CN202196026U - Controllable low-temperature sample table for x-ray diffraction instruments - Google Patents
Controllable low-temperature sample table for x-ray diffraction instruments Download PDFInfo
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- CN202196026U CN202196026U CN2011202398890U CN201120239889U CN202196026U CN 202196026 U CN202196026 U CN 202196026U CN 2011202398890 U CN2011202398890 U CN 2011202398890U CN 201120239889 U CN201120239889 U CN 201120239889U CN 202196026 U CN202196026 U CN 202196026U
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Abstract
A controllable low-temperature sample table for x-ray diffraction instruments comprises a sample platform (1) which is fixed with a sample room outer cover (2) through a bolt (3); two window ports are respectively formed on two sides of the sample room outer cover (2) and are sealed to beryllium windows (4) by beryllium sheets through the bolts; a sample rack (5) is mounted in the center of the sample platform (1) through a round mounting hole; two mounting holes are formed on one side of the sample platform (1), in which a pressure non-return valve (9) and a sample room thermocouple (7) are mounted respectively; another mounting hole is formed on the other side of the sample platform (1), in which a liquid nitrogen nozzle (8) is mounted; and another mounting hole is also formed on the sample rack (5) at the position near to the center, in which a sample thermocouple (6) is mounted. The sample table has a simple structure, is convenient to operate, has a lower cost, not only can realizes the controllable low-temperature test, but also is favorable for protecting samples with special protection requirements (air sensitivity) owning to the nitrogen atmosphere, and is suitable for various x-ray diffraction instruments.
Description
Technical field
The utility model relates to a kind of low temperature-controlled sample stage that is used for X-ray diffractometer.
Background technology
In the macromolecule research field; The cryogenic property of polymkeric substance such as polyolefin (for example tygon, gather interior alkene), degradation plastic, engineering plastics is directly connected to its application in all fields, and the X diffraction is the indispensable means of various adjuvants in research polymer crystals structure and the superpolymer; In catalyst research, problem such as activity of such catalysts, stability, inactivation and regeneration and catalyst crystalline phases structure are closely related, and X-ray diffraction method is the important method of testing that characterizes the catalyst crystalline phases structure.For can obtain solid sample under specific cryogenic conditions crystal phase structure information and with the variation of temperature variation crystal phase structure, designed a kind of low temperature-controlled sample stage that is used for X-ray diffractometer.
With regard to related patent U.S. Patent No., only retrieve the patent of " the X-ray diffraction Cryo Equipment " of one piece of bulletin in 1989, number of patent application CN2045852, this patent is compared with the design, and structure is too simple, and can not carry out program heating and cooling control.
Just present literature search situation; With X-ray diffraction method cryogenic substance is carried out crystal phase structure research; Two kinds of methods are arranged usually: the one, testing sample to be carried out measuring immediately after the sub zero treatment, this method exists in the sample test process temperature variation fast, and the test result accuracy is lower; Two be to use Austrian Anton Parr company to produce low temperature annex TTK450 measure, but there is complex structure in this low temperature annex TTK450, costs an arm and a leg, and changes effort, time-consuming problem during use.
Summary of the invention
The technical matters that the utility model will solve:
In order to overcome the deficiency of the low temperature sample chamber that is not used in the prior art on the common sample frame; The utility model provides a kind of X-ray diffractometer to use the low temperature-controlled sample stage; Use this sample stage to carry out X ray diffractive crystal structured testing under the cryogenic conditions, and can follow the trail of the sample crystal structure with the variation of temperature situation through temperature programmed control to solid sample.
The technical scheme of the utility model is:
A kind of X-ray diffractometer is used the low temperature-controlled sample stage, comprises example platform (1), and example platform (1) is fixed through bolt (3) with sample chamber outer cover (2) and formed sample chamber (10); Sample chamber outer cover (2) is each side opened a window, and the beryllium sheet becomes beryllium window (4) through bolt with closed windows; Specimen holder (5) is installed in the center of example platform (1) through the circular mounting hole; Be provided with two mounting holes in example platform (1) one side, pressure check valve door (9) and sample chamber thermopair (7) are housed respectively; Be provided with a mounting hole at example platform (1) opposite side, liquid nitrogen nozzle (8) is installed; Be provided with a mounting hole at specimen holder (5) near the position at center, sample thermopair (6) is installed.
Described sample chamber outer cover preferred material is a stainless steel.
The beneficial effect of the utility model is:
The essential distinction of the utility model and prior art is; The utility model design is on original standard model platform, to transform, and original standard model platform goes out the disk 15, example platform 1, specimen holder, pressure unit, the prelocalization frame that link to each other with the corner appearance and forms.Basis is practical mainly utilizes the disk 15 and example platform 1 that links to each other with the corner appearance in original standard model platform, and example platform 1 is transformed, and is prepared into the sample stage that can realize low temperature control.Have simple in structure, easy to operate, cost and reduce, not only can realize the low temperature-controlled test, and nitrogen atmosphere helps the sample that protection has special protection requirement (like air-sensitive), be applicable to various X-ray diffractometers.
Description of drawings
Fig. 1 is the left view of original standard model platform;
Fig. 2 is the other line diffractometer of an X low temperature-controlled sample stage front elevational schematic;
Fig. 3 is that synoptic diagram is looked on an X-ray diffractometer low temperature-controlled sample stage left side;
Fig. 4 is an X-ray diffractometer low temperature-controlled sample stage schematic top plan view;
Fig. 5 is that X-ray diffractometer low temperature-controlled sample stage is connected synoptic diagram with liquid nitrogen container, temperature controller, liquid nitrogen flow controller.
Embodiment
In the embodiment shown in fig. 1, the disk that basic composition is sample levels table top 1, links to each other 15 of standard model platform with angular instrument, sample levels table top 1 passes through bolt with disk 15, has constituted the basic framework of standard model platform.
In Fig. 2, Fig. 3, son embodiment illustrated in fig. 4, example platform 1 and sample chamber outer cover 2 are fixed together with bolt 3; In the sample chamber outer cover 2 each side open long 3 centimetres, loose 1 a centimetre rectangle window and will plate sheet with bolt with closed windows, be called beryllium window 4; Open a hole in the center of example platform 1, through the specimen holder 5 insertion sample chambers 10 of this hole with teflon; In the left side of example platform 1, open two holes according to order from left to right, at left hole setting pressure one-way cock 9, insert sample chamber thermopair 7 in right ports; Open a hole on the right side of example platform 1, insert liquid nitrogen nozzle 8 through this hole; A hole of vertically running through is up and down opened in the position that takes at specimen holder 5 centers, and this hole upper position inserts these holes near example platform with sample thermopair 6.
In Fig. 5 embodiment, be connected with temperature controller 12 with sample chamber thermopair 7 by the sample thermopair 6 with sample stage shown in Figure 5; Liquid nitrogen flow controller 13 is connected with liquid nitrogen container 11; Liquid nitrogen nozzle 8 is connected with liquid nitrogen container 11 through liquid nitrogen insulation delivery pipe 14; Liquid nitrogen flow controller 13 is connected with temperature controller 12.
In another embodiment of Fig. 5; Sample stage shown in Figure 2 is fixed on the angular instrument through the disk 15 that links to each other with angular instrument among Fig. 1; Take off specimen holder 5 then, sample is inserted in the specimen holder 5 and sample surfaces is flattened, afterwards with in the specimen holder 5 screw-in sample chambers 2.Begin test, in test process, set experimental temperature, start and measure, sample thermopair 6, sample chamber thermopair 7, pressure check valve door 9, liquid nitrogen container 11, liquid nitrogen flow controller 13, liquid nitrogen insulation delivery pipe 14, temperature controller 12 are started working at this moment; Temperature controller 12 is the temperature difference between thermopair 6, sample chamber thermopair 7 and the preset temperature per sample; Result of calculation is fed back to liquid nitrogen flow controller 13; Liquid nitrogen flow controller 13 is adjusted the flow velocity of liquid nitrogen on this basis; Reach the purpose of control temperature with this, when temperature reached preset experimental temperature, the X-ray diffraction instrument began sample is tested.
Claims (2)
1. an X-ray diffractometer is used the low temperature-controlled sample stage, comprises example platform (1), it is characterized in that example platform (1) and sample chamber outer cover (2) are fixing through bolt (3); Sample chamber outer cover (2) is each side opened a window, and the beryllium sheet becomes beryllium window (4) through bolt with closed windows; Specimen holder (5) is installed in the center of example platform (1) through the circular mounting hole; Be provided with two mounting holes in example platform (1) one side, pressure check valve door (9) and sample chamber thermopair (7) are housed respectively; Be provided with a mounting hole at example platform (1) opposite side, liquid nitrogen nozzle (8) is installed; Be provided with a mounting hole at specimen holder (5) near the position at center, sample thermopair (6) is installed.
2. X-ray diffractometer according to claim 1 is used the low temperature-controlled sample stage, it is characterized in that sample chamber outer cover preferred material is a stainless steel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202398890U CN202196026U (en) | 2011-07-08 | 2011-07-08 | Controllable low-temperature sample table for x-ray diffraction instruments |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202398890U CN202196026U (en) | 2011-07-08 | 2011-07-08 | Controllable low-temperature sample table for x-ray diffraction instruments |
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| Publication Number | Publication Date |
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| CN202196026U true CN202196026U (en) | 2012-04-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011202398890U Expired - Lifetime CN202196026U (en) | 2011-07-08 | 2011-07-08 | Controllable low-temperature sample table for x-ray diffraction instruments |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778468A (en) * | 2012-08-03 | 2012-11-14 | 丹东浩元仪器有限公司 | Low-temperature accessory for X-ray diffractometer |
| CN103630560A (en) * | 2013-11-04 | 2014-03-12 | 大连理工大学 | Device and method for CT (Computed Tomography) scanning of low-temperature sample |
| CN105954306A (en) * | 2016-04-22 | 2016-09-21 | 中国原子能科学研究院 | Variable-temperature sample stage device used for X-ray diffraction measurement of liquid |
| CN107357329A (en) * | 2017-07-14 | 2017-11-17 | 河北工业大学 | A kind of temperature regulating device for liquid-scattering measurement |
| CN107643306A (en) * | 2017-09-15 | 2018-01-30 | 中国科学院化学研究所 | XRD sample stages |
| CN109324010A (en) * | 2018-09-18 | 2019-02-12 | 惠科股份有限公司 | A kind of test device and method |
| CN111007092A (en) * | 2020-01-02 | 2020-04-14 | 中国科学院化学研究所 | Low-temperature XRD testing device, testing equipment and testing system |
| CN111678930A (en) * | 2020-07-23 | 2020-09-18 | 丹东通达科技有限公司 | Detection device for measuring sample characteristics at low temperature by X-ray diffractometer |
| CN113406128A (en) * | 2021-07-23 | 2021-09-17 | 重庆大学 | Temperature control accessory for X-ray diffractometer |
-
2011
- 2011-07-08 CN CN2011202398890U patent/CN202196026U/en not_active Expired - Lifetime
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778468A (en) * | 2012-08-03 | 2012-11-14 | 丹东浩元仪器有限公司 | Low-temperature accessory for X-ray diffractometer |
| CN103630560A (en) * | 2013-11-04 | 2014-03-12 | 大连理工大学 | Device and method for CT (Computed Tomography) scanning of low-temperature sample |
| CN103630560B (en) * | 2013-11-04 | 2016-01-13 | 大连理工大学 | A kind of device and method for cryogenic sample CT scan |
| CN105954306A (en) * | 2016-04-22 | 2016-09-21 | 中国原子能科学研究院 | Variable-temperature sample stage device used for X-ray diffraction measurement of liquid |
| CN107357329B (en) * | 2017-07-14 | 2022-07-26 | 河北工业大学 | Temperature control device for liquid scattering measurement |
| CN107357329A (en) * | 2017-07-14 | 2017-11-17 | 河北工业大学 | A kind of temperature regulating device for liquid-scattering measurement |
| CN107643306A (en) * | 2017-09-15 | 2018-01-30 | 中国科学院化学研究所 | XRD sample stages |
| CN107643306B (en) * | 2017-09-15 | 2019-07-09 | 中国科学院化学研究所 | XRD sample stage |
| CN109324010A (en) * | 2018-09-18 | 2019-02-12 | 惠科股份有限公司 | A kind of test device and method |
| CN109324010B (en) * | 2018-09-18 | 2021-08-31 | 惠科股份有限公司 | Testing device and method |
| CN111007092A (en) * | 2020-01-02 | 2020-04-14 | 中国科学院化学研究所 | Low-temperature XRD testing device, testing equipment and testing system |
| CN111678930A (en) * | 2020-07-23 | 2020-09-18 | 丹东通达科技有限公司 | Detection device for measuring sample characteristics at low temperature by X-ray diffractometer |
| CN113406128A (en) * | 2021-07-23 | 2021-09-17 | 重庆大学 | Temperature control accessory for X-ray diffractometer |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20120418 |
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| CX01 | Expiry of patent term |