CN102778468A - Low-temperature accessory for X-ray diffractometer - Google Patents
Low-temperature accessory for X-ray diffractometer Download PDFInfo
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- CN102778468A CN102778468A CN2012102756423A CN201210275642A CN102778468A CN 102778468 A CN102778468 A CN 102778468A CN 2012102756423 A CN2012102756423 A CN 2012102756423A CN 201210275642 A CN201210275642 A CN 201210275642A CN 102778468 A CN102778468 A CN 102778468A
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- tank body
- heating
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- ray diffractometer
- low temperature
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Abstract
The invention discloses a low-temperature accessory for an X-ray diffractometer, belonging to the technical field of X-ray diffractometers. The low-temperature accessory comprises a main body assembly, a tank body, an upper cover, a fixing connecting device of the upper cover, a heating piece assembly, a cooling tube assembly and a sample box, wherein the upper cover is in sealing connection with the tank body; the heating piece assembly is arranged inside the tank body; the cooling tube assembly is connected with the heating piece assembly; the sample box is arranged above a heating plate of the heating piece assembly; the heating piece assembly is internally provided with a cavity; the cavity is communicated with the cooling tube assembly; the upper cover is provided with an air inlet channel communicated with the tank body internally; an air outlet channel is formed at the other end of the tank body; an air discharge port is connected with the air outlet channel; the main body assembly for installation is connected with one end (where the air outlet channel is arranged) of the tank body; a standby plug is arranged on the air inlet channel; and a heating plate of the heating piece assembly is connected with a PID (Proportion Integration Differentiation) adjustor. According to the low-temperature accessory, the liquid nitrogen is adopted for refrigeration; the sample box is heated by using the PID to adjust and control the heating quantity, thus the sample is stabilized at a set temperature. The heating plate is made of silicon carbide and has the advantages of fast heating, small deformation and high precision.
Description
Technical field
The invention belongs to X diffractometer technical applications, particularly relate to a kind of X-ray diffractometer and use the low temperature annex.
Background technology
X-ray diffractometer is the equipment that the material crystals structure is studied; The angular instrument of X-ray diffractometer is according to Bragg diffraction appearance principle: n λ=2dsin θ design; It is different to utilize the surface of sample to rotate the reflected ray angle, and the structure of material, grain size, crystallinity etc. are detected.Conventional diffractometer can't spend-190+and 450 temperature range changes material structure and studies, and especially can not satisfy the analysis of at low temperatures material being carried out X-ray diffraction.
Summary of the invention
To the technical matters of above-mentioned existence, the present invention provides a kind of X-ray diffractometer to use the low temperature annex, and it is for the research material variation that crystal structure took place under low temperature condition.
The present invention includes base component, tank body, with loam cake, end cap, end cap and tank body that the tank body sealed at both ends is connected between fastener, place heating plate in the tank body, place sample box and reflector on the heating plate; Said loam cake have with tank body in the inlet channel that communicates; Inlet channel is provided with subsequent use stifled, and reflector is arranged at air intake opening place in the tank body, and end cap has outlet passageway; On this outlet passageway, be connected with deflating valve; The said base component that is used to install is connected the tank body end cap, and said tank body is provided with the X ray incidence window, and heating plate is connected with the PID regulator.
Said fastener comprises fastening block and dead ring, and dead ring places tank body end cap periphery, and at least three of fastening blocks arrange evenly that along the circumference between dead ring and the end cap cooperation is fastenedly connected.Said reflector is semicircle.All have water annulus on said tank body loam cake and the end cap.Cover on the said tank body and also have a plurality of ring grooves, form radiation rib.Said window is provided with diaphragm, and is fastening through sealing gasket and restraint zone.Vacuumize or filling with inert gas in the said tank body.Said heating plate is the silit heating plate.
Beneficial effect of the present invention:
The present invention adopts liquid nitrogen refrigerating, regulates control through PID and adds heat, and the heated sample box makes the sample in the sample box be stabilized in design temperature.Adopt silit to make heating plate, heating is fast, distortion is little, precision is high.
Have water annulus on the tank body container of the present invention, cooling or antifreeze during low temperature when being used for high temperature.
The present invention has air inlet, outlet passageway, when need of work, can vacuumize through the container of mechanical pump to sealing, makes the vacuum tightness in the container reach 10
-2Mbar.Fully satisfy application demand, expand the detection application power and the application of X-ray diffractometer.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Fig. 2 is the A-A cross-sectional schematic of Fig. 1.
Among the figure: 1. main body component, 2. loam cake, 3. heating member component, 4. sealing gasket I, 5. nut, 6. cooling tube component, 7. copper packing; 8. deflating valve, 9. sealing gasket II, 10. sealing gasket III, 11. heating plates, 12. restraint zones, 13. curved purchasing, 14. pins; 15. spring, 16. locating pieces, 17. spring leafs, 18. ceramic wafers, 19. sample boxs, 20. angular instruments; 21. tank body, 22. inlet channels, 23. outlet passageways, 24. water annulus, 25. spanners, 26. windows.
Embodiment
Specifically describe the present invention below in conjunction with accompanying drawing and embodiment.
Embodiment: like Fig. 1, shown in Figure 2, the loam cake 2 that the present invention includes main body component 1, tank body 21, is tightly connected with tank body 21, the fixed connection apparatus of loam cake 2, place heating member component 3, the cooling tube component 6 that is connected with heating member component 3 and sample box 19 in the tank body 21, said sample box 19 places the top of silit heating plate 11 on the heating member component 3; Adopt silit heating plate 11, heating is fast, distortion is little, precision is high, is provided with cavity in the heating member component 3; This cavity communicates with cooling tube component 6; Be used to carry cooled with liquid nitrogen, loam cake 2 have with tank body 21 in the inlet channel 22 that communicates, tank body 23 other ends have outlet passageway 23; Be sealedly connected with deflating valve 8 on this outlet passageway 23; That is: be provided with the second sealing gasket II 9 between deflating valve 8 and bleed passage, the said main body component 1 that is used to install is connected an end that has outlet passageway 23, and inlet channel 22 is provided with subsequent use stifled; Have X ray on the said tank body 23 and inject window 26; The heating plate 11 of heating member component 3 is connected with the PID regulator, is used to control the heat that adds of heating plate 11, and temperature is met the demands.
As shown in Figure 2, have water annulus 24 on the said tank body 21 near main body component 1 one ends.Be used for the high temperature cooling during detection, or low temperature is antifreeze.Inwall and 3 of heating member components that said tank body 21 has outlet passageway 23 are provided with thermal insulation ceramics plate 18.Spring leaf 17 is fixed on the heating member component 3, and when sample box 19 was installed, spring leaf 17 ejected, and compresses sample box.
As shown in Figure 2; Said fixed connection apparatus comprises crotch 13, pin 14, spring leaf 15 and locating piece 16; Said locating piece 16 is fixed on loam cake 2 one ends, and the crotch body is connected with locating piece 16 with spring leaf 15 through pin 14, the crotch end with assemble after loam cake 2 and tank body 21 ends cooperate.Pull the spanner 25 on the crotch body, the crotch body rotates around pin 14, crotch 13 is closed or unclamps, and realizes the opening and closing of loam cake 2.Said X ray is injected outside the window 26 and is equipped with diaphragm, and is fastening through restraint zone 12, is used for the diaphragm of fastening window 26.
The present invention adopts liquid nitrogen refrigerating, prevents that heating member component 3 from damaging, and through the heat that adds of PID regulator control heating member component 3, heated sample box 19 makes the sample in the sample box 19, is stabilized in design temperature.As required, when detecting the readily oxidizable substance article, vacuumize during work, make the vacuum tightness in tank body 21 containers reach 10 through tank body 21 containers of mechanical pump to sealing
-2Mbar.Perhaps, make the blanketing with inert gas sample.
Claims (8)
1. an X-ray diffractometer is used the low temperature annex; It is characterized in that: the loam cake that comprises main body component, tank body, is tightly connected with tank body, the fixed connection apparatus of loam cake, place the heating member component in the tank body, cooling tube component and the sample box that is connected with the heating member component, said sample box places above the heating plate of heating member component, is provided with cavity in the heating member component; This cavity communicates with the cooling tube component; Loam cake have with tank body in the inlet channel that communicates, the tank body other end has outlet passageway, and is connected with deflating valve on this outlet passageway; The said main body component that is used to install is connected an end that has outlet passageway; Inlet channel is provided with subsequent use stifled, has X ray on the said tank body and injects window, and the heating plate of heating member component is connected with the PID regulator.
2. X-ray diffractometer according to claim 1 is used the low temperature annex, it is characterized in that: have water annulus on the said tank body near main body component one end.
3. X-ray diffractometer according to claim 1 is used the low temperature annex, it is characterized in that: inwall and heating that said tank body has outlet passageway are provided with the thermal insulation ceramics plate between component.
4. X-ray diffractometer according to claim 1 is used the low temperature annex, it is characterized in that: said heating member component is provided with the spring leaf that compresses sample box.
5. X-ray diffractometer according to claim 1 is used the low temperature annex, it is characterized in that: the heating plate of said heating member component is a carborundum plate.
6. X-ray diffractometer according to claim 1 is used the low temperature annex; It is characterized in that: said fixed connection apparatus comprises crotch, pin, spring leaf and locating piece; Said locating piece is fixed on loam cake one end; The crotch body is connected with locating piece with spring leaf through pin, the crotch end with assemble after loam cake and tank body end cooperate.
7. X-ray diffractometer according to claim 1 is used the low temperature annex, it is characterized in that: said X ray is injected window and is provided with diaphragm, and is fastening through restraint zone.
8. X-ray diffractometer according to claim 1 is used the low temperature annex, it is characterized in that: vacuumize or filling with inert gas in the said tank body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102756423A CN102778468A (en) | 2012-08-03 | 2012-08-03 | Low-temperature accessory for X-ray diffractometer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102756423A CN102778468A (en) | 2012-08-03 | 2012-08-03 | Low-temperature accessory for X-ray diffractometer |
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| CN102778468A true CN102778468A (en) | 2012-11-14 |
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| CN2012102756423A Pending CN102778468A (en) | 2012-08-03 | 2012-08-03 | Low-temperature accessory for X-ray diffractometer |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983129A (en) * | 2014-05-16 | 2014-08-13 | 丹东通达科技有限公司 | Liquid nitrogen evaporator used for X-ray single-crystal diffractometer |
| CN104458780A (en) * | 2014-12-09 | 2015-03-25 | 中国科学院上海应用物理研究所 | In-situ test sample platform |
| CN104502367A (en) * | 2014-12-09 | 2015-04-08 | 中国科学院上海应用物理研究所 | In-situ testing platform for thermal chemical vapor deposition |
| CN108152167A (en) * | 2018-01-19 | 2018-06-12 | 中国科学技术大学 | The method that low temperature stretches rheometer and the test of macromolecule membrane cryogenic property |
| CN108572185A (en) * | 2017-03-13 | 2018-09-25 | 中国科学院兰州化学物理研究所 | X-ray single crystal diffractometer easy-weathering crystal cryo-microscope loading 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 |
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| JPH01260353A (en) * | 1988-04-12 | 1989-10-17 | Nec Corp | High temperature furnace for single crystal x-ray diffraction |
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| CN202196026U (en) * | 2011-07-08 | 2012-04-18 | 中国石油化工股份有限公司 | Controllable low-temperature sample stage for X-ray diffractometer |
| CN202735269U (en) * | 2012-08-03 | 2013-02-13 | 丹东浩元仪器有限公司 | Low-temperature accessory for X-ray diffractometer |
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2012
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| SU842520A1 (en) * | 1979-08-27 | 1981-06-30 | Физико-Технический Институт Низкихтемператур Ah Украинской Ccp | Low-temperature attachment to x-ray diffractometer |
| DE8423909U1 (en) * | 1984-08-11 | 1985-01-03 | Kernforschungsanlage Jülich GmbH, 5170 Jülich | EULERWIEGE FOR DEEP TEMPERATURE DIFFRAKTOMETRY |
| JPH01260353A (en) * | 1988-04-12 | 1989-10-17 | Nec Corp | High temperature furnace for single crystal x-ray diffraction |
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| JPH0476438A (en) * | 1990-07-19 | 1992-03-11 | Rigaku Corp | Sample low temperature device for x-ray diffraction device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103983129A (en) * | 2014-05-16 | 2014-08-13 | 丹东通达科技有限公司 | Liquid nitrogen evaporator used for X-ray single-crystal diffractometer |
| CN103983129B (en) * | 2014-05-16 | 2015-08-26 | 丹东通达科技有限公司 | A kind of liquid nitrogen evaporator for X-ray single crystal diffractometer |
| CN104458780A (en) * | 2014-12-09 | 2015-03-25 | 中国科学院上海应用物理研究所 | In-situ test sample platform |
| CN104502367A (en) * | 2014-12-09 | 2015-04-08 | 中国科学院上海应用物理研究所 | In-situ testing platform for thermal chemical vapor deposition |
| CN108572185A (en) * | 2017-03-13 | 2018-09-25 | 中国科学院兰州化学物理研究所 | X-ray single crystal diffractometer easy-weathering crystal cryo-microscope loading system |
| CN108152167A (en) * | 2018-01-19 | 2018-06-12 | 中国科学技术大学 | The method that low temperature stretches rheometer and the test of macromolecule membrane cryogenic property |
| 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 |
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Application publication date: 20121114 |