CN212622327U - In-situ X-ray characterization device - Google Patents
In-situ X-ray characterization device Download PDFInfo
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- CN212622327U CN212622327U CN202021256275.9U CN202021256275U CN212622327U CN 212622327 U CN212622327 U CN 212622327U CN 202021256275 U CN202021256275 U CN 202021256275U CN 212622327 U CN212622327 U CN 212622327U
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Abstract
The utility model provides an normal position X ray characterization device, include: the device comprises an in-situ cavity, an incident window and an exit window are respectively arranged at two axial ends of the in-situ cavity, and an external gas interface and an irradiation equipment interface are arranged on the in-situ cavity; a sample compartment disposed within the in situ cavity, the sample compartment being heatable; the crucible is arranged in the sample cabin and used for containing a sample; and the gas type, the vacuum degree, the irradiation condition and/or the heating temperature of the in-situ X-ray characterization device can be adjusted, so that the signal measurement of the sample under different conditions is realized. According to the utility model discloses, a can satisfy the normal position X ray sign device of multiple requirements such as high temperature, specific gas environment, fused salt contact and normal position irradiation simultaneously is provided.
Description
Technical Field
The utility model relates to a X ray characterization device field, more specifically relate to an normal position X ray characterization device.
Background
The X-ray characterization technology comprises the technologies of X-ray diffraction (XRD), X-ray absorption spectrum (XAFS), X-ray fluorescence (XFS) and the like, is a powerful means for researching material structures, and has wide application in subjects of condensed state physics, material science, chemical engineering, environmental geology and the like. With the development of experimental techniques and methods, in-situ X-ray characterization is becoming a focus of research. Many materials are subjected to high temperature environments during growth, preparation or service, and sometimes specific atmospheric environments, which makes it extremely necessary to develop high temperature, atmospheric in situ X-ray characterization devices. The nuclear energy material is contacted with molten salt in the service process, even is subjected to ion irradiation and other conditions, and the development of an X-ray characterization device for in-situ irradiation has very important application. At present, the development of X-ray characterization devices for high temperature and gas environment at home and abroad is not much, the existing high-temperature devices only can ensure high-temperature heating but can not be vacuumized, less specific gas environment can be applied, and equipment capable of carrying out molten salt contact and in-situ irradiation is not available at present or even not. In addition, the heating process of the heating device commonly used at present is not easy to control, and inaccurate temperature measurement is a common problem. Also, the heating devices commonly used today are too large to fit on a diffractometer.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing an normal position X ray sign device to solve among the prior art X ray sign device and can not satisfy the problem of multiple requirements such as high temperature, specific gas environment, fused salt contact and normal position irradiation simultaneously.
In order to solve the technical problem, the utility model discloses a following technical scheme:
an in-situ X-ray characterization apparatus is provided, comprising: the device comprises an in-situ cavity, an incident window and an exit window are respectively arranged at two axial ends of the in-situ cavity, and an external gas interface and an irradiation equipment interface are arranged on the in-situ cavity; a sample compartment disposed within the in situ cavity, the sample compartment being heatable; the crucible is arranged in the sample cabin and used for containing a sample; and the gas type, the vacuum degree, the irradiation condition and/or the heating temperature of the in-situ X-ray characterization device can be adjusted, so that the signal measurement of the sample under different conditions is realized.
Preferably, the in-situ cavity has a cylindrical shape, and the entrance window and the exit window respectively have a horn shape with gradually increasing size.
Preferably, the maximum inner diameter dimension of the exit window is larger than the maximum inner diameter dimension of the entrance window to maximize the scattered X-ray acceptance angle.
Preferably, the irradiation equipment interface is located at the top end of the in-situ cavity and aligned with the sample chamber to ensure that irradiation particles are uniformly irradiated on the surface of the sample from top to bottom.
Preferably, the in-situ cavity is further provided with a water inlet and a water outlet for externally connecting circulating cooling water, and the water inlet is lower than the water outlet.
Preferably, a thermocouple plug interface is further arranged on the in-situ cavity, and a thermocouple measuring end is arranged in the sample chamber and used for measuring the temperature of the sample.
Preferably, the bottom of the outer side of the in-situ cavity is provided with an auxiliary pipe communicated with the inside of the cavity, the vacuum pump interface is arranged on the side wall of the auxiliary pipe, and the bottom of the auxiliary pipe is provided with a diffractometer interface.
Preferably, a threaded sleeve is arranged at the interface of the diffractometer, the sleeve is used for connecting the in-situ X-ray characterization device with the diffractometer, and the diffractometer is used for controlling the position and the inclination angle of the in-situ X-ray characterization device so as to meet the geometric requirement of grazing incidence.
Preferably, the crucible comprises: the crucible body and the crucible cap are connected through threads.
Preferably, the crucible is made of graphite or boron nitride.
According to the utility model provides a pair of normal position X ray sign device, be equipped with thermocouple plug interface simultaneously, the heating circuit interface, the external gas interface, vacuum pump interface, and irradiation equipment interface, still be equipped with heatable sample cabin in the cavity simultaneously, consequently can make up gas at will, the vacuum, the irradiation, multiple experimental environment such as temperature, still satisfy fused salt contact and normal position irradiation's requirement simultaneously, incident window and emergent window adopt respectively to increase the size, the regulation of the sample position of being convenient for, whole device can be in the horizontal plane certain angle within range internal rotation, be convenient for satisfy various experimental requirements.
Therefore, according to the utility model discloses, a can satisfy the normal position X ray sign device of multiple requirements such as high temperature, specific gas environment, fused salt contact and normal position irradiation simultaneously is provided.
Drawings
Fig. 1 is a schematic diagram illustrating an operation principle of an in-situ X-ray characterization apparatus according to a preferred embodiment of the present invention;
FIG. 2 is a perspective view of the in situ X-ray characterization apparatus shown in FIG. 1;
FIG. 3 is another perspective view of the in situ X-ray characterization apparatus shown in FIG. 1;
fig. 4 is a schematic view of the structure of the sample chamber and the crucible.
Detailed Description
The present invention will be further described with reference to the following specific embodiments. It should be understood that the following examples are illustrative of the present invention only and are not intended to limit the scope of the present invention.
Referring to fig. 1 to 3, an in-situ X-ray characterization apparatus according to a preferred embodiment of the present invention includes: the device comprises an in-situ cavity 1, wherein an incident window 2 and an emergent window 3 are respectively arranged at two axial ends of the in-situ cavity 1, and an irradiation equipment interface 4, a thermocouple plug interface 5, a heating circuit interface 6 and an external gas interface 8 are arranged on the in-situ cavity 1; a sample chamber 7 arranged in the in-situ cavity 1, wherein the sample chamber 7 can be heated; the crucible is used for containing a sample 11 and is arranged in the sample cabin 7; and the type of gas in the in-situ X-ray characterization device, and/or the vacuum degree, and/or the irradiation condition, and/or the heating temperature can be adjusted, so that the signal measurement of the sample under different conditions is realized.
According to the preferred embodiment, as shown in fig. 2, the home position cavity 1 has a substantially cylindrical shape, and the entrance window 2 and the exit window 3 have horn shapes with gradually increasing sizes, respectively.
The incident window 2 and the exit window 3 are both sealed by polyimide film materials, so that the penetration of X rays can be guaranteed, certain vacuum degree can be guaranteed, visible light can also penetrate through, and the condition inside the cavity can be conveniently and visually observed. The whole surface of the incident window 2 is sealed by a polyimide film material, so that the sufficient size of the incident window is ensured, the position of a sample is convenient to adjust, the whole device can rotate within a certain angle range in a horizontal plane, and various experimental requirements are convenient to meet; the whole surface of the exit window 3 is sealed by a polyimide film, so that scattered X rays can be emitted in the maximum solid angle range, and various high-dimensional detectors 20 are conveniently arranged at the rear end part.
Preferably, the maximum inner diameter dimension of the exit window 3 is larger than the maximum inner diameter dimension of the entrance window 2 to maximize the scattered X-ray reception angle.
The incident window 2 and the emergent window 3 are sealed by flanges and rubber rings, so that the air tightness of the whole device is ensured.
As shown in fig. 1, the irradiation equipment interface 4 is disposed at the top end of the in-situ chamber 1 and is aligned with the sample chamber 7 in the vertical direction to ensure that the irradiation particles are uniformly irradiated on the surface of the sample 11 from top to bottom. It should be understood that the irradiation equipment interface 4 may also be sealed in place so that the port is closed when the irradiation equipment is not accessed and the device is used normally.
For example, a blind plate and a clip are provided at the interface 4 of the irradiation equipment, and the interface can be closed when the irradiation equipment is not connected.
As shown in fig. 3, the thermocouple plug interface 5 is disposed at an inclined lower side of the in-situ cavity 1 and can be connected with a thermocouple plug, a thermocouple line is disposed inside the in-situ cavity 1, and the thermocouple measuring end is disposed inside the sample chamber 7, so as to realize real-time measurement of the temperature of the sample.
As shown in fig. 2, the heating line interface 6 is disposed on the oblique lower side of the in-situ cavity 1, and can be inserted into the positive electrode and the negative electrode of the heating power supply respectively, so as to facilitate the installation and disassembly of the heating experimental device.
Referring to fig. 1 to 2, an auxiliary pipe 15 communicated with the inside of the in-situ cavity 1 is arranged at the bottom of the outer side of the in-situ cavity 1, an external gas port 8 is arranged on the side wall of the auxiliary pipe 15, and other gas is filled by unscrewing an air inlet valve and can be connected with a flow meter, so that the configuration of the air environment inside the in-situ cavity 1 can be completed.
According to the preferred embodiment, the external gas interface 8 is located below the in-situ cavity 1 and connected with the in-situ cavity 1 through the auxiliary pipe 15, so that the gas can be prevented from disturbing the sample 11 after the gas is introduced, and temperature fluctuation is reduced. If some experiments require reducing gases such as hydrogen or special chemical gas environments, a flexible gas pipe can be adopted to connect the external gas interface 8 with the gas supply device.
According to the preferred embodiment, the external gas interface 8 can also be used as a vacuum pump interface, and the interior of the in-situ cavity 1 can be vacuumized by starting the vacuum pump according to the requirement, so that the requirement of vacuum degree is met.
As shown in fig. 1, the bottom of the auxiliary tube 15 is further provided with a diffractometer interface 9, the diffractometer interface 9 is provided with a clamping sleeve with threads, the in-situ X-ray characterization device can be connected with the diffractometer angle measuring head of the 14B line station through the clamping sleeve, and the diffractometer can accurately control the position and the inclination angle of the in-situ X-ray characterization device, so that the diffractometer meets the geometric requirement of grazing incidence.
As shown in fig. 4, the crucible is divided into two parts, namely a crucible body 10 and a crucible cap 12, which are connected through screw threads and sealed inside a sample to be heated, so that the connection tightness is ensured, the sample 11 is contained in the crucible, the crucible is contained in the sample chamber 7, and the sample chamber 7 is designed to be in a shape with a concave middle, so that the heating efficiency and the temperature stability are ensured. Preferably, the crucible is made of graphite or boron nitride, which can both ensure the penetration of X-rays and withstand a certain heating temperature. The crucible is a consumable material, can be replaced after each experiment, and does not need to be reused.
According to the preferred embodiment, the sample chamber 7 is made of a ceramic material and has a heating wire inside, which, when energized, heats the entire sample chamber.
As shown in fig. 1, the in-situ cavity 1 is further provided with a water inlet 13 and a water outlet 14, a water path is arranged inside a shell of the in-situ cavity 1 and used for externally connecting circulating cooling water, and preferably, the water inlet 13 is lower than the water outlet 14 so as to ensure uniform cooling of the shell of the cavity and avoid the phenomenon of overhigh temperature.
According to the preferred embodiment, the heating wires, the thermocouples and other line interfaces are all placed on the outer side of the in-situ cavity, so that the inner space of the cavity is relatively loose, and the whole device is tidy and reliable.
The whole device can be heated to 1200 ℃, and the vacuum degree can reach 10-3And (6) handkerchief.
The whole set of device is less than 700g, and the requirement of the current angle measuring head of the line station diffractometer on bearing is met.
According to a preferred embodiment of the present invention, the specific working mode of the in-situ X-ray characterization apparatus is described as follows:
1) firstly, the in-situ X-ray characterization device is connected to a Huber5021 diffractometer, and the diffractometer can accurately control the position and the inclination angle of the device so as to meet the geometric requirement of grazing incidence;
2) placing a sample in a crucible body, screwing a crucible cap, sealing the sample in the crucible body, smearing a thin layer of molten salt on the surface of the sample if the molten salt is needed, and screwing the crucible cap;
3) placing the whole crucible in a sample cabin, screwing screws on flanges of an incident window and an exit window, and finally placing the whole device on an angle measuring head of a diffractometer until the installation process of the sample is finished; the surface height of the sample is higher than that of the sample cabin after the crucible is placed in the sample cabin, so that X-rays can be irradiated on the surface of the sample when a glancing experiment is carried out at the back;
4) connecting other external devices such as a heating wire, a thermocouple, a temperature control system and a vacuum pump outside the in-situ cavity, and selectively connecting an irradiation source or a gas flowmeter and the like according to the requirement;
5) connecting circulating water at a water inlet of the in-situ cavity to ensure that the circulating water flows in from a lower water inlet and flows out from a higher water outlet, and starting the circulating water;
6) after the light cutting of the surface of the sample is finished by a conventional means, the whole device is slightly inclined, so that a small included angle is formed between incident X rays and the surface of the sample, and the incident X rays can glash on the surface of the sample;
7) a surface detector is arranged behind the emergent window, and receives the emergent X-ray signals to complete information collection;
8) starting a vacuum pump to vacuumize the interior of the in-situ cavity or unscrewing an air inlet valve to fill a certain amount of air according to requirements to complete the configuration of the air environment in the in-situ cavity;
9) according to the needs of the experiment, a temperature rising and reducing curve is set, a temperature rising and reducing program is started, and signals are collected at proper time.
According to the utility model provides an in situ X ray characterization device, in the experimentation, can make up multiple experimental environment such as gas, vacuum, irradiation, temperature at will, measures the signal of sample.
What has been described above is only the preferred embodiment of the present invention, not for limiting the scope of the present invention, but various changes can be made to the above-mentioned embodiment of the present invention. All the simple and equivalent changes and modifications made according to the claims and the content of the specification of the present invention fall within the scope of the claims of the present invention. The present invention is not described in detail in the conventional technical content.
Claims (10)
1. An in-situ X-ray characterization apparatus, comprising:
the device comprises an in-situ cavity, an incident window and an exit window are respectively arranged at two axial ends of the in-situ cavity, and an external gas interface and an irradiation equipment interface are arranged on the in-situ cavity;
a sample compartment disposed within the in situ cavity, the sample compartment being heatable; and
the crucible is arranged in the sample cabin and used for containing a sample;
and the gas type, the vacuum degree, the irradiation condition and/or the heating temperature of the in-situ X-ray characterization device can be adjusted, so that the signal measurement of the sample under different conditions is realized.
2. The in-situ X-ray characterization device according to claim 1, wherein the in-situ cavity has a cylindrical shape, and the entrance window and the exit window each have a horn shape with gradually increasing size.
3. The in-situ X-ray characterization device according to claim 1, wherein the maximum inner diameter dimension of the exit window is larger than the maximum inner diameter dimension of the entrance window to maximize the scattered X-ray acceptance angle.
4. The in-situ X-ray characterization device according to claim 1, wherein the irradiation equipment interface is located at the top end of the in-situ cavity and aligned with the sample chamber to ensure uniform irradiation of the irradiation particles on the surface of the sample from top to bottom.
5. The in-situ X-ray characterization device according to claim 1, wherein the in-situ cavity is further provided with a water inlet and a water outlet for externally connecting circulating cooling water, and the water inlet is lower than the water outlet.
6. The in-situ X-ray characterization device according to claim 1, wherein a thermocouple plug interface is further provided on the in-situ cavity, and a thermocouple measurement end is provided in the sample chamber for measuring the temperature of the sample.
7. The in-situ X-ray characterization device according to claim 1, wherein an auxiliary tube communicating with the inside of the in-situ cavity is disposed at the bottom of the outside of the in-situ cavity, the external gas port is disposed at a side wall of the auxiliary tube, and a diffractometer port is disposed at the bottom of the auxiliary tube.
8. The in-situ X-ray characterization device according to claim 7, wherein a threaded ferrule is provided at the diffractometer interface, the connection of the in-situ X-ray characterization device and the diffractometer is achieved through the ferrule, and the control of the position and the tilt angle of the in-situ X-ray characterization device is achieved through the diffractometer, so that the geometric requirements of grazing incidence are met.
9. The in-situ X-ray characterization device according to claim 1, wherein the crucible comprises: the crucible body and the crucible cap are connected through threads.
10. The in-situ X-ray characterization device according to claim 1, wherein the crucible is made of graphite or boron nitride.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202021256275.9U CN212622327U (en) | 2020-06-30 | 2020-06-30 | In-situ X-ray characterization device |
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| CN202021256275.9U CN212622327U (en) | 2020-06-30 | 2020-06-30 | In-situ X-ray characterization device |
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| CN212622327U true CN212622327U (en) | 2021-02-26 |
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