CN106288796A - A kind of glancing incidence XAFS high-temp in-situ stove - Google Patents

A kind of glancing incidence XAFS high-temp in-situ stove Download PDF

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Publication number
CN106288796A
CN106288796A CN201610592451.8A CN201610592451A CN106288796A CN 106288796 A CN106288796 A CN 106288796A CN 201610592451 A CN201610592451 A CN 201610592451A CN 106288796 A CN106288796 A CN 106288796A
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CN
China
Prior art keywords
window
stove
situ
temp
heater
Prior art date
Application number
CN201610592451.8A
Other languages
Chinese (zh)
Inventor
于海生
魏向军
姜政
孙凡飞
汪丽华
黄宇营
张晓哲
Original Assignee
中国科学院上海应用物理研究所
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Priority to CN201610592451.8A priority Critical patent/CN106288796A/en
Publication of CN106288796A publication Critical patent/CN106288796A/en

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Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B17/00Furnaces of a kind not covered by any preceding group
    • F27B17/02Furnaces of a kind not covered by any preceding group specially designed for laboratory use
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/06Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
    • G01N23/083Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption the radiation being X-rays
    • G01N23/085X-ray absorption fine structure [XAFS], e.g. extended XAFS [EXAFS]
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/101Different kinds of radiation or particles electromagnetic radiation
    • G01N2223/1016X-ray

Abstract

nullThe present invention relates to a kind of glancing incidence XAFS high-temp in-situ stove,It has center longitudinal axis and includes the body of heater arranged round center longitudinal axis、Bell and stove seat,Wherein,Body of heater passes through stove seat supports,Bell is arranged at the top of body of heater and is secured to connect,Body of heater has main body and the furnace chamber limited by main body,The first window for X-ray incidence it is provided with in main body、The second window for X-ray outgoing and the 3rd window for fluorescence detection,The central axis of first window and the second window is positioned on a straight line,Straight line is perpendicular to center longitudinal axis,The central axis upright of the 3rd window is in the plane limited by center longitudinal axis and straight line,The 4th window for fluorescence detection it is provided with on bell,The central axis of the 4th window overlaps with center longitudinal axis,Sample stage it is provided with in furnace chamber,Angle between top surface and the straight line of sample stage is between 05 °.The glancing incidence XAFS high-temp in-situ stove of the present invention can carry out XAFS test to solid liquid interface.

Description

A kind of glancing incidence XAFS high-temp in-situ stove
Technical field
The present invention relates to a kind of high-temp in-situ stove, relate more specifically to a kind of glancing incidence XAFS high-temp in-situ stove.
Background technology
High-temp in-situ stove is often used in situ X-ray diffraction Absorption Fine Structure (XAFS) test, to obtain sample element The Local Structure information such as chemical valence state.Sample in high-temp in-situ stove of the prior art for being disposed vertically, incident X-rays with The angle of sample is usually 45 ° or 90 °, can carry out fluorescence method or transmission beam method test.The divergence of synchrotron radiation horizontal direction Bigger than vertical direction, it is disposed vertically sample it is difficult to ensure that x-ray projection is all within sample under the conditions of glancing incidence, thus cannot Realize glancing incidence XAFS test.Owing to can not accurately regulate the angle of X-ray and sample surfaces, it is impossible to control X-ray at sample The penetration depth on surface, also cannot be carried out the structural research of solid liquid interface.It addition, the body of heater of high-temp in-situ stove of the prior art Inwall be made up of stainless steel material, its decay resistance is poor, thus cannot be applicable to the XAFS such as villiaumite under hot conditions Testing research.
MSR fuel be mainly composed of fission fuel and the fluoride molten salt of fuel of can rising in value.Wherein, fluoride melts The operating temperature of salt is in the high temperature section of 650-1000 DEG C and highly corrosive.Obviously, existing high-temp in-situ stove cannot meet The In-situ XAFS condition that fluoride molten salt is tested.
Summary of the invention
The existing high-temp in-situ stove existed to solve above-mentioned prior art cannot carry out XAFS test to solid liquid interface Problem, it is desirable to provide a kind of glancing incidence XAFS high-temp in-situ stove.
Glancing incidence XAFS high-temp in-situ stove of the present invention, it has center longitudinal axis and includes round this center longitudinal axis Body of heater, bell and the stove seat arranged, wherein, body of heater passes through stove seat supports, and bell is arranged at top the company of being secured to of body of heater Connecing, this body of heater has main body and the furnace chamber limited by this main body, this main body is provided with for the incident first window of X-ray, The second window for X-ray outgoing and the 3rd window for fluorescence detection, first window and the central axis of the second window Being positioned on a straight line, this straight line is perpendicular to center longitudinal axis, and the central axis upright of the 3rd window is in straight with this by center longitudinal axis The plane that line is limited, bell is provided with the 4th window for fluorescence detection, the central axis of the 4th window and center The longitudinal axis overlaps, and is provided with sample stage in furnace chamber, and the angle between top surface and the straight line of sample stage is between 0-5 °.
Distance between 3rd window and first window is equal to the distance between the 3rd window and the second window.
First window and the second window are beryllium window window.
Angle between top surface and the straight line of sample stage is between 0.1-2 °.
Body of heater also includes heating system, and this heating system includes the heater strip being directly arranged at below sample stage, its In, this heating system removably connects or non-dismountable is connected to main body.
Body of heater also includes the thermal insulation cover arranged round sample stage, and this thermal insulation cover removably connects or non-dismountable connection In main body.
Sample stage and thermal insulation cover are formed by pyrolytic boron nitride material.
Main body is formed by Hastelloy C alloys 276.
Body of heater also includes the gas turnover pipeline connected with furnace chamber.
Sample stage removably connects or non-dismountable is connected to main body.
Solid liquid interface can be tested by the glancing incidence XAFS high-temp in-situ stove of the present invention, with study fused salt and alloy, The reciprocal action at the interface such as graphite and C-base composte material, and then obtain element chemical state and the local such as bond distance, ligancy knot Structure information, is understanding the aspects such as the physicochemical properties change of different component fused salt, structural material corrosion mechanism in fused salt Play irreplaceable fundamental role.
Accompanying drawing explanation
Fig. 1 is the front view of the glancing incidence XAFS high-temp in-situ stove according to the present invention;
Fig. 2 is the side view of the glancing incidence XAFS high-temp in-situ stove according to the present invention;
Fig. 3 is the sectional view of the glancing incidence XAFS high-temp in-situ stove according to the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings, provide presently preferred embodiments of the present invention, and be described in detail.
As Figure 1-Figure 2, there is center longitudinal axis A according to the glancing incidence XAFS high-temp in-situ stove of the present invention, and include enclosing Body of heater 1, bell 2 and the stove seat 3 arranged around this center longitudinal axis A, wherein, body of heater 1 is in cylindrical, and it is supported by stove seat 3 And it is arranged at suitable height and position, and bell 2 is rounded and is arranged at the top of body of heater 1 and is secured to connect.
As it is shown in figure 1, body of heater 1 has main body 11, it is provided with first window 12a, the second window 12b and the 3rd window 13.First window 12a and the second window 12b is the most opposed, i.e. first window 12a and the central axis of the second window 12b Being positioned on a straight line B, this straight line B is perpendicular to center longitudinal axis A.The central axis C (seeing Fig. 2) of the 3rd window 13 be perpendicular to by Distance between the plane that center longitudinal axis A and straight line B is limited, and the 3rd window 13 and first window 12a equal to it with the Distance between two window 12b.Being provided with the 4th window 21 on bell 2, it is positioned at the center of bell 2, the i.e. the 4th window The central axis of 21 overlaps with center longitudinal axis A.Wherein, first window 12a is used for X for the incidence of X-ray, the second window 12b The outgoing of ray, the two window is logical light window, preferably beryllium window window, has higher transmitance with the strongest Degree.3rd window 13 and the 4th window 21 are for fluorescence detection.
As it is shown on figure 3, body of heater 1 limits furnace chamber 14, it is that the sample 4 that arranges of low-angle (0-5 °) passes through clamping part with straight line B Part 151 (such as boron nitride flakes) is fixed on sample stage 15, and this sample stage 15 is multi-dimensional sample platform, by this sample stage 15 Rotation can regulate the angle of incident X-rays and sample surfaces.It is to say, the top surface of this sample stage 15 and straight line B it Between angle can be adjusted between 0-5 °, be particularly adjusted between 0.1-2 °, so, X-ray pass through first Window 12a enters cavity 14, incides on sample 4 with the angle of 0.1 °, and the X-ray after reflection is by the second window 12b Go out cavity 14;By rotating sample stage 15, then with outgoing after the angle incidence of 0.2 ° ... and then realize the measurement of reflectance And meet the geometry requirement of XAFS experiment.High-temp in-situ stove provided by the present invention can carry out Grazing Incidence X-Ray to sample Absorption spectra is tested.Due to X-ray plunder be maintained at less angular range in be adjusted, such that it is able to fused salt/solid Interface carries out online in-situ study test.
This body of heater 1 also includes heating system 16 (as shown in Figure 2), and this heating system 16 includes and is directly arranged at sample Heater strip below platform 15, so that sample 4 is heated, thus the height needed for maintaining research fused salt to change with alloy surface structure Temperature condition.This heater strip is evenly arranged in the bottom of sample, and length and density by regulation heater strip can ensure that high The thermal efficiency and uniform heat distribution.In glancing incidence XAFS tests, owing to the facula area on x-ray projection to sample is relatively big, Therefore, the temperature conditions in uniform heat distribution can ensure that facula area single.In order to prevent scattering and disappearing of heat, round This sample stage 15 is provided with thermal insulation cover 17 (as shown in Figure 3).Wherein, sample stage 15 and thermal insulation cover 17 are by pyrolytic boron nitride material Being formed, because villiaumite has the strongest corrosivity and volatile, and at high temperature, pyrolytic boron nitride is preferable anti-fluoride salt corrosion Material, so that it is guaranteed that sample stage and thermal insulation cover in use by sample etches, thus will not improve the use of stove in situ Safety and the reliability of experimental data.But, the main body 11 of body of heater 1 can not be formed by pyrolytic boron nitride, because pyrolysis nitridation Boron is not easy to water cooling.Therefore, the material selection of main body 11 has relatively strong corrosion resistant ability and is prone to the Hastelloy of water cooling C276.Owing to this Hastelloy C alloys 276 has preferable sealing, the vacuum in cavity 14 can be better than 10-3Pa。
As it is shown on figure 3, the bottom of body of heater 1 is additionally provided with gas turnover pipeline 18, including air inlet pipe 181 and escape pipe 182, Gas is imported in furnace chamber 14 by air inlet pipe 181, then derives furnace chamber 14 by escape pipe 182.It addition, according to the high temperature of the present invention The surrounding of stove can be provided with gas ionization chamber in situ, to guarantee that the temperature of the outer surface of high-temp in-situ stove is not higher than 80 DEG C, it is to avoid Miscellaneous equipment is caused hot injury.
In the present invention, sample stage 15, the heater strip of heating system 16 and thermal insulation cover 17 are disposed as removably connecting Mode, in order to carry out independently dismounting and changing after damaging components, is greatly enhanced the efficiency of experiment and the maintenance week of equipment Phase.
Above-described, only presently preferred embodiments of the present invention, it is not limited to the scope of the present invention, the present invention's is upper State embodiment can also make a variety of changes.The most every claims according to the present patent application and description are made Simply, equivalence change with modify, fall within the claims of patent of the present invention.Being of the most detailed description of the present invention Routine techniques content.

Claims (10)

1. a glancing incidence XAFS high-temp in-situ stove, it has center longitudinal axis and includes the stove arranged round this center longitudinal axis Body, bell and stove seat, wherein, body of heater passes through stove seat supports, and bell is arranged at the top of body of heater and is secured to connect, its feature Being, this body of heater has main body and the furnace chamber limited by this main body, and this main body is provided with the first window for X-ray incidence Mouth, the second window for X-ray outgoing and the 3rd window for fluorescence detection, first window and the central shaft of the second window Line is positioned on a straight line, and this straight line is perpendicular to center longitudinal axis, the central axis upright of the 3rd window in by center longitudinal axis and should The plane that straight line is limited, bell is provided with the 4th window for fluorescence detection, the central axis of the 4th window with in The heart longitudinal axis overlaps, and is provided with sample stage in furnace chamber, and the angle between top surface and the straight line of sample stage is between 0-5 °.
Glancing incidence XAFS high-temp in-situ stove the most according to claim 1, it is characterised in that the 3rd window and first window it Between distance equal to distance between the 3rd window and the second window.
Glancing incidence XAFS high-temp in-situ stove the most according to claim 1, it is characterised in that first window and the second window are Beryllium window window.
Glancing incidence XAFS high-temp in-situ stove the most according to claim 1, it is characterised in that the top surface of sample stage and straight line Between angle between 0.1-2 °.
Glancing incidence XAFS high-temp in-situ stove the most according to claim 1, it is characterised in that body of heater also includes heating system System, this heating system includes the heater strip being directly arranged at below sample stage, and wherein, this heating system removably connects or not It is removably connected to main body.
Glancing incidence XAFS high-temp in-situ stove the most according to claim 1, it is characterised in that body of heater also includes round sample The thermal insulation cover that sample platform is arranged, this thermal insulation cover removably connects or non-dismountable is connected to main body.
Glancing incidence XAFS high-temp in-situ stove the most according to claim 6, it is characterised in that sample stage and thermal insulation cover are by being pyrolyzed Boron nitride material is formed.
Glancing incidence XAFS high-temp in-situ stove the most according to claim 1, it is characterised in that main body is by Hastelloy C alloys 276 shape Become.
Glancing incidence XAFS high-temp in-situ stove the most according to claim 1, it is characterised in that body of heater also includes with furnace chamber even Logical gas turnover pipeline.
Glancing incidence XAFS high-temp in-situ stove the most according to claim 1, it is characterised in that sample stage removably connect or Non-dismountable it is connected to main body.
CN201610592451.8A 2016-07-26 2016-07-26 A kind of glancing incidence XAFS high-temp in-situ stove CN106288796A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109210941A (en) * 2018-09-06 2019-01-15 大连理工大学 A kind of Reflection X-ray original position diffraction heating furnace

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003081222A1 (en) * 2002-03-19 2003-10-02 X-Ray Optical Systems, Inc. Screening of combinatorial library using x-ray analysis
CN102590253A (en) * 2012-01-17 2012-07-18 中国科学院上海应用物理研究所 High-temperature fused salt synchrotron radiation in-situ research device
CN202471625U (en) * 2012-01-18 2012-10-03 中国科学院上海应用物理研究所 Tubular high-temperature molten salt synchrotron radiation in-situ research device
CN103175857A (en) * 2013-03-14 2013-06-26 中国科学院高能物理研究所 Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device
CN105675640A (en) * 2014-12-04 2016-06-15 日本株式会社日立高新技术科学 X fluorescent x-ray analyzer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003081222A1 (en) * 2002-03-19 2003-10-02 X-Ray Optical Systems, Inc. Screening of combinatorial library using x-ray analysis
CN102590253A (en) * 2012-01-17 2012-07-18 中国科学院上海应用物理研究所 High-temperature fused salt synchrotron radiation in-situ research device
CN202471625U (en) * 2012-01-18 2012-10-03 中国科学院上海应用物理研究所 Tubular high-temperature molten salt synchrotron radiation in-situ research device
CN103175857A (en) * 2013-03-14 2013-06-26 中国科学院高能物理研究所 Device specially used for grazing incidence XAFS (X-ray Absorption Fine Structure) experiment and regulating method of device
CN105675640A (en) * 2014-12-04 2016-06-15 日本株式会社日立高新技术科学 X fluorescent x-ray analyzer

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109210941A (en) * 2018-09-06 2019-01-15 大连理工大学 A kind of Reflection X-ray original position diffraction heating furnace

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