阅读说明：本技术 一种小角中子散射谱仪的原位搅拌连续进样装置 (In-situ stirring continuous sample introduction device of small-angle neutron scattering spectrometer ) 是由 黄粒朝 刘栋 杨敬浩 税悦 王亭亭 陈良 孙良卫 孙光爱 龚建 于 2019-11-12 设计创作，主要内容包括：本发明公开了一种用于小角中子散射谱仪的原位搅拌连续进样装置,该装置通过计算机控制的伺服电机带动焊接有比色皿池的带中子束入射孔的样品板定时定位移动以实现自动连续进样的目的；装有样品和磁力搅拌子的比色皿放置于比色皿池中,通过计算机控制磁力搅拌器以不同转速带动磁力搅拌子连续搅拌,以实现在自动连续进样的同时实现样品的连续搅拌。本发明提供的技术方案能够实现与小角中子散射易聚沉、沉降的胶体、粒子分散系样品的原位结构演化测试,且具有安装简易、容易拆卸、防止沉降、位移精确、自动化、节省人力等人优点,适用于小角中子散射研究中对于胶体、粒子分散系等易聚沉体系的微结构演化测试。(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.)

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.

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.