CN105263198A - Open heating device for synchrotron radiation in-situ test - Google Patents
Open heating device for synchrotron radiation in-situ test Download PDFInfo
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- CN105263198A CN105263198A CN201510653766.4A CN201510653766A CN105263198A CN 105263198 A CN105263198 A CN 105263198A CN 201510653766 A CN201510653766 A CN 201510653766A CN 105263198 A CN105263198 A CN 105263198A
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- heat
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Abstract
The invention relates to an open heating device for a synchrotron radiation in-situ test. Main points are that the middle part of a heat conducting block is provided with an open sample chamber, the heat conducting block is internally provided with a plurality of inert gas ventilation pipes outside the open sample chamber, the inert gas ventilation pipes sequentially penetrate, one ends of the gas ventilation pipes are open, the tail parts of the other ends of the inert gas ventilation pipes are communicated with the open sample chamber, and side surface of the heat conducting block are additionally provided with heating pieces respectively. Therefore, a sample can be isolated from the air without sealing the sample chamber, the sample chamber can be directly placed in the air, the sample is not oxidized in the heating process, the test device can be miniaturized, test conditions such as the temperature, the stress, a magnetic field and the like are controlled conveniently, a synchrotron radiation test device can be greatly simplified, and the test efficiency and the test precision are significantly improved, ray inlet and outlet windows are not required to be sealed, absorption and disturbance imposed on rays by a ray window sealing material and generation of a diffraction peak are eliminated, and the utilization ratio of rays is improved. In addition, the open heating device provided by the invention is convenient in test control, saves time and trouble, and can greatly improve the efficiency.
Description
Technical field
The present invention relates to a kind of heater of synchrotron radiation in-situ test, particularly a kind of open heater for synchrotron radiation in-situ test.
Background technology
New material, new technology are the major fields of current science and technology.Support new material, characterization method that the Fundamentals of Material Science research institute of development of new techniques relies on progressively is transitioned into dynamic micro-structural by the stable state microtechnic in past and monitors, the center of gravity of research is also developed gradually by the steady-state characteristic paying close attention to material and is deep into their dynamic processes under preparation process and using state deeply concerned.Synchrotron radiation in-situ testing technique is developing rapidly, is applicable to the advanced technology of dynamic process monitoring under material preparation process and using state.Be developed synchrotron radiation in-situ observation technology and device that heating up process material structure develops situation, develop synchrotron radiation in-situ observation technology and device that heating up process material structure under action of compressive stress develops situation, also have fine fiber material preparation process material structure to develop synchrotron radiation in-situ observation technology and the device of situation.The existing heater carrying out synchrotron radiation in-situ test is in a heated condition all enclosed, is all that sample is placed in airtight cavity, to ensure the isolation with air, realizes preventing sample oxidized in a heated condition.But, the method for this employing airtight cavity isolation sample and air is airtight in order to realize, require to carry out strict sealing to sample cavity, disapprove a bit leakage, not only high to device processing request, and need to be equipped with special vacuum pump and cooling device, make apparatus structure complicated.This airtight heater, efficiency and the precision of synchrotron radiation experiment are had a strong impact on, on the one hand, can not resistant to elevated temperaturesly limit because being subject to ray window encapsulant, the miniaturization of synchrotron radiation in-situ testing device cannot be realized, change to the installation of temperature regulating device at synchrotron radiation line station and sample and bring difficulty; On the other hand, in order to realize sample cavity sealing, must seal ray window, so far also not to the window material that ray is completely transparent, window aperture seal material inevitably produces ray and absorbs and interference diffraction maximum; Moreover airtight due to sample cavity, brings difficulty to the applying of the test such as applied stress, magnetic field parameter in test process and control.
Summary of the invention
For above problem, the object of this invention is to provide a kind of without the need to airtight just can by sample and isolated from atmosphere, sample cavity directly can be placed in air and sample is not oxidized in heating process, can testing apparatus is the miniaturized and open heater being used for synchrotron radiation in-situ test be convenient to the test conditions such as control temperature, stress, magnetic field, greatly can simplified synchrotron radiation testing apparatus, significantly promote conventional efficient and precision.
A kind of open heater for synchrotron radiation in-situ test, comprise heat-conducting block and be opened on heat-conducting block and cross open sample cavity and the open ray entrance aperture communicated and open ray perforation hole, it is characterized in that: the middle part of heat-conducting block is provided with open sample cavity, be provided with the inert gas breather line that some through successively and one end open other end afterbodys communicate with open sample cavity in heat-conducting block outside open sample cavity, and establish on the side of heat-conducting block heating plate is housed.Described open sample cavity refers to without the need to adopting seal approach to make sample and isolated from atmosphere as prior art, directly can be placed in atmospheric environment and carry out testing and avoiding sample oxidized; Described open ray entrance aperture and open ray perforation hole refer to without the need to adopting seal approach to make sample and isolated from atmosphere as prior art, directly can be placed in atmospheric environment and carry out testing and not making sample oxidized.
The object of the invention is to utilize to establish and be contained in heating plate on heat-conducting block lateral surface the inert gas flowing through the inert gas breather line that some through successively and one end open other end afterbodys communicate with open sample cavity is heated repeatedly, and the inert gas after repeatedly heating is inputted in open sample cavity, inert gas after recycling is input to the heating repeatedly in open sample cavity heats the test sample be arranged in open sample cavity, maintains lasting inert gas malleation simultaneously and sample and air insulated are realized.Obviously, the openend of described inert gas breather line is the input port of inert gas, the outlet that two openends and open ray go out, entrance aperture is air or inert gas of open sample cavity.So, the present invention not only have without the need to by airtight for sample cavity just can by sample and isolated from atmosphere, sample cavity directly can be placed in air and sample is not oxidized in heating process, can be miniaturized by testing apparatus, and be convenient to control temperature, stress, the test conditions such as magnetic field, can greatly simplify synchrotron radiation testing apparatus, the advantage of remarkable lifting conventional efficient and precision, also have without the need to ray being gone out as prior art, enter window aperture seal, eliminate ray window encapsulant to the absorption of ray and the generation disturbing diffraction maximum, improve ray utilance, promote experimental precision and conventional efficient, and test manipulation is convenient, save time and save trouble, greatly can improve effect, it is a kind of economical and practical heater for synchrotron radiation in-situ test.
Accompanying drawing explanation
Fig. 1 is structural upright schematic diagram of the present invention;
Fig. 2 is the vertical section stereogram of Fig. 1,
Fig. 3 is the central cross section stereogram of Fig. 1;
Fig. 4 is another kind of structural upright schematic diagram of the present invention;
Fig. 5 is another structural upright schematic diagram of the present invention;
Fig. 6 is the 4th kind of structural upright schematic diagram of the present invention;
Fig. 7 is the front view of I block in Fig. 6 and II block faying face,
Fig. 8 is the front view of II block in Fig. 6 and I block faying face.
In figure: UNICOM's mouth 7 of heat-conducting block 1, open ray perforation hole 2, open sample cavity 3, inert gas breather line 4, heating plate 5, open ray entrance aperture 6, inert gas breather line and open sample cavity.
Embodiment
Describe in detail below in conjunction with drawings and Examples:
Several structural upright schematic diagram of the present invention in figure, i.e. the several open heater for synchrotron radiation (XRD) in-situ test.Mainly comprise heat-conducting block 1 and be opened on heat-conducting block 1 and cross open sample cavity 3 and the open ray entrance aperture 6 communicated and open ray perforation hole 2, it is characterized in that: the middle part of heat-conducting block 1 is provided with open sample cavity 3, heat-conducting block 1 outside open sample cavity 3 is provided with the inert gas breather line 4 that some through successively and one end open other end afterbodys communicate with open sample cavity 3, and establishes on the side of heat-conducting block 1 heating plate 5 is housed.Obviously, the openend of inert gas breather line is the input port of inert gas; Inert gas breather line 4 in figure and open sample cavity 3 utilize inert gas breather line to be connected with UNICOM's mouth 7 of open sample cavity.Described open sample cavity 3 refers to the rectangular cavities of both ends open, and sample can freely run through wherein in test process, does not contact with sample cavity wall.
Fig. 1 ~ Fig. 3 is a kind of structural upright schematic diagram of the present invention, i.e. a kind of open heater for synchrotron radiation (XRD) in-situ test stress.The manufacture method of this heater is as follows:
(1) the good heat-conducting block 1 that one piece of length is 100mm, 20mm and 10mm is got, as copper billet or aluminium block.Being processed into as being labeled as the fast profile of 1 heat conduction in Fig. 1, then processing along long axis direction the rectangle sample chamber 3 that cross section is 1mm × 3mm at heat-conducting block 1 center.
(2) in the leading flank center of heat-conducting block 1, process the ray entrance aperture 6 that diameter is 1mm, in the trailing flank center of heat-conducting block 1, processing inside diameter is 2mm, and outside diameter is the tubaeform ray perforation hole 2 of 4mm.
Process the breather line 4 that diameter is 1.5mm in the top and the bottom of heat-conducting block 1, as shown in Figure 1, a, b and f tri-breather lines are positioned at the top of heat-conducting block 1, and c, d and e tri-breather lines are positioned at the bottom of heat-conducting block 1.Interim a, b, c, d, e five breather lines are through along the axis of heat-conducting block 1, and one end of a breather pipe connects with source of the gas, and the other end thin copper pipe matched is unified into closed gas circuit with b, c, d, e and f breather pipe successively.F pipeline one end connects with e pipeline, the other end is divided into two arms to the middle part of heat-conducting block 1, the interim centre position of an arm between beam orifice 2 with the left opening of sample cavity 3 is communicated with sample cavity, and the centre position of another arm between beam orifice 2 with the right opening of sample cavity 3 is communicated with sample cavity.
(3) at the leading flank attachment ceramic heating flake 5 of heat-conducting block 1.
When inert gas is from after the openend be opened in a one end (namely with source of the gas union end) enters, after flowing through b, c, d, e, f breather line successively, entered in sample cavity 3 by UNICOM's mouth 7 of inert gas breather line and open sample cavity.Flow out from the left and right port of beam orifice 2 and sample cavity 3 again after entering the gas of sample cavity and sample contacts.Gas is heated by heating plate 5 repeatedly when flowing through breather line 3, transfers heat to sample when entering sample cavity 3, and sample is heated.Because gas is inert gas, the original air in open sample cavity 3 can not only be discharged by lasting inert gas flow, can also form malleation in open sample cavity 3, stops air and flows into, make open sample cavity 3 become anaerobic district; So, while to sample heating, prevent again sample oxidized, achieve the object of sample cavity 3 without the need to heated sealed.
As long as this heater to be installed to the experiment porch at synchrotron radiation line station, sample through sample cavity 3, then applies tensile stress at the sample two ends of stretching out sample cavity 3.Then make ray be injected by beam orifice 6, the synchrotron radiation can carrying out the sample heating process under effect of stress is measured.Insert thermocouple from sample cavity port and make thermocouple be close to sample, and thermocouple and heating plate 5 are connected on temperature controller, just can realize the control of sample temperature.
Fig. 4 is another kind of structural upright schematic diagram of the present invention, and namely the present invention's another kind is used for the open heater of synchrotron radiation (XRD) in-situ test.In order to fully improve the heat efficiency, heating plate 5 is established and is contained on the lateral surface of the heat-conducting block 1 of inert gas breather line 4; Namely inert gas breather line 4 be arranged on heat block 1 upper and lower in, and heating plate 5 is also mounted on the lateral surface of heat block about 1, namely on the lateral surface of the heat-conducting block 1 of inert gas breather line 4.
Fig. 5 is another structural upright schematic diagram of the present invention, i.e. another open heater for synchrotron radiation (XRD) in-situ test of the present invention.Reach reservation temperature in order to ensure the indifferent gas physical efficiency flowed through in inert gas breather line 4, the two sides in figure outside heat-conducting block 1 are all pasted with heating plate 5.
Fig. 6 is the 4th kind of structural upright schematic diagram of the present invention, i.e. the 4th kind of open heater for synchrotron radiation (XRD) in-situ test of the present invention.Get two pieces of length and widths, height and be respectively 100mm, the good heat-conducting block of 30mm and 6mm, as copper billet.It being processed into respectively as being labeled as I and II liang of heat-conducting block profile in Fig. 6, then processing along long axis direction the open sample cavity 3 of rectangle that cross section is 1mm × 3mm at heat-conducting block II center with line cutting technology.In the binding face center of heat-conducting block II with heat-conducting block I, process the ray entrance aperture 6 that diameter is 1mm, then UNICOM's mouth 7 of two inert gas breather lines and open sample cavity is opened in the centre between beam orifice 6 and sample cavity 3 port.Then in the trailing flank center of heat-conducting block II, processing inside diameter is 2mm, and outside diameter is the tubaeform ray perforation hole 2 of 5mm.
(2) I piece of heat-conducting block 1 and the lower end offered as shown in Figure 7 on the binding face of II piece are provided with the inert gas breather line 4 of air inlet; And II piece of heat-conducting block 1 with the binding face of I block is offered two and is harmonious and UNICOM's mouth 7 of the inert gas breather line communicated with open sample cavity 3 and open sample cavity with the outlet side of the inert gas breather line of I block, as shown in Figure 8.
(3) by after the mirror polish that fits of heat-conducting block I and II, fit together, as shown in Figure 6.After making laminating, except air inlet and venthole can not leak gas.Gas enters from the air inlet of inert gas breather line 4, after flowing through breather line 4, is entered in open sample cavity 3 by UNICOM's mouth 7 of inert gas breather line and open sample cavity.Flow out from the left and right port of open ray entrance aperture 6 and open perforation hole 2 and open sample cavity 3 again after entering the inert gas of open sample cavity 3 and sample contacts.The heating plate 5 that inert gas is mounted on when flowing through inert gas breather line 4 on heat-conducting block I lateral surface heats repeatedly, then enters in open sample cavity 3, heat is directly passed to sample, sample is heated.Because gas is inert gas, the air in open sample cavity 3 can not only be discharged by lasting inert gas flow, can also form the malleation of relative outside air, stopped air inflow in open sample cavity 3; So in test process, open sample cavity 3 is anaerobic district, giving sample direct-fired while, protects sample again, make sample not oxidized.Therefore open ray entrance aperture 6 and open perforation hole 2 and open sample cavity 3 can be adopted, namely open ray entrance aperture 6 directly can be communicated with air with the left and right port of open perforation hole 2 and open sample cavity 3, without the need to sealing, achieve in open sample cavity 3 heated sample, the object of synchrotron radiation in-situ test sample and sample not oxidation by air in open ray entrance aperture 6 and open perforation hole 2.
(3) at the leading flank attachment ceramic heating flake 5 of heat-conducting block I, insert thermocouple from sample cavity port and make thermocouple be close to sample.Thermocouple and heating plate are connected temperature controller, just can realize the control of sample temperature.
(4) sample cavity is installed to the experiment porch at synchrotron radiation line station, sample through sample cavity 3, then applies tensile stress at the sample two ends of stretching out sample cavity.Then make ray be injected by ray entrance aperture 6, the synchrotron radiation can carrying out the sample heating process under effect of stress is measured.
In order to improve the thermal conductivity of heat-conducting block 1, to improve the heat efficiency, energy savings, can adopt copper heat-conducting block; In order to ensure thermal conductivity, to reduce costs and weight can adopt aluminium matter heat-conducting block; Namely heat-conducting block (1) is aluminum or copper heat-conducting block.
Heating plate 5 in figure is ceramic heating flake.For making the heat energy of heating plate 5 be fully utilized, fully improve the heat efficiency, heating plate 5 is established and is contained on the lateral surface of the heat-conducting block 1 of inert gas breather line 4; As Fig. 4 and Fig. 6 embodiment.When heating plate 5 is mounted on the face arranging open ray entrance aperture 6 or open ray perforation hole 2, the position of the corresponding ray of heating plate 5 incident 6 or perforation hole 2 is provided with corresponding hole, passes freely through for ray, as the embodiment of Fig. 1, Fig. 5 and Fig. 6.
Claims (9)
1. the open heater for synchrotron radiation in-situ test, comprise heat-conducting block (1) and be opened on heat-conducting block (1) and cross open sample cavity (3) and the open ray entrance aperture (6) communicated and open ray perforation hole (2), it is characterized in that: the middle part of heat-conducting block (1) is provided with open sample cavity (3), and sample freely can run through sample cavity; In open sample cavity (3) heat-conducting block outward (1), be provided with the inert gas breather line (4) that some through successively and one end open other end afterbodys communicate with open sample cavity (3), and establish on the side of heat-conducting block (1) heating plate (5) is housed.
2. the open heater for synchrotron radiation in-situ test according to claim 1, is characterized in that: heat-conducting block (1) is aluminum or copper heat-conducting block.
3. the open heater for synchrotron radiation in-situ test according to claim 1 and 2, it is characterized in that: heating plate (5) is ceramic heating flake, the position of corresponding ray incidence (6) and perforation hole (2) is provided with aperture, passes freely through for ray.
4. the open heater for synchrotron radiation in-situ test according to claim 3, it is characterized in that: open ray entrance aperture (6) and open ray perforation hole (2) are opened on the central part of open sample cavity (3) of heat-conducting block (1) both sides, pass perpendicularly through sample cavity, with sample cavity UNICOM.
5. the open heater for synchrotron radiation in-situ test according to claim 4, is characterized in that: heating plate (5) is established and is contained on the lateral surface of the heat-conducting block (1) of breather line (4).
6. the open heater for synchrotron radiation in-situ test according to claim 3, is characterized in that: heating plate (5) is established and is contained on the lateral surface of the heat-conducting block (1) of breather line (4).
7. the open heater for synchrotron radiation in-situ test according to claim 1 and 2, it is characterized in that: open ray entrance aperture (6) and open ray perforation hole (2) are opened on the central part of open sample cavity (3) of heat-conducting block (1) both sides, pass perpendicularly through sample cavity, with sample cavity UNICOM.
8. the open heater for synchrotron radiation in-situ test according to claim 7, is characterized in that: heating plate (5) is established and is contained on the lateral surface of the heat-conducting block (1) of breather line (4).
9. the open heater for synchrotron radiation in-situ test according to claim 1 and 2, is characterized in that: heating plate (5) is established and is contained on the lateral surface of the heat-conducting block (1) of breather line (4).
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| CN201510653766.4A CN105263198B (en) | 2015-10-10 | 2015-10-10 | A kind of open heating device for synchrotron radiation in-situ test |
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| CN105263198A true CN105263198A (en) | 2016-01-20 |
| CN105263198B CN105263198B (en) | 2019-02-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106714341A (en) * | 2016-12-21 | 2017-05-24 | 浙江师范大学 | Open-type heater manufacturing method used for synchronous-radiation in-situ test |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08254506A (en) * | 1995-03-17 | 1996-10-01 | Nippon Steel Corp | Sample chamber for x-ray measurement |
| CN102590253A (en) * | 2012-01-17 | 2012-07-18 | 中国科学院上海应用物理研究所 | High-temperature fused salt synchrotron radiation in-situ research device |
| CN102636595A (en) * | 2012-04-13 | 2012-08-15 | 延边大学 | Continuous gas in-tube solid phase microextraction device combined with gas chromatography for use |
| CN202471625U (en) * | 2012-01-18 | 2012-10-03 | 中国科学院上海应用物理研究所 | Tubular high-temperature molten salt synchrotron radiation in-situ research device |
-
2015
- 2015-10-10 CN CN201510653766.4A patent/CN105263198B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08254506A (en) * | 1995-03-17 | 1996-10-01 | Nippon Steel Corp | Sample chamber for x-ray measurement |
| CN102590253A (en) * | 2012-01-17 | 2012-07-18 | 中国科学院上海应用物理研究所 | High-temperature fused salt synchrotron radiation in-situ research device |
| CN202471625U (en) * | 2012-01-18 | 2012-10-03 | 中国科学院上海应用物理研究所 | Tubular high-temperature molten salt synchrotron radiation in-situ research device |
| CN102636595A (en) * | 2012-04-13 | 2012-08-15 | 延边大学 | Continuous gas in-tube solid phase microextraction device combined with gas chromatography for use |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106714341A (en) * | 2016-12-21 | 2017-05-24 | 浙江师范大学 | Open-type heater manufacturing method used for synchronous-radiation in-situ test |
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