CN205388580U - Be used for liquid X - ray scattering sample cell - Google Patents
Be used for liquid X - ray scattering sample cell Download PDFInfo
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- CN205388580U CN205388580U CN201620146283.5U CN201620146283U CN205388580U CN 205388580 U CN205388580 U CN 205388580U CN 201620146283 U CN201620146283 U CN 201620146283U CN 205388580 U CN205388580 U CN 205388580U
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Abstract
The of the utility model is used for liquid X the ray scattering sample cell, this sample cell includes cell body, sealing material and temperature sensor, wherein, the cell body is bilayer structure, comprises cell body outer wall and cell body inner wall with the different diameters in axle center, cell body outer wall both sides are provided with inlet tube and outlet pipe respectively, link to each other with the thermostatic water -circulator bath respectively, clearance between cell body outer wall and the cell body inner wall is used for storage water, and the inside of cell body inner wall is the sample cell for hold liquid and need checking sample, sealing material be beryllium window or mylar membrane, cover at cell body inner wall top. The utility model discloses can realize temperature control more rapidly, efficient, the homogeneity is good, simple structure, and easily preparation, low cost, the application is wide.
Description
Technical field
The utility model relates to liquid X-ray scattering experiment technical field, particularly relates to liquid X-ray scattering sample cell.
Background technology
Solution structure be solvation species in research solution microstructure and and macroscopic property between the science of relation.The research method of solution structure has two big classes, and one is the direct measurement of structure, i.e. uses instrument to be measured；Another kind of is computer simulation method, it is thus achieved that solution structure.It should be noted that single dependence molecular simulation can not obtain real solution structure data, lack checking；And the proprietary instrument not measured for solution structure up to now, also without supporting follow-up data processing method.In existing measuring method, experimental technique based on scattering is to obtain solution structure information method the most accurately.
The instrument that X-ray scattering method uses can be powder x-ray diffraction or the X-ray scattering device of synchrotron radiation light source in laboratory.The advantage of synchrotron radiation light source is that its brightness is big, stability is high, high directivity, collimation are good, becomes the perfect light source of liquid-scattering experiment.The either powder x-ray diffraction in laboratory or the X-ray scattering device of synchrotron radiation light source, its supporting sample cell all designs to solid sample, have no idea to solve holding and temperature control problem of fluid sample, therefore, a kind of liquid sample pool of exploitation is particularly important to solution scattering research, also becomes the basic demand that solution scattering measures.
Due to solution longrange disorder only shortrange order own, low to X-ray absorption rate, the crystal diffraction ability more orderly than the cycle to the scattering power of X-ray is much lower, and its scattered signal is easy to be covered by the scattered signal of window material.Additionally, different with temperature, the X-ray scattering difference of solution.Therefore, liquid sample pool is in addition to solving the holding of liquid, it is necessary to solve window material and the problem of temperature control.This patent is developed liquid sample pool and constant-temperature temperature-control device according to solution scattering feature and θ-2 θ type diffractometer specimen rotating holder attribute, designed, designed, is set up fluid sample test platform, and investigate its stability and reliability.
Utility model content
Technical problem to be solved in the utility model is the pond body the most shallow (about 2mm) in the solid sample pond existed for current techniques, liquid cannot be held, more with film, Chi Tikou cannot be sealed, the deficiency of the most uncontrollable temperature, it is provided that a kind of liquid sample pool measured for solution scattering.This sample cell by deepening pond body, select suitable sealed membrane to be sealed by Chi Tikou and Pool body design becomes to have outer wall and inwall, not only solve fluid sample holds problem, by being connected with outside thermostat, it is achieved that the temperature control of fluid sample；By the selection of window material with determine, the X-ray scattered signal overcoming window material covers the problem of solution scattered signal, and whole system has good stability and reliability, practical, it is easy to promote.
The technical solution of the utility model is:
A kind of for liquid X-ray scattering sample cell, including pond body, joint filling material and temperature sensor；
Wherein, pond body is double-decker, is made up of wall in the external wall in the pond of concentric different-diameter and pond body；External wall both sides, pond are respectively arranged with water inlet pipe and outlet pipe, are connected with thermostatic water-circulator bath respectively；In the external wall in pond and pond body, the gap between wall is used for storing water, and in the body of pond, the inside of wall is sample cell, is used for holding liquid and testing sample；
Described joint filling material is beryllium window or Mylar film, covers at Ti Neibi top, pond；
Described temperature sensor is fixed on the inner side of wall in the body of pond by gluing,
It is provided with adhesive bottom described pond body；
In the external wall in described pond and pond body, the semidiameter of wall is 1～2cm.
Described temperature sensor is connected by wire and digital display electronic thermometer.
Also including thermostatic water-circulator bath, this water-bath is connected with sample cell with outlet pipe by water inlet pipe respectively.
The beneficial effects of the utility model are:
X-ray scatterometry device both can use Laboratory X-ray light source, it is possible to uses synchrotron radiation light source.Synchrotron radiation light source, because brightness is big, stability is high, high directivity, collimation are good, becomes the perfect light source of liquid-scattering experiment, and liquid-scattering based on synchrotron radiation light source research becomes the focus of liquid structure research in recent years.Regardless of whether be the powder x-ray diffraction in laboratory, or the X-ray scattering device of synchrotron radiation light source, its supporting sample cell is both for solid sample design, and owing to this sample cell pond body is shallow, liquid cannot be contained therein；Without joint filling material, cause the rotation of when meeting of the liquid in the body of pond is adjoint to be measured 180 ° to be flowed out, and then cannot complete to measure；And the temperature of the single wall Pool body design the most uncontrollable pond vivo sample in solid sample pond, therefore, the utility model devises the sample cell of wall in the external wall in pond and pond body, by water inlet pipe and outlet pipe, the water in water bath with thermostatic control is circulated in the interlayer that the external wall in pond and inwall are formed, and then realize the temperature of fluid sample in the body of pond and control；The height of pond body designs at 1-2cm, both can meet holding of certain quantity of fluid sample, and in turn ensure that this sample cell can be fixed on the sample stage of original scattering device, because after pond height is too high, the space of original sample stage will be unable to lay sample stage；Using the ParafilmTM sample cell Chi Kou of suitable material, both ensure that the liquid in the body of pond will not flow out with the rotation of 180 ° during measuring, and in turn ensure that the signal of this sealed membrane material will not block the scattered signal of liquid itself, this puts most important.Because compared with solid, liquid is low to X-ray absorption rate, the crystal diffraction ability making X-ray diffraction energy force rate cycle of liquid orderly is much lower, only choose suitable sealed membrane material guarantee and will not shelter the scattering of liquid itself, solve and obtain the matter of utmost importance that liquid scattered information accurately faces.
Compared with prior art, the utility model uses water bath with thermostatic control to carry out temperature control, avoid the fluid temperature gradient brought by heating element heater temperature control and hot inhomogeneities (because heating element heater is typically attached to bottom the body of sample cell pond, then fluid temperature near bottom, more first raise), the most safer.The water inlet pipe of the utility model sample cell, outlet pipe design at two ends, eliminate water inlet pipe, dividing plate that outlet pipe is set up in sample cell when same one end, it is also possible to relatively rapidly realize temperature control, efficiency is high, and uniformity is good, simple in construction, being prone to make, with low cost, application is wide.In addition, the pond shape of the utility model design, size dimensions etc. fully combine the feature of existing scattering device, the selection of sealed membrane also achieves sample cell arbitrary orientation and the rotation of angle and not trickle, and do not disturb liquid-scattering signal, these advantages make the utility model sample cell can be not only used for the powder x-ray diffraction in laboratory, can also be used for the X-ray scattering device of synchrotron radiation light source, solve liquid during solution scattering measures cannot hold, the problem that temperature controls and shelters joint filling material signal, guarantee is provided for carrying out the scattering experiment of fluid sample smoothly, also necessary basis is laid for expansion powder diffractometer application in liquid-scattering is tested further.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings detailed description of the invention of the present utility model is described in further detail.
Fig. 1 is the utility model structural representation for liquid X-ray scattering sample cell.
Fig. 2 is the utility model side view for liquid X-ray scattering sample cell.
Fig. 3 is the utility model top view for liquid X-ray scattering sample cell.
In figure: 1. pond body, 2. sample cell, the 3. external wall in pond, 4. wall, 5. water inlet pipe, 6 outlet pipes in the body of pond.
Detailed description of the invention
The utility model is for liquid X-ray scattering sample cell (being called for short device, see Fig. 1-3), including 1. pond body, 2. sample cells, the 3. external wall in pond, 4. wall, 5. water inlet pipe, 6 outlet pipes in the body of pond.
Including pond body 1, joint filling material and temperature sensor；Wherein pond body 1 is double-decker, is made up of wall 4 in the external wall in the pond of concentric different-diameter 3 and pond body；External wall 3 both sides, pond are respectively arranged with water inlet pipe 5 and outlet pipe 6, are connected with thermostatic water-circulator bath respectively；In the external wall in pond 3 and pond body, the gap between wall 4 is used for storing water, and in the body of pond, the inside of wall 4 is sample cell 2, is used for holding liquid and testing sample；
Described joint filling material is beryllium window or Mylar film, covers wall 4 top in the body of pond；
Described temperature sensor is fixed on the inner side of wall 4 in the body of pond by gluing,
It is provided with adhesive bottom described pond body；It is connected for diffractometer flat samples platform.
In the external wall in described pond 3 and pond body, the semidiameter of wall 4 is 1～2cm.
Described temperature sensor is connected by wire and digital display electronic thermometer, the fluid temperature that display sensor spreads out of in real time.Wire is more than 80cm, it is ensured that temperature sensor is along with being pind down owing to wire falls short of and affect when sample cell rotates.
The utility model also includes thermostatic water-circulator bath, and this water-bath is connected with sample cell with outlet pipe 6 by water inlet pipe 5 respectively.
The temperature regulation of this sample cell have employed the way of water bath with thermostatic control, controls the temperature of liquid in sample cell by the temperature controlling water bath with thermostatic control.By water inlet pipe and water outlet pipe, the water in water bath with thermostatic control is introduced the external wall in pond and the interlayer of wall formation in the body of pond of sample cell, carries out water-bath circulation, and then realize the control to fluid sample temperature.
The pond a diameter of 5-8cm of external wall of described sample cell, inner diameter is 3-6cm, and in the external wall in pond and pond body, the semidiameter of wall is 1～2cm, and pond height is 1-2cm.
When described sample cell pond surface beryllium window or Mylar film seal, Mylar film thickness is in 3-7 μm, and beryllium window thickness is 0.05-0.15mm.
The water inlet pipe 5 of described sample cell is connected with outside thermostatic water-circulator bath respectively with outlet pipe 6, and its temperature can be controlled in-50.0 DEG C～99.9 DEG C according to the difference of thermostat medium.
Temperature sensor in sample cell is fixed in the pond body of sample cell (2) on wall (4) by the mode such as gluing, and is sealed against in sample cell (2) by sealed membrane, the fluid temperature in real-time monitored sample cell.The wire of this temperature sensor is more than 80cm.
Sample cell of the present utility model is in use, first by temperature sensor by wall (4) in the gluing pond body being fixed on pond body (1), fluid sample is added in the pond body (1) of sample cell (2), with sealed membrane (beryllium window or Mylar film) by hydraulic seal in the pond body (1) of open-topped sample cell (2), water inlet pipe (5) is connected with outside thermostatic water-circulator bath respectively with outlet pipe (6), adhesive is used bottom the pond body of sample cell, sample cell (2) entirety is connected with diffractometer flat samples platform, and carry design and fixing means by the torr of flat samples playscript with stage directions body, sample cell is fixed on sample stage.Now, open water bath with thermostatic control switch, set the temperature of fluid to be measured requirement, circulated by the water-bath of water inlet pipe and outlet pipe, the temperature of fluid sample is controlled, according to the temperature of display in real time on temperature sensor, the temperature of water bath with thermostatic control is adjusted, the temperature stabilization realizing fluid to be measured sample controls requiring temperature, and the preparation that now fluid sample measures is ready, can start the follow-up work that fluid sample scattering measures.
Owing to the utility model uses water bath with thermostatic control temperature control method, avoid the fluid temperature gradient brought by heating element heater temperature control and hot inhomogeneities (because heating element heater is typically attached to bottom the body of sample cell pond, then fluid temperature near bottom, more first raise), security is higher.And the water inlet pipe of the utility model sample cell, outlet pipe design at two ends, eliminate water inlet pipe, dividing plate that outlet pipe is set up in sample cell when same one end, it is also possible to relatively rapidly realizing temperature control, improve efficiency, uniformity is more preferable.In addition, pond shape due to the utility model design, size dimensions etc. fully combine the feature of existing scattering device, the selection of sealed membrane also achieves sample cell arbitrary orientation and the rotation of angle and not trickle, and do not disturb liquid-scattering signal, therefore the utility model sample cell can be not only used for the powder x-ray diffraction in laboratory, can also be used for the X-ray scattering device of synchrotron radiation light source, solve liquid during solution scattering measures cannot hold, the problem that temperature controls and liquid signal sheltered by joint filling material, simultaneously, make simple, with low cost, practical, application is wide.
The utility model unaccomplished matter is known technology.
Claims (3)
1. scatter a sample cell for liquid X-ray, it is characterized by include pond body, joint filling material and temperature sensor；
Wherein, pond body is double-decker, is made up of wall in the external wall in the pond of concentric different-diameter and pond body；External wall both sides, pond are respectively arranged with water inlet pipe and outlet pipe, are connected with thermostatic water-circulator bath respectively；In the external wall in pond and pond body, the gap between wall is used for storing water, and in the body of pond, the inside of wall is sample cell, is used for holding liquid and testing sample；
Described joint filling material is beryllium window or Mylar film, covers at Ti Neibi top, pond；
Described temperature sensor is fixed on the inner side of wall in the body of pond by gluing；
It is provided with adhesive bottom described pond body.
2. as claimed in claim 1 scatter sample cell for liquid X-ray, it is characterized by that the semidiameter of wall is 1 ~ 2cm in the external wall in described pond and pond body.
3. the liquid X-ray that is used for as claimed in claim 1 scatters sample cell, it is characterized by also to include thermostatic water-circulator bath, and this water-bath is connected with sample cell with outlet pipe by water inlet pipe respectively.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620146283.5U CN205388580U (en) | 2016-02-27 | 2016-02-27 | Be used for liquid X - ray scattering sample cell |
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| CN201620146283.5U CN205388580U (en) | 2016-02-27 | 2016-02-27 | Be used for liquid X - ray scattering sample cell |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107357329A (en) * | 2017-07-14 | 2017-11-17 | 河北工业大学 | A kind of temperature regulating device for liquid-scattering measurement |
| CN112213340A (en) * | 2020-10-16 | 2021-01-12 | 郑州大学 | Sample table for on-line determination of crystal structure and determination method thereof |
-
2016
- 2016-02-27 CN CN201620146283.5U patent/CN205388580U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107357329A (en) * | 2017-07-14 | 2017-11-17 | 河北工业大学 | A kind of temperature regulating device for liquid-scattering measurement |
| CN112213340A (en) * | 2020-10-16 | 2021-01-12 | 郑州大学 | Sample table for on-line determination of crystal structure and determination method thereof |
| CN112213340B (en) * | 2020-10-16 | 2023-07-21 | 郑州大学 | Sample stage for on-line determination of crystal structure and determination method thereof |
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