 from an active gas source 92 and/or an inactive gas source 94. In this case, water in a tank 63 is not sent by pressure. On the other hand, when the inside of the internal container 50 is set to steam atmosphere, the valves of the active gas source 92 and the inactive gas source 94 are closed, and water in the tank 63 is forcibly sent by a pump 65. Then, in either case, a gas or water in the internal container 50 is heated by a heating zone 4. In a testing in a gas atmosphere, the container 50 or 80 in a double structure is adopted, thus easily obtaining high-temperature and high-pressure gas atmosphere and testing a sample 66 under various kinds of conditions.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high-temperature and high-pressure test for various kinds of specimens and ceramics at high temperatures in various atmospheres such as water vapor, active and inert gas, etc. for testing fatigue, corrosion, tension and compression. The present invention relates to an atmosphere test apparatus.

[0002]

2. Description of the Related Art Recently, fine ceramics composite materials,
Research and development of new materials for ultra-high temperatures such as superalloys are being advanced, and strength tests and corrosion tests are being performed in an active / inert gas atmosphere at about 1000 to 2000 ° C. and 1 atm or less.

FIG. 1 shows a conventional example of a high-temperature tensile tester.
A test body 16 is mounted in an atmosphere container 14 provided between the base 10 of the tensile tester and the movable crosshead 12. The test body 16 has a load rod 1
8 and a load cell 20 for measuring the load weight, and is connected to the movable crosshead 12, and the lower part thereof is connected to the base 10 via a lower fixed rod 22. A heating element 24 is arranged in the atmosphere container 14 so as to surround the test body 16, and a heat insulating plate 26 is arranged so as to surround the heating element 24. Since the cooling water flows from the water storage tank 29 to the cooling jacket 28 provided outside the atmosphere container 14 and is cooled, the atmosphere container 14 can be made of ordinary stainless steel or the like. A bellows 31 that expands and contracts with the movement of the load rod 4 is provided above the atmosphere container 14.

At the time of the test, the test piece 16 is heated to a predetermined high temperature by energizing the heating element 24, and the atmosphere container 1 is heated by a vacuum pump 30 connected to the atmosphere container 14.
After depressurizing the inside 4, a predetermined gas is introduced by a gas source 32 connected to the atmosphere container 14. After the test body 16 is heated to a predetermined gas atmosphere in this way, the moving crosshead 12 is moved by a hydraulic pump or the like to apply a tensile load to the test body 16, and a high-temperature tensile test is performed in a predetermined gas atmosphere. The heating element 24 is usually made of the following heating resistance material according to the test temperature atmosphere. That is, when (1) the temperature is in the range of room temperature to 1200 ° C. and the atmosphere is the atmosphere, a nichrome wire (NiCr alloy), a Kanthal wire (FeCrAl alloy) or the like is used, and (2) a temperature of 1200 to 1200 ° C.
MoSi ₂ , SiC when the atmosphere is air at 1500 ° C
, Platinum (Pt), etc., and (3) a temperature of 15
In the case of a non-oxidizing atmosphere such as a vacuum or an inert gas at a temperature of 00 ° C. or more, molybdenum (Mo), tungsten (W), carbon (C), or the like is used.

[0005]

A test temperature of about 1500
The reason why the container 14 is set to a non-oxidizing atmosphere when the temperature is not less than ° C is that if the test is performed in the air or in an oxidizing atmosphere, the heating element is oxidized so much that a long-time test cannot be performed. Also, 1
It was difficult to test in an atmosphere in which oxidation occurs remarkably even at a temperature of 500 ° C. or less. As described above, in the conventional high-temperature test apparatus, the test atmosphere is limited in relation to the temperature. In addition, while research on the test in a high-temperature atmosphere is relatively advanced, research on the test in a high-pressure atmosphere is not so much advanced. More recently, 1500
It is expected that a test apparatus capable of performing a test in an extremely high temperature of 2000 ° C. or more, an ultra-high pressure of 10 to 20 atmospheres or more, and a special atmosphere such as superheated steam or supercritical water will be provided.

Accordingly, the present invention provides a high-temperature and high-pressure atmosphere test apparatus capable of performing a fatigue, creep test, and tensile / compression test of a sample in various atmospheres such as gas and water vapor and at high temperature and high pressure. It was made for the purpose of providing. to this end,
In the present invention, a high-temperature and high-pressure atmosphere test apparatus is used to form an internal container for accommodating a sample, a small annular space inserted into the internal container to form a small annular space, and a support member for supporting the sample, and a periphery of the internal container. A heater configured to heat the sample, an outer container arranged concentrically with the inner container via a heat insulating material outside the heater, and an atmosphere forming unit configured to form a predetermined atmosphere in the inner container. And adjusting means for adjusting the temperature and pressure of the atmosphere in the internal container. As described above, the container has a dual inner / outer structure, and the annular space between the inner container and the support member for the sample and the like is reduced, so that a high-temperature and high-pressure atmosphere can be easily obtained as compared with the related art, and under the atmosphere. Various material property tests can be performed.

[0007]

Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. The high-temperature and high-pressure test apparatus shown in FIG. 2 includes an internal atmosphere container (inner container) 50, an external atmosphere container (outer container) 80, a sample tray support (core) 60, a pressure balance controller 120, a high-pressure metering pump 66, and a temperature. It includes a controller 112 and the like. That is, this test apparatus has a dual container structure inside and outside, and can perform various tests on a sample in an atmosphere of superheated steam or supercritical water in addition to various gas atmospheres.

More specifically, an inner atmosphere container cover plate 54 and an outer atmosphere container cover plate 56 are attached to a fixed substrate 52, and the inner atmosphere container 50 is attached to the cover plate 54 via the cover plate 56. An external atmosphere container 80 is attached to 56. Since the internal atmosphere container 50 has an internal temperature of 1200 ° C. or higher, it has a bottomed cylindrical shape made of ceramics such as alumina, zirconia, silicon carbide, and silicon nitride, and a composite material thereof, and a new material. The lower opening is attached to the lid plate 54 with the bottom part facing upward. When the temperature is 1200 ° C. or lower, the container 50 may be made of a heat-resistant metal or quartz glass. 2 and 3
As shown in FIG. 7, a cylindrical core 60 is disposed concentrically with the container 50 with its lower end supported by the cover plate 54 in the container 50. The core 60 has an upper end 60a made of ceramics having excellent heat resistance, a lower end 60c made of metal, and an intermediate part 60b made of a heat insulating material. The core 60 may be made of two kinds or one kind of material. A small annular space 62 is formed between the container 50 and the core 60 over the entire length. A sample tray 64 is placed on the upper end of the core 60, and a sample (test piece) 66 such as a metal, a mineral composite, ceramics, or a new material is set therein.

The water in the water storage tank 63 of the water supply / drainage system is pressure-fed to the annular space 62 by the high-pressure quantitative piston pump 65 and is heated by the heater 104 to be described later to be steam, and the steam is recovered and cooled by the cooler 68. Become water. In this system, a pressure gauge 72, a pressure-holding valve 74, and a flow meter 76 are arranged.

An active gas source 92 and an inert gas source 94 are also connected to the annular space 62, and are appropriately pumped into the space 62 by a compressor 96. On the other hand, the external atmosphere container 80 has a bottomed cylindrical shape, and is attached to the external lid plate 56 with the bottom part facing downward, and the flange at the upper end of the cylindrical portion is attached to the lid plate 90. The hollow projection of the lower lid plate 56 is fitted into a circular hole formed in the center of the bottom 82, and supports the lower edge of the outer container 80. A water jacket 81 is arranged on the outer peripheral surface of the outer container 80 to cool the container 80 from the surroundings. Since the outer container 80 is used at normal temperature, it is made of a metal such as carbon steel and stainless steel with emphasis on pressure resistance without considering heat resistance.

Inner atmosphere container 50 and outer atmosphere container 80
A heating element (heater) 104 and a heat insulating material 106 are arranged in a large annular space 102 formed between them.
The heating element 104 is made of a nichrome wire (NiCr alloy), a Kanthal wire (FeCrAl alloy), molybdenum disilicide (MoSi ₂ ), molybdenum, tungsten, carbon, or the like, has a cylindrical shape, and surrounds the container 50. The heater 104
May be constituted by combining a plurality of rod-shaped, linear or plate-shaped heat insulating material pieces. The heating element 104 is supported by a support member 109.
The heater electrode 110
And heat is generated, and the temperature is controlled by the temperature controller 112. Note that the heater electrode 110 is cooled by cooling water. Insulation material 10
Reference numeral 6 denotes a supporting member 108 made of brick, ceramics, carbon, or the like, and includes a cylindrical portion 106a surrounding the heating element 104, a bottom portion 106b having a hole in the center, and a lid portion 106c for closing an upper opening of the cylindrical portion 106a. Is supported by the lid plate 90. Note that a reflection plate made of molybdenum, tungsten, stainless steel, or the like may be used instead of the heat insulating material 106.

The internal pressures of the annular spaces 62 and 102 are balanced by a pressure balancer 120. As shown in FIG. 4, the pressure balancer 120 has a first chamber 126 and a second chamber
8 are defined, and each chamber 126 and 128 is
Or 62. In a passage 132 extending from the first chamber 126 to an external inert gas source 130, a pressure adjusting mechanism 140 including a pair of valve bodies 134 is provided with a housing 1.
22. Since the pressure regulator 120 is not an essential part of the present invention, it will not be described in further detail here.
No. 8 discloses this. Note that this pressure balancer 12
Instead of 0, a known servo valve can be used.

The elevator 11 guided by the guide column 116
4 is engaged with the lower surface of the lid 90, and the lift 114 is moved up and down by the hydraulic cylinder 118,
The inner and outer containers 50 and 80, the heating element 104, the heat insulating material 106, and the upper lid 90 can be integrally moved up and down.
Although not described individually, portions requiring air-tightness and liquid-tightness are sealed by seal members as shown in the respective drawings.

Next, the operation of this embodiment will be described. When the interior of the inner container 50 is set to have a desired gas atmosphere, the valve is adjusted, and the active gas and / or
Alternatively, an inert gas is supplied to the annular space 62 of the inner container 50. In this case, the water in the tank 63 is not pumped. On the other hand, when the inside of the inner container 50 is set to the steam atmosphere, the valves of the active gas source 92 and the inert gas source 94 are closed, and the water in the tank 63 is pumped by the pump 65. In any case, the heating element 104 heats the gas or water in the inner container 50.

In a test in a gas atmosphere, a container 5 having a double structure was used.
Since 0 or 80 is adopted, a high-temperature and high-pressure gas atmosphere can be easily obtained, and the test of the sample 66 can be performed under various conditions. On the other hand, in a test in a steam atmosphere, a large amount of heat is required to convert water into steam, but the annular space 62 has a core 60 loosely fitted in the inner container 50 to reduce its volume. Therefore, the water in the space 62 is efficiently heated and evaporates in a short time to become water vapor from above, and the pressure in the space 62 changes accordingly. In order to efficiently heat the inner container 50, it is necessary to minimize the radiation of heat.
Help it. As shown in the vapor pressure diagram of water in FIG.
Water has a saturated steam pressure of 1 atm (kg / cm ² ) at 100 ° C., and when the pressure is lowered, the steam changes from the saturated steam to the superheated steam. The test temperature around the sample 66 1700 ° C., for pressure to the state of 10 kg / cm ^2, as shown in FIG. 3, the gas-liquid at the location of the saturation temperature 183 ° C., which corresponds to the saturation vapor pressure of 10 kg / cm ² An interface is formed. The lower half of the container 50 is hot water at 60 to 183 ° C, and the upper half is superheated steam at 183 to 1700 ° C.
Thus, the sample 66 is exposed to a predetermined high-temperature, high-pressure atmosphere, and its characteristics can be evaluated by observing the progress of corrosion fatigue over time.

Here, the temperature and pressure of the superheated steam in the annular space 62 can be changed by controlling the heating time of the heating element 104 and the amount of water supplied by the pump 65. After the temperature reaches 0 ° C., when water is pumped by a pump 65, a test in a so-called supercritical water atmosphere of 220 kg / cm ² or more is theoretically possible. Further, since the pressure in the space 62 and the pressure in the space 102 are almost equally balanced by the pressure balance adjuster 120, the thickness of the inner container 50 may be reduced, while the outer container 80 may be formed of the jacket 81.
As a result, it is possible to design with normal pressure resistance. In order to convert the water vapor in the container 50 into water, FIG.
The temperature and pressure may be controlled so as to be in the water region in the diagram of FIG. This control can be performed in parallel with heating and water supply, or with heating and water supply stopped.

In the second embodiment shown in FIG. 6, a load (compression force, tension force) is applied to a sample. The first
The same reference numerals are given to members and elements corresponding to the above-described embodiment, the description thereof will be omitted, and different configurations will be mainly described. Sample 1
The lower end of the lower rod 156 to which the chuck 154 for holding the lower end of the sample 52 is attached is fixed to the bottom plate 158, and the upper end of the upper rod 162 to which the chuck 160 for holding the lower end of the sample 152 is attached is on the lid plate 164. The outer container 170, which extends upward through the placed seal lid plate 166, has a structure similar to that of the outer container 80, but the inner container 180 has a cylindrical shape with both ends opened. Although there is no member corresponding to the core 60, the upper and lower rods 162 and 156 penetrate the cylinder 180, and the cross-sectional area of the annular space 172 is
Like 2, it is smaller. The illustration of the water and gas supply system is omitted.

In the second embodiment, a tensile force and an upward compressive force are applied to the upper rod 162 to perform a tensile and compressive test of the sample 152 in a steam atmosphere, a gas atmosphere, or the like. Can be. The present invention should not be construed as being limited to the above embodiments, and needless to say, modifications and improvements can be made without departing from the spirit of the present invention.

As described above, according to the present invention,
Much higher temperature and pressure (150-200
0 ° C, 10 atm) gas atmosphere or water vapor atmosphere can be used to perform material fatigue and tensile / compression tests.
In addition to ceramics, it can respond to the demands of a new era by applying it to composite materials, new materials, and properties of hydrothermal deposits. In addition, the above-mentioned effect can be achieved by making the container a dual structure of the inside and outside and at the same time, by a small measure of reducing the space between the inner container and the supporting member or the core inserted therein, so that the manufacturing cost also increases significantly. do not do.

[Brief description of the drawings]

FIG. 1 is a front sectional view showing one of conventional examples.

FIG. 2 is a front sectional view showing the first embodiment of the present invention.

FIG. 3 is a perspective view (partially cut away) of an inner container 50 in FIG. 2;

FIG. 4 is a sectional view of the pressure balancer 120 in FIG.

FIG. 5 is an explanatory diagram (water vapor pressure diagram) for explaining the operation of the embodiment in FIG. 2;

FIG. 6 is a front sectional view showing a second embodiment of the present invention.

[Explanation of symbols]

 50, 180 Inner container 60 Core 66, 160 Sample 80, 170 Outer container 92, 94 Gas source 104 Heater 106 Insulating material 112 Temperature controller 120 Pressure balancer

Claims (5)

[Claims] An internal container for accommodating a sample, a small annular space inserted through the internal container to form a small annular space, and a supporting member for supporting the sample; and a heating member disposed around the internal container and heating the sample. A heater to be provided; an outer container arranged concentrically with the inner container via a heat insulating material outside the heater; an atmosphere forming means for forming a predetermined atmosphere in the inner container; and an atmosphere in the inner container. And an adjusting means for adjusting the temperature and pressure of the sample. 2. An inner container for accommodating a sample, a core inserted through the inner container to form a small annular space and supporting the sample, and a core disposed around the inner container to heat the sample. A heater to be provided; an outer container disposed concentrically with the inner container via a heat insulating material outside the heater; a gas supply unit for supplying a predetermined gas into the inner container; and a gas in the inner container. And an adjusting means for adjusting the temperature and pressure of the sample. 3. An inner container for accommodating a sample, a core inserted into the inner container to form a small annular space and supporting the sample, and a core disposed around the inner container and heating the sample. A heater, a water supply means for supplying water into the inner container, and a water supply means for supplying water into the inner container, An adjusting means for adjusting the temperature and pressure of the critical water. 4. An inner container for accommodating a sample, a pair of rods inserted into the inner container to form a small annular space, and gripping the sample from both sides, and arranged around the inner container; A heater for heating a sample, an outer container arranged concentrically with the inner container via a heat insulating material outside the heater, a gas supply unit for supplying a predetermined gas into the inner container, and the inner container A high-temperature and high-pressure atmosphere test apparatus, comprising: adjusting means for adjusting the temperature and pressure of gas in the inside; and load means for applying a tensile force or a compressive force between the rods. 5. An inner container for accommodating a sample, a pair of rods inserted into the inner container to form a small annular space, and holding the sample from both sides, and arranged around the inner container; A heater for heating the sample; an outer container arranged concentrically with the inner container via a heat insulating material outside the heater; a water supply unit for supplying water to the inner container; A high-temperature and high-pressure atmosphere test apparatus comprising: adjusting means for adjusting the temperature and pressure of steam or supercritical water; and load means for applying a tensile force or a compressive force between the rods.