An ultra-high temperature radiation resistant adhesive

CN122608355APending Publication Date: 2026-08-21HENAN ANJU NEW MATERIAL TECH CO LTD +1
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Patent Information

Application Number
CN202610744644.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-05-27
Publication Date
2026-08-21

AI Technical Summary

Technical Problem

[0003]现有核电用粘接剂存在以下技术缺陷:1、高温稳定性不足:传统粘接剂在800℃以上高温环境下易发生热分解、氧化失效,导致粘结强度急剧下降甚至完全丧失,无法适应核电设备运行过程中可能出现的1200℃超高温极端工况;2、耐辐照性能差:核电环境中存在长期强辐照,常规粘接剂经辐照后会出现分子链断裂、结构破坏,导致力学性能和粘接性能显著衰减,难以满足60年长期服役要求

Benefits of technology

本发明耐辐照组分采用28KHz低频超声、低速缓慢加料,适配氧化钇+钛酸锆粉体吸附包覆;耐高温组分采用40KHz高频超声、快速加料,适配氧化铈+锆英砂分散固定,两种功能(耐辐照+耐高温)填料在专属工艺下均匀锚定在介孔二氧化硅孔道内,有效避免互相干扰而影响各自功能的体现。

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Abstract

This invention belongs to the field of adhesive technology. This invention provides an ultra-high temperature radiation-resistant adhesive, comprising: 48-53 parts quartz powder, 67-72 parts aluminate cement, 0.7-0.9 parts radiation-resistant component, 1-1.3 parts high-temperature resistant component, 3-3.5 parts alumina, 4-4.5 parts aluminum dihydrogen phosphate, 0.2-0.4 parts phthalate, 0.4-0.6 parts silane coupling agent, and 0.3-0.5 parts dispersant; the radiation-resistant component is composed of mesoporous silica nanoparticles supporting the radiation-resistant agent and inorganic binder; the radiation-resistant agent and inorganic... The total mass of the binder is 23-28% of the mass of the mesoporous silica nanoparticles, and the mass ratio of the radiation-resistant agent to the inorganic binder is 1:(1.3-1.7). The radiation-resistant agent consists of yttrium oxide and zirconium titanate in a mass ratio of (0.4-0.6):1. The high-temperature resistant component consists of mesoporous silica nanoparticles loaded with a high-temperature stabilizer, the mass of which is 10-13% of the mass of the mesoporous silica nanoparticles. The high-temperature stabilizer consists of cerium oxide and zircon sand in a mass ratio of (0.5-0.7):1. The binder prepared by this invention has both excellent high-temperature resistance and radiation resistance.
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Description

Technical Field

[0001] This invention belongs to the field of adhesive technology, and in particular relates to an ultra-high temperature radiation resistant adhesive. Background Technology

[0002] As a clean and efficient energy source, nuclear power's safe and stable operation relies on the extreme environmental adaptability of various key materials. Adhesives are indispensable key materials in the installation, maintenance, and component assembly of nuclear power equipment, and must simultaneously meet stringent requirements such as ultra-high temperatures, strong radiation, and low levels of harmful components.

[0003] Existing adhesives for nuclear power have the following technical defects: 1. Insufficient high-temperature stability: Traditional adhesives are prone to thermal decomposition and oxidation failure in high-temperature environments above 800℃, resulting in a sharp decrease or even complete loss of bonding strength, which cannot adapt to the extreme high-temperature conditions of 1200℃ that may occur during the operation of nuclear power equipment; 2. Poor radiation resistance: There is long-term strong radiation in the nuclear power environment. After irradiation, conventional adhesives will experience molecular chain breakage and structural damage, resulting in a significant decrease in mechanical and bonding properties, making it difficult to meet the requirements of 60-year long-term service. Summary of the Invention

[0004] To address the above problems, this invention proposes an ultra-high temperature radiation-resistant adhesive that combines excellent high temperature resistance and radiation resistance.

[0005] To achieve the above objectives, the technical solution adopted by the present invention is as follows: an ultra-high temperature radiation-resistant adhesive, comprising the following components by weight: 48-53 parts quartz powder, 67-72 parts aluminate cement, 0.7-0.9 parts radiation-resistant component, 1-1.3 parts high temperature-resistant component, 3-3.5 parts alumina, 4-4.5 parts aluminum dihydrogen phosphate, 0.2-0.4 parts phthalate, 0.4-0.6 parts silane coupling agent, and 0.3-0.5 parts dispersant; The radiation-resistant component consists of mesoporous silica nanoparticles loaded with a radiation-resistant agent and an inorganic binder; the total mass of the radiation-resistant agent and the inorganic binder is 23-28% of the mass of the mesoporous silica nanoparticles, and the mass ratio of the radiation-resistant agent to the inorganic binder is 1:(1.3-1.7); the radiation-resistant agent is composed of yttrium oxide and zirconium titanate in a mass ratio of (0.4-0.6):1. The high-temperature resistant component consists of mesoporous silica nanoparticles loaded with a high-temperature stabilizer, the mass of which is 10-13% of the mass of the mesoporous silica nanoparticles; the high-temperature stabilizer is composed of cerium oxide and zircon sand in a mass ratio of (0.5-0.7):1.

[0006] Furthermore, the method for preparing the radiation-resistant component is as follows: A1. Mix the radiation-resistant agent, inorganic binder, and ethanol-water solution to obtain a mixture; A2. Under ultrasonic and stirring conditions, mesoporous silica nanoparticles are added to the mixture obtained in A1, filtered, and dried to obtain the radiation-resistant component.

[0007] Further, the specific operation of A1 is as follows: first, mix 50-60 wt% of the radiation resistant agent with the inorganic binder for 20-25 min to obtain a premix; then add the remaining radiation resistant agent to the premix, continue mixing for 15-20 min, and then mix with the ethanol aqueous solution for 20-30 min.

[0008] Furthermore, in A2, the ultrasonic frequency is 25-30KHz, the stirring speed is 4000-9000rpm, and the addition speed is 0.3-0.8g / s.

[0009] Furthermore, the inorganic binder is aluminum phosphate.

[0010] Furthermore, the preparation method of the high-temperature resistant component is as follows: B1. Disperse the high-temperature stabilizer in an aqueous ethanol solution to obtain a dispersion; B2. Under ultrasonic and stirring conditions, mesoporous silica nanoparticles are added to the dispersion obtained in B1, filtered, and dried to obtain the high-temperature resistant component.

[0011] Furthermore, in B2, the ultrasonic frequency is 38-45KHz, the stirring speed is 5000rpm-8000rpm, and the addition speed is 2.5-3.5g / s.

[0012] Furthermore, the volume ratio of ethanol to water in the ethanol-water solution is 1:(5-8).

[0013] Furthermore, the silica content of the quartz powder is ≥98%, sulfur-free, and the particle size is 5-50μm; the Al2O3 content of the aluminate cement is ≥70%, sulfur-free; the phthalate is dibutyl phthalate, sulfur-free; the silane coupling agent is KH-550; and the dispersant is BG1900 polycarboxylate dispersant, purchased from Nanjing Baiju Technology Co., Ltd.

[0014] Furthermore, the preparation method of the ultra-high temperature radiation-resistant adhesive is as follows: S1. By weight, mix quartz powder and aluminate cement and stir at 2000-2500 rpm for 15-20 minutes to obtain the basic mixture; S2. Add alumina, aluminum dihydrogen phosphate, dispersant, phthalate and silane coupling agent to the basic mixture obtained in S1, heat to 40-50℃, and stir at 3000-3500 rpm for 25-30 min to obtain the secondary mixture. S3. Add the radiation-resistant component and the high-temperature resistant component to the secondary mixture obtained in S2, cool to room temperature, and disperse for 30-40 minutes under stirring at 5000-5500 rpm and ultrasonic assistance at 20-25 kHz to obtain the ultra-high temperature radiation-resistant adhesive.

[0015] The roles of each raw material component mentioned above are as follows: The quartz powder selected is high-purity quartz powder with a silica content ≥98% and free of sulfur. It possesses excellent high-temperature resistance, chemical stability, and high hardness, which not only enhances the structural strength and wear resistance of the adhesive but also strengthens the material's thermal shock resistance under ultra-high temperature environments, making it suitable for the extreme high-temperature conditions of nuclear power plants. Aluminate cement, as the core cementing component, is selected from products with an Al2O3 content ≥70% and free of sulfur, providing the adhesive with basic bonding strength and high-temperature resistance. Its inorganic properties ensure that it does not undergo organic decomposition failure under high temperature and irradiation environments. The radiation-resistant agent is preferably a compound system of yttrium oxide and zirconium titanate. The synergistic effect of these two components significantly improves the material's radiation resistance and suppresses radiation-induced structural defects. The inorganic binder is aluminum phosphate, which forms a dual bonding system with aluminate cement, enhancing bonding stability at high temperatures. The optimized ratio of the radiation-resistant agent and the inorganic binder enables long-term sustained release of functional components, ensuring stable performance during long-term service. The preferred high-temperature stabilizer is a blend of cerium oxide and zircon sand, which inhibits the phase transformation and volume shrinkage of the adhesive at high temperatures, ensuring no loss of bond strength at 1200℃. The optimal loading level balances the high-temperature stabilization effect with the carrier loading efficiency. The dispersant is a polycarboxylate-based dispersant, sulfur-free, which improves the dispersion uniformity of each component, avoids agglomeration, and enhances the overall performance consistency of the adhesive. The phthalate used is dibutyl phthalate, which is sulfur-free and acts as a dispersing aid, improving the adhesive's workability and enhancing interfacial compatibility between components, while reducing internal stress. The selected silane coupling agent is KH-550, which is sulfur-free. It can improve the interfacial compatibility between silica fume, aluminate cement, inorganic radiation-resistant and high-temperature-resistant functional powders, and mesoporous silica through bonding, break up powder agglomeration, and optimize the rheological properties of the slurry. It also acts as an intermediate transition, allowing organic additives such as phthalates and dispersants to be uniformly dispersed in the inorganic adhesive matrix, avoiding precipitation and segregation. It is beneficial to build a stable inorganic interfacial cross-linked structure after curing, thereby improving the initial bond strength and structural density of the adhesive system.

[0016] Compared with the prior art, the present invention has the following beneficial effects: The radiation-resistant component of this invention is fed slowly using 28kHz low-frequency ultrasound, which is suitable for adsorption and coating with yttrium oxide and zirconium titanate powder; the high-temperature resistant component is fed rapidly using 40kHz high-frequency ultrasound, which is suitable for dispersion and fixation with cerium oxide and zircon sand. The two functional (radiation-resistant + high-temperature resistant) fillers are uniformly anchored in the mesoporous silica channels under a special process, effectively avoiding mutual interference and affecting the performance of their respective functions.

[0017] After being independently loaded, two types of stable functional units are formed: radiation-resistant units (radiation-resistant components) are dedicated to blocking gamma rays and inhibiting radiation fracture; high-temperature resistant units (high-temperature resistant components) are dedicated to resisting high-temperature (1200℃) thermal shock. The two types of units are distributed in an alternating manner in the adhesive matrix to construct a two-way three-dimensional skeleton of radiation protection + high-temperature stability network, achieving a synergistic improvement effect of 1+1>2, and synergistically improving the high-temperature resistance and radiation resistance of the prepared adhesive test sample. Attached Figure Description

[0018] Figure 1 This is a comparative trend chart of the test data of the high temperature resistance and radiation resistance of the adhesive test samples prepared in Examples 1-3 and Comparative Examples 1-5 of the present invention. Figure 2 This is a comparative trend chart of the radiation-high temperature resistance test data of the adhesive test samples prepared in Examples 1-3 and Comparative Examples 1-5 of the present invention. Detailed Implementation

[0019] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0020] Unless otherwise specified, the raw materials used in the embodiments and comparative examples of this invention are all commercially available.

[0021] Example 1: (a) The preparation method of the radiation-resistant component is as follows: A1. Mix the radiation resistant agent, the inorganic binder aluminum phosphate, and an aqueous ethanol solution to obtain a mixture; The radiation-resistant agent is composed of yttrium oxide (99.9% purity) and zirconium titanate (99.8% purity) in a mass ratio of 0.5:1. The mass ratio of the radiation-resistant agent to the inorganic binder (aluminum phosphate, sulfur-free) is 1:1.5. The volume ratio of ethanol to water in the ethanol-water solution is 1:6, and the mass of the ethanol-water solution is 4.5 times the total mass of the radiation-resistant agent and the inorganic binder.

[0022] The specific operation is as follows: First, mix 55wt% of the radiation resistant agent and the inorganic binder at a stirring speed of 500rpm for 22min to obtain a premix; then add the remaining radiation resistant agent to the premix, keep the stirring speed constant, continue stirring and mixing for 18min, and then mix with the ethanol aqueous solution for 25min to obtain a mixture.

[0023] A2. Add mesoporous silica nanoparticles to a mixture under ultrasonic frequency of 28KHz and stirring speed of 6000rpm at an addition rate of 0.5g / s. The total mass of the radiation resistant agent and inorganic binder is 25% of the mass of the mesoporous silica nanoparticles. After addition, filter and dry to obtain the radiation resistant component.

[0024] (II) The preparation method of the high-temperature resistant component is as follows: B1. Disperse the high-temperature stabilizer in an aqueous ethanol solution to obtain a dispersion; The high-temperature stabilizer consists of cerium oxide (99.9% purity) and zircon sand (ZrSiO4 content 98%) in a mass ratio of 0.6:1. The volume ratio of ethanol to water in the ethanol aqueous solution is 1:6, and the mass of the ethanol aqueous solution is 4.5 times the mass of the high-temperature stabilizer.

[0025] The specific operation is as follows: mix the high temperature stabilizer with an ethanol aqueous solution and stir at 500 rpm for 25 minutes to obtain a dispersion.

[0026] B2. Add mesoporous silica nanoparticles to a dispersion with an ultrasonic frequency of 40 kHz and a stirring speed of 6000 rpm at an addition rate of 3.0 g / s. The mass of the high-temperature stabilizer is 12% of the mass of the mesoporous silica nanoparticles. Filter and dry to obtain the high-temperature resistant component.

[0027] (III) A method for preparing an ultra-high temperature radiation-resistant adhesive is as follows: S1. Mix 50 parts of quartz powder and 70 parts of aluminate cement, and stir at 2200 rpm for 17 minutes to obtain the basic mixture.

[0028] S2. Add 3.2 parts of alumina, 4.2 parts of aluminum dihydrogen phosphate, 0.3 parts of phthalate, 0.5 parts of silane coupling agent and 0.4 parts of dispersant to the basic mixture obtained in S1, heat to 45°C, and stir at 3200 rpm for 28 minutes to obtain the secondary mixture.

[0029] S3. Add 0.8 parts of the radiation-resistant component and 1.2 parts of the high-temperature resistant component to the secondary mixture obtained in S2, cool to room temperature, and disperse for 35 minutes under stirring at 5200 rpm and ultrasonic assistance at 23 kHz to obtain the ultra-high temperature radiation-resistant adhesive.

[0030] The phthalate is dibutyl phthalate, which is sulfur-free. The silane coupling agent is KH-550. The dispersant is BG1900 polycarboxylate dispersant, purchased from Nanjing Baiju Technology Co., Ltd.

[0031] The above preparation method selects sulfur-free and low-halogen raw materials and strictly controls the impurity content of each component, ensuring that the binder is sulfur-free and has a total halogen content of less than 1000 ppm. This avoids the release of corrosive gases under high temperatures or irradiation, ensuring the safe operation of nuclear power equipment. The resulting binder is an inorganic, water-soluble formulation, free of harmful and toxic substances, with volatile organic compound (VOC) content approaching zero, exhibiting high environmental safety. The mixing of each component and the loading of functional components all utilize conventional equipment, making process parameters easy to control. The product exhibits good performance stability, minimal batch-to-batch variation, and the overall preparation process is simple, suitable for industrial production.

[0032] Example 2: The difference between this example and Example 1 is that a method for preparing an ultra-high temperature radiation-resistant adhesive is as follows: S1. Mix 48 parts of quartz powder and 67 parts of aluminate cement, and stir at 2000 rpm for 20 minutes to obtain the basic mixture.

[0033] S2. Add 3 parts alumina, 4 parts aluminum dihydrogen phosphate, 0.2 parts phthalate, 0.4 parts silane coupling agent and 0.3 parts dispersant to the basic mixture obtained in S1, heat to 40℃, and stir at 3000 rpm for 30 min to obtain the secondary mixture.

[0034] S3. Add 0.7 parts of the radiation-resistant component and 1 part of the high-temperature resistant component to the secondary mixture obtained in S2, cool to room temperature, and disperse for 40 minutes under stirring at 5000 rpm and ultrasonic assistance at 20 kHz to obtain the ultra-high temperature radiation-resistant adhesive.

[0035] Example 3: The difference between this example and Example 1 is that a method for preparing an ultra-high temperature radiation-resistant adhesive is as follows: S1. Mix 53 parts of quartz powder and 72 parts of aluminate cement, and stir at 2500 rpm for 15 minutes to obtain the basic mixture.

[0036] S2. Add 3.5 parts of alumina, 4.5 parts of aluminum dihydrogen phosphate, 0.4 parts of phthalate, 0.6 parts of silane coupling agent and 0.5 parts of dispersant to the basic mixture obtained in S1, heat to 50°C, and stir at 3500 rpm for 25 minutes to obtain the secondary mixture.

[0037] S3. Add 0.9 parts of the radiation-resistant component and 1.3 parts of the high-temperature resistant component to the secondary mixture obtained in S2, cool to room temperature, and disperse for 30 minutes under stirring at 5500 rpm and ultrasonic assistance at 25 kHz to obtain the ultra-high temperature radiation-resistant adhesive.

[0038] Comparative Example 1: The difference between this comparative example and Example 1 is that the radiation-resistant component is not subjected to loading treatment, but only an equal amount of radiation-resistant agent and inorganic binder is added; and the high-temperature resistant component is not subjected to loading treatment, but only an equal amount of high-temperature stabilizer is added.

[0039] Comparative Example 2: The difference between this comparative example and Example 1 is that the radiation-resistant component is not subjected to loading treatment, but only equal amounts of radiation-resistant agent and inorganic binder are added.

[0040] Comparative Example 3: The difference between this comparative example and Example 1 is that the high-temperature resistant component is not subjected to loading treatment, but only an equal amount of high-temperature stabilizer is added.

[0041] Comparative Example 4: The difference between this comparative example and Example 1 is that the radiation-resistant component is not subjected to loading treatment, but is directly added with equal amounts of mesoporous silica nanoparticles, radiation-resistant agent and inorganic binder; and the high-temperature resistant component is not subjected to loading treatment, but is directly added with equal amounts of mesoporous silica nanoparticles and high-temperature stabilizer.

[0042] Comparative Example 5: The difference between this comparative example and Example 1 is that the radiation-resistant component and the high-temperature resistant component are replaced with a radiation-resistant-high-temperature composite component; that is, mesoporous silica nanoparticles, radiation-resistant agent, inorganic binder and high-temperature stabilizer are loaded together.

[0043] Specifically, the preparation method of the radiation-resistant-high-temperature composite component is as follows: A1. Mix the same amount of radiation resistant agent, inorganic binder aluminum phosphate, high temperature stabilizer and ethanol aqueous solution used in Example 1 at one time, and mix at a stirring speed of 500 rpm for 25 min to obtain a mixture; A2. Add the same amount of mesoporous silica nanoparticles as used in Example 1 to a mixture under conditions of ultrasonic frequency of 35KHz and stirring speed of 6000rpm, at a rate of 1.75g / s. After addition, filter and dry to obtain the radiation-resistant high-temperature composite component.

[0044] In the preparation of an ultra-high temperature radiation-resistant adhesive, the amounts of other components are the same as in Example 1, except that 0.8 parts of the radiation-resistant component and 1.2 parts of the high temperature-resistant component are replaced with 2 parts of the radiation-resistant-high temperature composite component.

[0045] Test Example: Test Subjects: Ultra-high temperature radiation resistant adhesive test samples prepared in Example 1 and Comparative Examples 1-3.

[0046] Test items and methods: First, each test sample was mixed with deionized water at a mass ratio of 100:18 to form a slurry; then, a homogeneous high-temperature resistant rigid substrate (alumina ceramic) was selected, and the samples were overlapped and bonded with a standard bonding area of ​​25mm×25mm. The slurry was evenly coated without gaps; then, the samples were allowed to stand at room temperature for 40 minutes for initial setting; then, they were cured in a curing chamber at 25℃ and 90% humidity for 72 hours to form a stable bonding layer; finally, they were dried in an oven at 110℃ for 2 hours and cooled to room temperature to obtain standard bonding test samples, which were then subjected to the following three performance tests.

[0047] ① High temperature resistance (1200℃×1h): Bond strength retention rate (%) = (bond strength after 1h high temperature treatment at 1200℃ / initial bond strength at room temperature) × 100%; the larger the retention rate value, the better the high temperature resistance of the corresponding test sample; ② Radiation resistance performance (5kGy / h×50h): Bond strength retention rate (%) = (bond strength after treatment with Co-60γ source at a dose rate of 5kGy / h for 50h / initial bond strength before irradiation) × 100%; the larger the retention rate value, the better the radiation resistance performance of the corresponding test sample. ③Radiation and high temperature resistance performance (5kGy / h×50h+1200℃×1h): Bond strength retention rate (%) = (bond strength after 50h treatment at 5kGy / h dose rate followed by 1h treatment at 1200℃ high temperature / initial bond strength before treatment) × 100%; the larger the retention rate value, the better the corresponding test sample has both radiation resistance and high temperature resistance performance.

[0048] Experimental results: see Table 1.

[0049] Table 1. Experimental Data Results Analysis: Combining the data in Table 1 and... Figures 1-2 Analysis of Examples 1-3 shows that the adhesive test samples prepared by the present invention (Examples 1-3) exhibit excellent high-temperature resistance (1200℃×1h): the bond strength retention rate is as high as 95.0% or more; radiation resistance (5kGy / h×50h): the bond strength retention rate is as high as 90.3% or more; and radiation-high-temperature resistance (5kGy / h×50h+1200℃×1h): the bond strength retention rate can also reach 85.2% or more. It is evident that the adhesive prepared by the present invention (Examples 1-3) possesses both excellent high-temperature resistance and radiation resistance.

[0050] Combining the data in Table 1 and Figures 1-2 The analysis focused on Example 1 and Comparative Examples 1-5: Specifically, by comparing Comparative Examples 1, 2, and 3, it can be seen that adding a high-temperature stabilizer loaded onto mesoporous silica nanoparticles to form a high-temperature resistant component can significantly improve the high-temperature resistance (1200℃×1h) of the prepared adhesive test sample; adding a radiation resistant agent and an inorganic binder loaded onto mesoporous silica nanoparticles to form a radiation resistant component can significantly improve the radiation resistance (5kGy / h×50h) of the prepared adhesive test sample.

[0051] Further analysis revealed that Comparative Example 1 had no load, resulting in agglomeration of functional powders, high porosity of the adhesive layer, and susceptibility to high-temperature cracking and irradiation-induced aging, thus exhibiting the lowest performance in all three aspects. Comparative Example 2 only showed resistance to high-temperature load, significantly improving its high-temperature thermal stability, but lacked a specific irradiation-resistant modifier, making the adhesive interface susceptible to damage from radiation and resulting in weak irradiation-resistant composite performance. Comparative Example 3 only showed resistance to irradiation load, exhibiting superior resistance to irradiation aging, but the high-temperature resistant filler was not modified by load and was unevenly dispersed, making it prone to structural loosening at ultra-high temperatures (1200℃), resulting in insufficient high-temperature tolerance.

[0052] When compared with Comparative Example 4, it can be seen that direct physical mixing (including mesoporous silica nanoparticles) results in performance data that are only slightly better than Comparative Example 1.

[0053] Further analysis revealed that in Comparative Example 4, all raw materials were directly and physically mixed, resulting in a simple mixture without liquid-phase premixing, gradient stirring, or directional ultrasonic loading. Consequently, the powder still agglomerated secondary. The mesoporous silica nanoparticles served only as ordinary fillers and could not play a role in carrier loading / modification. Their performance was only slightly better than that of the pure virgin powder group (Comparative Example 1).

[0054] In comparison with Comparative Example 5, it can be seen that when the (radiation-resistant + high-temperature-resistant) raw materials are co-loaded at one time to form a radiation-resistant-high-temperature composite component and then added, the radiation-resistant-high-temperature performance (5kGy / h×50h+1200℃×1h): the bond strength retention rate test data is actually lower than that of Comparative Example 4, which directly and completely physically mixed (including mesoporous silica nanoparticles).

[0055] Further analysis revealed that in Comparative Example 5, the raw materials (radiation resistant + high temperature resistant) were loaded together in a single process. The raw materials were mixed, and the physicochemical properties, particle size, and surface activity of yttrium oxide, zirconium titanate, cerium oxide, and zircon sand varied greatly. When mixed together, it was impossible to achieve directional and uniform loading, resulting in powders competing for space in the mesoporous silica channels and adsorption imbalance. The uniform 35kHz ultrasonic frequency and uniform feeding speed could not simultaneously adapt to the optimal loading conditions of the two types of fillers. Some functional powders floated on the surface and were easy to fall off, while some fillers were excessively piled up and blocked the channels. The radiation resistant functional phase and the high temperature stable phase interfered with each other at the interface, canceling out some of their functional advantages. They could not achieve the radiation resistance effect of a single radiation resistant load, nor the heat resistance effect of a single high temperature resistant load. Finally, after being subjected to the dual harsh effects of irradiation and high temperature, the strength attenuation was even greater, and the overall performance was not as good as that of a single component independently loaded, and even weaker than that of directly physically mixed mesoporous silica nanoparticles.

[0056] Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A high-temperature radiation-resistant adhesive, characterized in that, By weight, it comprises the following components: 48-53 parts quartz powder, 67-72 parts aluminate cement, 0.7-0.9 parts radiation-resistant component, 1-1.3 parts high-temperature resistant component, 3-3.5 parts alumina, 4-4.5 parts aluminum dihydrogen phosphate, 0.2-0.4 parts phthalate ester, 0.4-0.6 parts silane coupling agent, and 0.3-0.5 parts dispersant; The radiation-resistant component consists of mesoporous silica nanoparticles loaded with a radiation-resistant agent and an inorganic binder; the total mass of the radiation-resistant agent and the inorganic binder is 23-28% of the mass of the mesoporous silica nanoparticles, and the mass ratio of the radiation-resistant agent to the inorganic binder is 1:(1.3-1.7); the radiation-resistant agent is composed of yttrium oxide and zirconium titanate in a mass ratio of (0.4-0.6):

1. The high-temperature resistant component consists of mesoporous silica nanoparticles loaded with a high-temperature stabilizer, the mass of which is 10-13% of the mass of the mesoporous silica nanoparticles; the high-temperature stabilizer is composed of cerium oxide and zircon sand in a mass ratio of (0.5-0.7):

1.

2. The ultra-high temperature radiation-resistant adhesive according to claim 1, characterized in that, The method for preparing the radiation-resistant component is as follows: A1. Mix the radiation-resistant agent, inorganic binder, and ethanol-water solution to obtain a mixture; A2. Under ultrasonic and stirring conditions, mesoporous silica nanoparticles are added to the mixture obtained in A1, filtered, and dried to obtain the radiation-resistant component.

3. The ultra-high temperature radiation-resistant adhesive according to claim 2, characterized in that, The specific operation of A1 is as follows: First, mix 50-60 wt% of the radiation resistant agent with the inorganic binder for 20-25 min to obtain a premix; then add the remaining radiation resistant agent to the premix, continue mixing for 15-20 min, and then mix with the ethanol aqueous solution for 20-30 min.

4. The ultra-high temperature radiation-resistant adhesive according to claim 2, characterized in that, In A2, the ultrasonic frequency is 25-30KHz, the stirring speed is 4000-9000rpm, and the addition speed is 0.3-0.8g / s.

5. The ultra-high temperature radiation-resistant adhesive according to claim 2, characterized in that, The inorganic binder is aluminum phosphate.

6. The ultra-high temperature radiation-resistant adhesive according to claim 1, characterized in that, The preparation method of the high-temperature resistant component is as follows: B1. Disperse the high-temperature stabilizer in an aqueous ethanol solution to obtain a dispersion; B2. Under ultrasonic and stirring conditions, mesoporous silica nanoparticles are added to the dispersion obtained in B1, filtered, and dried to obtain the high-temperature resistant component.

7. The ultra-high temperature radiation-resistant adhesive according to claim 6, characterized in that, In B2, the ultrasonic frequency is 38-45KHz, the stirring speed is 5000rpm-8000rpm, and the addition speed is 2.5-3.5g / s.

8. The ultra-high temperature radiation-resistant adhesive according to claim 2 or 6, characterized in that, The volume ratio of ethanol to water in the ethanol-water solution is 1:(5-8).

9. The ultra-high temperature radiation-resistant adhesive according to claim 1, characterized in that, The silica content of the quartz powder is ≥98%, and the particle size is 5-50μm; the Al2O3 content of the aluminate cement is ≥70%; the phthalate is dibutyl phthalate; the silane coupling agent is KH-550; and the dispersant is a polycarboxylate dispersant.

10. The ultra-high temperature radiation-resistant adhesive according to claim 1, characterized in that, The preparation method of the ultra-high temperature radiation-resistant adhesive is as follows: S1. By weight, mix the quartz powder and aluminate cement and stir at 2000-2500 rpm for 15-20 minutes to obtain the basic mixture; S2. Add alumina, aluminum dihydrogen phosphate, dispersant, phthalate and silane coupling agent to the basic mixture obtained in S1, heat to 40-50℃, stir at 3000-3500 rpm for 25-30 min to obtain secondary mixture; S3. Add the radiation-resistant component and the high-temperature resistant component to the secondary mixture obtained in S2, cool to room temperature, stir at 5000-5500 rpm, and disperse under 20-25KHz ultrasonic assistance for 30-40 minutes to obtain the ultra-high temperature radiation-resistant adhesive.