CN216771563U

CN216771563U - In-situ solvent vapor treatment test accessory for X-ray diffractometer

Info

Publication number: CN216771563U
Application number: CN202123090557.3U
Authority: CN
Inventors: 张吉东; 孟圣斐; 宋新月
Original assignee: Suzhou Liying Technology Co ltd
Current assignee: Suzhou Liying Technology Co ltd
Priority date: 2021-12-10
Filing date: 2021-12-10
Publication date: 2022-06-17
Anticipated expiration: 2031-12-10

Abstract

The utility model discloses an in-situ solvent vapor treatment test accessory for an X-ray diffractometer, wherein the side wall of a test cavity is provided with two transmission windows for X-rays to sequentially pass through, a sample table is detachably arranged at the inner side of the test cavity along a transmission or reflection direction and is positioned between an incident window and an exit window, the sample table is provided with a light transmission part for arranging a sample, the X-rays passing through one transmission window pass through the sample and the light transmission part positioned at the transmission direction, or are emitted out through the other transmission window after being reflected by the sample and the light transmission part positioned at the reflection direction, the two arrangement directions of the sample table in the test cavity are adjusted, the sample table is positioned in the reflection path of the X-rays or positioned in the transmission path of the X-rays, the sample table is arranged in two postures in the same test cavity, and is matched with the X-ray diffractometer at the outer side of the test cavity, so that two test modes of reflection and transmission of the sample on the sample table can be completed, the problem that different test accessories need to be replaced in different test modes is solved.

Description

In-situ solvent vapor treatment test accessory for X-ray diffractometer

Technical Field

The utility model relates to the field of X-ray diffraction tests, in particular to an in-situ solvent vapor treatment test accessory for an X-ray diffractometer.

Background

In the prior art, due to the discovery of the X-ray crystal diffraction phenomenon, X-ray diffraction has long been used as an effective tool for researching the fine structure of a substance, and crystal structure information, such as cell parameters, crystal systems, space groups, the number of molecules in a cell, calculated density and the like, and molecular structure information, such as bond length, bond angle, non-bond distance, hydrogen bond, conformation, torsion angle and the like, even atom detailed information can be calculated through the test result of X-ray diffraction. The method of predicting the performance of a known sample structure or designing a new material with a specific function according to the known structure and performance relationship is always the aim of researchers, and how to summarize the rules of a large number of measured structures and relate the performance and the functions of the structures, particularly the design of a single crystal structure, the connection between a biological structure and a function and the like is indispensable for designing and manufacturing materials, medicines and the like required by human beings. The long-term progress of the X-ray diffraction technology depends on the continuous updating and development of an experimental method, the creation of a new methodology and the development of a new equipment module have great significance, the in-situ steam treatment methodology enables some intermediate processes to be observed, the continuity of data analysis is guaranteed, the test result is more reasonable, and meanwhile, a steam treatment module with stronger compatibility and higher test speed needs to be developed urgently. The resolution of many scientific problems will depend on this technology.

Patent document CN110031492A discloses an X-ray diffractometer solvent vapor treatment in-situ test accessory, which comprises a gas production device, a sample chamber and a gas chromatograph; the sample chamber is integrally of a sealing structure and at least comprises an air inlet, an air outlet and two polyimide windows arranged on the side wall of the sample chamber, and a sample table is arranged in the sample chamber; the exhaust port of the gas production device is communicated with the gas inlet of the sample chamber through a gas path pipe; the gas outlet of the sample chamber is communicated with the sample inlet of the gas chromatograph through a gas path pipe; the X-ray diffractometer is used for inputting X-rays through one polyimide window and irradiating the X-rays on a sample on the sample stage, and a generated diffraction signal is emitted through the other polyimide window. Patent document CN204439582U discloses a polycrystal X-ray diffraction-photocatalysis combined in-situ characterization analysis system, which comprises a polycrystal X-ray diffractometer, a gas chromatograph, a solar simulator and a photocatalytic reactor arranged on a sample stage of the polycrystal X-ray diffractometer, wherein the photocatalytic reactor consists of a sample holder and an outer cover connected with the sample stage; the outer cover comprises a stainless steel hollow cylinder body and a stainless steel bottom plate, wherein the stainless steel hollow cylinder body is provided with a window, an air inlet and an air outlet, and the stainless steel bottom plate is connected with the bottom end of the cylinder body; the window is arranged right above the cylinder body and extends to the two sides of the cylinder body; the gas inlet is connected with a gas cylinder arranged outside the polycrystalline X-ray diffractometer through a pressure reducing valve and a gas flowmeter, and the gas outlet is connected with a sample introduction system of a gas chromatograph arranged outside the polycrystalline X-ray diffractometer through the gas flowmeter; the solar simulator is arranged in the polycrystalline X-ray diffractometer, and the optical fiber port of the solar simulator is positioned right above the window of the photocatalytic reactor. However, in both of the above two solutions, the test of the sample in the reflection mode can be performed only, and different test accessories need to be replaced in different test modes, which inevitably easily causes complication in the test process.

SUMMERY OF THE UTILITY MODEL

The utility model aims to provide an in-situ solvent vapor treatment test accessory for an X-ray diffractometer, which aims to solve the problems in the prior art, a sample table can be detachably arranged at the inner side of a test cavity along a transmission or reflection direction, two test modes of reflection and transmission for a sample on the sample table are supported, and the problem that different test accessories need to be replaced in different test modes in the past test is solved.

In order to achieve the purpose, the utility model provides the following scheme: the utility model provides an in-situ solvent vapor treatment test accessory for an X-ray diffractometer, which comprises a test cavity and a sample table, wherein the side wall of the test cavity is provided with two transmission windows for X-rays to sequentially pass through, the sample table is detachably arranged on the inner side of the test cavity along a transmission or reflection direction and is positioned between the two transmission windows, the sample table is provided with a light transmission part for arranging a sample, the X-rays passing through one transmission window pass through the sample and the light transmission part positioned in the transmission direction, or are reflected by the sample and the light transmission part positioned in the reflection direction and then are emitted out through the other transmission window, a solvent vapor atmosphere is arranged in the test cavity, and the light transmission part is positioned in the solvent vapor atmosphere.

Preferably, the two transmission windows are symmetrically arranged on two sides of the light transmission part.

Preferably, a plurality of clamping grooves are formed in the inner side of the testing cavity, and the sample table is inserted into the corresponding clamping grooves in a sliding mode along the transmission or reflection direction.

Preferably, a plurality of absorbent cottons soaked with the volatile solvent are arranged on the sample table, and each absorbent cotton is surrounded around the light transmission part.

Preferably, the whole test cavity is of a closed structure, the closed structure is provided with an opening for the sample stage to enter and exit, and the opening is detachably connected with a sealing cover.

Preferably, the sealing cover is provided with a plurality of closable through holes for feeding the volatilizable solvent.

Preferably, each of the closable through holes faces the carrying side of the light-transmitting portion.

Preferably, the whole testing cavity is of a cylindrical structure, the transmission window is arranged on the circumferential wall of the cylindrical structure, and the sample stage located in the transmission or reflection direction extends along the axis of the cylindrical structure.

Preferably, the two transmission windows are both arranged on the bearing side of the light transmission part positioned in the reflection direction, and at least part of the light transmission part positioned in the transmission direction is opposite to the two transmission windows.

Preferably, one of said transmission windows is adjacent to an X-ray diffractometer and the other of said transmission windows is adjacent to an X-ray diffractometer detector for receiving X-rays.

Compared with the prior art, the utility model has the following technical effects:

firstly, the side wall of the testing cavity is provided with two transmission windows for X-rays to sequentially pass through, the sample platform is detachably arranged at the inner side of the testing cavity along the transmission or reflection direction and is positioned between the two transmission windows, the sample platform is provided with a light transmission part for placing a sample, the X-rays passing through one transmission window pass through the sample and the light transmission part positioned at the transmission direction or are reflected by the sample and the light transmission part positioned at the reflection direction and then are emitted out through the other transmission window, namely, the two placing directions of the sample platform in the testing cavity are adjusted, the sample is carried to be positioned in the reflection path of the X-rays or positioned in the transmission path of the X-rays, and then two testing modes of reflection and transmission of the sample on the sample platform can be completed by placing the sample platform in two postures in the same testing cavity and matching with a corresponding X-ray diffractometer at the outer side of the testing cavity, the problem that different test accessories need to be replaced in different test modes is solved.

Secondly, the two transmission windows are symmetrically arranged on the two sides of the light transmission part, so that in the specific test process, for the reflection path, the two symmetrical transmission windows can better ensure the adjustable range of the reflection path, the asymmetry of the two transmission windows is avoided, wherein the movement adjusting range of the X-ray corresponding to the wider transmission window is easily limited by the narrower transmission window, and in the transmission path, the two transmission windows are more ensured to be positioned on the same straight line with the sample by the symmetrically arranged light transmission parts, so that the transmission test of the sample can be realized.

Thirdly, the inboard of test cavity is equipped with a plurality of draw-in grooves, and the sample platform slides along transmission or reflection position and pegs graft in corresponding draw-in groove, not only utilizes the draw-in groove to realize the fixed to the sample platform, moreover in concrete installation, only need with the sample platform push into, peg graft in corresponding draw-in groove can, guaranteed the swift convenient technological effect of sample platform installation.

Fourth, the test cavity is whole to be closed column structure, closed column structure is equipped with the opening that is used for the sample platform business turn over, the opening part can be dismantled and be connected with sealed lid, utilize absorbent cotton to soak behind the solvent that volatilizees, seal whole test cavity, the solvent that volatilizees in closed environment so volatilizees, and then fill whole enclosure space, and it is simple effective, and can form solvent vapour atmosphere fast, need not to set up two bleeder vents among the prior art to the test cavity, incessant through the bleeder vent to the test cavity let in solvent vapour, not only the structure is complicated, high cost, and lead to the waste of solvent vapour.

Fifthly, the two transmission windows are arranged on the bearing side of the light transmission part in the reflection position, and at least part of the light transmission part in the transmission position is opposite to the two transmission windows, so that in the process of actually installing the transmission windows, the arrangement area of the transmission windows is limited on the bearing side of the corresponding light transmission part, the realization of the path of the transmission sample is ensured, and the problem that the path of the X-ray is blocked due to the fact that the span of the transmission windows is too long and is easily influenced by the clamping groove is avoided, or part of the transmission windows are arranged on the side, not bearing the sample, of the light transmission part and cannot be used as the path of the X-ray, the waste of the transmission windows is caused, and the manufacturing cost is increased.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.

FIG. 1 is a schematic view of the overall structure of a sample stage in a reflection orientation;

FIG. 2 is a side view of the sample stage in a reflecting orientation;

FIG. 3 is a schematic diagram of the overall structure of the sample stage in the transmission orientation;

FIG. 4 is a side view of the sample stage in a transmissive orientation;

FIG. 5 is a schematic view of the overall structure of the sealing cap;

the device comprises a cylindrical structure 1, a sample platform 2, a transmission window 3, a transmission clamping groove 4, a transmission part 5, absorbent cotton 6, a reflection clamping groove 7, a sealing cover 8 and a through hole 9 which can be sealed.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious 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.

In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.

As shown in fig. 1 to 5, the present invention provides an in-situ solvent vapor treatment test accessory for an X-ray diffractometer, which comprises a test cavity and a sample stage 2, wherein the test cavity for solvent vapor treatment can be made of various materials, such as light and rust-resistant aluminum material, acid and alkali resistant polytetrafluoroethylene material, etc., the side wall of the test cavity is provided with two transmission windows 3 for X-rays to sequentially pass through, preferably, the transmission windows 3 are polyimide windows, the sample stage 2 is detachably mounted inside the test cavity along a transmission or reflection direction and is located between the two transmission windows, the sample stage 2 is provided with a light transmission part 5 for placing a sample, the sample is various in types, such as films, powders, fibers, etc., the X-rays passing through one window 3 pass through the sample and the light transmission part 5 located in the transmission direction, or are reflected by the sample and the light transmission part 5 located in the reflection direction and then are emitted through the other window 3, that is to say, two placing positions of the sample table 2 in the test cavity are adjusted, and the sample is carried to be located in a reflection path of the X-ray or located in a transmission path of the X-ray, so that the sample table 2 is placed in two postures in the same test cavity and matched with a corresponding X-ray diffractometer outside the test cavity, two test modes of reflection and transmission of the sample on the sample table 2 can be completed, the problem that different test accessories need to be replaced in different test modes is solved, a solvent vapor atmosphere is arranged in the test cavity, the light transmission part 5 is located in the solvent vapor atmosphere, and then an in-situ X-ray diffraction test function in the solvent vapor treatment process can be expected to be realized, and the change of a material crystal structure in the solvent vapor treatment process can be obtained. Related deep research can further analyze the mechanism of the change of the crystal structure and provide powerful data support for regulating and controlling the crystal structure and related performance; and then the method can be deeply applied to the actual product application process to further improve the performance of the product. According to the current mastered requirements, the in-situ test method for the solvent vapor treatment of the X-ray diffractometer can be widely applied to the aspects of single crystal growth, separation and dewetting of a high polymer film, organic high polymer photoelectric materials and devices, methylamine lead perovskite solar cells, fiber material structure regulation and the like. In addition, the utility model can be used as a standard component to be applied to other diffractometers or synchrotron radiation X-ray diffraction devices, and has certain commercial popularization value. Especially, the latter, because of its high brightness and fast measurement capability, can realize the test of the crystal structure and even the microstructure change in the solvent vapor treatment process under the time scale of seconds or even milliseconds, and the combination of the utility model and the synchrotron radiation X-ray diffraction device can provide more powerful technical means for the development of future scientific research.

The two transmission windows 3 are symmetrically arranged on two sides of the light transmission part 5, so that in a specific test process, for a reflection path, the two symmetrical transmission windows 3 can better ensure the adjustable range of the reflection path, the two transmission windows 3 are prevented from being asymmetrical, wherein the wider movement adjusting range of the X-ray corresponding to the transmission window 3 is easily limited by the narrower transmission window 3, and in the transmission path, the symmetrically arranged light transmission parts 5 can better ensure that the two transmission windows 3 and a sample are positioned on the same straight line, so that the sample can be transmitted.

Preferably, the inboard of test cavity is equipped with a plurality of draw-in grooves, and sample platform 2 slides along transmission or reflection position and pegs graft in corresponding draw-in groove, not only utilizes the draw-in groove to realize the fixed to sample platform 2, moreover in specific installation, only need with sample platform 2 push, peg graft in corresponding draw-in groove can, guaranteed the swift convenient technological effect of sample platform 2 installation. Each specific card slot is divided into a reflection card slot 7 and a transmission card slot 4, namely when the sample table 2 is respectively positioned at the reflection position and the transmission position, the sample table is correspondingly inserted into the corresponding reflection card slot 7 and the transmission card slot 4. Preferably, the sample stage 2 is fixed with a slip corresponding to the insertion slot, the slip is inserted into the corresponding slot, or the sample stage 2 is integrally of a plate-shaped structure, and two sides of the sample stage are inserted into the corresponding slots.

Wherein, be equipped with a plurality of absorbent cotton 6 that are soaked with the solvent that can volatilize on sample platform 2, each absorbent cotton 6 encircles around printing opacity portion 5, and preferred, the test cavity is whole to be closed column structure, closed column structure is equipped with the opening that is used for sample platform 2 business turn over, the opening part can be dismantled and be connected with sealed lid 8, for example, adopt the closed mode of screw tightening, utilize absorbent cotton 6 to soak behind the solvent that can volatilize, seal whole test cavity, the solvent that can volatilize in closed environment so, and then fill whole enclosure space, it is simple effective, and can form solvent vapour atmosphere fast, need not to set up two bleeder vents to the test cavity among the prior art, incessant through the bleeder vent again to test the cavity and let in solvent vapour, not only the structure is complicated, and is with high costs, and lead to the waste of solvent vapour.

Furthermore, the sealing cover 8 is provided with a plurality of sealable through holes 9 for feeding the volatile solvent, so that the sealing cover 8 is used for sealing the opening when the volatile solvent is fed through the whole opening, the solvent in the absorbent cotton 6 is easily volatilized in the sealing process due to the large structure of the sealing cover, the amount of the solvent diffused to the outer side of the test cavity from the opening is large, waste is caused, or the concentration in the subsequent test cavity cannot reach the preset requirement and the like, the volatile solvent is directly fed onto the absorbent cotton 6 in the test cavity through the sealable through holes 9, so that the volatilization of the solvent in the absorbent cotton 6 is limited to the inner side of the test cavity as far as possible, the concentration of the solvent in the test cavity is ensured, preferably, in order to simplify the whole connecting structure, rubber plugs are arranged in the sealable through holes 9 for sealing, and the connecting strength between the sealable through holes 9 and the rubber plugs is greater than the air pressure formed after the solvent is volatilized in the test cavity.

As a preferred embodiment of the utility model, the rubber plug is matched with a syringe, the needle head of the syringe penetrates through the rubber plug to inject the solvent onto the absorbent cotton 6 in the test cavity, after the injection is finished, a pinhole generated on the rubber plug is rapidly closed, and the absorbent cotton 6 injected with the solvent is placed on the sample table 2 to form a solvent vapor atmosphere, so that the waste of the solvent on the absorbent cotton 6 after volatilization is further avoided, and the concentration of the volatile solvent in the test cavity is ensured.

Furthermore, each closable through hole 9 is respectively opposite to the bearing side of the light transmission part 5, on one hand, the absorbent cotton 6 is soaked firstly and then is directly sent into the inner side of the test cavity through the closable through hole 9, the bearing surface of the light transmission part 5 can be aligned to directly place the absorbent cotton 6 at a corresponding position, the sending time can be further reduced, the sealing of the rubber plug on the closable through hole 9 can be rapidly completed, on the other hand, after the non-soaked absorbent cotton 6 is placed on the sample platform 2 in advance, the injection needle of the injector directly penetrates through the closable through hole 9 to align the absorbent cotton 6 to inject the solvent.

Preferably, the test cavity is integrally of a cylindrical structure 1, the transmission window 3 is arranged on the circumferential wall of the cylindrical structure 1, the sample stage 2 located in the transmission or reflection direction extends along the axis of the cylindrical structure 1, specifically, the cylindrical structure 1 extends horizontally, the sample stage 2 is integrally of a plate-shaped structure, the sample stage 2 in the transmission direction extends vertically and is inserted into the inner side of the cylindrical structure 1, the sample stage 2 in the reflection direction extends horizontally and is inserted into the inner side of the cylindrical structure 1, and the transmission window 3 is preferably of an arc-shaped structure which is smoothly connected with the circumferential wall, so that the reflection angle of the X-ray can be adjusted more easily by using the arc-shaped structure, and the flexible adjustment characteristic of the whole device is ensured.

Further, the two transmission windows 3 are both arranged on the bearing side of the light transmission part 5 located at the reflection position, and at least part of the light transmission part 5 located at the transmission position faces the two transmission windows 3, so that in the process of actually installing the transmission windows 3, the arrangement area of the transmission windows 3 is limited on the bearing side of the corresponding light transmission part 5, and the realization of the path of the transmission sample is ensured, and the problem that the path of the X-ray is blocked due to the fact that the span of the transmission windows 3 is too long and is easily affected by the clamping groove is avoided, or the part of the transmission windows 3 is located on the side, not bearing the sample, of the light transmission part 5 and cannot be used as the path of the X-ray, so that the waste of the transmission windows 3 is caused, and the manufacturing cost is increased.

Furthermore, one of the transmission windows 3 is close to the X-ray diffractometer, and the other transmission window 3 is provided with an X-ray diffractometer detector for receiving X-rays, wherein incident X-rays emitted by the X-ray diffractometer can be incident on the sample through one transmission window 3, and a generated diffraction signal enters the X-ray diffractometer detector through the other transmission window 3.

The adaptation according to the actual needs is within the scope of the utility model.

It will be evident to those skilled in the art that the utility model is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the utility model being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

The principle and the implementation mode of the utility model are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the utility model; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the utility model.

Claims

1. The utility model provides an X-ray diffractometer is with normal position solvent vapour processing test annex, its characterized in that includes test cavity and sample platform, the lateral wall of test cavity has two transmission windows that are used for the X ray to pass in proper order, sample platform along transmission or reflection position demountable installation in test cavity inboard, and be located two between the transmission window, the sample platform has the printing opacity portion that is used for settling the sample, passes one the transmission window the X ray pass be located transmission position the sample with the printing opacity portion, perhaps by be located reflection position the sample with the printing opacity portion reflects the back, through another the transmission window jets out, have solvent vapour atmosphere in the test cavity, the printing opacity portion is located in the solvent vapour atmosphere.

2. The in situ solvent vapor treatment test accessory for an X-ray diffractometer as claimed in claim 1, wherein two of said transmission windows are symmetrically disposed on either side of said light-transmissive portion.

3. The in-situ solvent vapor treatment test accessory of claim 2, wherein the test chamber has a plurality of slots formed therein, and the sample stage is slidably received in the slots in either a transmissive or reflective orientation.

4. The in-situ solvent vapor treatment test accessory for the X-ray diffractometer according to any one of claims 1 to 3, wherein a plurality of absorbent cottons soaked with a volatile solvent are arranged on the sample stage, and each absorbent cotton surrounds the light-transmitting part.

5. The in-situ solvent vapor treatment test accessory for the X-ray diffractometer as claimed in claim 4, wherein the test chamber is a closed structure as a whole, the closed structure is provided with an opening for the sample stage to enter and exit, and a sealing cover is detachably connected to the opening.

6. The in-situ solvent vapor treatment test accessory of claim 5, wherein the sealing cover defines a plurality of closable through holes for feeding the volatilizable solvent.

7. The in situ solvent vapor treatment test accessory for an X-ray diffractometer as claimed in claim 6, wherein each of the closable through holes faces a carrying side of the light-transmissive portion.

8. The in-situ solvent vapor treatment test accessory for the X-ray diffractometer as claimed in claim 5, wherein the test chamber is a cylindrical structure as a whole, the transmission window is disposed on a circumferential wall of the cylindrical structure, and the sample stage in the transmission or reflection orientation extends along an axis of the cylindrical structure.

9. The in situ solvent vapor treatment test accessory for an X-ray diffractometer as claimed in claim 8 wherein both of said transmission windows are disposed on a load side of said light-transmissive portion in the reflection orientation and said light-transmissive portion in the transmission orientation is at least partially opposite both of said transmission windows.

10. The X-ray diffractometer in situ solvent vapor treatment test accessory of claim 9, wherein one of the transmission windows is adjacent to the X-ray diffractometer and the other transmission window is adjacent to an X-ray diffractometer detector for receiving X-rays.