CN209182268U - A kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement - Google Patents
A kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement Download PDFInfo
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- CN209182268U CN209182268U CN201822008901.1U CN201822008901U CN209182268U CN 209182268 U CN209182268 U CN 209182268U CN 201822008901 U CN201822008901 U CN 201822008901U CN 209182268 U CN209182268 U CN 209182268U
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Abstract
The utility model discloses a kind of temperature and pressure furnaces for fluid sample in-situ TiC particles and XAS combined measurement, which is characterized in that including furnace body, window film and pressing plate；The furnace body includes calandria and partition, and the calandria is annular in shape, and middle part forms inner hole, which is hollow structure, and heater strip is provided in cavity and forms heating chamber；The partition is arranged in inner hole, and divider upright is in the axis of inner hole, and its edge is connect with calandria, so that inner hole is divided into two pressing grooves, the strip sample cell through partition is offered on partition；The window film is covered on the two sides of sample cell；The pressing plate is arranged in window film and deviates from the side of sample cell, and is detachably connected with furnace body；Position on pressing plate corresponding to sample cell offers first through hole.The utility model has the advantage of so that temperature and pressure furnace can satisfy the angle requirement that XRD, XAS test experiments are, and can according to need exchange screen film, obtain the experimental data of high quality by reasonable structure setting.
Description
Technical field
The utility model belongs to technical field of experiment equipment, and in particular to one kind is used for fluid sample in-situ TiC particles and XAS
The temperature and pressure furnace of combined measurement.
Background technique
X-ray diffraction spectrum (XRD) and X-ray absorption spectrum (XAS) be research material microstructure two kinds of common technologies, two
Person's combined measurement can get the information in all directions such as sample atoms scale long-range order and local microstructure.It is closed using hydro-thermal method
During nano material, temperature and pressure is two important parameters for influencing liquid phase synthesis nano material, and method synthesis is received
Rice material generally selects temperature and pressure furnace as reaction tank.However, when acquiring X-ray diffraction spectrum and absorption spectra to reaction process, due to
XRD experiment needs the angular range measured to reach 20-120 degree, and conventional temperature and pressure furnace is difficult to meet its measurement angle through window
It is required that.
In document, such as Catalysis Today 275 (2016): 149 and Rev.Sci.Instr.85 (2014):
084105, in hydrothermal reaction process when in-situ acquisition X-ray diffraction spectrum, absorption spectra, the general capillary stone for selecting diameter 1-2mm
English glass tube is as reaction tank.But quartzy tube wall is serious to the absorption of X-ray, especially low energy X ray, frequently results in measurement
X-ray diffraction, absorption data are bad.
Utility model content
The technical problem to be solved by the utility model is to: reaction of the conventional temperature and pressure furnace as liquid phase synthesis nano material
Chi Shi is not able to satisfy angle requirement when in-situ TiC particles test.
The utility model solves above-mentioned technical problem using following technical scheme:
A kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement, including furnace body, window film and pressing plate；
The furnace body includes calandria and partition, and the calandria is annular in shape, and middle part forms inner hole, during which is
Hollow structure is provided with heater strip in cavity and forms heating chamber；The partition is arranged in inner hole, and divider upright is in the axis of inner hole
Line, and its edge is connect with calandria, so that inner hole is divided into two pressing grooves, the strip through partition is offered on partition
Shape sample cell；
The window film is covered on the two sides of sample cell；
The pressing plate is arranged in window film and deviates from the side of sample cell, and is detachably connected with furnace body；Correspond on pressing plate
The position of sample cell offers first through hole；
Described one end into sample outlet pipe is located in sample cell, and the other end is located at outside furnace body.
Preferably, a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model,
Sealing ring is equipped between the window film and pressing plate.
Preferably, a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model,
It further include lagging casing, the lagging casing is coated on pressing plate, and lagging casing corresponds to the position that first penetrates hole and opens up
There is second to penetrate hole.
Preferably, a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model,
The lagging casing includes two split type half shells, second is equipped in each half shell through hole, two half shells are set
It sets on the outside of corresponding pressing plate, and fastens and form the lagging casing.
Preferably, a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model,
The pressing plate includes ontology, and the side of the ontology is equipped with the annular convex platform for protruding outward, and penetrating hole around first, the ring
Shape boss, which protrudes into, compresses the window film and sealing ring in pressing groove, formed to sample cell and compress sealing.
Preferably, a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model,
The window film is diamond film, the beryllium film with protective layer, sapphire film or silicon nitride film.
Preferably, a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model,
The sealing ring is made of filamentary silver, aluminium wire or silica gel.
Preferably, a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model,
The sample cell is in rectangle.
Preferably, a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model,
The furnace body is equipped with rotation axis, and the rotation axis is vertically arranged with sample cell, and the lagging casing is equipped with and wears for rotation axis
The through-hole crossed.
Preferably, a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model,
Thermocouple is additionally provided in the heating chamber.
The utility model technology the utility model has the advantages that
To temperature when the temperature and pressure furnace that technical solutions of the utility model provide can meet hydro-thermal method nano materials simultaneously
With the requirement of pressure, and can satisfy XRD measurement when angle requirement；In addition, the material of window film can carry out as needed
Selection；
Select suitable window film, its absorption to X-ray can be reduced, improve the transmitance of X-ray, be effectively improved XRD,
The quality of data of XAS.
Detailed description of the invention
Fig. 1 is a kind of temperature and pressure for fluid sample in-situ TiC particles and XAS combined measurement described in the utility model embodiment
The top view of furnace；
Fig. 2 is the perspective view of the explosion of Fig. 1；
Fig. 3 is the cross-sectional view of Fig. 1, and lagging casing is not shown in figure；
Fig. 4 is working state schematic representation when carrying out XRD, XAS detection test simultaneously using the temperature and pressure furnace.
Specific embodiment
For convenient for those skilled in the art understand that technical solutions of the utility model, practical new to this now in conjunction with Figure of description
Type technical solution is described further.
Refering to fig. 1 to Fig. 3, the utility model embodiment discloses one kind and combines for fluid sample in-situ TiC particles with XAS
The temperature and pressure furnace of measurement comprising furnace body 1, window film 2, sealing ring 3, pressing plate 4, lagging casing 5 and (do not show in figure into sample outlet pipe
Out).
The furnace body 1 includes calandria 11 and partition 12, and the calandria 11 is annular in shape, and middle part forms inner hole (in figure
Do not mark), which is hollow structure, and heater strip (not shown) is provided in cavity and forms heating chamber；It is described
Partition 12 is arranged in inner hole, and partition 12 is perpendicular to the axis of inner hole, and its edge is connect with calandria 11, so that inner hole be divided
Two pressing grooves (being not marked in figure) are segmented into, the strip sample cell 13 through partition 12 is offered on partition 12；In this implementation
In example, the section of calandria 11 is square ring bodies, inner hole, sample cell 13 section be also in rectangle, and its longitudinal direction with plus
The longitudinal direction of hot body 11 is parallel.
The window film 2 is two panels, and shape is rectangle, and size and the pressing groove are adapted.Two panels window film 2 divides
It is not covered on the two sides of sample cell 13, to sealed sample 13.The material of window film 2 selects the transmitance of ray according to it
It selects.In general, diamond film, beryllium film, sapphire film, silicon nitride film etc. can use.But it should be noted that work as and use
When beryllium film, surface should plate the protective layer that a layer thickness is 10-20nm and need this is because the chemical property of beryllium is more active
It is avoided to react with solution.The material that may be used as protective layer has polyimides, aluminium oxide etc., according to furnace when specifically used
Temperature selects.However when using the beryllium film of plating as window film 2, its own with diffraction maximum, may with to test sample
The diffraction maximum of product interferes；The window film of other materials is larger to the absorption coefficient of X-ray, and therefore, diamond film is conduct
The optimal selection of window film.
The outside of the window film 2 is arranged in the pressing plate 4, to compress window film 2 to realize the compression of sample cell 13
Sealing, to reach sealing effect, is provided with sealing ring 3 between window film 2 and pressing plate 4.
Furnace temperature, the property of reaction liquid when according to reaction select suitable sealing ring 3.When furnace temperature is lower, sealing ring 3
Silica gel ring can be selected, but when furnace temperature is more than 300 DEG C, silica gel ring can lose sealing effect because of carbonization；It can also use similar
The soft metals material such as aluminium wire prepares sealing ring 3, and when making sealing ring 3 using wire, the diameter of wire is generally 1mm.
When experiment, commonly used is the sealing ring 3 being prepared by filamentary silver, and chemical property torpescence will not be reacted with reaction solution
And contaminated samples, and it is able to bear certain high temperature and pressure.
Pressing plate 4 is equipped with corresponding with sample cell 13 first and penetrates hole 43.Specifically, the pressing plate 4 includes ontology 41,
The side of the ontology 41 is equipped with the annular convex platform 42 for protruding outward and penetrating hole 43 around first, and the annular convex platform 42 is stretched
Enter and compress the window film 2 and sealing ring 3 in pressing groove, ontology 41 is connect by screw with calandria 11, by tightening screw
Pressure is generated, sealing ring 3 is promoted all to deform in the position of contact diamond film and seal groove, and then is generated reliable close
Envelope.
The lagging casing 5 includes the split type half shell 51 of two panels, and the half shell 51 is arranged in 4 outside of pressing plate,
The position for penetrating hole 43 corresponding to first offers second and penetrates hole 52；Two half shells 51, which mutually fasten, forms cladding pressing plate
4 lagging casing 5.
The disengaging sample is effective to connect sample cell 13 and extraneous reaction tank, so as to the disengaging of sample solution.Into sample outlet pipe
One end be arranged in sample cell 13, the other end is located at outside furnace body 1, so that sample cell 13 is in communication with the outside.
Further, for convenience of temperature is controlled, temperature and pressure furnace described in the present embodiment further includes having thermocouple (not show in figure
Out), K-type thermocouple can be used in the thermocouple, and test side is located in heating chamber.
As shown in figure 4, being acquired in liquid phase synthesis nano material reaction process simultaneously using temperature and pressure furnace described in the present embodiment
XRD, XAS data.Reaction solution is packaged in sample cell 13, is then placed it in the optical path of X-ray, and tilts certain angle
Degree, tilt angle is 135 ° in the present embodiment, acquires XRD, XAS data.When certain actual test, tilt angle root
It factually tests and needs to adjust in a certain range, to obtain optimal XAS data.
As a further improvement, rotation axis (not shown) can also be set at the middle part of the long side of furnace body 1, in this way
The temperature and pressure furnace can be set in a support (not shown) in experiment, and easily adjust tilt angle.Certainly, this
When lagging casing 5 on to be reserved for the through-hole (not shown) that rotation axis passes through.
It will be described in detail below and XRD, XAS data and conventional quartz capillary acquired using temperature and pressure furnace described in the present embodiment
The contrast effect of pipe acquisition XRD, XAS data.
Temperature and pressure furnace as embodiment uses with a thickness of 0.2mm, density 3.51g/cm3Diamond film as window film
2, when acquiring data, inclination angle alpha is 135 °, and the size of sample cell is 48 × 2 × 0.4 (mm)；Quartz wool as a comparison
The pipe thickness of tubule is 0.1mm, diameter 1mm, density 2.65g/cm3.Spot size (horizontal × vertical) when experiment
For 1.2 × 0.6mm.At this point, the amount of solution in x-ray bombardment sample cell is roughly the same with the amount of solution in capillary.
It is compared in the K ABSORPTION EDGE transmitance of Fe element
According to X-ray decay formula in the sample:
I=I0·e-μ(E)·d
In formula, I indicates the intensity after X-ray transparent sample；
I0Indicate the incident intensity of X-ray；
The thickness of d expression sample；
The absorption coefficient of μ (E) expression sample.
The ABSORPTION EDGE of Fe element is 7110eV, i.e., when the incident intensity of X-ray is 7110eV, diamond film is to X ray
Absorption is absorbed as 22.4cm-1, quartzy that 130.9cm is absorbed as to the absorption of X-ray-1。
Then X-ray pass through window film 2 made of unilateral diamond film with a thickness of
The transmitance of X-ray is 53%；
It follows that the transmitance after window film 2 made of the diamond film of X-ray transparent two sides is 53%*53%=
28.1%.
According to the above-mentioned strength formula that penetrates, the unilateral wall of quartz capillary is to the X ray that incident intensity is 7110eV
Transmitance is 27%, then quartz capillary is 27%*27%=7.3% to the transmitance of the X-ray of the intensity.Comparison it is found that
Using the temperature and pressure furnace of the present embodiment, select diamond film as window film, relative to quartz capillary, the transmitance of X-ray is mentioned
It is nearly 4 times high.
It is compared in the K ABSORPTION EDGE transmitance of Co element
The ABSORPTION EDGE of Co element is 7708eV, i.e. the incident intensity of X-ray is 7708eV, under this energy, diamond film
It is respectively 17.2cm with absorption coefficient of the quartz to X-ray-1And 103cm-1.Therefore using temperature and pressure furnace described in the present embodiment into
When row XRD, XAS are tested, the transmitance of X-ray is 37.6%；When using quartz capillary, the transmitance of X-ray is 12.7%.
Transmitance improves nearly 3 times.
It is compared in the K ABSORPTION EDGE transmitance of Ni element
The ABSORPTION EDGE of Ni element is 8830eV, i.e. the incident intensity of X-ray is 8830eV, under this energy, diamond film
It is respectively 11.3cm with absorption coefficient of the quartz to X-ray-1And 69.3cm-1.Therefore using temperature and pressure furnace described in the present embodiment into
When row XRD, XAS are tested, the transmitance of X-ray is 52.7%；When using quartz capillary, the transmitance of X-ray is 25.0%.
Transmitance improves more than 2 times.
Technical solutions of the utility model are exemplarily described utility model above in conjunction with attached drawing, it is clear that this is practical
Novel specific implementation is not subject to the restrictions described above, as long as using the method concept and technical solution progress of the utility model
Various unsubstantialities improve, or it is not improved the conception and technical scheme of utility model are directly applied into other occasions,
It both is within the protection scope of the present invention.
Claims (10)
1. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement, which is characterized in that including furnace body, window
Film, pressing plate and into sample outlet pipe；
The furnace body includes calandria and partition, and the calandria is annular in shape, and middle part forms inner hole, which is hollow knot
Structure is provided with heater strip in cavity and forms heating chamber；The partition is arranged in inner hole, divider upright in the axis of inner hole,
And its edge is connect with calandria, so that inner hole is divided into two pressing grooves, the strip through partition is offered on partition
Sample cell；
The window film is covered on the two sides of sample cell；
The pressing plate is arranged in window film and deviates from the side of sample cell, and is detachably connected with furnace body；Correspond to sample on pressing plate
The position in pond offers first through hole；
Described one end into sample outlet pipe is located in sample cell, and the other end is located at outside furnace body.
2. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement according to claim 1, feature
It is, sealing ring is equipped between the window film and pressing plate.
3. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement according to claim 1 or 2, special
Sign is, further includes lagging casing, and the lagging casing is coated on pressing plate, and lagging casing corresponds to the first position for penetrating hole
It sets and offers second through hole.
4. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement according to claim 3, feature
It is, the lagging casing includes two split type half shells, and second is equipped in each half shell through hole, two half-shells
Body is arranged on the outside of corresponding pressing plate, and fastens and form the lagging casing.
5. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement according to claim 2, feature
It is, the pressing plate includes ontology, and the side of the ontology is equipped with the annular convex platform for protruding outward and penetrating hole around first,
The annular convex platform, which protrudes into, compresses the window film and sealing ring in pressing groove, formed to sample cell and compress sealing.
6. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement according to claim 1, feature
It is, the window film is diamond film, the beryllium film with protective layer, sapphire film or silicon nitride film.
7. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement according to claim 2, feature
It is, the sealing ring is made of filamentary silver, aluminium wire or silica gel.
8. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement according to claim 1, feature
It is, the sample cell is in rectangle.
9. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement according to claim 3, feature
It is, the furnace body is equipped with rotation axis, and the rotation axis is vertically arranged with sample cell, and the lagging casing is equipped with for rotation
The through-hole that axis passes through.
10. a kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement according to claim 1, feature
It is, is additionally provided with thermocouple in the heating chamber.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109387529A (en) * | 2018-11-30 | 2019-02-26 | 中国科学院高能物理研究所 | A kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement |
| CN110687095A (en) * | 2019-10-12 | 2020-01-14 | 北京科技大学 | Device for in-situ high-temperature and high-pressure experiment |
-
2018
- 2018-11-30 CN CN201822008901.1U patent/CN209182268U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109387529A (en) * | 2018-11-30 | 2019-02-26 | 中国科学院高能物理研究所 | A kind of temperature and pressure furnace for fluid sample in-situ TiC particles and XAS combined measurement |
| CN110687095A (en) * | 2019-10-12 | 2020-01-14 | 北京科技大学 | Device for in-situ high-temperature and high-pressure experiment |
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