CN113248244A - Low-temperature ceramic insulating material suitable for complex insulating structure and preparation method thereof - Google Patents

Low-temperature ceramic insulating material suitable for complex insulating structure and preparation method thereof Download PDF

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CN113248244A
CN113248244A CN202110550711.6A CN202110550711A CN113248244A CN 113248244 A CN113248244 A CN 113248244A CN 202110550711 A CN202110550711 A CN 202110550711A CN 113248244 A CN113248244 A CN 113248244A
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ceramic
low
insulating material
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temperature
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CN113248244B (en
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唐红川
朱晟毅
肖强
宋伟
梁花
秦威
佘倩豪
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Electric Power Research Institute of State Grid Chongqing Electric Power Co Ltd
State Grid Corp of China SGCC
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Electric Power Research Institute of State Grid Chongqing Electric Power Co Ltd
State Grid Corp of China SGCC
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Abstract

The invention discloses a low-temperature ceramic insulating material suitable for a complex insulating structure and a preparation method thereof, wherein the ceramic insulating material comprises the following raw materials in percentage by mass: 10-20% of silicon rubber, 30-40% of porcelain forming filler, 15-30% of low-melting-point fluxing agent, 15-30% of fumed silica, and the balance of functional additives and inevitable impurities, wherein the functional additives comprise a structural control agent and a vulcanizing agent, and the total amount of the structural control agent and the vulcanizing agent is 1-3%. According to the invention, the excellent mechanical properties of the precursor obtained after mixing and vulcanization are utilized, the precursor is further processed and molded into a shape with a complex insulating structure and then sintered, and the ceramic body finished product obtained after sintering into ceramic has the performances of corrosion resistance, high temperature resistance, radiation protection, excellent heat conduction performance and the like, meanwhile, the ceramic forming temperature of the ceramic material is reduced, the compact ceramic body is prepared at 1000 ℃, the actual application requirement is met, and the defects of the existing ceramic insulating material are overcome.

Description

Low-temperature ceramic insulating material suitable for complex insulating structure and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of low-temperature ceramic insulating materials, in particular to a low-temperature ceramic insulating material suitable for a complex insulating structure and a preparation method thereof.
Background
With the increase of national economy, the power consumption demand is continuously increased, and the electrical insulating material plays an important role in ensuring the safety and reliability of electrical energy, has wide development prospect, and has different performance requirements on the insulating material in different fields. Commonly used electrical insulating materials are classified into three types, i.e., organic insulating materials, inorganic insulating materials, and hybrid insulating materials. Most of the organic insulating materials are high molecular polymers including plastics, rubber and fibers. Commonly used are silicone rubber, polyethylene, epoxy resins, and the like. Inorganic insulating materials are based on ionic structures and include mica, ceramic, glass, and the like. The mixed insulating material is formed by mixing and processing an organic insulating material and an inorganic insulating material, and is commonly used as a base, a shell and the like of an electric appliance.
The organic insulating material has good comprehensive performanceThe insulating material has the advantages of good insulating property and mechanical strength, electric arc resistance, aging resistance, moldability or pouring molding and easy processing. However, under severe working conditions such as high temperature, corrosion, radiation, etc., various properties of the organic insulating material will be affected. In recent years, organic insulating materials are increasingly difficult to deal with complex working environments, and faults are also developed endlessly. The ceramic insulating material has excellent mechanical and electrical properties, high stability, high temperature resistance, corrosion resistance, radiation resistance and high heat conductivity, and can make up for the defects of organic insulating materials in some aspects. However, due to the characteristics of interatomic bond and microstructure, the ceramic material has low ductility and toughness and large brittleness, and the preparation process is greatly limited. When the ceramic material is formed, the mechanical strength of the green body is not high, it is difficult to form the ceramic member into a complicated shape, and the sintering temperature of the ceramic material is high, for example, Al2O3The sintering temperature of the ceramic is 1650-1950 ℃ according to different components, and the Si is sintered by hot pressing3N4The hot pressing temperature is generally 1600-1800 ℃, the sintering temperature is about 1800 ℃ when the AlN ceramic is sintered under no pressure, and the hot pressing sintering is carried out at the high temperature of 1800-2000 ℃. Therefore, the sintering temperature of the common ceramic is generally higher than the melting point (1083.4 ℃) of the copper wire, and the ceramic has great limitation in the application in the fields of electrical equipment and the like.
Guojianhua et al invented a low-temperature ceramizable silicone rubber and a preparation method thereof (CN107163585A), and prepared a composite silicone rubber material which is used in the flame-retardant and fire-resistant fields of wires and cables. The prepared composite silicon rubber has elasticity and electrical insulation property of common silicon rubber, can be ablated to form a ceramic layer when encountering a fire, has certain residual strength, has three-point bending strength exceeding 3MPa, can keep an internal copper wire of a wire cable from being fused within 30min, enables a circuit to be still smooth in the fire, and prevents the fire range from being expanded. According to the understanding of the technical personnel in the field of ceramic silicon rubber, the ceramic silicon rubber is used as a common fireproof flame-retardant material in the technical field, the finished product is composite silicon rubber, namely, the composite silicon rubber material before being vitrified is used, when a fire disaster happens, the composite silicon rubber material is sintered and vitrified to obtain a ceramic layer, so that the fireproof flame-retardant effect is achieved, the performance of the sintered silicon rubber composite material is qualitatively changed (the silicon rubber is lost in sintering), and the obtained ceramic layer does not meet the requirement of serving as a power cable protective shell any more and needs to be replaced. Therefore, the silicon rubber composite material prepared by the invention is essentially an organic insulating material, when a fire disaster occurs, the flatness and the compactness of a formed ceramic layer are limited, the ceramic layer has only certain residual strength, the three-point bending strength exceeds 3MPa, the mechanical strength is not high, and meanwhile, the research on the electrical insulating property and the thermal conductivity of the ceramic layer is lacked, the service performance of the sintered ceramic layer can not meet the requirements of the ceramic insulating material, and the application requirements of severe working conditions such as high temperature, corrosion, radiation and the like can not be met. In the concrete application of electric power system, the mechanical strength, the heat conductivility of material to and electrical insulation performance are limited, need in time change after the conflagration, need to have a power failure to overhaul, can increase fortune dimension and maintenance cost, reduced the reliability, consequently received great restriction in practical application. Although the preparation method comprises a sintering process, the sintering process is obviously a test belonging to the ceramic forming performance, and whether the ceramic layer with certain residual strength can be formed in the fire environment or not is judged, so that the fire range is prevented from being expanded. The obtained finished product is essentially a composite silicon rubber material, sintering and ceramization are not needed, and only a ceramic body but not the composite silicon rubber material can be obtained after sintering.
Therefore, a novel insulating material is needed, which has the characteristics of good mechanical strength, excellent electrical insulating property, easiness in processing and forming, capability of meeting the requirement of a complex insulating structure, good rigidity, high temperature resistance, radiation resistance and excellent heat conductivity, and capability of meeting the application requirements of severe working conditions such as high temperature, corrosion, radiation and the like.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the invention provides a low-temperature ceramic insulating material suitable for a complex insulating structure and a preparation method thereof, and the ceramic material with a smooth and compact surface is prepared.
The technical scheme adopted by the invention is as follows: the low-temperature ceramic insulating material suitable for the complex insulating structure is characterized by comprising the following raw materials in percentage by mass: 10-20% of silicon rubber, 30-40% of porcelain forming filler, 15-30% of low-melting-point fluxing agent, 15-30% of fumed silica, and the balance of functional additives and inevitable impurities, wherein the functional additives comprise a structural control agent and a vulcanizing agent, and the total amount of the structural control agent and the vulcanizing agent is 1-3%.
Compared with the low-temperature ceramic silicon rubber of Guojianhua and the like and the preparation method thereof, although the components of the low-temperature ceramic silicon rubber are different from the main components of the low-temperature ceramic silicon rubber, the types and the proportions of the fillers, the differences cause the low-temperature ceramic silicon rubber to be substantially different from the main components of the low-temperature ceramic silicon rubber, and the components are ceramic insulating materials. The obtained ceramic insulating material has a density of 2.15-2.18 g-cm-3The apparent porosity is 1.5-1.7%, the bending strength can reach 85Mpa, the linear shrinkage before and after porcelain forming is 12.06-12.21%, and the range of the thermal diffusion coefficient is 0.6mm2·s-1-0.8mm2·s-1Has a thermal conductivity in the range of 1.2 W.m-1·K-1-1.7W·m-1·K-1Volume resistivity of (3.101-3.111) × 1012Omega · m, a relative dielectric constant of 8.09 to 8.12, and a tan delta value of (9.30 to 9.38) × 10-4The power frequency breakdown field intensity is (21.01-21.31) kV · mm-1Can be widely applied to electric powerHigh temperature, corrosion, radiation and other harsh working conditions such as aerospace, military, nuclear industry and the like. Guojianhua et al, the invention relates to a silicone rubber composite material, which is prepared by using silicone rubber as a base material with a proportion of 40% -80% as a main component and adding various fillers as auxiliary components. According to the invention, silicon rubber is used as a binder, the proportion is 18%, components such as a ceramic forming material are mixed and vulcanized by utilizing the silicon rubber to obtain a precursor, then the precursor is processed and formed into an insulating product with a complex structure by utilizing the good processing performance of the precursor, the silicon rubber disappears after sintering to form silicon dioxide, and the silicon dioxide participates in the subsequent ceramic forming reaction, so that the ceramic insulating material meeting the requirement of the complex insulating structure is finally obtained. Meanwhile, the ceramic insulating material has a flat and compact section, the three-point bending strength is 85MPa, the insulating property and the heat conducting property are excellent, the three-point bending strength of the ceramic silicon rubber of Guo Jianhua and other people is only 3.1-5.9 MPa, the flatness and the compactness of the ceramic layer are limited, and meanwhile, the ceramic insulating material lacks the research on the insulating property and the heat conducting property of the ceramic layer, does not meet the use efficiency requirement of the ceramic insulating material and cannot meet the application requirements of harsh working conditions such as high temperature, corrosion, radiation and the like. This is a substantial difference between the present invention and the patented technology.
Further, the substrate is preferably a methyl vinyl silicone rubber, which functions as a binder for the precursor and at the same time provides silica in the porcelain forming process. It is of course also possible to use one or more of other silicone rubbers such as methyl phenyl vinyl silicone rubber.
Further, the porcelain forming filler is preferably wollastonite, but it is also possible to use one or more of mica, diatomaceous earth, kaolin and a fibrous filler.
Further, the low-melting point fluxing agent is preferably low-melting point glass powder, and the melting point is 400-500 ℃. Of course, one or more low-melting point fluxes such as zinc oxide and zinc borate may be used.
Further, the structural control agent is preferably hydroxy silicone oil. It is of course also possible to use one or more of diphenyldihydroxysilane, diphenyldimethoxysilane, diphenyldiethoxysilane, hexamethyldisilazane and other structuring agents.
Further, the vulcanizing agent is preferably 2, 4-dichlorobenzoyl peroxide. It is of course also possible to use 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane (dipenta), dicumyl peroxide (DCP) and the like as one or more further vulcanizing agents.
Preferably, the ceramic insulating material consists of the following raw materials in percentage by mass: 18 percent of methyl vinyl silicone rubber, 36 percent of wollastonite, 22 percent of low-melting-point glass powder, 22 percent of gas-phase silicon dioxide, and 2 percent of hydroxyl silicone oil and 2, 4-dichlorobenzoyl peroxide.
The invention also comprises a preparation method of the low-temperature ceramic insulating material suitable for the complex insulating structure, which is characterized by comprising the following steps:
s1, mixing wollastonite, low-melting-point glass powder, fumed silica, a functional additive and silicon rubber uniformly in proportion, and then mixing at normal temperature to obtain a mixture;
s2, vulcanizing the mixture to obtain a precursor, cutting and molding the precursor, and sintering at 1000 ℃ for a certain time;
and S3, cooling along with the furnace after sintering is finished, and taking out to obtain the material.
Further, in S1, a structure control agent is added into the silicone rubber, then the fumed silica is slowly added in batches for multiple times, after being uniformly mixed, the wollastonite and the low-melting-point glass powder are added, and finally the vulcanizing agent is added, and after being uniformly mixed, the mixture is mixed and mixed.
Further, in the vulcanization treatment, the mixture is subjected to primary vulcanization at 120 ℃ for 5-20 min, and then subjected to secondary vulcanization at 150 ℃ for 3-5 h.
Further, during sintering, aluminum oxide powder is used for burning, the heating rate is 1 ℃/min, and the heat preservation time is 1-2 h.
Compared with the preparation process of Guo Jianhua and the like, the preparation process of the invention is very similar to the preparation process of the invention because the preparation method also comprises a sintering process, but the sintering process in the patent technology obviously belongs to the detection of ceramic forming performance, the preparation of the ceramic silicon rubber composite material does not need sintering and ceramization, and only a ceramic body but not a silicon rubber composite material can be obtained after sintering. Therefore, the preparation method of the patent obviously should not include a ceramic sintering process, which is the biggest difference from the preparation method of the present invention.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. compared with the ceramic silicon rubber material invented by Guojianhua and the like, the ceramic insulating material belongs to a ceramic insulating material, and a ceramic body is flat and compact, and has excellent electrical insulating property, excellent mechanical strength, high temperature resistance, corrosion resistance and excellent heat conducting property. The ceramic silicon rubber material prepared by the patent technology belongs to a composite silicon rubber material, and only has good fireproof and flame-retardant properties, after sintering in a fire disaster, a ceramic layer is low in mechanical strength, limited in density and flatness, limited in insulating property and heat-conducting property, and required to be replaced in time after the fire disaster, and cannot meet the application requirements of severe working conditions such as high temperature, corrosion, radiation and the like;
2. compared with the existing ceramic insulating material, the ceramic insulating material has the main advantages that: the biscuit (precursor) of the ceramic insulating material before porcelain forming has good mechanical strength and excellent processability, can be easily processed and formed into a ceramic component with a complex shape, and simultaneously, the sintering temperature of the ceramic insulating material during sintering is below 1000 ℃, which is far lower than that of the existing ceramic insulating material, thereby overcoming the defects of the existing ceramic insulating material;
3. according to the invention, the precursor before porcelain forming has excellent mechanical properties of silicon rubber and is easy to extrude or mold for forming, the precursor is further processed and formed into a shape with a complex insulating structure and then sintered, and a ceramic body finished product obtained after sintering into porcelain has excellent properties of a ceramic material, corrosion resistance, high temperature resistance, radiation resistance and heat conductivity, and simultaneously, the porcelain forming temperature of the ceramic material is reduced, so that a compact ceramic body is prepared at 1000 ℃, the porcelain forming temperature is far lower than that of the traditional ceramic material, the actual application requirements are met, and the ceramic material can be widely applied to harsh working conditions of high temperature, corrosion, radiation and the like in electric power, aerospace, military, nuclear industry and the like.
Drawings
FIG. 1 is a process flow chart of a preparation method of a low-temperature ceramic insulating material suitable for a complex insulating structure according to the invention;
FIG. 2 is a macroscopic surface topography before and after the formation of porcelain of a small round sample of the ceramic insulating material of the present invention;
FIG. 3 is a macroscopic surface topography before and after the formation of porcelain of a square sample of the ceramic insulating material of the present invention;
FIG. 4 is a macroscopic surface topography of a ceramic insulating material strip specimen according to the present invention before and after formation of porcelain;
FIG. 5 is a macroscopic surface topography before and after the formation of porcelain of a large round sample of the ceramic insulating material of the present invention;
fig. 6 is an SEM image of the ceramic insulating material prepared in example 3 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A method for preparing a low-temperature ceramic insulating material suitable for a complex insulating structure, as shown in fig. 1, comprises the following steps:
s1, weighing the porcelain forming filler, the low-melting-point fluxing agent, the fumed silica, the functional additive and the methyl vinyl silicone rubber in proportion respectively for later use;
s2, because the methyl vinyl silicone rubber is soft and fluid at normal temperature, 10-20% (mass percent) of methyl vinyl silicone rubber (preferably 18%) is added at normal temperature, then the structure control agent hydroxyl silicone oil is added, and 15-30% of reinforcing agent fumed silica (preferably 22%) is added, wherein the fumed silica has low density, and the addition is easy to harden the rubber material, so the addition needs to be carried out in batches, multiple times, small amounts and slowly;
s3, mixing by using a torque rheometer, uniformly mixing methyl vinyl silicone rubber and fumed silica, adding 30-40% of porcelain forming filler wollastonite (preferably 36%) and 15-30% of fluxing agent low-melting-point glass powder (the melting point is 450 ℃, and the preferred mixing amount is 22%), finally adding 1-3% of vulcanizing agent 2, 4-dichlorobenzoyl peroxide, and taking out and weighing after all raw materials are uniformly mixed to obtain a mixture, wherein the vulcanizing agent and the structural control agent are used in a total amount of 1-3%, and the preferred mixing amount is 2%;
s4, vulcanizing the mixture, putting the weighed mixture into a flat vulcanizing machine for primary vulcanization at the primary vulcanization temperature of 120 ℃ for 10min, taking out the mixture, performing secondary vulcanization by using an electric heating blast box at the secondary vulcanization temperature of 150 ℃ for 4h to obtain a precursor, cutting the precursor for molding, and cutting the precursor into a required shape by using a special cutter during cutting molding, such as a product with a complex structure;
s5, placing the processed and molded precursor into a corundum crucible, and sintering by using an air muffle furnace during the process2O3Burying and burning the powder; in the sintering process, a temperature gradient of 50 ℃ is set from normal temperature, and the heating rate is 1 ℃ min-1Namely, the temperature is increased and is kept for 1 hour every 50 ℃, the highest sintering temperature is 1000 ℃, and then the mixture is cooled along with a furnace and taken out to obtain the ceramic material.
In order to better carry out the invention, specific examples are listed below:
example 1
A low-temperature ceramic insulating material (small round sample) suitable for a complex insulating structure is prepared by the following steps:
s1, weighing 10g of methyl vinyl silicone rubber, placing the methyl vinyl silicone rubber into a torque rheometer, adding a small amount of hydroxyl silicone oil after mixing for 5 minutes, continuing to mix for 5 minutes, slowly adding 12g of fumed silica, adding 4g of fumed silica for three times, mixing for 10 minutes after the fumed silica is added, adding 20g of wollastonite, mixing for 10 minutes, adding 12g of glass powder, continuing to mix for 10 minutes, adding 0.15g of vulcanizing agent, and taking out the mixture after mixing for 10 minutes;
s2, putting the mixture into a flat-plate vulcanizing machine for primary vulcanization, wherein the primary vulcanization temperature is 120 ℃, the time is 10min, taking out the mixture, and then carrying out secondary vulcanization by using an electric heating blower box, wherein the secondary vulcanization temperature is 150 ℃, and the time is 4h, so as to obtain a vulcanized precursor;
s3, cutting the vulcanized precursor into a small circle by using a special cutter, placing the processed and molded precursor into a corundum crucible, and sintering by using an air muffle furnace during the process, wherein Al is adopted2O3Burying and burning the powder; in the sintering process, a temperature gradient of 50 ℃ is set from normal temperature, and the heating rate is 1 ℃ min-1And the maximum sintering temperature is 1000 ℃, and then the mixture is cooled along with the furnace and taken out to obtain the ceramic material.
Example 2
A low-temperature ceramic insulating material (square sample) suitable for a complex insulating structure is prepared by the following steps:
s1, weighing 12g of methyl vinyl silicone rubber, placing the methyl vinyl silicone rubber into a torque rheometer, adding a small amount of hydroxyl silicone oil after mixing for 5 minutes, continuing to mix for 5 minutes, slowly adding 15g of fumed silica, adding 5g of fumed silica for three times, mixing for 10 minutes after the fumed silica is added, adding 24g of wollastonite, mixing for 10 minutes, adding 15g of glass powder, continuing to mix for 10 minutes, adding 0.15g of vulcanizing agent, and taking out the mixture after mixing for 10 minutes;
s2, putting the mixture into a flat-plate vulcanizing machine for primary vulcanization, wherein the primary vulcanization temperature is 120 ℃, the time is 10min, taking out the mixture, and then carrying out secondary vulcanization by using an electric heating blower box, wherein the secondary vulcanization temperature is 150 ℃, and the time is 4h, so as to obtain a vulcanized precursor;
s3, cutting the vulcanized precursor into a square shape by using a special cutter, and placing the processed and molded precursor into a corundum crucibleIn the crucible, sintering is carried out using an air muffle furnace during which Al is used2O3Burying and burning the powder; in the sintering process, a temperature gradient of 50 ℃ is set from normal temperature, and the heating rate is 1 ℃ min-1And the maximum sintering temperature is 1000 ℃, and then the mixture is cooled along with the furnace and taken out to obtain the ceramic material.
Example 3
A low-temperature ceramic insulating material (strip sample) suitable for a complex insulating structure is prepared by the following steps:
s1, weighing 10g of methyl vinyl silicone rubber, placing the methyl vinyl silicone rubber into a torque rheometer, adding a small amount of hydroxyl silicone oil after mixing for 5 minutes, continuing to mix for 5 minutes, slowly adding 12g of fumed silica, adding 4g of fumed silica for three times, mixing for 10 minutes after the fumed silica is added, adding 20g of wollastonite, mixing for 10 minutes, adding 12g of glass powder, continuing to mix for 10 minutes, adding 0.15g of vulcanizing agent, and taking out the mixture after mixing for 10 minutes;
s2, putting the mixture into a flat-plate vulcanizing machine for primary vulcanization, wherein the primary vulcanization temperature is 120 ℃, the time is 10min, taking out the mixture, and then carrying out secondary vulcanization by using an electric heating blower box, wherein the secondary vulcanization temperature is 150 ℃, and the time is 4h, so as to obtain a vulcanized precursor;
s3, cutting the vulcanized precursor into a strip shape by using a special cutter, placing the processed and molded precursor into a corundum crucible, and sintering by using an air muffle furnace during the process, wherein Al is adopted2O3Burying and burning the powder; in the sintering process, a temperature gradient of 50 ℃ is set from normal temperature, and the heating rate is 1 ℃ min-1And the maximum sintering temperature is 1000 ℃, and then the mixture is cooled along with the furnace and taken out to obtain the ceramic material.
Example 4
A low-temperature ceramic insulating material (large circular sample) suitable for a complex insulating structure is prepared by the following steps:
s1, weighing 11g of methyl vinyl silicone rubber, placing the methyl vinyl silicone rubber into a torque rheometer, adding a small amount of hydroxyl silicone oil after mixing for 5 minutes, continuing to mix for 5 minutes, slowly adding 12g of fumed silica, adding 4g of fumed silica for three times, mixing for 10 minutes after the fumed silica is added, adding 21g of wollastonite, mixing for 10 minutes, adding 12g of glass powder, continuing to mix for 10 minutes, adding 0.16g of vulcanizing agent, and taking out the mixture after mixing for 10 minutes;
s2, putting the mixture into a flat-plate vulcanizing machine for primary vulcanization, wherein the primary vulcanization temperature is 120 ℃, the time is 10min, taking out the mixture, and then carrying out secondary vulcanization by using an electric heating blower box, wherein the secondary vulcanization temperature is 150 ℃, and the time is 4h, so as to obtain a vulcanized precursor;
s3, cutting the vulcanized precursor into a large circular shape by using a special cutter, placing the processed and molded precursor into a corundum crucible, and sintering by using an air muffle furnace during the period of time, wherein Al is adopted2O3Burying and burning the powder; in the sintering process, a temperature gradient of 50 ℃ is set from normal temperature, and the heating rate is 1 ℃ min-1And the maximum sintering temperature is 1000 ℃, and then the mixture is cooled along with the furnace and taken out to obtain the ceramic material.
As shown in FIGS. 2 to 5, the samples obtained in examples 1 to 4 were as shown in FIGS. 2 to 5, and the production method of the present invention was able to produce products having various shapes, which were not significantly changed in shape and structure before and after porcelain forming, and had a linear shrinkage of 10% to 12% before and after porcelain forming. Meanwhile, the section microstructure of the ceramic insulating material prepared by the invention is in a flat and compact state as can be obtained by combining with the figure 6.
Further, the main properties of the samples obtained in examples 1 to 4 of the present invention are shown in Table 1 (all measured by standard methods):
table 1 examples 1-4 main properties of the samples
Figure BDA0003070207920000111
Figure BDA0003070207920000121
Note: the thermal diffusivity is measured at an elevated temperature from ambient temperature to 300 ℃.
As can be seen from Table 1, the density of the ceramic insulating material of the present invention is 2.15 to 2.18 g.cm-3The apparent porosity is 1.5-1.7%, the bending strength can reach 85Mpa, the linear shrinkage before and after porcelain forming is 12.06-12.21%, and the range of the thermal diffusion coefficient is 0.6mm2·s-1-0.8mm2·s-1Has a thermal conductivity in the range of 1.2 W.m-1·K-1-1.7W·m-1·K-1Volume resistivity of (3.101-3.111) × 1012Omega · m, a relative dielectric constant of 8.09 to 8.12, and a tan delta value of (9.30 to 9.38) × 10-4The power frequency breakdown field intensity is (21.01-21.31) kV · mm-1The method can be widely applied to the harsh working conditions of high temperature, corrosion, radiation and the like in the electric power industry, the aerospace industry, the military industry, the nuclear industry and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. The low-temperature ceramic insulating material suitable for the complex insulating structure is characterized by comprising the following raw materials in percentage by mass: 10-20% of silicon rubber, 30-40% of porcelain forming filler, 15-30% of low-melting-point fluxing agent, 15-30% of fumed silica, and the balance of functional additives and inevitable impurities, wherein the functional additives comprise a structural control agent and a vulcanizing agent, and the total amount of the structural control agent and the vulcanizing agent is 1-3%.
2. The low temperature, vitrified ceramic insulation suitable for complex insulation structures of claim 1 wherein the porcelainizing filler is one or more of wollastonite, mica, diatomaceous earth, kaolin, fibrous fillers.
3. The low temperature, vitrified ceramic insulation suitable for complex insulation structures according to claim 1 wherein the fluxing agent is one or more of glass frit, zinc oxide, zinc borate.
4. The low temperature ceramic insulator material according to claim 1, wherein the structural control agent is one or more of hydroxy silicone oil, diphenyldihydroxysilane, diphenyldimethoxysilane, diphenyldiethoxysilane, hexamethyldisilazane.
5. The low temperature, vitrified ceramic insulation suitable for complex insulation structures according to claim 1 wherein the vulcanizing agent is one or more of 2, 4-dichlorobenzoyl peroxide, 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane, dicumyl peroxide.
6. The low temperature, vitrified ceramic insulation suitable for complex insulation structures according to claim 1, characterized in that the ceramic insulation consists of the following raw materials in mass percent: 18 percent of methyl vinyl silicone rubber, 36 percent of wollastonite, 22 percent of low-melting-point glass powder, 22 percent of gas-phase silicon dioxide, and 2 percent of hydroxyl silicone oil and 2, 4-dichlorobenzoyl peroxide.
7. The method for preparing a low temperature ceramicized ceramic insulating material for complex insulating structures as set forth in any of claims 1 to 6, comprising the steps of:
s1, mixing wollastonite, low-melting-point glass powder, fumed silica, a functional additive and silicon rubber uniformly in proportion, and then mixing at normal temperature to obtain a mixture;
s2, vulcanizing the mixture to obtain a precursor, processing and molding the precursor, and sintering at 1000 ℃ for a certain time;
and S3, cooling along with the furnace after sintering is finished, and taking out to obtain the material.
8. The method of claim 7, wherein in S1, the silicone rubber is added with the structure control agent, then the fumed silica is slowly added in batches for a plurality of times, after mixing, the wollastonite and the low melting point glass powder are added, finally the vulcanizing agent is added, and after mixing, the mixture is mixed evenly and then mixed.
9. The method for preparing a low temperature ceramic insulating material suitable for a complex insulating structure according to claim 7, wherein the vulcanization treatment is carried out by first vulcanizing the mixture at 120 ℃ for 5-20 min and then vulcanizing it at 150 ℃ for 3-5 h.
10. The method for preparing a low-temperature porcelain ceramic insulating material suitable for a complex insulating structure according to claim 7, wherein during sintering, aluminum oxide powder is used for burying and burning, the heating rate is 1 ℃/min, and the heat preservation time is 1-2 h.
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