Heating body for ultra-high temperature thermal field platform, preparation method and application thereof

By using pre-reduced graphene oxide film as the heating element, optimizing its aspect ratio and thickness, and combining it with high-temperature resistant ceramic materials, the problems of slow heating and inaccurate measurement in existing ultra-high temperature field equipment are solved, realizing rapid and accurate temperature field construction and measurement, which is suitable for aerospace and advanced materials experiments.

CN114258165BActive Publication Date: 2025-11-25NAT UNIV OF DEFENSE TECH
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Patent Information

Application Number
CN202011025385.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-09-25
Publication Date
2025-11-25
Estimated Expiration
2040-09-25

AI Technical Summary

Technical Problem

Existing ultra-high temperature field construction equipment suffers from slow heating rate, inaccurate temperature field measurement, and poor repeatability. Furthermore, common heating element materials cannot achieve large-area, rapid heating and precise temperature control.

Method used

By using pre-reduced graphene oxide film as the heating element, and by optimizing its aspect ratio, thickness and carrier material, combined with specific preparation processes including coating, heat treatment and curing steps, a lightweight, ultra-thin heating element with stable heating performance is prepared.

Benefits of technology

It achieves ultra-high temperature fields with fast heating rate, high temperature, and precise temperature control, and can construct temperature fields above 1500℃ in milliseconds. The temperature field has strong repeatability and is suitable for aerospace and advanced materials experiments.

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Abstract

The application discloses a heating body for an ultrahigh-temperature temperature field platform and a preparation method and application thereof, and relates to a pre-reduction graphene oxide film with a length greater than a width, a width less than or equal to 10 mm, and a thickness less than or equal to 200 microns. The preparation method comprises the following steps: preparing a graphene oxide film; and performing heat treatment on the graphene oxide film. In the application, the pre-reduction graphene oxide film is a light, ultrathin, stable heating performance and rapid Joule heat effect heating body material, has the advantages of a fast temperature rising rate, a high temperature and an accurate temperature adjustment, and when used as a heating source of the ultrahigh-temperature temperature field platform, can construct an ultrahigh-temperature temperature field which is accurate, controllable, fast in temperature rising rate and high in repeatability, and has high use value and good application prospect. The preparation method has the advantages of simple process, convenient operation and low cost, can realize large-scale preparation, is suitable for industrial production, and is beneficial to the popularization and application of the ultrahigh-temperature temperature field platform.
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Description

Technical Field

[0001] This invention belongs to the field of ultra-high temperature environment measurement, and relates to a heating element for an ultra-high temperature field platform, its preparation method and application. Background Technology

[0002] Due to its applicability in cutting-edge fields such as aerospace, advanced materials, and advanced processing technologies, the construction of ultra-high temperature fields has attracted widespread attention in recent years. Research shows that constructing ultra-high temperature fields with broad application value typically requires meeting three conditions: precise and controllable temperature field, rapid heating rate, and real-time measurement of the temperature field.

[0003] Currently, common methods for constructing ultra-high temperature environments mainly rely on equipment such as graphite furnaces, high-temperature combustion chambers, and wind tunnels. While graphite furnace heating can create a precise and controllable temperature field and measure it in real time, its heating rate is extremely slow, not exceeding 10°C / min in the high-temperature range, which cannot meet the experimental requirements of advanced material systems. Although high-temperature combustion chambers have a fast heating rate, their temperature field fluctuates greatly, and the temperature field measurement is relatively coarse. Wind tunnels can create a precise and controllable ultra-high temperature field with a fast heating rate and accurate temperature field measurement, but their experimental cycle is long, and they consume a lot of resources, making it impossible to conduct experiments frequently.

[0004] Furthermore, the key to achieving precise and controllable temperature fields, rapid heating rates, and high repeatability in ultra-high temperatures lies in obtaining a heating element material with excellent properties such as being lightweight, ultrathin, easy to prepare, stable in performance, and exhibiting rapid Joule heating. Currently, common heating element materials include tungsten and graphite, but these have the following problems: Because tungsten is a metallic material, it generates relatively low Joule heating, therefore it is usually prepared as a filamentary structure, making it impossible to construct large-area temperature fields; graphite has a large thickness and a slow heating rate, typically around 10... 3 ℃ / s; Graphene has low resistivity and its Joule heating effect is not obvious. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to overcome the shortcomings of the prior art and provide a lightweight, ultra-thin heating element with stable heating performance and rapid Joule heating effect for use in ultra-high temperature field platforms, as well as its preparation method and application.

[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0007] A heating element for an ultra-high temperature field platform, wherein the heating element is a pre-reduced graphene oxide film; the length of the pre-reduced graphene oxide film is greater than or equal to its width, and the width is less than or equal to 20 mm; the thickness of the pre-reduced graphene oxide film is less than or equal to 200 μm.

[0008] In a further improvement of the heating element for the ultra-high temperature field platform described above, the aspect ratio of the pre-reduced graphene oxide film is 1 to 50:1, the width is 0.1 mm to 10 mm, and the thickness of the pre-reduced graphene oxide film is 1 μm to 200 μm.

[0009] In a further improvement of the heating element for the ultra-high temperature field platform described above, the aspect ratio of the pre-reduced graphene oxide film is 1 to 10:1, the width is 0.3 mm to 8 mm, and the thickness of the pre-reduced graphene oxide film is 5 μm to 25 μm.

[0010] The heating element for the ultra-high temperature field platform described above is further improved by including a carrier material, wherein the pre-reduced graphene oxide film is fixed on the carrier material; the carrier material is a high-temperature resistant ceramic material; the high-temperature resistant ceramic material is an alumina ceramic material or a silicon carbide ceramic material.

[0011] As a general technical concept, the present invention also provides a method for preparing the above-mentioned heating element for an ultra-high temperature field platform, comprising the following steps:

[0012] S1. Coat the substrate with an aqueous solution of graphene oxide nanosheets and dry it to obtain a graphene oxide film.

[0013] S2. The graphene oxide film obtained in step S1 is subjected to heat treatment to obtain a pre-reduced graphene oxide film.

[0014] The above preparation method, in a further improvement, also includes the following steps:

[0015] S3. The pre-reduced graphene oxide film obtained in step S2 is bonded to the carrier material and cured to obtain a heating element for an ultra-high temperature field platform.

[0016] In a further improvement to the above preparation method, in step S3, a pre-reduced graphene oxide film is bonded to a carrier material using conductive silver paste; the curing is carried out in an air atmosphere; the curing is performed by fixing the pre-reduced graphene oxide film to the carrier material at a temperature of 100℃~170℃; and the curing time is 10min~60min.

[0017] In a further improvement to the above preparation method, in step S1, the coating involves placing an aqueous solution of graphene oxide nanosheets on a substrate and then using a scraper to coat the solution onto the substrate. The scraping speed of the scraper is 8 mm / s to 15 mm / s; the distance between the scraper and the substrate is 1 mm to 4 mm; the scraper is a blade; the substrate is a copper foil; the concentration of the aqueous solution of graphene oxide nanosheets is 4 mg / mL to 10 mg / mL; and the diameter of the graphene oxide nanosheets in the aqueous solution is 5 μm to 50 μm. The drying involves heating the substrate to 30°C to 40°C; and the drying time is 8 h to 36 h.

[0018] In a further improvement to the above preparation method, in step S2, the heat treatment is carried out under an inert atmosphere; the temperature of the heat treatment is 700℃~850℃; and the time of the heat treatment is 10min~60min.

[0019] As a general technical concept, the present invention also provides an application of the above-mentioned heating element or the heating element prepared by the above-mentioned method as a heat source in constructing an ultra-high temperature field platform.

[0020] Compared with the prior art, the advantages of the present invention are as follows:

[0021] (1) This invention provides a heating element for an ultra-high temperature field platform. The heating element is a pre-reduced graphene oxide film, wherein the length of the pre-reduced graphene oxide film is greater than or equal to its width, the width is less than or equal to 10 mm, and the thickness is less than or equal to 200 μm. In this invention, the pre-reduced graphene oxide film is a heating element material with excellent properties such as being lightweight, ultra-thin, having stable heating performance, and exhibiting rapid Joule heating. It has advantages such as fast heating rate, high temperature, and precise temperature adjustment. When used as a heating source for an ultra-high temperature field platform, it can construct an ultra-high temperature field (>1500℃) in milliseconds, with a heating rate as high as 10... 5 The temperature can reach up to 3000℃ / s, with broad application prospects. The temperature field is precisely controllable, and the temperature can be precisely controlled by current, achieving a temperature adjustment of 0.1℃. Moreover, the composition will not change in a vacuum or inert atmosphere, and a stable ultra-high temperature field can be maintained for more than 24 hours. The temperature field is adjustable and measurable in real time, and can be adjusted at any time according to application needs. Therefore, when the pre-reduced graphene oxide film of this invention is used as a heating element to construct an ultra-high temperature field platform, an ultra-high temperature field with precise controllability, fast heating rate, and strong repeatability can be constructed, which is of great significance for constructing an ultra-high temperature field platform with wide application value.

[0022] (2) In the heating element of the ultra-high temperature field platform, this invention optimizes the aspect ratio of the pre-reduced graphene oxide film to 1–50:1, the width to 0.1 mm–10 mm, and the thickness to 1 μm–200 μm. By optimizing the aspect ratio of the pre-reduced graphene oxide film, a large-area temperature field with higher temperature can be obtained under relatively small current conditions. Based on this, by optimizing the width of the pre-reduced graphene oxide film to 0.1 mm–10 mm and the thickness to 1 μm–200 μm, the uniform temperature distribution of the constructed temperature field is ensured while achieving rapid temperature rise, thereby realizing precise control of the large-area temperature field. To achieve better measurement accuracy, the following reasons apply: if the width of the pre-reduced graphene oxide film is too large, it will cause significant differences in the Joule heating effect in different regions of the film surface, resulting in large differences in the temperature distribution of the temperature field (large temperature fluctuations). If the width is too small, the heating rate of the temperature field will be too fast, which will increase the difficulty of temperature control. If the thickness of the pre-reduced graphene oxide film is too small, the thin heating element film will also cause the heating rate of the temperature field to be too fast, which will also increase the difficulty of temperature control. If the thickness is too large, the thick heating element film will cause the heating rate of the temperature field to be too slow, which is not conducive to obtaining high temperature measurement resolution.

[0023] (3) The heating element used in the ultra-high temperature field platform of the present invention also includes a carrier material, which is a high-temperature resistant ceramic material. The high-temperature resistant ceramic material used in the present invention can maintain the stability of its own structure under high temperature environment, and its structure and composition will not change significantly. At the same time, it will not affect the radiation performance of the pre-reduced graphene oxide film. Therefore, by fixing the pre-reduced graphene oxide film on the high-temperature resistant ceramic material, it is more conducive to constructing an ultra-high temperature field with precise and controllable temperature field, fast heating rate and strong repeatability.

[0024] (4) This invention also provides a method for preparing a heating element for an ultra-high temperature field platform. First, an aqueous solution of graphene oxide nanosheets is coated onto a substrate and dried to obtain a graphene oxide film. Then, the graphene oxide is pre-reduced to pre-reduced graphene oxide through heat treatment to obtain a pre-reduced graphene oxide film. Finally, the pre-reduced graphene oxide film is fixed onto a carrier material through curing to obtain a heating element for the ultra-high temperature field platform. The preparation method of this invention has advantages such as simple process, convenient operation, and low cost. It can achieve large-scale preparation, is suitable for industrial production, and is conducive to the widespread application of heating elements in the construction of ultra-high temperature field platforms.

[0025] (5) In the preparation method of this invention, the coating speed is optimized to be 8 mm / s to 15 mm / s, and the distance between the scraper and the substrate is 1 mm to 4 mm. The advantage of this is that the obtained graphene oxide film has a smooth surface, complete structure, good mechanical properties, and is convenient for subsequent processing. If the coating speed is too slow, it will cause liquid leakage, resulting in uneven film thickness. If the coating speed is too fast, the liquid will be subjected to excessive shear force, which is not conducive to obtaining a regular microstructure. If the distance between the scraper and the substrate is too small, it will reduce the mechanical properties of the film and be not conducive to subsequent processing. If the distance between the scraper and the substrate is too large, it will result in excessive film thickness and reduce the heating rate of the film.

[0026] (6) In the preparation method of the present invention, the drying conditions are optimized. Specifically, the substrate material is heated to 30°C to 40°C for drying, and the drying time is 8h to 36h. Under these conditions, since the drying temperature is relatively low, the evaporation rate of the solvent can be reduced, which is beneficial to obtaining a denser graphene oxide film.

[0027] (7) In the preparation method of the present invention, the heat treatment conditions are optimized. Specifically, the heat treatment is carried out in an argon atmosphere at a temperature of 700℃~850℃ for a time of 10min~60min. Under these conditions, some of the graphene oxide film is reduced, which is beneficial to improving the electrical and thermal conductivity of the pre-reduced graphene oxide film.

[0028] (8) In the preparation method of the present invention, the curing conditions are further optimized after the pre-reduced graphene oxide film is bonded to the carrier material. Specifically, the curing is carried out in an air atmosphere at a temperature of 100℃~170℃ for a time of 10min~60min. Under these conditions, the pre-reduced graphene oxide film can be better fixed on the carrier material, which is more conducive to constructing an ultra-high temperature field with precise and controllable temperature field, fast heating rate and strong repeatability.

[0029] (9) The present invention provides an application of a heating element in the construction of an ultra-high temperature field platform. The ultra-high temperature field platform constructed using the heating element of the present invention as the heat source has the advantages of precise and controllable temperature field, fast heating rate, strong repeatability and real-time measurement, which is of great significance for expanding the application range of the ultra-high temperature field platform. Attached Figure Description

[0030] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings.

[0031] Figure 1 This is a flowchart illustrating the preparation process of the heating element in Embodiment 1 of the present invention.

[0032] Figure 2This is a physical image of the heating element used in the ultra-high temperature field platform prepared in Embodiment 1 of the present invention.

[0033] Figure 3 This is a schematic diagram of the ultra-high temperature field platform constructed in Embodiment 1 of the present invention.

[0034] Figure 4 This is a schematic diagram of the vacuum chamber in Embodiment 1 of the present invention.

[0035] Figure 5 The images show the radiation spectrum intensity of the ultra-high temperature field platform constructed in Embodiment 1 of the present invention under different current conditions.

[0036] Figure 6 The images show the radiation spectrum intensity of the ultra-high temperature field platform constructed in Embodiment 1 of the present invention after being filtered by a 550nm filter under different current conditions.

[0037] Figure 7 This is a temperature change diagram of the ultra-high temperature field platform constructed in Embodiment 1 of the present invention under different current conditions.

[0038] Figure 8 This is a graph showing the heating rate and cooling rate of the ultra-high temperature field platform constructed in Embodiment 1 of the present invention.

[0039] Legend:

[0040] 1. Vacuum chamber; 2. Powered sample stage; 3. Sample displacement stage; 4. Fiber optic spectrometer; 5. Fiber optic cable; 6. CCD camera; 7. Spectral displacement stage; 8. Mechanical pump; 9. Vacuum gauge; 10. Source meter; 11. PLC controller; 12. Chamber door; 13. Observation window. Detailed Implementation

[0041] The present invention will be further described below with reference to the accompanying drawings and specific preferred embodiments, but this does not limit the scope of protection of the present invention.

[0042] Example 1

[0043] A heating element for an ultra-high temperature field platform, wherein the heating element is a pre-reduced graphene oxide film, which is prepared by heat treatment of graphene oxide nanosheets.

[0044] In this embodiment, the pre-reduced graphene oxide film has a length of 5 mm, a width of 0.5 mm, and a thickness of 10 μm.

[0045] In this embodiment, a high-temperature resistant carrier material is also included, and a pre-reduced graphene oxide film is fixed on the high-temperature resistant carrier material, wherein the high-temperature resistant carrier material is an alumina ceramic material.

[0046] A method for preparing the heating element for the ultra-high temperature field platform in this embodiment, such as... Figure 1 As shown, it includes the following steps:

[0047] (1) Graphene oxide nanosheets with a diameter of 40 μm to 50 μm were mixed with water to prepare an aqueous solution of graphene oxide nanosheets with a concentration of 8 mg / mL.

[0048] (2) Place the aqueous solution of graphene oxide nanosheets obtained in step (1) on a copper foil substrate, and use a scraper to evenly coat the aqueous solution of graphene oxide nanosheets on the substrate, wherein the distance between the scraper and the substrate is adjusted to 2 mm and the scraping speed is 12 mm / s; then heat the substrate coated with the aqueous solution of graphene oxide nanosheets to 35°C and slowly dry it for 24 h to obtain a graphene oxide film.

[0049] (3) The graphene oxide film obtained in step (2) is reduced at 800°C for 30 minutes under an argon atmosphere to obtain a pre-reduced graphene oxide film.

[0050] (4) Cut the pre-reduced graphene oxide film obtained in step (3) into 5mm×0.5mm pre-reduced graphene oxide strips, and use conductive silver paste to bond the pre-reduced graphene oxide strips to the alumina ceramic mold; then place the mold with the pre-reduced graphene oxide strips bonded to it in an air atmosphere and heat it at 150°C for 30 minutes to solidify the conductive silver paste, thereby obtaining a heating element for an ultra-high temperature field platform.

[0051] Figure 2 This is a photograph of the heating element used in the ultra-high temperature field platform prepared in Embodiment 1 of the present invention. Figure 2 As shown, the heating element is a pre-reduced graphene oxide film (strip); simultaneously, it is composed of... Figure 2 It can be seen that the two ends of the pre-reduced graphene oxide film (strip) are fixed on the alumina ceramic substrate by silver paste, and the two ends of the pre-reduced graphene oxide film (strip) are respectively connected to electrode materials.

[0052] An application of the heating element prepared in Embodiment 1 of the present invention as a heat source in constructing an ultra-high temperature field platform is as follows: using the heating element prepared in Embodiment 1 as a heat source to construct an ultra-high temperature field platform.

[0053] like Figure 3 , 4As shown, an ultra-high temperature field platform includes a vacuum chamber 1, within which an electrically powered sample stage 2 for supporting a heating element is located at the bottom. One heating element (pre-reduced graphene oxide film) is fixed on the electrically powered sample stage 2, and the electrode materials at both ends of the heating element are connected to a source meter 10 via wires. The source meter 10 has a current range of 1nA to 10A and a voltage range of 1mV to 200V.

[0054] In this embodiment, a sample moving stage 3 for carrying the sample to be tested is also provided inside the vacuum chamber 1, located directly above the energized sample stage 2. Specifically, the sample to be tested on the sample moving stage 3 is located directly above the heating element, and the distance between the heating element and the sample to be tested is adjusted by moving the sample moving stage 3, with a distance range of 1mm to 50mm. The sample moving stage 3 is a three-axis displacement stage, with an X-axis movement range of 0 to 20cm and an X-axis displacement accuracy of 0.1mm, a Y-axis movement range of 0 to 10cm and a Y-axis displacement accuracy of 0.1mm, and a Z-axis movement range of 0 to 40cm and a Z-axis displacement accuracy of 0.1mm. The sample moving stage 3 can be moved away when measuring the temperature field distribution on the surface of the luminescent element.

[0055] In this embodiment, the powered sample stage 2 and the sample displacement stage 3 are respectively connected to the PLC controller 11 (Lenovo desktop computer) via data cables with USB 3.0 interfaces.

[0056] This embodiment also includes a spectral acquisition device for collecting the radiation spectrum of the sample, located inside the vacuum chamber 1. This spectral acquisition device includes a fiber optic spectrometer 4 (OceanOptics HQ4000 fiber optic spectrometer, with a spectral wavelength detection range of 200-1200nm) and a CCD camera 6 (SpectroCam™ CCD camera). The fiber optic spectrometer 4 and the CCD camera 6 are connected via a fiber optic cable 5. The fiber optic spectrometer 4 is connected to a PLC controller 11 (Lenovo desktop computer) via a data cable with a USB 3.0 interface. The CCD camera 6 is fixed directly above the heating element via a spectral shift stage 7. The distance between the CCD camera 6 and the heating element is adjusted by moving the spectral shift stage 7, with a distance range of 17cm to 22cm. The spectral shift stage 7 is a two-axis shift stage, with an X-axis movement range of 0-20cm and a displacement accuracy of 0.1mm; and a Y-axis movement range of 0-10cm and a displacement accuracy of 0.1mm.

[0057] In this embodiment, a 550nm filter is provided in front of the lens of the CCD camera 6 to improve the accuracy of platform temperature testing.

[0058] In this embodiment, a mechanical pump 8 (TRP-24 mechanical pump) and a vacuum gauge 9 (ZDF-5201 composite vacuum gauge) are also connected to the vacuum chamber 1. The pumping rate of the mechanical pump 8 is >15L / min; the vacuum gauge 9 has a measurement range of 100kPa to 1Pa and a measurement accuracy of 1Pa. The vacuum chamber 1 has dimensions of 0.8m × 0.8m × 1m, and a door 12 is provided at the top. The door 12 has an observation window 13 with a diameter of 25cm. The observation window 13 of the vacuum chamber 1 is made of transparent glass, and the rest of the chamber is made of stainless steel.

[0059] A method of using the ultra-high temperature field platform in Embodiment 1 of the present invention includes the following steps:

[0060] (1) Construction of the ultra-high temperature field platform:

[0061] (1.1) First connect the vacuum chamber and the mechanical pump (TRP-24 mechanical pump), and then install the probe of the vacuum gauge (ZDF-5201 composite vacuum gauge) into the vacuum chamber, where the dimensions of the vacuum chamber are 0.8m×0.8m×1m.

[0062] (1.2) Install the mechanical control system (powered sample stage and sample displacement stage) at the bottom of the vacuum chamber.

[0063] (1.3) Fix the heating element on the powered sample stage, and use a soldering gun to solder the wires to both ends of the heating element. Connect the wires to the source meter (Keithley 2450 source meter).

[0064] (1.4) Fix the spectral shift stage and the fiber optic spectrometer (OceanOptics HQ4000 fiber optic spectrometer with a spectral wavelength detection range of 200-1200nm) inside the vacuum chamber. Fix the CCD camera (SpectroCam™ CCD camera) on the spectral shift stage. Connect the CCD camera and the fiber optic spectrometer with fiber optic cables. At the same time, connect the fiber optic spectrometer to the PLC controller (Lenovo desktop computer) with a data cable with a USB 3.0 interface to form a spectral acquisition device.

[0065] (2) Formation of ultra-high temperature field:

[0066] Close the vacuum chamber door, turn on the mechanical pump, and pump air at a pumping rate of 25 L / min. When the vacuum level is below 5 Pa, turn on the power source and start heating the heating element to form an ultra-high temperature field.

[0067] (3) Testing of ultra-high temperature field:

[0068] (3.1) Use a CCD camera to locate the point where the temperature of the heating element or the sample to be tested needs to be measured, wherein the exposure time of the CCD camera is 3000ms.

[0069] (3.2) The radiation spectrum of the positioning point is collected using a fiber optic spectrometer to obtain the temperature field distribution on the surface of the heating element or the sample to be tested. The spectral acquisition time of the fiber optic spectrometer is 100ms.

[0070] During the test, the vacuum chamber was kept in a vacuum state.

[0071] In this invention, the temperature of the positioning point can be calculated and fitted according to Planck's radiation law, where the radiation intensity I on the material surface is... (λ,T) There is a certain relationship between it and temperature T:

[0072]

[0073] Where λ is the radiation wavelength, T is the absolute temperature, γ is the shape factor that interacts with the sample shape, and ε grey k is the surface emissivity of the thin film. B , c represents Boltzmann's constant, Planck's constant, and the speed of light, respectively. Furthermore, by rapidly acquiring spectral information from different locations on the surface of the heating element or the sample, the temperature field of the heating element or the sample can be quickly fitted. Therefore, by characterizing the radiation spectrum distribution of the material surface using spectrometers, the temperature field distribution of the material surface can be calculated.

[0074] Figure 5 This is a radiation spectrum intensity diagram of the ultra-high temperature field platform constructed in Embodiment 1 of the present invention under different current conditions. Figure 5 It can be seen that in the ultra-high temperature field platform constructed with the heating element of the present invention as the heat source, the intensity of the temperature field radiation spectrum continuously increases with the increase of the current.

[0075] Figure 6 This is a radiation spectrum intensity diagram of the ultra-high temperature field platform constructed in Embodiment 1 of the present invention, after being filtered by a 550nm filter under different current conditions. Figure 6 It is known that in the ultra-high temperature field platform constructed with the heating element of the present invention as the heat source, the radiation spectrum is filtered and converted into light of single intensity, which is crucial for improving the accuracy of the platform temperature test; the filter is installed in front of the lens of the spectrometer (CCD camera).

[0076] Figure 7 This is a temperature variation diagram of the ultra-high temperature field platform constructed in Embodiment 1 of the present invention under different current conditions. Figure 7 It can be seen that in the ultra-high temperature field platform constructed using the heating element of this invention as the heat source, the surface temperature of the heating element exhibits a distribution trend of being high in the middle and low at both ends, and the temperature increases with increasing current; simultaneously, the temperature range of the temperature field can be precisely controlled by controlling the magnitude of the current. Furthermore, from... Figure 7 It can be seen that the surface of the heating element composed of pre-reduced graphene oxide film forms an ultra-high temperature field due to the Joule heating effect.

[0077] Figure 8 This is a graph showing the heating and cooling rates of the ultra-high temperature field platform constructed in Embodiment 1 of the present invention. Figure 8 It can be seen that in the ultra-high temperature field platform constructed using the heating element of this invention as the heat source, the heating rate can reach 4×10⁻⁶. 5 ℃ / s, cooling rate can reach 10 5 It has an extremely fast temperature rise and fall rate of ℃ / s.

[0078] Example 2

[0079] A heating element for an ultra-high temperature field platform is basically the same as that in Example 1, except that in Example 2, the length of the pre-reduced graphene oxide film is 5 mm, the width is 0.5 mm, and the thickness is 25 μm.

[0080] A method for preparing a heating element for an ultra-high temperature field platform is basically the same as in Example 1, except that in Example 2, the distance between the scraper and the substrate is 3 mm. In this example, multiple scraping processes can be performed until the target thickness is achieved.

[0081] The heating element in Example 2 was used as the heat source to construct an ultra-high temperature field platform.

[0082] Example 3

[0083] A heating element for an ultra-high temperature field platform is basically the same as that in Example 1, except that in Example 3, the length of the pre-reduced graphene oxide film is 5 mm, the width is 0.5 mm, and the thickness is 100 μm.

[0084] A method for preparing a heating element for an ultra-high temperature field platform is basically the same as in Example 1, except that in Example 3, the distance between the scraper and the substrate is 4 mm. In this example, multiple scraping processes can be performed until the target thickness is achieved.

[0085] The heating element in Example 3 was used as the heat source to construct an ultra-high temperature field platform.

[0086] Example 4

[0087] A heating element for an ultra-high temperature field platform is basically the same as that in Example 1, except that in Example 4, the length of the pre-reduced graphene oxide film is 10 mm, the width is 1 mm, and the thickness is 10 μm.

[0088] The heating element in Example 4 was used as the heat source to construct an ultra-high temperature field platform.

[0089] Example 5

[0090] A heating element for an ultra-high temperature field platform is basically the same as that in Example 1, except that in Example 5, the length of the pre-reduced graphene oxide film is 10 mm, the width is 4 mm, and the thickness is 10 μm.

[0091] The heating element in Example 5 was used as the heat source to construct an ultra-high temperature field platform.

[0092] Example 6

[0093] A heating element for an ultra-high temperature field platform is basically the same as that in Example 1, except that in Example 6, the length of the pre-reduced graphene oxide film is 20 mm, the width is 2 mm, and the thickness is 10 μm.

[0094] The heating element in Example 6 was used as the heat source to construct an ultra-high temperature field platform.

[0095] Example 7

[0096] A heating element for an ultra-high temperature field platform is basically the same as that in Example 1, except that in Example 7, the length of the pre-reduced graphene oxide film is 50 mm, the width is 5 mm, and the thickness is 10 μm.

[0097] The heating element in Example 7 was used as the heat source to construct an ultra-high temperature field platform.

[0098] Example 8

[0099] A heating element for an ultra-high temperature field platform is basically the same as that in Example 1, except that in Example 8, the length of the pre-reduced graphene oxide film is 5 mm, the width is 0.1 mm, and the thickness is 10 μm.

[0100] The heating element in Example 8 was used as the heat source to construct an ultra-high temperature field platform.

[0101] Table 1. Characteristics of heating elements of different sizes and the constructed ultra-high temperature field platforms in Examples 1-8 of the present invention.

[0102]

[0103]

[0104] Comparative Example 1:

[0105] A heating element is basically the same as that in Example 1, except that the carrier material in Comparative Example 1 is a nickel-based high-temperature alloy.

[0106] An ultra-high temperature field platform was constructed using the heating element from Comparative Example 1 as the heat source. The results showed that at lower temperatures, the constructed temperature field was not significantly different from that in Example 1. However, at high temperatures, the high-temperature alloy generated electron and metal ion radiation, which significantly affected the measurement of the temperature field.

[0107] The above embodiments are merely preferred embodiments of the present invention, and the scope of protection of the present invention is not limited to the above embodiments. All technical solutions falling within the scope of the present invention's concept are within the scope of protection of the present invention. It should be noted that for those skilled in the art, improvements and modifications made without departing from the principles of the present invention should also be considered within the scope of protection of the present invention.

Claims

1. A heating element for an ultra-high temperature hot zone platform, characterized by, The heating body is a pre-reduced graphene oxide film; the pre-reduced graphene oxide film has an aspect ratio of 1-10:1 and a width of 0.3 mm-8 mm; the pre-reduced graphene oxide film has a thickness of 5 μm-25 μm; the pre-reduced graphene oxide film is prepared by the following steps: (1) coating a graphene oxide nanosheet aqueous solution on a substrate, drying at 30-40 ℃ for 8-36 h to obtain a graphene oxide film; (2) heating the graphene oxide film obtained in step (1) to 700-850 ℃ under an inert atmosphere for 10-60 min to obtain a pre-reduced graphene oxide film; the heating body further comprises a carrier material, and the pre-reduced graphene oxide film is fixed on the carrier material; the carrier material is a high-temperature-resistant ceramic material; the high-temperature-resistant ceramic material is an alumina ceramic material or a silicon carbide ceramic material.

2. A method for producing a heat generator for an ultra-high temperature hot field platform according to claim 1, characterized by, The method comprises the following steps: S1, coating a graphene oxide nanosheet aqueous solution on a substrate, drying to obtain a graphene oxide film; S2, heat-treating the graphene oxide film obtained in step S1 to obtain a pre-reduced graphene oxide film.

3. The production method according to claim 2, characterized by, The method further comprises the following steps: S3, bonding the pre-reduced graphene oxide film obtained in step S2 to a carrier material, and curing to obtain a heating body for an ultrahigh-temperature thermal field platform.

4. The production method according to claim 3, characterized by, In step S3, the pre-reduced graphene oxide film is bonded to the carrier material by using conductive silver paste; the curing is performed in an air atmosphere; the curing is performed by fixing the pre-reduced graphene oxide film to the carrier material at a temperature of 100-170 ℃; the curing time is 10-60 min.

5. The production method according to any one of claims 2 to 4, characterized by, In step S1, the coating is performed by placing the graphene oxide nanosheet aqueous solution on the substrate and scraping the graphene oxide nanosheet aqueous solution on the substrate by using a scraper; the scraping rate of the scraper is 8-15 mm / s; the distance between the scraper and the substrate is 1-4 mm; the scraper is a doctor blade; the substrate is a copper foil; the concentration of the graphene oxide nanosheet aqueous solution is 4-10 mg / mL; the flake diameter of the graphene oxide nanosheets in the graphene oxide nanosheet aqueous solution is 5-50 μm; the drying is performed by heating the substrate to 30-40 ℃; the drying time is 8-36 h.

6. The production method according to any one of claims 2 to 4, characterized by, In step S2, the heat treatment is performed in an inert atmosphere; the heat treatment temperature is 700-850 ℃; the heat treatment time is 10-60 min.

7. Use of the heating body of claim 1 or the heating body prepared by the method of any one of claims 2-6 as a heating source in constructing an ultrahigh-temperature thermal field platform.

Citation Information

Patent Citations

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