CN105911229B - A kind of high temperature high confining pressure fluid-solid interaction experimental rig and test method - Google Patents
A kind of high temperature high confining pressure fluid-solid interaction experimental rig and test method Download PDFInfo
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- CN105911229B CN105911229B CN201610496411.3A CN201610496411A CN105911229B CN 105911229 B CN105911229 B CN 105911229B CN 201610496411 A CN201610496411 A CN 201610496411A CN 105911229 B CN105911229 B CN 105911229B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D27/00—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00
- G05D27/02—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00 characterised by the use of electric means
Abstract
The invention discloses a kind of high temperature high confining pressure fluid-solid interaction experimental rig and test method, including pressure vessel, the axial depression bar of two symmetrically sealed is provided with pressure vessel horizontal direction, sample is placed between two depression bars, the heater of heating sample is socketed with outside pressure vessel, its surface is provided with hydraulic fluid mouth and optical window, heater is placed in the groove of base, pressure vessel contact surface is provided with temperature sensor, hydraulic fluid mouth is communicated to sample lay down location, optical window face sample center, and the optical measuring system of observation sample spectrum is installed.Present invention use is chemically reacted for sample under high confining pressure and hot conditions and spectral measurement, can under the fluid condition of HTHP in-situ observation solid sample microstructure feature and spectra collection, and the product of in site measurement solid and fluid interaction, measurement data is more nearly reality, data measured is more accurate reliable, is more beneficial for instructing the correct practice of sample to use analysis.
Description
Technical field
The present invention relates to a kind of high temperature high confining pressure fluid-solid interaction experimental rig and test method, belong to high temperature
High-Voltage Experimentation engineering device technique field.
Background technology
High temperature and pressure experiment is many scientific domains, such as planet and geoscience, condensed state physics, chemistry, material supply section
The important research means of etc. research field, and have been achieved for many important research achievements.In geoscience, HTHP
Test that epistemically the material composition inside ball and state and Petrogenesis And Metallogenesis etc. provide substantial amounts of experimental data for people.
For example, by studying the high temperature and pressure experiment of mantle rocks, it was recognized that earth mantle about 650km seismic wave discontinuity surface is
Caused by the phase in version of olivine/pyroxene-perovskite structure.In physics and chemical field, super-pressure can make between atom
Distance Shortened and the interaction between electronic shell occurs, and electron structure is changed and formed be totally different from often
Depress the chemical bond of material.For example, have realized that so far at high enough pressure any material can all occur it is nonmetallic with
Transformation between metallic state.Wherein, transformation of the metallic state to insulator not only occur under high pressure for sodium and lithium, and in room temperature and
The phenomenon melted under 1000000 atmospheric pressure still can not understand and explain so far.In material science, High-Voltage Experimentation research makes
It was recognized that there is superconducting property under high pressure low temperature for the material of non-superconducting under atmospheric low-temperature.For example, except known 23 kinds
Element has outside superconducting property under atmospheric low-temperature, it was found that has 29 kinds of elements to have superconducting property under high pressure.Except pure material
Outside, the Hg-Ba-Ca cuprates obtained under elevated pressure conditions are the materials for having so far highest superconducting temperature（Under 30Pa pressure
Superconducting transition temperature reach 164K）.This has guided a new approach to find and synthesizing superconducting material.In addition, HTHP
Element can also be synthesized it is many there is important or advantageous property new material, such as boron nitride superhard material, magnetic material,
Thermoelectric material, hydrogen storage material and solar energy materials etc..In recent years, high pressure（High temperature）Experiment is also in Oil-gas origin and biology
In field be applied.
In nature（Such as earth interior, seabed and water body）, engineering technology（As machinery, geology, ocean, thermoelectricity, nuclear power,
Boiler, building, digging, hydrometallurgy, chemical industry, the Hydrothermal Synthesiss of material and modification etc.）, scientific exploration（Such as ultrasound probing and sea
Ocean detection）In scientific experiment, high temp/high pressure is widely present（Hydrostatic pressing/differential stress）Interaction between fluid and solid.
Mechanical-chemical coupling effect in interaction process then causes interaction process to become complicated various.On the one hand, in high temperature
Under high pressure, fluid matasomatism can make the composition of solid sample when solid sample（Including chemical composition and thing phase composition）, structure（Bag
Include microcosmic, Jie's sight and macroscopic view）And property（Including macroscopic property, the physical property such as mechanics, acoustics, electricity, calorifics, spectroscopy,
And the chemical property such as Adsorption and desorption, dissolving, crystallization, alteration and electrochemistry）Significantly change；And on the other hand, in height
The solid sample of warm high pressure in turn again convection body composition（Formed including chemical composition, preservation kind and phase）, microcosmic knot
Structure and property（Including macroscopic property, various physical properties, and hydrogen fugacity/activity, oxygen fugacity/activity, water fugacity/activity,
The chemical property such as Eh values and pH value）Produce material impact.Therefore, the experimental study of high-temperature, high pressure fluid-solid interaction is
The research work particularly important into many science and technology fields.However, currently used for high-temperature, high pressure fluid-solid interaction
The experimental facilities generally existing operating temperature pressure of experimental study is relatively low, function limitation is single, integrated level is not high and body weight is excessive
And the defects of lacking flexibility, seriously hinder progress of each field in this aspect.
At present, Static pressure device and dynamic high-pressure installation can be divided into according to pressure method, high temperature and pressure test device.Static pressure
Pressue device can realize high-temperature and high-pressure conditions or environment by following several approach：1. high pressure kettle device, it is possible to achieve temperature
Degree and limited pressure, generally below 800 DEG C and 200MPa；2. big forcing press, mainly there are multiaspect top formula forcing press and piston-cylinder
Two kinds of devices of formula forcing press, multiface upsetting machine can produce the isobaric hydrostatic pressing of three axles and the three anisobaric pressure fields in axial direction, can
2000 DEG C and 10GPa respectively may be about with the maximum temperature and pressure of realization, can be carried out under high-temperature and high-pressure conditions compared with large sample
Experimental study, the piston cylinder formula forcing presses such as material phase transformation, melting, the synthesis of mineral or material can form 0~5GPa standard
Hydrostatic pressing, operating temperature are up to 1600 DEG C；3. Diamond primary ore, it is possible to achieve high temperature and 500GPa more than 6000 DEG C
The experiment of pressure, it can almost carry out the high temperature and pressure experiment research of earth interior all substances.Dynamic high-pressure installation mainly impacts
Ripple and laser pressue device.Pressure can be carried out to study up to 1000GPa high temperature and pressure experiment.
The problem of above-mentioned high-pressure installation is present mainly has：
（1）Under the conditions of the hydrostatic pressing of HTHP, it is difficult to accurately independent control temperature and pressure；（2）Existing high pressure
Kettle system bulk is larger, it is difficult to docked with microscope and various spectrometers, can not in-situ observation solid sample surface topography it is special
The means in site measurement reaction product such as spectrum can not be used by seeking peace.
The content of the invention
The technical problem to be solved in the present invention is：A kind of high temperature high confining pressure fluid-solid interaction experimental rig is provided
And test method, realize the surface microstructure feature of in-situ observation solid under high temperature high confining pressure and measure the surface of solids and solution
In reaction product, temperature reaches 700 DEG C, and confined pressure pressure reaches 200MPa, and test is more accurate reliable, domestic at present to solve
Above-mentioned variety of problems present in outer similar experimental rig.
The technical scheme that the present invention takes is：A kind of high temperature high confining pressure fluid-solid interaction experimental rig, including pressure
Force container, the axial depression bar of two symmetrically sealed is provided with the pressure vessel horizontal direction, is placed between the two axial depression bar
Sample, the pressure vessel are socketed with the heater of heated solution and sample outside, and its surface is provided with hydraulic fluid mouth and optical window
Mouthful, the heater is placed in the groove of base, pressure vessel contact surface is provided with temperature sensor, the hydraulic fluid mouth connects
Sample lay down location, the optical window face sample center are led to, and the micro- white light picture of observation sample and microspectrum are installed
Optical measuring system.
Preferably, said temperature sensor, heater, optical measuring system are connected to controller, and controller is also connected with
There are hydrostatic sensor and hydraulic pump, and be wired to host computer.
Preferably, above-mentioned hydraulic fluid mouth is connected to hydraulic pump by pipeline, and the hydraulic pump is connected to liquid reserve tank by pipeline,
For hydraulic fluid mouth with being provided with four-way valve and flow stop valve one on hydraulic pump connecting pipe, the another two-port of four-way valve connects liquid respectively
Pressure sensor and relief valve, the pipeline enclosure that hydraulic pump is connected with liquid reserve tank are provided with flow stop valve two.
Preferably, above-mentioned optical window communicates first through hole, the second through hole, hyalomere and third through-hole including face, the
One through hole is arranged on pressure vessel, and the second through hole is set on the heating, and the third through-hole is arranged on base side wall,
The hyalomere is arranged at first through hole by briquetting, and it is arranged in briquetting groove, and loophole is provided with briquetting groove,
Its outer surface is close at first through hole, is arranged in pressure vessel groove.
A kind of test method of high temperature high confining pressure fluid-solid interaction experimental rig, this method comprise the following steps：
（1）Sample is loaded in pressure vessel, fixed sample is sealed by two symmetrical axial depression bars；
（2）Compactedness is calculated according to different temperatures, confined pressure condition and pressure vessel containment, by hydraulic fluid mouth to pressure vessel
Inside it is passed through a certain amount of fluid；
（3）Heater will be heated sample and solution by heated pressure container；
（4）At different temperatures, the chemical solution that sample and different pressures are observed by optical measuring system interacts
Micro- white light picture and microphotogram under Shi Gaowen high confining pressures.
Beneficial effects of the present invention：Compared with prior art, effect of the present invention is as follows：
（1）The present invention can independently simultaneously precise control of temperature and pressure, two kinds of the independent and accurate control pressure of the present invention be done
Method, first, the flexible change volume of depression bar, this method will not change the component of reaction system；Second, hydraulic pump can be with pump flow
Body can also suck out the fluid inside pressure vessel, and this method can change the component of reaction system；
（2）The present invention is provided with optical window, can be with the micro-image of in-situ observation specimen surface, thus can be in height
Under the conditions of warm high confining pressure, the microstructure of specimen surface is directly observed using microscope（Such as corrode caused surface）；
（3）Present invention use is chemically reacted for sample under the conditions of high temperature and high confining pressure and spectral measurement, can
Reaction product under the fluid condition of high temperature high confining pressure in site measurement solid sample surface and fluid, measurement data more adjunction
Near actual, data measured is more accurate reliable, is more beneficial for instructing the correct practice of sample to use analysis；
（4）The present invention is provided with optical window, and can in-situ observation sample microspectrum, such as measuring various has Raman
The Raman spectrum of active material, Raman spectrum can accurately measure the lattice vibration energy of material.When material by different temperatures and
When confined pressure acts on, its lattice structure will produce change, and lattice vibration energy will also change, and Raman frequency shift will also change
Become, the stress of crystals, micro Raman spectra method can be accurately calculated according to the relation between stress and relative Raman frequency shift
For mechanical meaurement, have the characteristics that non-contact, lossless, spatial resolution is high and can be with deep focus, can be in different temperatures
Under pressure condition, the ess-strain and Raman spectrum of the measurement solid sample of system, and establish the reason of Raman frequency shift and stress
By relational model, basic data is provided and supported for research work and engineering technology；
（5）The present invention is simple in construction, and has the characteristics of small volume, in light weight, cost is low.
Brief description of the drawings
Fig. 1 is the layout drawing of the structural representation of the present invention；
Fig. 2 is Fig. 1 forward sight structural representation；
Fig. 3 is the close-up schematic view A in Fig. 1；
Fig. 4 is the hydraulic system structure schematic diagram of the present invention.
Embodiment
Below in conjunction with the accompanying drawings and the present invention is described further specific embodiment.
Embodiment 1：As Figure 1-Figure 4, a kind of high temperature high confining pressure fluid-solid interaction experimental rig, including pressure
Force container 2, two symmetrically sealed axially left side depression bars 3 and right side depression bar 4, left side pressure are provided with the horizontal direction of pressure vessel 2
Sample 5 is placed between bar 3 and right side depression bar 4, the heater 6 of heated solution and sample 5, its surface are socketed with outside pressure vessel 2
Hydraulic fluid mouth 9 and optical window 10 are provided with, the heater 6 is placed in the groove 26 of base 1, with the contact surface of pressure vessel 2
Temperature sensor 29 is provided with, hydraulic fluid mouth 9 is communicated to the lay down location of sample 5, the center of 10 face sample of optical window 5, and is provided with
Observe micro- the white light picture and microspectrum of sample 5（Raman, infrared etc.）Optical measuring system 30.
Raman spectrum can accurately measure the lattice vibration energy of material.When material is stressed effect, its lattice structure
Change will be produced, lattice vibration energy will also change, and Raman frequency shift will also change.According to stress and relative Raman
Relation between frequency displacement can accurately calculate the stress of crystals.Under the conditions of different temperatures difference confined pressure and axial stress,
The ess-strain and Raman spectrum of solid sample are systematically measured, the theoretic relationmodel of Raman frequency shift and stress can be established.
Preferably, the above-mentioned outer end of left side depression bar 3 connection loading device 7, loading device 7 are fixedly attached on base 1.
Preferably, above-mentioned loading device 7 includes reinforcing screw 18 and adaptor 19, reinforcing screw 18 can spiral movably connect
It is connected in the side wall of base 1, its thread head center is connected with adaptor 19, and the end set of adaptor 19 has a universal ball end 20, and ten thousand
Left side depression bar 3 is transferred force to bulb 20, the adjusting screw 25 on right side is connected on base 1, and it connects right side one end of depression bar 4
Bulb 43 is provided with, above-mentioned reinforcing screw 18 is combined by adjusting screw 25, the movement of left and right sides depression bar is realized, so as to ensure
Sample can occupy center position face optical window, and the data for being easy to optic testing system to gather are more accurate and more may be used
Lean on, and by adjusting screw and reinforce turning for screw, it is easy to adjust quick.
Preferably, said temperature sensor 29, heater 6, optical measuring system 30 are connected to controller, and controller is also
Hydrostatic sensor and hydraulic pump are connected with, and is wired to host computer.
Preferably, above-mentioned hydraulic fluid mouth 9 is connected to hydraulic pump 37 by pipeline, and hydraulic pump 37 is connected to liquid reserve tank by pipeline
36, hydraulic fluid mouth 9 on the connecting pipe of hydraulic pump 37 with being provided with four-way valve 38 and flow stop valve 1,38 another both ends of four-way valve
Mouth connects hydrostatic sensor 39 respectively and relief valve 40, the pipeline enclosure that hydraulic pump 37 is connected with liquid reserve tank 36 are provided with flow cutoff
Valve 2 42.
Preferably, above-mentioned optical window 10 communicates first through hole 14, the second through hole 15, hyalomere 13 and the 3rd including face
Through hole 16, first through hole 14 are arranged on pressure vessel 2, and the second through hole 15 is arranged on heater 6, the third through-hole 16
It is arranged in the side wall of base 1, hyalomere 13 is arranged at first through hole 14 by briquetting 12, and it is arranged in the groove of briquetting 12,
Loophole is provided with the groove of briquetting 12, its outer surface is close at first through hole 14, is fixedly connected on and is being pressed by screw 17
In the groove of force container 2.
Embodiment 2：A kind of test method of high temperature high confining pressure fluid-solid interaction experimental rig, this method include
Following steps：
（1）Sample is loaded in pressure vessel, fixed sample is sealed by two axially symmetric depression bars；
（2）Compactedness is calculated according to different temperatures, confined pressure condition and pressure vessel containment, by hydraulic fluid mouth to pressure vessel
Inside it is passed through a certain amount of fluid；
（3）Heater will be heated sample and solution by heated pressure container；
（4）When being interacted at different temperatures by the chemical solution of optical measuring system observation sample and different pressures
Micro- white light picture and microphotogram under high temperature high confining pressure.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention, therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (4)
- The experimental rig 1. a kind of high temperature high confining pressure fluid-solid interacts, it is characterised in that：Including pressure vessel（2）, it is described Pressure vessel（2）The axial depression bar of two symmetrically sealed is provided with horizontal direction（3,4）, the two axial depression bar（3,4）Between put Put sample（5）, the pressure vessel（2）It is socketed with heated solution and sample outside（5）Heater（6）, its surface is provided with Hydraulic fluid mouth（9）And optical window（10）, the heater（6）It is placed in base（1）Groove（26）It is interior, with pressure vessel（2） Contact surface is provided with temperature sensor（29）, the hydraulic fluid mouth（9）It is communicated to sample（5）Lay down location, the optical window（10） Face sample（5）Center, and observation sample is installed（5）The optical measuring system of spectrum（30）；Left side depression bar（3）Outer end connects Loading device（7）, loading device（7）It is fixedly attached to base（1）On, loading device（7）Including reinforcing screw（18）And switching Part（19）, reinforce screw（18）Can spiral be movably attached in base（1）In side wall, its thread head center is connected with adaptor （19）, adaptor（19）End set has universal ball end（20）, universal ball end（20）Transfer force to left side depression bar（3）, right side Adjusting screw（25）It is connected to base（1）On, it connects right side depression bar（4）One end is provided with bulb（43）.
- A kind of 2. high temperature high confining pressure fluid-solid interaction experimental rig according to claim 1, it is characterised in that： The temperature sensor（29）, heater（6）, optical measuring system（30）Controller is connected to, controller is also associated with liquid Pressure sensor and hydraulic pump, and host computer is wired to, hydraulic fluid mouth（9）Hydraulic pump is connected to by pipeline（37）, institute State hydraulic pump（37）Liquid reserve tank is connected to by pipeline（36）, hydraulic fluid mouth（9）With hydraulic pump（37）Four are provided with connecting pipe Port valve（38）And flow stop valve one（41）, four-way valve（38）Another two-port connects hydrostatic sensor respectively（39）And relief valve （40）, hydraulic pump（37）With liquid reserve tank（36）The pipeline enclosure of connection is provided with flow stop valve two（42）.
- A kind of 3. high temperature high confining pressure fluid-solid interaction experimental rig according to claim 1, it is characterised in that： Optical window（10）First through hole is communicated including face（14）, the second through hole（15）, hyalomere（13）And third through-hole（16）, institute State first through hole（14）It is arranged on pressure vessel（2）On, second through hole（15）It is arranged on heater（6）On, described Three through holes（16）It is arranged on base（1）In side wall, the hyalomere（13）Pass through briquetting（12）Installed in first through hole（14）Place, It is arranged on briquetting（12）In groove, briquetting（12）Loophole is provided with groove, its outer surface is close to first through hole（14） Place, is arranged on pressure vessel（2）In groove.
- 4. the experiment for the experimental rig that interacted according to a kind of any described high temperature high confining pressure fluid-solids of claim 1-3 Method, it is characterised in that：This method comprises the following steps：（1）Sample is loaded in pressure vessel, fixed sample is sealed by two symmetrical axial depression bars；（2）Compactedness is calculated according to different temperatures, confined pressure condition and pressure vessel containment, led to by hydraulic fluid mouth into pressure vessel Enter a certain amount of fluid；（3）Heater will be heated sample and solution by heated pressure container；（4）At different temperatures, it is high when being interacted by the chemical solution of optical measuring system observation sample and different pressures Micro- white light picture and microphotogram under warm high confining pressure.
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| CN106908170B (en) * | 2017-03-14 | 2019-04-19 | 吉首大学 | A kind of Raman frequency shift temp measuring method and system |
| CN107796959B (en) * | 2017-10-13 | 2019-10-29 | 中国科学院地球化学研究所 | Different oxygen fugacity in-situ control methods in a kind of diamond anvil cell electrical measurement |
| CN109682937B (en) * | 2019-03-04 | 2024-02-06 | 中国科学院地球化学研究所 | Large-cavity high-temperature high-pressure gas-liquid two-phase flow experimental device and experimental method |
| CN109738594B (en) * | 2019-03-04 | 2023-09-01 | 中国科学院地球化学研究所 | Hydrothermal large-cavity high-temperature high-pressure flow experimental device and experimental method |
| CN109731531B (en) * | 2019-03-04 | 2024-01-23 | 中国科学院地球化学研究所 | Hydrothermal large-cavity high-temperature high-pressure experimental device and experimental method |
| CN112403393B (en) * | 2020-12-17 | 2021-12-31 | 吉林大学 | High-temperature and high-pressure resistant in-situ optical observation reaction kettle shell |
| CN112403392B (en) * | 2020-12-17 | 2021-10-08 | 吉林大学 | High-temperature high-pressure reaction kettle for in-situ optical measurement of large-capacity liquid environment |
| CN113848171B (en) * | 2021-05-26 | 2022-08-26 | 国家电投集团科学技术研究院有限公司 | In-situ optical measuring device for simulating pressurized water reactor loop water environment |
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| FR2785680B1 (en) * | 1998-11-09 | 2000-12-08 | Inst Francais Du Petrole | DEVICE FOR TESTING ROCK SAMPLES AT RELATIVELY HIGH PRESSURE AND TEMPERATURE |
| CN101718725B (en) * | 2009-12-08 | 2011-09-14 | 中国科学院广州能源研究所 | Device for measuring sample thermo-physical property in situ |
| CN103406070A (en) * | 2013-08-26 | 2013-11-27 | 中国科学院地球化学研究所 | Multifunctional high-temperature and high-pressure reaction kettle |
| CN104596907B (en) * | 2015-01-28 | 2017-05-31 | 太原理工大学 | Rock big displacement shears the measuring method of seepage flow under HTHP |
| CN105181930A (en) * | 2015-09-07 | 2015-12-23 | 中国地质大学（北京） | Method and device for measuring chemical reaction and physical change of oil rock and water rock |
| CN205786560U (en) * | 2016-06-30 | 2016-12-07 | 中国科学院地球化学研究所 | A kind of high temperature high confining pressure fluid-solid interaction assay device |
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