CN102590253A - High-temperature fused salt synchrotron radiation in-situ research device - Google Patents
High-temperature fused salt synchrotron radiation in-situ research device Download PDFInfo
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- CN102590253A CN102590253A CN2012100144600A CN201210014460A CN102590253A CN 102590253 A CN102590253 A CN 102590253A CN 2012100144600 A CN2012100144600 A CN 2012100144600A CN 201210014460 A CN201210014460 A CN 201210014460A CN 102590253 A CN102590253 A CN 102590253A
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Abstract
The invention discloses a high-temperature fused salt synchrotron radiation in-situ research device. The high-temperature fused salt synchrotron radiation in-situ research device comprises a fused salt test tube, a vacuum furnace, a heating device, a first ionization chamber, a second ionization chamber or a charge coupled device (CCD) detector and an external fluorescence detector, wherein a cavity is formed in the vacuum furnace; an incident window, a transmission window and a fluorescence window are arranged on the furnace wall of the vacuum furnace; the incident window and the transmission window are arranged coaxially and collinearly; the axial line of the fluorescence window is vertical to that of the incident window and/or the transmission window; the heating device is arranged in the cavity of the vacuum furnace and is used for heating the fused salt test tube arranged in the heating device; an incident hole, a transmission hole and a fluorescence hole corresponding to the incident window, the transmission window and the fluorescence window respectively are formed on the heating device; the first ionization chamber corresponding to the incident window is arranged outside the vacuum furnace; the second ionization chamber or the CCD detector corresponding to the transmission window is arranged outside the vacuum furnace; and the external fluorescence detector corresponding to the fluorescence window is arranged outside the vacuum furnace.
Description
Technical field
The present invention relates to a kind of radiation original position research device, relate in particular to a kind of synchrotron radiation original position research device.
Background technology
Along with rapid economic development, energy-consuming and demand are also growing.Greatly developing nuclear energy is one of the valid approach the most that solves high energy consumption.Based on thorium uranium fuel round-robin thorium base nuclear power system have aboundresources, nuke rubbish few, be beneficial to advantages such as nuclear non-proliferation, adaptability be good; Be six kind the 4th generation nuclear reactor one of them, also be one of forward position direction of the current science and technology field of nuclear energy in the world.With other five kinds of rods that use solid fuel act as a fuel the 4th generation nuclear reactor different, its uses high-temp liquid fuse salt to act as a fuel.Because its fuel has flowability, therefore need not use chilled water or the liquid metal cooling medium that acts as a fuel to carry out exchange heat with solid fuel bar, liquid fuel can directly get into and carry out exchange heat in the heat exchanger.But the fuel principal ingredient of MSR is the fluoride molten salt of fission fuel and breed fuel, and following kind: UF is arranged
4, PuF
3, ThF
4In addition, also comprise such as NaF, ZrF in the fluoride molten salt
4, LiF and BeF
2The physicochemical property (for example fusing point, boiling point, flowability, heat conductivity, thermal stability and chemical corrosivity) and moderation of neutrons and the absorption characteristic that are used to improve fused salt Deng composition.In addition, villiaumite also can be brought into play crucial effects at the pyrochemistry processing of nuke rubbish, the cooling and the high-temperature reactor of high-temperature reactor to the heat transfer of hydrogen manufacturing factory.
Mix villiaumite and be operated in 650-1000 ℃ high temperature section, military service under the intense radiation environment, its composition and structure all have material impact to its thermal efficiency, many physicochemical property, moderation of neutrons and absorption characteristic and to the corrosivity of container.For this reason, we need some powerful in-situ testing methods that it is characterized.Third generation synchrotron radiation light source can provide high-quality X ray; For the research of fused salt material provides superior experiment porch; For example (X-ray Absorption Fine Structure is called for short: the sign (f electronics and the valent state that XAFS) are used to study molten salt mixture intermediate ion kind and structure the X ray absorption fine structure; Partial structurtes comprise coordination number, bond distance, bond angle and interionic distance etc.; Composition, temperature and oxidation state are to influence of molten salt nature etc.); X-ray diffraction is used for structural characterization; (Small-Angle X-ray Scattering is called for short: SAXS) be used for characterizing network structure, melt crystallization crumb structure granularity and the shape and the evolution thereof etc. of high-temperature fusant low-angle scattering of X-rays; The sigmatron scattering salt coordination environment research etc. that can be used for fissioning.High-temperature molten salt synchrotron radiation original position research device is that above-mentioned these means of testing provide a reliable platform; It can utilize method original positions such as XAFS, low-angle scattering of X-rays and diffraction, inelastic scattering to obtain information such as fused salt intermediate ion kind, chemical valence state and structure, changes in the fused salt physicochemical property of understanding different component, aspects such as the purification of the valence state control of corrosion mechanism, fuel salt and the fission product thereof of structured material in fused salt and dissolving and fused salt and regeneration technology process optimization bring into play irreplaceable fundamental role.
High-temperature molten salt synchrotron radiation original position research device is equally applicable to except villiaumite; The research of high-temperature fusants such as chlorate of the same clan, Bromide and iodized salt and carbonate and silicate; The kind that comprises metal in the hydrothermal fluid in the geochemistry subject forms and the mineral dissolution degree; The mineral deposit is studied and is reconnoitred and geothermal system research, and the chemical engineering system (as, molten salt electrolysis of metals is smelted and refining; Hydrometallurgy is electrolytical fuel cell and accumulator etc. with fused salt), coenocorrelation research etc.For example, obtain the stoichiometry of metal composite in the hydrothermal fluid and dissolving, transmission and the precipitation process that stable information helps to understand metal in the hydrothermal system.
But; The high-temperature molten salt in-situ test is faced with some challenges at present; It comprises that working temperature is up to 1000 ℃ of high temperature, strong fused salt corrosion, moisture absorption and melt volatilization etc.; Therefore necessarily require high-temperature molten salt synchrotron radiation original position research device to have for avoiding evaporating and the high-air-tightness required with ambient atmospheric reactions, with and the compatibility of heating system and peripheral experimental provision.
First difficulty that the development of this device is run into is exactly the selection of high temperature resistant molten salt corrosion material: with the fluoride salt of fusion is that the high-temperature molten salt of representative has strong corrosivity; All fluoride salts at high temperature very easily react with oxygen, therefore in the material that directly contacts with it, should avoid the existence of oxide.For this reason, it is difficult the fluoride salt of fusion being applied to industry.But according to the experience accumulation of using fluoride salt, nickel-base alloy, refractory metal, glass carbon (vitreous carbon), (for example, SiC and AlN) such as boron nitride and anaerobic potteries is considered to that the fluoride salt of fusion is had enough stability.Take all factors into consideration refractory salt corrosion property and penetrability, boron nitride is one and selects preferably.In addition, glass carbon has the advantage of low diffraction undesired signal when doing SAXS and low angle diffraction, but its price is expensive more many than pyrolysis boron nitride.
France and Japan carry out the work in this field earlier.Research group (A.Rollet, C.Bessada, the Y.Auger of France; P.Melin; M.Gailhanou D.Thiaudiere) is called " Nuclear Instruments and Methods in Physics Research B " (Vol.226,2004 in name; A kind of high-temperature molten salt synchrotron radiation original position research device is disclosed in the document 447-452 page or leaf); It adopts the insertion slot type design, and core component comprises a pyrolytic boron nitride sample cell, and the raw material of its loading is the pyrolytic boron nitride of high-purity, low-porosity, high heat conductance; The test disk, its mixed-powder compacting by certain proportion villiaumite and BN powder forms, and the fusion villiaumite is adsorbed by the boron nitride matrix.Design safety is good like this, and it is comparatively convenient that sample is installed with replacing.
Tokyo research group of engineering institute (H.Matsuura, S.Watanabe, H.Akatsuka; Y.Okamoto A.K.Adya) is called " Journal of Fluorine Chemistry " (Vol.130,2009 in name; A kind of high-temperature molten salt synchrotron radiation original position research device is disclosed in the document 53-60 page or leaf); Two alumina ceramic plates of its tubbiness stove heating element for twining with Pt-Rh20% precious metal alloys heater strip, potsherd and light path parallel are stood, and the thermal efficiency is lower.Basic with French consistent of its sample cell.Adopt Woelm Alumina/monox in heat insulation and water-cooled aluminium shell in heat radiation, be lower than safety value with working temperature and the environment temperature that guarantees exterior window.Vacuum drying oven cavity inner wall auxiliary heat shielding material is nickel foil or aluminium foil, and exterior window is
Kapton that has plated the aluminium film.Adopt (R type thermopair) platinum-13rhodium-platinum thermocouple thermometric and temperature control.Stove is manufactured and designed by Rigaku Corp. (Japanese Co., Ltd. of science), and its great advantage is for ease of varying and maintenance and repair.
Though the device of above-mentioned two research groups all has some advantages; But there are two main problems in their design: the one, and it is the method for skeleton absorbing high temp fused salt that their sample cell all adopts with high-melting-point BN powder; This moment, fused salt was filminess; Have bigger surface tension effects, this has just destroyed the virgin state of fused salt probably, thereby introduces illusion; The 2nd, there is not the fluorescence detection pattern.Mainly according to the weight percent content of element to be measured in the sample, content should adopt transmission method more than 10% in the selection of XAFS high temperature experimental technique; Content then need adopt fluorescence XAFS method below 10%.It is thus clear that, when the weight percent content of the element to be measured in the sample less than 10% and even when being merely tens of ppm magnitude, said apparatus can't be tested it.
Summary of the invention
The purpose of this invention is to provide a kind of high-temperature molten salt synchrotron radiation original position research device, this device should detect the liquid fused salt of larger volume, but also should increase the fluorescence detection pattern; In addition, this device also should have bigger search angle, and should heat equably sample, thereby satisfies the requirement of various tests.
According to the purpose of foregoing invention, the present invention proposes a kind of high-temperature molten salt synchrotron radiation original position research device, it comprises:
One fused salt test tube;
One vacuum drying oven; It in it cavity; Offer an incidence window, a transmission window and a fluorescence window on the furnace wall of vacuum drying oven, wherein incidence window and the coaxial conllinear setting of transmission window, the axis normal of the axis of fluorescence window and incidence window and/or transmission window;
One heating arrangement, it is located in the cavity of vacuum drying oven, be used for the fused salt test tube of being located in it is heated, heating arrangement be provided with incidence window, transmission window and fluorescence window corresponding respectively one go into perforation, a beam orifice and a fluorescence aperture;
One first ionization chamber, its corresponding incidence window is located at the outside of vacuum drying oven, and an incident X-ray is successively through first ionization chamber, incidence window with go into perforation and be radiated on the invisible spectro sample of fused salt;
One second ionization chamber or a ccd detector, its corresponding transmission window is located at the outside of vacuum drying oven, in order to collect the transmission signal corresponding with the incident X-ray;
One fluorescent probe, its corresponding fluorescence window is located at the outside of vacuum drying oven, in order to collect the fluorescence signal corresponding with the incident X-ray.
When adopting the present technique scheme to test, sample is placed in the fused salt test tube, and the fused salt test tube is placed in the vacuum drying oven, and through heating arrangement it is evenly heated.The incident X-ray is successively through first ionization chamber, incidence window with go into perforation and be radiated on the invisible spectro sample of fused salt; The incident X-ray passes through beam orifice, transmission window successively through the transmission signal of sample, is radiated at second ionization chamber or ccd detector, and second ionization chamber or ccd detector are collected transmission signal so that it is carried out subsequent analysis; The incident X-ray passes through fluorescence aperture, fluorescence window successively through the fluorescence signal of sample, is radiated on the fluorescent probe, and fluorescent probe is collected fluorescence signal so that it is carried out subsequent analysis.
Preferably, in above-mentioned high-temperature molten salt synchrotron radiation original position research device, the material of fused salt test tube is pyrolytic boron nitride or glass carbon.These two kinds of materials all have the advantage of purity height, temperature conductivity height, good leak tightness.Glass carbon has the advantage of low diffraction undesired signal when doing the test of SAXS and low angle diffraction, but its price is high more a lot of than pyrolysis boron nitride.Two kinds of materials respectively have quality, can require to select according to actual experiment.
Preferably, in above-mentioned high-temperature molten salt synchrotron radiation original position research device, also comprise:
One positioning table, it is set to and can on X, Y, three directions of Z, moves, and can rotate around a rotating shaft, and vacuum drying oven is arranged on the positioning table; Positioning table can be adjusted the relative position of sample and incident X-ray light path; And guarantee that transmission signal, fluorescence signal can shine on second ionization chamber or ccd detector and the fluorescent probe through transmission window, fluorescence window respectively; Thereby make the experimenter to carry out test experiments easily with incident X-ray, second ionization chamber or ccd detector, fluorescent probe registration coupon;
One helium feeder, it is connected with vacuum drying oven through a helium air intake opening of being located on the vacuum drying oven, and this helium feeder can provide high-purity helium atmosphere protection for sample test;
One vacuum pump dolly, it is connected with vacuum drying oven through a bleeding point of being located on the vacuum drying oven; The vacuum pump dolly can make test experiments in vacuum environment, carry out, and perhaps before charging into helium, a purer vacuum environment is provided, and in addition, this vacuum pump dolly also has mobile advantage easily;
One attemperating unit, it is connected with heating arrangement, and the closed-loop control heating arrangement is to the heating-up temperature of fused salt test tube, and attemperating unit can accurately be controlled the temperature of sample;
The furnace wall of vacuum drying oven is provided with several water-cooled torus; One chilled water circulation appearance is connected with each water-cooled torus conducting with at least one coolant outlet through at least one cooling water inlet of being located on the vacuum drying oven, and cold torus can guarantee that shell and window are under the safe working temperature.That is to say that adopt encircling type large tracts of land side and the design of top interlayer water-cooled in the present technique scheme, double-deck water-cooled vacuum drying oven sidewall of bell-jar and roof are bilayer, the void layer between the two-layer alloy wall is the cooling water path of large tracts of land encircling type.
In above-mentioned high-temperature molten salt synchrotron radiation original position research device, be equipped with on incidence window, transmission window and the fluorescence window one be used for X-ray film, film is the pure beryllium film or the Kapton of aluminizer.Pure beryllium film is better to the penetrability of X-ray, and its sealing is strong, intensity is high, thereby is easy to guarantee vacuum environment, and comparatively durable in use, but its cost is very high, and has certain toxicity, needs careful operation; The Kapton cost of aluminizer is lower, nontoxic, also can tolerate the temperature about 200 ℃, but it is prone to the gas leakage of breaking.Two kinds of films respectively have quality, can require to select according to actual experiment.
Preferably, in above-mentioned high-temperature molten salt synchrotron radiation original position research device, going into perforation is cylindrical hole, and beam orifice and fluorescence aperture are bellmouth.Bellmouth is positioned at the inwall of heating arrangement than an end of minor diameter, and a larger-diameter end is positioned at the outer wall of heating arrangement, thereby can obtain bigger search angle.
Preferably, in above-mentioned high-temperature molten salt synchrotron radiation original position research device, heating arrangement comprises: a heating base, and it is cylindrical basically; Its axial direction of heating base upper edge offers a through hole, in order to place the fused salt test tube; The test tube below is lined with hot pressed boron height control rod in the through hole.The hot pressed boron height control rod group that height control is formed through different length realizes.So design is convenient to adjust the height of fused salt liquid level and is cleared up the fused salt (the fused salt plug of avoiding leaking amasss) that leaks behind the test tube cracking.Its axial direction of heating base upper edge also offers a thermocouple jack; Have the ring groove of a circumferential direction on the outer circumference surface of heating base upper and lower; Be respectively equipped with a heating ring in each ring groove; Heating ring comprises that annular array that the ceramic insulating tube of vertical discharging forms and bending navigate within the metallic resistance silk among the ceramic insulating tube up and down, and ceramic insulating tube has the notch that the resistive filament winding worked in two ends up and down.
Preferably, in above-mentioned high-temperature molten salt synchrotron radiation original position research device, the material of heating base is a hot pressed boron.Though the hot pressed boron porosity is high, impurity is many; Be not suitable for as the container that contact with fused salt, but its be easy to process, price is low, temperature conductivity is greater than 20W/ (mK); Be ten times of conventional ceramic, so can be processed into the complex parts that thermal stress is low, thermal shock resistance is good.
Preferably, in above-mentioned high-temperature molten salt synchrotron radiation original position research device, tinsel is Pt-20%Rh alloying metal silk, molybdenum filament or tantalum wire.Pt-20%Rh alloying metal silk has fusing point height, anti-oxidant, good toughness, long advantage of life-span, but it costs an arm and a leg; Molybdenum filament and tantalum wire low price, but the life-span is short partially.These tinsels respectively possess some good points, and can require to select according to actual experiment.
Preferably, in above-mentioned high-temperature molten salt synchrotron radiation original position research device, the bottom surface of vacuum drying oven is provided with a heat insulation base, and the heat insulation base is provided with a groove, and heating arrangement is arranged in the groove.The heat insulation base except that intercept heat to the positioning table transmission that is connected with the bottom, also play the location heating arrangement effect, thereby sample is positioned.
Preferably, in above-mentioned high-temperature molten salt synchrotron radiation original position research device, the internal diameter of fused salt test tube is 1.5-4.5mm, and its external diameter is 2-5mm.Regulate the caliber of fused salt test tube and can realize the adjusting of sample the absorption coefficient of X-ray.
High-temperature molten salt synchrotron radiation original position research device of the present invention has the following advantages:
(1) high-temperature molten salt synchrotron radiation original position research device of the present invention can detect the liquid fused salt of larger volume, and to adopt with high-melting-point BN powder be the phenomenon that the sample of skeleton absorbing high temp fused salt can be introduced illusion thereby eliminated;
(2) high-temperature molten salt synchrotron radiation original position research device of the present invention has the fluorescence detection pattern, thereby can test less than 10% sample the weight percent content of element to be measured;
(3) high-temperature molten salt synchrotron radiation original position research device of the present invention have that search angle is higher, good airproof performance, the advantage that can evenly heat and can in the environment of vacuum or helium atmosphere, test sample, thereby make it can satisfy the requirement of various tests.
Description of drawings
Fig. 1 is the perspective view of high-temperature molten salt synchrotron radiation original position research device of the present invention under a kind of embodiment.
Fig. 2 is the high-temperature molten salt synchrotron radiation original position research device of the present invention syndeton synoptic diagram of each experimental provision in one embodiment.
Fig. 3 is the high-temperature molten salt synchrotron radiation original position research device of the present invention perspective view of vacuum drying oven in one embodiment.
Fig. 4 is the high-temperature molten salt synchrotron radiation original position research device of the present invention cross sectional side view of vacuum drying oven in one embodiment.
Fig. 5 is the high-temperature molten salt synchrotron radiation original position research device of the present invention cross sectional plan view of vacuum drying oven in one embodiment.
Fig. 6 is the high-temperature molten salt synchrotron radiation original position research device of the present invention perspective view of heating arrangement in one embodiment.
Fig. 7 is the high-temperature molten salt synchrotron radiation original position research device of the present invention planar structure synoptic diagram of heating arrangement in one embodiment.
Fig. 8 is the high-temperature molten salt synchrotron radiation original position research device of the present invention vertical view of heating arrangement in one embodiment.
Fig. 9 is the cut-open view of E-E face among Fig. 7.
Figure 10 is the cut-open view of G-G face among Fig. 8.
Figure 11 is the high-temperature molten salt synchrotron radiation original position research device of the present invention perspective view of the heating ring of heating arrangement in one embodiment.
Embodiment
To combine Figure of description and concrete embodiment that high-temperature molten salt synchrotron radiation original position research device of the present invention is done further detailed description below.
Fig. 1 has shown and has invented the structure of described high-temperature molten salt synchrotron radiation original position research device at present embodiment.As shown in Figure 1, vacuum drying oven 100 is located on the positioning table, is respectively equipped with incidence window, transmission window and fluorescence window on its furnace wall, wherein incidence window and the coaxial conllinear setting of transmission window, the axis normal of the axis of fluorescence window and incidence window and transmission window.Fused salt test tube and heating arrangement are located at the cavity interior (like Fig. 4, shown in Figure 5) of vacuum drying oven 100 supportingly.The position of positioning table adjustment vacuum drying oven 100, it comprises X axial translation positioning table 701, Y axial translation positioning table 702, Z axial translation positioning table 703 and the rotary sample positioning table 704 that connects successively.X, Y, Z axial translation positioning table 701,702,703 can make vacuum drying oven 100 on X, Y, three directions of Z, move, and rotary sample positioning table 704 can make vacuum drying oven rotate around a rotating shaft.First ionization chamber 400, second ionization chamber or ccd detector 500, the corresponding respectively incidence window of fluorescent probe 600, transmission window, fluorescence window are located at the outside of vacuum drying oven 100.Incident X-ray A injects the inner chamber of vacuum drying oven 100 through first ionization chamber 400, and second ionization chamber or ccd detector 500, fluorescent probe 600 receive transmission signal and fluorescence signal through transmission window, fluorescence window respectively.
Fig. 2 has shown the high-temperature molten salt synchrotron radiation original position research device of the present invention syndeton of each experimental provision in the present embodiment.As shown in Figure 2, vacuum drying oven 100 is located on the positioning table 700, and it is connected with helium feeder, chilled water circulation appearance 901, vacuum pump dolly 1001 and attemperating unit 311 respectively.Wherein, The helium feeder comprises helium tank 801, reduction valve 802, the flowmeter 803 that conducting successively connects; Flowmeter 803 is connected with helium air intake opening conducting on the vacuum drying oven 100; This helium feeder provides helium can for vacuum drying oven 100, and it can be experimentized under the environment of helium.Chilled water circulation appearance 901 is through cooling water inlet and coolant outlet on the vacuum drying oven 100, is connected with water-cooled torus conducting in vacuum drying oven 100 housings.Vacuum pump dolly 1001 is connected with bleeding point conducting on vacuum drying oven 100 bells through valve 1002; It can guarantee that vacuum drying oven 100 inside are in the condition of high vacuum degree environment in the 10-2-10-3Pa scope; Vacuum meter 1003 is located on the gas circuit of vacuum pump dolly 1001 and vacuum drying oven 100, in order to detect the vacuum tightness in the stove.Attemperating unit 311 is connected with vacuum drying oven 100 interior heating arrangement and computing machines respectively; It adopts close-loop control mode control heating arrangement that the fused salt test tube is heated; Temperature is controlled in the working temperature of room temperature-1000 ℃, the highlyest is no more than 1100 ℃, its constant temperature precision is ± 1 ℃; Attemperating unit 311 not only can be controlled heating arrangement and sample heated and show on computers and related data also play the effect into the heating arrangement electric energy transmitting.
Fig. 3 has shown the high-temperature molten salt synchrotron radiation original position research device of the present invention external structure of vacuum drying oven in the present embodiment.Fig. 4, Fig. 5 have shown the high-temperature molten salt synchrotron radiation original position research device of the present invention inner structure of vacuum drying oven in the present embodiment respectively.Like Fig. 3, Fig. 4 and shown in Figure 5, vacuum drying oven comprises body of heater 101, bell 102 and switching chassis 103.Wherein, switching chassis 103 is used for being fixedly connected of vacuum drying oven and positioning table.Bell 102 is provided with trip bolt 112, cooling water inlet 109a, the coolant outlet 109b of bleeding point 110, band hanger, also is provided with water-cooled torus 111 in its tegmental wall.Wherein, the trip bolt 112 of band hanger is used for bell 102 and body of heater 101 are sealedly and fixedly connected and are convenient to the lifting and the fine setting location of vacuum drying oven, and bleeding point 110 is connected with the conducting of vacuum pump dolly, in order to the vacuum drying oven inner chamber is evacuated to vacuum; Bleeding point 110 also is provided with a dust plug, is used for when bleeding point 110 is not connected with the vacuum pump dolly, preventing that dust impurity from entering into vacuum drying oven inside.The furnace wall of body of heater 101 is provided with incidence window 104, transmission window 105, fluorescence window 106, cooling water inlet 109a, coolant outlet 109b, and attemperating unit interface 108 and the helium import 113 of being located near attemperating unit interface 108 belows.Helium air intake opening 113 gos deep into to the sample center through stainless-steel tube, closure molecule pump valve door in the time of can at high temperature reaching high vacuum, and crack mechanical pump valve fills helium sample is protected while taking out.Incidence window 104 and transmission window 105 coaxial conllinear settings, the axis normal of the axis of fluorescence window 106 and incidence window 104 and transmission window 105.Incidence window 104, transmission window 105, fluorescence window 106 are equipped with the film that is used for printing opacity, and this film is the Kapton of pure beryllium film or aluminizer.Wherein, helium import 113 is used for being connected with the conducting of helium feeder, thereby realizes to vacuum drying oven helium being provided.The attemperating unit interface is used for being connected with the attemperating unit data, and obtains power supply.Also be provided with some water-cooled torus 111 and cooling water inlet 109a and coolant outlet 109b in the furnace wall of body of heater 101; Chilled water circulation appearance is connected with each water-cooled torus 111 conducting with coolant outlet 109b through cooling water inlet 109a respectively; Form cooling water path, thereby guarantee that vacuum drying oven shell and each window are in safe temperature.The bottom centre of vacuum drying oven inner chamber is provided with a heat insulation base 107 that groove, its except can intercept heat to the positioning table transmission that is connected with the bottom, also play the effect of location heating arrangement, thereby sample positioned.Fused salt test tube 201 is located in the heating arrangement 300, and heating arrangement 300 is fixed in the groove of heat insulation base 107.Hot pressed boron height control rod 203 is used to adjust the height of fused salt liquid level, and the while also is convenient to behind the test tube cracking, take out test tube and clears up leaking fused salt.
Fig. 6 has shown the high-temperature molten salt synchrotron radiation original position research device of the present invention external structure of heating arrangement in the present embodiment.Fig. 7, Fig. 8, Fig. 9, Figure 10 have shown the high-temperature molten salt synchrotron radiation original position research device of the present invention inner structure of heating arrangement in the present embodiment respectively.Like Fig. 6-shown in Figure 10, fused salt test tube 201 is provided with pipe cap 202, and its material is pyrolytic boron nitride or glass carbon, and internal diameter is 1.5-4.5mm, and external diameter is 2-5mm, regulates the caliber of fused salt test tube 201 and can realize the adjusting of sample to the absorption coefficient of X-ray.Heating arrangement comprises heating base 301, thermopair and heating ring 311.Heating base 301 is a right cylinder, and its axial direction of its upper edge offers through hole 306, in order to place fused salt test tube 201; Heating base 301 be provided with incidence window, transmission window, fluorescence window corresponding respectively go into perforation 302, beam orifice 303, fluorescence aperture 304.Wherein, go into perforation 302 and be cylindrical hole, beam orifice 303 is bellmouth with fluorescence aperture 304, and its subtended angle to heating base 301 outsides is 22 °, to obtain bigger search angle.Its axial direction of heating base 301 upper edges also offers thermocouple jack 305, and in order to place thermopair, this thermopair is connected with temperature control equipment.Have the ring groove 307 of circumferential direction on the outer circumference surface of heating base 301 upper and lowers, be respectively equipped with heating ring 311 in each ring groove 307; The bottom of heating base 301 is provided with a locating slot 308 that is complementary with the heat insulation base, in order to heating arrangement is fixed on the heat insulation base.The material of heating base 301 is a hot pressed boron.
Figure 11 has shown the high-temperature molten salt synchrotron radiation original position research device of the present invention structure of the heating ring of heating arrangement in the present embodiment.Heating ring comprises that annular array that the ceramic insulating tube 310 of vertical discharging forms and bending navigate within the metallic resistance silk 309 among the ceramic insulating tube up and down.Ceramic insulating tube has the notch that the resistive filament winding worked in two ends about in the of 310.After putting on the ceramic insulating tube formation array of metallic resistance silk, draw at two ends, closed loop wrapping and heating pedestal.Between metallic resistance silk 309 two ends for avoiding short circuit to stagger up and down and across an insulated porcelain tube.Material wiry can adopt Pt-20%Rh alloying metal silk, molybdenum filament or tantalum wire.
In conjunction with Fig. 1 and Fig. 5, when experimentizing, need advanced luggage appearance, the villiaumite purity of test is not less than 99.9%, and villiaumite is melted, solidifies, grinds to form several micron-sized uniform powder potpourris, packs in the fused salt test tube 201, obtains sample.Dress appearance whole process is all operated in vacuum glove box, and through paraffin or high-purity band enhanced leaktightness, avoids sample to make moist and oxygen uptake.After sample changes vacuum drying oven 100 over to, at room temperature be evacuated to vacuum to cavity earlier, heating paraffin or high-purity band burn off, further is evacuated to 10 more then
-2-10
-3The high vacuum of Pa, and with sample be heated to temperature required begin the test.The fused salt test tube 201 that is mounted with sample is located in the through hole of heating base of heating arrangement 300, and heating arrangement 300 is located in the groove of heat insulation base 107, makes and forms light path B, C, D in vacuum drying oven 100 cavitys; Wherein, light path B successively through first ionization chamber 400, incidence window 104, go into perforation 302, shine on the sample; Light path C passes through beam orifice 303, transmission window 105, second ionization chamber or ccd detector 500 successively from sample; Light path D passes through fluorescence aperture 304, fluorescence window 106, fluorescent probe 600 successively from sample.In test process, incident X-ray A shines on the sample through light path B, and transmission signal that obtains then and fluorescence signal shine on second ionization chamber or ccd detector 500 and the fluorescent probe 600 through light path C and light path D respectively.Second ionization chamber or ccd detector 500 receive transmission signal and fluorescence signal with fluorescent probe 600, so that subsequent analysis.
Be noted that above enumerate be merely specific embodiment of the present invention, obviously the invention is not restricted to above embodiment, many similar variations are arranged thereupon.If those skilled in the art all should belong to protection scope of the present invention from all distortion that content disclosed by the invention directly derives or associates.
Claims (10)
1. high-temperature molten salt synchrotron radiation original position research device, it comprises:
One fused salt test tube;
One vacuum drying oven; It in it cavity; Offer an incidence window, a transmission window and a fluorescence window on the furnace wall of said vacuum drying oven, wherein said incidence window and the coaxial conllinear setting of transmission window, the axis normal of the axis of said fluorescence window and incidence window and/or transmission window;
One heating arrangement; It is located in the cavity of said vacuum drying oven; Be used for the said fused salt test tube of being located in it is heated, said heating arrangement be provided with said incidence window, transmission window and fluorescence window corresponding respectively one go into perforation, a beam orifice and a fluorescence aperture;
One first ionization chamber, its corresponding said incidence window is located at the outside of vacuum drying oven, and an incident X-ray is successively through first ionization chamber, incidence window with go into perforation and be radiated on the invisible spectro sample of fused salt;
One second ionization chamber or a ccd detector, its corresponding said transmission window is located at the outside of vacuum drying oven, in order to collect and the corresponding transmission signal of said incident X-ray;
One fluorescent probe, its corresponding said fluorescence window is located at the outside of vacuum drying oven, in order to collect and the corresponding fluorescence signal of said incident X-ray.
2. high-temperature molten salt synchrotron radiation original position research device as claimed in claim 1 is characterized in that the material of said fused salt test tube is pyrolytic boron nitride or glass carbon.
3. according to claim 1 or claim 2 high-temperature molten salt synchrotron radiation original position research device is characterized in that, also comprises:
One positioning table, it is set to and can on X, Y, three directions of Z, moves, and can rotate around a rotating shaft, and said vacuum drying oven is arranged on the positioning table;
One helium feeder, it is connected with said vacuum drying oven through a helium air intake opening of being located on the vacuum drying oven;
One vacuum pump dolly, it is connected with said vacuum drying oven through a bleeding point of being located on the vacuum drying oven;
One attemperating unit, it is connected with said heating arrangement, and the closed-loop control heating arrangement is to the heating-up temperature of fused salt test tube;
The furnace wall of said vacuum drying oven is provided with several water-cooled torus, and a chilled water circulation appearance is connected with each water-cooled torus conducting with at least one coolant outlet through at least one cooling water inlet of being located on the vacuum drying oven.
4. according to claim 1 or claim 2 high-temperature molten salt synchrotron radiation original position research device; It is characterized in that; Be equipped with on said incidence window, transmission window and the fluorescence window one be used for X-ray film, said film is the pure beryllium film or the Kapton of aluminizer.
5. according to claim 1 or claim 2 high-temperature molten salt synchrotron radiation original position research device is characterized in that, said to go into perforation be cylindrical hole, and said beam orifice and fluorescence aperture are bellmouth.
6. according to claim 1 or claim 2 high-temperature molten salt synchrotron radiation original position research device is characterized in that said heating arrangement comprises: a heating base, and it is cylindrical basically; Its axial direction of said heating base upper edge offers a through hole, and in order to place said fused salt test tube, the bottom of said through hole is provided with hot pressed boron height control rod; Its axial direction of said heating base upper edge also offers a thermocouple jack; Have the ring groove of a circumferential direction on the outer circumference surface of said heating base upper and lower; Be respectively equipped with a heating ring in said each ring groove; Said heating ring comprises that annular array that the ceramic insulating tube of vertical discharging forms and bending navigate within the metallic resistance silk among the ceramic insulating tube up and down, and said ceramic insulating tube has the notch that the resistive filament winding worked in two ends up and down.
7. high-temperature molten salt synchrotron radiation original position research device as claimed in claim 6 is characterized in that the material of said heating base is a hot pressed boron.
8. high-temperature molten salt synchrotron radiation original position research device as claimed in claim 6 is characterized in that said tinsel is Pt-20%Rh alloying metal silk, molybdenum filament or tantalum wire.
9. according to claim 1 or claim 2 high-temperature molten salt synchrotron radiation original position research device is characterized in that the bottom surface of said vacuum drying oven is provided with a heat insulation base, and said heat insulation base is provided with a groove, and said heating arrangement is arranged in the said groove.
10. according to claim 1 or claim 2 high-temperature molten salt synchrotron radiation original position research device is characterized in that the internal diameter of said fused salt test tube is 1.5-4.5mm, and its external diameter is 2-5mm.
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