CN202471625U - Tubular high-temperature molten salt synchrotron radiation in-situ research device - Google Patents
Tubular high-temperature molten salt synchrotron radiation in-situ research device Download PDFInfo
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- CN202471625U CN202471625U CN2012200239540U CN201220023954U CN202471625U CN 202471625 U CN202471625 U CN 202471625U CN 2012200239540 U CN2012200239540 U CN 2012200239540U CN 201220023954 U CN201220023954 U CN 201220023954U CN 202471625 U CN202471625 U CN 202471625U
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Abstract
The utility model discloses a tubular high-temperature molten salt synchrotron radiation in-situ research device, which comprises a heating furnace, a vacuum tube, a first ionization chamber and a second ionization chamber or a charge coupled device (CCD) detector, wherein the vacuum tube is arranged in the heating furnace and is provided with an incident window and a transmitting window respectively at two ends along the axial direction; the incident window and the transmitting window are arranged opposite to each other; a sample clamping device is arranged in the vacuum tube; the first ionization chamber is formed outside the vacuum tube corresponding to the incident window; and the second ionization chamber or the CCD detector is arranged outside the vacuum tube corresponding to the transmitting window. The tubular high-temperature molten salt synchrotron radiation in-situ research device has the advantages that according to the research device, the manufacturing cost and the using cost of the research device are effectively reduced; the research device provides comprehensive atmosphere protection and a vacuum environment for a sample, and the testing reliability is improved; and due to the research device, the safety of an experiment for testing radioactive samples can be improved, and the probability of radioactive contamination is effectively reduced.
Description
Technical field
The utility model relates to a kind of research device, relates in particular to a kind of synchrotron radiation original position research device.
Background technology
Villiaumite has important use in the nuclear energy research and development.For example, villiaumite is in core status because of its fuel and thermal barrier as fusedsalt reactor in this heap type.In addition, the effect that villiaumite also can be handled in the pyrochemistry of nuke rubbish, performance is difficult to substitute in the cooling of high-temperature reactor and high-temperature reactor to the heat transfer of hydrogen manufacturing factory.
Mix villiaumite and be operated in 650-1000 ℃ high temperature section, 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 high-temp in-situ means of testing that it is characterized.Third generation synchrotron radiation light source because of have the brightness height, collimation is good and penetrability is strong etc., and advantage is particularly suitable for in-situ test; Superior experiment porch can be provided for the research of fused salt material; 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 fused salt phase transformation and the structural characterization under the different temperatures; (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 of high-temperature fusant small angle X ray scattering; X ray inelastic scattering technology is used to band structure of surveying fused salt etc.Tubular type high-temperature molten salt synchrotron radiation original position research device is that above-mentioned these means of testing provide a reliable platform.
Tubular type 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, the stoichiometry and the stable information of metal composite is to understand the prerequisite of the dissolving of metal in the hydrothermal system, transmission and precipitation process in the acquisition hydrothermal fluid.Tubular type high-temperature molten salt synchrotron radiation original position research device provides necessary means for this type research.
But; The high-temperature molten salt in-situ test is faced with some challenges at present; It comprises the high temperature of working temperature up to 1000 ℃, strong fused salt corrosion, moisture absorption, melt volatilization and narrow space restriction etc.; Therefore require the original position research device small and exquisite, and have high-air-tightness, heating and cooling system efficiently and with the favorable compatibility of 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 with the oxygen reaction, therefore in the existence that directly should avoid oxide with it in the material of contact.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, X ray penetrability and cost and processability, boron nitride is one and selects preferably.
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; The 447-452 page or leaf) disclose a kind of tubular type high-temperature molten salt synchrotron radiation original position research device in the document, it has at first designed pyrolytic boron nitride villiaumite sample cell.Pyrolytic boron nitride has the advantage of high-purity, low-porosity and high heat conductance, and being processed into behind the holding piece that the centre is the thin-walled blind hole to provide the good closed atmosphere protection and the test condition of uniformity of temperature profile for the sample testing disk.The test disk is formed by the compacting of the mixed-powder of certain proportion villiaumite and BN powder, and fusion villiaumite quilt still is that solid-state high-melting-point boron nitride matrix is adsorbed when high temperature test.Holding piece is fastening through stainless steel screw.After this sample cell is mixed the heating arrangement of insertion slot type, make sample install and change convenient, experiment safe.Yet there is a big drawback in this design, the original just very expensive blind hole pyrolytic boron nitride holding piece of cost of material, and its thin-walled place thickness has only 0.2mm, very easily breaks, and therefore this holding piece is difficult to processing, and yield rate is low; In addition, because the holding piece thin-walled once can receive the pollution of fused salt after the test, thereby can not reuse, and then cause very high experimental cost.
Tokyo (the H.Matsuura of research group of engineering institute; S.Watanabe, H.Akatsuka, Y.Okamoto; A.K.Adya) be called " Journal of Fluorine Chemistry " (Vol.130 in name; A kind of tubular type high-temperature molten salt synchrotron radiation original position research device is disclosed in the document 2009, the 53-60 pages or leaves), in the tubbiness vacuum drying oven of its design; Flat narrow rectangle light hole is offered in trial in the center of holding piece, adopted higher boron nitride/villiaumite ratio to suppress mixed-powder test disk again.Therefore, when villiaumite at high temperature melts,, can not overflow even without the support of thin-walled because it is adsorbed to receive abundant solid-state nitration boron yet.And the holding piece of this through hole is prone to processing, so its experimental cost is lower.But their light hole of design is flat narrow, and is bigger with the contact area of sample disk, still can be polluted when therefore reusing.What is more important is a through hole owing to what open, and sample can contact and can not get protection unavoidably with moisture with surrounding air in the process that shifts out the vacuum glove box and the vacuum drying oven of packing into.Their the tubbiness vacuum drying oven of design is an internal heat type, and is also comparatively huge and heavy, is not easy to whole moving in the glove box.In addition, its heater strip that adopts is Pt-Rh20% precious metal alloys silks, and is though the life-span is long, with high costs.Heater strip is wrapped on two sample cell alumina ceramic plates, and sample cell is clipped in the middle, and potsherd and light path parallel are stood, and positive vertical with sample cell.It is heat insulation to adopt Woelm Alumina/monox to be used for, and adopts interlayer water-cooled aluminum alloy casing to be used for heat radiation, can guarantee that the working temperature of exterior window and environment temperature are lower than safety value.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.Thermopair adopts (R type thermopair) platinum rhodium 13-platinum, in order to thermometric and temperature control.This technical scheme great advantage is for ease of varying and maintenance and repair.But its drawback is also very obvious, and promptly tubbiness vacuum drying oven cost of manufacture is high, and the thermal efficiency is low, and can not thorough inert atmosphere or vacuum protection be provided for sample, is not suitable for the test of environment sensitive sample.
Summary of the invention
The purpose of the utility model provides a kind of tubular type high-temperature molten salt synchrotron radiation original position research device; This research device should be when reducing testing cost; Thorough atmosphere protection of sample and vacuum environment are provided, and should heat equably sample.
According to the purpose of above-mentioned utility model, the utility model provides a kind of tubular type high-temperature molten salt synchrotron radiation original position research device, it comprises:
One heating furnace;
One vacuum tube, it is located in the heating furnace, and vacuum tube is respectively equipped with an incidence window and a transmission window along the two ends of its axial direction, and incidence window and transmission window are corresponding to be provided with; Be provided with a sample holder device in the vacuum tube;
One first ionization chamber, its corresponding incidence window is located at the outside of vacuum tube;
One second ionization chamber or a ccd detector, its corresponding transmission window is located at the outside of vacuum tube.
When adopting the present technique scheme to test, sample is loaded on the sample holder device, and the sample holder device is placed in the vacuum tube, and through heating furnace it is evenly heated.The incident X-ray is radiated on the sample on the sample holder device through first ionization chamber, incidence window successively; The incident X-ray passes through 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.
Preferably, in above-mentioned tubular type high-temperature molten salt synchrotron radiation original position research device, vacuum tube comprises:
One quartz ampoule is provided with a sample steady arm in it, the sample holder device is located on the sample steady arm;
Two water collars; Be connected with the sealed at both ends of quartz ampoule respectively; Be respectively equipped with helium inlet and helium outlet on two water collars; Also be provided with a chilled water torus on the jacket wall of each water collar, also be respectively equipped with a cooling water inlet and a coolant outlet on each water collar, the cooling water inlet on each water collar and coolant outlet are connected with chilled water torus conducting on this cooling jacket;
Two flanges are connected with two water collars respectively, and incidence window and transmission window are located at respectively on two flanges.
Vacuum tube advantages of small volume in the present technique scheme, in light weight, can with the hands hold up easily, put into vacuum glove box and adorn appearance, operation such as vary, omnidistance all in the inert atmosphere protection or vacuum environment of strictness to guarantee sample.
Preferably, in above-mentioned tubular type 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 heating furnace 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 can shine on second ionization chamber or the ccd detector through transmission window; Thereby make the experimenter to carry out test experiments easily with incident X-ray, second ionization chamber or ccd detector registration coupon.
One helium feeder, it is connected with the helium inlet through pipeline, and this pipeline is provided with a gas admittance valve; The helium feeder can make test experiments in helium atmosphere, carry out.
One vacuum pump dolly, it is connected with the helium outlet through pipeline, and this pipeline is provided with a vent valve; 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.
One attemperating unit, it is connected with heating furnace, and the closed-loop control heating furnace is to the heating-up temperature of vacuum tube; Attemperating unit can accurately be controlled the temperature of sample.
One chilled water circulation appearance, it is connected with coolant outlet with each cooling water inlet.Chilled water circulation appearance can provide stable cooling circulating water for water collar, in time takes away the heat that heating furnace distributes from the quartz ampoule two ends, guarantees the safe working temperature that forms and stove are outer.
Preferably, in above-mentioned tubular type high-temperature molten salt synchrotron radiation original position research device, also be provided with a thermopair in the vacuum tube, it is connected with attemperating unit.Thermopair is in order to measuring the temperature of sample, and feeds back to attemperating unit.
Preferably, in above-mentioned tubular type high-temperature molten salt synchrotron radiation original position research device, heating furnace is the openable heating furnace, and it comprises a top and a bottom that is hinged, and top or bottom can be rotated to open or closed heating furnace around jointed shaft.The type of heating of heating furnace is an external-heat, and it can carry out the heating of uniform high-efficiency ground to vacuum tube.In addition, the heater strip of heating furnace can be selected comparatively cheap material for use, to save cost.
Preferably, in above-mentioned tubular type high-temperature molten salt synchrotron radiation original position research device, the sample holder device comprises:
First holding piece and second holding piece that are provided with in pairs; The center of first holding piece has first through hole; Be uniform-distribution with several fastener holes around first through hole; The center of second holding piece has a shoulder hole, be uniform-distribution with around the shoulder hole several with first holding piece on the corresponding fastener hole of fastener hole, shoulder hole comprises successively a macropore and an aperture of linking; The diameter of macropore is set to the external diameter greater than sample, and the diameter of first through hole and aperture is set to the external diameter less than sample;
Several screws, correspondence is passed the fastener hole on first holding piece and second holding piece respectively;
The nut that several and each screw are provided with in pairs is connected with each screw respectively.
In the present technique scheme; Sample is embedded in the macropore of shoulder hole of second holding piece; Through screw, nut and corresponding fastener hole first holding piece and second holding piece are fixed together again, thereby sample is fixed in the macropore between first through hole and the aperture.Because the diameter in sample testing zone is generally less than 5mm; Therefore the sample testing zone can keep certain distance with the surface of contact (periphery) of two holding piece fixing sample on sample; Thereby make that two holding pieces are reusable after easy clean, and can not pollute sample.Adopt this technical scheme can effectively practice thrift the cost of test experiments.
Preferably, in above-mentioned tubular type high-temperature molten salt synchrotron radiation original position research device, the sample steady arm has a deep-slotted chip breaker, also be provided with on the internal groove side wall of deep-slotted chip breaker one with the locating slot of sample holder device coupling, sample holder device correspondence is located in this locating slot.
Alternatively; In the another kind of embodiment of above-mentioned tubular type high-temperature molten salt synchrotron radiation original position research device; The sample holder device comprises: respectively be provided with a blind hole on first holding piece and second holding piece that are provided with in pairs, corresponding of said first holding piece and second holding piece, be uniform-distribution with several fastener holes around said each blind hole; The somewhat larger in diameter of said blind hole also respectively has the optical transmission window of a correspondence in the external diameter of sample on said first holding piece and second holding piece;
Several screws, correspondence is passed the fastener hole on first holding piece and second holding piece respectively;
The nut that several and said each screw are provided with in pairs is connected with said each screw respectively.
In above-mentioned tubular type high-temperature molten salt synchrotron radiation original position research device, said sample holder device is arranged with the tank body of a sealing outward, and the bottom of said tank body and top all have window.
Preferably, said tank body comprises a can body and the cover that is threaded with said can body.
When sample is radioactivity fused salt sample; In order to prevent to reveal; The sample holder device is set to said structure; Can be so that sample place in process of the test in first holding piece and the triple barriers of second holding piece, sealed tube body and vacuum tube, thus the probability that radiomaterial leaks and pollutes obviously reduced.
The described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device has the following advantages:
(1) the described technical scheme of the utility model effectively reduces the manufacturing and the use cost of research device;
(2) the described research device of the utility model provides thorough atmosphere protection of sample and vacuum environment, has improved the reliability of test experiments;
(3) the described research device of the utility model can also improve the security to the experiment of radioactivity sample testing, effectively reduces its alpha-contamination probability.
Description of drawings
Fig. 1 is the syndeton synoptic diagram of the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device under a kind of embodiment.
Fig. 2 is the perspective view of the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device under a kind of embodiment.
Fig. 3 is the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device perspective view of vacuum tube in one embodiment.
Fig. 4 is the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device structural representation of water collar in one embodiment.
Fig. 5 is the cross section view of A-A face among Fig. 4.
Fig. 6 is the cross section view of B-B face among Fig. 4.
Fig. 7 is the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device split structural drawing of sample holder device in one embodiment.
Fig. 8 is the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device structural representation of second holding piece in one embodiment.
Fig. 9 is the cross section view of C-C face among Fig. 8.
Figure 10 is the local enlarged diagram at L place among Fig. 9.
Figure 11 is the perspective view of a kind of in one embodiment sample steady arm of the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device.
Figure 12 is the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device perspective view of heating furnace in one embodiment.
Figure 13 is the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device split structural representation of sample clamping device in another embodiment.
Embodiment
To combine Figure of description and concrete embodiment that the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device is done further detailed description below.
Embodiment 1
Fig. 1 has shown the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device syndeton of each experimental provision in the present embodiment.As shown in Figure 1, vacuum tube 100 is located in the heating furnace 300, and it is connected with helium feeder, chilled water circulation appearance 901 and vacuum pump dolly 1001 respectively; Heating furnace 300 is located on the positioning table 700, and it is connected with attemperating unit 301.Wherein, The helium feeder comprises helium tank 801, reduction valve 802, the flowmeter 803 that conducting successively connects; Helium inlet conducting on flowmeter 803 and the vacuum tube 100 is connected, thereby can helium be provided to vacuum tube 100, and it can be experimentized under the environment of helium; In addition, on the helium inlet, also be provided with gas admittance valve 804 opening and closing with control helium pipeline; Chilled water circulation appearance 901 is through cooling water inlet and coolant outlet on the vacuum tube 100, is connected with water-cooled torus conducting in vacuum tube 100 water collars; Helium outlet conducting on vacuum pump dolly 1001 and the vacuum tube 100 is connected, and it can guarantee that vacuum tube 100 inside are in the condition of high vacuum degree environment of 10-3～10-4Pa; In addition, in the helium outlet, also be provided with vent valve 1002, vacuum meter 1003 is located on the gas circuit of vacuum pump dolly 1001 and vacuum tube 100, in order to detect the vacuum tightness in the vacuum tube 100; Attemperating unit 301 is connected with a heating furnace 300 and a computer data respectively; It adopts 300 pairs of vacuum tubes 100 of close-loop control mode control heating furnace to heat; Temperature is controlled in the working temperature of room temperature-1100 ℃, the highlyest is no more than 1200 ℃, its constant temperature precision is ± 1 ℃; Attemperating unit 301 also is connected with vacuum tube 100 interior thermopairs, in order to measure vacuum tube 100 temperature inside; In addition, attemperating unit 301 not only can be controlled 300 pairs of vacuum tubes 100 of heating furnace and heat and show related data on computers, also plays the effect into heating furnace 300 electric energy transmittings.
Fig. 2 has shown the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device structure in the present embodiment.As shown in Figure 2, vacuum tube 100 is located in the heating furnace 300, and heating furnace 300 is located on the positioning table 700.Be respectively equipped with incidence window and transmission window on the end face at vacuum tube 100 two ends, the corresponding setting of incidence window with transmission window.Sample is loaded on the sample holder device, and the sample holder device is located in the vacuum tube 100 as shown in Figure 3 through the sample steady arm).First ionization chamber, 500 corresponding incidence windows are located at the outside of vacuum tube 100, and second ionization chamber or ccd detector 600 corresponding transmission windows are located at the outside of vacuum tube 100.Positioning table 700 can be adjusted the position of the vacuum tube 100 in the heating furnace 300, makes first ionization chamber 500 can aim at incidence window and transmission window respectively with second ionization chamber or ccd detector 600, and guarantees that the incident X-ray is through the sample center.Positioning table 700 comprises X axial translation positioning table, Y axial translation positioning table, Z axial translation positioning table and the rotary sample positioning table that connects successively.X, Y, Z axial translation positioning table can provide vacuum drying oven moving on X, Y, three directions of Z; The rotary sample positioning table can make vacuum tube 100 rotate around a rotating shaft.
Please continue to consult Fig. 2, in the present embodiment, the incident X-ray through first ionization chamber 500, incidence window, shines on the sample, with sample generation reciprocation successively; The sample that is heated to uniform temperature partly absorbs and scattering X-ray, penetrates from transmission window then, is received by second ionization chamber or ccd detector 600; Can original position obtain the information such as ionic species, chemical valence state and structure in the sample after the treated analysis of the signal that receives.
Fig. 3 has shown the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device structure of vacuum tube in the present embodiment.Fig. 4 has shown the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device structure of the water collar at vacuum tube two ends in the present embodiment.Fig. 5 is the sectional view of A-A face among Fig. 4.Fig. 6 is the sectional view of B-B face among Fig. 4.Like Fig. 3-shown in Figure 6; Two water collar 102a, 102b are that the sealed at both ends of the quartz ampoule 101 of 260mm is connected with length respectively; Two flange 103a, 103b are connected with two water collar 102a, 102b respectively, and incidence window and transmission window 105 are located at two flange 102a respectively, 102b is last.Sample is loaded on the sample holder device 200, and sample holder device 200 is located in the vacuum tube through sample steady arm 400.Also be provided with thermopair 106 in the vacuum tube, it is connected with attemperating unit, with the temperature in the monitoring vacuum tube.Be equipped with the film that is used for printing opacity on incidence window and the transmission window 105, this 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 ℃, the gas leakage but its transaction is broken.Two kinds of films respectively have quality, can require to select according to actual experiment.At water collar 102a, last helium interface 108 (the last helium import 10Sa of being of water collar 102a that is equipped with of 102b; Water collar 102b goes up and to be helium outlet 108b), cooling water inlet 109a, coolant outlet 109b and the interior chilled water torus 107 of jacket wall of being located at water collar 102a, 102b.Wherein, helium import 108a is connected with the helium feeder, thinks that vacuum tube provides the helium experimental situation; Helium outlet 108b is connected with the vacuum pump dolly, so that vacuum tube is evacuated to high vacuum environment; In addition, on helium import 108a and helium outlet 108b, be respectively equipped with gas admittance valve and vent valve.Cooling water inlet 109a, coolant outlet 109b are connected with the conducting of chilled water circulation appearance respectively; Cooling water inlet 109a, coolant outlet 109b also are connected with 107 conductings of chilled water torus respectively; Thereby form a chilled water loop; Chilled water enters in the chilled water torus 107 from cooling water inlet 109a, turns back to the chilled water circulation appearance from coolant outlet 109b then, and then the vacuum tube two ends are cooled off; Water collar 102a, 102b adopt the aldary of high thermal conductivity to process, thereby have strengthened the cooling effect of water collar.Vacuum tube advantages of small volume in the present embodiment, in light weight, can with the hands hold up easily, put into vacuum glove box and adorn appearance, operation such as vary, omnidistance all in the inert atmosphere protection or vacuum environment of strictness to guarantee sample.
Fig. 7 has shown the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device structure of sample holder device in the present embodiment.Fig. 8 has shown the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device structure of second holding piece in the present embodiment.Fig. 9 is the cross section view of C-C face among Fig. 8.Figure 10 is the local enlarged diagram at L place among Fig. 9.Like Fig. 7-shown in Figure 10, first holding piece 202 and second holding piece 203 are provided with in pairs, and its diameter is 30mm, and thickness is 1mm, and its material can be selected hot pressed boron for use; Though the hot pressed boron porosity is higher, impurity is many, and it is easy to processing, and price is more cheap than pyrolytic boron nitride, and its temperature conductivity and thermal shock resistance are all not low; Adopt hot pressed boron to make holding piece and can further reduce experimental cost; First holding piece, 202 centers offer first through hole, 204, the first through holes 204 around be uniform-distribution with four fastener hole 206a; Second holding piece, 203 centers offer shoulder hole 205, and shoulder hole 205 comprises successively macropore 205a and the aperture 205b that is connected, shoulder hole 205 be uniform-distribution with on every side four with first holding piece 202 on the corresponding fastener hole 206b of fastener hole 206a.The diameter of macropore 205a is set to the external diameter greater than sample 201, and the diameter of first through hole 204 and aperture 205b is set to the external diameter less than sample 201.Sample 201 is embedded in the macropore 205a of shoulder hole 205 of second holding piece 203; First holding piece 202 and second holding piece 203 are fixed together, thereby sample 201 is fixed in the macropore 205a between first through hole 204 and the aperture 205b with relative fastener hole 206a, 206b through screw 207, nut 208 again.Because the diameter of sample 201 test zones is generally less than 5mm; Therefore sample 201 test zones can keep certain distance with the surface of contact (periphery) of two holding piece 202,203 fixing sample 201 on sample 201; Thereby make that two holding pieces 202,203 are reusable after easy clean, and can not pollute sample 201.
Sample is formed by the mixed-powder compacting of a certain proportion of fused salt and boron nitride, can regulate the absorption coefficient of sample to X-ray through changing the fused salt and the ratio of boron nitride and the thickness of sample.In the present embodiment, the fused salt in the sample is a villiaumite, and its purity is higher than 99.9%, and between 1/9～1/4, when too high as if the weight ratio of villiaumite and boron nitride, at high temperature villiaumite will overflow in the matrix from boron nitride the weight ratio of villiaumite and boron nitride usually; If the weight ratio of villiaumite and boron nitride is crossed when hanging down, boron nitride matrix powder might influence the Local Structure of villiaumite sample.The making step of sample is following:
(1) villiaumite is melted, solidifies, grinds to form mean grain size less than 10 microns uniform powder potpourri;
(2) these mixture of powders are evenly mixed above half an hour by special ratios with boron nitride matrix powder;
(3) powder mixture that will pass through step (2) gained becomes the sample of disk type.
The said sample making step all carries out in the vacuum glove box that is full of dry argon gas inert gas.In the present embodiment, the diameter of sample is 10mm, and thickness is 0.4～1mm.
Figure 11 has shown the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device structure of sample steady arm in the present embodiment.In conjunction with Fig. 3, Figure 11; Sample steady arm 400 length are about the half the of quartz ampoule length; It has the deep-slotted chip breaker 401 that width is 9mm; Also be provided with the locating slot 402 that matees with sample holder device 200 on the internal groove side wall of deep-slotted chip breaker 401, its width is 2mm, and sample holder device 200 correspondences are located in this locating slot 402.In experimentation, the fused salt that overflows in the sample can drop in the deep-slotted chip breaker 401, thereby the fused salt of having avoided overflowing drops in vacuum tube.
Figure 12 has shown the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device structure of heating furnace in the present embodiment.Shown in figure 12, when carrying out test experiments, vacuum tube 100 is positioned in the heating furnace 300 and heats.Heating furnace 300 is the openable heating furnace, and it comprises the upper and lower that is hinged, and top or bottom can be rotated to open or closed heating furnace around jointed shaft.In the present embodiment, the heater strip of heating furnace 300 is selected cheap nickel-chromium resistance wire for use, thereby can further reduce experimental cost.
Embodiment 2
Figure 13 has shown the described tubular type high-temperature molten salt of the utility model synchrotron radiation original position research device split structural representation of sample clamping device in another embodiment.Shown in figure 13; Radioactivity fused salt sample 201 (diameter 10mm; Thickness 200 μ m) be arranged between first holding piece 211 and second holding piece 212 through the blind hole on the opposite face of first holding piece 211 and second holding piece 212; Be provided with eight fastener holes 206 around the blind hole in uniform way; Correspondingly eight screws 207 and nut 208 and pad are clamped in radioactivity fused salt sample 201 between first holding piece 211 and second holding piece 212 securely, are equipped with corresponding optical transmission window on first holding piece 211 and second holding piece 212, and first holding piece 211 and second holding piece 212 in the present embodiment are the pyrolytic boron nitride material; And its diameter is 30mm, and thickness is 1mm.First holding piece 211 that is fixedly connected and second holding piece 212 are located in the tank body of a sealing, and this tank body comprises cover 209 and the can body 210 that is threaded with cover 209, and is same, also are respectively equipped with optical transmission window on the bottom surface of cover 209 and can body 210.Radioactivity fused salt sample 201 just places in first holding piece 211 and second holding piece 212, tank body and the triple barriers of vacuum tube like this, can reduce greatly the risk that radiomaterial leaks takes place.
In the present embodiment, except the said sample clamping device, other elements of tubular type high-temperature molten salt synchrotron radiation original position research device and embodiment 1 and indistinction are so repeat no more at this.
Be noted that the above specific embodiment of enumerating that is merely the utility model, obviously the utility model is not limited to above embodiment, and many similar variations are arranged thereupon.If those skilled in the art from all distortion that the disclosed content of the utility model directly derives or associates, all should belong to the protection domain of the utility model.
Claims (10)
1. tubular type high-temperature molten salt synchrotron radiation original position research device, it comprises:
One heating furnace;
One vacuum tube, it is located in the said heating furnace, and said vacuum tube is respectively equipped with an incidence window and a transmission window along the two ends of its axial direction, and said incidence window and transmission window are corresponding to be provided with; Be provided with a sample holder device in the said vacuum tube;
One first ionization chamber, its corresponding said incidence window is located at the outside of vacuum tube;
One second ionization chamber or a ccd detector, its corresponding said transmission window is located at the outside of vacuum tube.
2. tubular type high-temperature molten salt synchrotron radiation original position research device as claimed in claim 1 is characterized in that said vacuum tube comprises:
One quartz ampoule is provided with a sample steady arm in it, said sample holder device is located on the sample steady arm;
Two water collars; Be connected with the sealed at both ends of said quartz ampoule respectively; Be respectively equipped with helium inlet and helium outlet on said two water collars; Also be provided with a chilled water torus on the jacket wall of said each water collar, also be respectively equipped with a cooling water inlet and a coolant outlet on said each water collar, the cooling water inlet on said each water collar and coolant outlet are connected with chilled water torus conducting on this cooling jacket;
Two flanges are connected with said two water collars respectively, and said incidence window and transmission window are located at respectively on said two flanges.
3. tubular type high-temperature molten salt synchrotron radiation original position research device as claimed in claim 2 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 heating furnace is arranged on the positioning table;
One helium feeder, it is connected with said helium inlet through pipeline, and this pipeline is provided with a gas admittance valve;
One vacuum pump dolly, it is connected with said helium outlet through pipeline, and this pipeline is provided with a vent valve;
One attemperating unit, it is connected with said heating furnace, and the closed-loop control heating furnace is to the heating-up temperature of vacuum tube;
One chilled water circulation appearance, it is connected with coolant outlet with said each cooling water inlet.
4. tubular type high-temperature molten salt synchrotron radiation original position research device as claimed in claim 3 is characterized in that also be provided with a thermopair in the said vacuum tube, it is connected with said attemperating unit.
5. like any described tubular type high-temperature molten salt synchrotron radiation original position research device among the claim 1-4; It is characterized in that; Said heating furnace is the openable heating furnace; It comprises a top and a bottom that is hinged, and said top or bottom can be rotated to open or closed heating furnace around jointed shaft.
6. like any described tubular type high-temperature molten salt synchrotron radiation original position research device among the claim 1-4, it is characterized in that said sample holder device comprises:
First holding piece and second holding piece that are provided with in pairs; The center of said first holding piece has first through hole; Be uniform-distribution with several fastener holes around first through hole; The center of said second holding piece has a shoulder hole, be uniform-distribution with around the said shoulder hole several with first holding piece on the corresponding fastener hole of fastener hole, said shoulder hole comprises successively a macropore and an aperture of linking; The diameter of said macropore is set to the external diameter greater than sample, and the diameter of said first through hole and aperture is set to the external diameter less than sample;
Several screws, correspondence is passed the fastener hole on first holding piece and second holding piece respectively;
The nut that several and said each screw are provided with in pairs is connected with said each screw respectively.
7. like any described tubular type high-temperature molten salt synchrotron radiation original position research device among the claim 1-4, it is characterized in that said sample holder device comprises:
First holding piece and second holding piece that are provided with in pairs; Respectively be provided with a blind hole on corresponding of said first holding piece and second holding piece; Be uniform-distribution with several fastener holes around said each blind hole; The somewhat larger in diameter of said blind hole also respectively has the optical transmission window of a correspondence in the external diameter of sample on said first holding piece and second holding piece;
Several screws, correspondence is passed the fastener hole on first holding piece and second holding piece respectively;
The nut that several and said each screw are provided with in pairs is connected with said each screw respectively.
8. tubular type high-temperature molten salt synchrotron radiation original position research device as claimed in claim 6; It is characterized in that; Said sample steady arm has a deep-slotted chip breaker; Also be provided with on the internal groove side wall of said deep-slotted chip breaker one with the locating slot of said sample holder device coupling, said sample holder device correspondence is located in this locating slot.
9. tubular type high-temperature molten salt synchrotron radiation original position research device as claimed in claim 7 is characterized in that, said sample holder device is arranged with the tank body of a sealing outward, and the bottom of said tank body and top all have optical transmission window.
10. tubular type high-temperature molten salt synchrotron radiation original position research device as claimed in claim 9 is characterized in that said tank body comprises a can body and the cover that is threaded with said can body.
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| CN2012200239540U CN202471625U (en) | 2012-01-18 | 2012-01-18 | Tubular high-temperature molten salt synchrotron radiation in-situ research device |
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| CN106802428B (en) * | 2017-01-19 | 2019-01-01 | 中国科学院上海应用物理研究所 | A kind of x-ray imaging detector of radiation hardness and high heat load |
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