CN106248703A - A kind of synchrotron radiation in-situ testing device - Google Patents

A kind of synchrotron radiation in-situ testing device Download PDF

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Publication number
CN106248703A
CN106248703A CN201610911264.1A CN201610911264A CN106248703A CN 106248703 A CN106248703 A CN 106248703A CN 201610911264 A CN201610911264 A CN 201610911264A CN 106248703 A CN106248703 A CN 106248703A
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CN
China
Prior art keywords
flange
testing device
synchrotron radiation
situ testing
top cover
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CN201610911264.1A
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Chinese (zh)
Inventor
何燕
王娟
肖学章
李爱国
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Shanghai Institute of Applied Physics of CAS
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Shanghai Institute of Applied Physics of CAS
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Priority to CN201610911264.1A priority Critical patent/CN106248703A/en
Publication of CN106248703A publication Critical patent/CN106248703A/en
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    • 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]

Abstract

The present invention relates to a kind of synchrotron radiation in-situ testing device, top flange and wall flange are connected to cavity pipe by stainless steel tube respectively, heating assembly is supported by top flange and fixes, and substitute gas flange and supported by wall flange and fix, two end plates is provided with the first ray window and is directly fixed on the two ends of cavity pipe, and form flange is supported by end plate and fixes;Top cover flange is fixing with top flange to be connected, the end face of top cover flange is provided with air plug, the bottom surface of top cover flange is provided with heating flange, sample stage suspension is fixed on below top cover flange by suspension rod by heating flange, being provided with thermocouple on sample stage, thermocouple is connected with air plug by adding heat pipe, and sample stage is fixed with the specimen holder for installing sample, specimen holder has the second ray window, the center of sample, the center of the first ray window and the center alignment of the second ray window.The synchrotron radiation in-situ testing device of the present invention measures in the environment of sample is maintained at isolation air and water.

Description

A kind of synchrotron radiation in-situ testing device
Technical field
The present invention relates to put for the suction studying hydrogen storage material the device of hydrogen mechanism, relate more specifically to a kind of synchrotron radiation In-situ testing device.
Background technology
The novel hydrogen storage material of the research and development high power capacity large-scale application to promoting Hydrogen Energy is significant.Mg (BH4)2Complex hydrides is the high power capacity storage hydrogen material of a kind of great application potential, just promotes the key problem of its actual application It is to improve its reversible hydrogen adsorption and desorption kinetics performance comprehensively.Catalytic modification is effectively to reduce hydrogen discharging temperature, improvement coordination hydrogenation Thing inhales an important means of hydrogen desorption kinetics performance.Therefore, Mg (BH is verified4)2The catalytic modification mechanism of system is to break through its storage The key of the actual application of hydrogen.Current research all shows that the doping of catalyst can effectively accelerate to put hydrogen process, improves hydrogen discharge reaction Dynamic performance.The size of doped nanoparticle is the least, the degree of disorder is the highest, and its catalytic modification effect is the best.Owing to routine is real Test cell structure analysis method cannot the amorphous state intermediate product that generate in amorphous catalyst and course of reaction thereof be carried out finely Structure detection, it is impossible to directly and really characterize amorphous state additive structure during hydrogen discharge reaction and the change of chemical state Change, therefore cannot fundamentally explain the mechanism of the catalytic modification that doping caused.
Utilize synchrotron radiation X-ray Absorption Fine Structure (X-ray Absorption Fine Structure, XAFS) skill Art is to that the on-spot study of the catalytic modification mechanism of all kinds of complex hydrides is the field of novel hydrogen storage material modification in recent years Important research trend.For Synchrotron Radiation Technology is compared to Routine Test Lab measuring technology, even more important exactly can be to urging Formed material crystal, atom and electronic structure change in course of reaction is carried out in situ, dynamic characterization research, for hydrogen storage material Catalytic modification study mechanism provides comprehensive and three-dimensional research means, thus for instructing rational design and the efficient storage of preparation Hydrogen material catalyst provides theoretical direction.Chaudhuri etc. (S.Chaudhuri, et al., J.Am.Chem.Soc, 2006, 128:11404-11415) by NaAlH4The EXAFS research of Ti base catalyst during hydrogen storage material suction hydrogen, it is proposed that Ti Catalyst accelerates NaAlH4Inhale the interaction mode of hydrogen process.Minerlla etc. (C.B.Minella, et al., J.Phys.Chem.C, 2013,117:4394-4403) have studied Ti-and Nb base catalytic additive at Ca (BH by XANES4)2 Change in chemical state rule in complex hydrides.And the Chen Ping seminar of the domestic Dalian Chemistry and Physics Institute (X.L.Zhang, et al., Energy Environ.Sci..2011,4:3593-3600;J.P.Guo,et al.,Angew.Chem.Int.Ed..2015, 54:2950-2954) utilizing the various transition metal based catalysts of XAFS technical research to lithium borohydride ammonate and imido always The catalytic modification mechanism of base lithium hydrogen storage material.Liu Yong cutting edge of a knife or a sword seminar (Y.Zhang, et al., the Int.J of Zhejiang University Hydrogen Energy,2013,38:13318-13327;Y.Zhang,et al.,Dalton Trans.,2015,44: The hydrogen discharging temperature of Li-B-N-H matrix composite system, and profit 14514-14522) is effectively reduced by a small amount of doping CoO catalyst The CoO catalyst mechanism of action in Li-B-N-H based hydrogen storage material is have extensively studied by XAFS technology.
As can be seen here, the microstructure utilizing synchrotron radiation characterization technique to be catalyzed constituent element during hydrogen storage material is put hydrogen is drilled Change process carries out in situ detection to research Amorphous Transition Metals catalyst to Mg (BH4)2Grinding of hydrogen storage system catalyticing mechanism Study carefully and there is irreplaceable effect.But, in currently available technology, corresponding synchrotron radiation in-situ testing device can not It is used for Mg (BH4)2Hydrogen storage system catalyticing mechanism is studied.
Summary of the invention
It is desirable to provide a kind of synchrotron radiation in-situ testing device, it can in-situ characterization Mg (BH4)2Hydrogen storage system Structure change in catalytic process, provides technical support for on-spot study hydrogen storage system catalyst mechanism.
Synchrotron radiation in-situ testing device of the present invention, including form flange, cavity components, heating assembly with substitute Gas flange;This cavity components includes top flange, stainless steel tube, cavity pipe, wall flange and two end plates, top flange and sidewall Flange is connected to this cavity pipe by stainless steel tube respectively, and heating assembly is supported and fixing by this top flange, and substitutes gas Flange is supported by this wall flange and fixes, and two end plates is provided with the first ray window and is directly fixed on the two of cavity pipe End, form flange is supported by end plate and fixes;This heating assembly includes air plug, top cover flange, adds heat pipe, sample stage, sample Seat, heating flange and suspension rod, top cover flange is fixing with top flange to be connected, and the end face of top cover flange is provided with air plug, top cover method Blue bottom surface is provided with heating flange, and the lower section of top cover flange, sample are fixed in sample stage suspension by this heating flange by suspension rod Being provided with thermocouple in sample platform, this thermocouple is connected with air plug by adding heat pipe, and sample stage is fixed with for installing sample Specimen holder, this specimen holder has the second ray window, the center of sample, the center of the first ray window and the second ray window Center alignment.
Cavity pipe is cylinder, and top flange and wall flange are connected to the sidewall of cavity pipe, and two end plates is directly solid Front and back due to cavity pipe.
This cavity components also includes the test platform for synchrotron radiation in-situ testing device is fixed to experiment line station On bearing, this bearing is fixed on the bottom of cavity pipe.
It is furnished with heat insulating washer between heating flange and top cover flange.
The outside adding heat pipe is cased with ceramic bead or ceramics pole.
O RunddichtringO it is furnished with between top cover flange and top flange.
Compton film it is provided with between form flange and end plate.
O RunddichtringO pad it is provided with between end plate and Compton film and Compton film and form flange.
Substitute and between gas flange and wall flange, be furnished with O RunddichtringO.
Substitute gas Flange joint generation big Lip river gram ball valve.
The synchrotron radiation in-situ testing device of the present invention measures in the environment of sample is maintained at isolation air and water, Meet catalysis doping Mg (BH4)2The study condition of hydrogen storage system.And, the volume of the synchrotron radiation in-situ testing device of the present invention Little, it is possible to install in glove box, solve the problem that hydrogen storage system can not contact water and air.
Accompanying drawing explanation
Fig. 1 is the sectional view of the synchrotron radiation in-situ testing device according to the present invention;
Fig. 2 is the structural representation of the cavity components of Fig. 1;
Fig. 3 is the structural representation of the heating assembly of Fig. 1.
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.
Fig. 1 is the sectional view of the synchrotron radiation in-situ testing device according to the present invention, wherein, and this synchrotron radiation in-situ test Device includes form flange 1, cavity components 2, heating assembly 3 and substitutes gas flange 4.Cavity components 2 is formed as the same of the present invention The support of step radiation in-situ testing device, heating assembly 3 passes through cavity components 2 and supports and be arranged at the inside of cavity components 2, and Form flange 1 and substitute gas flange 4 and support again by cavity components 2 but be arranged at the outside of cavity components 2.
Fig. 2 is the structural representation of the cavity components of Fig. 1, this cavity components 2 include top flange 21, stainless steel tube 22, Cavity pipe 23, wall flange 24, end plate 25 and bearing 26.Wherein, cavity pipe 23 in cylinder, top flange 21 and wall flange 24 are connected on the sidewall of this cavity pipe 23 by stainless steel tube 22 respectively, and front and back end plate 25 (is provided centrally with the first ray Window 27) it is directly fixed on end (the most cylindrical end face and bottom surface are front and back in the drawings) before and after cavity pipe 23.Knot Conjunction Fig. 1 understands, and heating assembly 3 is supported by this top flange 21 and fixed, and substitutes gas flange 4 and is supported by this wall flange 24 With fixing, form flange 1 is supported by end plate 25 before and after being somebody's turn to do and is fixed.It addition, bearing 26 is directly fixed on the side of cavity pipe 23 Bottom wall, for whole in-situ testing device being fixed to the test platform at experiment line station.Preferably, cavity pipe 23 is by stainless Steel material is formed, and small volume (about 204mm*150mm*271mm), to facilitate turnover glove box.Preferably, in order to ensure to obtain Obtain diffraction ring quantity enough, through calculating, a diameter of 50mm of the first ray window 27.
Fig. 3 is the structural representation of the heating assembly of Fig. 1, and this heating assembly 3 includes air plug 31, top cover flange 32, heating Pipe 33, ceramic bead 34, earthenware 35, sample stage 36, thermocouple tabletting 37, specimen holder 38, heat insulating washer 39, heating flange 310 With suspension rod 311.The end face of top cover flange 32 is provided with air plug 31, and it is used for connecting outside attemperating unit and accurately controlling test The temperature of sample.The bottom surface of top cover flange 32 is provided with heating flange 310, and it is for hanging sample stage 36 by suspension rod 311 It is fixed on below top cover flange 32.In the present embodiment, for reducing heat transmission, heating flange 310 and top cover flange 32 it Between be furnished with heat insulating washer 39, in case stop-pass is crossed top cover flange 32 and transferred heat to cavity components 2 and make the temperature of cavity components 2 Spend height.
Being provided with thermocouple on sample stage 36, this thermocouple is fixed on sample stage near sample by thermocouple tabletting 37 Place, the variations in temperature of monitoring sample.This thermocouple is connected with air plug 31 by adding heat pipe 33, thus to add heat pipe 33 right by this Whole sample stage 36 heats.The outside adding heat pipe 33 is cased with ceramic bead 34 or ceramics pole 35, adds on heat pipe 33 to reduce Heat loss.Specimen holder 38 (being provided centrally with the second ray window 312) it is fixed with, by means of suspension rod 311 to sample on sample stage 36 The rigid support of sample platform 36, the center of the second ray window 312 on sample stage 36 and the first ray window on end plate 25 front and back The center alignment of mouth 27.Sample is close to specimen holder 38 and is arranged and be fixed in the second ray window 312 by specimen holder, and sample The center alignment of center and the second ray window 312.In the present embodiment, sample stage 36 is made of copper, effectively by heat It is delivered to sample, makes sample thermally equivalent.
Understanding in conjunction with Fig. 1 and Fig. 2, the top cover flange 32 of heating assembly 3 is fixing even with the top flange 21 of cavity components 2 Connect.For ensureing the air-tightness of whole device, between top cover flange 32 and top flange 21, it is furnished with O RunddichtringO.
In the present embodiment, the center alignment of the center of form flange 1 and front and back end plate 25.The center of form flange 1 has Circular window, to reduce the loss to X-ray.It is provided with Compton film between form flange 1 and front and back end plate 25.For ensureing gas Close property, is front and back provided with O RunddichtringO pad between end plate 25 and Compton film and Compton film and form flange 1.
In the present embodiment, substitute and between gas flange 4 and wall flange 24, be furnished with O RunddichtringO, to guarantee whole device Air-tightness.Have stainless steel tube additionally, substitute on gas flange 4, be used for connecting generation big Lip river gram ball valve, device is carried out evacuation or Fill gas.This just greatly reduces the volume of this in-situ testing device, to guarantee that whole device can be put into glove box and enter Row is installed.
The specifically used process of the synchrotron radiation in-situ testing device of the present invention includes: be installed on by sample in glove box In second ray window 312 of the specimen holder 38 of heating assembly 3, fixing, by taking out in heating assembly 3 is inserted cavity components 2 After ventilation flange 4 evacuation or populated desired gas, check device air-tightness, then by former for the synchrotron radiation of the present invention Bit test device takes out from glove box.Outside attemperating unit is connected, by bearing 26 by the synchronization of the present invention by air plug 31 Radiation in-situ testing device is fixed on experiment test platform.During test, X-ray sequentially passes through form flange 1, Compton film, front End plate 25 and the second ray window 312 are also irradiated on sample, afterwards via end plate 25, Compton film and form flange 1 Shine on the detector of experiment porch.
Obviously, the synchrotron radiation in-situ testing device of the present invention is carried out in the environment of sample is maintained at isolation air and water Measure, meet catalysis doping Mg (BH4)2The study condition of hydrogen storage system.And, the synchrotron radiation in-situ testing device of the present invention Volume little, it is possible to install in glove box, solve the problem that hydrogen storage system can not contact water and air.Preferably, A diameter of 50mm of the first ray window 27, can record more diffraction ring, thus obtain more diffraction maximum.
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 synchrotron radiation in-situ testing device, it is characterised in that include form flange, cavity components, heating assembly and take out Ventilation flange;
This cavity components includes top flange, stainless steel tube, cavity pipe, wall flange and two end plates, top flange and sidewall method Orchid is connected to this cavity pipe by stainless steel tube respectively, and heating assembly is supported and fixing by this top flange, and takes out ventilation Orchid is supported by this wall flange and fixes, and two end plates is provided with the first ray window and is directly fixed on the two ends of cavity pipe, Form flange is supported by end plate and fixes;
This heating assembly includes air plug, top cover flange, adds heat pipe, sample stage, specimen holder, heating flange and suspension rod, top cover flange Fixing with top flange and be connected, the end face of top cover flange is provided with air plug, and the bottom surface of top cover flange is provided with heating flange, and this adds The lower section of top cover flange is fixed in sample stage suspension by full-boiled process orchid by suspension rod, sample stage is provided with thermocouple, this thermocouple Being connected with air plug by adding heat pipe, sample stage is fixed with the specimen holder for installing sample, this specimen holder has the second ray Window, the center of sample, the center of the first ray window and the center alignment of the second ray window.
Synchrotron radiation in-situ testing device the most according to claim 1, it is characterised in that cavity pipe is cylinder, top Flange and wall flange are connected to the sidewall of cavity pipe, and two end plates is directly fixed on the front and back of cavity pipe.
Synchrotron radiation in-situ testing device the most according to claim 1, it is characterised in that this cavity components also includes use In the bearing being fixed to by synchrotron radiation in-situ testing device on the test platform at experiment line station, this bearing is fixed on cavity pipe Bottom.
Synchrotron radiation in-situ testing device the most according to claim 1, it is characterised in that heating flange and top cover flange it Between be furnished with heat insulating washer.
Synchrotron radiation in-situ testing device the most according to claim 1, it is characterised in that the outside adding heat pipe is cased with pottery Pearl or ceramics pole.
Synchrotron radiation in-situ testing device the most according to claim 1, it is characterised in that top cover flange and top flange it Between be furnished with O RunddichtringO.
Synchrotron radiation in-situ testing device the most according to claim 1, it is characterised in that set between form flange and end plate It is equipped with Compton film.
Synchrotron radiation in-situ testing device the most according to claim 7, it is characterised in that end plate and Compton film and health O RunddichtringO pad it is provided with between general film and form flange.
Synchrotron radiation in-situ testing device the most according to claim 1, it is characterised in that substitute gas flange and wall flange Between be furnished with O RunddichtringO.
Synchrotron radiation in-situ testing device the most according to claim 9, it is characterised in that substitute gas Flange joint generation big Lip river gram ball valve.
CN201610911264.1A 2016-10-19 2016-10-19 A kind of synchrotron radiation in-situ testing device Pending CN106248703A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109126677A (en) * 2018-10-24 2019-01-04 中国科学院高能物理研究所 Reaction in-situ device
CN116465914A (en) * 2023-05-08 2023-07-21 天津大学 Four-degree-of-freedom high-temperature vacuum environment box used under neutron diffraction condition

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CN103884725A (en) * 2012-12-21 2014-06-25 中国科学院高能物理研究所 X-ray absorption spectrum in-situ heating apparatus
CN105928961A (en) * 2016-06-13 2016-09-07 北京工业大学 In-situ testing sample stage and in-situ testing method
CN206132669U (en) * 2016-10-19 2017-04-26 中国科学院上海应用物理研究所 Synchrotron radiation in situ test device

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Publication number Priority date Publication date Assignee Title
CN2126918Y (en) * 1992-07-03 1993-02-10 中国科学院大连化学物理研究所 In-situ cell of expanded x-ray absorption fine structural spectrum
US6212253B1 (en) * 1998-03-03 2001-04-03 Max-Planck-Gesellschaft Apparatus and method for X-ray absorption spectroscopy
CN101629915A (en) * 2009-08-14 2010-01-20 中国科学院山西煤炭化学研究所 Sample reservoir for carrying out in-situ characterization on crystallization process of molecular sieve based catalyst, and use method thereof
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109126677A (en) * 2018-10-24 2019-01-04 中国科学院高能物理研究所 Reaction in-situ device
CN116465914A (en) * 2023-05-08 2023-07-21 天津大学 Four-degree-of-freedom high-temperature vacuum environment box used under neutron diffraction condition
CN116465914B (en) * 2023-05-08 2023-11-03 天津大学 Four-degree-of-freedom high-temperature vacuum environment box used under neutron diffraction condition

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Application publication date: 20161221