CN105263198B - A kind of open heating device for synchrotron radiation in-situ test - Google Patents
A kind of open heating device for synchrotron radiation in-situ test Download PDFInfo
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- CN105263198B CN105263198B CN201510653766.4A CN201510653766A CN105263198B CN 105263198 B CN105263198 B CN 105263198B CN 201510653766 A CN201510653766 A CN 201510653766A CN 105263198 B CN105263198 B CN 105263198B
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 62
- 238000012360 testing method Methods 0.000 title claims abstract description 40
- 230000005469 synchrotron radiation Effects 0.000 title claims abstract description 38
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 27
- 239000011261 inert gas Substances 0.000 claims abstract description 35
- 238000009423 ventilation Methods 0.000 claims abstract description 33
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000003566 sealing material Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000002045 lasting effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000013459 approach Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The present invention relates to a kind of open heating devices for synchrotron radiation in-situ test.Main points are: open sample cavity is provided in the middle part of heat-conducting block, it is equipped with several inert gas ventilation pipes that successively perforation and other end tail portion open at one end are communicated with open sample cavity in the heat-conducting block outside open sample cavity, and is provided with heating sheet on the side of heat-conducting block.So, without by sample cavity is closed can be by sample and isolated from atmosphere, sample cavity can be placed directly in atmosphere and sample is not oxidized during heating, test device can be minimized, convenient for controlling temperature, stress, the test conditions such as magnetic field, synchrotron radiation test device can be greatly simplified, it is obviously improved conventional efficient and experimental precision, it is not necessary that ray is gone out, enter window aperture seal, ray window sealing material is eliminated to the absorption and interference of ray and the generation of diffraction maximum, improve ray utilization rate, and test manipulation is convenient, it is time saving to save trouble, effect can be greatly improved.
Description
Technical field
The present invention relates to a kind of heating devices of synchrotron radiation in-situ test, especially a kind of to survey in situ for synchrotron radiation
The open heating device of examination.
Background technique
New material, new technology are the major fields of current science and technology.Support the material science base of new material, development of new techniques
The characterization method that plinth research institute relies on gradually is transitioned into the monitoring of dynamic micro-structure, the weight of research by past stable state microtechnic
The heart, which is also gradually developed by the steady-state characteristic of concern substance, is deep into their deeply concerned dynamics under preparation process and use state
Process.Synchrotron radiation in-situ testing technique is to rapidly develop, and is suitable for dynamic under material preparation process and use state
The advanced technology of process monitoring.It is developed the synchrotron radiation in-situ observation skill of heating up process material structure evolution
Art and device develop the synchrotron radiation in-situ observation technology of heating up process material structure evolution under action of compressive stress
And device, also there is the synchrotron radiation in-situ observation technology and equipment of fine fiber material preparation process material structure evolution.It is existing
Some is performed under heating conditions the heating device of synchrotron radiation in-situ test, is all enclosed, is all to set sample
In airtight cavity, to guarantee to be isolated with air, realizing in a heated condition prevents sample to be oxidized.But this use
The method of sample and air is isolated in airtight cavity, closed in order to realize, it is desirable that carry out stringent sealing to sample cavity, disapproved
A bit leakage, not only it is high to device processing request, and need to be equipped with special vacuum pump and cooling device, so that device knot
Structure is complicated.This airtight heating device has seriously affected the efficiency and precision of synchrotron radiation experiment, on the one hand, because by ray
Window aperture seal material resistant to high temperature cannot limit, and cannot achieve the miniaturization of synchrotron radiation in-situ testing device, give temperature regulating device
Difficulty is brought in the installation at synchrotron radiation line station and sample replacement；On the other hand, in order to realize that sample cavity seals, it is necessary to penetrating
Linear window is sealed, and so far there are no the window material fully transparent to ray, window aperture seal material is inevitably right
Ray, which generates, absorbs and interferes diffraction maximum；Furthermore it is closed due to sample cavity, it is surveyed to applied stress, magnetic field in test process etc.
The application and control for trying parameter bring difficulty.
Summary of the invention
In view of the above problems, the object of the present invention is to provide one kind without it is closed can by sample and isolated from atmosphere, can general
Sample cavity is placed directly in atmosphere and sample is not oxidized during heating, can minimize test device and convenient for control
The test conditions such as temperature, stress, magnetic field can greatly simplify synchrotron radiation test device, be obviously improved conventional efficient and precision
The open heating device for synchrotron radiation in-situ test.
A kind of open heating device for synchrotron radiation in-situ test, including heat-conducting block and be provided on heat-conducting block horizontal
Wear open sample cavity and the open ray entrance aperture communicated and open ray perforation hole, it is characterised in that: in heat-conducting block
Middle part be provided with open sample cavity, in the heat-conducting block outside open sample cavity be equipped with it is several successively perforation and it is open at one end
The inert gas ventilation pipe that other end tail portion is communicated with open sample cavity, and heating is provided on the side of heat-conducting block
Piece.The open sample cavity refers to without using seal approach to make sample and isolated from atmosphere as the prior art, can be with
Atmospheric environment is placed directly within to be tested and sample is avoided to be oxidized；The open ray entrance aperture and the outgoing of open ray
Hole refers to without using seal approach to make sample and isolated from atmosphere as the prior art, can be placed directly in atmospheric environment into
Row experiment is without being oxidized sample.
The purpose of the present invention is using setting heating sheet on heat-conducting block lateral surface to flowing through several successively perforations and one
The inert gas for the inert gas ventilation pipe that end opening other end tail portion is communicated with open sample cavity heats repeatedly, and will be anti-
Inert gas after being added with heat inputs in open sample cavity, after recycling the heating repeatedly being input in open sample cavity
Inert gas heats the test sample being arranged in open sample cavity, while lasting inert gas positive pressure being maintained to make
What sample and air insulated were realized.Obviously, the open end of the inert gas ventilation pipe is the input port of inert gas, is opened
Two open ends and open ray for putting formula sample cavity go out, entrance aperture is air or the outlet of inert gas.So the present invention
Not only have without that sample cavity can be placed directly within to sample and isolated from atmosphere in atmosphere and sample exists by sample cavity is closed
It is not oxidized in heating process, test device can be minimized, and convenient for control temperature, stress, the test conditions such as magnetic field, it can be with
The advantages of greatly simplifying synchrotron radiation test device, being obviously improved conventional efficient and precision, also have without as the prior art that
Ray is gone out, enters window aperture seal by sample, is eliminated generation of the ray window sealing material to the absorption of ray and interference diffraction maximum, is mentioned
High ray utilization rate, promotes experimental precision and conventional efficient, and tests that manipulation is convenient, time saving to save trouble, can greatly improve effect,
It is a kind of economical and practical heating device for synchrotron radiation in-situ test.
Detailed description of the invention
Fig. 1 is structural upright schematic diagram of the invention；
Fig. 2 is the vertical section perspective view of Fig. 1,
Fig. 3 is the central cross section perspective view of Fig. 1；
Fig. 4 is another structural upright schematic diagram of the invention；
Fig. 5 is yet another construction stereoscopic schematic diagram of the invention；
Fig. 6 is the 4th kind of structural upright schematic diagram of the invention；
Fig. 7 is the front view of the I block and II block faying face in Fig. 6,
Fig. 8 is the front view of the II block and I block faying face in Fig. 6.
In figure: heat-conducting block 1, open ray perforation hole 2, open sample cavity 3, inert gas ventilation pipe 4, heating sheet
5, open ray entrance aperture 6, inert gas ventilation pipe and open sample cavity connection mouth 7.
Specific embodiment
It is described in detail below in conjunction with drawings and examples:
It is several structural upright schematic diagram of the invention in figure, i.e., it is several to be used for synchrotron radiation (XRD) in-situ test
Open heating device.It mainly include that heat-conducting block 1 and being provided on heat-conducting block 1 crosses open sample cavity 3 and what is communicated open
Put formula ray entrance aperture 6 and open ray perforation hole 2, it is characterised in that: the middle part of heat-conducting block 1 is provided with open sample
Chamber 3, on the heat-conducting block 1 outside open sample cavity 3 be equipped with it is several successively perforation and other end tail portion open at one end with it is open
The inert gas ventilation pipe 4 that sample cavity 3 communicates, and heating sheet 5 is provided on the side of heat-conducting block 1.Obviously, inert gas
The open end of ventilation pipe is the input port of inert gas；Inert gas ventilation pipe 4 and open sample cavity 3 in figure are benefits
It is connected with inert gas ventilation pipe with the connection mouth 7 of open sample cavity.The open sample cavity 3 refers to that both ends are opened
The rectangular cavities of mouth, sample can not contact during the test with sample cavity wall freely therethrough.
FIG. 1 to FIG. 3 is a kind of structural upright schematic diagram of the invention, i.e., a kind of open former for synchrotron radiation (XRD)
The heating device of bit test stress.The heating device the production method is as follows:
(1) taking one piece of length is the good heat-conducting block 1 of 100mm, 20mm and 10mm, such as copper billet or aluminium block.It is processed
At 1 thermally conductive fast shape is labeled as shown in figure 1, then processing cross section along long axis direction at 1 center of heat-conducting block is 1mm × 3mm
Rectangle sample chamber 3.
(2) in the leading flank center of heat-conducting block 1, the ray entrance aperture 6 that diameter is 1mm is processed, in heat-conducting block 1
Trailing flank center, processing inside diameter is 2mm, and outside diameter is the tubaeform ray perforation hole 2 of 4mm.
The ventilation pipe 4 that diameter is 1.5mm is processed in the top and the bottom of heat-conducting block 1, as shown in Figure 1, a, b and f tri- logical
Feed channel is located at the top of heat-conducting block 1, and c, d and tri- ventilation pipes of e are located at the lower part of heat-conducting block 1.Interim a, b, c, d, e five
Ventilation pipe along heat-conducting block 1 axially through, one end of a snorkel couples with gas source, the other end with the thin copper pipe to match according to
Secondary and b, c, d, e and f snorkel are unified into closure gas circuit.F pipeline one end couples with e pipeline, the middle part of the other end to heat-conducting block 1
At two branch pipes, middle position of the interim branch pipe between beam orifice 2 and the left opening of sample cavity 3 is connected to sample cavity, separately
Middle position of one branch pipe between beam orifice 2 and the right opening of sample cavity 3 is connected to sample cavity.
(3) ceramic heating flake 5 is mounted in the leading flank of heat-conducting block 1.
After inert gas enters from the open end (i.e. with gas source union end) being provided on the one end a, followed by b, c,
D, after e, f ventilation pipe, entered in sample cavity 3 by the connection mouth 7 of inert gas ventilation pipe and open sample cavity.Into sample
The gas of product chamber is flowed out from the left and right port of beam orifice 2 and sample cavity 3 again after contacting with sample.Gas is flowing through ventilation pipe 3
When be heated piece 5 and heat repeatedly, transfer heat to sample when into sample cavity 3, heat sample.Because gas is indifferent gas
Original air in open sample cavity 3 can not only be discharged for body, lasting inert gas flow, moreover it is possible in open sample cavity 3
Middle formation positive pressure prevents air inflow, open sample cavity 3 is made to become anaerobic area；So prevent while being heated to sample again
Stop sample to be oxidized, realizes the purpose that sample cavity 3 is not necessarily to heated sealed.
As long as the heating device to be installed to the experiment porch at synchrotron radiation line station, sample passes through sample cavity 3, then is stretching out
The sample both ends of sample cavity 3 apply tensile stress.It injects ray by beam orifice 6, the sample under stress can be carried out
The synchrotron radiation of product heating process measures.Thermocouple is inserted into from sample cavity port and thermocouple is made to be close to sample, and by thermocouple
It is connected on temperature controller with heating sheet 5, can realize the control of sample temperature.
Fig. 4 is another structural upright schematic diagram of the invention, i.e., the present invention is another in situ for synchrotron radiation (XRD)
The open heating device of test.In order to sufficiently improve the thermal efficiency, heating sheet 5, which is set, is installed adjacent to inert gas ventilation pipe 4
On the lateral surface of heat-conducting block 1；I.e. the upper and lower interior of heat block 1 is arranged in inert gas ventilation pipe 4, and heating sheet 5 is also mounted on
On the lateral surface of about 1 heat block, i.e., on the lateral surface of the heat-conducting block 1 of inert gas ventilation pipe 4.
Fig. 5 is yet another construction stereoscopic schematic diagram of the invention, i.e., another is in situ for synchrotron radiation (XRD) by the present invention
The open heating device of test.In order to ensure the inert gas flowed through in inert gas ventilation pipe 4 can reach reservation temperature,
Heating sheet 5 is all pasted in figure on the two sides outside heat-conducting block 1.
Fig. 6 is the 4th kind of structural upright schematic diagram of the invention, i.e., of the invention the 4th kind former for synchrotron radiation (XRD)
The open heating device of bit test.Taking two pieces of lengths is respectively the good heat-conducting block of 100mm, 30mm and 6mm, such as copper billet.
It is processed into respectively as being labeled as I and II liang of heat-conducting block shape in Fig. 6, then with line cutting technology on II center edge of heat-conducting block
Long axis direction processes the open sample cavity 3 of rectangle that cross section is 1mm × 3mm.In the binding face of heat-conducting block II and heat-conducting block I
Center processes the ray entrance aperture 6 that diameter is 1mm, then the centre between 3 port of beam orifice 6 and sample cavity opens two
The connection mouth 7 of a inert gas ventilation pipe and open sample cavity.Then in the trailing flank center of heat-conducting block II, processing
Inside diameter is 2mm out, and outside diameter is the tubaeform ray perforation hole 2 of 5mm.
(2) lower end as shown in Figure 7 is opened up on I piece of binding face with II piece of heat-conducting block 1 be provided with the lazy of air inlet
Property gas ventilation pipeline 4；And two inert gas snorkels with I block are opened up on II piece of binding face with I block of heat-conducting block 1
The outlet side in road is harmonious and the connection mouth 7 of the inert gas ventilation pipe that communicates with open sample cavity 3 and open sample cavity,
As shown in Figure 8.
(3) it by after the face polishing that fits of heat-conducting block I and II, fits together, as shown in Figure 6.After making fitting, in addition into
Port and venthole will not gas leakage.Gas enters from the air inlet of inert gas ventilation pipe 4, after flowing through ventilation pipe 4, by lazy
Property gas ventilation pipeline and open sample cavity connection mouth 7 enter open sample cavity 3 in.Into open sample cavity 3
Inert gas contacted with sample after again from a left side for open ray entrance aperture 6 and open perforation hole 2 and open sample cavity 3,
Right output port outflow.Inert gas is mounted on the heating sheet 5 on I lateral surface of heat-conducting block when flowing through inert gas ventilation pipe 4
It heats repeatedly, subsequently into open sample cavity 3, heat is directly passed to sample, heats sample.Because gas is inertia
The air in open sample cavity 3 can not only be discharged for gas, lasting inert gas flow, moreover it is possible in open sample cavity 3
The positive pressure for forming opposite outside air, has prevented air inflow；So during the test, open sample cavity 3 is anaerobic
Area protects sample again while directly heating to sample, keeps sample not oxidized.Therefore can be entered using open ray
Perforation 6 and open perforation hole 2 and open sample cavity 3, i.e., open ray entrance aperture 6 and open perforation hole 2 and opening
The left and right port of formula sample cavity 3 can directly be connected to atmosphere, without sealing, realize heated in open sample cavity 3 sample,
The synchrotron radiation in-situ test sample in open ray entrance aperture 6 and open perforation hole 2 and sample not oxidation by air
Purpose.
(3) ceramic heating flake 5 is mounted in the leading flank of heat-conducting block I, be inserted into thermocouple from sample cavity port and make thermocouple
It is close to sample.Thermocouple and heating sheet are coupled into temperature controller, can realize the control of sample temperature.
(4) sample cavity is installed to the experiment porch at synchrotron radiation line station, sample passes through sample cavity 3, then is stretching out sample
The sample both ends of chamber apply tensile stress.It injects ray by ray entrance aperture 6, the sample under stress can be carried out
The synchrotron radiation of heating process measures.
It is energy saving to improve the thermal efficiency in order to improve the thermal conductivity of heat-conducting block 1, copper heat-conducting block can be used；In order to
Ensure thermal conductivity, reduces cost and aluminum heat-conducting block can be used in weight；I.e. heat-conducting block (1) is aluminum or copper heat-conducting block.
Heating sheet 5 in figure is ceramic heating flake.To make the thermal energy of heating sheet 5 be fully utilized, heat is sufficiently improved
Efficiency, heating sheet 5 are set on the lateral surface for the heat-conducting block 1 for being installed adjacent to inert gas ventilation pipe 4；Such as Fig. 4 and Fig. 6 embodiment.
It is corresponding in heating sheet 5 when heating sheet 5 is mounted on the face that open ray entrance aperture 6 or open ray perforation hole 2 is arranged
It is provided with corresponding hole on the position of ray incidence 6 or perforation hole 2, is passed freely through for ray, such as the implementation of Fig. 1, Fig. 5 and Fig. 6
Example.
Claims (9)
1. a kind of open heating device for synchrotron radiation in-situ test, including heat-conducting block (1) and it is provided with heat-conducting block (1)
On cross open sample cavity (3) and the open ray entrance aperture (6) communicated and open ray perforation hole (2), feature
It is: is provided with open sample cavity (3) in the middle part of heat-conducting block (1), sample freely runs through sample cavity；In open sample cavity
(3) outside it is communicated equipped with several successively perforation and other end tail portions open at one end with open sample cavity (3) in heat-conducting block (1)
Inert gas ventilation pipe (4), and heating sheet (5) are provided on the side of heat-conducting block (1).
2. the open heating device according to claim 1 for synchrotron radiation in-situ test, it is characterised in that: thermally conductive
Block (1) is aluminum or copper heat-conducting block.
3. the open heating device according to claim 1 or 2 for synchrotron radiation in-situ test, it is characterised in that:
Heating sheet (5) is ceramic heating flake, the position of corresponding ray incident (6) and perforation hole (2) is provided with aperture, for ray freedom
It passes through.
4. the open heating device according to claim 3 for synchrotron radiation in-situ test, it is characterised in that: open
Formula ray entrance aperture (6) and open ray perforation hole (2) are provided in the open sample cavity (3) of heat-conducting block (1) two sides
It entreats on position, sample cavity is passed perpendicularly through, with sample cavity connection.
5. the open heating device according to claim 4 for synchrotron radiation in-situ test, it is characterised in that: heating
Piece (5) is set on the lateral surface for the heat-conducting block (1) for being installed adjacent to ventilation pipe (4).
6. the open heating device according to claim 3 for synchrotron radiation in-situ test, it is characterised in that: heating
Piece (5) is set on the lateral surface for the heat-conducting block (1) for being installed adjacent to ventilation pipe (4).
7. the open heating device according to claim 1 or 2 for synchrotron radiation in-situ test, it is characterised in that:
Open ray entrance aperture (6) and open ray perforation hole (2) are provided with the open sample cavity (3) of heat-conducting block (1) two sides
Central part on, sample cavity is passed perpendicularly through, with sample cavity connection.
8. the open heating device according to claim 7 for synchrotron radiation in-situ test, it is characterised in that: heating
Piece (5) is set on the lateral surface for the heat-conducting block (1) for being installed adjacent to ventilation pipe (4).
9. the open heating device according to claim 1 or 2 for synchrotron radiation in-situ test, it is characterised in that:
Heating sheet (5) is set on the lateral surface for the heat-conducting block (1) for being installed adjacent to ventilation pipe (4).
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| Application Number | Priority Date | Filing Date | Title |
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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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| Application Number | Priority Date | Filing Date | Title |
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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 CN105263198A (en) | 2016-01-20 |
| CN105263198B true CN105263198B (en) | 2019-02-26 |
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| CN106714341B (en) * | 2016-12-21 | 2020-04-21 | 浙江师范大学 | Manufacturing method of open heater for synchrotron radiation in-situ test |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (1)
| 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 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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