CN110632106A - In-situ stirring continuous sample introduction device of small-angle neutron scattering spectrometer - Google Patents
In-situ stirring continuous sample introduction device of small-angle neutron scattering spectrometer Download PDFInfo
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- 238000001998 small-angle neutron scattering Methods 0.000 title claims abstract description 46
- 238000003756 stirring Methods 0.000 title claims abstract description 37
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 29
- 238000005070 sampling Methods 0.000 claims abstract description 25
- 238000002347 injection Methods 0.000 claims abstract description 13
- 239000007924 injection Substances 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 9
- 238000002474 experimental method Methods 0.000 claims description 10
- 238000001956 neutron scattering Methods 0.000 claims description 9
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- 230000004913 activation Effects 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000007769 metal material Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 18
- 239000000377 silicon dioxide Substances 0.000 description 9
- 235000012239 silicon dioxide Nutrition 0.000 description 8
- 238000000034 method Methods 0.000 description 7
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- 239000002131 composite material Substances 0.000 description 4
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- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 229910052805 deuterium Inorganic materials 0.000 description 2
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- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
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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
- G01N23/201—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 by measuring small-angle scattering
- G01N23/202—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 by measuring small-angle scattering using neutrons
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/054—Investigating materials by wave or particle radiation by diffraction, scatter or reflection small angle scatter
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/106—Different kinds of radiation or particles neutrons
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Abstract
The invention discloses an in-situ stirring continuous sampling device for a small-angle neutron scattering spectrometer, which drives a sample plate with a neutron injection hole, which is welded with a cuvette cell, to be positioned and moved at regular time through a servo motor controlled by a computer so as to realize the purpose of automatic continuous sampling; the cuvette filled with the sample and the magnetic stirrer is placed in the cuvette pool, and the magnetic stirrer is controlled by the computer to drive the magnetic stirrer to continuously stir at different rotating speeds so as to realize continuous stirring of the sample while realizing automatic continuous sample introduction. The technical scheme provided by the invention can realize the in-situ structure evolution test of the colloid and particle dispersion system samples which are easy to aggregate and settle in small-angle neutron scattering, has the advantages of simple installation, easy disassembly, settlement prevention, accurate displacement, automation, labor saving and the like, and is suitable for the microstructure evolution test of the colloid, particle dispersion system and other easy-to-aggregate systems in small-angle neutron scattering research.
Description
Technical Field
The invention belongs to the technical field of neutron scattering in-situ automatic measurement, and particularly relates to an in-situ stirring continuous sample introduction device for a small-angle neutron scattering spectrometer.
Background
Small-angle neutron scattering is a special measurement technique for investigating the structure of matter in the size range of a few to hundreds of nanometers by analyzing the scattering intensity of long-wavelength neutrons (around 0.2-2 nm) in a small angle range (approximately below 2 °). Therefore, the small-angle neutron scattering technology can be used for in-situ detection of polymers, biomacromolecules, colloidal solutions and the like.
In the research of materials such as soft substances (macromolecules, biomacromolecules, gel and the like), the small-angle neutron scattering method has unique advantages in deuterium labeling and contrast change. By utilizing the ability of neutrons to discriminate between hydrogen and deuterium isotopes, isotope substitution can be utilized to enhance or change the contrast without changing the chemical composition of the system. This makes the small-angle neutron scattering method an effective means for the structural characterization of colloid or nanoparticles with molecular chains grafted on the surface. However, the time resolution of neutron scattering has been limited by the beam intensity. For concentrated colloidal dispersions with weak signals or insoluble nanoparticles, long-term experiments will result in coagulation of the colloid or sedimentation of the particles, thus making the experiments impossible.
At present, the neutron scattering (diffraction) technology in China is in a starting stage, and a matching device which is designed and researched aiming at a neutron scattering (diffraction) spectrometer and has continuous sample feeding and stirring functions is not found. However, the X-ray is not suitable for researching the single molecular chain conformation problem, and similar exploration based on a synchrotron radiation light source and a commercial light source is not found. Although great importance is attached to the development and application of the small-angle neutron scattering technology internationally, and the shear rheological devices on a part of small-angle neutron scattering platforms can realize neutron scattering tests in a stirring state, the devices have large sample quantity, need manual sample changing and cannot continuously send samples. Especially for samples with multiple types and small sample amount, the testing work cannot be efficiently or even cannot be completed.
Disclosure of Invention
Aiming at the problems, the invention provides an in-situ stirring continuous sampling device for a small-angle neutron scattering spectrometer, which drives a sample plate with a neutron injection hole and a cuvette pool welded by a servo motor controlled by a computer to be positioned and moved at fixed time so as to realize the purpose of automatic continuous sampling; the cuvette filled with the sample and the magnetic stirrer is placed in the cuvette pool, and the magnetic stirrer is controlled by the computer to drive the magnetic stirrer to continuously stir at different rotating speeds so as to realize continuous stirring of the sample while realizing automatic continuous sample introduction.
The utility model provides an in situ stirring continuous sampling device for small-angle neutron scattering spectrometer, goes into perforated sample board, cell pool including taking the neutron beam, take the neutron beam to go into to be equipped with the cell pool on the perforated sample board, be equipped with the cell in the cell pool, cell pool outside is equipped with magnetic stirrers, takes the neutron beam to go into the perforated sample board and has the guide rail, guide rail one end is equipped with servo motor, the servo motor output is connected with the screw rod, has cup jointed the slider on the screw rod, the slider is connected with the sample board of taking the neutron beam to go into the perforation, takes the neutron beam to go into perforated sample board one side and is equipped with the computer.
Further, a base is arranged below the magnetic stirrer; the guide rail is arranged on the upper part of the base and is fixedly connected with the base.
And a magnetic stirrer is placed in the cuvette.
The base is fixed on a working platform of the small-angle neutron scattering spectrometer through a buckle. The quick-release fixing method of the buckle is adopted, so that the accuracy of the fixing position can be ensured, the neutron beam incidence windows before and after the sample is replaced are all at the same position, the manpower is greatly saved, and the possibility of misoperation is reduced.
Further, the magnetic stirrer is arranged below the cuvette pool. The magnetic stirrer is fixed in the center of the base in an embedded mode, so that the firmness is improved.
Further, the cuvette pool is welded and fixed below the hole of the sample plate with the neutron inlet hole.
Furthermore, the holes of the sample plate with the neutron injection holes are circular holes with the same diameter and the same distance, so that the incident neutron intensity passing through each hole is ensured, and the positions irradiating the sample are the same.
The guide rail, the sample plate with the neutron beam injection hole, the cuvette pool, the sliding block and the screw are made of metal materials resistant to neutron activation, such as stainless steel, aluminum and chromium, and safety of the device after a neutron scattering experiment can be guaranteed.
The small-angle neutron scattering spectrometer is one of a reactor neutron source, a pulse reactor neutron source or a spallation neutron source.
The main working process of the in-situ stirring continuous sampling device for the small-angle neutron scattering spectrometer and the small-angle neutron scattering experiment station in combination is as follows:
a. the in-situ stirring continuous sampling device for the small-angle neutron scattering spectrometer is clamped on a small-angle neutron scattering experimental line station through a base, a light path for small-angle neutron scattering is adjusted by a laser light source, a neutron beam spot and the center of a neutron beam incident hole are on the same central axis, and then the position of the base is fixed.
b. And taking the in-situ stirring continuous sampling device for the small-angle neutron scattering spectrometer down from the base, respectively filling a series of samples to be tested into the cuvette, and adding the magnetic stirrers.
c. The device is integrally installed on a small-angle neutron scattering experiment line station, and a computer power supply is started;
d. opening a software control window of a computer, setting the movement time interval and each movement distance of the servo motor, and ensuring that the servo motor moves to the next neutron beam injection hole each time; starting a magnetic stirrer and setting a stirring speed; and sets the time interval of the acquisition software and is linked with the servo motor.
e. And opening a second gate of the small-angle neutron scattering spectrometer, starting a neutron light source, starting a timing positioning movement control program and a small-angle neutron scattering acquisition program, setting corresponding acquisition time, activating linkage, and starting testing.
f. Molecular chain conformation information of the sample under different conditions is finally obtained by analyzing neutron scattering data of different samples under different rotating speed conditions in a suspension state.
The technical scheme provided by the invention has the following beneficial effects:
the slide block can realize continuous automatic sample changing under the mechanical motion of a screw rod controlled by a servo motor, the magnetic stirrer can realize the consistency of rotating speeds, and a computer can control the sample plate with a neutron injection hole driven by the slide block to be positioned and moved at regular time to be synchronous with an acquisition system of a small-angle neutron scattering spectrometer; the whole system can realize the small-angle neutron scattering test of colloid and particle dispersion systems.
The in-situ stirring continuous sampling device for the small-angle neutron scattering spectrometer can realize the application of in-situ stirring continuous sampling conditions combined with the small-angle neutron scattering spectrometer, solves the contradiction between weak small-angle neutron scattering signals and colloid and the easiness in coagulation and sedimentation of particle dispersion systems, has the advantages of simplicity in installation, easiness in disassembly, time synchronization, accuracy in strain, automation, labor saving and the like, and is suitable for observing the surface molecular chains and the self-assembly behaviors of particles with different stirring rates, different concentrations and different concentrations.
Drawings
FIG. 1 is a structural diagram of an in-situ stirring continuous sampling device for a small-angle neutron scattering spectrometer according to the present invention;
FIG. 2 is a schematic view of a cuvette cell welding position;
in the figure, 1, a computer, 2, a base, 3, a magnetic stirrer, 4, a servo motor, 5, a guide rail, 6, a sample plate with a neutron injection hole, 7, a cuvette cell, 8, a slide block, 9, a screw, 10, a cuvette and 11, a magnetic stirrer are arranged.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The utility model provides an in situ stirring continuous sampling device for small-angle neutron scattering spectrometer, goes into perforated sample board 6, cell pool 7 including taking the neutron beam, it is equipped with cell pool 7 on going into perforated sample board 6 to take the neutron beam, be equipped with the cell in the cell pool 7, cell pool outside is equipped with magnetic stirrers 3, take the neutron beam to go into perforated sample board 6 and have guide rail 5, 5 one end of guide rail are equipped with servo motor 4, the 4 output of servo motor is connected with screw rod 9, slider 8 has been cup jointed on the screw rod 9, slider 8 is connected with the sample board 6 that takes the neutron beam to go into the perforation, 6 one side of taking the neutron beam to go into perforated sample board is equipped with computer 1.
A base 2 is arranged below the magnetic stirrer 3; the guide rail 5 is arranged on the upper part of the base 2 and is fixedly connected with the base 2.
A magnetic stirrer 11 is placed in the cuvette 10.
The base 2 is fixed on a working platform of the small-angle neutron scattering spectrometer through a buckle.
The magnetic stirrer is arranged below the cuvette pool. The magnetic stirrer 3 is fixed in the center of the base 2 in an embedded manner, so that the stability is improved.
The cuvette pool 7 is welded and fixed below the hole of the sample plate 6 with the neutron incident hole.
The sample plate 6 holes with neutron injection holes are circular holes with the same diameter and the same distance, so that the incident neutron intensity passing through each hole is ensured, and the irradiation positions of the samples are the same.
The guide rail 5, the sample plate 6 with the neutron beam injection hole, the cuvette pool 10, the slide block 8 and the screw 9 are made of metal materials resistant to neutron activation, such as stainless steel, aluminum and chromium, and can ensure the safety of the device after a neutron scattering experiment.
The small-angle neutron scattering spectrometer is one of a reactor neutron source, a pulse reactor neutron source or a spallation neutron source.
Example 1
The polymer chains on the surface of the silicon dioxide with different surface grafting densities and chain lengths are wound and self-assembled.
Purpose of the experiment:
the silicon dioxide nano particles are widely applied to the reinforcement of various composite materials due to high specific surface area and high surface energy, and the surface chemical grafting can effectively improve the dispersion degree of the silicon dioxide particles in a high polymer material and interact with a polymer so as to further improve the mechanical property of the composite material, so that the understanding of the particle-particle interaction and the particle-polymer interaction becomes a key point. By utilizing a grafting method, deuterated polymer chains with different grafting densities and different molecular chain lengths are grafted on the surface of the silicon dioxide, so that the particle-particle interaction is adjusted. The experiment aims to compare the difference between molecular chains on the surface of particles in a colloidal state and a composite material, and the winding and self-assembly behaviors of the molecular chains on the surface of silicon dioxide in the colloidal state are researched by stirring and keeping the particles suspended. Thereby understanding the particle-particle interactions in composite reinforcement and thereby providing a design concept for new fillers.
The experimental process comprises the following steps:
toluene diisocyanate is used as a connecting agent, polyethylene glycol monomethyl ether molecular chains with different molecular chain lengths are grafted on the surface of the silicon dioxide, and the surface grafting density is regulated and controlled by changing the proportion of the silicon dioxide and the polyethylene glycol monomethyl ether, so that a series of silicon dioxide with different grafting densities and grafting chain lengths is obtained. The grafted silica was dispersed in toluene, respectively, and loaded into a cuvette with a magnetic stirrer, and placed on a sample plate. The stirring speed is set to be 600 revolutions per minute through a computer, so that the samples are always in a suspension dispersion state, the testing time of each sample is set to be 30 minutes, each sample moves 2cm to the next sample, and the small-angle neutron scattering collection is set according to the same time. The sample-to-detector distance of the small-angle neutron scattering spectrometer was set to 10 m. And starting the continuous sampling device and the small-angle scattering acquisition program, positioning and moving the sample plate with the neutron beam injection perforation from left to right according to the set program, and automatically stopping working after the test of the last sample is finished. In the embodiment, the in-situ stirring continuous sampling device is combined with a neutron small-angle scattering spectrometer, so that the surface molecular chain winding and self-assembly behavior evolution in different grafting states is obtained; meanwhile, after the early-stage experiment program is set, the whole experiment process within about 5 hours can be monitored through remote control, and manpower and material resources are saved.
Claims (10)
1. The utility model provides an in situ stirring continuous sampling device for small-angle neutron scattering spectrometer, go into perforated sample board (6), cell pool (7) including taking the neutron beam, a serial communication port, be equipped with cell pool (7) on taking neutron beam to go into perforated sample board (6), be equipped with cell (10) in cell pool (7), cell pool (7) outside is equipped with magnetic stirrers (3), it has guide rail (5) to take neutron beam to go into perforated sample board (6), guide rail (5) one end is equipped with servo motor (4), servo motor (4) output is connected with screw rod (9), slider (8) have been cup jointed on screw rod (9), slider (8) are connected with sample board (6) of taking the neutron beam to go into the perforation, it is equipped with computer (1) to take neutron beam to go into perforated sample board (6) one side.
2. The in-situ stirring continuous sampling device according to claim 1, wherein a base (2) is arranged below the magnetic stirrer (3); the guide rail (5) is arranged on the upper part of the base (2) and is fixedly connected with the base (2).
3. The in-situ stirring continuous sampling device according to claim 1, wherein a magnetic stirrer (11) is placed in the cuvette (10).
4. The in-situ stirring continuous sampling device according to claim 2, wherein the base (2) is fixed on a working platform of the small-angle neutron scattering spectrometer by a buckle.
5. The in-situ stirring continuous sampling device according to claim 2, wherein the magnetic stirrer (3) is fixed at the center inside the base (2) in an embedded manner.
6. The in-situ stirring continuous sampling device according to claim 1, wherein the cuvette cell (7) is fixed by welding below the hole of the sample plate (6) with neutron incidence.
7. The in-situ stirring continuous sampling device as claimed in claim 1, wherein the sample plate (6) holes with neutron injection holes are circular holes with the same diameter and the same interval.
8. The in-situ stirring continuous sampling device according to claim 1, wherein the materials of the guide rail (5), the sample plate (6) with neutron injection holes, the cuvette cell (10), the slide block (8) and the screw (9) are metallic materials resistant to neutron activation, and are stainless steel, aluminum and chromium.
9. The in-situ stirring continuous sampling device according to claim 1, wherein the small-angle neutron scattering spectrometer is one of a reactor neutron source, a pulse reactor neutron source or a spallation neutron source.
10. The in-situ stirring continuous sampling device according to any one of claims 1 ~ 9, wherein the device is operated as follows:
a. clamping an in-situ stirring continuous sample introduction device for a small-angle neutron scattering spectrometer on a small-angle neutron scattering experimental line station through a base, adjusting a light path of small-angle neutron scattering by using a laser light source to enable a neutron beam spot and the center of a neutron beam incident hole to be on the same central axis, and fixing the position of the base;
b. taking down an in-situ stirring continuous sampling device for a small-angle neutron scattering spectrometer from a base, respectively loading a series of samples to be tested into a cuvette and adding a magnetic stirrer;
c. the device is integrally installed on a small-angle neutron scattering experiment line station, and a computer power supply is started;
d. opening a software control window of a computer, setting the movement time interval and each movement distance of the servo motor, and ensuring that the servo motor moves to the next neutron beam injection hole each time; starting a magnetic stirrer and setting a stirring speed; setting a time interval of acquisition software, and linking with a servo motor;
e. opening a second gate of the small-angle neutron scattering spectrometer, starting a neutron light source, starting a timing positioning movement control program and a small-angle neutron scattering acquisition program, setting corresponding acquisition time, activating linkage, and starting testing;
f. molecular chain conformation information of the sample under different conditions is finally obtained by analyzing neutron scattering data of different samples under different rotating speed conditions in a suspension state.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111167536A (en) * | 2020-02-12 | 2020-05-19 | 大连理工大学 | In-situ stirring reaction sample stage |
| CN111707690A (en) * | 2020-07-22 | 2020-09-25 | 中国工程物理研究院核物理与化学研究所 | Precession magnetic field generating device for spin echo small-angle neutron scattering spectrometer |
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