A fuse ceramic material and a method for producing the same

Abstract

The application relates to the field of ceramic materials, in particular to a fuse ceramic material and a preparation method thereof. 2‑x The fuse ceramic material is made of a transition metal ion liquid polymer and a sintering aid. 2‑x The mass ratio of the transition metal ion liquid polymer and the sintering aid is 1:3%-6%:0.5%-1%, and the ceramic material prepared by the application has excellent mechanical properties, and the comprehensive performance can meet the strict requirements of mechanical reliability of the fuse.

Description

Technical Field

[0001] This invention relates to the field of ceramic materials, specifically to a ceramic material for fuses and its preparation method. Background Technology

[0002] Fuses are critical protective components in electrical circuits, and their core component, the fusible element, is typically encapsulated within a ceramic tube. The ceramic tube material must possess excellent electrical insulation properties and good thermal stability to withstand the high-temperature impacts and high mechanical strength during the fusing process. Currently, alumina ceramics have become the mainstream material for fuse ceramic tubes due to their high insulation, high-temperature resistance, and chemical stability.

[0003] However, pure alumina ceramics suffer from high brittleness and insufficient thermal shock resistance. To improve their performance, existing technologies typically employ whisker reinforcement. Aluminum titanate, with its low coefficient of thermal expansion and good thermal shock resistance, can significantly improve the thermal shock resistance and mechanical strength of alumina ceramics when combined with them. While the traditional alumina-titanium dioxide system can generate aluminum titanate through a high-temperature solid-state reaction, the resulting aluminum titanate often exhibits equiaxed grains, limiting its reinforcing effect. Summary of the Invention

[0004] Purpose of the invention: In view of the above-mentioned technical problems, the present invention proposes a ceramic material for fuses and its preparation method.

[0005] The technical solution adopted is as follows: A type of fuse ceramic material, made of TiO 2-x It is made from transition metal ion liquid polymers and sintering aids.

[0006] Furthermore, the aforementioned TiO 2-x The mass ratio of transition metal ion liquid polymer to sintering aid is 1:3%-6%:0.5%-1%.

[0007] Furthermore, the TiO 2-x The preparation method of transition metal ion liquid polymer is as follows: Nano-titanium dioxide and sodium borohydride were ball-milled and mixed evenly. The resulting powder mixture was then subjected to a reduction reaction under an argon atmosphere. After the reaction was completed, the mixture was cooled to room temperature, washed with deionized water and anhydrous ethanol, and then dried to obtain TiO2. 2-x Nanoparticles, TiO 2-x Nanoparticles are modified with a silane coupling agent and dispersed in a solvent. Then, an allyl transition metal ionic liquid and a free radical initiator are added to carry out polymerization.

[0008] Furthermore, the mass ratio of the nano-titanium dioxide to sodium borohydride is 1:0.3-0.6.

[0009] Furthermore, the temperature of the reduction reaction is 450-500℃.

[0010] Furthermore, the transition metal in the allyl transition metal ionic liquid is iron.

[0011] Furthermore, the structural formula of the allyl transition metal ionic liquid is as follows: Wherein, R is an alkyl group.

[0012] Furthermore, R can be any one of methyl, ethyl, propyl, butyl, pentyl, or hexyl.

[0013] Furthermore, the structural formula of the allyl transition metal ionic liquid is as follows: .

[0014] Furthermore, the sintering aid is composed of SiO2, ZrO2, Y2O3 and MgO, and the mass ratio of SiO2, ZrO2, Y2O3 and MgO is 1-5:1-5:1-5:1-5.

[0015] This invention also provides a method for preparing a ceramic material for fuses: Will TiO 2-x The transition metal ion liquid polymer and sintering aid are mixed, ball-milled, granulated, pressed into green bodies, heated to 500-600℃ and held for 3-6 hours under an argon atmosphere, and then heated to 1500-1550℃ and held for 2-4 hours.

[0016] The beneficial effects of this invention are: This invention constructs TiO 2-x A dual-catalytic synergistic system of oxygen vacancies and transition metal ion liquid polymers, in which TiO2... 2-x TiO2 provides catalytic active centers for solid-phase diffusion and surface reactions. 2-x Oxygen vacancies and Ti present on the surface and in the bulk phase 3+ Defects will cause Al to be affected by vacancy mechanisms. 3+ The diffusion activation energy decreases, and the defect sites, acting as Lewis acid centers, strongly adsorb Al. 3+The formation of an Al-O-Ti active precursor transforms the nucleation of Al2TiO5 from random three-dimensional growth to anisotropic one-dimensional growth controlled by defect sites, ultimately resulting in the in-situ generation of high aspect ratio whiskers at a lower temperature. The transition metal ions released after the high-temperature decomposition of the transition metal ion liquid polymer form a nanoscale liquid-phase catalyst, promoting the axial elongation of the whiskers through a gas-liquid-solid mechanism. This dual-catalytic design allows whisker growth to combine the advantages of high nucleation density and high growth rate. The thermal expansion coefficient of the in-situ generated Al2TiO5 whiskers differs significantly from that of the alumina matrix. This thermal expansion mismatch generates compressive residual stress at the whisker-matrix interface, enhancing interfacial bonding strength and inducing whisker bridging and pull-out mechanisms during crack propagation, thus improving the fracture toughness of the material. Simultaneously, the load transfer effect of the whisker network on the matrix significantly improves the flexural strength, achieving a synergistic effect of reinforcement and toughening. The introduction of a silane coupling agent establishes the TiO2-TiO5-coupling mechanism. 2-x The chemical bonding between TiO₂ and the ionic liquid polymer, and the organic segments of the polymer preventing nanoparticle aggregation through steric hindrance and electrostatic repulsion, enable TiO₂ to... 2-x Achieving molecular-level uniform dispersion within the alumina matrix ensures that whiskers grow uniformly throughout the entire three-dimensional space rather than agglomerating locally. This avoids the uneven distribution and directional alignment problems of traditional externally added whiskers. Simultaneously, the multi-component composite design of the sintering aid promotes densification through liquid-phase sintering and through Y... 3+ and Mg 2+ By lattice doping to stabilize the high-temperature Al2TiO5 phase and using ZrO2 for phase transformation toughening, a high-performance fuse ceramic material with low porosity, clean grain boundaries, and uniform whisker distribution is finally obtained. Its comprehensive performance can meet the stringent requirements of fuses for mechanical reliability. Attached Figure Description

[0017] Figure 1 The image shows a cross-sectional SEM image of the ceramic fuse material prepared in Example 1.

[0018] Figure 2 for Figure 1 A magnified view of the selected area. Detailed Implementation

[0019] Unless otherwise specified in the examples, the conditions were performed under standard conditions or as recommended by the manufacturer. Reagents or instruments whose manufacturers are not specified are all commercially available products. Techniques not mentioned in this invention refer to existing technologies. Unless otherwise specified, the following examples and comparative examples are parallel experiments, using the same processing steps and parameters. Example 1:

[0020] A ceramic material for fuses, comprising, by mass ratio of 1:5%:0.8% TiO2-x It is made from transition metal ion liquid polymers and sintering aids.

[0021] The sintering aid consists of SiO2, ZrO2, Y2O3 and MgO in a mass ratio of 1:1:1:1.

[0022] Among them, TiO 2-x The preparation method of transition metal ion liquid polymer is as follows: 10g of P25 nano-TiO2 and 3.5g of sodium borohydride were ball-milled for 5 hours under an argon atmosphere, with the ball-milling temperature controlled at ≤50℃. The resulting mixed powder was placed in a sealed small porcelain boat and then pushed into a tube furnace. The temperature was raised to 475℃ and maintained for 2 hours under an argon atmosphere. After the reaction was completed, the mixture was cooled to room temperature. The product was washed three times each with deionized water and anhydrous ethanol and then dried in a vacuum oven at 60℃ for 24 hours to obtain TiO2. 2-x Nanoparticles.

[0023] 0.025 mol of 1-allyl-3-methylimidazolium chloride and 0.025 mol of FeCl3·3H2O were successively added to a 50 mL round-bottom flask. Under nitrogen protection, the mixture was stirred at room temperature for 6 h. After standing, the product separated into an aqueous phase and an ionic liquid phase. The upper aqueous phase was poured off, and the ionic liquid phase was washed with distilled water, distilled under reduced pressure, and then dried in a vacuum drying oven at 70 °C for 24 h to obtain 1-allyl-3-methylimidazolium ferric chloride. 5 g of TiO2 was then added to the flask. 2-x Nanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 15 min. Then, 0.5 g of KH-570 was added, and the mixture was stirred at room temperature for 30 min. The temperature was then raised to 80 °C and refluxed for 2 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum oven at 60 °C for 24 h to obtain KH-570 modified TiO2. 2-x Nanoparticles, modifying the above-mentioned KH-570 TiO2 2-x Nanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 10 min. Then, 1 g of 1-allyl-3-methylimidazolium ferric chloride was added, and the mixture was stirred for 30 min. Finally, 0.02 g of free radical initiator AIBN was added, and the mixture was heated to 60 °C under nitrogen protection for 6 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum drying oven at 70 °C for 24 h to obtain TiO2. 2-x @Transition metal ion liquid polymer. The preparation method of the above-mentioned fuse ceramic material: Will TiO 2-xThe transition metal ion liquid polymer and sintering aid were added to the ball mill jar of a planetary ball mill, mixed and ball-milled for 10 hours with anhydrous ethanol as the milling medium, and then dried. The mixture was granulated using polyvinyl alcohol as a binder. The resulting granules were pressed into green bodies, which were then heated to 550°C and held for 4 hours under an argon atmosphere, followed by heating to 1525°C and holding for 3 hours. The SEM image is shown below. Figure 1 and Figure 2 As shown, Al2TiO5 whiskers are formed. Example 2:

[0024] A type of ceramic material for fuses, comprising components in a mass ratio of 1:6%:1%. TiO 2-x It is made from transition metal ion liquid polymers and sintering aids.

[0025] The sintering aid consists of SiO2, ZrO2, Y2O3 and MgO in a mass ratio of 1:1:1:1.

[0026] Among them, TiO 2-x The preparation method of transition metal ion liquid polymer is as follows: 10g of P25 nano-TiO2 and 6g of sodium borohydride were ball-milled for 5 hours under an argon atmosphere, with the milling temperature controlled at ≤50℃. The resulting powder mixture was placed in a sealed ceramic boat and then pushed into a tube furnace. The temperature was raised to 500℃ and maintained for 2 hours under an argon atmosphere. After the reaction was completed, the mixture was cooled to room temperature. The product was washed three times each with deionized water and anhydrous ethanol and then dried in a vacuum oven at 60℃ for 24 hours to obtain TiO2. 2-x Nanoparticles.

[0027] 0.025 mol of 1-allyl-3-methylimidazolium chloride and 0.025 mol of FeCl3·3H2O were successively added to a 50 mL round-bottom flask. Under nitrogen protection, the mixture was stirred at room temperature for 6 h. After standing, the product separated into an aqueous phase and an ionic liquid phase. The upper aqueous phase was poured off, and the ionic liquid phase was washed with distilled water, distilled under reduced pressure, and then dried in a vacuum drying oven at 70 °C for 24 h to obtain 1-allyl-3-methylimidazolium ferric chloride. 5 g of TiO2 was then added to the flask. 2-x Nanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 15 min. Then, 0.5 g of KH-570 was added, and the mixture was stirred at room temperature for 30 min. The temperature was then raised to 80 °C and refluxed for 2 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum oven at 60 °C for 24 h to obtain KH-570 modified TiO2. 2-x Nanoparticles, modifying the above-mentioned KH-570 TiO2 2-xNanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 10 min. Then, 1 g of 1-allyl-3-methylimidazolium ferric chloride was added, and the mixture was stirred for 30 min. Finally, 0.02 g of free radical initiator AIBN was added, and the mixture was heated to 60 °C under nitrogen protection for 6 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum drying oven at 70 °C for 24 h to obtain TiO2. 2-x @Transition metal ion liquid polymer. The preparation method of the above-mentioned fuse ceramic material: Will TiO 2-x The transition metal ion liquid polymer and sintering aid are added to the ball mill jar of a planetary ball mill, mixed and ball-milled for 10 hours with anhydrous ethanol as the ball milling medium, and then dried. The granules are granulated with polyvinyl alcohol as a binder, and the resulting granules are pressed into green blanks. The green blanks are heated to 600°C and held for 6 hours under an argon atmosphere, and then heated to 1550°C and held for 4 hours. Example 3:

[0028] A ceramic material for fuses, comprising components in a mass ratio of 1:3%:0.5% TiO 2-x It is made from transition metal ion liquid polymers and sintering aids.

[0029] The sintering aid consists of SiO2, ZrO2, Y2O3 and MgO in a mass ratio of 1:1:1:1.

[0030] Among them, TiO 2-x The preparation method of transition metal ion liquid polymer is as follows: 10g of P25 nano-TiO2 and 3g of sodium borohydride were ball-milled for 5 hours under an argon atmosphere, with the ball-milling temperature controlled at ≤50℃. The resulting mixed powder was placed in a sealed small porcelain boat and then pushed into a tube furnace. The temperature was raised to 450℃ and maintained for 2 hours under an argon atmosphere. After the reaction was completed, the mixture was cooled to room temperature. The product was washed three times each with deionized water and anhydrous ethanol and then dried in a vacuum oven at 60℃ for 24 hours to obtain TiO2. 2-x Nanoparticles.

[0031] 0.025 mol of 1-allyl-3-methylimidazolium chloride and 0.025 mol of FeCl3·3H2O were successively added to a 50 mL round-bottom flask. Under nitrogen protection, the mixture was stirred at room temperature for 6 h. After standing, the product separated into an aqueous phase and an ionic liquid phase. The upper aqueous phase was poured off, and the ionic liquid phase was washed with distilled water, distilled under reduced pressure, and then dried in a vacuum drying oven at 70 °C for 24 h to obtain 1-allyl-3-methylimidazolium ferric chloride. 5 g of TiO2 was then added to the flask. 2-xNanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 15 min. Then, 0.5 g of KH-570 was added, and the mixture was stirred at room temperature for 30 min. The temperature was then raised to 80 °C and refluxed for 2 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum oven at 60 °C for 24 h to obtain KH-570 modified TiO2. 2-x Nanoparticles, modifying the above-mentioned KH-570 TiO2 2-x Nanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 10 min. Then, 1 g of 1-allyl-3-methylimidazolium ferric chloride was added, and the mixture was stirred for 30 min. Finally, 0.02 g of free radical initiator AIBN was added, and the mixture was heated to 60 °C under nitrogen protection for 6 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum drying oven at 70 °C for 24 h to obtain TiO2. 2-x @Transition metal ion liquid polymer. The preparation method of the above-mentioned fuse ceramic material: Will TiO 2-x The transition metal ion liquid polymer and sintering aid are added to the ball mill jar of a planetary ball mill, mixed and ball-milled for 10 hours with anhydrous ethanol as the ball milling medium, and then dried. The granules are granulated with polyvinyl alcohol as a binder, and the resulting granules are pressed into green blanks. The green blanks are heated to 500°C and held for 3 hours under an argon atmosphere, and then heated to 1500°C and held for 2 hours. Example 4:

[0032] A ceramic material for fuses, comprising components in a mass ratio of 1:6%:0.5% TiO 2-x It is made from transition metal ion liquid polymers and sintering aids.

[0033] The sintering aid consists of SiO2, ZrO2, Y2O3 and MgO in a mass ratio of 2:2:1:1.

[0034] Among them, TiO 2-x The preparation method of transition metal ion liquid polymer is as follows: 10g of P25 nano-TiO2 and 6g of sodium borohydride were ball-milled for 5 hours under an argon atmosphere, with the ball-milling temperature controlled at ≤50℃. The resulting mixed powder was placed in a sealed small porcelain boat and then pushed into a tube furnace. The temperature was raised to 450℃ and maintained for 2 hours under an argon atmosphere. After the reaction was completed, the mixture was cooled to room temperature. The product was washed three times each with deionized water and anhydrous ethanol and then dried in a vacuum oven at 60℃ for 24 hours to obtain TiO2. 2-x Nanoparticles.

[0035] 0.025 mol of 1-allyl-3-methylimidazolium chloride and 0.025 mol of FeCl3·3H2O were successively added to a 50 mL round-bottom flask. Under nitrogen protection, the mixture was stirred at room temperature for 6 h. After standing, the product separated into an aqueous phase and an ionic liquid phase. The upper aqueous phase was poured off, and the ionic liquid phase was washed with distilled water, distilled under reduced pressure, and then dried in a vacuum drying oven at 70 °C for 24 h to obtain 1-allyl-3-methylimidazolium ferric chloride. 5 g of TiO2 was then added to the flask. 2-x Nanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 15 min. Then, 0.5 g of KH-570 was added, and the mixture was stirred at room temperature for 30 min. The temperature was then raised to 80 °C and refluxed for 2 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum oven at 60 °C for 24 h to obtain KH-570 modified TiO2. 2-x Nanoparticles, modifying the above-mentioned KH-570 TiO2 2-x Nanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 10 min. Then, 1 g of 1-allyl-3-methylimidazolium ferric chloride was added, and the mixture was stirred for 30 min. Finally, 0.02 g of free radical initiator AIBN was added, and the mixture was heated to 60 °C under nitrogen protection for 6 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum drying oven at 70 °C for 24 h to obtain TiO2. 2-x @Transition metal ion liquid polymer. The preparation method of the above-mentioned fuse ceramic material: Will TiO 2-x The transition metal ion liquid polymer and sintering aid are added to the ball mill jar of a planetary ball mill, mixed and ball-milled for 10 hours with anhydrous ethanol as the ball milling medium, and then dried. The granules are granulated with polyvinyl alcohol as a binder, and the resulting granules are pressed into green blanks. The green blanks are heated to 600°C and held for 3 hours under an argon atmosphere, and then heated to 1550°C and held for 2 hours. Example 5:

[0036] A ceramic material for fuses, comprising components in a mass ratio of 1:3%:1% TiO 2-x It is made from transition metal ion liquid polymers and sintering aids.

[0037] The sintering aid consists of SiO2, ZrO2, Y2O3 and MgO in a mass ratio of 1:1:2:2.

[0038] Among them, TiO 2-x The preparation method of transition metal ion liquid polymer is as follows: 10g of P25 nano-TiO2 and 3g of sodium borohydride were ball-milled for 5 hours under an argon atmosphere, with the milling temperature controlled at ≤50℃. The resulting powder mixture was placed in a sealed ceramic boat and then pushed into a tube furnace. The temperature was raised to 500℃ and maintained for 2 hours under an argon atmosphere. After the reaction was completed, the mixture was cooled to room temperature. The product was washed three times each with deionized water and anhydrous ethanol and then dried in a vacuum oven at 60℃ for 24 hours to obtain TiO2. 2-x Nanoparticles.

[0039] 0.025 mol of 1-allyl-3-methylimidazolium chloride and 0.025 mol of FeCl3·3H2O were successively added to a 50 mL round-bottom flask. Under nitrogen protection, the mixture was stirred at room temperature for 6 h. After standing, the product separated into an aqueous phase and an ionic liquid phase. The upper aqueous phase was poured off, and the ionic liquid phase was washed with distilled water, distilled under reduced pressure, and then dried in a vacuum drying oven at 70 °C for 24 h to obtain 1-allyl-3-methylimidazolium ferric chloride. 5 g of TiO2 was then added to the flask. 2-x Nanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 15 min. Then, 0.5 g of KH-570 was added, and the mixture was stirred at room temperature for 30 min. The temperature was then raised to 80 °C and refluxed for 2 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum oven at 60 °C for 24 h to obtain KH-570 modified TiO2. 2-x Nanoparticles, modifying the above-mentioned KH-570 TiO2 2-x Nanoparticles were added to 50 ml of anhydrous ethanol and ultrasonically dispersed for 10 min. Then, 1 g of 1-allyl-3-methylimidazolium ferric chloride was added, and the mixture was stirred for 30 min. Finally, 0.02 g of free radical initiator AIBN was added, and the mixture was heated to 60 °C under nitrogen protection for 6 h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum drying oven at 70 °C for 24 h to obtain TiO2. 2-x @Transition metal ion liquid polymer. The preparation method of the above-mentioned fuse ceramic material: Will TiO 2-x The transition metal ion liquid polymer and sintering aid are added to the ball mill jar of a planetary ball mill, mixed and ball-milled for 10 hours with anhydrous ethanol as the ball milling medium, and then dried. The granules are granulated with polyvinyl alcohol as a binder, and the resulting granules are pressed into green blanks. The green blanks are heated to 500°C and held for 6 hours under an argon atmosphere, and then heated to 1500°C and held for 4 hours.

[0040] Comparative Example 1: This is basically the same as Example 1, except that TiO2 is not added. 2-x @Transition metal ion liquid polymer.

[0041] Comparative Example 2: Basically the same as Example 1, except that TiO2 is used. 2-x Nanoparticles replace TiO 2-x @Transition metal ion liquid polymer.

[0042] Among them, TiO 2-x The preparation method of nanoparticles is as follows: 10g of P25 nano-TiO2 and 3.5g of sodium borohydride were ball-milled for 5 hours under an argon atmosphere, with the ball-milling temperature controlled at ≤50℃. The resulting mixed powder was placed in a sealed small porcelain boat and then pushed into a tube furnace. The temperature was raised to 475℃ and maintained for 2 hours under an argon atmosphere. After the reaction was completed, the mixture was cooled to room temperature. The product was washed three times each with deionized water and anhydrous ethanol and then dried in a vacuum oven at 60℃ for 24 hours to obtain TiO2. 2-x Nanoparticles.

[0043] Comparative Example 3: This is essentially the same as Example 1, except that P25 nano-TiO2 is used instead of TiO2. 2-x @Transition metal ion liquid polymer.

[0044] Comparative Example 4: This is essentially the same as Example 1, except that TiO2@transition metal ionic liquid polymer is used instead of TiO2. 2-x @Transition metal ion liquid polymer.

[0045] The preparation method of TiO2@transition metal ion liquid polymer is as follows: 0.025 mol of 1-allyl-3-methylimidazolium chloride and 0.025 mol of FeCl3·3H2O were successively added to a 50 ml round-bottom flask. Under nitrogen protection, the mixture was stirred at room temperature for 6 h. After standing, the product separated into two layers: an aqueous phase and an ionic liquid phase. The upper aqueous phase was poured off, and the ionic liquid phase was washed with distilled water, distilled under reduced pressure, and then dried in a vacuum drying oven at 70 °C for 24 h to obtain 1-allyl-3-methylimidazolium ferric chloride. 5g of P25 nano-TiO2 was added to 50ml of anhydrous ethanol and ultrasonically dispersed for 15min. 0.5g of KH-570 was added, and the mixture was stirred at room temperature for 30min. The temperature was then raised to 80℃ and refluxed for 2h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum oven at 60℃ for 24h to obtain KH-570 modified TiO2 nanoparticles. The KH-570 modified TiO2 nanoparticles were then added to 50ml of anhydrous ethanol and ultrasonically dispersed for 10min. 1g of 1-allyl-3-methylimidazolium ferric chloride was added, and the mixture was stirred for 30min. 0.02g of free radical initiator AIBN was added, and the mixture was heated to 60℃ under nitrogen protection for 6h. After cooling to room temperature, the mixture was centrifuged, washed three times with anhydrous ethanol, and dried in a vacuum oven at 70℃ for 24h to obtain TiO2@transition metal ion liquid polymer.

[0046] Performance testing: The ceramic materials prepared in Examples 1-5 and Comparative Examples 1-4 of this invention were made into samples for performance testing; This paper uses the indentation method to test the fracture toughness of the specimens; This paper uses the three-point bending method to test the bending strength of the specimens. The specimens are prepared into 3×4×40mm strips by slicing, grinding and polishing. The bending strength is measured on a WD-10 electronic universal testing machine with a span of 30mm and a loading rate of 0.5mm / min. Five strips are prepared for each group for measurement and calculation. The average value of the results is taken as the bending strength of the tested specimen.

[0047] The test results are shown in Table 1 below: As shown in Table 1 above, the ceramic material prepared by the present invention has excellent mechanical properties, and its comprehensive performance can meet the stringent requirements of fuses for mechanical reliability.

[0048] As can be seen from the comparison between Example 1 and Comparative Example 1, TiO 2-x The addition of transition metal ion liquid polymers has played a positive role in improving the mechanical properties of ceramic materials.

[0049] As can be seen from the comparison between Example 1 and Comparative Example 2, the addition of TiO2... 2-xNanoparticles do not improve the mechanical properties of ceramic materials as much as adding TiO2. 2-x @Transition metal ion liquid polymer.

[0050] A comparison between Example 1 and Comparative Example 3 shows that the improvement in the mechanical properties of ceramic materials by adding P25 nano-TiO2 is not as significant as that by adding TiO2. 2-x @Transition metal ion liquid polymer.

[0051] A comparison between Example 1 and Comparative Example 4 shows that the improvement in the mechanical properties of ceramic materials by adding TiO2@transition metal ionic liquid polymer is not as significant as that by adding TiO2. 2-x @Transition metal ion liquid polymer.

[0052] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A ceramic material for fuses, characterized in that, Depend on TiO 2-x It is made from transition metal ion liquid polymers and sintering aids.

2. The ceramic material for fuses as described in claim 1, characterized in that, The TiO 2-x The mass ratio of transition metal ion liquid polymer to sintering aid is 1:3%-6%:0.5%-1%.

3. The ceramic material for fuses as described in claim 1, characterized in that, The TiO 2-x The preparation method of transition metal ion liquid polymer is as follows: Nano-titanium dioxide and sodium borohydride were ball-milled and mixed evenly. The resulting powder mixture was then subjected to a reduction reaction under an argon atmosphere. After the reaction was completed, the mixture was cooled to room temperature, washed with deionized water and anhydrous ethanol, and then dried to obtain TiO2. 2-x Nanoparticles, TiO 2-x Nanoparticles are modified with a silane coupling agent and dispersed in a solvent. Then, an allyl transition metal ionic liquid and a free radical initiator are added to carry out polymerization.

4. The ceramic material for fuses as described in claim 3, characterized in that, The mass ratio of nano-titanium dioxide to sodium borohydride is 1:0.3-0.

6.

5. The ceramic material for fuses as described in claim 3, characterized in that, The reduction reaction is carried out at a temperature of 450-500℃.

6. The ceramic material for fuses as described in claim 3, characterized in that, The transition metal in the allyl transition metal ionic liquid is iron.

7. The ceramic material for fuses as described in claim 6, characterized in that, The structural formula of the allyl transition metal ionic liquid is as follows: Wherein, R is an alkyl group.

8. The ceramic material for fuses as described in claim 7, characterized in that, R can be any one of methyl, ethyl, propyl, butyl, pentyl, or hexyl.

9. The ceramic material for fuses as described in claim 1, characterized in that, The sintering aid is composed of SiO2, ZrO2, Y2O3 and MgO, and the mass ratio of SiO2, ZrO2, Y2O3 and MgO is 1-5:1-5:1-5:1-5.

10. A method for preparing a fuse ceramic material as described in any one of claims 1-9, characterized in that, Specifically as follows: Will TiO 2-x The transition metal ion liquid polymer and sintering aid are mixed, ball-milled, granulated, pressed into green bodies, heated to 500-600℃ and held for 3-6 hours under an argon atmosphere, and then heated to 1500-1550℃ and held for 2-4 hours.

Images