CN214794541U - X-ray grazing incidence in-situ characterization device with temperature regulation function - Google Patents
X-ray grazing incidence in-situ characterization device with temperature regulation function Download PDFInfo
- Publication number
- CN214794541U CN214794541U CN202120647771.5U CN202120647771U CN214794541U CN 214794541 U CN214794541 U CN 214794541U CN 202120647771 U CN202120647771 U CN 202120647771U CN 214794541 U CN214794541 U CN 214794541U
- Authority
- CN
- China
- Prior art keywords
- ray
- device cavity
- grazing incidence
- situ characterization
- window
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The utility model discloses an X-ray grazing incidence in-situ characterization device with temperature regulation function, relating to the technical field of material synthesis-performance integration in-situ characterization, which comprises an X-ray window, a sample table, a heating element, a connecting frame and a device cavity, wherein the X-ray window is cylindrical, one end of the device cavity is provided with a first opening, and the X-ray window is covered at the first opening end of the device cavity; one end of the connecting frame is located in the device cavity and connected with one end of the device cavity, the other end of the connecting frame is located in the X-ray window, the sample table is located at the other end of the connecting frame, and the heating element is located below the sample table. The beneficial effects of the utility model reside in that: the method can realize the catalytic reaction test of a heterogeneous catalytic system under different temperature conditions, understand the active site change and the active source of the catalyst in the whole reaction process and further disclose the catalytic reaction mechanism of the catalyst.
Description
Technical Field
The utility model relates to a material synthesis-performance integration normal position sign technical field, concretely relates to X ray grazes incident normal position sign device with temperature regulation function.
Background
In heterogeneous catalytic reaction systems with high temperatures, such as large-scale industrial catalysis, in-situ characterization of the catalyst is of great importance. Although many studies have been made on catalysts using in situ and operational studies, including studies using combinatorial techniques, the knowledge in the literature about the surface composition of catalysts under reaction conditions is very limited, since most techniques characterize most catalysts. However, changes in surface composition are most relevant to explain the catalytic events that occur at the catalyst surface. It is further important to note that the average volume structure of the material does not represent the surface composition, as demonstrated by a recent study by Karim et al. With respect to the size-dependent redox behavior of iron, it is shown that iron grows in layers during oxidation, forming Fe (0)/FeO/Fe3O4/Fe2O3Core-shell structure. Dynamic surface changes of the catalyst under the reaction conditions (e.g., surface segregation processes) are generally not taken into account. The assumption is made primarily based on an average bulk structure that leads to misleading conclusions about the mechanism of action or deactivation of the active phase, active sites, promoters, thus hindering further optimization and development of the catalyst. For example, despite intensive research into High Temperature Water Gas Shift (HTWGS) iron-based catalysts, the nature of the active sites and the HTWGS reaction mechanism (redox and association reactions) are under constant debate. The unsolved problems and conflicting results relate to the interaction of chromium oxide with iron oxide (around the iron oxide phase, magnetite forms a Cr-rich shell, and Cr3+Strong interaction with magnetite) as a means of stabilizing the iron oxide against sintering.
At present, for the research of the surface structure of a catalyst in a heterogeneous catalytic system, more ex-situ characterization means is adopted for testing, but for the research of the structure of the catalyst in a metastable state/non-equilibrium state, the ex-situ surface test cannot effectively characterize the middle real reaction environment, and more seriously, unreal experimental data can be easily obtained, so that the research thought of researchers is misled. In order to research the structure change of the real active site of the catalyst, the current common practice is to utilize the in-situ infrared spectrum technology, which is a key technology for researching surface adsorbed substances and is particularly important for disclosing reaction intermediates. However, it does not provide characteristics with respect to the redox properties of the catalyst surface. One of the most important factors controlling the catalytic activity, selectivity and stability of the catalyst, especially for redox reactions, is the redox nature of the surface (oxidation state and interaction between oxidation states during the reaction). For example, patent publication No. CN207730645U discloses a temperature-controllable electrochemical in-situ raman infrared combined spectrum cell, but infrared spectroscopy is limited by the vibration characteristic of its molecular structure, and only can realize the study of the structural change of small molecules on the surface of the catalyst, but cannot realize effective breakthrough in the study of active sites of the catalyst itself, especially in the study of electronics.
Compared with the existing in-situ infrared spectroscopy technology, the grazing incidence X-ray spectroscopy technology, such as scattering, diffraction, absorption and other spectroscopy technologies, is more meaningful because not only the structural change of the surface of the catalyst can be obtained, but also the change information of the electronic structure and the like of the catalyst can be provided. Therefore, how to design an in-situ characterization device with grazing incidence X-ray spectroscopy technology will provide great help for research on the real active sites of the catalyst in the heterogeneous catalytic system and the root source of catalytic activity.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that an incident X ray spectrum device is glancing to normal position high temperature electricity is provided.
The utility model discloses a following technical means realizes solving above-mentioned technical problem:
the utility model provides an X-ray grazing incidence in-situ characterization device with temperature regulation function, which comprises an X-ray window, a sample table, a heating element, a connecting frame and a device cavity, wherein the X-ray window is cylindrical, one end of the device cavity is provided with a first opening, and the X-ray window is covered at the first opening end of the device cavity;
the one end of link is located the device cavity, is connected with the one end of device cavity, the other end of link is located the X ray window, the sample platform is located the other end of link, the heating member is located sample platform below.
The working principle is as follows: and placing the powder sample on a sample table, covering the X-ray window at the first opening end of the cavity of the device, and then installing the device on an X-ray diffractometer.
Has the advantages that: the utility model provides a X ray grazing incidence normal position characterization device with temperature regulation function passes through cylindric X ray window, benefit from the geometric shape of cylinder, X ray incident angle can be the vertical state with the curved surface of cylinder completely, X ray pierces through the effective distance minimum of window, thereby guarantee the low angle of X ray, the realization of all aspects angles such as high angle, the completion is grazed XRD data acquisition work under the complex conditions such as incidence, and simultaneously, the space holding degree of cylindric structure itself is big, also can realize the compatibility of various shapes to inside sample platform, can help the sample to react under high temperature, and the window still keeps the condition of certain stable temperature, the normal clear of heterogeneous catalytic reaction system under the high temperature condition has been guaranteed. Provides great help for researchers to research the active sites of the catalyst in different reaction processes.
The connecting frame is mainly used for supporting and cooling the sample table, the sample table is connected with the device cavity through the connecting frame, and a temperature transition interval is provided for the heated sample table.
The device in the utility model not only can realize heterogeneous catalytic system's under the different temperature conditions catalytic reaction test, can also realize surveying catalyst surface structure's geometry and electronics structure through grazing incident X ray spectroscopy methodology, multiple spectroscopy methods such as X ray scattering, diffraction and absorption, finally know the active site change and the active source of catalyst in whole reaction process, reveal its catalytic reaction mechanism from more deep level.
Preferably, one end of the device cavity is provided with a second opening, the second opening is opposite to the first opening, and the second opening is provided with a panel.
Preferably, the panel is detachably connected with the device cavity, and one end of the connecting frame is connected with the side wall of the panel.
Preferably, the panel is provided with a gas connecting end communicated with the device cavity.
Has the advantages that: the gas connecting end is connected with an external vacuum pump body and various gas bottle devices and is used for processing vacuum or other various atmospheres required in the device cavity.
Preferably, the outer side wall of the device cavity is provided with a water-cooling shell, and the water-cooling shell is provided with a water-cooling connecting end.
Has the advantages that: the safe operation temperature of the cavity of the device is ensured under the high-temperature use condition, and the water-cooling connecting end is used for the connecting function of the water-cooling shell and a water source.
Preferably, the panel lateral wall is equipped with electricity link, sample platform below is equipped with temperature sensor, temperature sensor and heating member all are connected with electricity link through the circuit.
Has the advantages that: the electricity link is used for heating member and temperature sensor's connection function for provide the power and accurate control temperature.
Preferably, the X-ray grazing incidence in-situ characterization device with the temperature regulation function further comprises a supporting unit, the supporting unit comprises a supporting rod and a base, one end of the supporting rod is connected with the base, and the other end of the supporting rod is connected with the outer side wall of the device cavity.
Has the advantages that: the supporting unit is designed to be matched with different sample platforms of different diffractometers, and is used for matching zero position control of the sample platform.
Preferably, the X-ray window is mounted on the device cavity through a window cover plate.
Preferably, an annular connecting plate is arranged on the outer side wall of one end of the X-ray window, a through hole is formed in the center of the window cover plate, a groove matched with the annular connecting plate is formed in the window cover plate, the X-ray window penetrates through the through hole, and the window cover plate is detachably connected with the device cavity.
Preferably, the device cavity is cylindrical, and the X-ray window is arranged coaxially with the device cavity.
The utility model discloses a theory of operation: and placing the powder sample on a sample table, covering the X-ray window at the first opening end of the cavity of the device, and then installing the device on an X-ray diffractometer.
The utility model has the advantages that: the utility model provides a X ray grazing incidence normal position characterization device with temperature regulation function passes through cylindric X ray window, benefit from the geometric shape of cylinder, X ray incident angle can be the vertical state with the curved surface of cylinder completely, X ray pierces through the effective distance minimum of window, thereby guarantee the low angle of X ray, the realization of all aspects angles such as high angle, the completion is grazed XRD data acquisition work under the complex conditions such as incidence, and simultaneously, the space holding degree of cylindric structure itself is big, also can realize the compatibility of various shapes to inside sample platform, can help the sample to react under high temperature, and the window still keeps the condition of certain stable temperature, the normal clear of heterogeneous catalytic reaction system under the high temperature condition has been guaranteed.
The connecting frame is mainly used for supporting and cooling the sample table, the sample table is connected with the device cavity through the connecting frame, and a temperature transition interval is provided for the heated sample table.
Drawings
Fig. 1 is a schematic structural diagram of an X-ray grazing incidence in-situ characterization device with a temperature adjustment function according to an embodiment of the present invention;
fig. 2 is a side view of an X-ray grazing incidence in-situ characterization device with temperature adjustment function according to an embodiment of the present invention;
FIG. 3 is a schematic cross-sectional view taken along the line A in FIG. 2;
in the figure: an X-ray window 111; an annular connecting plate 112; a window cover plate 113; a sample stage 114; a heating furnace 115; a temperature sensor 116; a connecting frame 117; a device cavity 118; a panel 119; a water-cooled connection end 120; a gas connection end 121; electrical connection terminals 122; a support rod 123; a base 124.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the embodiments of the present invention are described in detail and completely, and obviously, the described embodiments are some, but not all embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
It is noted that, in this document, relational terms such as first and second, and the like, if any, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
An X-ray grazing incidence in-situ characterization device with temperature regulation function, as shown in fig. 1 and 3, comprises an X-ray window 111, a sample stage 114, a heating element, a connecting frame 117, a window cover plate 113 and a device cavity 118.
As shown in fig. 1, in order to ensure that all aspects of angles such as low angle and high angle of the X-ray are achieved, and complete the XRD data acquisition under complex conditions such as grazing incidence, the X-ray window 111 in this embodiment is cylindrical. The X-ray window 111 is made of a material with high X-ray penetrability, such as a polymer material and metallic beryllium, so that the penetrability of X-rays is ensured, and the stability of the window structure is ensured. The thickness of the window is chosen to ensure penetration of the X-rays, typically between 0.05 and 1mm or less than 0.05mm, to ensure that the penetration of the X-ray energy at the 8kev position can be more than 50%. Wherein the material of the X-ray window 111 is prior art.
The device cavity 118 is cylindrical, the appearance can be designed to be more exquisite, the minimum diameter can be set to be 20mm, and the size of the sample stage 114 of various commercial X-ray diffractometers can be easily met; the design structure is compact, and the high-temperature heat is kept well. The X-ray window 111 is arranged coaxially with the device cavity 118 in this embodiment.
As shown in fig. 1 and 3, the device cavity 118 is hollow, and the material of the device cavity 118 is selected from a metal material, such as a light aluminum alloy, but not limited to a metal material. A first opening is formed in one end of the device cavity 118, a window cover plate 113 is mounted on the first opening, and the X-ray window 111 is covered on the first opening of the device cavity 118 through the window cover plate 113. The outer side wall of one end of the X-ray window 111 is fixedly provided with an annular connecting plate 112, the center of the window cover plate 113 is provided with a through hole, the window cover plate 113 is provided with a groove matched with the annular connecting plate 112, the X-ray window 111 penetrates through the through hole, the window cover plate 113 is arranged on the device cavity 118 through a screw, and the screw can be an M3 screw.
The other end of the device cavity 118 is provided with a second opening, and the panel 119 is mounted on the second opening by screws. One end of the connecting frame 117 is located in the device cavity 118, and one end of the connecting frame 117 is centrally connected with the panel 119 installed on the second opening, and the connecting mode may be welding, bonding or threaded connection, and the specific connecting mode is set according to actual needs. The other end of the connecting frame 117 is located within the X-ray window 111. The panel 119 is made of a metal material, such as a light aluminum alloy material, and the panel 119 is used for integrating a supporting function of the sample stage 114, a gas inlet and outlet function, and a power supply control function in the whole device.
The connecting frame 117 is made of ceramic, the connecting frame 117 is rod-shaped, and the diameter of the connecting frame 117 is 3mm in the embodiment, but the specific size is set according to actual needs. The sample stage 114 is fixedly installed at one end of the connecting frame 117, the sample stage 114 is located in the X-ray window 111, and the installation mode of the sample stage 114 and the connecting frame 117 is the prior art.
A heating element is arranged under the sample table 114 and used for heating a sample in the sample table 114, the sample table 114 is used for placing a sample to be detected, the area to be detected is a round bin with the diameter of 10mm, and the material is metal or ceramic which is sensitive to temperature and insensitive to X-ray crystallization. The heating element is a heating furnace 115, a temperature sensor 116 is also arranged below the sample table 114, and the installation mode of the heating furnace 115 and the temperature sensor 116 is the prior art. The heating furnace 115 and the temperature sensor 116 are used for adjusting and controlling the temperature of the sample stage 114, the heating furnace 115 is electrically heated in a heating resistance wire mode, and the temperature sensor 116 can be a common thermocouple or a Pt100 temperature sensor 116.
The outer side wall of the device cavity 118 is provided with a water-cooling housing (not shown), and the water-cooling housing is provided with a water-cooling connecting end 120. The water-cooled connecting end 120 is used for connecting the water-cooled shell and a water source, and the safe operation temperature of the device cavity 118 is ensured under the high-temperature use condition of the device.
The panel 119 is fixedly provided with two gas connecting ends 121 communicated with the device cavity 118, and the gas connecting ends 121 are connected with an external vacuum pump body and various gas bottle devices for processing vacuum or other various atmospheres required in the device cavity 118.
In order to match different diffractometer sample stage 114 racks and be used for matching zero position control of sample stage 114, the X-ray grazing incidence in-situ characterization device with the temperature regulation function further comprises a supporting unit, the supporting unit comprises a supporting rod 123 and a base 124, one end of the supporting rod 123 is fixedly connected with the base 124, and the other end of the supporting rod 123 is fixedly connected with the outer side wall of the device cavity 118.
The working principle of the embodiment is as follows: the powder sample is placed on sample stage 114, X-ray window 111 is mounted to apparatus cavity 118, and then mounted on the X-ray diffractometer.
The beneficial effects of the embodiment are that: the device is designed through the structure of the cylindrical X-ray window 111, not only solves the difficulty of low-angle incidence of X-rays, but also ensures the space utilization rate of the internal structure, so that the structure can be added with conditions such as temperature and the like. In addition, the in-situ device can realize the catalytic reaction test of the heterogeneous catalytic system under different temperature conditions, wherein the temperature adjusting range is from room temperature to 500 ℃. Meanwhile, the geometric and electronic structure detection of the surface structure of the catalyst can be realized through grazing incidence X-ray spectroscopy methodologies, such as X-ray scattering, diffraction, absorption and other spectroscopy methods, and finally the active site change and the active source of the catalyst in the whole reaction process are known, so that the catalytic reaction mechanism of the catalyst is further disclosed.
The device in the utility model not only can realize heterogeneous catalytic system's under the different temperature conditions catalytic reaction test, can also realize surveying catalyst surface structure's geometry and electronics structure through grazing incident X ray spectroscopy methodology, multiple spectroscopy methods such as X ray scattering, diffraction and absorption, finally know the active site change and the active source of catalyst in whole reaction process, reveal its catalytic reaction mechanism from more deep level.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention in its corresponding aspects.
Claims (10)
1. An X-ray grazing incidence in-situ characterization device with a temperature regulation function is characterized in that: the device comprises an X-ray window, a sample table, a heating element, a connecting frame and a device cavity, wherein the X-ray window is cylindrical, a first opening is formed in one end of the device cavity, and the X-ray window is covered at the first opening end of the device cavity;
the one end of link is located the device cavity, is connected with the one end of device cavity, the other end of link is located the X ray window, the sample platform is located the other end of link, the heating member is located sample platform below.
2. The grazing incidence in-situ characterization device with temperature adjustment function according to claim 1, wherein: a second opening is formed in one end of the device cavity and is opposite to the first opening, and a panel is arranged on the second opening.
3. The grazing incidence in-situ characterization device with temperature adjustment function according to claim 2, wherein: the panel is detachably connected with the device cavity, and one end of the connecting frame is connected with the side wall of the panel.
4. The grazing incidence in-situ characterization device with temperature adjustment function according to claim 2, wherein: and the panel is provided with a gas connecting end communicated with the device cavity.
5. The grazing incidence in-situ characterization device with temperature adjustment function according to claim 2, wherein: the panel lateral wall is equipped with the electricity link, sample platform below is equipped with temperature sensor, temperature sensor and heating member all are connected with the electricity link through the circuit.
6. The grazing incidence in-situ characterization device with temperature adjustment function according to claim 1, wherein: the outer side wall of the device cavity is provided with a water-cooling shell, and the water-cooling shell is provided with a water-cooling connecting end.
7. The grazing incidence in-situ characterization device with temperature adjustment function according to claim 1, wherein: the X-ray grazing incidence in-situ characterization device with the temperature regulation function further comprises a supporting unit, the supporting unit comprises a supporting rod and a base, one end of the supporting rod is connected with the base, and the other end of the supporting rod is connected with the outer side wall of the cavity of the device.
8. The grazing incidence in-situ characterization device with temperature adjustment function according to claim 1, wherein: the X-ray window is installed on the device cavity through the window cover plate.
9. The grazing incidence in-situ characterization device with temperature adjustment function according to claim 8, wherein: the X-ray window is characterized in that an annular connecting plate is arranged on the outer side wall of one end of the X-ray window, a through hole is formed in the center of the window cover plate, a groove matched with the annular connecting plate is formed in the window cover plate, the X-ray window penetrates through the through hole, and the window cover plate is detachably connected with the device cavity.
10. The grazing incidence in-situ characterization device with temperature adjustment function according to claim 1, wherein: the device cavity is cylindrical, and the X-ray window and the device cavity are coaxially arranged.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120647771.5U CN214794541U (en) | 2021-03-30 | 2021-03-30 | X-ray grazing incidence in-situ characterization device with temperature regulation function |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120647771.5U CN214794541U (en) | 2021-03-30 | 2021-03-30 | X-ray grazing incidence in-situ characterization device with temperature regulation function |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN214794541U true CN214794541U (en) | 2021-11-19 |
Family
ID=78667947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202120647771.5U Active CN214794541U (en) | 2021-03-30 | 2021-03-30 | X-ray grazing incidence in-situ characterization device with temperature regulation function |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN214794541U (en) |
-
2021
- 2021-03-30 CN CN202120647771.5U patent/CN214794541U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Saadatkhah et al. | Experimental methods in chemical engineering: Thermogravimetric analysis—TGA | |
| Baranov et al. | Optimization of power consumption for gas sensor nodes: A survey | |
| CN202024941U (en) | On-line monitoring device for material weightlessness in microwave field | |
| Wu et al. | Use of cobalt oxide CoOOH in a carbon monoxide sensor operating at low temperatures | |
| Ivanov et al. | Investigation of catalytic hydrogen sensors with platinum group catalysts | |
| Binions et al. | Zeolite-modified discriminating gas sensors | |
| Roslyakov et al. | Microhotplate catalytic sensors based on porous anodic alumina: Operando study of methane response hysteresis | |
| CN101558294A (en) | High temperature and pressure sensor | |
| CN112485198A (en) | High-low temperature in-situ spectrum reaction tank | |
| CN214794541U (en) | X-ray grazing incidence in-situ characterization device with temperature regulation function | |
| Zhang et al. | Microwave dielectric heating behavior of supported MoS2 and Pt catalysts | |
| JP2004500577A (en) | Hydrogen monitoring and removal system | |
| CN107643358B (en) | Hydrogen sensor based on catalysis composite heat release principle | |
| Gheytani et al. | Formaldehyde Electro‐catalytic Oxidation onto Carbon Paste Electrode Modified by MIL‐101 (Cr) Nanoparticles | |
| Wang et al. | Mesoporous WO3 modified by Mo for enhancing reduction of CO2 to solar fuels under visible light and thermal conditions | |
| Hansma et al. | Chemisorption and catalysis on oxidized aluminum metal | |
| Haidry et al. | Sensing mechanism of low temperature NO2 sensing with top–bottom electrode (TBE) geometry | |
| Schmidt et al. | Elucidation of structure–activity relations in proton electroreduction at Pd surfaces: Theoretical and experimental study | |
| CN109946363A (en) | One kind is based on the porous SnO that classifies2/Zn2SnO4The C of sensitive electrode2H2Sensor and preparation method thereof | |
| WO2003002999A1 (en) | Method and detection of presence of hydrogen gas and measurement of content of hydrogen gas | |
| Hao et al. | A novel catalytic-type gas sensor based on alumina ceramic substrates loaded with catalysts and printed electrodes | |
| EP2304454A2 (en) | A magnetometer | |
| Hassaninejad‐Darzi | Application of synthesized NaA nanozeolite as a novel supported electrode for the formaldehyde electro‐catalytic oxidation | |
| US20200096490A1 (en) | Method for analyzing gas and device for analyzing gas | |
| CN102698657B (en) | Catalytic reaction device of mercury |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |