CN110687095A - Device for in-situ high-temperature and high-pressure experiment - Google Patents

Device for in-situ high-temperature and high-pressure experiment Download PDF

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Publication number
CN110687095A
CN110687095A CN201910969993.6A CN201910969993A CN110687095A CN 110687095 A CN110687095 A CN 110687095A CN 201910969993 A CN201910969993 A CN 201910969993A CN 110687095 A CN110687095 A CN 110687095A
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ceramic
pottery
cover
glass slide
temperature
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CN110687095B (en
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钟日晨
崔浩
黎子萌
凌一凡
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65Raman scattering

Abstract

The invention provides a device for an in-situ high-temperature and high-pressure experiment, and belongs to the technical field of geological experiments. The device includes adiabatic shell, ceramic top cap, the glass slide, the pottery mainboard, the thermocouple, pottery bottom and base, the pottery bottom is fixed on the base, the pottery mainboard is arranged in on the pottery bottom and is covered, ceramic top cap on the pottery mainboard, the pottery top cap sets up adiabatic shell outward, set up glass slide one on the pottery bottom, set up glass slide two in the sample storehouse of pottery mainboard lower floor, the capillary quartz capsule sample is arranged in on glass slide two, capillary quartz capsule sample upper portion sets up the silver platform of heat conduction, the silver bench portion of heat conduction sets up the glass slide. And a plurality of thermocouples are fixed at the lower part of the second glass slide. The device can be heated to a maximum temperature of 500 deg.C, and can be maintained at the target temperature for a long time. Meanwhile, the mica heat insulation shell can effectively protect the microscope lens and prevent the microscope lens from being damaged due to overhigh temperature.

Description

Device for in-situ high-temperature and high-pressure experiment
Technical Field
The invention relates to the technical field of geological tests, in particular to a device for in-situ high-temperature and high-pressure tests.
Background
The geochemistry research is indispensable in the research of the current geoscience frontier field, and has very important significance for deeply understanding the aspects of the earth structure evolution, the prospecting exploration and the like. In which, the in-situ hydrothermal geochemistry experiment plays a crucial role in simulating the crust environment, researching the mineral origin and the deposit formation process, etc.
The in-situ hydrothermal geochemical experiment refers to a technology which can carry out a series of detection and analysis on a system which is carrying out chemical reaction by using other experimental instruments such as a Raman spectrometer and the like while carrying out the geochemical experiment under a water-containing system so as to obtain an experimental result under corresponding temperature and pressure. Instruments commonly used for conducting in situ Hydrothermal geochemical experiments mainly include a Hydrothermal diamond compact cell (HDAC) and a fused capillary quartz tube (FSCC).
Compared with a hydrothermal diamond pressure cavity, the fused capillary quartz tube has the following advantages: 1) the fused capillary quartz tube can effectively prevent experimental result deviation caused by solvent volatilization when a liquid sample is added; 2) when Raman detection is carried out, the fused capillary quartz tube hardly generates fluorescence interference, and necessary conditions can be provided for quantitative experiments. In the experiment for exploring the mineralization process, quantitative analysis plays a role in playing a key role.
The current apparatus for heating fused capillary quartz tubes is a Linkam cold and hot stage, which can accommodate up to 2.5cm of quartz tubes in a sample chamber. During heating, the pressure in the quartz tube first rises along the gas-liquid coexistence line, and after the system in the tube is uniform to a liquid phase, the pressure in the tube sharply rises along the isochoric line. Thus for the same temperature range, the maximum value of the pressure in the tube depends on the uniform temperature (T) of the bubbles in the systemh) The uniform temperature is related to the filling degree of the liquid sample in the tube (i.e. the ratio of the length of the liquid sample in the quartz tube to the total length of the cavity). Because the two ends of the fused capillary quartz tube need to be sealed by oxyhydrogen flame welding when manufacturing the fused capillary quartz tube, in order to prevent liquid in the tube from being heated and evaporated when welding, certain spaces (generally 2mm air columns) need to be reserved at the two ends. When the Linkam cold and hot table is used for the fused capillary quartz tube experiment, the maximum liquid filling degree in the quartz tube is 84%, and the maximum internal pressure of the system can be greatly limited by the filling degree.
In order to improve the liquid filling degree, the invention designs a brand-new in-situ high-temperature high-pressure experimental device which can be loaded with a melting capillary quartz tube with the maximum length of 7cm, and the maximum liquid filling degree can reach 91%. Meanwhile, in order to improve the bearing capacity of the quartz tube, the inner diameter and the outer diameter of the quartz tube used in the invention are respectively 25 +/-2 and 363 +/-10 microns, and compared with the existing commonly used quartz tube (the inner diameter and the outer diameter are respectively 100 and 365 microns), the bearing capacity is obviously improved.
Disclosure of Invention
The invention aims to provide a device for in-situ high-temperature and high-pressure experiments.
The device includes adiabatic shell, ceramic top cap, the glass slide, slide I, slide II, ceramic mainboard, the thermocouple, pottery bottom and base, the pottery bottom is fixed on the base, ceramic mainboard is arranged in on the ceramic bottom cap, ceramic mainboard upper cover ceramic top cap, ceramic top cap sets up adiabatic shell outward, set up slide I on the pottery bottom, set up slide II in the sample storehouse of ceramic mainboard lower floor, slide II is arranged in to the capillary quartz capsule sample, capillary quartz capsule sample upper portion sets up the heat conduction silver platform, heat conduction silver bench portion sets up the glass slide, the fixed a plurality of thermocouples in slide II lower part.
Wherein, the ceramic top cover, the ceramic main board and the ceramic bottom cover are made of alumina ceramics.
The base is made of aluminum alloy materials.
The ceramic top cover, the ceramic main board, the ceramic bottom cover and the base are connected through bolts, and nuts are arranged between the ceramic bottom cover and the base.
The ceramic main board is hollow in the center and is designed into a step shape, and a circle of resistance wire arranging holes are designed around the uppermost step and are used for arranging resistance wires; a cover glass is placed on the middle step; the step at the lowest layer is a sample chamber, and a capillary quartz tube sample is arranged on a second glass slide of the sample chamber.
The center of the heat conducting silver platform is provided with a slit.
The insulating shell is a mica heat insulating cover.
The number of the thermocouples is not less than 1, and the thermocouples are arranged in the grooves on the surface of the ceramic main plate.
The inner diameter of the capillary quartz tube sample is 23-27 μm, and the outer diameter is 353-373 μm.
The technical scheme of the invention has the following beneficial effects:
the device can be heated to a maximum temperature of 500 deg.C, and can be maintained at the target temperature for a long time. Meanwhile, the mica heat insulation shell can effectively protect the microscope lens and prevent the microscope lens from being damaged due to overhigh temperature.
Drawings
FIG. 1 is a schematic view of the apparatus assembly for in-situ high temperature and high pressure experiments according to the present invention;
FIG. 2 is a cross-sectional view of the apparatus for in-situ high temperature and high pressure experiments according to the present invention;
FIG. 3 is a diagram of the apparatus for in-situ high temperature and high pressure experiment according to the present invention, wherein (a) is a top cover, (b) is a main plate, (c) is a bottom cover, and (d) is a base;
FIG. 4 is a temperature calibration curve of an apparatus according to an embodiment of the present invention;
FIG. 5 is a temperature-pressure curve of a high-density capillary quartz tube test process in an embodiment of the present invention;
FIG. 6 shows SO in fused capillary quartz tube in an embodiment of the present invention4 2-Concentration varies with temperature.
Wherein: 1-a thermally insulating enclosure; 2-ceramic top cover; 3-cover glass; 4, first glass slide; 5-glass slide II; 6-a ceramic main board; 7-a thermocouple; 8-a ceramic bottom cover; 9-a base; 10-capillary quartz tube sample; 11-resistance wire; 12-thermally conductive silver stage.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
The invention provides a device for in-situ high-temperature and high-pressure experiments.
As shown in fig. 1, 2 and 3, the device comprises a heat insulation shell 1, a ceramic top cover 2, a cover glass 3, a first glass slide 4, a second glass slide 5, a ceramic main board 6, a thermocouple 7, a ceramic bottom cover 8 and a base 9, wherein the ceramic bottom cover 8 is fixed on the base 9, the ceramic main board 6 is arranged on the ceramic bottom cover 8, the ceramic top cover 2 is covered on the ceramic main board 6, the heat insulation shell 1 is arranged outside the ceramic top cover 2, the first glass slide 4 is arranged on the ceramic bottom cover 8, the second glass slide 5 is arranged in a sample bin at the lowest layer of the ceramic main board 6, a capillary quartz tube sample 10 is arranged on the second glass slide 5, a heat conduction silver platform 12 is arranged at the upper part of the capillary quartz tube sample 10, the cover glass 3 is arranged at the upper part of the heat conduction silver platform 12.
The top cover, the main board and the bottom cover of the device are made of alumina ceramics, so that the device can play the roles of insulation and heat insulation, and the base of the hot table is made of aluminum alloy materials. The above components are connected through M5 metric bolt, and the nut is arranged between the hot table main body part and the base to separate, thereby reducing heat dissipation.
In the specific design, a circle of resistance wire arrangement holes with the diameter of 1mm are designed around the uppermost step in the center of the ceramic main board 6 and used for arranging resistance wires 11 to heat a capillary quartz tube sample 10 in the device. A cover glass 3 with the specification of 85 multiplied by 20 multiplied by 0.1mm is placed on the middle stage of the ceramic main board 6, so that the temperature fluctuation of the sample chamber caused by air convection in the heating process is prevented, and the signal loss of detection instruments such as Raman spectrum and the like by the cover glass is greatly reduced. The lowest step of the ceramic main plate 6 is a sample chamber, and a capillary quartz tube for experiments is placed on a glass slide I4 with the specification of 80X 18X 1 mm. As the width of the sample chamber is larger, in order to increase the heat conduction efficiency and avoid temperature gradient, a heat conduction silver platform 12 with a slit of 70 multiplied by 1mm at the center is arranged in the sample chamber, thereby ensuring that the temperature can be uniformly conducted to the quartz tube in the slit. A second glass slide 5 with the specification of 90 multiplied by 25 multiplied by 1mm is placed on the step of the ceramic bottom cover 8, so that the purposes of reducing air convection and preserving heat are achieved. The heat insulation shell 1 at the outermost layer of the heat station is a mica heat insulation cover, so that heat loss in the experimental process can be prevented to the maximum extent.
In order to measure the temperature in the sample chamber, one or more K-type thermocouples 7 can be fixed at the lower part of the second sample chamber glass slide 5, and the temperature measuring points of the thermocouples are tightly attached to the glass slide, so that the temperature measuring accuracy is improved. The surface of the ceramic main board 6 is provided with 8 grooves with the width and the depth of 1mm, and the grooves can be used for heating couples and resistance wire leads. During the experiment, the knob voltage regulator is used for heating the device, and the output voltage of the knob voltage regulator is adjusted to adjust the heating power of the heating table, so that the temperature control purpose in the experiment process is achieved.
The temperature calibration of the device is realized by the following steps: i) welding and sealing a series of fused capillary quartz tubes which are different in filling degree and only contain deionized water; ii) putting different quartz tubes into the device for heating respectively, and recording T of each quartz tubeh(ii) a iii) on the National Institute of Standards and Technology (NIST) website, finding out the theoretical T according to the filling degree (pure water system, i.e. representative system density) of each quartz tubeh(http:// webboot. nist. gov); iv) control ThThe theoretical and actual values of (a) are used to make a temperature calibration curve, as shown in fig. 4. The result of the temperature calibration of the device shows that the T is actually measuredhThe difference between the temperature and the theoretical value is almost the same, so that the temperature measuring effect of the device can be determined to be more accurate, and the temperature correcting accuracy is within 4 ℃.
According to the design scheme, a set of device can be manufactured. The heating stage uses a nichrome wire with a diameter of 0.2mm as a heating wire, and the total resistance is about 30 omega. The device can be heated to a maximum temperature of 500 ℃ and can be thermostatted at the target temperature for a longer time. Meanwhile, the mica heat insulation shell can effectively protect the microscope lens and prevent the microscope lens from being damaged due to overhigh temperature.
The following description is given with reference to specific examples.
Study on association mode of magnesium sulfate at high temperature and high pressure
The specific implementation method comprises the following steps:
step 1, preparing MgSO (MgSO) with concentration of 1.2m4The solution was dissolved and two fused capillary quartz tube samples, MgSO 2, having a length of about 7cm were packed4The solution filling degree was 80% and 96%.
And 2, respectively heating the two samples by using a device, carrying out laser Raman detection on the two samples, and collecting Raman spectra according to a certain temperature gradient.
And 3, calculating the pressure in the quartz tube at each temperature by using the existing state equation (figure 5).
Step 4, according to the collectionThe obtained Raman spectrum is combined with a concentration standard sample to calculate SO in the solution at different temperatures4 2-Concentration (fig. 6).
SO in the quartz tube along with the temperature rise in the experimental process4 2-The concentration is gradually reduced to show SO at high temperature4 2-With Mg2+A tendency to associate more readily. However, for two different quartz tube samples, their SO' s4 2-The concentration trend was consistent (fig. 6). From the equation of state, it can be estimated that the high density quartz tube (96% fill) can reach a pressure of about 3.3kbar at about 250 ℃ (fig. 5), while the low density quartz tube (80% fill) has a pressure of only 0.13bar at about 250 ℃ (not shown). The experimental result shows that under the condition of warm pressure in the experiment, the pressure is opposite to SO4 2-With Mg2+The association of (a) has little influence.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (9)

1. The utility model provides a device for normal position high temperature high pressure experiment which characterized in that: comprises a heat insulation shell (1), a ceramic top cover (2), a cover glass (3), a first glass slide (4), a second glass slide (5), a ceramic main plate (6), a thermocouple (7), a ceramic bottom cover (8) and a base (9), ceramic bottom (8) are fixed on base (9), ceramic bottom (8) are arranged in on ceramic mainboard (6), ceramic top cap (2) is covered on ceramic mainboard (6), ceramic top cap (2) are set up adiabatic shell (1) outward, set up slide one (4) on ceramic bottom (8), set up slide two (5) in the sample storehouse of ceramic mainboard (6) lower floor, slide two (5) are arranged in to capillary quartz capsule sample (10), capillary quartz capsule sample (10) upper portion sets up heat conduction silver platform (12), heat conduction silver platform (12) upper portion sets up glass cover (3), a plurality of thermocouples (7) are fixed to slide two (5) lower parts.
2. The apparatus according to claim 1, wherein: the ceramic top cover (2), the ceramic main plate (6) and the ceramic bottom cover (8) are made of alumina ceramics.
3. The apparatus according to claim 1, wherein: the base (9) is made of an aluminum alloy material.
4. The apparatus according to claim 1, wherein: the ceramic top cover (2), the ceramic main board (6), the ceramic bottom cover (8) and the base (9) are connected through bolts, and nuts are arranged between the ceramic bottom cover (8) and the base (9).
5. The apparatus according to claim 1, wherein: the ceramic main board (6) is hollow in the center and is designed into a step shape, and a circle of resistance wire arranging holes are formed in the periphery of the uppermost step and used for arranging resistance wires (11); a cover glass is placed on the middle step; the step at the lowest layer is a sample chamber, and a capillary quartz tube sample is arranged on a second glass slide (5) of the sample chamber.
6. The apparatus according to claim 1, wherein: the center of the heat conducting silver platform (12) is provided with a slit.
7. The apparatus according to claim 1, wherein: the insulation shell (1) is a mica heat insulation cover.
8. The apparatus according to claim 1, wherein: the number of the thermocouples (7) is not less than 1, and the thermocouples (7) are arranged in the grooves on the surface of the ceramic main plate (6).
9. The apparatus according to claim 1, wherein: the inner diameter of the capillary quartz tube sample (10) is 23-27 μm, and the outer diameter is 353-373 μm.
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