A small heating XRD reaction cell

Abstract

The utility model discloses the utility model technical scheme provides a kind of small heating XRD reaction pool, including reaction pool main body, the cylindrical cavity being arranged in reaction pool main body, the heat insulation component being arranged in cylindrical cavity, sample stage and the heating component of being sleeved in the outside of sample stage, and the water cooling structure being arranged in reaction pool main body. Cylindrical cavity top is provided with observation window piece and the pool cover for installing observation window piece, observation window piece is provided with sealing ring with the reaction pool main body;Thermocouple is inserted and connected in sample stage. The XRD reaction pool of the scheme can be directly adapted to brueker D6 diffractometer, without additional modification, reduce operation complexity and cost. Through heating sleeve, 600 ℃ high temperature can be realized, cooperate thermocouple close-range temperature measurement and closed-loop control, control temperature fluctuation at ±0.1 ℃, solve the problem of low temperature upper limit and poor uniformity of traditional equipment. Heat insulation component and water cooling structure cooperate, reduce heat loss and protect supporting equipment, improve safety.

Description

Technical Field

[0001] This utility model relates to the field of XRD reaction cells, and more specifically, to a small heated XRD reaction cell. Background Technology

[0002] X-ray diffraction (XRD) is an important tool for analyzing the microstructure of materials in fields such as materials science and chemistry, and it is widely used in in-situ analysis of materials, including high-temperature phase transitions and catalytic reactions. The Bruker D6 diffractometer, as a mainstream instrument in this field, requires a high-temperature reaction chamber to conduct in-situ experiments in order to observe the dynamic structural changes of materials under high-temperature conditions.

[0003] However, current high-temperature XRD reaction cells adapted to the Bruker D6 diffractometer have many technical limitations, making it difficult to meet the requirements of high-precision experiments: First, the upper temperature limit of traditional XRD high-temperature reaction cells is relatively low, which cannot cover the need for higher temperature conditions in high-temperature materials research, thus limiting in-depth exploration in related fields; Second, their compatibility with the Bruker D6 diffractometer is poor, often requiring additional modifications, which increases operational complexity and experimental costs; Third, temperature uniformity is insufficient, with temperature fluctuations typically exceeding ±1℃, resulting in poor temperature stability during experiments and directly affecting the accuracy of XRD analysis data; Fourth, poor sealing under high-temperature conditions can easily cause samples to come into contact with outside air, leading to sample oxidation or contamination and interfering with the reliability of experimental results.

[0004] Therefore, developing a small heating reaction cell that can achieve precise temperature control (±0.1℃), has high sealing performance, and can be directly adapted to a Bruker D6 diffractometer to solve the above-mentioned problems in the existing technology and meet the needs of high-temperature in-situ XRD experiments has become an urgent technical issue to be addressed in this field. Utility Model Content

[0005] The purpose of this invention is to provide a small heated XRD reaction cell to solve the technical problems existing in the background art.

[0006] This utility model provides a small heated XRD reaction cell, including a reaction cell body, a cylindrical cavity disposed within the reaction cell body, a heat insulation component disposed within the cylindrical cavity, a sample stage, a heating component sleeved outside the sample stage, and a water-cooling structure disposed within the reaction cell body.

[0007] The cylindrical cavity is provided with an observation window and a cell cover for mounting the observation window at the top. The observation window and the reaction cell body are provided with a sealing ring. The cell cover is detachably mounted on the reaction cell body. A thermocouple is inserted into the sample stage.

[0008] In a preferred embodiment, the thermal insulation assembly includes a thermal insulation sleeve adapted to the internal dimensions of the cylindrical cavity and quartz wool located inside the thermal insulation sleeve.

[0009] In a preferred embodiment, the sample stage is T-shaped and has a sample slot at the top for storing samples.

[0010] In a preferred embodiment, the heating assembly includes a heating sleeve fitted outside the sample stage, and the reaction cell body is provided with an outlet groove for the connecting wire of the heating sleeve to pass through.

[0011] In a preferred embodiment, the reaction tank body is provided with a channel one, and the sample stage is provided with a channel two corresponding to the position of the channel one, and the thermocouple passes through the channel two and is inserted into the channel one.

[0012] In a preferred embodiment, the water-cooling structure includes a water-cooling channel surrounding the main body of the reaction tank, an inlet pipe and an outlet pipe connecting the water-cooling channel, and the water-cooling channel is located outside the cylindrical cavity.

[0013] In a preferred embodiment, the top of the reaction tank body protrudes, and the tank cover is provided with a notch to accommodate the protruding part. The tank cover is fixed to the reaction tank body by bolts.

[0014] In a preferred embodiment, the observation window is a beryllium window.

[0015] The beneficial effects of this utility model's technical solution are:

[0016] The XRD reaction cell in this solution is directly compatible with the Bruker D6 diffractometer without additional modifications, reducing operational complexity and cost. A heating sleeve can achieve temperatures up to 600℃, and with close-range thermocouple temperature measurement and closed-loop control, temperature fluctuations are controlled within ±0.1℃, solving the problems of low temperature upper limits and poor uniformity in traditional equipment. The thermal insulation components and water-cooling structure work together to reduce heat loss and protect supporting equipment, improving safety. A beryllium window ensures X-ray penetration efficiency, and the protruding parts, recessed positioning, and sealing ring design achieve zero-leakage sealing at high temperatures, preventing sample oxidation and contamination. Overall, this solution improves the accuracy, repeatability, and ease of operation of experimental data, meeting the requirements of high-temperature in-situ XRD experiments. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the overall structure of this utility model.

[0018] Figure 2 This is an exploded view of the structure of this utility model.

[0019] Figure 3 This is a cross-sectional view of the present invention.

[0020] Explanation of reference numerals in the attached drawings: 1. Reaction cell body; 2. Cylindrical cavity; 3. Insulation sleeve; 4. Sample stage; 5. Sample tank; 6. Heating sleeve; 7. Outlet groove; 8. Channel 1; 9. Channel 2; 10. Thermocouple; 11. Observation window; 12. Cell cover; 13. Sealing ring; 14. Notch; 15. Protruding part; 16. Water cooling channel; 17. Water inlet pipe; 18. Water outlet pipe; 19. Gas inlet pipe; 20. Gas outlet pipe. Detailed Implementation

[0021] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments. The embodiments of the present invention are given for the purpose of illustration and description, and are not intended to be exhaustive or to limit the present invention to the disclosed forms. Many modifications and variations will be apparent to those skilled in the art. The embodiments were chosen and described to better illustrate the principles and practical applications of the present invention, and to enable those skilled in the art to understand the present invention and design various embodiments with various modifications suitable for a particular purpose.

[0022] like Figures 1-3 As shown, this utility model provides a small heated XRD reaction cell, including a reaction cell body 1, a cylindrical cavity 2 disposed within the reaction cell body 1, a heat insulation component disposed within the cylindrical cavity 2, a sample stage 4, a heating component sleeved outside the sample stage 4, and a water-cooling structure disposed within the reaction cell body 1. The top of the cylindrical cavity 2 is provided with an observation window 11 and a cell cover 12 for mounting the observation window 11. The observation window 11 and the reaction cell body 1 are provided with a sealing ring 13. The observation window 11 is a beryllium window. The cell cover 12 is detachably mounted on the reaction cell body 1. A thermocouple 10 is inserted into the sample stage 4.

[0023] In the above scheme, the reaction cell body 1 serves as the basic load-bearing structure, the cylindrical cavity 2 provides a closed space for sample reaction, and the inlet pipe 19 and outlet pipe 20 can introduce and discharge the gas required for the reaction into and out of the cylindrical cavity 2. The heat insulation component reduces heat loss from the heating component, which provides a high-temperature environment for the sample. The water-cooling structure removes excess heat from the reaction cell body 1 through circulating water to control the external temperature. The observation window 11 is a beryllium window, which utilizes its high X-ray transmittance to ensure normal acquisition of diffraction signals. The sealing ring 13 deforms under the pressure of the cell cover 12 to fill the gap between the observation window 11 and the reaction cell body 1 to achieve a seal. Thermocouple 10 is directly inserted into the sample stage 4 to sense the temperature of the sample area in real time and feed it back to the temperature control system.

[0024] The integrated design of each component solves the problems of low upper temperature limit, poor sealing and insufficient adaptability of traditional reaction cells; the beryllium window ensures X-ray penetration efficiency and improves signal quality; the sealing ring 13 enhances airtightness at high temperature and prevents sample oxidation or contamination; the thermocouple 10 provides a basis for precise temperature control in real time, and improves the accuracy of experimental data and the convenience of operation.

[0025] The thermal insulation component includes a thermal insulation sleeve 3 adapted to the internal dimensions of the cylindrical cavity 2 and quartz wool located inside the thermal insulation sleeve 3. The thermal insulation sleeve 3 (such as made of alumina) serves as the main thermal insulation barrier, preventing heat from the heating component from being conducted to the outside of the cylindrical cavity 2. The quartz wool has good thermal insulation and buffering properties, further reducing heat loss caused by thermal radiation and thermal convection. Together, they form a highly efficient thermal insulation layer.

[0026] The heat insulation components can significantly reduce heat loss, allowing more heat from the heating components to be used to raise the sample temperature. This not only meets the high-temperature requirement of 600℃ but also reduces temperature fluctuations. At the same time, it prevents excessive heat transfer to other parts of the reaction tank body 1. Combined with the water-cooling structure, it can stably maintain the outer surface temperature of the reaction tank and improve equipment safety.

[0027] The sample stage 4 is T-shaped, with a sample slot 5 at the top for storing the sample. The T-shaped structure increases the contact area between the sample stage 4 and the heating component, allowing heat to be conducted more evenly throughout the sample stage 4. The sample slot 5 physically limits and fixes the sample position, ensuring that the sample is always in a stable region under X-ray irradiation. The improved heating uniformity of the sample stage 4 reduces local temperature differences in the sample and lowers experimental data deviations. The sample slot 5 prevents the sample from shifting at high temperatures or during operation, ensuring the consistency of diffraction signals and improving experimental repeatability.

[0028] The heating assembly includes a heating sleeve 6 fitted around the sample stage 4, and a lead-out groove 7 is provided on the reaction tank body 1 for the connecting wires of the heating sleeve 6 to pass through. The heating sleeve 6 surrounds the sample stage 4 and generates heat through electric current to directly heat the sample stage 4 and the sample, thereby raising the temperature. The lead-out groove 7 provides a passage for the connecting wires of the heating sleeve 6, preventing exposed wires or compression that could affect the sealing and structural stability of the equipment. The heating sleeve 6 is in close contact with the sample stage 4, resulting in high heat conduction efficiency and rapid heating to 600℃, meeting the needs of high-temperature materials research. The lead-out groove 7 standardizes the wiring layout, ensuring a compact equipment structure, facilitating installation and maintenance, and preventing wiring interference with sealing performance.

[0029] The reaction tank body 1 is provided with a channel 8, and the sample stage 4 is provided with a channel 9 corresponding to the position of channel 8. The thermocouple 10 passes through channel 9 and is inserted into channel 8. The thermocouple 10 is directly inserted into the sample stage 4 through channel 9, close to the sample area, which can collect sample temperature data in real time and accurately. The collected temperature signal is transmitted to an external temperature controller through channel 8, forming a "temperature measurement-feedback-adjustment" closed loop. The temperature controller dynamically adjusts the current of the heating sleeve 6 according to the signal to achieve precise temperature control.

[0030] The above settings enable thermocouple 10 to measure temperature at close range, resulting in high data accuracy. When used with a temperature controller, temperature fluctuations can be controlled within ±0.1℃, solving the problem of insufficient temperature uniformity in traditional equipment. The closed-loop control mechanism ensures temperature stability, providing a reliable temperature environment for high-temperature in-situ XRD experiments.

[0031] The water-cooling structure includes a water-cooling channel 16 surrounding the reaction tank body 1, an inlet pipe 17 connecting the water-cooling channel 16, and an outlet pipe 18. The water-cooling channel 16 is located outside the cylindrical cavity 2. Cooling water enters the water-cooling channel 16 through the inlet pipe 17. As it flows through the interior of the reaction tank body 1, it absorbs a small amount of heat leaking from the insulation components and is then discharged through the outlet pipe 18, forming a continuous heat dissipation cycle. This keeps the outer surface temperature of the reaction tank body 1 near room temperature. This prevents the outer surface of the reaction tank body 1 from overheating due to high temperatures, thus preventing damage to the circuitry or structure of supporting equipment such as the Bruker D6 diffractometer. Simultaneously, it keeps the outer surface temperature of the reaction tank ≤30℃, improving operational safety and preventing burns to laboratory personnel.

[0032] The reaction tank body 1 has a protruding part 15 at its top, and the tank cover 12 has a recess 14 to accommodate the protruding part 15. The tank cover 12 is fixed to the reaction tank body 1 by bolts. The cooperation between the protruding part 15 and the recess 14 enables precise positioning of the tank cover 12 and the reaction tank body 1, ensuring that the observation window 11 is aligned with the X-ray beam path. When the bolts are tightened, axial pressure is generated, causing the tank cover 12 to press the observation window 11 and the sealing ring 13 tightly. After being compressed and deformed, the sealing ring 13 fills the tiny gap between the observation window 11 and the reaction tank body 1, enhancing the sealing effect.

[0033] Precise positioning avoids signal attenuation caused by the observation window 11 deviating from the optical path, ensuring the quality of diffraction data; the combination of bolt tightening and sealing ring 13 deformation can still achieve zero leakage sealing at a high temperature of 600℃, completely solving the problem of sample oxidation or contamination; the detachable design of the pool cover 12 facilitates sample replacement and equipment cleaning, improving operational convenience.

[0034] The XRD reaction cell in this design is directly compatible with the Bruker D6 diffractometer, requiring no additional modifications and reducing operational complexity and cost. A high temperature of 600℃ can be achieved through the heating sleeve 6, and with close-range temperature measurement by the thermocouple 10 and closed-loop control, temperature fluctuations are controlled within ±0.1℃, solving the problems of low upper temperature limits and poor uniformity in traditional equipment. The thermal insulation components and water-cooling structure work together to reduce heat loss and protect supporting equipment, improving safety. The beryllium window ensures X-ray penetration efficiency, and the protruding part 15, the notch 14, and the sealing ring 13 design achieve zero-leakage sealing at high temperatures, preventing sample oxidation and contamination. Overall, this design improves the accuracy, repeatability, and ease of operation of experimental data, meeting the requirements of high-temperature in-situ XRD experiments.

[0035] Obviously, the described embodiments are only a part of the embodiments of this utility model, and not all of them. All other embodiments obtained by those skilled in the art and related fields based on the embodiments of this utility model without creative effort should fall within the protection scope of this utility model. Structures, devices, and operating methods not specifically described and explained in this utility model, unless otherwise specified or limited, shall be implemented according to conventional means in the art.

Claims

1. A small heated XRD reaction cell, characterized in that: It includes a reaction tank body, a cylindrical cavity disposed within the reaction tank body, a heat insulation component disposed within the cylindrical cavity, a sample stage, a heating component sleeved outside the sample stage, and a water-cooling structure disposed within the reaction tank body. The cylindrical cavity is provided with an observation window and a cell cover for mounting the observation window at the top. The observation window and the reaction cell body are provided with a sealing ring. The cell cover is detachably mounted on the reaction cell body. A thermocouple is inserted into the sample stage.

2. The small heated XRD reaction cell according to claim 1, characterized in that: The thermal insulation assembly includes a thermal insulation sleeve adapted to the internal dimensions of the cylindrical cavity and quartz wool located inside the thermal insulation sleeve.

3. A small heated XRD reaction cell according to claim 1, characterized in that: The sample stage is T-shaped and has a sample slot at the top for storing samples.

4. A small heated XRD reaction cell according to claim 1, characterized in that: The heating assembly includes a heating sleeve fitted outside the sample stage, and the reaction cell body is provided with an outlet groove for the connecting wire of the heating sleeve to pass through.

5. A small heated XRD reaction cell according to claim 1, characterized in that: The reaction tank body is provided with a channel one, and the sample stage is provided with a channel two corresponding to the position of the channel one. The thermocouple passes through the channel two and is inserted into the channel one.

6. A small heated XRD reaction cell according to claim 1, characterized in that: The water-cooling structure includes a water-cooling channel surrounding the main body of the reaction tank, an inlet pipe and an outlet pipe connecting the water-cooling channel, and the water-cooling channel is located outside the cylindrical cavity.

7. A small heated XRD reaction cell according to claim 1, characterized in that: The main body of the reaction tank has a protruding top, and the tank cover has a notch to accommodate the protruding part. The tank cover is fixed to the main body of the reaction tank by bolts.

8. A small heated XRD reaction cell according to claim 1, characterized in that: The observation window is a beryllium window.

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