CN110031492A - X-ray diffractometer solvent vapour handles in-situ test attachment - Google Patents
X-ray diffractometer solvent vapour handles in-situ test attachment Download PDFInfo
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- CN110031492A CN110031492A CN201910347086.8A CN201910347086A CN110031492A CN 110031492 A CN110031492 A CN 110031492A CN 201910347086 A CN201910347086 A CN 201910347086A CN 110031492 A CN110031492 A CN 110031492A
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- sample room
- sample
- ray diffractometer
- air inlet
- solvent vapour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating 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
- G01N23/20—Investigating 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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
X-ray diffractometer solvent vapour processing in-situ test attachment belongs to X-ray diffractometer in-situ testing technique field, it is therefore intended that solves the problems, such as that existing X-ray diffractometer cannot achieve and characterizes in solvent vapour treatment process to the real-time in-situ of material microstructure variation.X-ray diffractometer solvent vapour processing in-situ test attachment of the invention includes aerogenesis apparatus, sample room and gas chromatograph；The sample room generally sealing structure is provided with sample stage in the sample room including at least air inlet, gas outlet and two polyimides windows that sample room side wall is arranged in；The exhaust outlet of the aerogenesis apparatus is connected to by gas circuit pipe with the air inlet of the sample room；The gas outlet of the sample room is connected to by gas circuit pipe with the injection port of the gas chromatograph；X-ray diffractometer is through in a polyimides window incident X-rays and the sample that is radiated on the sample stage, the diffracted signal of generation is emitted through another polyimides window.
Description
Technical field
The invention belongs to X-ray diffractometer in-situ testing technique fields, and in particular to it is in situ that one kind is suitable for multiple material
Spread out in solvent vapour treatment process to the real-time monitoring of solvent strength and to the X-ray of the home position observation analysis of material microstructure
Instrument solvent vapour processing in-situ test attachment is penetrated, is the further exploitation to X-ray diffraction in-situ test attachment.
Background technique
Due to the discovery of X-ray crystal diffraction phenomenon, so that X-ray diffraction is for a long time by micro- as a kind of research substance
The effective tool of fine texture can calculate crystalline texture information by the test result of X-ray diffraction, such as cell parameter, crystallographic system, sky
Between group, Molecules in structure cell, calculate density etc. and molecular structure information, such as bond distance, bond angle, nonbonding distance, hydrogen bond, structure
As, torsion angle etc., the even details of atom.
According to known sample structure prediction performance, or design according to known structure and property relationship the green wood of certain specific function
Material, always is the target that researcher seek assiduously, and how to summarize a large amount of rules of geodesic structure and with its performance, function phase
Connection, especially mono-crystalline structures design, biological structure and function contact, to the material and drug for manufacturing and designing human needs
Etc. indispensable.
The rapid progress of X-ray diffraction technology develops by the continuous renewal of experimental method, and new methodology starts, new
EM equipment module exploitation is all significant, the appearance of steam treated methodology in situ so that some pilot process are observed so that
The continuity of data analysis is guaranteed that test result is more reasonable, but stronger, the faster steam of test speed compatible simultaneously
Processing module is urgently developed.The solution of many problem in science will rely on technique.
Existing X-ray diffractometer lack can provide solvent environment and the test on environment in diffractometer without influence original position it is attached
Part cannot achieve and characterize in solvent vapour treatment process to the real-time in-situ of material microstructure variation.
Summary of the invention
It is an object of the invention to propose a kind of X-ray diffractometer solvent vapour processing in-situ test attachment, existing X is solved
X ray diffractometer x cannot achieve the problem of characterizing in solvent vapour treatment process to the real-time in-situ of material microstructure variation, more
The missing of X-ray diffractometer situ solvent steam treated procedural test function is mended.
To achieve the above object, X-ray diffractometer solvent vapour of the invention processing in-situ test attachment includes producing gas dress
It sets, sample room and gas chromatograph；
Including at least air inlet, gas outlet and sample room side wall is arranged in the sample room generally sealing structure
Two X-ray transmission windows are provided with sample stage in the sample room；
The exhaust outlet of the aerogenesis apparatus is connected to by gas circuit pipe with the air inlet of the sample room；The sample room goes out
Port is connected to by gas circuit pipe with the injection port of the gas chromatograph；The incident X-rays of X-ray diffractometer are through an X-ray
Transmissive window is radiated on the sample on the sample stage, and the diffracted signal of generation is emitted through another X-ray transmission window.
The sample room further include sample room ontology and with sample room ontology upper end opening be tightly connected upper cover, it is described
On the cover, the air inlet and the gas outlet and the gas circuit pipe pass through tapered for air inlet and gas outlet setting
Silicone rubber seal washer and tapered nut are tightly connected.
The upper cover and the sample room are threadedly coupled, and are set between upper cover lower end surface and sample room opening upper surface
It is equipped with washer.
The sample room further includes being located at the indoor air inlet pipe and an air outlet pipe of sample；Described air inlet pipe one end and the sample
The air inlet of room is tightly connected by tapered silicone rubber seal washer and tapered nut, and the other end extend into sample room bottom, institute
The gas outlet for stating escape pipe one end and the sample room is tightly connected by tapered silicone rubber seal washer and tapered nut.
The air inlet pipe and the escape pipe are stainless steel or polyethylene material.
The in-situ test attachment further includes sample holder, and the sample room is located on the sample holder.
The sample room material is aluminium or polytetrafluoroethylene (PTFE) material.
The invention has the benefit that X-ray diffractometer solvent vapour processing in-situ test attachment of the invention can be real
Show the in situ X-ray diffraction diffraction test function of solvent vapour treatment process, material crystalline in available solvent vapour treatment process
The variation of structure.Relevant further investigation can further parse crystalline texture variation mechanism, for regulation crystalline texture and its
Relevant performance provides strong data supporting；Actual products application can be deeply applied to later to come in the process further
Improve the performance of product.
In terms of the crystal growth, macromolecule membrane mutually separate with wetting removal in terms of, organic polymer photoelectric material and device
Aspect, methylamine lead iodine perovskite solar battery aspect, fibrous material structure regulating etc. have very big application prospect.
The present invention also can be used as standard component and be applied on other diffractometers or synchrotron radiation X ray device, and have
Certain commercialization promotional value.Especially the latter, due to its high brightness, rapid survey ability, it can be achieved that even at several seconds
The variation of crystalline texture or even micro-structure under several milliseconds of time scale during test solvent steam treated, the present invention and same
The combination for walking radiation X ray diffraction device will provide stronger technological means to the development of the following scientific research and support.
Detailed description of the invention
Fig. 1 is that X-ray diffractometer solvent vapour of the invention handles in-situ test attachment overall structure diagram；
Fig. 2 is that X-ray diffractometer solvent vapour of the invention handles sample room structural schematic diagram in in-situ test attachment；
Wherein: 1, aerogenesis apparatus, 101, exhaust outlet, 2, gas circuit pipe, 3, sample room, 301, air inlet, 302, gas outlet,
303, X-ray transmission window, 304, sample stage, 305, sample room ontology, 306, upper cover, 307, air inlet pipe, 308, escape pipe, 4, gas
Chromatography, 5, sample holder, 6, sample, 7, X-ray diffractometer.
Specific embodiment
Embodiments of the present invention are described further with reference to the accompanying drawing.
Referring to attached drawing 1 and attached drawing 2, X-ray diffractometer solvent vapour processing in-situ test attachment of the invention includes producing gas
Device 1, sample room 3 and gas chromatograph 4；
The sample room 3 generally sealing structure includes at least air inlet 301, gas outlet 302 and is arranged in sample room
Two X-ray transmission windows 303 of 3 side walls are provided with sample stage 304 in the sample room 3；The X-ray transmission window 303 can be with
It is polyimides window.
The exhaust outlet 101 of the aerogenesis apparatus 1 is connected to by gas circuit pipe 2 with the air inlet 301 of the sample room 3；It is described
The gas outlet 302 of sample room 3 is connected to by gas circuit pipe 2 with the injection port of the gas chromatograph 4；The incidence of X-ray diffractometer 7
X-ray is radiated on the sample 6 on the sample stage 304 through an X-ray transmission window 303, and the diffracted signal of generation is through another
A outgoing of X-ray transmission window 303 is simultaneously received by the detector of X-ray diffractometer 7.
The sample room 3 further includes sample room ontology 305 and is tightly connected with 305 upper end opening of sample room ontology upper
Lid 306, the air inlet 301 and the gas outlet 302 are arranged in the upper cover 306, the air inlet 301 and the outlet
Mouth 302 passes through tapered silicone rubber seal washer with the gas circuit pipe 2 and tapered nut realizes close connection.
The upper cover 306 and the sample room 3 are threadedly coupled, 3 opening upper end of 306 lower end surface of upper cover and the sample room
Washer is provided between face.
The sample room 3 further includes air inlet pipe 307 and escape pipe 308 in sample room 3；The air inlet pipe 307 1
The air inlet 301 of end and the sample room 3 realizes air-tight connection, the other end by tapered silicone rubber seal washer and tapered nut
It extend into 3 bottom of sample room, the gas outlet 302 of described 308 one end of escape pipe and the sample room 3 passes through tapered silicone rubber seal
Washer and tapered nut, which are realized, to be tightly connected, and the other end is located at 3 top of sample room.
The air inlet pipe 307 and the escape pipe 308 are stainless steel or polyethylene material.
The in-situ test attachment further includes sample holder 5, and the sample room 3 is located on the sample holder 5.Sample branch
Frame 5 is arranged on the table.
3 material of sample room is aluminium or polytetrafluoroethylene (PTFE) material.
Type of solvent caused by aerogenesis apparatus 1 of the invention is a variety of, such as vapor, organic solvent or corrosive gas
Deng；6 wide variety of sample placed on sample stage 304, such as film, powder or fiber.
By taking film sample as an example, liquid solvent can be washed into gas by the aerogenesis apparatus 1, enter gas through exhaust outlet 101
In road pipe 2, and then the air inlet 301 of sample room 3 is reached, reaches 3 bottom of sample room through air inlet pipe 307, in sample room 3 gradually
Form solvent vapour atmosphere；The incident X-rays of the X-ray diffractometer 7 are radiated at the sample stage through X-ray transmission window 303
On sample 6 on 304, the diffracted signal of generation is emitted through another X-ray transmission window 303 and is diffracted the detector of instrument and connects
It receives；Meanwhile the gas in the sample room 3 can be entered by gas outlet 302 and gas circuit pipe 2 gas chromatograph 4 into
Sample mouth is simultaneously collected, detects.
Claims (7)
1.X x ray diffractometer x solvent vapour handles in-situ test attachment, which is characterized in that including aerogenesis apparatus (1), sample room
(3) and gas chromatograph (4)；
The sample room (3) generally sealing structure includes at least air inlet (302), gas outlet (301) and is arranged in sample
Two X-ray transmission windows (303) of room (3) side wall, the sample room (3) is interior to be provided with sample stage (304)；
The exhaust outlet (101) of the aerogenesis apparatus (1) is connected by the air inlet (302) of gas circuit pipe (2) and the sample room (3)
It is logical；The gas outlet (301) of the sample room (3) is connected to by gas circuit pipe (2) with the injection port of the gas chromatograph (4)；X is penetrated
Line diffractometer (7) is through X-ray transmission window (303) incident X-rays and the sample (6) that is radiated on the sample stage (304)
On, the diffracted signal of generation is emitted through another X-ray transmission window (303).
2. X-ray diffractometer solvent vapour according to claim 1 handles in-situ test attachment, which is characterized in that described
Sample room (3) further includes sample room ontology (305) and the upper cover with the sealed connection of sample room ontology (305) upper end opening
(306), the air inlet (302) and the gas outlet (301) are arranged on the upper cover (306), the air inlet (302) and
The gas outlet (301) and the gas circuit pipe (2) are tightly connected by tapered silicone rubber seal washer and tapered nut.
3. X-ray diffractometer solvent vapour according to claim 2 handles in-situ test attachment, which is characterized in that described
Upper cover (306) and the sample room (3) are threadedly coupled, upper cover (306) lower end surface and the sample room (3) opening upper surface it
Between be provided with washer.
4. X-ray diffractometer solvent vapour according to claim 2 or 3 handles in-situ test attachment, which is characterized in that institute
Stating sample room (3) further includes air inlet pipe (307) and escape pipe (308) in sample room (3)；The air inlet pipe (307) one
The air inlet (302) of end and the sample room (3) is tightly connected by tapered silicone rubber seal washer and tapered nut, the other end
It extend into sample room (3) bottom, the gas outlet (301) of described escape pipe (308) one end and the sample room (3) passes through tapered silicon
Rubber gasket and tapered nut are tightly connected.
5. X-ray diffractometer solvent vapour according to claim 4 handles in-situ test attachment, which is characterized in that described
Air inlet pipe (307) and the escape pipe (308) are stainless steel tube or polyethylene material.
6. X-ray diffractometer solvent vapour according to claim 1,2 or 3 handles in-situ test attachment, which is characterized in that
The in-situ test attachment further includes sample holder (5), and the sample room (3) is located on the sample holder (5).
7. X-ray diffractometer solvent vapour according to claim 1,2 or 3 handles in-situ test attachment, which is characterized in that
Sample room (3) material is aluminium or polytetrafluoroethylene (PTFE) material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910347086.8A CN110031492A (en) | 2019-04-26 | 2019-04-26 | X-ray diffractometer solvent vapour handles in-situ test attachment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910347086.8A CN110031492A (en) | 2019-04-26 | 2019-04-26 | X-ray diffractometer solvent vapour handles in-situ test attachment |
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| Publication Number | Publication Date |
|---|---|
| CN110031492A true CN110031492A (en) | 2019-07-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910347086.8A Pending CN110031492A (en) | 2019-04-26 | 2019-04-26 | X-ray diffractometer solvent vapour handles in-situ test attachment |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH085800A (en) * | 1994-06-22 | 1996-01-12 | Nikon Corp | X-ray microscope |
| JP2005221362A (en) * | 2004-02-05 | 2005-08-18 | Rigaku Corp | X-ray analyzer and sample analysis system |
| CN204439582U (en) * | 2015-03-19 | 2015-07-01 | 中国科学院兰州化学物理研究所 | Polycrystal X ray diffraction-photocatalysis coupling in-situ characterization analytic system |
| CN106645075A (en) * | 2017-03-01 | 2017-05-10 | 金华职业技术学院 | Device used for in situ measurement of solvent vapor expansion in polymer thin film |
| CN108918323A (en) * | 2018-07-24 | 2018-11-30 | 山西中谱能源科技有限公司 | The physical chemistry system that solid, liquid two-phase material mass and spectrum measure simultaneously off field |
-
2019
- 2019-04-26 CN CN201910347086.8A patent/CN110031492A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH085800A (en) * | 1994-06-22 | 1996-01-12 | Nikon Corp | X-ray microscope |
| JP2005221362A (en) * | 2004-02-05 | 2005-08-18 | Rigaku Corp | X-ray analyzer and sample analysis system |
| CN204439582U (en) * | 2015-03-19 | 2015-07-01 | 中国科学院兰州化学物理研究所 | Polycrystal X ray diffraction-photocatalysis coupling in-situ characterization analytic system |
| CN106645075A (en) * | 2017-03-01 | 2017-05-10 | 金华职业技术学院 | Device used for in situ measurement of solvent vapor expansion in polymer thin film |
| CN108918323A (en) * | 2018-07-24 | 2018-11-30 | 山西中谱能源科技有限公司 | The physical chemistry system that solid, liquid two-phase material mass and spectrum measure simultaneously off field |
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Application publication date: 20190719 |
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