Quick-response thermistor material suitable for intelligent space expansion structure and preparation method of quick-response thermistor material

By preparing Y1/3Tb1/3Pr1/3NbO4 medium entropy thermistor material, the stability and accuracy of existing thermistors in high temperature environments are solved, and a wide range of temperature monitoring and rapid response is achieved, which is suitable for temperature sensing in intelligent space expansion structures.

CN120441316APending Publication Date: 2025-08-08XINJIANG TECH INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202510579936.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-07
Publication Date
2025-08-08

AI Technical Summary

Technical Problem

Existing thermistor materials are prone to damage in high temperature, high voltage, and high wear scenarios, and the resistance-temperature characteristics are not stable enough, and the temperature coefficient accuracy and consistency are poor, making it difficult to meet the temperature monitoring needs of intelligent space expansion structures.

Method used

The Y1/3Tb1/3Pr1/3NbO4 medium entropy thermistor material was prepared by high entropy strategy. Through mixed grinding, calcining, cold isostatic molding and high temperature sintering, ceramic materials with a wide range of temperature monitoring intervals, high linearity, fast response and high reliability were obtained.

Benefits of technology

It realizes high-precision temperature monitoring in the range of 150-1050℃, and the material has a low drift rate at high temperatures, ensuring the stability and functionality of the intelligent space expansion structure, and is suitable for complex and extreme environments.

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Abstract

The invention discloses a fast-response thermistor material suitable for an intelligent space expansion structure and a preparation method thereof. The method comprises the following steps: by taking yttrium oxide, tetraterbium heptaoxide, niobium pentoxide and praseodymium oxide as raw materials, mixing, grinding, calcining, regrinding, performing cold isostatic pressing, sintering at a high temperature and the like, thereby obtaining the fast-response thermistor material suitable for the intelligent space expansion structure. The niobate thermistor material is obtained. The thermistor has the advantages of being high in high-temperature stability, high in linearity, low in heat conductivity and the like, and the prepared niobate ceramic wafer-shaped high-density ceramic material is good in density, has the excellent negative temperature coefficient characteristic, and is fast in response and high in reliability; the temperature sensing material is suitable for high-precision and stable temperature monitoring in the work of an intelligent space expansion structure.
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Description

Technical Field

[0001] The invention relates to a fast-response thermistor material suitable for an intelligent space deployment structure and a preparation method thereof. Technical Background

[0002] Smart deployable space structures refer to physical structures that can dynamically adjust or deploy using intelligent technology. They are widely used in spacecraft (such as satellite antennas and solar panels), smart buildings (such as retractable roofs), and agricultural greenhouses (such as smart glass greenhouses). Their core goal is to optimize space utilization efficiency, energy management, and safety through environmental sensing and adaptive control. Smart deployable space structures have broad application prospects in hinges, rigid solar arrays, flexible solar wings, antennas, and sunshades, and are expected to be used in major aerospace projects such as my country's space station and lunar exploration programs. Spacecraft must cope with complex environments such as vacuum, extreme temperatures, and radiation, and smart deployable space structures must similarly withstand these conditions. Temperature control points in smart deployable space structures are typically located at heat-sensitive components, dynamic interfaces, or areas exposed to extreme environments. Their core goal is to ensure structural functionality, material stability, and mission reliability. Dynamic interfaces are monitored at temperatures between 100 and 300°C, while areas exposed to thermal environments are monitored at temperatures between 100 and 1000°C and above. Material interfaces and composite material areas can reach temperatures as high as 400 to 800°C. The temperature control points of the intelligent space deployment structure are the "nerve endings" of its thermal management system. Through precise layout and advanced sensing technology, they ensure the reliability and functionality of the structure in extreme temperature environments.

[0003] Thermistors, whose resistance changes with temperature and their rapid response, have become crucial components for temperature monitoring and control in intelligent space deployment structures. Currently, most temperature monitoring components are made of fiber optic materials, which offer resistance to electromagnetic interference, flame retardancy, and explosion resistance, as well as suitability for long-distance monitoring. However, fiber optic materials have a narrow temperature range and can be damaged or degraded in high-temperature environments. They are also more susceptible to breakage in high-mechanical load environments. Ceramic thermistors, on the other hand, offer adaptability to a variety of extreme environments and versatile integration capabilities, particularly excelling in high-temperature, high-pressure, and high-wear scenarios.

[0004] The present invention adopts a high entropy strategy to design the configuration of YNbO4 to form a medium entropy thermistor ceramic with a wide temperature range and high linearity. First, the high entropy effect can effectively adjust the YNbO4 material to obtain a wide temperature monitoring range of 150-1050℃ and a linear fit of 99.9%. This not only solves the problem of thermistor's resistance-temperature characteristics being unstable and the accuracy and consistency of the temperature coefficient being poor, but also ensures the realization of the intelligent space deployment structure to monitor the different temperature ranges of the temperature control points at various parts during environmental operation. Secondly, the thermal conductivity of the YNbO4 material adjusted by the high entropy effect is between 1.742-2.412W·m- 1 K -1 , which enables the thermistor prepared from this material to exhibit its fast response characteristics; it has the characteristics of high sensitivity and fast response, and can monitor temperature changes in real time in order to respond as quickly as possible. Finally, the drift rate of the material is stabilized below 10% after 500 hours of aging treatment at 1000°C, indicating that it has high reliability at high temperatures and can ensure that the material maintains good stability during the monitoring process. Its adaptability to various extreme environments and multifunctional integration capabilities enable it to perform outstandingly in high temperature, high pressure, and high wear scenarios. Summary of the Invention

[0005] The purpose of the present invention is to solve the problems of accuracy, durability and stability of temperature monitoring of intelligent space deployment structure, and to provide a fast response thermistor material and preparation method suitable for intelligent space deployment structure. The material is made of yttrium trioxide, terbium heptoxide, niobium pentoxide or hexapronemium undecoxide, and is obtained by mixing, grinding, calcining, re-grinding, cold isostatic pressing and high temperature sintering. 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 medium entropy thermistor material. The single-phase thermistor of the present invention has the advantages of strong high temperature stability, high linearity, low thermal conductivity and low aging drift rate. 1 / 3Tb 1 / 3 Pr 1 / 3 NbO4's disc-shaped high-density ceramic material has good density and excellent negative temperature coefficient characteristics, making it suitable as a temperature sensing element for temperature monitoring in intelligent space deployment structure equipment.

[0006] The invention discloses a fast-response thermistor material suitable for intelligent space deployment structure, which uses entropy strategy to semiconduct YNbO4, and uses yttrium trioxide, terbium heptoxide, niobium pentoxide or hexaprone undecoxide as raw materials to prepare YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 thermistor ceramics, the specific operation is carried out according to the following steps:

[0007] a. According to the molecular formula YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3The molar ratio of YNbO4 was calculated by weighing the raw materials yttrium trioxide, terbium heptoxide, niobium pentoxide or praseodymium undecoxide, mixing and grinding for 6-8 hours, then calcining at 1400℃ for 6-8 hours, and grinding again for 6 hours to obtain dispersed YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 powder;

[0008] b. The powder obtained in step a was molded into a mold with a diameter of 10 mm, and a pressure of 20 MPa was applied. After holding the pressure for 15 seconds, YNbO4 and Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 ceramic green body material;

[0009] c. Vacuum-pack the ceramic green body obtained in step b and cold isostatically press it at 200-300 MPa for 1-3 min. Then, place it in a muffle furnace at 1500-1700°C for 8 h. After cooling to room temperature, a disc-shaped high-density YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 medium entropy ceramic material;

[0010] d. The disc-shaped high-density ceramic obtained in step c was polished on both sides with 1500-mesh fine sandpaper for 1 minute, then ultrasonically cleaned with anhydrous ethanol for 30 minutes, coated with platinum paste electrodes on both sides, and then annealed at 900°C for 1 hour to obtain a temperature range of 150-1050°C and a material constant of B. 150℃ / 1050℃ =5530K-13722K suitable for temperature monitoring of intelligent space deployment structure YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 thermistor material.

[0011] A method for preparing a fast-response thermistor material suitable for an intelligent space deployment structure is carried out in the following steps:

[0012] a. According to the molecular formula YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3The molar ratio of YNbO4 was calculated by weighing the raw materials yttrium trioxide, terbium heptoxide, niobium pentoxide or praseodymium undecoxide, mixing and grinding for 6-8 hours, then calcining at 1400℃ for 6-8 hours, and grinding again for 6 hours to obtain dispersed YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 powder;

[0013] b. The powder obtained in step a was molded into a mold with a diameter of 10 mm, and a pressure of 20 MPa was applied. After holding the pressure for 15 seconds, YNbO4 and Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 ceramic green body material;

[0014] c. Vacuum-pack the ceramic green body obtained in step b and cold isostatically press it at 200-300 MPa for 1-3 min. Then, place it in a muffle furnace at 1500-1700°C for 8 h. After cooling to room temperature, a disc-shaped high-density YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 ceramic materials;

[0015] d. The disc-shaped high-density ceramic obtained in step c was polished on both sides with 1500-mesh fine sandpaper for 1 minute, then ultrasonically cleaned with anhydrous ethanol for 30 minutes, coated with platinum paste electrodes on both sides, and then annealed at 900°C for 1 hour to obtain a temperature range of 150-1050°C and a material constant of B. 150℃ / 1050℃ =5530K-13722K suitable for temperature monitoring of intelligent space deployment structure YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 thermistor material.

[0016] YNbO4, Y 1 / 2 Tb 1 / 2 NbO4、Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 medium entropy thermistor material, where Y 1 / 3 Tb 1 / 3 Pr 1 / 3NbO4 has relatively good high-temperature stability and good NTC performance, and can achieve high-precision and stable measurements in extreme environments. It can be used as a temperature sensing element for temperature monitoring in smart space deployment structures.

[0017] Compared with the prior art: the present invention prepares Y 1 / 3 Tb 1 / 3 Pr 1 / 3 The process of NbO4 medium entropy thermistor material is unique:

[0018] First, the Y obtained by the present invention 1 / 3 Tb 1 / 3 Pr 1 / 3 The NbO4 medium-entropy thermistor material enables high-density, high-temperature NTC thermistors that can be used in a wide temperature range of 150-1050°C for long periods of time. This addresses the issues of thermistors' unstable resistance-temperature characteristics and poor accuracy and consistency of their temperature coefficients, while also ensuring the ability to monitor different temperature ranges at various temperature control points in intelligent space deployment structures during environmental operations.

[0019] Secondly, the Y obtained by the present invention 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 medium entropy thermistor material has the characteristics of fast response and can monitor temperature changes in real time to react as quickly as possible;

[0020] Finally, the Y obtained by the present invention 1 / 3 Tb 1 / 3 Pr 1 / 3 After aging treatment, the drift rate of the NbO4 medium-entropy thermistor material is stabilized below 10%, indicating that it has high reliability and can ensure that the material maintains good stability during the monitoring process.

[0021] The method of the present invention solves the current accuracy, rapidity and stability problems of temperature monitoring of structures deployed in intelligent spaces, and provides technical support for the stable application of medium and high temperature thermistors in complex and special environments; the obtained Y 1 / 3 Tb 1 / 3 Pr 1 / 3 The NbO4 medium entropy thermistor material has a good linear relationship between Ln(ρ) and 1000 / T at temperatures of 150-1050℃, and the Pearson coefficient can reach 0.999; the thermal conductivity is 1.742-2.412W·m -1 K -1 . BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 Y prepared by the present invention 1 / 3 Tb 1 / 3 Pr1 / 3 XRD spectrum of entropy thermosensitive material in NbO4;

[0023] Figure 2 Y prepared by the present invention 1 / 3 Tb 1 / 3 Pr 1 / 3 Resistance-temperature characteristic curve of NbO4 thermosensitive material;

[0024] Figure 3 Y prepared by the present invention 1 / 3 Tb 1 / 3 Pr 1 / 3 Thermal conductivity change curve of NbO4 thermosensitive material. DETAILED DESCRIPTION

[0025] Example 1

[0026] a. According to molecular formula Y 1 / 3 Tb 1 / 3 Pr 1 / 3 The molar ratio of yttrium trioxide (4.68 g), terbium heptoxide (7.75 g), niobium pentoxide (5.51 g) and praseodymium undecoxide (7.05 g) were weighed and ground for 6 h, then calcined at 1400 ° C for 8 h and ground again for 6 h to obtain dispersed Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 powder 25g;

[0027] b. The powder obtained in step a was molded into a mold with a diameter of 10 mm, and a pressure of 20 MPa was applied. After holding the pressure for 15 seconds, Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 ceramic green body material;

[0028] c. The ceramic green body material obtained in step b was vacuum packaged and cold isostatically pressed at a pressure of 300 MPa for 3 minutes, then kept at a temperature of 1700° C. for 8 hours, and cooled to room temperature to obtain a disc-shaped Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 ceramic bulk material;

[0029] d. The disc-shaped high-density ceramic obtained in step c was polished on both sides with 1500-mesh fine sandpaper for 1 minute, then ultrasonically cleaned with anhydrous ethanol for 30 minutes, coated with platinum paste electrodes on both sides, and then annealed at 900°C for 1 hour to obtain a temperature range of 150-1050°C and a material constant of B. 150℃ / 1050℃ =5530K suitable for temperature monitoring of intelligent space deployment structure 1 / 3 Tb 1 / 3 Pr1 / 3 NbO4 medium entropy thermistor material.

[0030] Example 2

[0031] a. According to molecular formula Y 1 / 2 Tb 1 / 2 The molar ratio of NbO4 was calculated by weighing 4.99g of yttrium trioxide, 8.261g of terbium heptoxide, and 11.7481g of niobium pentoxide. The raw materials were mixed and ground for 6h, then calcined at 1350℃ for 8h and ground again for 6h to obtain dispersed Y 1 / 2 Tb 1 / 2 NbO4 powder 25g;

[0032] b. The powder obtained in step a was molded into a mold with a diameter of 10 mm, and a pressure of 20 MPa was applied. After holding the pressure for 15 seconds, Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 ceramic green body material;

[0033] c. The ceramic green body material obtained in step b was vacuum packaged and cold isostatically pressed at a pressure of 300 MPa for 3 minutes, then kept at a temperature of 1700° C. for 8 hours, and cooled to room temperature to obtain a disc-shaped Y 1 / 2 Tb 1 / 2 NbO4 ceramic bulk material;

[0034] d. The disc-shaped high-density ceramic obtained in step c was polished on both sides with 1500-mesh fine sandpaper for 1 minute, then ultrasonically cleaned with anhydrous ethanol for 30 minutes, coated with platinum paste electrodes on both sides, and then annealed at 900°C for 1 hour to obtain a temperature range of 150-1050°C and a material constant of B. 150℃ / 1050℃ =6989K suitable for temperature monitoring of intelligent space deployment structure 1 / 2 Tb 1 / 2 NbO4 low entropy thermistor material.

[0035] Example 3

[0036] a. According to the molar ratio of the molecular formula YNbO4, 22.9659 g of yttrium trioxide and 27.034 g of niobium pentoxide were weighed and mixed and ground for 6 hours. The mixture was then calcined at 1300°C for 8 hours and ground again for 6 hours to obtain 50 g of dispersed YNbO4 powder.

[0037] b. The powder obtained in step a was molded into a mold with a diameter of 10 mm, a pressure of 20 MPa was applied, and the pressure was maintained for 15 seconds to obtain a YO4 ceramic green body material;

[0038] c. vacuum-packaging the ceramic green body material obtained in step b, cold isostatically pressing the green body material at 300 MPa for 3 min, then keeping the temperature at 1450° C. for 8 h, and cooling the green body material to room temperature to obtain a YNbO4 ceramic block material in the form of a disc;

[0039] d. The disc-shaped high-density ceramic obtained in step c was polished on both sides with 1500-grit fine sandpaper for 1 minute, then ultrasonically cleaned with anhydrous ethanol for 30 minutes, coated with platinum paste electrodes on both sides, and then annealed at 900°C for 1 hour to obtain a temperature range of 450-1050°C and a material constant of B. 450℃ / 1050℃ =13722K YNbO4 thermistor material suitable for temperature monitoring of intelligent space deployment structures.

[0040] The above is only a specific embodiment of the present invention, but the design concept of the present invention is not limited thereto.

Claims

1. A fast-response thermistor material suitable for intelligent space deployment structures, characterized by: YNbO4 is semiconducted by using entropy strategy, and YNbO4, ... 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 thermistor ceramics, the specific operation is carried out according to the following steps: a. According to the molecular formula YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 The molar ratio of YNbO4 was calculated by weighing the raw materials yttrium trioxide, terbium heptoxide, niobium pentoxide or praseodymium undecoxide, mixing and grinding for 6-8 hours, then calcining at 1400℃ for 6-8 hours, and grinding again for 6 hours to obtain dispersed YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 powder; b. The powder obtained in step a was molded into a mold with a diameter of 10 mm, and a pressure of 20 MPa was applied. After holding the pressure for 15 seconds, YNbO4 and Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 ceramic green body material; c. Vacuum-pack the ceramic green body obtained in step b and cold isostatically press it at 200-300 MPa for 1-3 min. Then, place it in a muffle furnace at 1500-1700°C for 8 h. After cooling to room temperature, a disc-shaped high-density YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 ceramic materials; d. The disc-shaped high-density ceramic obtained in step c was polished on both sides with 1500-mesh fine sandpaper for 1 minute, then ultrasonically cleaned with anhydrous ethanol for 30 minutes, coated with platinum paste electrodes on both sides, and then annealed at 900°C for 1 hour to obtain a temperature range of 150-1050°C and a material constant of B. 150℃ / 1050℃ = 5530K-13722K suitable for temperature monitoring of intelligent space deployment structure YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 thermistor material.

2. A method for preparing a fast-response thermistor material suitable for an intelligent space deployment structure, characterized by: Follow these steps: a. According to the molecular formula YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 The molar ratio of YNbO4 was calculated by weighing the raw materials yttrium trioxide, terbium heptoxide, niobium pentoxide or praseodymium undecoxide, mixing and grinding for 6-8 hours, then calcining at 1400℃ for 6-8 hours, and grinding again for 6 hours to obtain dispersed YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 powder; b. The powder obtained in step a was molded into a mold with a diameter of 10 mm, and a pressure of 20 MPa was applied. After holding the pressure for 15 seconds, YNbO4 and Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 ceramic green body material; c. Vacuum-pack the ceramic green body obtained in step b and cold isostatically press it at 200-300 MPa for 1-3 min. Then, place it in a muffle furnace at 1500-1700°C for 8 h. After cooling to room temperature, a disc-shaped high-density YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 medium entropy ceramic material; d. The disc-shaped high-density ceramic obtained in step c was polished on both sides with 1500-mesh fine sandpaper for 1 minute, then ultrasonically cleaned with anhydrous ethanol for 30 minutes, coated with platinum paste electrodes on both sides, and then annealed at 900°C for 1 hour to obtain a temperature range of 150-1050°C and a material constant of B. 150℃ / 1050℃ = 5530K-13722K suitable for temperature monitoring of intelligent space deployment structure YNbO4, Y 1 / 2 Tb 1 / 2 NbO4 or Y 1 / 3 Tb 1 / 3 Pr 1 / 3 NbO4 thermistor material.